CN110054340A - The waste water adsorption method of cumyl peroxide - Google Patents
The waste water adsorption method of cumyl peroxide Download PDFInfo
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- CN110054340A CN110054340A CN201910445703.8A CN201910445703A CN110054340A CN 110054340 A CN110054340 A CN 110054340A CN 201910445703 A CN201910445703 A CN 201910445703A CN 110054340 A CN110054340 A CN 110054340A
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- cumyl peroxide
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- waste water
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C15/00—Cyclic hydrocarbons containing only six-membered aromatic rings as cyclic parts
- C07C15/02—Monocyclic hydrocarbons
- C07C15/085—Isopropylbenzene
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/10—Purification; Separation; Use of additives by extraction, i.e. purification or separation of liquid hydrocarbons with the aid of liquids
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/02—Temperature
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/03—Pressure
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/16—Regeneration of sorbents, filters
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Water Supply & Treatment (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention provides a kind of waste water adsorption methods of cumyl peroxide, removal for isopropylbenzene in waste water in cumyl peroxide crystallization process, the following steps are included: S1, the crystallization waste water of cumyl peroxide to be transferred in extraction equipment to progress grease extraction and separation, liquid waste material and oily waste material are separated；S2, it liquid waste material is transferred in high pressure distillation tank carries out rectifying, to separate the ethyl alcohol and other liquid wastes in liquid waste material；S3, oily waste material is transferred in adsorption tanks, and adsorbing medium is added into adsorption tanks, adsorb oily waste material；S4, heating heating is carried out to the adsorbing medium for being adsorbed with oily waste material, to separate isopropylbenzene and other oily waste materials.The waste water adsorption method of cumyl peroxide of the invention can effectively recycle isopropylbenzene, reduce the waste of cumyl peroxide synthesis material by adsorbing to the isopropylbenzene in cumyl peroxide cleaning solution/centrifugate.
Description
Technical field
The present invention relates to chemical production field more particularly to a kind of waste water adsorption methods of cumyl peroxide.
Background technique
Cumyl peroxide (dicumyl peroxide), also known as vulcanizing agent DCP, two cumin of peroxidating.Molecular formula
C18H22O2, relative molecular mass 270.37 is a kind of white crystals, and fusing point is 41~42 DEG C.It is not soluble in water, it is dissolved in ethyl alcohol, second
Ether, acetic acid, benzene and petroleum ether.It is stable at room temperature, it is light-exposed gradually become it is yellowish.Cumyl peroxide is a kind of Strong oxdiative
Agent, active o content 5.92% (purity 100%), 5.62% (purity 95%), 120~125 DEG C of decomposition temperature.
Cumyl peroxide (DCP) is an excellent organic peroxide, can be used as the initiator of monomer polymerization, high score
Vulcanizing agent, crosslinking agent, curing agent, the flame-retardant additive of sub- material；Be widely used in rubber, polyolefin, foamed plastics, cable,
In the industry such as shoemaking, insulated paint, it is proposed that additive amount is about 3%.
Cumyl peroxide generates peroxidating isopropyl by cumene oxidation mainly with isopropylbenzene starting material at present
Benzene, concentration and recovery isopropylbenzene, dicumyl peroxide reduction generate propyloxy phenyl alcohol (also referred to as pheiiyldimetliyl methanol), and peroxidating is different
Propyl benzene synthesizes cumyl peroxide with propyloxy phenyl alcohol, and crystallization purifying obtains the processes such as pure cumyl peroxide.And isopropyl
Benzene will inevitably remain in cumyl peroxide, the washing of cumyl peroxide as synthesis cumyl peroxide
The isopropylbenzene in cumyl peroxide can be effectively removed, however, if the cumyl peroxide washing containing isopropylbenzene is non-
Direct emission is chased after, the waste of synthesis material on the one hand will be caused, increases production cost；On the other hand bad shadow will be caused to environment
It rings, wastewater treatment process repeatedly, increases energy consumption and is unfavorable for subsequent production and use.
In view of this, it is necessory to provide a kind of waste water adsorption method of cumyl peroxide, to solve the above problems.
