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CN117085347A - Fine chemical production device and process - Google Patents

Fine chemical production device and process Download PDF

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Publication number
CN117085347A
CN117085347A CN202311025488.9A CN202311025488A CN117085347A CN 117085347 A CN117085347 A CN 117085347A CN 202311025488 A CN202311025488 A CN 202311025488A CN 117085347 A CN117085347 A CN 117085347A
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CN
China
Prior art keywords
tower
reaction
light component
outlet
weight
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202311025488.9A
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Chinese (zh)
Inventor
曹德龙
滕文彬
张生安
郝小军
张仁杰
张利平
祝秀林
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong Haike Xinyuan Material Technology Co ltd
Original Assignee
Shandong Haike Xinyuan Material Technology Co ltd
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Publication date
Application filed by Shandong Haike Xinyuan Material Technology Co ltd filed Critical Shandong Haike Xinyuan Material Technology Co ltd
Priority to CN202311025488.9A priority Critical patent/CN117085347A/en
Publication of CN117085347A publication Critical patent/CN117085347A/en
Pending legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C41/00—Preparation of ethers; Preparation of compounds having groups, groups or groups
    • C07C41/01—Preparation of ethers
    • C07C41/16—Preparation of ethers by reaction of esters of mineral or organic acids with hydroxy or O-metal groups
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/32—Other features of fractionating columns ; Constructional details of fractionating columns not provided for in groups B01D3/16 - B01D3/30
    • B01D3/322—Reboiler specifications
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/42—Regulation; Control
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80—Mixing plants; Combinations of mixers
    • B01F33/836—Mixing plants; Combinations of mixers combining mixing with other treatments
    • B01F33/8362—Mixing plants; Combinations of mixers combining mixing with other treatments with chemical reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
    • B01J31/0277—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature
    • B01J31/0278—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature containing nitrogen as cationic centre
    • B01J31/0281—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature containing nitrogen as cationic centre the nitrogen being a ring member
    • B01J31/0284—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides comprising ionic liquids, as components in catalyst systems or catalysts per se, the ionic liquid compounds being used in the molten state at the respective reaction temperature containing nitrogen as cationic centre the nitrogen being a ring member of an aromatic ring, e.g. pyridinium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
    • B01J2231/40—Substitution reactions at carbon centres, e.g. C-C or C-X, i.e. carbon-hetero atom, cross-coupling, C-H activation or ring-opening reactions
    • B01J2231/42—Catalytic cross-coupling, i.e. connection of previously not connected C-atoms or C- and X-atoms without rearrangement
    • B01J2231/4277—C-X Cross-coupling, e.g. nucleophilic aromatic amination, alkoxylation or analogues
    • B01J2231/4288—C-X Cross-coupling, e.g. nucleophilic aromatic amination, alkoxylation or analogues using O nucleophiles, e.g. alcohols, carboxylates, esters

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention is suitable for the technical field of fine chemical industry, and provides a production device and a process of fine chemicals. The process is simple and efficient, the conversion rate of the ethylene carbonate is 100%, and the selectivity of the phenoxyethanol is more than 95%; the device has simple structure, convenient operation and stable and reliable product quality, can effectively reduce the device investment of phenoxyethanol and improve the market competitiveness of the product.

Description

Fine chemical production device and process
Technical Field
The invention belongs to the technical field of fine chemical industry, and particularly relates to a production device and a production process of fine chemicals.
Background
Phenoxyethanol is also called ethylene glycol phenyl ether (EPH for short) and is colorless viscous liquid with high boiling point and low volatility. EPH has wide application in the fields of medicine, daily chemicals, paint, printing ink, pesticide and the like; meanwhile, EPH is a low-sensitization, low-toxicity, stable in chemical property, efficient and broad-spectrum antiseptic bactericide, and is effective on bacteria, mold and saccharomycetes; EPH is soluble in water and oil, has excellent comprehensive properties, and is used more and more frequently in daily chemical industry.
Currently, methods for synthesizing phenoxyethanol include a chlorohydrin method, an ethylene oxide method and the like, wherein the ethylene oxide method is a main production method of industrial phenoxyethanol. The ethylene oxide method uses phenol and ethylene oxide as raw materials, and the ethylene oxide is inflammable and explosive and has carcinogenicity, so the production process has severe requirements on equipment and process.
Therefore, in view of the above-mentioned current situation, there is an urgent need to develop a simple and efficient apparatus and process for producing fine chemicals to overcome the shortcomings in the current practical application.
Disclosure of Invention
An object of an embodiment of the present invention is to provide a device and a process for producing fine chemicals, which aim to solve the problems mentioned in the background art.
The embodiment of the invention is realized in such a way that the production device of the fine chemicals comprises a raw material mixing tank, a reaction rectifying tower, a light component removing tower and a heavy component removing tower, wherein the inlet material of the raw material mixing tank is phenol, ethylene carbonate and catalyst mixed material, the material outlet of the raw material mixing tank is connected with the inlet of the reaction rectifying tower through a reaction preheater, the material outlet of the tower bottom of the reaction rectifying tower is connected with the material inlet of the light component removing tower, the material outlet of the tower bottom of the light component removing tower is connected with the material inlet of the heavy component removing tower, and the material outlet of the tower bottom of the heavy component removing tower is a catalyst concentrate outlet.
Further technical proposal, the raw material mixing tank is provided with a stirrer, and the raw material mixing tank is provided with a heating half pipe or a jacket.
According to a further technical scheme, the reaction rectifying tower is provided with a reaction condenser, a reaction reflux buffer tank and a reaction reboiler, the top of the reaction rectifying tower is connected with the inlet of the reaction reflux buffer tank through the reaction condenser, the outlet material of the reaction reflux buffer tank flows back to the top of the reaction rectifying tower, and the reaction condenser is also provided with CO 2 An outlet; and a tower bottom material outlet of the reaction rectifying tower is connected with a reaction reboiler, and outlet materials of the reaction reboiler flow back to the tower bottom of the reaction rectifying tower.
According to a further technical scheme, the light component removing tower is provided with a light component removing condenser, a light component removing reflux buffer tank and a light component removing reboiler, the top of the light component removing tower is connected with the inlet of the light component removing reflux buffer tank through the light component removing condenser, the outlet material of the light component removing reflux buffer tank is refluxed to the top of the light component removing tower, and the outlet of the light component removing reflux buffer tank further comprises a phenol outlet; and a tower bottom material outlet of the light component removing tower is connected with a light component removing reboiler, and outlet materials of the light component removing reboiler flow back to the tower bottom of the light component removing tower.
According to a further technical scheme, the de-weight tower is provided with a de-weight condenser, a de-weight reflux buffer tank and a de-weight reboiler, the top of the de-weight tower is connected with the inlet of the de-weight reflux buffer tank through the de-weight condenser, the outlet material of the de-weight reflux buffer tank flows back to the top of the de-weight tower, and the outlet of the de-weight reflux buffer tank further comprises a phenoxyethanol outlet; and a tower bottom material outlet of the heavy removal tower is connected with a heavy removal reboiler, and outlet materials of the heavy removal reboiler flow back to the tower bottom of the heavy removal tower.
According to a further technical scheme, the reaction rectifying tower is a packed tower or a plate tower, and the number of the plates is 20-40; the reaction condenser is provided with a non-condensable gas material outlet; the reaction reflux buffer tank is provided with an internal heating coil; the light component removing tower is a packed tower or a plate tower, and the number of the plates is 30-60; the light reflux buffer tank is provided with an internal heating coil; the heavy-removal tower is a packed tower or a plate tower, and the number of the plates is 30-60; the de-weight reflow buffer tank is provided with an internal heating coil.
Another object of an embodiment of the present invention is a process for producing fine chemicals, comprising the steps of:
step 1, pretreatment of raw materials
Phenol, ethylene carbonate and catalyst from the boundary area are heated and dissolved in a raw material mixing tank according to the mass ratio of 1.1-2.0:1:0.005-0.08; conveying the dissolved materials to a reaction preheater for reaction pretreatment;
step 2, synthesizing phenoxyethanol
The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to total reflux synthesis reaction of phenoxyethanol in a reaction rectifying tower, and the main reaction of the synthesis is as follows:
condensing carbon dioxide gas generated by the reaction through a reaction condenser, and then separating CO 2 The outlet is conveyed to a subsequent working section for recovery treatment; reactant mixture discharged from the tower kettle of the reaction rectifying tower is conveyed to a light component removing tower for rectifying treatment; the conversion rate of the reacted ethylene carbonate is 100 percent, and the selectivity of the phenoxyethanol is 95 to 99.5 percent;
step 3, purification of phenoxyethanol
The reaction materials from the tower bottom of the reaction rectifying tower are subjected to secondary rectifying treatment of a light component removing tower and a heavy component removing tower, so that a cosmetic grade phenoxyethanol product can be obtained, the content of the phenoxyethanol is more than or equal to 99.5%, and the content of phenol is less than 10mg/kg.
