CN112176444A

CN112176444A - Oxidation-resistant fiber containing taxus chinensis and preparation method thereof

Info

Publication number: CN112176444A
Application number: CN202011177079.7A
Authority: CN
Inventors: 刘翔鸥
Original assignee: Shenzhen Qianwei Ecological Textile Co ltd
Current assignee: Shenzhen Qianwei Ecological Textile Co ltd
Priority date: 2020-10-28
Filing date: 2020-10-28
Publication date: 2021-01-05

Abstract

The invention discloses an anti-oxidation fiber containing taxus chinensis and a preparation method thereof, wherein the fiber raw materials mainly comprise the following components in parts by weight: 60-80 parts of a base polymer, 20-40 parts of an additive, 5-10 parts of an auxiliary agent, 3-8 parts of a nanoparticle additive, 2-5 parts of a powder filler and 6-10 parts of an alcohol additive. The invention limits the weight ratio of the raw materials and the modification conditions through the melt spinning process, so that the prepared fiber has excellent waterproofness, tensile strength, decontamination and foreign flavor removal.

Description

Oxidation-resistant fiber containing taxus chinensis and preparation method thereof

Technical Field

The invention relates to the field of fibers, in particular to an anti-oxidation fiber containing taxus chinensis and a preparation method thereof.

Background

The fiber is a natural or synthetic filament-like substance, and the textile fiber means a fiber used for textile cloth. The textile fiber has good physical properties such as certain length, fineness, elasticity, strength and the like, and also has good chemical stability. Textile fibers are classified into both natural fibers and chemical fibers. Flax, cotton yarn, hemp rope and the like are obtained from plants and belong to natural fibers; wool and silk are derived from animals, and are also natural fibers. There are many types of chemical fibers such as nylon, rayon, fiberglass, and the like.

At present, the variety of the textile fiber is more and more, the functions are also various, and therefore, the requirement for functionality is met, and the method becomes a main path for the development of novel textile fiber. In automobiles, trains, airplanes and cinema, restaurants and tea bars in public places, a plurality of textiles such as seat sheaths, wallcoverings, curtains, interior trims and the like are used, and the textiles have good flame retardance, comfortableness, air permeability and sound insulation.

However, in the process of implementing the technical solution of the invention in the embodiment of the present application, the inventor of the present application finds that at least the following technical problems exist in the prior art:

the prior art (CN1331767A) discloses a method for producing a cellulose-containing textile material, which requires a large amount of cross-linking agent, and although the cross-linking agent can make the fiber have good mechanical strength, the cross-linking agent has poor environmental pollution and environmental stability, and cannot make the material maintain durable mechanical properties, and the addition of less antioxidant component in the fiber easily causes the oxidation of the fiber during the use process, and reduces the service life of the fiber.

Therefore, it is a significant topic to research a textile fiber with good affinity to living things and environment, environmental protection, strong oxidation resistance, high tensile strength and good functionality.

Disclosure of Invention

In order to solve the problems, the invention provides an anti-oxidation fiber containing taxus chinensis in a first aspect, which comprises the following raw materials in parts by weight: 60-80 parts of a base polymer, 20-40 parts of an additive, 5-10 parts of an auxiliary agent, 3-8 parts of a nanoparticle additive, 2-5 parts of a powder filler and 6-10 parts of an alcohol additive.

In a preferred embodiment, the base polymer is at least one of an ester polymer, an amide polymer, a vinyl alcohol polymer, a nitrile polymer, and a vinyl chloride polymer; the additive is at least one of taxus chinensis extract, black tonka bean extract, aloe leaf extract, camphor leaf extract, chamomile extract, chlorella extract and modified 3-aldehyde-7-diethylamino coumarin; the auxiliary agent is at least one of di-tert-butyl-p-cresol, phenyl-alpha-aniline, zinc dialkyl dithiophosphate, diphenylamine and p-diphenol; the nanoparticle additive is at least one of titanium sugar, cerium dioxide, PAN and perovskite; the powder filler is SiO₂At least one of DE-FLUON, boron nitride and Al powder; the alcohol additive is at least one of glycerol, polyethylene glycol, methyl glycol and triethanolamine.

