CN110642808A - Production method of segmented epichlorohydrin - Google Patents
Production method of segmented epichlorohydrin Download PDFInfo
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- CN110642808A CN110642808A CN201910978157.4A CN201910978157A CN110642808A CN 110642808 A CN110642808 A CN 110642808A CN 201910978157 A CN201910978157 A CN 201910978157A CN 110642808 A CN110642808 A CN 110642808A
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- C—CHEMISTRY; METALLURGY
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- 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
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- C07D303/00—Compounds containing three-membered rings having one oxygen atom as the only ring hetero atom
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- C07D303/08—Compounds containing oxirane rings with hydrocarbon radicals, substituted by halogen atoms, nitro radicals or nitroso radicals
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Abstract
The invention provides a production method of segmented epichlorohydrin, which comprises the steps of adding chloropropene, aqueous hydrogen peroxide, a titanium-silicon catalyst and a pH regulator into a solvent-free reaction system to carry out epoxidation reaction of chloropropene; carrying out oil-water separation on reaction liquid of the solvent-free reaction system, and refining an oil phase product to obtain epoxy chloropropane; the water phase containing the catalyst enters a solvent reaction system, and the epoxidation reaction is continuously carried out under the participation of the solvent; and separating the reaction liquid of the solvent reaction system, and refining the reaction clear liquid to obtain the epichlorohydrin. The method has the advantages of simple process, mild conditions, low solvent consumption, high yield of target products, realization of online application of the catalyst, green, safe and environment-friendly process, great reduction of production cost and energy consumption, wide industrial application prospect and good social and economic benefits, improves the production efficiency, effectively improves the conversion rate of the hydrogen peroxide, and has the advantages of low solvent consumption, and great reduction of the yield of the target products.
Description
Technical Field
The invention relates to a method for producing organic matters, in particular to a method for producing sectional epoxy chloropropane.
Background
Epichlorohydrin (ECH) is an important organic chemical raw material and a fine chemical product, and has wide application. The epoxy chloropropane is mainly used for preparing epoxy group and phenoxy resin, and the epoxy resin prepared by using the epoxy chloropropane as a main raw material has the characteristics of strong cohesiveness, chemical medium corrosion resistance, low shrinkage, good chemical stability, high impact strength, excellent dielectric property and the like, and has wide application in the industries of coatings, adhesives, reinforcing materials, casting materials, electronic laminated products and the like. Meanwhile, epichlorohydrin is also a stabilizer and a chemical intermediate of oxygen-containing substances, is used for synthesizing glycerol, nitroglycerin explosive, glass fiber reinforced plastic, electrical insulators, surfactants, medicines, pesticides, coatings, sizing materials, ion exchange resins, plasticizers, (condensed) glycerin derivatives, chlorohydrin rubber and other products, curing propylene-based rubber, is used as a solvent for cellulose ester, resin and cellulose ether, and is used for producing chemical stabilizers, chemical dyes, water treatment agents and the like.
At present, the method for producing epichlorohydrin mainly comprises a propylene high-temperature chlorination method, an acetate propylene-propylene alcohol method, an acrolein method, a glycerol chlorination method and a chloropropene direct epoxidation method. In the process of producing epichlorohydrin by performing chloropropene epoxidation reaction by adopting the traditional processes such as a glycerol chlorination method and the like, a large amount of saponification wastewater is generated, so that the environment is polluted, and the national environmental protection policy is not met; in the chloropropene direct epoxidation process, when a large amount of other third-party solvents are used, the problems of low product yield, overlarge circulation amount in a system, high separation difficulty, high system energy consumption and the like are caused.
Disclosure of Invention
The invention aims to provide a method for producing segmented epichlorohydrin, which aims to solve the problems of low raw material utilization rate, low reaction efficiency, high energy consumption and environmental pollution in the prior art, and the product yield is to be improved.
