Synthetic process of poly-alpha-pyrrolidone based on anion open loop polymerization

A polybutyrolactam and anion ring-opening technology, applied in the field of nylon synthesis technology, can solve the problems of low reaction speed, complicated procedures, difficult to use on a large scale, and achieve the effects of simplifying production technology and equipment and reducing production costs.

Inactive Publication Date: 2018-05-18
CHTC BIO BASED MATERIAL ENG & TECH NINGBO CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In summary, the synthesis of polybutyrolactam in the prior art has the following defects: complex procedure, high cost, low reaction s

Method used

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  • Synthetic process of poly-alpha-pyrrolidone based on anion open loop polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] A kind of anionic ring-opening polymerization method synthesizes polybutyrolactam, and its steps are as follows:

[0034] Step 1. Reaction container handling

[0035] Add 200g of butyrolactam into a four-necked flask, said four-necked flask: the specification is 500ml, and it has been deoxygenated and dried; the four-necked flask is respectively connected with nitrogen, mechanical stirring paddle, temperature sensor and vent;

[0036] The deoxygenation and drying: the four-neck flask is dried in an oven, and the flask is ventilated with nitrogen at room temperature for 15 minutes to ensure that the air is removed, and the nitrogen flux is kept at 500ml / min.

[0037] Step 2, Nitrogen

[0038] The four-neck flask was heated to 110°C under nitrogen, and the nitrogen flux was kept at 500 ml / min.

[0039] Step 3. Activation

[0040] Add 13.33g of potassium tert-butoxide solid into the four-neck flask, stir to dissolve, set the rotation speed at 200r / min, activate for 3h, ...

Embodiment 2

[0049] A kind of anionic ring-opening polymerization method synthesizes polybutyrolactam, and step is as follows:

[0050] Step 1. Reaction container handling

[0051] Add 200g of butyrolactam into a four-necked flask, said four-necked flask: the specification is 500ml, and it has been deoxygenated and dried; the four-necked flask is respectively connected with nitrogen, mechanical stirring paddle, temperature sensor and vent;

[0052] The deoxygenation and drying: the four-neck flask is dried in an oven, and the flask is ventilated with nitrogen at room temperature for 15 minutes to ensure that the air is removed, and the nitrogen flux is kept at 500ml / min.

[0053] Step 2, Nitrogen

[0054] The four-neck flask was heated to 120 °C under nitrogen, and the nitrogen flux was kept at 500 ml / min.

[0055] Step 3. Activation

[0056] Add 9.5-10 g of potassium tert-butoxide solid into the four-neck flask, stir to dissolve, set the rotation speed at 300 r / min, activate for 6 hour...

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Abstract

The invention provides a synthetic process of poly-alpha-pyrrolidone based on anion open loop polymerization, which is characterized in that the mass ratio of butyrolactam, potassium tert-butoxide andbenzoyl chloride applied in the synthetic process is 15-20: 0.9-0.14: 0.7-3-0.99. The synthetic process includes processing of a reaction container, nitrogen filling, activation, polymerization, andpreparation of a finished production; the molecular weight of the prepared poly-alpha-pyrrolidone is 15000-20000, the product yield is 60-90%.

Description

technical field [0001] The invention relates to a nylon synthesis process, in particular to a direct polymerization process of polybutyrolactam (nylon 4) based on an anionic ring-opening mechanism. Background technique [0002] Polybutyrolactam 4 (PA4, commonly known as nylon 4) is a polyamide with 4 carbon atoms in its structural unit. According to its molecular weight and structure, its melting point is 260~270°C. Its toughness, elongation at break, elastic recovery and moisture absorption Properties such as resistance are similar to or even better than cotton and other polyamides. Nylon 4 has a high density of amide bonds in its molecular chain structure, so it has a very similar hydrophilicity to cotton and silk, and can be used as a drawing fiber. The research on its fiber products has long been valued. In general, polyamide products, such as nylon 6 and nylon 66, cannot be degraded in the natural environment, but nylon 4 has excellent biodegradability, and has potenti...

Claims

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Application Information

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IPC IPC(8): C08G69/18C08G69/14
CPCC08G69/14C08G69/18C08G2230/00
Inventor 赵一甲王乐军刘怡宁赵鹏飞
Owner CHTC BIO BASED MATERIAL ENG & TECH NINGBO CO LTD
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