阅读说明：本技术 一种板蓝根提取物改性涤纶纤维及其制备方法 (Radix isatidis extract modified polyester fiber and preparation method thereof ) 是由 黄效华 郑天勇 姜义军 甄丽 黄效龙 王丙伟 姜亚明 刘宇 于 2020-07-02 设计创作，主要内容包括：本发明涉及一种板蓝根提取物改性涤纶纤维及其制备方法,所述的改性涤纶纤维包括板蓝根提取物、白芍提取物、吡咯烷酮羧酸钠、三聚氰胺磷酸盐和三乙胺。本发明中将板蓝根提取物和白芍提取物与多孔纳米材料和亲水剂进行改性处理,由于纳米多孔材料具有较大的比表面积,将植物提取物“封装”在多孔材料孔道内,不会破坏植物提取物的成分,从而提高涤纶短纤的性能和亲水力,本发明加入板蓝根提取物提高了涤纶短纤的抗菌性能,加入白芍提取物和吡咯烷酮羧酸钠能够有效避免涤纶起球的问题,加入三聚氰胺磷酸盐和三乙胺能够有效提高涤纶的抗熔性能；本发明所述制备方法可以提高涤纶短纤的机械性能、透气性、吸湿性和抗熔性,还能够有效防止涤纶纤维起球。(The invention relates to radix isatidis extract modified polyester fiber and a preparation method thereof. According to the invention, the isatis root extract and the white peony root extract are modified with the porous nano material and the hydrophilic agent, and the nano porous material has a larger specific surface area, so that the plant extract is 'packaged' in a porous material pore channel, and the components of the plant extract cannot be damaged, thereby improving the performance and hydrophilicity of the polyester staple fiber; the preparation method can improve the mechanical property, air permeability, moisture absorption and melt resistance of the polyester staple fiber, and can also effectively prevent the polyester fiber from pilling.)

1. The radix isatidis extract modified polyester fiber is characterized by comprising an radix isatidis extract, a radix paeoniae alba extract, sodium pyrrolidone carboxylate, melamine phosphate and triethylamine; preferably, the mass percent of the isatis root extract is 0.1-5%, the mass percent of the white peony root extract is 0.1-1%, the mass percent of the sodium pyrrolidone carboxylate is 0.5-0.9%, the mass percent of the melamine phosphate is 0.05-0.8%, and the mass percent of the triethylamine is 0.2-0.6%.

2. The radix isatidis extract modified polyester fiber as claimed in claim 1, wherein the radix isatidis extract and the radix paeoniae alba extract are subjected to modification treatment, and the modification method comprises the following steps:

(1) adding the modified substance into water, stirring until the modified substance is completely dissolved, adding the porous nano material, uniformly stirring, and drying to obtain a porous nano material wrap;

(2) adding a long-chain alkane chain extender containing GMA side groups, bromoethane and PVA into the porous nano material wrap, uniformly stirring, and simultaneously heating at a low temperature to obtain a modified nano composite material; wherein the modified substances are radix Isatidis extract and radix Paeoniae alba extract, and are subjected to modification treatment;

the content of active ingredients in the isatis root extract or the white paeony root extract is more than or equal to 98 percent, the water content is less than or equal to 5 percent, and the total number of colonies is less than 99 cfu/g.

3. The radix isatidis extract modified polyester fiber as claimed in claim 2, wherein in the step (1), the mass ratio of the modified substance to water is 1: 5-10; the modified substance is added into water and stirred until the modified substance is completely dissolved, and the modified substance needs to be heated to 60-90 ℃.

4. The radix isatidis extract modified polyester fiber as claimed in claim 2, wherein in the step (1), the porous nano material is montmorillonite, zeolite powder, aerogel or porous nano TiO₂Microsphere, porous nano SiO₂One or more of microspheres; the mass ratio of the modified substance to the porous nano material is 1: 5-10; the drying temperature is 50-70 ℃, and the drying time is 30-60 min.

5. The radix isatidis extract modified polyester fiber according to claim 2, wherein in the step (2), the mass ratio of the total mass of the long-chain alkane chain extender containing GMA side groups, bromoethane and PVA to the porous nanomaterial aggregate is 1: and (5-7), wherein the mass ratio of the long-chain alkane chain extender containing the GMA side group to the bromoethane to the PVA is (2-4): 1-3): 1.

6. The radix isatidis extract modified polyester fiber as claimed in claim 2, wherein in the step (2), the low-temperature heating temperature is 50-60 ℃, and the low-temperature heating time is 30-60 min.

7. The radix isatidis extract modified polyester fiber as claimed in claim 2, wherein in the step (2), the stirring speed is 30-60r/min, and the stirring time is 30-120 min.