The purpose of the invention is realized as follows:
a production method of segmented epichlorohydrin comprises the following steps:
(a) adding chloropropene, aqueous hydrogen peroxide, a titanium-silicon catalyst and a pH regulator into a solvent-free reaction system to perform epoxidation reaction of chloropropene;
(b) the reaction liquid of the solvent-free reaction system is subjected to oil-water separation to obtain an oil phase (mainly containing chloropropene and epichlorohydrin) and a catalyst-containing water phase (mainly containing water and H)2O2And a catalyst), wherein the oil phase is refined to obtain epichlorohydrin; the water phase containing the catalyst enters a solvent reaction system, and the epoxidation reaction is continuously carried out under the participation of the solvent;
(c) and separating the reaction liquid of the solvent reaction system to obtain reaction clear liquid and catalyst slurry, and refining the reaction clear liquid to obtain the epichlorohydrin.
The solvent-free reaction system and the solvent reaction system can select the number of reaction sections, the type of the reactors, the number of the reactors and the like according to the actual situation of a production field. The solvent-free reaction system and the solvent reaction system can adopt a single-stage reaction or at least two-stage multi-stage reaction; in each stage of reaction, a single reactor can be adopted, or a plurality of reactors connected in series and/or in parallel can be adopted, and the volumes of the reactors can be the same or different; the reactor can be one or more of a slurry bed reactor, a micro-reactor and a tubular reactor. Preferably, the solvent-free reaction system employs a two-stage reaction, and the solvent reaction system employs a one-stage reaction.
In the solvent-free reaction system and/or the solvent reaction system, if a multi-stage reaction or a plurality of reactors are adopted, the process parameters in each reactor are within the following proper range, and the process parameters in each reactor can be the same or different; when the water phase containing the catalyst obtained after the oil-water separation of the reaction liquid in the previous stage reactor enters the next stage reactor or the reaction system with the solvent, chloropropene can be supplemented into the reactor in the next stage reactor or the reactor in the reaction system with the solvent to carry out the epoxidation reaction.
In the step (a), in each reaction section, the mol ratio of chloropropene to hydrogen peroxide is 1 ~ 20: 1, the mass of a titanium-silicon catalyst accounts for 1% ~ 20% of the total mass of the reaction raw materials, the pH of the reaction system is adjusted to 1 ~ 11 by using a pH regulator, preferably, the mol ratio of chloropropene to hydrogen peroxide is 1 ~ 6: 1, the mass of the titanium-silicon catalyst accounts for 1% ~ 10% of the total mass of the reaction raw materials, and the pH of the reaction system is 2 ~ 8.
In the step (a), the reaction temperature is 20 ~ 85 ℃, the reaction pressure is normal pressure or low pressure, and the reaction residence time is 30 ~ 400min, preferably, the reaction temperature is 30 ~ 60 ℃, the reaction pressure is 0 ~ 0.5MPa, and the reaction residence time is 30 ~ 300 min;
in step (a), the mass fraction of hydrogen peroxide in the aqueous hydrogen peroxide solution is 5% ~ 70%, preferably 27.5% ~ 50%.
In the step (b), in each reaction section, the mol ratio of chloropropene to hydrogen peroxide is 1 ~ 20: 1, the mass of the titanium-silicon catalyst accounts for 1% ~ 20% of the total mass of the reaction raw material, the pH of the reaction system is adjusted to 1 ~ 11 by adopting a pH regulator, the mol ratio of the solvent to the hydrogen peroxide is 0.5 ~ 10: 1, preferably, the mol ratio of chloropropene to hydrogen peroxide is 1 ~ 6: 1, the mass of the titanium-silicon catalyst accounts for 1% ~ 10% of the total mass of the reaction raw material, the pH of the reaction system is 2 ~ 8, and the mol ratio of the solvent to the hydrogen peroxide is 1 ~ 6: 1.
In the step (b), the solvent is one or more of methanol, acetonitrile and heavy aromatic hydrocarbon; the reaction solvent is preferably methanol.