In the further technical scheme, in the step 1, the temperature of the materials heated and dissolved in the raw material mixing tank is 50-80 ℃; the temperature of the material treated by the reaction preheater is 80-110 ℃; the catalyst is an ionic liquid, and the structural formula of the catalyst is shown as follows:
wherein R1 is methyl, ethyl or propyl; r2 is butyl, amyl, hexyl, heptyl or octyl.
In the further technical scheme, in the step 2, the tower top pressure of the reaction rectifying tower is 15-100 kpa; the temperature of the material condensed by the reaction condenser is 30-50 ℃; the temperature of the tower bottom of the reaction rectifying tower is 130-190 ℃; the reaction reflux buffer tank is provided with an internal heating coil, and when the temperature of the material is lower than 20 ℃, heating is started until the temperature rises to 50 ℃, and heating is stopped.
In the further technical scheme, in the step 3, the reflux ratio of the top of the light component removal tower is 0.5-3.0, and phenol obtained from the top of the light component removal tower can be recycled; the pressure at the top of the light component removing tower is 1-15 kpa; the temperature of the material condensed by the light component removing condenser is 50-70 ℃; the temperature of the tower bottom of the light component removal tower is 100-140 ℃; the light-removal reflux buffer tank is provided with an internal heating coil, and when the temperature of the material is lower than 50 ℃, heating is started until the temperature rises to 60 ℃ and heating is stopped; the reflux ratio of the top of the de-weight tower is 0.5-3.0, and the top of the de-weight tower is the cosmetic grade phenoxyethanol; the catalyst concentrate obtained from the tower bottom of the heavy-removal tower is conveyed to a subsequent working section for recovery treatment; the pressure at the top of the heavy-removal tower is 1-15 kpa; the temperature of the material condensed by the de-duplication condenser is 30-50 ℃; the temperature of the tower bottom of the weight removing tower is 110-160 ℃; the weight-losing reflux buffer tank is provided with an internal heating coil, when the temperature of the material is lower than 20 ℃, the heating is started until the temperature rises to 30 ℃, and the heating is stopped.
The device and the process for producing the fine chemicals provided by the embodiment of the invention have the beneficial effects that:
1) The process is simple and efficient, the conversion rate of the ethylene carbonate is 100%, and the selectivity of the phenoxyethanol is more than 95%;
2) The ionic liquid catalyst provided has stable property, can be recycled, and is beneficial to industrial application;
3) The device has simple structure, convenient operation and stable and reliable product quality, can effectively reduce the device investment of phenoxyethanol and improve the market competitiveness of the product.
Drawings
Fig. 1 is a schematic structural view of a fine chemical production apparatus according to an embodiment of the present invention.
In the figure: 1-raw material mixing tank, 2-reaction rectifying tower, 3-light removal tower, 4-heavy removal tower, 5-reaction preheater, 6-reaction condenser, 7-light removal condenser, 8-heavy removal condenser, 9-reaction reflux buffer tank, 10-light removal reflux buffer tank, 11-heavy removal reflux buffer tank, 12-reaction reboiler, 13-light removal reboiler, 14-heavy removal reboiler, 15-phenol, ethylene carbonate and catalyst mixture and 16-CO 2 An outlet, a 17-phenol outlet, a 18-phenoxyethanol outlet, and a 19-catalyst concentrate outlet.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Specific implementations of the invention are described in detail below in connection with specific embodiments.
Referring to fig. 1, a production device for fine chemicals provided by an embodiment of the invention relates to phenol and ethylene carbonate as raw materials, and comprises a raw material mixing tank 1, a reaction rectifying tower 2, a light component removing tower 3 and a heavy component removing tower 4, wherein the inlet material of the raw material mixing tank 1 is phenol, ethylene carbonate and catalyst mixed material 15, the material outlet of the raw material mixing tank 1 is connected with the inlet of the reaction rectifying tower 2 through a reaction preheater 5, the material outlet of the tower bottom of the reaction rectifying tower 2 is connected with the material inlet of the light component removing tower 3, the material outlet of the tower bottom of the light component removing tower 3 is connected with the material inlet of the heavy component removing tower 4, and the material outlet of the tower bottom of the heavy component removing tower 4 is a catalyst concentrate outlet 19.
In one embodiment, the raw material mixing tank 1 is provided with a stirrer, and the raw material mixing tank 1 has a heating half pipe or a jacket.
In one embodiment, the reactive distillation column 2 is provided with a reactive condenser 6, a reactive reflux buffer tank 9 and a reactive reboiler 12, the top of the reactive distillation column 2 is connected with the inlet of the reactive reflux buffer tank 9 through the reactive condenser 6, the outlet material of the reactive reflux buffer tank 9 flows back to the top of the reactive distillation column 2, and the reactive condenser 6 is also provided with CO 2 An outlet 16; and a tower kettle material outlet of the reaction rectifying tower 2 is connected with a reaction reboiler 12, and the outlet material of the reaction reboiler 12 flows back to the tower kettle of the reaction rectifying tower 2.
Preferably, the reactive rectifying tower 2 is a packed tower or a plate tower, and the number of theoretical plates is 20-40; the reaction condenser 6 is provided with a noncondensable gas material outlet; the reaction reflux drum 9 is equipped with an internal heating coil.
In one embodiment, the light component removing tower 3 is provided with a light component removing condenser 7, a light component removing reflux buffer tank 10 and a light component removing reboiler 13, the top of the light component removing tower 3 is connected with the inlet of the light component removing reflux buffer tank 10 through the light component removing condenser 7, the outlet material of the light component removing reflux buffer tank 10 flows back to the top of the light component removing tower 3, and the outlet of the light component removing reflux buffer tank 10 also comprises a phenol outlet 17, namely the phenol is discharged; the tower kettle material outlet of the light component removing tower 3 is connected with a light component removing reboiler 13, and the outlet material of the light component removing reboiler 13 flows back to the tower kettle of the light component removing tower 3.
Preferably, the light component removing tower 3 is a packed tower or a plate tower, and the number of theoretical plates is 30-60; the light reflux drum 10 is equipped with an internal heating coil.
In one embodiment, the de-weight tower 4 is provided with a de-weight condenser 8, a de-weight reflux buffer tank 11 and a de-weight reboiler 14, the top of the de-weight tower 4 is connected with the inlet of the de-weight reflux buffer tank 11 through the de-weight condenser 8, the outlet material of the de-weight reflux buffer tank 11 flows back to the top of the de-weight tower 4, and the outlet of the de-weight reflux buffer tank 11 also comprises a phenoxyethanol outlet 18, namely, the outlet for phenoxyethanol is used for discharging; the tower kettle material outlet of the weight removing tower 4 is connected with a weight removing reboiler 14, and the outlet material of the weight removing reboiler 14 flows back to the tower kettle of the weight removing tower 4.
Preferably, the heavy-removal tower 4 is a packed tower or a plate tower, and the number of theoretical plates is 30-60; the de-weight reflux drum 11 is equipped with an internal heating coil.
As shown in fig. 1, an embodiment of the present invention also provides a process for producing fine chemicals, which is suitable for synthesizing phenol ethanol from phenol and ethylene carbonate, comprising the steps of:
step 1, pretreatment of raw materials
Phenol, ethylene carbonate and catalyst from the boundary area are heated and dissolved in a raw material mixing tank 1 according to the mass ratio of 1.1-2.0:1:0.005-0.08; the dissolved materials are conveyed to a reaction preheater 5 for reaction pretreatment;
step 2, synthesizing phenoxyethanol
The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to total reflux synthesis reaction of phenoxyethanol in a reactive rectifying tower 2, and the main reaction of the synthesis is as follows:
the carbon dioxide gas generated by the reaction is condensed by a reaction condenser 6 and then is extracted from CO 2 The outlet 16 is conveyed to a subsequent working section for recovery treatment; the reactant mixture discharged from the tower kettle of the reactive rectifying tower 2 is conveyed to a light component removing tower 3 for rectifying treatment; the conversion rate of the reacted ethylene carbonate is 100 percent, and the phenoxyethanol The selectivity of the alcohol is 95-99.5%;
step 3, purification of phenoxyethanol
The reaction materials from the tower bottom of the reaction rectifying tower 2 are subjected to secondary rectifying treatment by a light component removing tower 3 and a heavy component removing tower 4, so that a cosmetic grade phenoxyethanol product can be obtained, wherein the content of the phenoxyethanol is more than or equal to 99.5%, and the content of phenol is less than 10mg/kg.