8. A preparation method of the radix isatidis extract modified polyester fiber as claimed in any one of claims 1 to 7, wherein the method comprises the following steps:

(S1) preparation of composite modifier: mixing the modified nano composite material, sodium pyrrolidone carboxylate, melamine phosphate and triethylamine, and then adding a fat-soluble solvent for grinding to obtain a composite modifier;

(S2) preparing modified polyester fiber: and melting and mixing the PET slices in a double-screw extruder, adding the composite modifier, mixing and spinning to obtain the modified polyester fiber.

9. The method for preparing isatis root extract modified polyester fiber as claimed in claim 8, wherein the fat-soluble solvent in step (S1) is wax, higher fatty glyceride or stearic acid.

10. The method for preparing radix Isatidis extract modified Dacron fiber according to claim 8, wherein the grinding particle size in step (S1) is 8000-10000 mesh.

Technical Field

The invention belongs to the technical field of spinning, and particularly relates to radix isatidis extract modified polyester fiber and a preparation method thereof.

Background

The polyester staple fiber is obtained by spinning polyester (polyethylene terephthalate, PET for short, polymerized by PTA and MEG) into a tow and cutting the tow. With the continuous development of society and the continuous improvement of the living standard of people, the concept of health of people is continuously enhanced. As a class of materials which people have more contact in everyday life, textiles also receive more and more attention on their hygiene performance. The wide existence of microorganisms such as bacteria and the like makes the textile extremely easy to become a hotbed for bacterial breeding in the processes of taking, storing, transporting and the like. The polyester fiber molecules are symmetrical in structure and are arranged closely and orderly, so that the polyester fiber has good mechanical properties and chemical properties.

Radix Isatidis (common alias: indigo root, radix Isatidis) is a Chinese medicinal material produced in various places of China, and is divided into north radix Isatidis and south radix Isatidis, the north radix Isatidis is derived from root of Isatis tinctoria and radix Isatidis of Brassicaceae; radix Isatidis is rhizome and root of herba Kalimeridis of Acanthaceae; has effects of clearing away heat and toxic materials, cooling blood, relieving swelling, and relieving sore throat. The water extract has effects in inhibiting Bacillus subtilis, Staphylococcus aureus, Spanish coccus, Escherichia coli, Salmonella typhi, Bacillus paratyphi, Shigella dysenteriae, and enteritis bacillus; the acetone extract has similar effect and is effective for hemolytic streptococcus (all by agar small-hole plate method), and has similar antibacterial effect on A-type meningococcus as that of garlic and honeysuckle flower. The antibacterial and antiviral active ingredients of isatis root and dyers woad leaf are thought to be indigoside. Radix Isatidis also has effects of resisting leptospira, removing toxic substance, improving immunity, and resisting tumor.

The polyester staple fibers disclosed at present cannot meet the requirements of simultaneously having good antibacterial performance, mechanical performance, air permeability, moisture absorption performance and melt resistance, and the polyester staple fibers are easy to pill after long-time friction.

The present invention has been made in view of the above circumstances.

Disclosure of Invention

In order to solve the problems in the prior art, the invention provides radix isatidis extract modified polyester fiber and a preparation method thereof.

The first purpose of the invention is to provide radix isatidis extract modified polyester fiber, which comprises radix isatidis extract, radix paeoniae alba extract, sodium pyrrolidone carboxylate, melamine phosphate and triethylamine; preferably, the mass percent of the isatis root extract is 0.1-5%, the mass percent of the white peony root extract is 0.1-1%, the mass percent of the sodium pyrrolidone carboxylate is 0.5-0.9%, the mass percent of the melamine phosphate is 0.05-0.8%, and the mass percent of the triethylamine is 0.2-0.6%.

Further, the isatis root extract and the white paeony root extract are subjected to modification treatment, and the modification method comprises the following steps:

(1) adding the modified substance into water, stirring until the modified substance is completely dissolved, adding the porous nano material, uniformly stirring, and drying to obtain a porous nano material wrap;

(2) adding a long-chain alkane chain extender containing GMA side groups, bromoethane and PVA into the porous nano material wrap, uniformly stirring, and simultaneously heating at a low temperature to obtain a modified nano composite material; wherein the modified substances are radix Isatidis extract and radix Paeoniae alba extract, and are subjected to modification treatment;

the content of active ingredients in the isatis root extract or the white paeony root extract is more than or equal to 98 percent, the water content is less than or equal to 5 percent, and the total number of colonies is less than 99 cfu/g.

According to the invention, the plant extract and the porous nano material are subjected to modification treatment, and the plant extract is encapsulated in the pore canal of the porous material due to the large specific surface area of the nano porous material, so that the components of the plant extract cannot be damaged when modified polyester fiber is prepared later, and the antibacterial property of the modified polyester is improved; the long-chain alkane chain extender containing GMA side groups, bromoethane and PVA are added in the modification process and are uniformly mixed, and low-temperature heating is carried out simultaneously, so that the hydrophilicity of the modified nano composite material can be effectively improved, and the moisture absorption of the subsequently prepared polyester staple fibers is further improved.