In the step (b), the reaction temperature is 20 ~ 85 ℃, the reaction pressure is normal pressure or low pressure, the reaction residence time is 30 ~ 400min, preferably, the reaction temperature is 30 ~ 60 ℃, the reaction pressure is 0 ~ 0.5MPa, and the reaction residence time is 30 ~ 300 min.
In the step (b), chloropropene is removed from the oil phase through raw material recovery, and epichlorohydrin is obtained after product refining.
In the step (c), the reaction clear liquid is refined to obtain epoxy chloropropane through product refining, and the reaction process water is obtained through process water treatment.
In the step (c), after the solvent of the catalyst slurry is removed, the catalyst slurry is utilized by one of the following three ways: can directly enter a reaction system (a solvent-free reaction system and/or a solvent reaction system) to participate in epoxidation reaction; can enter a reaction system (a solvent-free reaction system and/or a solvent reaction system) to participate in the epoxidation reaction in a part, and can carry out catalyst regeneration in a part; the catalyst may be entirely regenerated. Preferably, after the solvent is removed from the catalyst slurry, a part of the catalyst slurry enters a reaction system (a solvent-free reaction system and/or a solvent reaction system) to participate in the epoxidation reaction, and a part of the catalyst slurry is regenerated.
In the steps (b) and (c), the separation can adopt one or more of cyclone separation, centrifugal separation, plate-frame filtration, membrane separation, filter bag separation, extraction separation and sedimentation; preferably, one or more of cyclone separation, membrane separation, extraction separation and centrifugal separation are adopted.
The method takes chloropropene and hydrogen peroxide as raw materials, adopts a combination mode of solvent-free reaction and reaction with solvent participation, and combines a multi-section reaction separation process, thereby improving the production efficiency, reducing the ineffective decomposition rate of the hydrogen peroxide, effectively improving the conversion rate of the hydrogen peroxide (more than or equal to 97 percent based on epichlorohydrin), and basically avoiding oxygen in the gas phase at the upper part of each section of reactor without complicated gas phase deoxidation process and equipment; the solvent consumption is less, no third party solvent participates, and the system circulation amount is small; the side reaction and the by-product are few, the yield of the target product is high, and the reaction selectivity of the epichlorohydrin is more than or equal to 98 percent (calculated by the epichlorohydrin).
The method has the advantages of simple process, mild conditions, realization of online application of the catalyst, less waste water, waste gas and waste residue, no generation of saponified wastewater, green, safe and environment-friendly process, great reduction of production cost and energy consumption of environmental protection equipment investment, equipment operation cost and the like, and wide industrial application prospect and good social and economic benefits.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The invention is further illustrated by the following examples, which are given by way of illustration only and are not intended to limit the scope of the invention in any way.
Procedures and methods not described in detail in the following examples are conventional methods well known in the art, and reagents used in the examples are commercially available or prepared by methods well known to those of ordinary skill in the art. The following examples all achieve the objects of the present invention.