In one embodiment, in the step 1, the temperature of the material heated and dissolved in the raw material mixing tank 1 is 50-80 ℃; the temperature of the material treated by the reaction preheater 5 is 80-110 ℃; the catalyst is an ionic liquid, and the structural formula of the catalyst is shown as follows:
wherein R1 is methyl, ethyl or propyl; r2 is butyl, amyl, hexyl, heptyl or octyl.
In one embodiment, in the step 2, the pressure at the top of the reactive distillation column 2 is 15 to 100kpa; the temperature of the material condensed by the reaction condenser 6 is 30-50 ℃; the temperature of the 2 tower bottoms of the reactive distillation tower is 130-190 ℃; the reaction reflux buffer tank 9 is provided with an internal heating coil, and when the temperature of the material is lower than 20 ℃, heating is started until the temperature rises to 50 ℃ and heating is stopped.
In one embodiment, in the step 3, the reflux ratio of the top of the light component removal tower 3 is 0.5-3.0, and the phenol obtained from the top of the light component removal tower 3 can be recycled; the pressure at the top of the light component removal tower 3 is 1-15 kpa; the temperature of the material condensed by the light component removing condenser 7 is 50-70 ℃; the temperature of the tower kettle of the light component removal tower 3 is 100-140 ℃; the light reflux drum 10 is equipped with an internal heating coil and when the temperature of the material is below 50 c, the heating is turned on until the temperature rises to 60 c and the heating is stopped.
The reflux ratio of the top of the weight removing tower 4 is 0.5-3.0, and the top of the weight removing tower 4 is the cosmetic grade phenoxyethanol; the catalyst concentrate obtained from the tower kettle of the weight removing tower 4 is conveyed to a subsequent working section for recovery treatment; the pressure at the top of the heavy-removal tower 4 is 1-15 kpa; the temperature of the material condensed by the de-duplication condenser 8 is 30-50 ℃; the temperature of the tower bottom of the weight removing tower 4 is 110-160 ℃; the de-weight reflow buffer tank 11 is provided with an internal heating coil, when the temperature of the material is lower than 20 ℃, the heating is started until the temperature rises to 30 ℃ and the heating is stopped.
Example 1
Referring to fig. 1, a production device for fine chemicals provided by an embodiment of the invention relates to phenol and ethylene carbonate as raw materials, and comprises a raw material mixing tank 1, a reaction rectifying tower 2, a light component removing tower 3 and a heavy component removing tower 4, wherein the inlet material of the raw material mixing tank 1 is phenol, ethylene carbonate and catalyst mixed material 15, the material outlet of the raw material mixing tank 1 is connected with the inlet of the reaction rectifying tower 2 through a reaction preheater 5, the material outlet of the tower bottom of the reaction rectifying tower 2 is connected with the material inlet of the light component removing tower 3, the material outlet of the tower bottom of the light component removing tower 3 is connected with the material inlet of the heavy component removing tower 4, and the material outlet of the tower bottom of the heavy component removing tower 4 is a catalyst concentrate outlet 19.
In one embodiment, the raw material mixing tank 1 is provided with a stirrer, and the raw material mixing tank 1 has a heating half pipe or a jacket.
In one embodiment, the reactive distillation column 2 is provided with a reactive condenser 6, a reactive reflux buffer tank 9 and a reactive reboiler 12, the top of the reactive distillation column 2 is connected with the inlet of the reactive reflux buffer tank 9 through the reactive condenser 6, the outlet material of the reactive reflux buffer tank 9 flows back to the top of the reactive distillation column 2, and the reactive condenser 6 is also provided with CO 2 An outlet 16; and a tower kettle material outlet of the reaction rectifying tower 2 is connected with a reaction reboiler 12, and the outlet material of the reaction reboiler 12 flows back to the tower kettle of the reaction rectifying tower 2.
Preferably, the reactive rectifying tower 2 is a packed tower or a plate tower, and the number of theoretical plates is 20; the reaction condenser 6 is provided with a noncondensable gas material outlet; the reaction reflux drum 9 is equipped with an internal heating coil.
In one embodiment, the light component removing tower 3 is provided with a light component removing condenser 7, a light component removing reflux buffer tank 10 and a light component removing reboiler 13, the top of the light component removing tower 3 is connected with the inlet of the light component removing reflux buffer tank 10 through the light component removing condenser 7, the outlet material of the light component removing reflux buffer tank 10 flows back to the top of the light component removing tower 3, and the outlet of the light component removing reflux buffer tank 10 also comprises a phenol outlet 17, namely the phenol is discharged; the tower kettle material outlet of the light component removing tower 3 is connected with a light component removing reboiler 13, and the outlet material of the light component removing reboiler 13 flows back to the tower kettle of the light component removing tower 3.
Preferably, the light component removing tower 3 is a packed tower or a plate tower, and the number of theoretical plates is 30; the light reflux drum 10 is equipped with an internal heating coil.
In one embodiment, the de-weight tower 4 is provided with a de-weight condenser 8, a de-weight reflux buffer tank 11 and a de-weight reboiler 14, the top of the de-weight tower 4 is connected with the inlet of the de-weight reflux buffer tank 11 through the de-weight condenser 8, the outlet material of the de-weight reflux buffer tank 11 flows back to the top of the de-weight tower 4, and the outlet of the de-weight reflux buffer tank 11 also comprises a phenoxyethanol outlet 18, namely, the outlet for phenoxyethanol is used for discharging; the tower kettle material outlet of the weight removing tower 4 is connected with a weight removing reboiler 14, and the outlet material of the weight removing reboiler 14 flows back to the tower kettle of the weight removing tower 4.
Preferably, the heavy-removal tower 4 is a packed tower or a plate tower, and the number of theoretical plates is 30; the de-weight reflux drum 11 is equipped with an internal heating coil.
As shown in fig. 1, an embodiment of the present invention also provides a process for producing fine chemicals, which is suitable for synthesizing phenol ethanol from phenol and ethylene carbonate, comprising the steps of:
step 1, pretreatment of raw materials
Phenol, ethylene carbonate and catalyst from the boundary zone are heated and dissolved in the raw material mixing tank 1 according to the mass ratio of 1.1:1:0.005; the dissolved materials are conveyed to a reaction preheater 5 for reaction pretreatment;
Step 2, synthesizing phenoxyethanol
The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to total reflux synthesis reaction of phenoxyethanol in a reactive rectifying tower 2, and the main reaction of the synthesis is as follows:
the carbon dioxide gas generated by the reaction is condensed by a reaction condenser 6 and then is extracted from CO 2 The outlet 16 is conveyed to a subsequent working section for recovery treatment; the reactant mixture discharged from the tower kettle of the reactive rectifying tower 2 is conveyed to a light component removing tower 3 for rectifying treatment; the conversion rate of the reacted ethylene carbonate is 100 percent, and the selectivity of the phenoxyethanol is 96.5 percent;
step 3, purification of phenoxyethanol
The reaction materials from the tower bottom of the reaction rectifying tower 2 are subjected to secondary rectification treatment of the light component removing tower 3 and the heavy component removing tower 4, so that a cosmetic grade phenoxyethanol product can be obtained, the content of the phenoxyethanol is 99.65%, and the content of phenol is 4.5mg/kg.
In one embodiment, in step 1, the material temperature after heating and dissolution of the raw material mixing tank 1 is 50 ℃; the temperature of the material treated by the reaction preheater 5 is 80 ℃; the catalyst is an ionic liquid, and the structural formula of the catalyst is shown as follows:
wherein R1 is methyl; r2 is butyl.
In one embodiment, in step 2, the reactive distillation column 2 overhead pressure is 15kpa; the temperature of the material condensed by the reaction condenser 6 is 30 ℃; the temperature of the 2 tower bottoms of the reactive rectifying tower is 130 ℃; the reaction reflux buffer tank 9 is provided with an internal heating coil, and when the temperature of the material is lower than 20 ℃, heating is started until the temperature rises to 50 ℃ and heating is stopped.
In one embodiment, in the step 3, the reflux ratio of the top of the light component removal tower 3 is 0.5, and the phenol obtained from the top of the light component removal tower 3 can be recycled; the tower top pressure of the light component removing tower 3 is 1kpa; the temperature of the material condensed by the light component removing condenser 7 is 50 ℃; the temperature of the tower kettle of the light component removal tower 3 is 100 ℃; the light reflux drum 10 is equipped with an internal heating coil and when the temperature of the material is below 50 c, the heating is turned on until the temperature rises to 60 c and the heating is stopped.