Summary of the invention
The purpose of the present invention is to provide a kind of waste water adsorption method of cumyl peroxide, the cumyl peroxides
Waste water adsorption method by being adsorbed to the isopropylbenzene in cumyl peroxide cleaning solution/centrifugate, can effectively recycle
Isopropylbenzene reduces the waste of cumyl peroxide synthesis material.
For achieving the above object, it the present invention provides a kind of waste water adsorption method of cumyl peroxide, is used for
In cumyl peroxide crystallization process in waste water isopropylbenzene removal, comprising the following steps:
S1, the crystallization waste water of cumyl peroxide is transferred to progress grease extraction and separation, separating liquid in extraction equipment
Shape waste material and oily waste material；
S2, the liquid waste material be transferred in high pressure distillation tank carry out rectifying, with separate the ethyl alcohol in liquid waste material and
Other liquid wastes；
S3, the oily waste material is transferred in adsorption tanks, and adsorbing medium is added into adsorption tanks, adsorb the oily
Waste material；
S4, heating heating is carried out to the adsorbing medium for being adsorbed with oily waste material, to separate isopropylbenzene and other oily waste materials.
As a further improvement of the present invention, the extractant in the step S1 is two o-phthalic acid dibutyl esters.
As a further improvement of the present invention, the step S2 specifically:
S21, the liquid waste is passed through from the bottom to top in the high pressure distillation tank, so that liquid waste flows through high pressure steaming
Enter in high pressure distillation chamber body after evaporating the adsorbing medium in tank；
After S22, pressurization, 10~15min of heating, the drain tap above high pressure distillation tank is opened, in high pressure distillation tank
Pressure recovery to normal pressure after, close drain tap continue distillation under pressure, when the air pressure in high pressure distillation tank not variation when, steam
Evaporate end；
The gas that S23, distillation generate is transferred into condensing unit and is condensed, to separate acquisition ethanol solution.
As a further improvement of the present invention, in the step S22, the vapo(u)rizing temperature of liquid waste is 101~107 DEG C,
Pressure is 1.5~2.2MPa.
As a further improvement of the present invention, the step S3 specifically:
S31, the oily waste material in step S1 is from top to bottom transferred in adsorption tanks, and carries out low-temperature heat；
S32, adsorbing medium is transferred in adsorption tanks, is stirred so that adsorbing medium comes into full contact with oily waste material；
S33, standing 20~30min oily waste material absorption terminate.
As a further improvement of the present invention, the low-temperature heat of oily waste material is 30~37 DEG C in the step S31.
As a further improvement of the present invention, the adsorbing medium is beta-zeolite molecular sieve.
As a further improvement of the present invention, the adsorbing medium is the H beta-zeolite molecular sieve through ammonification.
As a further improvement of the present invention, the step S4 is specially that the adsorbing medium for being adsorbed with oily waste material heats up
200 ± 15 DEG C are heated to, to separate isopropylbenzene and other oily waste materials.
The beneficial effects of the present invention are: the waste water adsorption method of cumyl peroxide of the invention by extraction, rectifying,
The means of absorption and desorption effectively remove the isopropylbenzene that cumyl peroxide is blended in waste water in washing separation process,
And isopropylbenzene after the recovery can continue to use after desorption, effectively reduce the production cost of cumyl peroxide, be suitable for
It promotes and uses.
Detailed description of the invention
Fig. 1 is the flow diagram of the wash crystallization method of cumyl peroxide of the present invention.
Fig. 2 is the flow diagram of step S2 in Fig. 1.
Fig. 3 is the flow diagram of step S3 in Fig. 1.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, right in the following with reference to the drawings and specific embodiments
The present invention is described in detail.
Herein, it should be noted that in order to avoid having obscured the present invention because of unnecessary details, only show in the accompanying drawings
Gone out the structure and/or processing step closely related with the solution of the present invention, and be omitted with relationship of the present invention less other
Details.
In addition, it should also be noted that, the terms "include", "comprise" or its any other variant be intended to it is non-exclusive
Property include so that include a series of elements process, method, article or equipment not only include those elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Element.
