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Synthesis method of nylon 6

A synthesis method and nylon technology, applied in the field of dehydration technology, can solve problems such as increasing production cost, and achieve the effect of reducing production cost

Inactive Publication Date: 2005-05-25
SHANGHAI GENIUS ADVANCED MATERIAL (GRP) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this process, during the vacuum dehydration process of caprolactam at a temperature of 120-170 ° C and a pressure of 0.02-0.2 MPa, caprolactam crystals will be precipitated, and the monomer loss will be between 5% and 15%. It takes 20-60 minutes for vacuum dehydration, and the water content of the system can reach below 300ppm, which will inevitably increase the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The solid adsorbent silica gel is 500g, the pore diameter is 30 ; the molecular sieve is 300 g, the pore diameter is 10 .

[0018] Silica gel directly at 250℃, N 2 Flow rate 12ml / min, activation time 3h, molecular sieve washing 3 times, N 2 The flow rate is 6ml / min, the temperature is 200℃, and the activation time is 3h. After 100 parts of caprolactam is melted, pass through a refined column to the polymerization vessel, add 0.04 part of potassium hydroxide at a temperature of 130±5°C and a residual pressure of 0.30MPa for vacuum dehydration for 3 minutes. After removing the vacuum with dry nitrogen, add 0.04 part of 2,4 Or 2, 6 toluene diisocyanate (TDI) and 2.0 parts of polypropylene oxide, heated to 180° C., reacted for 15 minutes to obtain nylon 6 resin with a relative viscosity of 3.6. The performance test indicators are shown in Table 1.

Embodiment 2

[0020] The solid adsorbent silica gel is 400g, the pore diameter is 40 , the activated alumina is 300 g, the pore diameter is 15 .

[0021] Silica gel directly at 280℃, N 2 Flow rate 12ml / min, activation time 3h, activated alumina washing 3 times, N 2 The flow rate is 10ml / min, the temperature is 270℃, and the activation time is 3h. After 100 parts of caprolactam is melted, pass through a refined column to the polymerization kettle, add 0.04 part of sodium hydroxide at a temperature of 130±5°C and a residual pressure of 0.30MPa for vacuum dehydration for 4 minutes. After removing the vacuum with dry nitrogen, add 0.05 parts of 2,4 Or 2, 6 toluene diisocyanate (TDI) and 1.0 part of polypropylene oxide, heated to 170° C., reacted for 20 minutes to obtain nylon 6 resin with a relative viscosity of 3.5. The performance test indicators are shown in Table 1.

Embodiment 3

[0023] The solid adsorbent activated alumina is 400g, the pore diameter is 20 , the molecular sieve is 300 g, the pore diameter is 10 .

[0024] Activated alumina was washed 3 times at 270℃, N 2 Flow rate 9ml / min, activation time 3h, molecular sieve washing 3 times, N 2 The flow rate is 6ml / min, the temperature is 200℃, and the activation time is 3h. After 100 parts of caprolactam is melted, pass through a refined column to the polymerization vessel, add 0.05 part of potassium hydroxide at a temperature of 130±5°C and a residual pressure of 0.20MPa for vacuum dehydration for 3 minutes. After removing the vacuum with dry nitrogen, add 0.04 parts of 2,4 Or 2,6 toluene diisocyanate (TDI) and 1.5 parts of polypropylene oxide, heated to 190°C, reacted for 12 minutes to obtain a nylon 6 resin with a relative viscosity of 3.3. The performance test indicators are shown in Table 1.

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PUM

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Abstract

A process for synthesizing nylon-6, especially the MC nylon, features that the solid adsorbent is used to refine the fused hexanolactam to prevent the hexanolactam from being educed out in vacuum dewatering. Its advantages are short reaction time, less energy consumption and no pollution.

Description

Invention field [0001] The invention relates to a synthetic process of nylon 6, in particular to a dehydration process in the synthetic process of nylon. technical background [0002] The traditional process for synthesizing nylon 6 with alkaline catalysts, such as those disclosed in US4131712, US4433146, and US5260246 patents, first add caprolactam and alkaline catalysts to the melting kettle in a certain proportion, heat the system to 120-170°C, and then Perform vacuum dehydration at 0.02~0.2MPa to make the water content of the system less than 300ppm, add the co-catalyst and composite additives, and then add them to the polymerization kettle, raise the temperature to 200~220℃, the system pressure is 0.02~0.5Mpa, and the system is opened Through ring polymerization, nylon 6 products with a relative viscosity of 3.0 to 4.0 are obtained. In this process, caprolactam crystals will precipitate during vacuum dehydration at a temperature of 120 to 170°C and a pressure of 0.02 to 0.2 ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/16
Inventor 杨桂生司林旭刘玉
Owner SHANGHAI GENIUS ADVANCED MATERIAL (GRP) CO LTD