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Anion slurry polymerization method for preparing caprolactam homopolymer and copolymer

A technology of caprolactam and acid chloride, which is applied in the field of anionic slurry polymerization for the preparation of caprolactam homopolymers and copolymers, and can solve the problems of difficulty in stable control of the molecular weight of reaction products, residues, and limited secondary forming and processing of slices.

Inactive Publication Date: 2007-08-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the anionic polymerization of caprolactam developed at home and abroad mainly includes monomer casting nylon (MC nylon) and reactive extrusion (RIM) technology, but the mature monomer casting technology (MC nylon) is only suitable for processing large castings and other materials, and cannot Formed into conventional thermoplastic resin chips for flexible processing, inflexible applications
Reactive extrusion (RIM) technology is a technology that tries to combine the advantages of low temperature and high speed of anionic polymerization with the flexible processing advantages of thermoplastic chips. However, this method has two shortcomings: first, because the anionic polymerization reaction is very violent, the reaction The molecular weight of the product is difficult to control stably; secondly, because the reaction is an active polymerization, after the reaction is terminated, the active center still remains in the product slice, and when the secondary forming process is heated, the active center will cause the molecules to produce branched chains and crosslinks, which will not Facilitate normal processing
The reactive extrusion method has no effective active center passivation measures, which limits the secondary forming process of making slices

Method used

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  • Anion slurry polymerization method for preparing caprolactam homopolymer and copolymer
  • Anion slurry polymerization method for preparing caprolactam homopolymer and copolymer
  • Anion slurry polymerization method for preparing caprolactam homopolymer and copolymer

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preparation example Construction

[0010] The preparation method of the present invention is specifically described below.

[0011] Homopolymerization of caprolactam

[0012] Put the caprolactam monomer into the reactor and heat it to a temperature of 70-120°C, vacuumize to remove the trace moisture absorbed by the monomer until the moisture content is lower than 0.02wt%, and then add 1.0×10 based on the weight of the monomer -3 -8.0×10 -3 % of alkali or alkali metal catalyst, continue vacuuming at 90-120°C, remove the water generated by the reaction until the moisture content is lower than 0.015wt%, and add 1.2-4.8mol% acid chloride, lattice co-catalysts such as Nicholas' reagent or isocyanate, and at the same time add an inert aliphatic hydrocarbon dispersant in an amount of 4-30 wt% of the monomer weight. Heating under stirring until the temperature reaches 140-160°C, the reaction system changes from clear and transparent to turbid, and a large amount of granular polymers are produced within 10-20 minutes....

Embodiment 1

[0033] Embodiment 1: the synthesis of nylon 6 homopolymer

[0034] Add 10kg of caprolactam monomer to a 50-liter reactor, heat to a temperature of 70-120°C, vacuumize to remove the trace moisture absorbed by the monomer until the moisture content is lower than 0.02wt%, and add 0.2×10 -2 The sodium hydroxide catalyst of wt%, continues to vacuumize at 90-120 ℃, gets rid of the water that reaction generates to moisture content and is lower than 0.015wt%, adds the cocatalyst toluene diisocyanate of 1.63mol% and 2.5 liters of dispersant kerosene ( Industrial pure, boiling point range 160-220°C). After reacting at 155°C for 30 minutes, nylon 6 slurry with a monomer conversion rate of 45% was obtained. At this reaction temperature, acetic acid (1.0 wt% based on the amount of caprolactam) with pKa=4.74 was added, and stirred for 20 minutes to remove residual catalyst and residual The active center is passivated, then discharged, filtered, washed, and dried to obtain dry powder PA6. A...

Embodiment 2

[0035] Embodiment 2: Preparation of low melting point hot melt adhesive

[0036] Add 10kg of caprolactam monomer into a 50-liter reactor, heat to a temperature of 70-120°C, vacuumize to remove the trace moisture absorbed by the monomer until the moisture content is lower than 0.02wt%, and add 0.2×10 -2 Wt% sodium hydroxide catalyst, continue vacuuming at 90-120°C for 30 minutes, remove the water generated by the reaction until the moisture content is lower than 0.015wt%, add 2.0mol% co-catalyst toluene diisocyanate, and add a molecular weight of 1000 PEG (6% of the weight of caprolactam), add 2.5 liters of dispersant kerosene (industrial pure, boiling point range 180-220°C) under stirring, heat up to 115-170°C and stir for 20-30 minutes to obtain a single PA6 / PEG copolymer slurry with a volume conversion rate of 40-45%. After discharge, it is filtered, washed, and dried to obtain a powdery PA6 / PEG copolymer. After testing, its melting point is 120°C and its molecular weight is...

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Abstract

The invention relates to a method for preparing aminocaprolactam homopolymer and copolymer. It takes aminocaprolactam as monomer, takes aliphatic hydrocarbon as dispersing agent, takes alkali or base metal as catalyst, takes acyl chloride, format agent or isocyanate as catalyst promoter to carry out slurry polymerization process for anion and copolymerization with polyether, and gets powder nylon 6 homopolymer and copolymer low-melting point thermosol at low temperature below 160 Deg. C and in a short time. The invention is characterized in that it possesses feature of easy controllable stability for molecular weight and liner molecular construction, it is easy to ass residual catalyst deactivator to make product possess good property for spinning and second-time shaping at the end of reaction or after reaction.

Description

field of invention [0001] The present invention relates to a method for preparing caprolactam homopolymer and copolymer by anionic slurry polymerization technique, the obtained caprolactam homopolymer and copolymer and the use thereof. Background of the invention [0002] At present, the synthesis of polycaprolactam (nylon 6) mainly includes the hydrolytic ring-opening polymerization technology of caprolactam and the anionic polymerization technology represented by monomer casting (MC nylon) and reactive extrusion (RIM). [0003] The hydrolysis ring-opening technology uses caprolactam as the monomer and a small amount of water as the ring-opening agent to carry out the polymerization reaction in the VK polymerization tube at 250-280°C for 20-28 hours. The reaction temperature is relatively high and the time is relatively long. Since this technology is an equilibrium reversible reaction, the product always contains 3-10% monomers and oligomers, so hot water extraction is requ...

Claims

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Application Information

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IPC IPC(8): C08G69/14C08G69/18
Inventor 李小宁赵莉杨中开
Owner CHINA PETROLEUM & CHEM CORP
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