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Method for preparing N-vinyl pyrrolidone in dehydration mode with N-hydroxyethyl pyrrolidone

A technology of hydroxyethylpyrrolidone and vinylpyrrolidone, which is applied in the field of preparing N-vinylpyrrolidone, and can solve problems such as increasing the market competitiveness of the dehydration method

Active Publication Date: 2016-08-10
XIAN ORIGIN CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalytic performance and reaction process of the catalyst used in this method need to be further improved in order to reduce the cost of the dehydration method and increase the market competitiveness of the dehydration method

Method used

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  • Method for preparing N-vinyl pyrrolidone in dehydration mode with N-hydroxyethyl pyrrolidone
  • Method for preparing N-vinyl pyrrolidone in dehydration mode with N-hydroxyethyl pyrrolidone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0102] Embodiment 1: Preparation of N-vinylpyrrolidone

[0103] The implementation steps of this embodiment are as follows:

[0104] A. Preparation of catalyst

[0105] Prepare according to the catalyst preparation method described in Example 16 of US5625076 specification. Dissolve 10.7g of cesium nitrate in 150ml of deionized water at 90°C, add 30g of white carbon black, stir evenly, and evaporate the solution to dryness by a rotary evaporator. Then the evaporated sample was calcined at 550 °C for 2 hours to obtain the Cs / SiO 2 catalyst.

[0106]B, preparation of N-vinylpyrrolidone

[0107] The acidic component CO 2 Mix with N-hydroxyethylpyrrolidone vapor and inert gas N 2 Mix and heat to the reaction temperature to obtain a gaseous raw material mixture, the specific composition of the gaseous raw material mixture is 0.05CO 2 +0.05NHP+0.9N 2 ;Then,

[0108] Let the raw material mixture be at a temperature of 340°C, a pressure of 0.1MPa and a gas phase space velocity...

Embodiment 2

[0111] Embodiment 2: Preparation of N-vinylpyrrolidone

[0112] The implementation steps of this embodiment are as follows:

[0113] A. Preparation of catalyst

[0114] The catalyst prepared in Example 1 was used.

[0115] B, preparation of N-vinylpyrrolidone

[0116] The acidic component CO 2 Mix with N-hydroxyethylpyrrolidone vapor and water vapor, heat to the reaction temperature to obtain a gaseous raw material mixture, the specific composition of the gaseous raw material mixture is 0.9CO 2 +0.05NHP+0.05H 2 O; then,

[0117] Let the raw material mixture be at a temperature of 350°C, a pressure of 0.1MPa and a gas phase space velocity of 2000h -1 Under the conditions of the Cs / SiO loaded with the preparation of Example 1 2 The fixed-bed reactor of the catalyst, after 10 hours of reaction to reach stability, collect the N-vinylpyrrolidone product discharged from the fixed-bed reactor.

[0118] Using the same analysis method as in Example 1, the N-vinylpyrrolidone pro...

Embodiment 3

[0119] Embodiment 3: Preparation of N-vinylpyrrolidone

[0120] The implementation steps of this embodiment are as follows:

[0121] A. Preparation of catalyst

[0122] The catalyst in Example 1 was used.

[0123] B, preparation of N-vinylpyrrolidone

[0124] The acidic component CO 2 Mix with N-hydroxyethylpyrrolidone vapor and inert gas N 2 Mix and heat to the reaction temperature to obtain a gaseous raw material mixture, the specific composition of the gaseous raw material mixture is 0.3CO 2 +0.4NHP+0.3N 2 ;Then,

[0125] Let the raw material mixture be at a temperature of 370°C, a pressure of 0.1MPa and a gas phase space velocity of 2000h -1 Under the conditions of the Cs / SiO loaded with the preparation of Example 1 2 The fixed-bed reactor of the catalyst, after 10 hours of reaction to reach stability, collect the N-vinylpyrrolidone product discharged from the fixed-bed reactor.

[0126] Using the same analysis method as in Example 1, the N-vinylpyrrolidone produc...

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Abstract

The invention relates to a method for preparing N-vinyl pyrrolidone in a dehydration mode with N-hydroxyethyl pyrrolidone. The method includes the steps that gas with acidic components or alkaline components or liquid with alkaline components and N-hydroxyethyl pyrrolidone are mixed, the mixture passes through a dehydration-catalyst fixed bed reactor under the conditions that temperature ranges from 300 DEG C to 500 DEG C, pressure ranges from 0.01 MPa to 0.1 MPa, and the gas phase airspeed ranges from 10 h-<1> to 5,000 h-<1>, and the N-vinyl pyrrolidone product is obtained. The preparing method is obviously better than the prior art in the conversion rate respect, the selectivity respect and the service life respect.

Description

【Technical field】 [0001] The invention belongs to the technical field of chemical industry. More specifically, the present invention relates to a method for preparing N-vinylpyrrolidone by dehydration of N-hydroxyethylpyrrolidone. 【Background technique】 [0002] N-vinylpyrrolidone (NVP) is the monomer of polyvinylpyrrolidone (PVP), which is widely used in the fields of medicine, cosmetics, disinfectants, oil field collection and water treatment. At present, the industrial synthesis methods of NVP are mainly acetylene method (also known as Reppe method) and dehydration method. The acetylene method is synthesized by acetylene and α-pyrrolidone under high temperature and pressure. This method was industrialized by the German BASF company in 1939. The acetylene method has insurmountable shortcomings such as inflammability and explosion, many wastes, high equipment requirements, and high operating costs. Domestic Scientists at home and abroad have been researching alternative s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/267
Inventor 潘喜强王瑞高亚娜郭彦鑫吴西宁曾清湖李玉洁
Owner XIAN ORIGIN CHEM TECH
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