CN110437178A - A kind of method of green high-efficient synthesizing epoxypropane - Google Patents
A kind of method of green high-efficient synthesizing epoxypropane Download PDFInfo
- Publication number
- CN110437178A CN110437178A CN201910835117.4A CN201910835117A CN110437178A CN 110437178 A CN110437178 A CN 110437178A CN 201910835117 A CN201910835117 A CN 201910835117A CN 110437178 A CN110437178 A CN 110437178A
- Authority
- CN
- China
- Prior art keywords
- reaction
- propylene
- solvent
- hydrogen peroxide
- green high
- 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.)
- Withdrawn
Links
Classifications
-
- 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/89—Silicates, aluminosilicates or borosilicates of titanium, zirconium or hafnium
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/02—Synthesis of the oxirane ring
- C07D301/03—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds
- C07D301/12—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds with hydrogen peroxide or inorganic peroxides or peracids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
- C07D303/02—Compounds containing oxirane rings
- C07D303/04—Compounds containing oxirane rings containing only hydrogen and carbon atoms in addition to the ring oxygen atoms
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Epoxy Compounds (AREA)
Abstract
The present invention provides a kind of methods of green high-efficient synthesizing epoxypropane.The technical solution is based on propylene ring oxidation reaction and prepares propylene oxide, using hydrogen peroxide direct oxidation method, using propylene as raw material, epoxidation reaction occurs in catalytic rectifying tower under the action of TS-1 microspherical catalyst, reactant obtains the propylene oxide of high concentration after separating-purifying.The present invention reacts no coupling product and generates, and single layer conversion ratio >=97%, selectivity >=99%, is a kind of method of green syt propylene oxide, is suitble to large-scale industrial production.This method atom utilization is high, selectivity is high, product yield is high and reaction no coupling product, environmentally friendly.
Description
Technical field
The present invention relates to field of chemical technology, and in particular to a kind of method of green high-efficient synthesizing epoxypropane.
Background technique
Propylene oxide is one of important derivatives of propylene, is a kind of important Organic Chemicals, in the derivative of propylene
It is only second to polypropylene and acrylonitrile in object, occupies third position.Due to containing-C-O-C- ternary ether structure in epoxide, have
Biggish surface tension, thus have very high reactivity, to acid and nucleopilic reagent it is very sensitive, can with hydrogen halides, water, alcohol,
The plurality of reagents such as amine are reacted and open loop, and a variety of halohydrins, propylene glycol, ether alcohol, secondary amine alcohol or quaternary amine alcohol etc. are produced.Propylene oxide is most
Big purposes is as main material production polyether polyol, reproduction polyurethane;Next can be used for producing widely used third
Glycol, propylene glycol etc.;Can also be used in other field include production nonionic surface active agent, oil field demulsifier, fire retardant,
Syntholube, farm chemical emulgent, unsaturated acid ester, adhesive etc..
Currently, preparing there are mainly three types of the methods of propylene oxide: chlorohydrination, conjugated oxidation and direct oxidation method.
Chlorohydrination is with propylene, chlorine, quick lime and water.Chlorohydrin action is occurred by chlorine gas and water and propylene first, it is raw
Produce intermediate chloropropyl alcohol, then with limewash and its occur saponification be made propylene oxide, by reaction product be sent into primary distillation tower with
Rectifying column carries out product separation, obtains product.Chlorohydrination industrialization is more than 80 years existing, and technique is more mature, and advantage is technique stream
Journey is short, small investment, operating flexibility is big, selectivity is good, production is safer.But there is also more disadvantages: the process requirement is a large amount of
Chlorine, severe corrosion to equipment;The waste water, waste residue and exhaust emission environment of a large amount of chloride containing calcium is discharged.
Conjugated oxidation is to react synthesizing epoxypropane by organic peroxide and propylene.Not according to raw material and joint product
Together, the conjugated oxidation of use mainly includes iso-butane cooxidation technique, ethylbenzene cooxidation technique, cumyl hydroperoxide method.Altogether
Oxidizing process overcomes the disadvantages of chlorohydrination corrosion is big, sewage is more, and product cost is low, and environmental pollution is also relatively small.But it should
Process flow is long, raw material variety is more, requires purified propylene high;Technological operation need to carry out at a higher pressure, want to equipment
Ask high, construction investment is also corresponding higher.
Direct oxidation method technique uses oxidant direct oxidation propylene synthesizing epoxypropane, is divided into according to the difference of oxidant
Hydrogen peroxide direct oxidation method and oxygen direct oxidation method.For chlorohydrination and conjugated oxidation, direct oxidation method process
It is relatively easy, by-product is less and pollution-free.Although having above-mentioned advantage on technology path, popular response mode can be generated
Certain by-product, and there is selectivity it is lower, product yield is not high the defects of.In this case, how based on direct
The technical issues of technology path of oxidizing process develops a kind of new propylene oxide synthesis technology, becomes urgently and solves.