Example 1
The solvent-free reaction system of the embodiment adopts a two-stage reaction mode and comprises a first-stage reactor and a second-stage reactor; the solvent reaction system adopts a one-stage reaction mode. Referring to the schematic process flow diagram of the invention given in fig. 1, the process of the invention comprises the following steps:
adding chloropropene, hydrogen peroxide, a titanium silicon catalyst and a pH regulator into a first-stage reactor of a solvent-free reaction system according to the following proportion, wherein the hydrogen peroxide is a hydrogen peroxide aqueous solution, the mass concentration of the hydrogen peroxide is 50%, the molar ratio of chloropropene to hydrogen peroxide is 3, the mass of the titanium silicon catalyst accounts for 5% of the total mass of reaction raw materials, ammonia water is used as the pH regulator of the solution to regulate the pH value of the solution to be 3, the reaction temperature is controlled to be 40 ℃, the pressure is normal pressure, and the reaction retention time is 60 min;
performing oil-water separation on the produced liquid of a first-stage reactor of the solvent-free reaction system, recovering and removing chloropropene from the oil phase through raw materials, and refining the product to obtain a product epichlorohydrin; introducing the water phase containing the catalyst into a second-stage reactor of a solvent-free reaction system, supplementing chloropropene into the second-stage reactor, enabling the molar ratio of chloropropene to hydrogen peroxide to be 3, using ammonia water as a solution pH regulator, regulating the pH value of the solution to be 3, controlling the reaction temperature to be 40 ℃, the pressure to be normal pressure, and the reaction retention time to be 60 min;
carrying out oil-water separation on reaction liquid of a second-stage reactor of the solvent-free reaction system, wherein chloropropene is removed from the oil phase through raw material recovery, and a product epichlorohydrin is obtained after the product is refined; the water phase containing the catalyst enters a reactor at the first section of the solvent reaction system;
mixing a catalyst-containing water phase with a solvent methanol in a reactor at one section of a solvent reaction system, supplementing chloropropene into the reactor, so that the molar ratio of chloropropene to hydrogen peroxide is 5, the molar ratio of methanol to hydrogen peroxide is 2, using ammonia water as a solution pH regulator, regulating the pH value of the solution to be 3, controlling the reaction temperature to be 43 ℃, the pressure to be normal pressure, and the reaction retention time to be 60 min;
separating the reaction produced liquid of a reactor at one section of a solvent reaction system, refining the clear liquid containing the epoxy chloropropane by products and treating the clear liquid by process water to obtain the epoxy chloropropane and the reaction process water, and mechanically applying the slurry containing the catalyst after removing the solvent by a solvent removal system.
The detection proves that the conversion rate of the hydrogen peroxide is 99.4 percent, and the reaction selectivity is 98.1 percent.
Example 2
The solvent-free reaction system of the embodiment adopts a two-stage reaction mode and comprises a first-stage reactor and a second-stage reactor; the solvent reaction system adopts a one-stage reaction mode. Referring to the schematic process flow diagram of the invention given in fig. 1, the process of the invention comprises the following steps:
adding chloropropene, hydrogen peroxide, a mechanically applied titanium-silicon catalyst, a fresh titanium-silicon catalyst and a pH regulator into a first-stage reactor of a solvent-free reaction system according to the following proportion, wherein the concentration of the hydrogen peroxide in the aqueous solution of the hydrogen peroxide is 50 percent, the molar ratio of the chloropropene to the hydrogen peroxide is 3, the mass of the titanium-silicon catalyst accounts for 5 percent of the total mass of reaction raw materials, the mass ratio of the mechanically applied titanium-silicon catalyst to the fresh titanium-silicon catalyst is 7:3, ammonia water is used as the pH regulator of the solution to regulate the pH value of the solution to be 3, the reaction temperature is controlled to be 40 ℃, the pressure is normal pressure, and the reaction retention time is 60 min;
carrying out oil-water separation on the produced liquid of a first-stage reactor of a solvent-free reaction system, wherein chloropropene is removed from the oil phase through raw material recovery, and a product epichlorohydrin is obtained after the product is refined; introducing the water phase containing the catalyst into a second-stage reactor of a solvent-free reaction system, supplementing chloropropene into the water phase to ensure that the mol ratio of chloropropene to hydrogen peroxide is 3, using ammonia water as a solution pH regulator, regulating the pH value of the solution to be 3, controlling the reaction temperature to be 40 ℃, the pressure to be normal pressure, and the reaction retention time to be 60 min;
carrying out oil-water separation on reaction liquid of a second-stage reactor of the solvent-free reaction system, recovering and removing chloropropene from an oil phase through a raw material, and refining a product to obtain a product epichlorohydrin; the water phase containing the catalyst enters a reactor at the first section of the solvent reaction system;
mixing the water phase containing the catalyst with a solvent methanol in a reactor at one section of a solvent reaction system, supplementing chloropropene into the reactor, so that the molar ratio of chloropropene to hydrogen peroxide is 5, the molar ratio of methanol to hydrogen peroxide is 2, using ammonia water as a solution pH regulator, regulating the pH value of the solution to be 3, controlling the reaction temperature to be 43 ℃, the pressure to be normal pressure, and the reaction retention time to be 60 min;
separating the reaction produced liquid of a reactor at one section of a solvent reaction system, refining the clear liquid containing the epoxy chloropropane by products and treating the clear liquid by process water to obtain the epoxy chloropropane and the reaction process water, and mechanically applying the catalyst-containing slurry after removing the solvent by a solvent removal system.