Refering to Figure 1, being a kind of waste water adsorption method of cumyl peroxide provided by the invention.The peroxidating
The waste water adsorption method of diisopropylbenzene (DIPB) can be used for the removal of isopropylbenzene in waste water in cumyl peroxide crystallization process, specific next
Say, the waste water adsorption method of cumyl peroxide the following steps are included:
S1, the crystallization waste water of cumyl peroxide is transferred to progress water-oil separating extraction in extraction equipment, with separation
Liquid waste material and oily waste material；
S2, it liquid waste material is transferred in high pressure distillation tank carries out rectifying, to separate ethyl alcohol in liquid waste material and other
Liquid waste；
S3, the oily waste material is transferred in adsorption tanks, and adsorbing medium is added into adsorption tanks, adsorb the oily
Waste material；
S4, heating heating is carried out to the adsorbing medium for being adsorbed with oily waste material, to separate isopropylbenzene and other oily waste materials.
Step S1~the S4 will be described in detail in following description part.
Step S1 is mainly for separating of the oily waste material and liquid waste in the crystallization waste water of cumyl peroxide, preferably
Extractant in step sl be two o-phthalic acid dibutyl esters, specifically, two o-phthalic acid dibutyl esters can effectively reduce
Isopropylbenzene and the miscible dissolution degree of liquid waste, therefore use two o-phthalic acid dibutyl esters that can efficiently separate knot as extractant
Brilliant waste water oily waste material and liquid waste.
It please refers to shown in Fig. 2, step S2 specifically:
S21, liquid waste is passed through from the bottom to top in high pressure distillation tank, so that liquid waste flows through in high pressure distillation tank
Enter in high pressure distillation chamber body after adsorbing medium；
After S22, pressurization, 10~15min of heating, the drain tap above high pressure distillation tank is opened, in high pressure distillation tank
Pressure recovery to normal pressure after, close drain tap continue distillation under pressure, when the air pressure in high pressure distillation tank not variation when, steam
Evaporate end；
The gas that S23, distillation generate is transferred into condensing unit and is condensed, to separate acquisition ethanol solution.
In the step s 21, the bottom of high pressure distillation tank is arranged in adsorbing medium, so, when liquid waste from the bottom to top into
When entering in high pressure distillation tank, liquid waste can come into full contact with adsorbing medium, further to remove remaining oil in extraction process
Shape waste material, it is preferred that adsorbing medium used by the step s 21 is beta-zeolite molecular sieve.
Further, in step S22, controlling the vapo(u)rizing temperature in high pressure distillation chamber body is 101~107 DEG C, pressure
For 1.5~2.2MPa, with distilling to liquid waste, specifically, the suction due to beta-zeolite molecular sieve for oily waste material
Attached degree is higher than liquid waste, therefore, liquid waste can be distilled recycling during high temperature distillation, and oily waste material will continue to inhale
It is attached in beta-zeolite molecular sieve, prevents oily waste material from mixing again with liquid waste, can further promote the separation journey of crystallization waste water
Degree.
It please refers to shown in Fig. 3, step S3 specifically:
S31, the oily waste material in step S1 is from top to bottom transferred in adsorption tanks, and carries out low-temperature heat；
S32, adsorbing medium is transferred in adsorption tanks, is stirred so that adsorbing medium comes into full contact with oily waste material；
S33, standing 20~30min oily waste material absorption terminate.
Specifically, the low-temperature heat of oily waste material is 30~37 DEG C in the step s 21, so set, when in step S2
Adsorbing medium when being added, may make oily waste material and adsorbing medium completely and uniform absorption.Further, in step s3
Adsorbing medium used is and identical beta-zeolite molecular sieve in step S22 adsorbs certainly in other embodiments of the invention
Medium is the H beta-zeolite molecular sieve through ammonification, so set, the adsorption capacity between isopropylbenzene and adsorbing medium can be effectively promoted,
It prevents in subsequent desorption process isopropylbenzene with other oily waste materials while being desorbed, effectively improve the rate of recovery of isopropylbenzene.
The oily waste material being adsorbed on adsorbing medium is desorbed specifically by high temperature in step S4, further,
It is specially that the adsorbing medium heating for being adsorbed with oily waste material is heated to 200 ± 15 DEG C in step S4,20~35min of continuous heating
Afterwards, other oily waste materials in addition to isopropylbenzene are desorbed；And isopropylbenzene will continue to be adsorbed in adsorbing medium, crystallize in waste water
Isopropylbenzene is recovered.