Summary of the invention
The present invention is directed to be directed to the technological deficiency of the prior art, a kind of method of green high-efficient synthesizing epoxypropane is provided,
To solve in the prior art, the propylene oxide based on direct oxidation method is conventionally synthesized technique, and selective lower, product yield is not
High technical problem.
Another technical problem to be solved by the present invention is that the propylene oxide based on direct oxidation method is conventionally synthesized technique, can give birth to
At certain by-product.
The invention solves another technical problem be how to fully ensure that propylene oxide synthesis technology to environment green, nothing
Pollution.
To realize the above technical purpose, the invention adopts the following technical scheme:
A kind of method of green high-efficient synthesizing epoxypropane, this method are in the catalytic distillation that TS-1 microspherical catalyst is housed
In tower, with 100~160 DEG C of temperature, the pressure of 0.3~0.6MPa, propylene, solvent, hydrogen peroxide are subjected to hybrid reaction.
Preferably, the above method is the following steps are included: the rectifying section of catalytic rectifying tower is paved with the TS-1 microballoon catalysis
Agent, propylene, hydrogen peroxide, solvent become mixing gas phase after feed system pretreatment and enter catalytic rectifying tower;The gaseous mixture
Mutually enter rectifying section and carry out epoxidation reaction, obtains heavy constituent reaction solution;The heavy constituent reaction solution enters stripping section, separates
To propylene oxide.
Preferably, the TS-1 microspherical catalyst is using butyl titanate as titanium source, tetraethyl orthosilicate is silicon source, 4 third
Base ammonium hydroxide is what template was prepared.
Preferably, the TS-1 microspherical catalyst is prepared by the following method:
1) with SiO in tetraethyl orthosilicate2Molal quantity: the molal quantity of tetrapropylammonium hydroxide: TiO in butyl titanate2's
Molal quantity: the molal quantity of water is 1:0.3~1:0.02~0.05:30~50 ratio, by the aqueous solution of tetrapropylammonium hydroxide
It is uniformly mixed with the aqueous solution of tetraethyl orthosilicate, is then under agitation added thereto butyl titanate, mix, it is quiet
Set 8~12h;
2) by step 1) products therefrom with 80~90 DEG C of crystallization for 24 hours, then with 110~130 DEG C of 2~10h of crystallization, then with
160~180 DEG C of crystallization for 24 hours, product are filtered, washed, is dried, is roasted to get TS-1 fine catalyst is arrived;
3) step 2) products therefrom is uniformly mixed with the silicon dioxde solution that mass fraction is 30%, is sprayed onto high speed rotation
On turntable, it is centrifuged material of dishing out, is fallen in 400 DEG C of nitrogen atmospheres, collects the dry matter fallen to get micro- to the TS-1
Sphere catalyst.
Preferably, the dosage of the TS-1 microspherical catalyst is the 0.1~15% of material gross mass.
Preferably, the molal quantity of propylene: the molal quantity of hydrogen peroxide: the molal quantity of solvent is 1:2~3:5~7.5.
Preferably, reaction velocity is 1500-4000h-1。
Preferably, isobutylene feed speed is 0.01~30mL/min, acetic acid charging rate is 0.01~6mL/min,
Oxygen feeding speed is 10~1000mL/min, and nitrogen feed speed is 20~8000mL/min.
Preferably, the solvent be methanol, ethyl alcohol, propyl alcohol, isopropanol, the tert-butyl alcohol, acetonitrile, acetone, butanone wherein
A kind of or in which any two kinds of mixture.
The present invention provides a kind of methods of green high-efficient synthesizing epoxypropane.It is anti-that the technical solution is based on epoxidation of propylene
Propylene oxide should be prepared, using hydrogen peroxide direct oxidation method, using propylene as raw material, under the action of TS-1 microspherical catalyst in
Epoxidation reaction occurs in catalytic rectifying tower, reactant obtains the propylene oxide of high concentration after separating-purifying.Present invention reaction
No coupling product generates, single layer conversion ratio >=97%, and selectivity >=99%, is a kind of method of green syt propylene oxide, is suitble to
Large-scale industrial production.This method atom utilization is high, selectivity is high, product yield is high and reaction no coupling product, to environment
It is friendly.
Specific embodiment
Below by specific embodiments of the present invention will be described in detail.In order to avoid excessive unnecessary details, In
It will not be described in detail in following embodiment to belonging to well known structure or function.Approximation used in following embodiment
Language can be used for quantitative expression, show to allow quantity to have certain variation in the case where not changing basic function.It is fixed except having
Adopted outer, technical and scientific term used in following embodiment has the phase being commonly understood by with those skilled in the art of the invention
Same meaning.