The reflux ratio of the top of the weight removing tower 4 is 0.5, and the top of the weight removing tower 4 is the cosmetic grade phenoxyethanol; the catalyst concentrate obtained from the tower kettle of the weight removing tower 4 is conveyed to a subsequent working section for recovery treatment; the pressure at the top of the heavy-removal tower 4 is 1kpa; the temperature of the material condensed by the de-duplication condenser 8 is 30 ℃; the temperature of the tower bottom of the weight removing tower 4 is 110 ℃; the de-weight reflow buffer tank 11 is provided with an internal heating coil, when the temperature of the material is lower than 20 ℃, the heating is started until the temperature rises to 30 ℃ and the heating is stopped.
Example 2
Referring to fig. 1, a production device for fine chemicals provided by an embodiment of the invention relates to phenol and ethylene carbonate as raw materials, and comprises a raw material mixing tank 1, a reaction rectifying tower 2, a light component removing tower 3 and a heavy component removing tower 4, wherein the inlet material of the raw material mixing tank 1 is phenol, ethylene carbonate and catalyst mixed material 15, the material outlet of the raw material mixing tank 1 is connected with the inlet of the reaction rectifying tower 2 through a reaction preheater 5, the material outlet of the tower bottom of the reaction rectifying tower 2 is connected with the material inlet of the light component removing tower 3, the material outlet of the tower bottom of the light component removing tower 3 is connected with the material inlet of the heavy component removing tower 4, and the material outlet of the tower bottom of the heavy component removing tower 4 is a catalyst concentrate outlet 19.
In one embodiment, the raw material mixing tank 1 is provided with a stirrer, and the raw material mixing tank 1 has a heating half pipe or a jacket.
In one embodiment, the reactive distillation column 2 is provided with a reactive condenser 6, a reactive reflux buffer tank 9 and a reactive reboiler 12, the top of the reactive distillation column 2 is connected with the inlet of the reactive reflux buffer tank 9 through the reactive condenser 6, the outlet material of the reactive reflux buffer tank 9 flows back to the top of the reactive distillation column 2, and the reactive condenser 6 is also provided with CO 2 An outlet 16; and a tower kettle material outlet of the reaction rectifying tower 2 is connected with a reaction reboiler 12, and the outlet material of the reaction reboiler 12 flows back to the tower kettle of the reaction rectifying tower 2.
Preferably, the reactive rectifying tower 2 is a packed tower or a plate tower, and the number of theoretical plates is 30; the reaction condenser 6 is provided with a noncondensable gas material outlet; the reaction reflux drum 9 is equipped with an internal heating coil.
In one embodiment, the light component removing tower 3 is provided with a light component removing condenser 7, a light component removing reflux buffer tank 10 and a light component removing reboiler 13, the top of the light component removing tower 3 is connected with the inlet of the light component removing reflux buffer tank 10 through the light component removing condenser 7, the outlet material of the light component removing reflux buffer tank 10 flows back to the top of the light component removing tower 3, and the outlet of the light component removing reflux buffer tank 10 also comprises a phenol outlet 17, namely the phenol is discharged; the tower kettle material outlet of the light component removing tower 3 is connected with a light component removing reboiler 13, and the outlet material of the light component removing reboiler 13 flows back to the tower kettle of the light component removing tower 3.
Preferably, the light component removing tower 3 is a packed tower or a plate tower, and the number of theoretical plates is 50; the light reflux drum 10 is equipped with an internal heating coil.
In one embodiment, the de-weight tower 4 is provided with a de-weight condenser 8, a de-weight reflux buffer tank 11 and a de-weight reboiler 14, the top of the de-weight tower 4 is connected with the inlet of the de-weight reflux buffer tank 11 through the de-weight condenser 8, the outlet material of the de-weight reflux buffer tank 11 flows back to the top of the de-weight tower 4, and the outlet of the de-weight reflux buffer tank 11 also comprises a phenoxyethanol outlet 18, namely, the outlet for phenoxyethanol is used for discharging; the tower kettle material outlet of the weight removing tower 4 is connected with a weight removing reboiler 14, and the outlet material of the weight removing reboiler 14 flows back to the tower kettle of the weight removing tower 4.
Preferably, the heavy-removal tower 4 is a packed tower or a plate tower, and the number of theoretical plates is 50; the de-weight reflux drum 11 is equipped with an internal heating coil.
As shown in fig. 1, an embodiment of the present invention also provides a process for producing fine chemicals, which is suitable for synthesizing phenol ethanol from phenol and ethylene carbonate, comprising the steps of:
step 1, pretreatment of raw materials
Phenol, ethylene carbonate and catalyst from the boundary zone are heated and dissolved in a raw material mixing tank 1 according to the mass ratio of 1.5:1:0.02; the dissolved materials are conveyed to a reaction preheater 5 for reaction pretreatment;
Step 2, synthesizing phenoxyethanol
The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to total reflux synthesis reaction of phenoxyethanol in a reactive rectifying tower 2, and the main reaction of the synthesis is as follows:
the carbon dioxide gas generated by the reaction is condensed by a reaction condenser 6 and then is extracted from CO 2 The outlet 16 is conveyed to a subsequent working section for recovery treatment; the reactant mixture discharged from the tower kettle of the reactive rectifying tower 2 is conveyed to a light component removing tower 3 for rectifying treatment; the conversion rate of the reacted ethylene carbonate is 100 percent, and the selectivity of the phenoxyethanol is 99.5 percent;
step 3, purification of phenoxyethanol
The reaction materials from the tower bottom of the reaction rectifying tower 2 are subjected to secondary rectification treatment of the light component removing tower 3 and the heavy component removing tower 4, so that a cosmetic grade phenoxyethanol product can be obtained, the content of the phenoxyethanol is 99.62%, and the content of the phenol is 2.3mg/kg.
In one embodiment, in step 1, the material temperature after heating and dissolution of the raw material mixing tank 1 is 70 ℃; the temperature of the material treated by the reaction preheater 5 is 100 ℃; the catalyst is an ionic liquid, and the structural formula of the catalyst is shown as follows:
wherein R1 is methyl; r2 is amyl.
In one embodiment, in step 2, the reactive distillation column 2 overhead pressure is 50kpa; the temperature of the material condensed by the reaction condenser 6 is 40 ℃; the temperature of the tower bottom of the reactive rectifying tower 2 is 160 ℃; the reaction reflux buffer tank 9 is provided with an internal heating coil, and when the temperature of the material is lower than 20 ℃, heating is started until the temperature rises to 50 ℃ and heating is stopped.
In one embodiment, in the step 3, the reflux ratio of the top of the light component removal tower 3 is 1.5, and the phenol obtained from the top of the light component removal tower 3 can be recycled; the pressure at the top of the light component removal tower 3 is 8kpa; the temperature of the material condensed by the light component removing condenser 7 is 60 ℃; the temperature of the tower kettle of the light component removal tower 3 is 120 ℃; the light reflux drum 10 is equipped with an internal heating coil and when the temperature of the material is below 50 c, the heating is turned on until the temperature rises to 60 c and the heating is stopped.
The reflux ratio of the top of the weight removing tower 4 is 2.0, and the top of the weight removing tower 4 is the cosmetic grade phenoxyethanol; the catalyst concentrate obtained from the tower kettle of the weight removing tower 4 is conveyed to a subsequent working section for recovery treatment; the pressure at the top of the heavy-removal tower 4 is 8kpa; the temperature of the material condensed by the de-duplication condenser 8 is 40 ℃; the temperature of the tower bottom of the weight removing tower 4 is 140 ℃; the de-weight reflow buffer tank 11 is provided with an internal heating coil, when the temperature of the material is lower than 20 ℃, the heating is started until the temperature rises to 30 ℃ and the heating is stopped.
Example 3
Referring to fig. 1, a production device for fine chemicals provided by an embodiment of the invention relates to phenol and ethylene carbonate as raw materials, and comprises a raw material mixing tank 1, a reaction rectifying tower 2, a light component removing tower 3 and a heavy component removing tower 4, wherein the inlet material of the raw material mixing tank 1 is phenol, ethylene carbonate and catalyst mixed material 15, the material outlet of the raw material mixing tank 1 is connected with the inlet of the reaction rectifying tower 2 through a reaction preheater 5, the material outlet of the tower bottom of the reaction rectifying tower 2 is connected with the material inlet of the light component removing tower 3, the material outlet of the tower bottom of the light component removing tower 3 is connected with the material inlet of the heavy component removing tower 4, and the material outlet of the tower bottom of the heavy component removing tower 4 is a catalyst concentrate outlet 19.
