Titanium-based heterogeneous amination composite catalyst as well as preparation method and application thereof

一种复合催化剂、催化剂载体的技术，应用在催化剂活化/制备、物理/化学过程催化剂、化学仪器和方法等方向，能够解决操作过程复杂、操作控制困难、效率低等问题，达到优化反应历程、比表面积大、防止漏流的效果

Inactive Publication Date: 2020-11-24
MAIQI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In addition, the purity of N-methylpyrrolidone in China is currently between 99.5% and 99.9%, and its metal particle content is basically between 20 and 30ppb. The national standard has not yet proposed the control requirements for the particle size of N-methylpyrrolidone, but domestic Liquid crystal panel enterprises generally require the content of metal ions in N-methylpyrrolidone to be ≤5ppb, and the particle content to be ≤5 / ml (0.5μm)
[0005] In order to further improve the purity of N-methylpyrrolidone, at present, methods of improving the overall process steps or enhancing the purification process are mostly adopted, but these processes still have the defects of complicated operation process, difficult operation control, high energy consumption and low efficiency.

Method used

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  • Titanium-based heterogeneous amination composite catalyst as well as preparation method and application thereof
  • Titanium-based heterogeneous amination composite catalyst as well as preparation method and application thereof
  • Titanium-based heterogeneous amination composite catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0107] Embodiment 1 of the present invention discloses a titanium-based heterogeneous amination composite catalyst, which is prepared by the following method:

[0108] (1) Al(NO 3 ) 3 9H 2 O, Mo(NO 3 ) 3 ·5H 2 O, Ni(NO 3 ) 2 ·6H 2 Dissolve O in deionized water, prepare a 0.5mol / L solution, raise the temperature to 60°C, add the carrier and stir well, gradually add 0.02mol / L dilute nitric acid or dilute sulfuric acid dropwise during the stirring process, mix well, and control the pH value 5 to 6, and gradually lowered to room temperature to obtain mixed solution A; Al(NO 3 ) 3 9H 2 O, Mo(NO 3 ) 3 ·5H 2 O, Ni(NO 3 ) 2 ·6H 2 The molar ratio of Al, Mo and Ni in O is 1:1.2:0.5;

[0109] (2) put C 16 h 36 o 4 Dissolve Si in 0.02mol / L dilute nitric acid or dilute sulfuric acid, control the temperature at 20-30°C, add C 16 h 36 o 4 Ti, stir, add ammonia water dropwise, control the pH value to 6.5~7.5, continue to stir for 10h, move to the hydration heat reaction...

Embodiment 2

[0113] Embodiment 2 of the present invention discloses a titanium-based heterogeneous amination composite catalyst, which is prepared by the following method:

[0114] (1) Al(NO 3 ) 3 9H 2 O, Mo(NO 3 ) 3 ·5H 2 Dissolve O in deionized water, prepare a 1mol / L solution, raise the temperature to 60-80°C, add the carrier and stir well, gradually add 0.5mol / L dilute nitric acid or dilute sulfuric acid dropwise during the stirring process, mix well, and control the pH The value is 5-6, gradually lowered to room temperature, and mixed solution A is obtained; Al(NO 3 ) 3 9H 2 O, Mo(NO 3 ) 3 ·5H 2 The molar ratio between Al and Mo components in O is 1:0.9;

[0115] (2) put C 16 h 36 o 4 Dissolve Si in 0.02mol / L dilute nitric acid or dilute sulfuric acid, control the temperature at 20-30°C, add C 16 h 36 o 4 Ti, stir, add ammonia water dropwise, control the pH value to 6.5~7.5, continue to stir for 15h, move to the hydration heat reaction kettle and react at 200°C for 24...

Embodiment 3

[0119] Embodiment 3 of the present invention discloses a titanium-based heterogeneous amination composite catalyst, which is prepared by the following method:

[0120] (1) Al(NO 3 ) 3 9H 2 O, Mo(NO 3 ) 3 ·5H 2 O, H 2 PtC l6 ·6H 2 Dissolve O in deionized water, prepare a 0.8mol / L solution, raise the temperature to 70°C, add the carrier and stir well, gradually add 0.3mol / L dilute nitric acid or dilute sulfuric acid dropwise during the stirring process, mix well, and control the pH value 5 to 6, and gradually lowered to room temperature to obtain mixed solution A; Al(NO 3 ) 3 9H 2 O, Mo(NO 3 ) 3 ·5H 2 O, H 2 PtC l6 ·6H 2 The molar ratio of Al, Mo and Pt in O is 1:1.1:0.05;

[0121] (2) put C 16 h 36 o 4 Dissolve Si in 0.02mol / L dilute nitric acid or dilute sulfuric acid, control the temperature at 20-30°C, add C 16 h 36 o 4 Ti, stir, add ammonia water dropwise, control the pH value to 6.5~7.5, continue to stir for 12h, move to the hydration heat reaction k...

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Abstract

The invention discloses a titanium-based heterogeneous amination composite catalyst. The composite catalyst comprises the following components in percentage by mass: 25-35% of Ti, 5-10% of Si, 2-10% of Co, 2-5% of Mn, 1-3% of Mo, 0.5-1.0% of Mg, 0.2-0.5% of Ag and the balance of a carrier. The invention discloses application of the catalyst in the production of N-methyl pyrrolidone. The titanium-based heterogeneous amination composite catalyst obtained by the preparation method disclosed by the invention is large in specific surface area and high in compressive strength, and the production efficiency of the N-methyl pyrrolidone can be effectively improved.

Description

[0001] The present invention is based on the application date of May 08, 2020, the application number of 202010383330.9, and the invention name is a titanium-based heterogeneous amination composite catalyst and its application in the production of N-methylpyrrolidone for liquid crystal panels. A divisional application filed with the application file. technical field [0002] The invention relates to the technical field of preparation of fine chemical products, in particular to a titanium-based heterogeneous amination composite catalyst and a preparation method thereof. Background technique [0003] N-Methylpyrrolidone is a fine chemical with excellent performance. Because of its strong dissolving power, it has a strong dissolving power for polar or non-polar substances. It is known as "universal solvent". As a solvent or organic raw material, it is widely used in industrial fields such as coatings, inks, electronic chemicals, advanced cleaning agents, and power lithium-ion b...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/89B01J37/02C07D207/267
CPCC07D207/267
Inventor 闫广学肖强李凯周淑飞杨理李清霞吴正岭刘红义杨素阁
Owner MAIQI CHEM CO LTD
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