As a preferred embodiment, the base polymer is a copolymer of methyl ester and cyanoethylene; the weight ratio of methyl formate to cyanoethylene is 1: 3 to 4.

As a preferred scheme, the nanoparticle additive is titanium sugar nanoparticles which are modified in two steps.

As a preferable scheme, the two-step modification of the titanium sugar nanoparticles is carboxylation modification and imidazole skeleton modification respectively.

As a preferable scheme, the auxiliary agent is di-tert-butyl-p-cresol and diphenylamine; the weight ratio of di-tert-butyl-p-cresol to diphenylamine is 1-3: 1 to 3.

As a preferred scheme, the additives are taxus chinensis extract, black coumarins extract and modified 3-aldehyde-7-diethylamino coumarin; the weight ratio of the taxus chinensis extract to the black tonka bean extract to the modified 3-aldehyde-7-diethylaminocoumarin is 20-30: 1-2: 0.1 to 1.

As a preferable scheme, the powder filler is N- (beta-aminoethyl) -alpha-aminopropyl trimethyl oxygen silicane surface modified spherical SiO₂(ii) a The fineness of the powder filler is 20-50 nm.

The second aspect of the present invention provides a method for preparing the above anti-oxidation fiber containing taxus chinensis, comprising the following steps: (1) heating the base polymer to 140-150 ℃ until the base polymer is molten, adding an additive, an auxiliary agent and a powder filler, and continuously stirring for 4-5 hours until the system is completely compatible; (2) heating to 160-170 ℃, adding a nanoparticle additive and an alcohol additive, rapidly stirring, and immediately introducing into a melting granulator for bubble removal granulation to obtain spinning granules; (3) and adding the spinning granules into a spinning machine at a constant speed for spinning, and quickly cooling and condensing the formed spinning granules into tow fibers through a low-temperature air box.

As a preferable scheme, the spinning machine is a melt spinning double-screw extruder, and the heating temperature of the spinning granules in the spinning process is 160-165 ℃.

Has the advantages that: the invention provides an anti-oxidation fiber containing taxus chinensis and a preparation method thereof. The tensile strength of the fiber is improved by the melt spinning process and the addition of the powder filler; the light resistance of the fiber is improved by the nano particle additive; after the taxus extract is added, the taxol in the taxus and the auxiliary agent have synergistic effect, so that the fiber obtains excellent oxidation resistance, and meanwhile, the special properties of the taxol also provide the functions of decontamination, peculiar smell removal, inflammation diminishing, bacteriostasis and the like for the fiber.

Detailed Description

The disclosure may be understood more readily by reference to the following detailed description of preferred embodiments of the invention and the examples included therein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.

The term "prepared from …" as used herein is synonymous with "comprising". The terms "comprises," "comprising," "includes," "including," "has," "having," "contains," "containing," or any other variation thereof, as used herein, are intended to cover a non-exclusive inclusion. For example, a composition, process, method, article, or apparatus that comprises a list of elements is not necessarily limited to only those elements but may include other elements not expressly listed or inherent to such composition, process, method, article, or apparatus.

The conjunction "consisting of …" excludes any unspecified elements, steps or components. If used in a claim, the phrase is intended to claim as closed, meaning that it does not contain materials other than those described, except for the conventional impurities associated therewith. When the phrase "consisting of …" appears in a clause of the subject matter of the claims rather than immediately after the subject matter, it defines only the elements described in the clause; other elements are not excluded from the claims as a whole.

When an amount, concentration, or other value or parameter is expressed as a range, preferred range, or as a range of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, when a range of "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2 and 4 to 5", "1 to 3 and 5", and the like. When a range of values is described herein, unless otherwise stated, the range is intended to include the endpoints thereof and all integers and fractions within the range.

The singular forms "a", "an" and "the" include plural referents unless the context clearly dictates otherwise. "optional" or "any" means that the subsequently described event or events may or may not occur, and that the description includes instances where the event occurs and instances where it does not.

