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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: 2008-07-02
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] Solid adsorbent silica gel 500g, micropore diameter is 30 Molecular sieve 300g, pore diameter at 10

[0018] Silica gel directly at 250°C, 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°C, and the activation time is 3h. After melting 100 parts of caprolactam, pass through the refining column into the polymerization kettle, add 0.04 parts of potassium hydroxide at a temperature of 130±5°C, and vacuum dehydrate for 3 minutes under a residual pressure of 0.30 MPa. After eliminating the vacuum with dry nitrogen, add 0.04 parts of 2,4 Or 2,6 toluene diisocyanate (TDI) and 2.0 parts of polypropylene oxide, heated up to 180°C, and reacted for 15 minutes to obtain nylon 6 resin with a relative viscosity of 3.6. Its performance test indicators are shown in Table 1.

Embodiment 2

[0020] Solid adsorbent silica gel 400g, pore diameter at 40 Activated alumina 300g, micropore diameter at 15

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

Embodiment 3

[0023] Solid adsorbent activated alumina 400g, micropore diameter at 20 Molecular sieve 300g, pore diameter at 10

[0024] Activated alumina washed 3 times at 270°C, 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°C, and the activation time is 3h. After melting 100 parts of caprolactam, pass through the refining column into the polymerization kettle, add 0.05 parts of potassium hydroxide at a temperature of 130±5°C, and vacuum dehydrate for 3 minutes under a residual pressure of 0.20 MPa. After the vacuum is eliminated with dry nitrogen, add 0.04 parts of 2,4 Or 2,6 toluene diisocyanate (TDI) and 1.5 parts of polypropylene oxide, heated up to 190°C, and reacted for 12 minutes to obtain a nylon 6 resin with a relative viscosity of 3.3. Its performance test indicators are shown in Table 1.

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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

field of invention [0001] The invention relates to a synthesis process of nylon 6, in particular to a dehydration process in the synthesis process of nylon. technical background [0002] The traditional process of using basic catalysts to synthesize nylon 6, such as the technology disclosed in US4131712, US4433146, and US5260246 patents, first adds caprolactam and basic catalysts to the melting tank according to a certain ratio, and raises the temperature of the system to 120-170 ° C. Carry out vacuum dehydration at 0.02-0.2MPa to make the water content of the system less than 300ppm, then add co-catalyst and compound additives, then add them to the polymerization kettle, raise the temperature to 200-220°C, and the system pressure is 0.02-0.5Mpa, and the system is opened Ring polymerization to obtain a nylon 6 product with a relative viscosity of 3.0 to 4.0. In this process, during the vacuum dehydration process of caprolactam at a temperature of 120-170 ° C and a pressure ...

Claims

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Application Information

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