Embodiment 1
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2:5.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, reaction
Device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, weight after reaction
Component enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 2
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2:6.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, reaction
Device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, weight after reaction
Component enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 3
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2:5.5.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, instead
Answer device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, after reaction
Heavy constituent enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 4
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2:7.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, reaction
Device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, weight after reaction
Component enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 5
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2:6.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, reaction
Device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, weight after reaction
Component enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 6
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2.4:5.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, instead
Answer device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, after reaction
Heavy constituent enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 7
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2.1:5.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, instead
Answer device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, after reaction
Heavy constituent enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 8
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2:5.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, reaction
Device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, weight after reaction
Component enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 9
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2.7:5.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, instead
Answer device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, after reaction
Heavy constituent enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 10
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2.6:5.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, instead
Answer device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, after reaction
Heavy constituent enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 11
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2.5:5.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, instead
Answer device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, after reaction
Heavy constituent enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 12
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2.4:5.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, instead
Answer device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, after reaction
Heavy constituent enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 13
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2.3:5.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, instead
Answer device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, after reaction
Heavy constituent enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 14
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:3:5.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, reaction
Device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, weight after reaction
Component enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 15
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2:7.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, reaction
Device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, weight after reaction
Component enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=97.2%, selectivity >=99%.
Embodiment 16
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:3:5.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, reaction
Device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, weight after reaction
Component enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=97.8%, selectivity >=99%.
Embodiment 17
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2.2:5.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, instead
Answer device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, after reaction
Heavy constituent enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=98%, selectivity >=99%.
Embodiment 18
TS-1 microspherical catalyst 300ml, feedstock ratio are as follows: material proportion (molar ratio) third are loaded in catalytic rectifying tower
Alkene: hydrogen peroxide: solvent=1:2:7.Air speed is 1500h-1.It is 150 DEG C that reaction bed temperature is controlled in reaction process, reaction
Device inlet pressure 0.6MPa.Propylene, hydrogen peroxide, solvent are to enter catalytic rectifying tower after mixing in preheated device, weight after reaction
Component enters stripping section, and propylene oxide is obtained after separating-purifying.Single transformation rate >=97%, selectivity >=99%.
The embodiments of the present invention have been described in detail above, but content is only the preferred embodiment of the present invention,
It is not intended to limit the invention.All any modifications, equivalent replacements, and improvements etc. done in application range of the invention, should all
It is included within protection scope of the present invention.
Claims (9)
1. a kind of method of green high-efficient synthesizing epoxypropane, it is characterised in that: this method is equipped with TS-1 microspherical catalyst
Catalytic distillation tower in, with 100~160 DEG C of temperature, the pressure of 0.3~0.6MPa, propylene, solvent, hydrogen peroxide are carried out
Hybrid reaction.
2. a kind of method of green high-efficient synthesizing epoxypropane according to claim 1, which is characterized in that including following step
Rapid: the rectifying section of catalytic rectifying tower is paved with the TS-1 microspherical catalyst, and propylene, hydrogen peroxide, solvent are located in advance in feed system
Become mixing gas phase after reason and enters catalytic rectifying tower;The mixing gas phase enters rectifying section and carries out epoxidation reaction, is recombinated
Divide reaction solution;The heavy constituent reaction solution enters stripping section, isolated propylene oxide.
3. a kind of method of green high-efficient synthesizing epoxypropane according to claim 1, it is characterised in that the TS-1 is micro-
Sphere catalyst is using butyl titanate as titanium source, and tetraethyl orthosilicate is silicon source, and tetrapropylammonium hydroxide is prepared for template
's.
4. a kind of method of green high-efficient synthesizing epoxypropane according to claim 1, it is characterised in that the TS-1 is micro-
Sphere catalyst is prepared by the following method:
1) with SiO in tetraethyl orthosilicate2Molal quantity: the molal quantity of tetrapropylammonium hydroxide: TiO in butyl titanate2Mole
Number: the molal quantity of water is 1:0.3~1:0.02~0.05:30~50 ratio, by the aqueous solution and silicon of tetrapropylammonium hydroxide
The aqueous solution of sour tetra-ethyl ester is uniformly mixed, and is then under agitation added thereto butyl titanate, is mixed, and stands 8
~12h;
2) by step 1) products therefrom with 80~90 DEG C of crystallization for 24 hours, then with 110~130 DEG C of 2~10h of crystallization, then with 160
~180 DEG C of crystallization for 24 hours, product are filtered, washed, is dried, is roasted to get TS-1 fine catalyst is arrived;
3) step 2) products therefrom is uniformly mixed with the silicon dioxde solution that mass fraction is 30%, is sprayed onto high speed rotation turntable
On, it is centrifuged material of dishing out, is fallen in 400 DEG C of nitrogen atmospheres, is collected the dry matter fallen and urged to get to the TS-1 microballoon
Agent.
