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A kind of preparation method of temperature regulation fiber

A temperature-regulating, fiber technology, applied in the field of temperature-regulating fiber preparation, can solve the problem of long, usually 2 to 48 hours, or even up to 120 hours, limiting the application and development of functional fibers, temperature-regulating fibers, and spinneret pressure resistance. problems such as stability and drafting effects, to achieve the effects of excellent temperature adjustment function, shortened dissolution time, and easy industrial production.

Active Publication Date: 2020-12-08
龙丝(上海)新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Studies have found that ionic liquids can directly dissolve cellulose. Chinese patents such as CN 200610078784.5, CN200680012598.X, CN200710085298.0, and CN201310158819.6 have disclosed methods for dissolving cellulose with ionic liquids. At present, there are also methods of using ionic liquids to connect fibers Related reports on the preparation of functional composite fibers from cellulose and other functional substances, for example, Chinese patent CN200510077288.3 discloses a method of using ionic liquid as a solvent to mix and dissolve animal hair and cellulose raw materials to prepare biological protein wool fibers; Chinese patent CN201510313099.5 discloses A method for preparing keratin composite fibers by dissolving keratin and cellulose using ionic liquid as a solvent; however, there is no relevant report about using ionic liquid to dissolve cellulose and phase change energy storage materials to prepare temperature-regulating fibers
Moreover, when using ionic liquids (alkyl quaternary ammonium salts, alkyl imidazolium salts, alkyl pyrrole salts, etc.) The obtained spinning dope has a high viscosity and poor spinnability, which has a great influence on the pressure resistance and draft of the spinneret in the subsequent spinning process, which is not conducive to the subsequent spinning; in addition, the ionic liquid is When dissolving cellulose, the dissolution time is longer, usually 2 to 48 hours, or even as high as 120 hours; and the dissolution temperature is relatively high, usually around 100 ° C, or even as high as 150 ° C, and the energy consumption is high; The use of ionic liquids to prepare functional fibers is still in the laboratory stage and cannot be realized on an industrial scale, which severely limits the application and development of functional fibers (including temperature-regulating fibers).

Method used

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  • A kind of preparation method of temperature regulation fiber
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  • A kind of preparation method of temperature regulation fiber

Examples

Experimental program
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Effect test

Embodiment 1

[0046]1. Preparation of 1,4-bis[1-(3-methylimidazole)]butyl dichloride salt:

[0047]Under the protection of nitrogen and at 80°C, 1.2mol of N-methylimidazole was slowly added dropwise to 1mol of 1,4-dichlorobutane. After the dropping was completed, the reaction was refluxed for 72 hours to complete the reaction. The reaction solution was cooled to room temperature. The product was washed with ether to remove unreacted raw materials, and a white solid material was obtained, namely, 1,4-bis[1-(3-methylimidazole)]butyl dichloride (HPLC purity 98.8%, yield 88 %).

[0048]2. Preparation of 1,4-bis[1-(3-methylimidazole)]butyl diperchlorate:

[0049]Dissolve 1 mol of 1,4-bis[1-(3-methylimidazole)] butyl dichloride and 1.2 mol of lithium perchlorate in 1L of water, then stir the reaction at 80°C for 36 hours, and cool to room temperature. Continue stirring at room temperature for 12 hours. Disperse the reaction solution into an equal volume of chloroform and separate. The chloroform phase is washed...

Embodiment 2

[0066]The difference between this example and Example 1 is only: 0.5 parts by mass of silica, 1.5 parts by mass of paraffin phase change microcapsules and 8.5 parts by mass of cotton pulp (cellulose content is 99%, degree of polymerization is 600) are mixed After being uniform, add 100 parts by mass and 80 wt% of the ionic liquid aqueous solution, and the rest of the contents are the same as those described in Example 1.

[0067]After testing, the temperature-regulating fiber prepared in this example has a breaking strength of about 2.6 cN / dtex when the monofilament fineness is 6.6 dtex; and the experiment shows that under the same conditions, 80wt% of 1-butane 3-methylimidazole chloride salt, 1,4-bis[1-(3-methylimidazole)]butyl dichloride salt or 1,4-bis[1-(3-methylimidazole)]butyl When dissolving phase change paraffin microcapsules and cotton pulp in a single ionic liquid aqueous solution based on diperchlorate, it needs to be stirred at 110~130℃ for 3~5 hours to obtain a stable and ...

Embodiment 3

[0069]This embodiment is different from Example 1 only in that: 0.5 parts by mass of silica, 2.8 parts by mass of paraffin phase change microcapsules and 7.2 parts by mass of cotton pulp (cellulose content is 99%, degree of polymerization is 600) are mixed After being uniform, add 100 parts by mass and 80 wt% of the ionic liquid aqueous solution, and the rest of the contents are the same as those described in Example 1.

[0070] After testing, the temperature-regulating fiber prepared in this example has a breaking strength of about 2.8 cN / dtex when the monofilament fineness is 6.6 dtex; and the experiment shows that under the same conditions, 80wt% of 1-butane 3-methylimidazole chloride salt, 1,4-bis[1-(3-methylimidazole)]butyl dichloride salt or 1,4-bis[1-(3-methylimidazole)]butyl When dissolving phase change paraffin microcapsules and cotton pulp in a single ionic liquid aqueous solution based on diperchlorate, it needs to be stirred at 110~130℃ for 3~5 hours to obtain a stable and ...

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Abstract

The invention discloses a preparation method of temperature regulating fibers. The preparation method comprises the following steps: (a) mixing a dispersing agent, a phase change energy storage material and cellulose, and then dissolving the mixture into an aqueous solution of ionic liquid to prepare a mixed spinning dope; (b) filtering the obtained mixed spinning dope, spinning, solidifying, stretching, washing, bleaching, oiling, and drying to obtain the temperature regulating fibers; the ionic liquid is obtained by mixing 1-butyl-3-methylimidazolium chloride with bi-1,4-bis[1-(3-methylimidazole)]butyl dichloride and bi-1,4-bis[1-(3-methylimidazolyl)]butyl diperchlorate. Experiments show that the temperature regulating fibers prepared by the method have excellent mechanical properties, temperature regulation performance and stability performance, are simple in preparation process and low in cost, do no need any organic solvent, are environmentally friendly and free from pollution, donot require special equipment and harsh conditions, and are easy to realize industrial production, thus having a very high practical value.

Description

Technical field[0001]The invention relates to a method for preparing temperature-regulating fibers, and belongs to the technical field of functional cellulose fibers.Background technique[0002]Cellulose is the most widely distributed and most abundant polysaccharide in nature, accounting for more than 50% of the carbon content in the plant kingdom, and is one of the most abundant natural organic matter in nature. Cellulose is mainly derived from plants, such as cotton, wood, cotton linters, wheat straw, rice straw, reeds, hemp, mulberry, etc. The cellulose content of cotton is close to 100%, which is the purest natural source of cellulose, while general wood Among them, cellulose accounts for 40-50%, there are 10-30% hemicellulose and 20-30% lignin. As a degradable green biological material, natural fiber is gradually playing an increasingly important role with its superior properties such as light weight, degradability, low price, high modulus, and high strength. Therefore, obtainin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F2/02D01F1/10D01D5/06
CPCD01D5/06D01F1/10D01F2/02
Inventor 俞啸华郭建雄
Owner 龙丝(上海)新材料科技有限公司