The detection proves that the conversion rate of the hydrogen peroxide is 98.8 percent, and the reaction selectivity is 98.2 percent.
Example 3
The solvent-free reaction system of this example employs a one-stage reaction mode, and the solvent reaction system also employs a one-stage reaction mode. Referring to the schematic process flow diagram of the invention given in fig. 1, the process comprises the following steps:
adding chloropropene, hydrogen peroxide, a mechanically applied titanium-silicon catalyst, a fresh titanium-silicon catalyst and a pH regulator into a first-stage reactor of a solvent-free reaction system according to the following proportion, wherein the concentration of the hydrogen peroxide in the aqueous solution of the hydrogen peroxide is 50 percent, the molar ratio of the chloropropene to the hydrogen peroxide is 3, the mass of the titanium-silicon catalyst accounts for 5 percent of the total mass of reaction raw materials, the mass ratio of the mechanically applied titanium-silicon catalyst to the fresh titanium-silicon catalyst is 7:3, ammonia water is used as the pH regulator of the solution to regulate the pH value of the solution to be 3, the reaction temperature is controlled to be 40 ℃, the pressure is normal pressure, and the reaction retention time is 60 min;
oil-water separation is carried out on the produced liquid of a first-stage reactor of the solvent-free reaction system, chloropropene is removed from the oil phase through raw material recovery, and epichlorohydrin is obtained after the product is refined; the water phase containing the catalyst enters a reactor at the first section of the solvent reaction system;
mixing the water phase containing the catalyst with a solvent methanol in a reactor at one section of a solvent reaction system, supplementing chloropropene into the reactor, so that the molar ratio of chloropropene to hydrogen peroxide is 2, the molar ratio of methanol to hydrogen peroxide is 2, using ammonia water as a solution pH regulator, regulating the pH value of the solution to be 3, controlling the reaction temperature to be 43 ℃, the pressure to be normal pressure, and the reaction retention time to be 60 min;
separating the reaction produced liquid of a reactor at one section of a solvent reaction system, refining the clear liquid containing the epoxy chloropropane by products and treating the clear liquid by process water to obtain the epoxy chloropropane and the reaction process water, and mechanically applying the catalyst-containing slurry after removing the solvent by a solvent removal system.
The detection proves that the conversion rate of the hydrogen peroxide is 99.6 percent, and the reaction selectivity is 98 percent.
Claims (10)
1. A production method of segmented epichlorohydrin is characterized by comprising the following steps:
(a) adding chloropropene, aqueous hydrogen peroxide, a titanium-silicon catalyst and a pH regulator into a solvent-free reaction system to perform epoxidation reaction of chloropropene;
(b) carrying out oil-water separation on reaction liquid of the solvent-free reaction system to obtain an oil phase and a water phase containing a catalyst, wherein the oil phase is refined to obtain epichlorohydrin; the water phase containing the catalyst enters a solvent reaction system, and the epoxidation reaction is continuously carried out under the participation of the solvent;
(c) and separating the reaction liquid of the solvent reaction system to obtain reaction clear liquid and catalyst slurry, and refining the reaction clear liquid to obtain the epichlorohydrin.