5. a kind of method of green high-efficient synthesizing epoxypropane according to claim 1, it is characterised in that the TS-1 is micro-
The dosage of sphere catalyst is the 0.1~15% of material gross mass.
6. a kind of method of green high-efficient synthesizing epoxypropane according to claim 1, it is characterised in that mole of propylene
Number: the molal quantity of hydrogen peroxide: the molal quantity of solvent is 1:2~3:5~7.5.
7. a kind of method of green high-efficient synthesizing epoxypropane according to claim 1, it is characterised in that reaction velocity is
1500-4000h-1。
8. a kind of method of green high-efficient synthesizing epoxypropane according to claim 7, it is characterised in that isobutylene feed
Speed is 0.01~30mL/min, and acetic acid charging rate is 0.01~6mL/min, and oxygen feeding speed is 10~1000mL/min,
Nitrogen feed speed is 20~8000mL/min.
9. a kind of method of green high-efficient synthesizing epoxypropane according to claim 1, it is characterised in that the solvent is
Methanol, ethyl alcohol, propyl alcohol, isopropanol, the tert-butyl alcohol, acetonitrile, acetone, the one of which of butanone or in which any two kinds of mixture.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910835117.4A CN110437178A (en) | 2019-09-05 | 2019-09-05 | A kind of method of green high-efficient synthesizing epoxypropane |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910835117.4A CN110437178A (en) | 2019-09-05 | 2019-09-05 | A kind of method of green high-efficient synthesizing epoxypropane |
Publications (1)
Publication Number | Publication Date |
---|---|
CN110437178A true CN110437178A (en) | 2019-11-12 |
Family
ID=68439136
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910835117.4A Withdrawn CN110437178A (en) | 2019-09-05 | 2019-09-05 | A kind of method of green high-efficient synthesizing epoxypropane |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN110437178A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116199647A (en) * | 2021-12-01 | 2023-06-02 | 中国石油化工股份有限公司 | Method for producing epoxypropane |
-
2019
- 2019-09-05 CN CN201910835117.4A patent/CN110437178A/en not_active Withdrawn
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN116199647A (en) * | 2021-12-01 | 2023-06-02 | 中国石油化工股份有限公司 | Method for producing epoxypropane |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN1261422C (en) | Integrated process for preparation of olefin oxides | |
CN101279958B (en) | Method for preparing epoxy chloropropane by epoxidation of propylene chloride | |
CN1280280C (en) | Process for continuous production of olefinic oxide | |
CN102858758A (en) | Process for the manufacture of propylene oxide | |
CN105367520B (en) | The method for preparing expoxy propane | |
CN110252394B (en) | Catalyst for preparing propylene oxide by propylene oxidation, preparation and application thereof | |
CN102822226B (en) | The method of preparation divinylarene | |
CN110773147B (en) | Catalyst for preparing epoxypropane by propylene epoxidation and preparation method thereof | |
CN103212437A (en) | Method for preparing titanium-based catalyst and synthesizing epoxypropane and dicumyl peroxide | |
CN110437178A (en) | A kind of method of green high-efficient synthesizing epoxypropane | |
CN110357835A (en) | A kind of preparation method of epichlorohydrin | |
CN101525320B (en) | Preparation method of 3,4-epoxycyclohexylcarboxylate-3',4'-epoxycyclohexyl methyl ester | |
CN102442977A (en) | Olefin epoxidation method | |
CN113087717B (en) | A method for preparing dicyclopentadiene dioxide and alkylene oxide by using titanium silicon molecular sieve catalyst | |
CN108047168A (en) | A kind of synthetic method of epoxyoleic acid ethylene oxidic ester | |
CN102442976B (en) | Olefin Epoxidation Method | |
KR101872391B1 (en) | Method for producing oxidized olefin through olefin epoxidation | |
CN114426550B (en) | Preparation method of dicyclopentadiene dioxide DCPDDO | |
CN102464632B (en) | Method for preparing epoxy chloropropane | |
CN108947939A (en) | A kind of synthetic method of terpinolene 4,8- epoxides | |
CN103920531A (en) | Titanium-silicon molecular sieve catalyst, its preparation method and application thereof | |
CN111100140A (en) | Method for catalytic oxidation of dicyclopentadiene by solid acid | |
CN102442978B (en) | A kind of olefin epoxidation method | |
KR101819023B1 (en) | Refining mehtod for crude propylene oxide product and preparation method for propylene oxide | |
CN105272948B (en) | The method for preparing epoxychloropropane |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
WW01 | Invention patent application withdrawn after publication |
Application publication date: 20191112 |
|
WW01 | Invention patent application withdrawn after publication |