In one embodiment, the raw material mixing tank 1 is provided with a stirrer, and the raw material mixing tank 1 has a heating half pipe or a jacket.
In one embodiment, the reactive distillation column 2 is provided with a reactive condenser 6, a reactive reflux buffer tank 9 and a reactive reboiler 12, and the top of the reactive distillation column 2 is connected with the reactive distillation column through the reactive condenser 6The inlet of the reflux buffer tank 9 is connected, the outlet material of the reflux buffer tank 9 is refluxed to the top of the reactive rectifying tower 2, and the reactive condenser 6 is also provided with CO 2 An outlet 16; and a tower kettle material outlet of the reaction rectifying tower 2 is connected with a reaction reboiler 12, and the outlet material of the reaction reboiler 12 flows back to the tower kettle of the reaction rectifying tower 2.
Preferably, the reactive rectifying tower 2 is a packed tower or a plate tower, and the number of theoretical plates is 40; the reaction condenser 6 is provided with a noncondensable gas material outlet; the reaction reflux drum 9 is equipped with an internal heating coil.
In one embodiment, the light component removing tower 3 is provided with a light component removing condenser 7, a light component removing reflux buffer tank 10 and a light component removing reboiler 13, the top of the light component removing tower 3 is connected with the inlet of the light component removing reflux buffer tank 10 through the light component removing condenser 7, the outlet material of the light component removing reflux buffer tank 10 flows back to the top of the light component removing tower 3, and the outlet of the light component removing reflux buffer tank 10 also comprises a phenol outlet 17, namely the phenol is discharged; the tower kettle material outlet of the light component removing tower 3 is connected with a light component removing reboiler 13, and the outlet material of the light component removing reboiler 13 flows back to the tower kettle of the light component removing tower 3.
Preferably, the light component removing tower 3 is a packed tower or a plate tower, and the number of theoretical plates is 60; the light reflux drum 10 is equipped with an internal heating coil.
In one embodiment, the de-weight tower 4 is provided with a de-weight condenser 8, a de-weight reflux buffer tank 11 and a de-weight reboiler 14, the top of the de-weight tower 4 is connected with the inlet of the de-weight reflux buffer tank 11 through the de-weight condenser 8, the outlet material of the de-weight reflux buffer tank 11 flows back to the top of the de-weight tower 4, and the outlet of the de-weight reflux buffer tank 11 also comprises a phenoxyethanol outlet 18, namely, the outlet for phenoxyethanol is used for discharging; the tower kettle material outlet of the weight removing tower 4 is connected with a weight removing reboiler 14, and the outlet material of the weight removing reboiler 14 flows back to the tower kettle of the weight removing tower 4.
Preferably, the heavy-removal tower 4 is a packed tower or a plate tower, and the number of theoretical plates is 60; the de-weight reflux drum 11 is equipped with an internal heating coil.
As shown in fig. 1, an embodiment of the present invention also provides a process for producing fine chemicals, which is suitable for synthesizing phenol ethanol from phenol and ethylene carbonate, comprising the steps of:
step 1, pretreatment of raw materials
Phenol, ethylene carbonate and catalyst from the boundary zone are heated and dissolved in a raw material mixing tank 1 according to the mass ratio of 2:1:0.08; the dissolved materials are conveyed to a reaction preheater 5 for reaction pretreatment;
Step 2, synthesizing phenoxyethanol
The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to total reflux synthesis reaction of phenoxyethanol in a reactive rectifying tower 2, and the main reaction of the synthesis is as follows:
the carbon dioxide gas generated by the reaction is condensed by a reaction condenser 6 and then is extracted from CO 2 The outlet 16 is conveyed to a subsequent working section for recovery treatment; the reactant mixture discharged from the tower kettle of the reactive rectifying tower 2 is conveyed to a light component removing tower 3 for rectifying treatment; the conversion rate of the reacted ethylene carbonate is 100 percent, and the selectivity of the phenoxyethanol is 97.4 percent;
step 3, purification of phenoxyethanol
The reaction materials from the tower bottom of the reaction rectifying tower 2 are subjected to secondary rectification treatment of a light component removing tower 3 and a heavy component removing tower 4, so that a cosmetic grade phenoxyethanol product can be obtained, the content of the phenoxyethanol is 99.96%, and the content of phenol is 1.6mg/kg.
In one embodiment, in step 1, the material temperature after heating and dissolution of the raw material mixing tank 1 is 80 ℃; the temperature of the material treated by the reaction preheater 5 is 110 ℃; the catalyst is an ionic liquid, and the structural formula of the catalyst is shown as follows:
wherein R1 is methyl; r2 is hexyl.
In one embodiment, in step 2, the reactive distillation column 2 overhead pressure is 100kpa; the temperature of the material condensed by the reaction condenser 6 is 50 ℃; the temperature of the 2 tower bottoms of the reactive rectifying tower is 190 ℃; the reaction reflux buffer tank 9 is provided with an internal heating coil, and when the temperature of the material is lower than 20 ℃, heating is started until the temperature rises to 50 ℃ and heating is stopped.
In one embodiment, in the step 3, the reflux ratio of the top of the light component removal tower 3 is 3.0, and the phenol obtained from the top of the light component removal tower 3 can be recycled; the tower top pressure of the light component removing tower 3 is 15kpa; the temperature of the material condensed by the light component removing condenser 7 is 70 ℃; the temperature of the tower kettle of the light component removal tower 3 is 140 ℃; the light reflux drum 10 is equipped with an internal heating coil and when the temperature of the material is below 50 c, the heating is turned on until the temperature rises to 60 c and the heating is stopped.
The reflux ratio of the top of the weight removing tower 4 is 3.0, and the top of the weight removing tower 4 is the cosmetic grade phenoxyethanol; the catalyst concentrate obtained from the tower kettle of the weight removing tower 4 is conveyed to a subsequent working section for recovery treatment; the tower top pressure of the heavy-removal tower 4 is 15kpa; the temperature of the material condensed by the de-duplication condenser 8 is 50 ℃; the temperature of the tower bottom of the weight removing tower 4 is 160 ℃; the de-weight reflow buffer tank 11 is provided with an internal heating coil, when the temperature of the material is lower than 20 ℃, the heating is started until the temperature rises to 30 ℃ and the heating is stopped.
Example 4
Referring to fig. 1, a production device for fine chemicals provided by an embodiment of the invention relates to phenol and ethylene carbonate as raw materials, and comprises a raw material mixing tank 1, a reaction rectifying tower 2, a light component removing tower 3 and a heavy component removing tower 4, wherein the inlet material of the raw material mixing tank 1 is phenol, ethylene carbonate and catalyst mixed material 15, the material outlet of the raw material mixing tank 1 is connected with the inlet of the reaction rectifying tower 2 through a reaction preheater 5, the material outlet of the tower bottom of the reaction rectifying tower 2 is connected with the material inlet of the light component removing tower 3, the material outlet of the tower bottom of the light component removing tower 3 is connected with the material inlet of the heavy component removing tower 4, and the material outlet of the tower bottom of the heavy component removing tower 4 is a catalyst concentrate outlet 19.
In one embodiment, the raw material mixing tank 1 is provided with a stirrer, and the raw material mixing tank 1 has a heating half pipe or a jacket.
In one embodiment, the reactive distillation column 2 is provided with a reactive condenser 6, a reactive reflux buffer tank 9 and a reactive reboiler 12, the top of the reactive distillation column 2 is connected with the inlet of the reactive reflux buffer tank 9 through the reactive condenser 6, the outlet material of the reactive reflux buffer tank 9 flows back to the top of the reactive distillation column 2, and the reactive condenser 6 is also provided with CO 2 An outlet 16; and a tower kettle material outlet of the reaction rectifying tower 2 is connected with a reaction reboiler 12, and the outlet material of the reaction reboiler 12 flows back to the tower kettle of the reaction rectifying tower 2.
Preferably, the reactive rectifying tower 2 is a packed tower or a plate tower, and the number of theoretical plates is 30; the reaction condenser 6 is provided with a noncondensable gas material outlet; the reaction reflux drum 9 is equipped with an internal heating coil.
In one embodiment, the light component removing tower 3 is provided with a light component removing condenser 7, a light component removing reflux buffer tank 10 and a light component removing reboiler 13, the top of the light component removing tower 3 is connected with the inlet of the light component removing reflux buffer tank 10 through the light component removing condenser 7, the outlet material of the light component removing reflux buffer tank 10 flows back to the top of the light component removing tower 3, and the outlet of the light component removing reflux buffer tank 10 also comprises a phenol outlet 17, namely the phenol is discharged; the tower kettle material outlet of the light component removing tower 3 is connected with a light component removing reboiler 13, and the outlet material of the light component removing reboiler 13 flows back to the tower kettle of the light component removing tower 3.
