Preparation and application method of metal-free catalyst used for fixed bed acetylene hydrochlorinate preparation of vinyl chloride

An acetylene hydrochlorination and catalyst technology, which is applied in chemical instruments and methods, physical/chemical process catalysts, molecular sieve catalysts, etc. and stability, avoiding collapse, and improving the specific surface area

Active Publication Date: 2018-07-06
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this doping method often cannot effectively and uniformly utilize the nitrogen component in non-metallic compounds. At the same time, the catalytic activity of the metal-free catalyst prepared by the simple "impregnation-calcination" method is relatively low, which is not enough to meet the needs of actual production.

Method used

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  • Preparation and application method of metal-free catalyst used for fixed bed acetylene hydrochlorinate preparation of vinyl chloride
  • Preparation and application method of metal-free catalyst used for fixed bed acetylene hydrochlorinate preparation of vinyl chloride
  • Preparation and application method of metal-free catalyst used for fixed bed acetylene hydrochlorinate preparation of vinyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Add 1g of SBA-15 molecular sieve to a sulfuric acid solution with a mass concentration of 10%, stir at room temperature for more than 6 hours, then filter, separate and wash the molecular sieve to neutrality, and put the obtained filter cake at 120 ℃ Down drying obtains sample A;

[0032] (2) Under the condition of stirring at room temperature, dissolve 0.8g sucrose and 1.6g thiourea in deionized water with 1.5 times the water absorption rate of sample A to obtain a uniform solution, then add the solution to sample A and mix thoroughly, After standing still and sealed for 24 hours, the resulting mixture was transferred to a rotary evaporator and evaporated to dryness in a water bath at 60°C to obtain a precursor;

[0033] (3) Fully grind and mix 3.4g precursor and 13.6g polytetrafluoroethylene powder, transfer the mixture to an alumina tube furnace, and raise the temperature to 300 °C at a rate of 5 °C / min under a flowing inert gas atmosphere. ℃ for 1 hour, then co...

Embodiment 2

[0036] (1) Add 1g of MCM-41 molecular sieve to a sulfuric acid solution with a mass concentration of 10%, stir at room temperature for more than 6 hours, then filter, separate and wash the molecular sieve to neutrality, and put the obtained filter cake at 100 ℃ Down drying obtains sample A;

[0037] (2) Under the condition of stirring at room temperature, dissolve 1g of glucose and 3g of thiourea in deionized water with 2.5 times the water absorption rate of sample A at the same time to obtain a uniform solution, then add the solution to sample A and mix thoroughly, and statically Store in a sealed place for 24 hours, then transfer the resulting mixture to a rotary evaporator, and evaporate to dryness in a water bath at 80°C to obtain a precursor;

[0038] (3) Fully grind and mix 5g precursor and 15g polytetrafluoroethylene powder, transfer the mixture to an alumina tube furnace, and raise the temperature to 300°C at a heating rate of 10°C / min under a flowing inert gas atmosph...

Embodiment 3

[0041] (1) Add 1g of MCM-48 molecular sieve to a sulfuric acid solution with a mass concentration of 10%, stir at room temperature for more than 6 hours, then filter, separate and wash the molecular sieve to neutrality, and put the obtained filter cake at 120 ℃ Down drying obtains sample A;

[0042] (2) Under the condition of stirring at room temperature, dissolve 1.2g sucrose and 2.4g thiourea in deionized water with 2 times the water absorption rate of sample A to obtain a uniform solution, then add the solution to sample A and mix well, at room temperature After standing still and sealed for 48 hours, the resulting mixture was transferred to a rotary evaporator and evaporated to dryness in a water bath at 70°C to obtain a precursor;

[0043] (3) Fully grind and mix 4.6g precursor and 13.8g polytetrafluoroethylene powder, transfer the mixture to an alumina tube furnace, and raise the temperature to 300 at a rate of 7 °C / min under a flowing inert gas atmosphere. ℃ for 1 hour...

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Abstract

The invention relates to a preparation method and an application application method of a metal-free catalyst used for fixed bed acetylene hydrochlorinate preparation of vinyl chloride. Compared with other metal-free catalysts prepared through dipping-calcining method, the metal-free catalyst used for fixed bed acetylene hydrochlorinate preparation of vinyl chloride possesses following advantages:the nitrogen content of the metal-free catalyst used for fixed bed acetylene hydrochlorinate preparation of vinyl chloride is increased through in-suit doping combined ammonia gas treatment; the catalyst specific surface area is increased effectively through calcining of a precursor with polytetrafluoroethylene at a certain heating program, and at the same time nitrogen sulfur codoping and oxidation are adopted to increase the ratio of active sites and the number of surface oxygen-containing function groups, so that the metal-free catalyst possesses relatively activity and selectivity in fixedbed acetylene hydrochlorinate preparation of vinyl chloride. The preparation method is green, and is friendly to the environment; the raw materials are widely available and cheap; the metal-free catalyst can be used for replacing toxic mercuric chloride catalyst; and the application prospect in industrialized production is promising.

Description

technical field [0001] The invention belongs to the field of preparation technology and application technology of catalysts for organic synthesis, and relates to a preparation method and a use method of a metal-free catalyst used for acetylene hydrochlorination to prepare vinyl chloride. Background technique [0002] As one of the most widely used general-purpose plastics in the world, polyvinyl chloride has played an increasingly important role in people's production and life in recent years. Due to China's special energy structure of "poor oil, little gas, and rich coal", the monomer for producing polyvinyl chloride, vinyl chloride, mainly uses mercuric chloride (HgCl) loaded on activated carbon. 2 ) catalyst by acetylene hydrochlorination. However, the high toxicity of mercuric chloride itself and its easy sublimation in the reaction make this production process have serious safety and environmental problems. Therefore, searching for an efficient and environmentally fri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/03C07C17/08C07C21/06
CPCB01J29/005B01J29/0308C07C17/08C07C21/06
Inventor 李伟董晓斌关庆鑫
Owner NANKAI UNIV
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