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A kind of catalyst for preparing chloroacetic acid by catalyzing acetic acid and its preparation and application

A technology of chloroacetic acid and catalyst, which is applied in the field of catalysts for catalyzing acetic acid to prepare chloroacetic acid, can solve problems such as high production labor intensity, product quality decline, and reduced reaction performance, so as to reduce production cost and labor intensity, solve separation problems, and improve selective effect

Active Publication Date: 2021-12-07
SHANGHAI INSTALLATION ENG GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The sulfur catalytic chlorination method mainly has the following problems: (1) the sulfur catalyst is powdery in the reaction system, and it is difficult to separate it from the product and unreacted raw materials after the reaction. The product chloroacetic acid contains a small amount of sulfur. In the case of increasingly high quality requirements, even chloroacetic acid containing a very small amount of sulfur cannot meet the requirements of pharmaceutical fields, food fields, electrical appliances, etc.
(2) The composition of the mother liquor obtained after separating chloroacetic acid is complex, and direct reuse leads to a reduction in reaction performance and a further decline in product quality
(3) A small amount of chloroacetic acid will be deeply chlorinated to generate dichloroacetic acid in the reaction process, and the separation of dichloroacetic acid and chloroacetic acid is extremely difficult. Usually, the method of selective catalytic dechlorination is used to convert dichloroacetic acid into chloroacetic acid, but the product A small amount of sulfur can seriously poison the catalytic dechlorination catalyst, and the catalyst will be deactivated quickly, which will increase the cost of the catalyst in production
(4) It is difficult to dispose of the generated solid waste containing sulfur, and it is also difficult to dispose of the generated liquid waste
(5) Intermittent operation is adopted, the batch quality is unstable, the production capacity of a single set is small, the production labor intensity is high, and the cost is high
Even with continuous operation, there is still the problem of separation of catalyst acetic anhydride

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 70kg of phenol and 100kg of formaldehyde solution into the reactor, stir and mix evenly, add 87.5kg of Cu powder, add 35kg of MgO powder, stir and disperse evenly, heat up to 50°C, react for 0.5h, raise the temperature to 80°C, react for 5h, Add 7kg of paraformaldehyde solid in the reaction kettle, stir and mix evenly to obtain a viscous liquid mixture, discharge it while it is hot, and send it into a granulator to obtain strip particles with a diameter of 3mm and a length of 5mm. Dry at 105°C, then raise the temperature to 130°C for further reaction and solidification, and keep for 1h. in N 2 Under protection, the temperature is raised to 400°C, kept for 300min, the particles are carbonized / graphitized, and the temperature is lowered. Slowly add the obtained carbonized / graphitized particles into the fixed bed reactor to feed 5% HNO 3 Aqueous solution, keep the space velocity at 0.8h -1 , Cu and MgO inside the particles are dissolved and eluted, and after detecti...

Embodiment 2

[0044] Add 13kg of phenol and 100kg of formaldehyde solution into the reactor, stir and mix evenly, add 32kg of Ni powder, add 26kg of ZnO powder, stir and disperse evenly, heat up to 65°C, react for 1h, heat up to 90°C, react for 3h, pour into the reactor Add 11kg of paraformaldehyde solids, stir and mix evenly to obtain a viscous liquid mixture, discharge it while it is hot, and send it into a granulator to obtain strip-shaped granules with a diameter of 3mm and a length of 5mm. It was dried at ℃, then heated to 130℃ for further reaction and solidification, and maintained for 1h. in N 2 Raise the temperature to 750°C under protection, keep it for 10 minutes, carbonize / graphitize the particles, and cool down. Slowly add the obtained carbonized / graphitized particles into the fixed bed reactor to feed 12.5% ​​HNO 3 Aqueous solution, keep the space velocity at 0.5h -1 , the Ni and ZnO inside the particles are dissolved and eluted, and a three-dimensional network-like channel ...

Embodiment 3

[0048] Add 50kg of phenol and 80kg of formaldehyde solution into the reactor, stir and mix evenly, add 75kg of Ni powder, add 10kg of CaO powder, stir and disperse evenly, heat up to 55°C, react for 0.7h, heat up to 85°C, react for 2h, to the reaction Add 17.5kg of hexamethylenetetramine in the kettle, stir and mix evenly to obtain a viscous mixture, discharge it while it is hot, and send it into a granulator to obtain strip-shaped granules with a diameter of 3mm and a length of 5mm. The granules are dried at 105°C, then heated to 160°C for further reaction and solidification, and maintained for 2 hours. in N 2 Under protection, the temperature was raised to 700°C, kept for 50 minutes, the particles were carbonized / graphitized, and the temperature was lowered. Slowly add the obtained carbonized / graphitized particles into the fixed bed reactor to feed 10.5% HNO 3 Aqueous solution, keep the space velocity at 0.25h -1 , the Ni and ZnO inside the particles are dissolved and elu...

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Abstract

The invention relates to a catalyst for preparing chloroacetic acid from acetic acid and its preparation and application. The preparation method of the catalyst is as follows: (1) Mix phenol and formaldehyde aqueous solution, add metal powder and metal oxide, disperse and then heat the reaction (2) continue to add paraformaldehyde solid and / or hexamethylenetetramine in the reaction gained solution, stir and mix evenly, obtain the viscous liquid mixture, discharge while hot, granulate, obtain bar-shaped particle: ( 3) Dry the obtained strip-shaped particles, heat up and solidify, and then continue to heat up under the protection of an inert gas to obtain carbonized / graphitized particles; (4) finally elute the obtained carbonized / graphitized particles with aqueous nitric acid solution to obtain the target product. Compared with the prior art, the present invention effectively solves the problems of separation of the catalyst and the reaction solution, greatly improves the selectivity of the main product chloroacetic acid, and greatly reduces the production cost and labor intensity.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation, and relates to a catalyst for catalyzing acetic acid to prepare chloroacetic acid, as well as its preparation and application. Background technique [0002] Chloroacetic acid (that is, monochloroacetic acid) is an important fine chemical intermediate, known as industrial vitamins, and there are hundreds of downstream products using chloroacetic acid as raw materials. It is widely used in food, materials, electronic appliances and other fields, and occupies an important position in the chemical industry. [0003] The output of chloroacetic acid is increasing year by year. The output of chloroacetic acid in my country accounts for 50% of the world's total output. It is the main producer of chloroacetic acid products. Over the years, the production capacity has increased rapidly, but the production technology has developed very slowly. Most manufacturers The technology of the former Sov...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J21/18B01J35/10C07C51/363C07C53/16
CPCB01J21/18B01J35/10C07C51/363C07C53/16
Inventor 曹贵平张钧钧吕慧殷舫
Owner SHANGHAI INSTALLATION ENG GRP
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