Preferably, the light component removing tower 3 is a packed tower or a plate tower, and the number of theoretical plates is 45; the light reflux drum 10 is equipped with an internal heating coil.
In one embodiment, the de-weight tower 4 is provided with a de-weight condenser 8, a de-weight reflux buffer tank 11 and a de-weight reboiler 14, the top of the de-weight tower 4 is connected with the inlet of the de-weight reflux buffer tank 11 through the de-weight condenser 8, the outlet material of the de-weight reflux buffer tank 11 flows back to the top of the de-weight tower 4, and the outlet of the de-weight reflux buffer tank 11 also comprises a phenoxyethanol outlet 18, namely, the outlet for phenoxyethanol is used for discharging; the tower kettle material outlet of the weight removing tower 4 is connected with a weight removing reboiler 14, and the outlet material of the weight removing reboiler 14 flows back to the tower kettle of the weight removing tower 4.
Preferably, the heavy-removal tower 4 is a packed tower or a plate tower, and the number of theoretical plates is 45; the de-weight reflux drum 11 is equipped with an internal heating coil.
As shown in fig. 1, an embodiment of the present invention also provides a process for producing fine chemicals, which is suitable for synthesizing phenol ethanol from phenol and ethylene carbonate, comprising the steps of:
step 1, pretreatment of raw materials
Phenol, ethylene carbonate and catalyst from the boundary zone are heated and dissolved in the raw material mixing tank 1 according to the mass ratio of 1.6:1:0.03; the dissolved materials are conveyed to a reaction preheater 5 for reaction pretreatment;
Step 2, synthesizing phenoxyethanol
The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to total reflux synthesis reaction of phenoxyethanol in a reactive rectifying tower 2, and the main reaction of the synthesis is as follows:
the carbon dioxide gas generated by the reaction is condensed by a reaction condenser 6 and then is extracted from CO 2 The outlet 16 is conveyed to a subsequent working section for recovery treatment; the reactant mixture discharged from the tower kettle of the reactive rectifying tower 2 is conveyed to a light component removing tower 3 for rectifying treatment; the conversion rate of the reacted ethylene carbonate is 100 percent, and the selectivity of the phenoxyethanol is 99.1 percent;
step 3, purification of phenoxyethanol
The reaction materials from the tower bottom of the reaction rectifying tower 2 are subjected to secondary rectification treatment of a light component removing tower 3 and a heavy component removing tower 4, so that a cosmetic grade phenoxyethanol product can be obtained, the content of the phenoxyethanol is 99.84%, and the content of phenol is 1.1mg/kg.
In one embodiment, in step 1, the material temperature after heating and dissolution of the raw material mixing tank 1 is 70 ℃; the temperature of the material treated by the reaction preheater 5 is 100 ℃; the catalyst is an ionic liquid, and the structural formula of the catalyst is shown as follows:
wherein R1 is ethyl; r2 is hexyl.
In one embodiment, in step 2, the reactive distillation column 2 overhead pressure is 60kpa; the temperature of the material condensed by the reaction condenser 6 is 40 ℃; the temperature of the tower bottom of the reactive rectifying tower 2 is 160 ℃; the reaction reflux buffer tank 9 is provided with an internal heating coil, and when the temperature of the material is lower than 20 ℃, heating is started until the temperature rises to 50 ℃ and heating is stopped.
In one embodiment, in the step 3, the reflux ratio of the top of the light component removal tower 3 is 2.0, and the phenol obtained from the top of the light component removal tower 3 can be recycled; the tower top pressure of the light component removing tower 3 is 9kpa; the temperature of the material condensed by the light component removing condenser 7 is 60 ℃; the temperature of the tower kettle of the light component removal tower 3 is 120 ℃; the light reflux drum 10 is equipped with an internal heating coil and when the temperature of the material is below 50 c, the heating is turned on until the temperature rises to 60 c and the heating is stopped.
The reflux ratio of the top of the weight removing tower 4 is 2.0, and the top of the weight removing tower 4 is the cosmetic grade phenoxyethanol; the catalyst concentrate obtained from the tower kettle of the weight removing tower 4 is conveyed to a subsequent working section for recovery treatment; the pressure at the top of the heavy-removal tower 4 is 9kpa; the temperature of the material condensed by the de-duplication condenser 8 is 40 ℃; the temperature of the tower bottom of the weight removing tower 4 is 140 ℃; the de-weight reflow buffer tank 11 is provided with an internal heating coil, when the temperature of the material is lower than 20 ℃, the heating is started until the temperature rises to 30 ℃ and the heating is stopped.
Example 5
Referring to fig. 1, a production device for fine chemicals provided by an embodiment of the invention relates to phenol and ethylene carbonate as raw materials, and comprises a raw material mixing tank 1, a reaction rectifying tower 2, a light component removing tower 3 and a heavy component removing tower 4, wherein the inlet material of the raw material mixing tank 1 is phenol, ethylene carbonate and catalyst mixed material 15, the material outlet of the raw material mixing tank 1 is connected with the inlet of the reaction rectifying tower 2 through a reaction preheater 5, the material outlet of the tower bottom of the reaction rectifying tower 2 is connected with the material inlet of the light component removing tower 3, the material outlet of the tower bottom of the light component removing tower 3 is connected with the material inlet of the heavy component removing tower 4, and the material outlet of the tower bottom of the heavy component removing tower 4 is a catalyst concentrate outlet 19.
In one embodiment, the raw material mixing tank 1 is provided with a stirrer, and the raw material mixing tank 1 has a heating half pipe or a jacket.
In one embodiment, the reactive distillation column 2 is provided with a reactive condenser 6, a reactive reflux buffer tank 9 and a reactive reboiler 12, the top of the reactive distillation column 2 is connected with the inlet of the reactive reflux buffer tank 9 through the reactive condenser 6, the outlet material of the reactive reflux buffer tank 9 flows back to the top of the reactive distillation column 2, and the reactive condenser 6 is also provided with CO 2 An outlet 16; and a tower kettle material outlet of the reaction rectifying tower 2 is connected with a reaction reboiler 12, and the outlet material of the reaction reboiler 12 flows back to the tower kettle of the reaction rectifying tower 2.
Preferably, the reactive rectifying tower 2 is a packed tower or a plate tower, and the number of theoretical plates is 30; the reaction condenser 6 is provided with a noncondensable gas material outlet; the reaction reflux drum 9 is equipped with an internal heating coil.
In one embodiment, the light component removing tower 3 is provided with a light component removing condenser 7, a light component removing reflux buffer tank 10 and a light component removing reboiler 13, the top of the light component removing tower 3 is connected with the inlet of the light component removing reflux buffer tank 10 through the light component removing condenser 7, the outlet material of the light component removing reflux buffer tank 10 flows back to the top of the light component removing tower 3, and the outlet of the light component removing reflux buffer tank 10 also comprises a phenol outlet 17, namely the phenol is discharged; the tower kettle material outlet of the light component removing tower 3 is connected with a light component removing reboiler 13, and the outlet material of the light component removing reboiler 13 flows back to the tower kettle of the light component removing tower 3.
Preferably, the light component removing tower 3 is a packed tower or a plate tower, and the number of theoretical plates is 50; the light reflux drum 10 is equipped with an internal heating coil.
In one embodiment, the de-weight tower 4 is provided with a de-weight condenser 8, a de-weight reflux buffer tank 11 and a de-weight reboiler 14, the top of the de-weight tower 4 is connected with the inlet of the de-weight reflux buffer tank 11 through the de-weight condenser 8, the outlet material of the de-weight reflux buffer tank 11 flows back to the top of the de-weight tower 4, and the outlet of the de-weight reflux buffer tank 11 also comprises a phenoxyethanol outlet 18, namely, the outlet for phenoxyethanol is used for discharging; the tower kettle material outlet of the weight removing tower 4 is connected with a weight removing reboiler 14, and the outlet material of the weight removing reboiler 14 flows back to the tower kettle of the weight removing tower 4.
Preferably, the heavy-removal tower 4 is a packed tower or a plate tower, and the number of theoretical plates is 50; the de-weight reflux drum 11 is equipped with an internal heating coil.
