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Method for preparing polybutyrolactam through anionic ring-opening slurry polymerization

A polybutyrolactam and anion ring-opening technology, which is applied in the field of nylon synthesis technology, can solve problems such as detonation and uneven heat transfer, and achieve the effects of simple post-processing, easy process control, and cost reduction

Active Publication Date: 2020-11-13
TIANE CHEM FIBER GROUP CORP BAODING +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] (2) Solve the problems of implosion and uneven heat transfer in the polymerization process;

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Embodiment 1 A kind of anionic ring-opening slurry polymerization prepares the method for polybutyrolactam

[0046] Specific steps are as follows:

[0047] (1) Alkali preactivated monomer

[0048] Add 100g of 2-pyrrolidone into a 250ml three-necked flask filled with an inert protective gas, add 8g of sodium ethoxide under the protection of an inert gas, and incubate at 80°C for 1 hour to obtain an activation solution.

[0049] (2) Acylation catalyst pre-acylation monomer

[0050] Under the protection of an inert gas environment, 90 g of 2-pyrrolidone was added, and 0.54 g of an acylation catalyst was added under the protection of an inert gas, and stirred for 1.5 hours.

[0051] The acylation catalyst is benzoyl chloride.

[0052] (3) Pre-mixing of dispersing solvent and activation solution

[0053] Cool the activation solution to 40°C, add 120 g of dispersing solvent to the activation solution under the protection of inert gas, stir at a speed of 100 r / min, and con...

Embodiment 2

[0058] Embodiment 2 A kind of anionic ring-opening slurry polymerization prepares the method for polybutyrolactam

[0059] Proceed as follows:

[0060] (1) Alkali preactivated monomer

[0061] Add 100g of 2-pyrrolidone into a 250ml three-necked flask filled with inert protective gas, add 10g of potassium tert-butoxide, and keep warm at 90°C for 1.5h to obtain an activation solution.

[0062] (2) Acylation catalyst pre-acylation monomer

[0063] Take another reaction flask, put 40g of 2-pyrrolidone into 0.8g acylation catalyst under inert gas protection environment, and stir for 2 hours.

[0064] The acylation catalyst is benzoyl chloride.

[0065] (3) Pre-mixing of dispersing solvent and activation solution

[0066] Cool the activation solution to 35°C, and add 100 g of dispersing solvent after removing impurities and water to the activation solution under the protection of an inert gas, with the stirring speed at 150 r / min, and continue to mix in an airtight manner for 1 ...

Embodiment 3

[0072] On the basis of Example 1, change the acylation catalyst of step (2) to terephthaloyl chloride, and the addition amount is 0.39g; the dispersive solvent of step (3) is heptane, and the sealing reaction time of step (4) is 12h, all the other methods are the same as embodiment 1, the polymer polybutyrolactam of preparation, Ubbelohde viscometer test molecular weight is about 38000, and GPC molecular weight distribution P value is 1.83; Yield is 90.2%, and the initial thermal decomposition temperature of product is 280 ℃; the tensile strength reaches 57Mpa.

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Abstract

The invention provides a method for preparing polybutyrolactam through anionic ring-opening slurry polymerization. The method comprises the following steps: pre-activation of monomer with alkali, pre-acylation of the monomer with an acylation catalyst, premixing of a dispersive solvent and an activation solution, and multi-component polymerization. The molecular weight of nylon 4 prepared by the invention is 30000 or above; the polybutyrolactam prepared by using the method has yield of 80 to 95%; and according to the preparation method disclosed by the invention, polymerization reaction time is 8-72 hours, preferably, 8-48 hours. Materials cannot be caked, so the problem of implosion in the process of polymerization is solved.

Description

technical field [0001] The invention belongs to a nylon synthesis process, in particular to a polymerization process for preparing polybutyrolactam (nylon 4) based on an anion ring-opening mechanism. Background technique [0002] As the first of the five major engineering plastics, polyamide (PA) has the advantages of good mechanical properties, wear resistance and corrosion resistance, and has a wide range of applications. Polybutyrolactam 4 (PA4, commonly known as nylon 4) is a polyamide with 4 carbon atoms in its structural unit. It has good wear resistance, corrosion resistance, fatigue resistance and outstanding dyeing performance. It has the highest hydrophilicity among resin-like resins and is currently the only degradable nylon. [0003] Due to the difficulty of ring-opening of butyrolactam, the early synthesis methods of nylon 4 were almost all anionic ring-opening polymerization, and considering the simplicity of the process, most of them were bulk polymerization....

Claims

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Application Information

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IPC IPC(8): C08G69/18C08G69/16C08G69/20C08G69/24
CPCC08G69/18C08G69/16C08G69/20C08G69/24
Inventor 赵黎明赵鹏飞吴德王乐军王东兴刘佳陈涛宋亚男
Owner TIANE CHEM FIBER GROUP CORP BAODING
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