2. The staged epichlorohydrin production process of claim 1, wherein the solvent-free reaction system employs a single-stage reaction or at least a two-stage reaction; each reaction section adopts a single reactor or a plurality of reactors connected in series and/or in parallel;
the solvent reaction system adopts a single-stage reaction or at least two-stage reaction; a single reactor or a plurality of reactors connected in series and/or in parallel are adopted in each reaction section.
3. The segmented epichlorohydrin production method according to claim 2, wherein the reactor is one or more of a slurry bed reactor, a microreactor and a tubular reactor.
4. The segmented epichlorohydrin production method according to claim 2, wherein in each of the steps (a) and (b), the molar ratio of chloropropene to hydrogen peroxide is 1 ~ 20: 20, the mass of the titanium-silicon catalyst accounts for 1% ~ 20% of the total mass of the reaction raw materials, and the pH of the reaction system is adjusted to 1 ~ 11 by using a pH regulator.
5. The segmented epichlorohydrin production method according to claim 1, wherein in the steps (a) and (b), the reaction temperature is 20 ~ 85 ℃, the reaction pressure is normal pressure or low pressure, and the reaction residence time is 30 ~ 400 min.
6. The segmented epichlorohydrin production process according to claim 1, wherein the mass fraction of hydrogen peroxide in the aqueous hydrogen peroxide solution in steps (a) and (b) is 5% ~ 70%.
7. The segmented epichlorohydrin production process of claim 1, wherein in the step (b), the molar ratio of the solvent to the hydrogen peroxide is 0.5 ~ 10: 1.
8. The segmented epichlorohydrin production method according to claim 1, wherein in the step (b), the solvent is one or more of methanol, acetonitrile and heavy aromatic hydrocarbon.
9. The segmented epichlorohydrin production method according to claim 1, wherein in the steps (b) and (c), the separation is one or more of cyclone separation, centrifugal separation, plate-and-frame filtration, membrane separation, filter bag separation, extraction separation and sedimentation.
10. The segmented epichlorohydrin production method according to claim 1, wherein in the step (c), the catalyst slurry is subjected to solvent removal and then is utilized in one of three ways: entering the solvent-free reaction system and/or the solvent reaction system to participate in epoxidation reaction; all the catalyst is regenerated; one part enters the solvent-free reaction system and/or the solvent reaction system to participate in the epoxidation reaction, and the other part is regenerated.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112957770A (en) * | 2021-03-11 | 2021-06-15 | 江苏扬农化工集团有限公司 | Continuous extraction device and continuous extraction method for epichlorohydrin |
| CN113717130A (en) * | 2021-10-08 | 2021-11-30 | 中化学科学技术研究有限公司 | Continuous production device and method of epoxy cyclohexane |
| CN116514741A (en) * | 2023-07-04 | 2023-08-01 | 山东民基新材料科技有限公司 | Process for producing epoxy chloropropane by utilizing micro-interface reaction |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112957770A (en) * | 2021-03-11 | 2021-06-15 | 江苏扬农化工集团有限公司 | Continuous extraction device and continuous extraction method for epichlorohydrin |
| CN112957770B (en) * | 2021-03-11 | 2023-02-21 | 江苏扬农化工集团有限公司 | Continuous extraction device and continuous extraction method for epichlorohydrin |
| CN113717130A (en) * | 2021-10-08 | 2021-11-30 | 中化学科学技术研究有限公司 | Continuous production device and method of epoxy cyclohexane |
| CN113717130B (en) * | 2021-10-08 | 2024-04-05 | 中化学科学技术研究有限公司 | Continuous production method of epoxycyclohexane |
| CN116514741A (en) * | 2023-07-04 | 2023-08-01 | 山东民基新材料科技有限公司 | Process for producing epoxy chloropropane by utilizing micro-interface reaction |
| CN116514741B (en) * | 2023-07-04 | 2023-09-26 | 山东民基新材料科技有限公司 | Process for producing epoxy chloropropane by utilizing micro-interface reaction |
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