Step S4 further includes the adsorbing medium for being adsorbed with isopropylbenzene being desorbed again, and the desorption temperature of isopropylbenzene is
340±15℃。
In conclusion the waste water adsorption method of cumyl peroxide of the invention passes through extraction, rectifying, absorption and desorption
Means, effectively remove cumyl peroxide and be blended in isopropylbenzene in waste water in washing separation process, and is after the recovery
Isopropylbenzene can continue to use after desorption, effectively reduce the production cost of cumyl peroxide, be suitable for promoting and using.
The above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to preferred embodiment to this hair
It is bright to be described in detail, those skilled in the art should understand that, it can modify to technical solution of the present invention
Or equivalent replacement, without departing from the spirit and scope of the technical solution of the present invention.
Claims (9)
1. the waste water adsorption method of a kind of cumyl peroxide, for isopropyl in waste water in cumyl peroxide crystallization process
The removal of benzene, it is characterised in that the following steps are included:
S1, the crystallization waste water of cumyl peroxide is transferred to progress grease extraction and separation in extraction equipment, separation liquid is useless
Material and oily waste material；
S2, it the liquid waste material is transferred in high pressure distillation tank carries out rectifying, to separate ethyl alcohol in liquid waste material and other
Liquid waste；
S3, the oily waste material is transferred in adsorption tanks, and adsorbing medium is added into adsorption tanks, it is useless to adsorb the oily
Material；
S4, heating heating is carried out to the adsorbing medium for being adsorbed with oily waste material, to separate isopropylbenzene and other oily waste materials.
2. the waste water adsorption method of cumyl peroxide according to claim 1, it is characterised in that: in the step S1
Extractant be two o-phthalic acid dibutyl esters.
3. the waste water adsorption method of cumyl peroxide according to claim 2, it is characterised in that the step S2 tool
Body are as follows:
S21, the liquid waste is passed through from the bottom to top in the high pressure distillation tank, so that liquid waste flows through high pressure distillation tank
In adsorbing medium after enter high pressure distillation chamber body in；
After S22, pressurization, 10~15min of heating, the drain tap above high pressure distillation tank is opened, to the pressure in high pressure distillation tank
Power is restored to normal pressure, closes drain tap and continues distillation under pressure, when the air pressure in high pressure distillation tank not in variation, distillation knot
Beam；
The gas that S23, distillation generate is transferred into condensing unit and is condensed, to separate acquisition ethanol solution.
4. the waste water adsorption method of cumyl peroxide according to claim 3, it is characterised in that: the step S22
In, the vapo(u)rizing temperature of liquid waste is 101~107 DEG C, and pressure is 1.5~2.2MPa.
5. the waste water adsorption method of cumyl peroxide according to claim 1, it is characterised in that the step S3 tool
Body are as follows:
S31, the oily waste material is from top to bottom transferred in adsorption tanks, and carries out low-temperature heat；
S32, adsorbing medium is transferred in adsorption tanks, is stirred so that adsorbing medium comes into full contact with oily waste material；
S33, standing 20~30min oily waste material absorption terminate.
6. the waste water adsorption method of cumyl peroxide according to claim 5, it is characterised in that: the step S31
The low-temperature heat of middle oily waste material is 30~37 DEG C.
7. the separator of cumyl peroxide according to claim 1, it is characterised in that: the adsorbing medium is β
Zeolite molecular sieve.
8. the separator of cumyl peroxide according to claim 1, it is characterised in that: the adsorbing medium is warp
The H beta-zeolite molecular sieve of ammonification.
9. the separator of cumyl peroxide according to claim 1, it is characterised in that the step S4 is specially
The adsorbing medium for being adsorbed with oily waste material heating is heated to 200 ± 15 DEG C, to separate isopropylbenzene and other oily waste materials.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115974320A (en) * | 2022-12-30 | 2023-04-18 | 乌鲁木齐市华泰隆化学助剂有限公司 | A kind of treatment method of organic peroxide initiator production waste water separation organic phase |
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| CN115974320A (en) * | 2022-12-30 | 2023-04-18 | 乌鲁木齐市华泰隆化学助剂有限公司 | A kind of treatment method of organic peroxide initiator production waste water separation organic phase |
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