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Melting direct-spinning method of copolymerized modified low-melting-point nylon fibers

A technology of copolymerization modification and nylon fiber, which is applied in the field of nylon materials, can solve the problems of low polymer number-average molecular weight, oligomer control, and slow reaction speed, and achieve the goals of lowering the melting point of nylon, ensuring quality, and increasing the devolatilization area Effect

Active Publication Date: 2020-06-19
ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to ensure that the polymerization process is carried out in a liquid state, the polymerization temperature must be at least 10°C higher than the melting point of nylon 6. At this time, the polymerization temperature still cannot control the oligomer in the range of direct spinning of the melt, and there is another disadvantage of low temperature polymerization , that is, the reaction speed is slow, and the number-average molecular weight of the polymer obtained is relatively low; while the polymerization process at a lower temperature is actually divided into two parts, one part is a melt polymerization process, and the other part is a solid phase polymerization process. The process of polymerization is to obtain polymers with sufficient number-average molecular weight for product development, but there is no effective way to turn solid polymers formed at low temperatures into suitable spinning methods. If fibers are spun from low-temperature polymers , the polymer must be melted first, however, at this time due to the existence of a chemical reaction balance, low molecular weight compounds are formed, so that there is no advantage compared with the normal polymerization method

Method used

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  • Melting direct-spinning method of copolymerized modified low-melting-point nylon fibers
  • Melting direct-spinning method of copolymerized modified low-melting-point nylon fibers
  • Melting direct-spinning method of copolymerized modified low-melting-point nylon fibers

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0075] The first step: at a temperature of 130°C, caprolactam, caprolactone, deionized water, HOOC (CH 2 ) 4 COOH, NH 2 (CH 2 ) 6 COOH was mixed in proportion; wherein relative to caprolactam, deionized water was added in an amount of 3wt%, HOOC(CH 2 ) 2 The amount of COOH added is 0.3wt%, NH 2 (CH 2 ) 4 The amount of COOH added is 0.03wt%, and the amount of caprolactone added is 30wt%;

[0076] The second step: After the mixture obtained in the first step is heated by the melt pump and the pre-heater, it is transported to the ring-opening kettle for ring-opening reaction. The polymerization temperature is controlled at 205 ° C, and the polymerization pressure is controlled at 1.3 MPa; the reaction time is The 0.6h prepolymer is transported to the top of the tower by a melt pump, mixed with fresh caprolactam, and the reflux rate is 1.5wt% of the caprolactam flow rate. When the following conditions are met, the reaction is terminated: the number average molecular weigh...

Embodiment 2

[0083] The first step: at a temperature of 90°C, caprolactam, -CO(CH 2 ) 2 CONH(CH 2 ) 4 NH-, deionized water, HOOC(CH 2 ) 3 COOH and nylon 66 salt were mixed in proportion; wherein relative to caprolactam, the amount of deionized water added was 1.2wt%, HOOC(CH 2 ) 3 The amount of COOH added is 0.15wt%, the amount of nylon 66 salt added is 0.07wt%, -COCONHCH 2 NH-added amount is 40wt%;

[0084] The second step: After the mixture obtained in the first step is heated by the melt pump and the pre-heater, it is transported to the ring-opening kettle for ring-opening reaction. The polymerization temperature is controlled at 240 ° C, and the polymerization pressure is controlled at 1.5 MPa; the reaction time is The 1.3h prepolymer is transported to the top of the tower by a melt pump, mixed with fresh caprolactam, and the reflux flow is 0.7wt% of the caprolactam flow. When the following conditions are met, the reaction is terminated: the number average molecular weight of t...

Embodiment 3

[0091] The first step: at a temperature of 130°C, caprolactam, NH 2 (CH 2 ) 10 COOH, deionized water, phthalic acid, NH 2 (CH 2 )5 COOH is mixed in proportion; among them, relative to caprolactam, the amount of deionized water added is 1.2wt%, the amount of phthalic acid added is 0.3wt%, and the amount of NH 2 (CH 2 ) 5 The amount of COOH added is 0.04wt%, NH 2 (CH 2 ) 10 The amount of COOH added is 50wt%;

[0092] The second step: After the mixture obtained in the first step is heated by the melt pump and the pre-heater, it is transported to the ring-opening kettle for ring-opening reaction. The polymerization temperature is controlled at 248 ° C, and the polymerization pressure is controlled at 0.6 MPa; the reaction time is The 1.2h prepolymer is transported to the top of the tower by a melt pump, mixed with fresh caprolactam, and the reflux flow is 0.8wt% of the caprolactam flow. When the following conditions are met, the reaction is terminated: the number average...

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Abstract

The present invention relates to the field of nylon materials, and discloses a melting direct-spinning method of copolymerized modified low-melting-point nylon fibers. The method comprises the steps of 1) material preparation, wherein caprolactam, a copolymerized modified component, an end-capping agent, water and a catalyst are heated and mixed; 2) ring opening, wherein a mixture is heated for ring opening; 3) pre-polycondensation, wherein a pre-polymerization reaction and devolatilization are performed; 4) final polycondensation, wherein a final polycondensation reaction and devolatilizationare performed; 5) devolatilization before spinning; and 6) spinning, wherein a product is directly conveyed to spinning threads for spinning to obtain the copolymerized modified low-melting-point nylon fibers. According to the method, the copolymerized modified component is added for destroying the regularity of nylon molecular chains and reducing the hydrogen bond density and crystallinity of the nylon molecular chains, thereby achieving the purpose of lowering the melting point of nylon; and according to different varieties and content of added copolymerized components, the melting point ofthe nylon can be controlled to be 90-200 DEG C, so that the application range of the low-melting-point nylon is greatly expanded.

Description

technical field [0001] The invention relates to the field of nylon materials, in particular to a melt direct spinning method of copolymerized modified low-melting-point nylon fibers. Background technique [0002] Low-melting-point nylon fibers can be used to make non-woven fabrics, and can also be used to develop various clothing, household items (such as window screens, mosquito nets, etc.), carpets, various bags, etc. Using low-melting point nylon fibers instead of artificial seams can not only reduce production The cost is reduced, the production efficiency is improved, and the hot-melt adhesive can be bonded to the fabric for a very long time, which improves the durability of the garment and makes the garment round and straight. [0003] There are two main methods for the preparation of low-melting nylon (PA): one is the blending method, that is, PA slices are mixed with functional powder, and extruded and granulated by a screw to obtain low-melting PA; the other is the ...

Claims

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Application Information

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IPC IPC(8): D01F6/80D01F6/90C08G69/44C08G69/16C08G69/46D01D5/08B01D1/22
CPCD01F6/80D01F6/90C08G69/44C08G69/16C08G69/46D01D5/08B01D1/22
Inventor 黄家鹏徐锦龙王松林汤廉何宁艳王华平王朝生
Owner ZHEJIANG HENGYI PETROCHEMICAL RES INST CO LTD
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