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Preparation method of high-hydrophilicity polyamide 6 and high-hydrophilicity polyamide 6 fiber

A polyamide and hydrophilic technology, which is applied in the field of preparation of functional polymers, can solve the problems of high price of irradiation γ-ray sources, difficulty in industrial production, difficulty in ensuring uniformity, etc., to achieve suitable industrial production, easy operation and realization , the effect of simple preparation method

Active Publication Date: 2022-02-11
WUHAN TEXTILE UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN103361977A planted salicylaldehyde and quaternary ammonium salt functional groups on the surface of polyamide materials "lattice" to improve the hydrophilicity and antibacterial properties of the material surface. This modification is limited to the surface of the material and cannot be used inside the material. modified
The irradiation grafting method can conveniently graft hydrophilic monomers onto fibers, but the irradiation gamma ray source is expensive, and the uniformity is difficult to guarantee and it is not easy to industrialize production

Method used

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  • Preparation method of high-hydrophilicity polyamide 6 and high-hydrophilicity polyamide 6 fiber
  • Preparation method of high-hydrophilicity polyamide 6 and high-hydrophilicity polyamide 6 fiber
  • Preparation method of high-hydrophilicity polyamide 6 and high-hydrophilicity polyamide 6 fiber

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preparation example Construction

[0032] A kind of preparation method of highly hydrophilic polyamide 6 provided by the invention comprises the following steps:

[0033] S1. Preparation of dicarboxyimidazole quaternary ammonium salt

[0034] N-(trimethylsilyl) imidazole is reacted with ethyl chloroacetate to obtain imidazole quaternary ammonium salt substituted by ethyl diacetate; then ethyl acetate is hydrolyzed to obtain dicarboxy imidazole quaternary ammonium salt; wherein, the hydrolysis is acidic Conditional hydrolysis, the hydrolysis reaction time is 6-15h. The acid used for hydrolysis is preferably hydrochloric acid.

[0035] The reaction temperature of N-(trimethylsilyl)imidazole and ethyl chloroacetate is 50-80°C, the time is 12-30h, and the reaction atmosphere is nitrogen atmosphere.

[0036]

[0037] S2. Preparation of caprolactam prepolymer

[0038] Ring-opening polymerization of caprolactam, and then adding hexamethylenediamine to obtain a caprolactam prepolymer with amino groups at both end...

Embodiment 1-6

[0047] A preparation method for highly hydrophilic polyamide 6, comprising the following steps:

[0048] 1. Synthesis of dicarboxyimidazole quaternary ammonium salt

[0049] Under a nitrogen atmosphere, ethyl chloroacetate was added to N-(trimethylsilyl)imidazole, and reacted at 60° C. for 24 hours to obtain a solid crude product. Afterwards, the crude product was cooled to room temperature, dissolved in a small amount of water, and extracted three times with ethyl acetate to remove unreacted monomers. Then, an appropriate amount of hydrochloric acid aqueous solution was added to the water phase for hydrolysis, and stirred at room temperature for 12 hours. Hydrogen chloride and solvent were removed by rotary evaporation to obtain a solid product with a yield of 93%.

[0050] see figure 1 Shown, can explain the successful synthesis of dicarboxyimidazole quaternary ammonium salt.

[0051] 2. Synthesis of Caprolactam Prepolymer

[0052] Set up the reaction device, first pass...

Embodiment 7-8

[0061] A method for preparing highly hydrophilic polyamide 6. Compared with Example 3, the difference is that the amount of hexamethylenediamine added in Step 2 is changed, and the others are roughly the same as Example 3, and will not be repeated here.

[0062] Preparation conditions and performance test results of table 2 embodiment 3 and embodiment 7-8

[0063]

[0064] It can be seen from Table 2 that with the increase of the addition of hexamethylenediamine, the water contact angle and fiber moisture regain of the hydrophilic polyamide 6 do not change much, indicating that the addition of hexamethylenediamine has little effect on the hydrophilicity of the fiber ; But too much addition of hexamethylenediamine increases the number of short-chain molecular weights in polyamide 6, resulting in a decrease in breaking strength.

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Abstract

The invention provides a preparation method of high-hydrophilicity polyamide 6 and high-hydrophilicity polyamide 6 fiber. The preparation method comprises the following steps: reacting N-(trimethylsilyl) imidazole with ethyl chloroacetate to obtain bis(ethyl acetate) substituted imidazole quaternary ammonium salt; then hydrolyzing the bis(ethyl acetate) groups to obtain dicarboxyl imidazole quaternary ammonium salt; carrying out ring opening polymerization on caprolactam, and then adding hexamethylenediamine for blocking to prepare a caprolactam prepolymer with amino groups at two ends; and finally, adding the dicarboxyl imidazole quaternary ammonium salt, and carrying out copolyamidation reaction of amino and carboxyl to obtain the high-hydrophilicity polyamide 6. According to the invention, a dicarboxyl imidazole biquaternary ammonium salt chain segment is introduced into a polyamide 6 main chain, and the content of the dicarboxyl imidazole biquaternary ammonium salt chain segment is regulated, so that the molecular chain composition of the obtained copolyamide is regulated, the hydrophilicity and processability of the polyamide are regulated, and the novel polyamide 6 which has excellent comprehensive performance and is suitable for spinning is prepared. The prepared nylon 6 fiber has high hydrophilicity and high strength.

Description

technical field [0001] The invention relates to the technical field of preparation of functional polymers, in particular to a preparation method of highly hydrophilic polyamide 6 and highly hydrophilic polyamide 6 fibers. Background technique [0002] The progress of society has greatly improved people's living standards, and people's clothing functions are no longer limited to keeping warm and cold, but also require comfortable wearing, moisture absorption and perspiration, and antibacterial and antibacterial functions. This requires fiber fabrics to have some additional functions. Polyamide, commonly known as nylon, is a widely used polymer material. Among them, nylon 6 is more widely used due to its price advantage, and it has a large share in civil textiles. However, the high crystallinity of nylon 6 reduces its hydrophilicity and water absorption, and its moisture absorption and perspiration effect is poor, which greatly limits the comprehensive application of nylon 6...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/26C08G69/28C08G69/14D01F6/80
CPCC08G69/26C08G69/28C08G69/14D01F6/80
Inventor 王栋白婷王雯雯付从昂夏明易礼婷张吉聪李晓光沈红燕
Owner WUHAN TEXTILE UNIV
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