Further, in the step (1), the mass ratio of the modifying substance to the water is 1: 5-10; the modified substance is added into water and stirred until the modified substance is completely dissolved, and the modified substance needs to be heated to 60-90 ℃.

Further, in the step (1), the porous nano material is montmorillonite, zeolite powder, aerogel or porous nano TiO₂Microsphere, porous nano SiO₂One or more of microspheres; the mass ratio of the modified substance to the porous nano material is 1: 5-10; the drying temperature is 50-70 ℃, and the drying time is 30-60 min.

Further, in the step (2), the mass ratio of the total mass of the long-chain alkane chain extender containing the GMA side group, the bromoethane and the PVA to the porous nanomaterial wrap is 1: and (5-7), wherein the mass ratio of the long-chain alkane chain extender containing the GMA side group to the bromoethane to the PVA is (2-4): 1-3): 1.

Further, in the step (2), the low-temperature heating temperature is 50-60 ℃, and the low-temperature heating time is 30-60 min; the stirring speed is 30-60r/min, and the stirring time is 30-120 min.

The second object of the invention is to provide a preparation method of the radix isatidis extract modified polyester fiber, which comprises the following steps:

(S1) preparation of composite modifier: mixing the modified nano composite material, sodium pyrrolidone carboxylate, melamine phosphate and triethylamine, adding a fat-soluble solvent, and grinding to obtain a composite modifier;

(S2) preparing modified polyester fiber: and melting and mixing the PET slices in a double-screw extruder, adding the composite modifier, mixing and spinning to obtain the modified polyester fiber.

Further, in the step (S1), the fat-soluble solvent is wax, higher fatty glyceride or stearic acid.

Further, the grinding particle size in the step (S1) is 8000-10000 mesh.

Further, the mass ratio of the composite modifier to the PET chips in the step (S2) is 1-8: 100.

Compared with the prior art, the invention has the beneficial effects that:

(1) according to the invention, the isatis root extract and the porous nano material are subjected to modification treatment, and the isatis root extract and the white paeony root extract are 'packaged' in the pore canal of the porous material due to the large specific surface area of the nano porous material, so that the components of the isatis root extract and the white paeony root extract cannot be damaged when modified polyester fiber is prepared later, and the performance of the polyester staple fiber is improved; the long-chain alkane chain extender containing GMA side groups, bromoethane and PVA are added in the modification process and are uniformly mixed, and low-temperature heating is carried out simultaneously, so that the hydrophilicity of the modified nano composite material can be effectively improved, and the moisture absorption of the subsequently prepared polyester staple fibers is further improved; the antibacterial performance of the polyester staple fibers is improved by adding the isatis root extract, the antibacterial performance of the polyester staple fibers is good for staphylococcus aureus, escherichia coli and candida albicans, and the antibacterial rate is still in a compound standard after washing for 50 times; according to the invention, the radix paeoniae alba extract and the sodium pyrrolidone carboxylate are added, so that the alkalinity can be effectively reduced, the fiber is not easy to slide out of the surface of the fabric, and even if the fiber slides out to form small balls, the strength of the polyester fiber is properly reduced due to the addition of the radix paeoniae alba extract and the sodium pyrrolidone carboxylate, the small balls can be easily removed, and the problem of pilling of the polyester fiber is further avoided; according to the invention, the melamine phosphate and the triethylamine are added, and the mutual action of the melamine phosphate and the triethylamine can effectively prevent the polyester fiber from dripping, effectively prevent flame from spreading and spreading, and further effectively improve the melt resistance of the polyester;

(2) according to the invention, the obtained modified nano composite material, the sodium pyrrolidone carboxylate, the melamine phosphate and the triethylamine are added into a fat-soluble solvent for grinding, can be uniformly dispersed, and are mixed with PET slices and spun to obtain the modified polyester fiber, so that the mechanical property, the antibacterial property, the air permeability, the hygroscopicity and the meltresistance of the polyester staple fiber can be improved, and the polyester fiber is not easy to pill.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.

The isatis root extracts in the following examples and comparative examples are loose powder in appearance, free of agglomeration, brown yellow in color and uniform; the content of active ingredients is more than or equal to 98 percent, the water content is less than or equal to 5 percent, the total number of colonies is less than 99cfu/g, salmonella and escherichia coli can not be detected, and the quality guarantee period is 18 months; the white peony root extract has loose appearance powder, no agglomeration, yellow-white color and uniform and consistent color; the content of active ingredients is more than or equal to 98 percent, the water content is less than or equal to 5 percent, the total number of colonies is less than 99cfu/g, salmonella and escherichia coli can not be detected, and the shelf life is 18 months.