As shown in fig. 1, an embodiment of the present invention also provides a process for producing fine chemicals, which is suitable for synthesizing phenol ethanol from phenol and ethylene carbonate, comprising the steps of:
step 1, pretreatment of raw materials
Phenol, ethylene carbonate and catalyst from the interfacial zone in a mass ratio of 1.7:1:0.05 are heated and dissolved in a raw material mixing tank 1; the dissolved materials are conveyed to a reaction preheater 5 for reaction pretreatment;
Step 2, synthesizing phenoxyethanol
The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to total reflux synthesis reaction of phenoxyethanol in a reactive rectifying tower 2, and the main reaction of the synthesis is as follows:
the carbon dioxide gas generated by the reaction is condensed by a reaction condenser 6 and then is extracted from CO 2 The outlet 16 is conveyed to a subsequent working section for recovery treatment; the reactant mixture discharged from the tower kettle of the reactive rectifying tower 2 is conveyed to a light component removing tower 3 for rectifying treatment; the conversion rate of the reacted ethylene carbonate is 100 percent, and the selectivity of the phenoxyethanol is 98.3 percent;
step 3, purification of phenoxyethanol
The reaction materials from the tower bottom of the reaction rectifying tower 2 are subjected to secondary rectification treatment of a light component removing tower 3 and a heavy component removing tower 4, so that a cosmetic grade phenoxyethanol product can be obtained, the content of the phenoxyethanol is 99.59%, and the content of phenol is 0.9mg/kg.
In one embodiment, in step 1, the material temperature after heating and dissolution of the raw material mixing tank 1 is 70 ℃; the temperature of the material treated by the reaction preheater 5 is 100 ℃; the catalyst is an ionic liquid, and the structural formula of the catalyst is shown as follows:
wherein R1 is ethyl; r2 is heptyl.
In one embodiment, in step 2, the reactive distillation column 2 overhead pressure is 60kpa; the temperature of the material condensed by the reaction condenser 6 is 40 ℃; the temperature of the tower bottom of the reactive rectifying tower 2 is 160 ℃; the reaction reflux buffer tank 9 is provided with an internal heating coil, and when the temperature of the material is lower than 20 ℃, heating is started until the temperature rises to 50 ℃ and heating is stopped.
In one embodiment, in the step 3, the reflux ratio of the top of the light component removal tower 3 is 2.0, and the phenol obtained from the top of the light component removal tower 3 can be recycled; the pressure at the top of the light component removal tower 3 is 8kpa; the temperature of the material condensed by the light component removing condenser 7 is 60 ℃; the temperature of the tower kettle of the light component removal tower 3 is 120 ℃; the light reflux drum 10 is equipped with an internal heating coil and when the temperature of the material is below 50 c, the heating is turned on until the temperature rises to 60 c and the heating is stopped.
The reflux ratio of the top of the weight removing tower 4 is 2.0, and the top of the weight removing tower 4 is the cosmetic grade phenoxyethanol; the catalyst concentrate obtained from the tower kettle of the weight removing tower 4 is conveyed to a subsequent working section for recovery treatment; the pressure at the top of the heavy-removal tower 4 is 8kpa; the temperature of the material condensed by the de-duplication condenser 8 is 40 ℃; the temperature of the tower bottom of the weight removing tower 4 is 140 ℃; the de-weight reflow buffer tank 11 is provided with an internal heating coil, when the temperature of the material is lower than 20 ℃, the heating is started until the temperature rises to 30 ℃ and the heating is stopped.
Example 6
Referring to fig. 1, a production device for fine chemicals provided by an embodiment of the invention relates to phenol and ethylene carbonate as raw materials, and comprises a raw material mixing tank 1, a reaction rectifying tower 2, a light component removing tower 3 and a heavy component removing tower 4, wherein the inlet material of the raw material mixing tank 1 is phenol, ethylene carbonate and catalyst mixed material 15, the material outlet of the raw material mixing tank 1 is connected with the inlet of the reaction rectifying tower 2 through a reaction preheater 5, the material outlet of the tower bottom of the reaction rectifying tower 2 is connected with the material inlet of the light component removing tower 3, the material outlet of the tower bottom of the light component removing tower 3 is connected with the material inlet of the heavy component removing tower 4, and the material outlet of the tower bottom of the heavy component removing tower 4 is a catalyst concentrate outlet 19.
In one embodiment, the raw material mixing tank 1 is provided with a stirrer, and the raw material mixing tank 1 has a heating half pipe or a jacket.
In one embodiment, the reactive distillation column 2 is provided with a reactive condenser 6, a reactive reflux buffer tank 9 and a reactive reboiler 12, the top of the reactive distillation column 2 is connected with the inlet of the reactive reflux buffer tank 9 through the reactive condenser 6, the outlet material of the reactive reflux buffer tank 9 flows back to the top of the reactive distillation column 2, and the reactive condenser 6 is also provided with CO 2 An outlet 16; and a tower kettle material outlet of the reaction rectifying tower 2 is connected with a reaction reboiler 12, and the outlet material of the reaction reboiler 12 flows back to the tower kettle of the reaction rectifying tower 2.
Preferably, the reactive rectifying tower 2 is a packed tower or a plate tower, and the number of theoretical plates is 30; the reaction condenser 6 is provided with a noncondensable gas material outlet; the reaction reflux drum 9 is equipped with an internal heating coil.
In one embodiment, the light component removing tower 3 is provided with a light component removing condenser 7, a light component removing reflux buffer tank 10 and a light component removing reboiler 13, the top of the light component removing tower 3 is connected with the inlet of the light component removing reflux buffer tank 10 through the light component removing condenser 7, the outlet material of the light component removing reflux buffer tank 10 flows back to the top of the light component removing tower 3, and the outlet of the light component removing reflux buffer tank 10 also comprises a phenol outlet 17, namely the phenol is discharged; the tower kettle material outlet of the light component removing tower 3 is connected with a light component removing reboiler 13, and the outlet material of the light component removing reboiler 13 flows back to the tower kettle of the light component removing tower 3.
Preferably, the light component removing tower 3 is a packed tower or a plate tower, and the number of theoretical plates is 50; the light reflux drum 10 is equipped with an internal heating coil.
In one embodiment, the de-weight tower 4 is provided with a de-weight condenser 8, a de-weight reflux buffer tank 11 and a de-weight reboiler 14, the top of the de-weight tower 4 is connected with the inlet of the de-weight reflux buffer tank 11 through the de-weight condenser 8, the outlet material of the de-weight reflux buffer tank 11 flows back to the top of the de-weight tower 4, and the outlet of the de-weight reflux buffer tank 11 also comprises a phenoxyethanol outlet 18, namely, the outlet for phenoxyethanol is used for discharging; the tower kettle material outlet of the weight removing tower 4 is connected with a weight removing reboiler 14, and the outlet material of the weight removing reboiler 14 flows back to the tower kettle of the weight removing tower 4.
Preferably, the heavy-removal tower 4 is a packed tower or a plate tower, and the number of theoretical plates is 50; the de-weight reflux drum 11 is equipped with an internal heating coil.
As shown in fig. 1, an embodiment of the present invention also provides a process for producing fine chemicals, which is suitable for synthesizing phenol ethanol from phenol and ethylene carbonate, comprising the steps of:
step 1, pretreatment of raw materials
Phenol, ethylene carbonate and catalyst from the boundary zone are heated and dissolved in the raw material mixing tank 1 according to the mass ratio of 1.4:1:0.03; the dissolved materials are conveyed to a reaction preheater 5 for reaction pretreatment;
Step 2, synthesizing phenoxyethanol
The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to total reflux synthesis reaction of phenoxyethanol in a reactive rectifying tower 2, and the main reaction of the synthesis is as follows:
the carbon dioxide gas generated by the reaction is condensed by a reaction condenser 6 and then is discharged fromCO 2 The outlet 16 is conveyed to a subsequent working section for recovery treatment; the reactant mixture discharged from the tower kettle of the reactive rectifying tower 2 is conveyed to a light component removing tower 3 for rectifying treatment; the conversion rate of the reacted ethylene carbonate is 100 percent, and the selectivity of the phenoxyethanol is 95.2 percent;
step 3, purification of phenoxyethanol
The reaction materials from the tower bottom of the reaction rectifying tower 2 are subjected to secondary rectification treatment of the light component removing tower 3 and the heavy component removing tower 4, so that a cosmetic grade phenoxyethanol product can be obtained, the content of the phenoxyethanol is 99.72%, and the content of phenol is 1.2mg/kg.
In one embodiment, in step 1, the material temperature after heating and dissolution of the raw material mixing tank 1 is 60 ℃; the temperature of the material treated by the reaction preheater 5 is 90 ℃; the catalyst is an ionic liquid, and the structural formula of the catalyst is shown as follows:
wherein R1 is propyl; r2 is octyl.
In one embodiment, in step 2, the reactive distillation column 2 overhead pressure is 70kpa; the temperature of the material condensed by the reaction condenser 6 is 40 ℃; the temperature of the tower bottom of the reactive rectifying tower 2 is 160 ℃; the reaction reflux buffer tank 9 is provided with an internal heating coil, and when the temperature of the material is lower than 20 ℃, heating is started until the temperature rises to 50 ℃ and heating is stopped.
