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Method for reducing content of hydrolyzed chlorine in isocyanate

A technology of isocyanate and chlorine content, which is applied in the field of isocyanate, can solve the problems of cumbersome operation in the activation process, and achieve the effect of simple method, safe operation, and reduction of hydrolyzed chlorine content

Active Publication Date: 2022-04-12
LIMING RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method of preparing adsorbent needs to synthesize a specific adsorbent, and the activation process is cumbersome.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 50.01g of 2,4-TDI (hydrolyzed chlorine 0.150wt%) to a 250ml four-neck flask equipped with mechanical stirring, thermometer, reflux tube, nitrogen inlet, and air bag, add 50g of acetonitrile, stir to dissolve, and add tetrabutyl bromide Ammonium chloride 0.20g, sodium azide 0.55g, heat up to 80°C and react for 4 hours, cool down to room temperature, add 0.50g of magnesium silicate and stir for 30 minutes, filter to remove the solid, distill off acetonitrile under reduced pressure to obtain 49.3g of transparent liquid , yield 98.6%, hydrolyzed chlorine 0.0090wt%.

Embodiment 2

[0030] Add 40.20g of butyl isocyanate (hydrolyzed chlorine 1.833wt%) to a 250ml four-neck flask equipped with mechanical stirring, thermometer, reflux tube, nitrogen inlet, and air bag, add 120.41g of acetonitrile, stir to dissolve, add tetrabutyl bromide Ammonium 3.30g, sodium azide 8.10g, heated up to 25°C and reacted for 8 hours, cooled down to room temperature, added 0.40g of magnesium silicate and stirred for 30 minutes, filtered to remove the solid, and distilled off acetonitrile under reduced pressure to obtain 39.42g of transparent liquid, Yield 98.1%, hydrolyzed chlorine 0.0094wt%.

Embodiment 3

[0032] Add 50.15g of CHDI (hydrolyzed chlorine 0.120wt%), 150.05g of ethylene glycol dimethyl ether, stir to dissolve, and add tetrabutyl Ammonium bromide 0.16g, sodium azide 0.44g, heat up to 60°C and react for 6 hours, cool down to room temperature, add 0.50g of magnesium silicate and stir for 30 minutes, filter to remove solids, distill ethylene glycol dimethyl under reduced pressure Ether, 49.2g of transparent liquid was obtained, the yield was 98.1%, and the hydrolyzed chlorine was 0.0089wt%.

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PUM

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Abstract

The invention relates to a method for reducing the content of hydrolyzed chlorine in isocyanate, which comprises the following steps: (1) dissolving isocyanate with high hydrolyzed chlorine in a solvent, and adding an azidation reagent; (2) raising the temperature and reacting for a period of time; (3) cooling, adding an adsorbent, stirring, and filtering; and (4) performing reduced pressure distillation on the filtrate to obtain the product. According to the method, acyl chloride impurities in isocyanate are converted into isocyanate through a simple operation process, generated chloride is separated out, the method for reducing the content of hydrolyzed chlorine in isocyanate is provided, and the method has the advantages that operation is safe, the method is simple, and industrial production is easy.

Description

technical field [0001] The invention relates to the field of isocyanate, in particular to a method for reducing the content of hydrolyzed chlorine in isocyanate. Background technique [0002] Isocyanate is one of the important raw materials for the preparation of polyurethane materials, and is widely used in various elastomers, foam plastics, synthetic fibers, synthetic leather, coatings, thermal insulation materials, waterproof materials, shoemaking and other fields. Hydrolyzed chlorine content is an important indicator of isocyanate products. Hydrolyzed chlorine refers to the hydrolyzable chlorine atoms (including bromine atoms) present in isocyanate products, which are introduced by various chlorine-containing by-products. [0003] Excessive hydrolyzed chlorine content will not only deepen the color of the product, but also adversely affect the process of polyurethane production and the overall quality control of the product. In some application fields, these chlorine-c...

Claims

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Application Information

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IPC IPC(8): C07C263/20C07C265/14C07C265/04
Inventor 池俊杰邢校辉谢洪涛贾利亚李文江王建伟
Owner LIMING RES INST OF CHEM IND
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