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Preparation method of catalyst for synthesizing dichloropropanol by glycerin method

A technology of dichloropropanol and catalyst, which is applied in the field of preparation of catalysts for synthesizing dichloropropanol with glycerol method, can solve the problems of difficult catalyst recovery, complicated separation process, and large environmental pollution, and achieves easy separation and simple preparation method , the effect of reducing production costs

Active Publication Date: 2018-12-25
江苏成达化工工程设计有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to: provide a kind of preparation method of the catalyst that glycerol method is used to synthesize dichloropropanol, solve existing method that adopts glycerin as raw material to adopt organic acid, organic nitrile, phosphotungstic acid etc. to catalyze the synthesis of dichloropropanol. Catalysts are easy to generate various by-products with raw materials, which leads to complicated separation process and difficulty in catalyst recovery, which leads to high production costs and serious environmental pollution.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] Embodiment 1: according to attapulgite: water=1: 20 mass ratio, get attapulgite and soak in water for 24 hours, stir, cross 120 mesh sieves, add mass concentration 7% dilute hydrochloric acid to the filtrate to adjust PH to be 3, leave standstill for 12 hours, washed with water until neutral, centrifuged, dried at 120°C, and roasted at 250°C for 3 hours to obtain modified attapulgite; use ethyl orthosilicate, deionized water, absolute ethanol, modified attapulgite, The mass ratio of tungstic acid is 14:25:20:0.8:0.56 into the reactor, stirred at 50°C until gel is formed, aged for 24 hours, dried at 80°C for 5 hours, and calcined at 260°C for 4 hours to obtain the catalyst.

[0010] Use the catalyst of Example 1 to catalyze the synthesis of dichloropropanol: take 50g of glycerin, take by weighing 1.5g of the catalyst of Example 1 (by 3% of the glycerin mass), add it to the reaction tank equipped with stirring, temperature measurement and water separation device In the co...

Embodiment 2

[0011] Embodiment 2: according to attapulgite: water=1: 20 mass ratio, get attapulgite and soak in water for 12 hours, stir, cross 120 mesh sieves, add mass concentration 7% dilute hydrochloric acid to the filtrate to adjust PH to be 4, leave standstill for 12 hours, washed with water until neutral, centrifuged, dried at 120°C, and roasted at 280°C for 3 hours to obtain modified attapulgite; use ethyl orthosilicate, deionized water, absolute ethanol, modified attapulgite, The mass ratio of tungstic acid is 14:28:22:0.9:1.67 into the reactor, stirred at 50°C until gel is formed, aged for 24 hours, dried at 90°C for 5.5 hours, and calcined at 270°C for 5 hours to obtain the catalyst.

[0012] The catalyst of Example 2 was used to catalyze the synthesis of dichloropropanol, the reaction conditions were the same as in Example 1, the yield of the catalyst for the first catalysis was 92.8%, and the yield of the fifth repeated use was 90.3%.

Embodiment 3

[0013] Embodiment 3: according to attapulgite: water=1: 20 mass ratio, get attapulgite and soak in water for 24 hours, stir, cross 120 mesh sieves, add mass concentration 7% dilute hydrochloric acid to the filtrate to adjust PH to be 4, leave standstill for 12 hours, washed with water until neutral, centrifuged, dried at 120°C, and roasted at 310°C for 3 hours to obtain modified attapulgite; use ethyl orthosilicate, deionized water, absolute ethanol, modified attapulgite, The mass ratio of tungstic acid is 14:30:23:1:2.78 into the reactor, stirred at 50°C until gel is formed, aged for 24 hours, dried at 100°C for 6 hours, and calcined at 280°C for 6 hours to obtain the catalyst.

[0014] The catalyst of Example 3 was used to catalyze the synthesis of dichloropropanol, the reaction conditions were the same as in Example 1, the yield of the first catalysis of the catalyst was 94.5%, and the yield of the fifth repeated use was 92.6%.

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PUM

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Abstract

The invention discloses a preparation method of a catalyst for glycerol method-based synthesis of dichloropropanol. The method comprises taking attapulgite according to a mass ratio of attapulgite to water of 1: 20, immersing the attapulgite in water for 24h, stirring the solution, screening the solution through a sieve of 120 meshes, adding dilute hydrochloric acid with a mass concentration of 7% into the filtrate to adjust pH to 3-6, standing the filtrate for 12 hours, carrying out water washing until pH is 7, carrying out centrifugal separation, carrying out drying at 120 DEG C, carrying out roasting at 250-350 DEG C for 3 hours to obtain modified attapulgite, mixing ethyl orthosilicate, deionized water, absolute ethanol, the modified attapulgite and phosphotungstic acid according to a ratio of 14: 25-35: 20-25: 0.8-1.2: 0.56-5 at a temperature of 50 DEG C to obtain gel, carrying out aging for 24 hours, carrying out drying at a temperature of 80-120 DEG C for 5 to 7 hours, and carrying out roasting at a temperature of 260-300 DEG C for 4 to 8 hours so that the catalyst is obtained. The catalyst prepared by the invention has the advantages of high activity, good stability, no corrosion on the equipment, easy separation from the product, recyclability and high yield of glycerol hydrochlorination catalytic synthesis of dichloropropanol.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to a method for preparing a catalyst for synthesizing dichloropropanol by a glycerin method, in particular to a method for preparing a catalyst for synthesizing dichloropropanol by a glycerin method and using silicon dioxide and attapulgite to compositely support phosphotungstic acid catalyst Preparation. Background technique [0002] Dichloropropanol is an important chemical intermediate and an important raw material for the synthesis of epichlorohydrin, crosslinking agent, water treatment agent, and medicine, and has a good market prospect. The production methods of dichloropropanol mainly include propylene high-temperature chlorination method, propylene acetate method, and glycerin hydrochlorination method. The high-temperature chlorination of propylene and the propylene acetate method use propylene, a product of petroleum cracking, as the raw material. The costs of these two proc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/199C07C29/62C07C31/36
CPCB01J27/199C07C29/62C07C31/36
Inventor 钱运华张明轩叶斐斐李东杜卫刚杨勇周伟吴彩金程晓春
Owner 江苏成达化工工程设计有限公司