In one embodiment, in the step 3, the reflux ratio of the top of the light component removal tower 3 is 2.0, and the phenol obtained from the top of the light component removal tower 3 can be recycled; the pressure at the top of the light component removal tower 3 is 8kpa; the temperature of the material condensed by the light component removing condenser 7 is 60 ℃; the temperature of the tower kettle of the light component removal tower 3 is 120 ℃; the light reflux drum 10 is equipped with an internal heating coil and when the temperature of the material is below 50 c, the heating is turned on until the temperature rises to 60 c and the heating is stopped.
The reflux ratio of the top of the weight removing tower 4 is 2.0, and the top of the weight removing tower 4 is the cosmetic grade phenoxyethanol; the catalyst concentrate obtained from the tower kettle of the weight removing tower 4 is conveyed to a subsequent working section for recovery treatment; the pressure at the top of the heavy-removal tower 4 is 8kpa; the temperature of the material condensed by the de-duplication condenser 8 is 40 ℃; the temperature of the tower bottom of the weight removing tower 4 is 140 ℃; the de-weight reflow buffer tank 11 is provided with an internal heating coil, when the temperature of the material is lower than 20 ℃, the heating is started until the temperature rises to 30 ℃ and the heating is stopped.
The embodiment of the invention provides a device and a process for producing fine chemicals, which have the following main advantages:
1) The process is simple and efficient, the conversion rate of the ethylene carbonate is 100%, and the selectivity of the phenoxyethanol is more than 95%;
2) The ionic liquid catalyst provided has stable property, can be recycled, and is beneficial to industrial application;
3) The device has simple structure, convenient operation and stable and reliable product quality, can effectively reduce the device investment of phenoxyethanol and improve the market competitiveness of the product.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.

Claims (10)

1. The utility model provides a production device of fine chemicals, includes raw materials blending tank, reaction rectifying column, light ends removal tower and heavy ends removal tower, its characterized in that, the entry material of raw materials blending tank is phenol, ethylene carbonate and catalyst mixture, and the material export of raw materials blending tank passes through reaction pre-heater and reaction rectifying column's entry linkage, and reaction rectifying column's tower cauldron material export and light ends removal tower's material entry linkage, light ends removal tower's tower cauldron material export and heavy ends removal tower's material entry linkage, and heavy ends removal tower's tower cauldron material export is catalyst concentrate export.
2. The apparatus for producing fine chemicals according to claim 1, wherein said raw material mixing tank is equipped with a stirrer, and the raw material mixing tank has a heating half pipe or a jacket.
3. The apparatus for producing fine chemicals according to claim 1 or 2, characterized in that the reaction rectifying column is equipped with a reaction condenser, a reaction reflux buffer tank and a reaction reboiler;
the top of the reaction rectifying tower is connected with the inlet of a reaction reflux buffer tank through a reaction condenser, the outlet material of the reaction reflux buffer tank is refluxed to the top of the reaction rectifying tower, and the reaction condenser is also provided with CO 2 An outlet;
and a tower bottom material outlet of the reaction rectifying tower is connected with a reaction reboiler, and outlet materials of the reaction reboiler flow back to the tower bottom of the reaction rectifying tower.
4. The fine chemical production apparatus according to claim 3, wherein the light component removal tower is equipped with a light component removal condenser, a light component removal reflux buffer tank, and a light component removal reboiler;
the top of the light component removing tower is connected with the inlet of a light component removing reflux buffer tank through a light component removing condenser, the outlet material of the light component removing reflux buffer tank is refluxed to the top of the light component removing tower, and the outlet of the light component removing reflux buffer tank also comprises a phenol outlet;
And a tower bottom material outlet of the light component removing tower is connected with a light component removing reboiler, and outlet materials of the light component removing reboiler flow back to the tower bottom of the light component removing tower.
5. The fine chemical production apparatus according to claim 4, wherein the de-weight column is provided with a de-weight condenser, a de-weight reflux drum, and a de-weight reboiler;
the top of the de-weight tower is connected with the inlet of a de-weight reflux buffer tank through a de-weight condenser, the outlet material of the de-weight reflux buffer tank is refluxed to the top of the de-weight tower, and the outlet of the de-weight reflux buffer tank also comprises a phenoxyethanol outlet;
and a tower bottom material outlet of the heavy removal tower is connected with a heavy removal reboiler, and outlet materials of the heavy removal reboiler flow back to the tower bottom of the heavy removal tower.
6. The fine chemical production apparatus according to claim 5, wherein the reactive distillation column is a packed column or a tray column, and the number of trays is 20 to 40;
the reaction condenser is provided with a non-condensable gas material outlet;
the reaction reflux buffer tank is provided with an internal heating coil;
the light component removing tower is a packed tower or a plate tower, and the number of the plates is 30-60;
the light reflux buffer tank is provided with an internal heating coil;
the heavy-removal tower is a packed tower or a plate tower, and the number of the plates is 30-60;
The de-weight reflow buffer tank is provided with an internal heating coil.
7. A process for the production of fine chemicals, comprising the steps of:
step 1, pretreatment of raw materials
Phenol, ethylene carbonate and catalyst from the boundary area are heated and dissolved in a raw material mixing tank according to the mass ratio of 1.1-2.0:1:0.005-0.08; conveying the dissolved materials to a reaction preheater for reaction pretreatment;
step 2, synthesizing phenoxyethanol
The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to total reflux synthesis reaction of phenoxyethanol in a reaction rectifying tower, and the main reaction of the synthesis is as follows:
condensing carbon dioxide gas generated by the reaction through a reaction condenser, and then separating CO 2 The outlet is conveyed to a subsequent working section for recovery treatment; reactant mixture discharged from the tower kettle of the reaction rectifying tower is conveyed to a light component removing tower for rectifying treatment; the conversion rate of the reacted ethylene carbonate is 100 percent, and the selectivity of the phenoxyethanol is 95 to 99.5 percent;
step 3, purification of phenoxyethanol
The reaction materials from the tower bottom of the reaction rectifying tower are subjected to secondary rectifying treatment of a light component removing tower and a heavy component removing tower, so that a cosmetic grade phenoxyethanol product can be obtained, the content of the phenoxyethanol is more than or equal to 99.5%, and the content of phenol is less than 10mg/kg.
8. The process for producing fine chemicals according to claim 7, wherein in step 1, the material temperature after heating and dissolution of said raw material mixing tank is 50 to 80 ℃;
the temperature of the material treated by the reaction preheater is 80-110 ℃;
the catalyst is an ionic liquid, and the structural formula of the catalyst is shown as follows:
wherein R1 is methyl, ethyl or propyl; r2 is butyl, amyl, hexyl, heptyl or octyl.
9. The process for producing fine chemicals according to claim 8, wherein in step 2, the reaction rectifying column top pressure is 15 to 100kpa;
the temperature of the material condensed by the reaction condenser is 30-50 ℃;
the temperature of the tower bottom of the reaction rectifying tower is 130-190 ℃;
the reaction reflux buffer tank is provided with an internal heating coil, and when the temperature of the material is lower than 20 ℃, heating is started until the temperature rises to 50 ℃, and heating is stopped.
10. The process for producing fine chemicals according to claim 9, wherein in step 3, the reflux ratio of the top of the light component removal column is 0.5 to 3.0, phenol obtained from the top of the light component removal column can be recycled, the top pressure of the light component removal column is 1 to 15kpa, and the bottom temperature of the light component removal column is 100 to 140 ℃;
The temperature of the material condensed by the light component removing condenser is 50-70 ℃;
the light-removal reflux buffer tank is provided with an internal heating coil, and when the temperature of the material is lower than 50 ℃, heating is started until the temperature rises to 60 ℃ and heating is stopped;
the reflux ratio of the top of the de-weight tower is 0.5-3.0, the top of the de-weight tower is the cosmetic grade phenoxyethanol, the catalyst concentrate obtained at the bottom of the de-weight tower is conveyed to the subsequent working section for recovery treatment, the pressure of the top of the de-weight tower is 1-15 kpa, and the temperature of the bottom of the de-weight tower is 110-160 ℃;
the temperature of the material condensed by the de-duplication condenser is 30-50 ℃;
the weight-losing reflux buffer tank is provided with an internal heating coil, when the temperature of the material is lower than 20 ℃, the heating is started until the temperature rises to 30 ℃, and the heating is stopped.
CN202311025488.9A 2023-08-15 2023-08-15 Fine chemical production device and process Pending CN117085347A (en)

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Application Number Priority Date Filing Date Title
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