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Preparation method of epoxy chloropropane

A technology of epichlorohydrin and chloropropene, applied in chemical instruments and methods, molecular sieve catalysts, organic chemistry, etc., can solve the problems of high energy consumption, difficult control of reaction temperature, and easy occurrence of side reactions in the saponification and separation process, and achieve side effects The effect of less reaction, easy separation of products, and reduction of potential safety hazards

Active Publication Date: 2020-09-01
TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chlorohydrin method has the following disadvantages: using highly toxic chlorine as a raw material, it significantly reduces safety; the chemical properties of chlorine are active, and side reactions are prone to occur, such as direct addition reactions with chloropropene to generate low-value trichloropropane. It is necessary to add a large amount of water to dilute the chlorine concentration in the reaction system, and control the concentration of the target product dichloropropanol to be lower than 4%, which not only makes the energy consumption of the saponification separation process high, but also produces more than 40 tons of chlorine-containing wastewater per ton of epichlorohydrin. There are also about 2 tons of waste residue, and the by-product trichloropropane is as high as 7%, which is difficult to handle
However, since the epoxidation process of allyl chloride is a strong exothermic reaction, it is difficult to control the reaction temperature when a fixed bed is used, resulting in more by-products and potential safety hazards.

Method used

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  • Preparation method of epoxy chloropropane

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preparation example Construction

[0011] An embodiment of the present invention provides a method for preparing epichlorohydrin, which includes: using a fixed-bed catalytic reactor to reversely feed chloropropene and hydrogen peroxide, and using the balance of solvent vaporization and condensation to maintain the solvent at the level containing the catalyst In the reaction bed layer, allyl chloride and hydrogen peroxide react in the reaction bed layer to generate epichlorohydrin.

[0012] The use of fixed bed technology is an effective method to solve the difficult separation of catalysts in the slurry bed reaction process. It has the characteristics of easy solid-liquid separation, good operating flexibility, large production capacity and simple process. However, since the epoxidation process of allyl chloride is a strong exothermic reaction, it is difficult to control the reaction temperature when a fixed bed is used, resulting in more by-products and potential safety hazards.

[0013] The present invention ...

Embodiment 1

[0034] Embodiment 1 catalyst preparation

[0035] Put 95 grams of commercially available titanium-silicon molecular sieve TS-1 and 5 grams of silica sol on the forming agent to form a columnar catalyst with a diameter of 3 mm and a length of 3 mm, numbered CAT-1.

[0036] Put 80 grams of commercially available titanium-silicon molecular sieve Ti-MWW and 20 grams of aluminum sol on the molding agent to form a spherical catalyst with a diameter of 2.5 mm, numbered CAT-2.

[0037] 60 grams of titanium-silicon molecular sieve TS-2, 20 grams of silica sol and 20 grams of aluminum sol made by the patent CN1111092C modification method are used to form a trilobate-shaped catalyst with an equivalent diameter of 1 mm and a length of 2 mm on the molding agent, numbered CAT -3.

Embodiment 2

[0039] Put 5 grams of Catalyst CAT-1 into figure 1 In the reaction bed layer 3 of the shown reactor, separation fillers are respectively loaded at the upper end 7 and the lower end 8 of the reactor. Put an appropriate amount of solvent methanol into the reactor, and control the temperature in the middle of the reaction bed 3 to 60°C through the heat supply at the lower end 8 of the reactor and the heat extraction at the upper end 7, so that the solvent methanol reaches the equilibrium of vaporization and condensation, and stays at the Catalyst reaction bed 3. With hydrogen peroxide feed space velocity as 1h -1 , transporting 30% hydrogen peroxide to the reactor from the upper end of the reactor, and transporting allyl chloride to the reactor from the lower end of the reactor at the same time, the molar ratio of allyl chloride to hydrogen peroxide is 1:1, and carries out countercurrent epoxidation reaction.

[0040] Results: The conversion rate of hydrogen peroxide was 100%, ...

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Abstract

The invention provides a preparation method of epoxy chloropropane. The preparation method comprises the following steps: performing reverse feeding on chloropropene and hydrogen peroxide by adoptinga fixed bed catalytic reactor, maintaining a solvent in a reaction bed layer containing a catalyst by utilizing the balance of solvent gasification and condensation, and reacting chloropropene and hydrogen peroxide in the reaction bed layer to generate epoxy chloropropane. The preparation method provided by the invention is beneficial to promoting sufficient reaction of chloropropene and hydrogenperoxide in the reaction bed layer, so epoxy chloropropane with relatively high purity is generated, meanwhile, potential safety hazards are reduced, the problem that a catalyst is difficult to separate in the slurry bed reaction process is solved, and the temperature control problem in traditional fixed bed reaction is solved; and reaction and separation are combined in one fixed bed reactor, soepoxy chloropropane is prepared with simple process, low energy consumption and high efficiency.

Description

technical field [0001] The invention relates to the field of preparation of organic chemical intermediates, in particular to a method for preparing epichlorohydrin. Background technique [0002] Epichlorohydrin is an important organic chemical intermediate, mainly used in the production of epoxy resin. In the existing industrial chlorohydrin method, dichloropropanol is prepared through chlorohydrinization reaction of chloropropene, chlorine gas and water, and then further saponified to obtain epichlorohydrin. In the chloroalcoholation reaction, chlorine gas is used as the oxidant and chlorine source, and water provides hydroxyl groups. The reaction mechanism is that the hypochlorous acid oxidized the double bond of chloropropene generated by the reaction of chlorine gas and water, and the electrons on the double bond are transferred to the chlorine atom. At the same time, the chlorine atom Addition to the double bond, followed by nucleophilic attack of the hydroxyl group on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/12C07D303/08B01J29/89B01J35/02
CPCC07D301/12C07D303/08B01J29/89B01J35/50B01J35/40
Inventor 张振涛林民杨俊玲张钰张化福
Owner TECHNICAL INST OF PHYSICS & CHEMISTRY - CHINESE ACAD OF SCI
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