Loaded mercury-free catalyst for vinyl chloride preparation by hydrochlorination of acetylene and preparation method thereof

A technology of acetylene hydrochlorination and mercury catalyst, applied in catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, etc., can solve the problems that have not yet been seen, improve catalyst performance, etc. , to achieve the effect of simple pretreatment device, simple preparation method and good catalytic performance

Inactive Publication Date: 2012-04-18
XINJIANG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report in the open literature to improve the performance of the catalyst by pretreating the activated carbon carrier.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1: Weigh 5-20 g of dry activated carbon, place it in 30% hydrochloric acid solution and stir evenly. Heating and magnetic stirring in a water bath at 50-80°C, dipping, cooling and reflux for 3-8 hours, then filtering, washing to weak acidity, drying at 105°C for 2-8 hours for later use. 10~30mL of H 2 PdCl 4 The impregnating solution is impregnated on the activated carbon, and after impregnating by ultrasonic or rotary evaporation for 2-8 hours, the obtained impregnated product is dried at 110-120° C. for 3-10 hours, and the loading amount of Pd in ​​the catalyst on the carrier is 0.1-3wt%.

[0018] Put 1-5g of the above-mentioned catalyst into a fixed-bed reactor (quartz glass material) with an inner diameter of 10mm, at a gas space velocity of 120h -1 , the reaction temperature is 160°C, the reaction gas ratio is V(HCl):V(C 2 h 2 )=1.15 under the condition that this catalyst is carried out the test of acetylene hydrochlorination reaction activity, analy...

Embodiment 2

[0019] Embodiment 2: Weigh 5-20 g of dry activated carbon, place it in 20% phosphoric acid solution and stir evenly. Heating and magnetic stirring in a water bath at 50-80°C, dipping, cooling and reflux for 3-8 hours, then filtering, washing to weak acidity, drying at 105°C for 3-10 hours for later use. 10~30mL of H 2 PdCl 4 The impregnating solution is impregnated on the activated carbon, and after impregnating by ultrasonic or rotary evaporation for 2-8 hours, the obtained impregnated product is dried at 110-120° C. for 3-10 hours, and the loading amount of Pd in ​​the catalyst on the carrier is 0.1-3wt%.

[0020] Put 1-5g of the above-mentioned catalyst into a fixed-bed reactor (quartz glass material) with an inner diameter of 10mm, at a gas space velocity of 120h -1 , the reaction temperature is 160°C, the reaction gas ratio is V(HCl):V(C 2 h 2 )=1.15 under the condition that this catalyst is carried out the test of acetylene hydrochlorination reaction activity, analys...

Embodiment 3

[0021] Example 3: Soak 5-20 g of dry activated carbon carrier in 30% nitric acid solution, apply ultrasonic treatment for about 1-6 hours, then filter, wash with distilled water to weak acidity, and dry at 105° C. for 3-10 hours for later use. 10~30mL of H 2 PdCl 4 The impregnating liquid is impregnated on the above-mentioned activated carbon, and after impregnating by ultrasonic or rotary evaporation for 2-8 hours, the obtained impregnated product is dried at 110-120° C. for 3-10 hours. The loading amount of Pd on the carrier in the catalyst is 0.1-3wt%.

[0022] Put the above-mentioned 1-5g catalyst into a 10mm fixed-bed reactor (quartz glass material), at a gas space velocity of 120h -1 , the reaction temperature is 160°C, the reaction gas ratio is V(HCl):V(C 2 h 2 )=1.15 under the condition that this catalyst is carried out the test of acetylene hydrochlorination reaction activity, analysis tail gas, the conversion rate of acetylene of catalyst is 97.78%, vinyl chlorid...

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PUM

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Abstract

The invention discloses a loaded mercury-free catalyst for vinyl chloride preparation by hydrochlorination of acetylene and a preparation method thereof. The catalyst comprises precious metals/active carbon. The load capacity of the active components in the catalyst on a carrier is 0.1-3 wt%. The catalyst is prepared by carrier pretreatment and dipping, and a test for acetylene hydrochlorination activity is performed under a condition with a raw material gas space velocity of 120 h-1, a raw material gas ratio of V(HCl):V(C2H2) of 1.15, a normal pressure, and a reaction temperature of 160 DEG C. The advantages of the invention are that: the catalyst has good environmental benefits; the catalyst has a simple composition, and high catalytic activity; the acetylene conversion rate is more than 96%; the selectivity is high; the vinyl chloride selectivity is up to above 98%.

Description

(1) Technical field [0001] The invention relates to a preparation method of a supported noble metal catalyst for acetylene hydrochlorination, and belongs to the field of catalyst preparation technology and application in organic synthesis. (2) Background technology [0002] Vinyl chloride (VCM) is mainly used in the synthesis of polyvinyl chloride resin (PVC). Polyvinyl chloride resin is one of the top five engineering plastics in the world, widely used in industry, construction, agriculture, daily life, packaging, electric power, public utilities and other fields. In my country, due to the continuous economic growth, the progress of resin synthesis technology and processing technology, especially the development of urbanization and real estate industry, the market demand for PVC is strong, and it has become the largest PVC production and consumption country in the world. [0003] At present, there are three main methods for industrial production of vinyl chloride monomer: ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J37/34B01J37/02C07C21/06C07C17/08
Inventor 王吉德马磊王丰朱沛叶王璐
Owner XINJIANG UNIVERSITY
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