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N-methyl pyrrolidone for liquid crystal display panel and production process thereof

A technology of methylpyrrolidone and liquid crystal panels, applied in the field of N-methylpyrrolidone for liquid crystal panels and its production process, can solve the problems of difficult operation and control, large waste of materials, low efficiency, etc. Facilitate the control effect

Inactive Publication Date: 2020-11-06
MAIQI CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] For the removal of impurity metal ions in N-methylpyrrolidone, U.S. Patent No. 4,965,370 removes impurity metal ions by adding alkali metals or alkali metal salts, and then obtains high-purity NMP through continuous fractional distillation; CN110551051A discloses a method for removing metal ions The method of content and particle size is the technology of amination of methylamine and γ-butyrolactone (GBL) to prepare N-methylpyrrolidone, in which the most critical metal ion particles are removed in the final stage of filtration and demagnetization control stage , but did not explain whether the fiber after filtration needs to be renewed or revived; CN108299266A discloses a method for preparing high-purity N-methylpyrrolidone that uses a permeable air synovial membrane module to remove moisture in the raw material solution, and then passes through strong Acidic styrene-based cation-exchange resin or weakly acidic acrylic-based cation-exchange resin to filter metal ions or particles; CN102399179B The production method of ultra-pure N-methylpyrrolidone uses industrial-grade N-methylpyrrolidone as raw material, pretreated, 4A molecular sieve Adsorption and dehydration, through β-cyclodextrin composite membrane and 18-crown-6-composite membrane for two membrane filtrations, the filtrate is rectified under reduced pressure, the collected fractions are condensed and then passed through a microporous membrane for three-stage membrane filtration, Obtain the target product; CN102190611 and CN102001986A publicly show that resin treatment and filtration are used, but the resin needs regeneration and material replacement, industrial sewage treatment and material waste are large, and the metal ion content in the product belongs to trace impurities, and the resin regeneration link uses Regeneration solutions such as hydrochloric acid require high-purity reagents, and it is difficult to ensure the content of metal impurities, which indirectly increases the cost of production and environmental protection treatment, and is not suitable for industrial production and purification.
But generally speaking, the above-mentioned methods have complicated operation process, difficult operation control, high energy consumption and low efficiency.
[0006] 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)

Method used

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  • N-methyl pyrrolidone for liquid crystal display panel and production process thereof
  • N-methyl pyrrolidone for liquid crystal display panel and production process thereof
  • N-methyl pyrrolidone for liquid crystal display panel and production process thereof

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Experimental program
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Effect test

Embodiment 1

[0097] A kind of production technology of N-methylpyrrolidone for liquid crystal panel, comprises the following steps:

[0098] 1. Reaction section: including two-step reaction.

[0099]The first step of amination reaction: First, inject monomethylamine and γ-butyrolactone with a molar ratio of 1.2:1 into the mixing tank respectively by the feed pump, control the stirring preheating temperature at 30°C, stir for 5 minutes, and carry out another Preheating, the preheating temperature is 120°C, and then pumped into a fixed-bed reactor filled with catalyst for amination reaction through a metering pump, the reaction temperature is 200°C, the reaction pressure is 5MPa; the liquid hourly space velocity is 0.5h -1 , to obtain N-methylpyrrolidone crude liquid, the crude liquid is discharged through the material outlet of the reactor, and the content of gamma-butyrolactone in the crude liquid discharged through the discharge port is controlled to be less than or equal to 0.01%;

[01...

Embodiment 2

[0107] A kind of production technology of N-methylpyrrolidone for liquid crystal panel, comprises the following steps:

[0108] 1. Reaction section: including two-step reaction.

[0109] The first step of amination reaction: First, inject monomethylamine and γ-butyrolactone with a molar ratio of 1.3:1 into the mixing tank respectively by the feed pump, control the stirring preheating temperature at 35°C, stir for 8 minutes, and carry out another Preheating, the preheating temperature is 160°C, and then pumped into a fixed bed reactor filled with catalyst for amination reaction through a metering pump, the reaction temperature is 230°C, the reaction pressure is 5.5MPa; the liquid hourly space velocity is 5h -1 , to obtain N-methylpyrrolidone crude liquid, the crude liquid is discharged through the material outlet of the reactor, and the content of gamma-butyrolactone in the crude liquid discharged through the discharge port is controlled to be less than or equal to 0.01%;

[0...

Embodiment 3

[0117] A kind of production technology of N-methylpyrrolidone for liquid crystal panel, comprises the following steps:

[0118] 1. Reaction section: including two-step reaction.

[0119]The first step of amination reaction: First, inject monomethylamine and γ-butyrolactone with a molar ratio of 1.5:1 into the mixing tank by the feed pump, control the stirring preheating temperature at 40°C, stir for 10 minutes, and carry out another Preheating, the preheating temperature is 200°C, and then pumped into a fixed-bed reactor filled with catalyst for amination reaction through a metering pump, the reaction temperature is 260°C, the reaction pressure is 6MPa; the liquid hourly space velocity is 10h -1 , to obtain N-methylpyrrolidone crude liquid, the crude liquid is discharged through the material outlet of the reactor, and the content of gamma-butyrolactone in the crude liquid discharged through the discharge port is controlled to be less than or equal to 0.01%;

[0120] The secon...

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Abstract

The invention discloses a production process of N-methyl pyrrolidone for a liquid crystal display panel. The process comprises a reaction section, an intermittent purification section, a gas strippingpurification section and a secondary rectification purification section, compared with the prior art, the method has the advantages that the N-methyl pyrrolidone product can reach the SEMI C8 standard completely by innovating reaction raw materials, a reaction process and a purification process and strictly controlling process parameters without traditional fiber filtration, and the quality of the product can basically reach the SEMI C12 standard after pressurized adsorption filtration.

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, and more specifically relates to N-methylpyrrolidone for liquid crystal panels and a production process 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...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/267
CPCC07D207/267
Inventor 闫广学肖强周淑飞李清霞吴正岭李凯杨素阁杨理刘红义
Owner MAIQI CHEM CO LTD
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