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Method for reducing content and granularity of metal ions in N-methylpyrrolidone

A technology of methylpyrrolidone and metal ions, applied in the chemical industry, can solve the problems of large waste of materials, difficulty in ensuring the content of metal impurities, unsuitable for production and purification, and achieve the effect of low particle size

Active Publication Date: 2019-12-10
SHANDONG QINGYUN CHANGXIN CHEM SCI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The existing patents CN102190611 and CN102001986A disclose that resin treatment and filtration are used, but the resin needs regeneration and material replacement. In industrial production, the industrial sewage treatment and material waste are relatively large. In addition, the content of metal ions in the product is trace Impurities, hydrochloric acid and other regeneration solutions used in resin regeneration require high-purity reagents, which are 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.
[0004] At present, the purity of domestic N-methylpyrrolidone is between 99.5% and 99.9%, and its metal ion content is basically between 20 and 30ppb. The national standard has not yet proposed particle size control requirements, but the domestic semiconductor industry has proposed The particle size content is less than or equal to 5 / mL, so it is necessary to develop this ultra-high-purity N-methylpyrrolidone

Method used

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  • Method for reducing content and granularity of metal ions in N-methylpyrrolidone
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  • Method for reducing content and granularity of metal ions in N-methylpyrrolidone

Examples

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Embodiment 1

[0102] This example provides a method for N-methylpyrrolidone to reduce the content and particle size of metal ions, including the following steps: adding monomethylamine and γ-butyrolactone with a molar ratio of 1:1 to a temperature of 265°C and a pressure of After 1.2 hours of reaction in a 7MPa reactor, the inlet temperature of the crude product obtained by removing water and monomethylamine in an atmospheric column with a temperature of 138°C, a number of trays of 25, a tray height of 5.5m, and a reflux ratio of 0.9 is 128°C, the number of trays is 25, the height of trays is 5.5m, and the reflux ratio is 1. The high boiling point of the rectification tower is 1, and the fine product obtained is filtered by a magnetic field with a magnetic induction intensity of 11000Gs and enters the storage tank. After flowing out of the storage tank, it passes through a primary filter including 15 0.4μm titanium rod filter elements, 15 0.15 The secondary filter of μm polytetrafluoroethyl...

Embodiment 2

[0107] This example provides a method for N-methylpyrrolidone to reduce the metal ion content and particle size, including the following steps: adding monomethylamine and γ-butyrolactone with a molar ratio of 1.1:1 to a temperature of 270°C and a pressure of After reacting in a 9MPa reactor for 2 hours, water and monomethylamine are removed in an atmospheric column with a temperature of 142°C, a plate number of 35, a plate height of 4.5m, and a reflux ratio of 1.1. The obtained crude product enters at a temperature of 132°C, the number of trays is 35, the height of trays is 4.5m, and the reflux ratio is 1.1. The high boiling point of the rectification tower is 1.1, and the fine product obtained is filtered by a magnetic field with a magnetic induction intensity of 13000Gs and then enters the storage tank. After flowing out of the storage tank, it passes through a primary filter including 25 0.5μm titanium rod filter elements, 25 0.25 The secondary filter of μm polytetrafluoroe...

Embodiment 3

[0112] This example provides a method for N-methylpyrrolidone to reduce the content and particle size of metal ions, including the following steps: adding monomethylamine and γ-butyrolactone with a molar ratio of 1:1 to a temperature of 265°C and a pressure of After reacting for 1.5h in the 8MPa reactor, water and monomethylamine are removed in an atmospheric column with a temperature of 140°C, a plate number of 30, a plate height of 5m, and a reflux ratio of 1. The obtained crude product enters at a temperature of 130°C, the number of trays is 30, the height of trays is 5m, and the reflux ratio is 1. The high boiling point is removed from the rectification tower, and the fine product obtained enters the storage tank after being filtered by a magnetic field with a magnetic induction intensity of 12000Gs. After flowing out from the storage tank, it passes through a primary filter including 20 pieces of 0.45μm titanium rod filter elements, and 20 pieces of 0.2μm polymer filter el...

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Abstract

The invention relates to the technical field of chemical engineering, more specifically to a method for reducing the content and granularity of metal ions in N-methylpyrrolidone. The method includes the following steps: methylamine and gamma-butyrolactone are added to a reactor, after reaction, the reaction system is introduced into a normal-pressure tower to remove water and methylamine, an obtained crude product enters a negative-pressure tower for removing low-boiling-point substances, then high-boiling-point substances are removed in a rectification tower, the processed crude product enters a storage tank, and then in turn passes through a primary filter, a secondary filter and a third filter after flowing out from the storage tank, and then filling is carried out by a dust-free filling line, so that ultrahigh-purity N-methylpyrrolidone is obtained. The invention provides the method for reducing the content and granularity of metal ions in N-methylpyrrolidone, and the purity of theobtained ultrahigh-purity N-methylpyrrolidone can reach 99.90% and more, and the particle content is less than or equal to 5 / mL when the particle size of impurity particles is greater than 0.5 [mu]m,and also a low-granularity product is obtained when the high purity is met.

Description

technical field [0001] The invention relates to the technical field of chemical industry, more specifically, the invention relates to a method for reducing metal ion content and particle size by N-methylpyrrolidone. Background technique [0002] Ultra-high-purity N-methylpyrrolidone (NMP) is a common solvent in the electronics industry. The quality of NMP products directly affects the production and quality of high-end electronic products. The large-scale production of electronic-grade N-methylpyrrolidone technology is mainly monopolized by developed countries such as the United States, Germany, and Japan. At present, the electronic-grade N-methylpyrrolidone used by electronic companies in my country mainly relies on imports. [0003] The existing patents CN102190611 and CN102001986A disclose that resin treatment and filtration are used, but the resin needs regeneration and material replacement. In industrial production, the industrial sewage treatment and material waste are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/267
CPCC07D207/267
Inventor 王焕婷刘宝顺赵金军刘洪河
Owner SHANDONG QINGYUN CHANGXIN CHEM SCI TECH
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