Approximating language, as used herein throughout the specification and claims, is intended to modify a quantity, such that the invention is not limited to the specific quantity, but includes portions that are literally received for modification without substantial change in the basic function to which the invention is related. Accordingly, the use of "about" to modify a numerical value means that the invention is not limited to the precise value. In some instances, the approximating language may correspond to the precision of an instrument for measuring the value. In the present description and claims, range limitations may be combined and/or interchanged, including all sub-ranges contained therein if not otherwise stated.

In addition, the indefinite articles "a" and "an" preceding an element or component of the invention are not intended to limit the number requirement (i.e., the number of occurrences) of the element or component. Thus, "a" or "an" should be read to include one or at least one, and the singular form of an element or component also includes the plural unless the stated number clearly indicates that the singular form is intended.

In order to solve the above problems, the first aspect of the present invention provides an oxidation-resistant taxus chinensis-containing fiber raw material comprising the following components in parts by weight: 60-80 parts of a base polymer, 20-40 parts of an additive, 5-10 parts of an auxiliary agent, 3-8 parts of a nanoparticle additive, 2-5 parts of a powder filler and 6-10 parts of an alcohol additive.

In some preferred embodiments, the base polymer is at least one of an ester polymer, an amide polymer, a vinyl alcohol polymer, a nitrile polymer, and a vinyl chloride polymer; the additive is at least one of taxus chinensis extract, black tonka bean extract, aloe leaf extract, camphor leaf extract, chamomile extract, chlorella extract and modified 3-aldehyde-7-diethylamino coumarin; the auxiliary agent is at least one of di-tert-butyl-p-cresol, phenyl-alpha-aniline, zinc dialkyl dithiophosphate, diphenylamine and p-diphenol; the nanoparticle additive is at least one of titanium sugar, cerium dioxide, PAN and perovskite; the powder filler is SiO₂At least one of DE-FLUON, boron nitride and Al powder; the alcohol additive is at least one of glycerol, polyethylene glycol, methyl glycol and triethanolamine.

In some preferred embodiments, the base polymer is a copolymer of methyl ester and cyanoethylene; the weight ratio of methyl formate to cyanoethylene is 1: 3 to 4.

The acrylic polymer copolymerized by methyl methacrylate and cyanoethylene is used as the basic polymer of the fiber, so that the tensile strength and the production efficiency of the composite fiber are improved, and the environment-friendly property is higher. The applicant speculates that the addition of the methyl ester flexible monomer increases the thermal decomposition temperature of the cyanoethylene polymer, and decreases the melting temperature when the weight ratio of methyl ester to cyanoethylene is 1: 3-4, the melting temperature of the polymer is far lower than the decomposition temperature, and the composite fiber can be prepared through melt spinning.

The invention relates to a self-made methyl ester and cyanoethylene copolymer, which comprises the following steps: (1) heating a water bath kettle to 50-60 ℃, measuring distilled water, adding the distilled water into a three-neck flask, and introducing N₂Protection; (2) weighing emulsifier OP-10 and SDS (CAS number: 151-21-3), adding into a three-neck flask, stirring, and reflux-cooling with a condenser; (3) measuring a predetermined amount of cyanoethylene (CAS number: 107-13-1) and methyl ester (CAS number: 80-62-6), uniformly mixing, and adding n-dodecyl mercaptan (CAS number: 112-55-0) into a three-neck flask; (4) after reacting for 1 hour, adding ammonium persulfate for the first time;mixing the cyanoethylene and the methyl ester uniformly, taking out 10% of the mixed solution, and directly adding the mixed solution into a reaction system for reaction for 1-2 hours; (5) after the reaction is finished, adding an ammonium persulfate initiator for the second time, dropwise adding the rest of the mixed solution into a three-neck flask, controlling the dropwise adding speed to be 2 drops/s, and reacting for 4-5 hours; (6) and after the reaction is finished, taking out the reaction liquid, adding a magnesium sulfate demulsifier for demulsification, and finally filtering and drying the demulsified product to obtain the final product.

The cyanoethylene in the present invention may be commercially available, for example, an analytically pure cyanoethylene product produced by chemical Limited of Shandong province, Jinan Aochen.

The methyl ester of the present invention may be a commercially available, for example, analytical grade methyl ester product sold by the company Aladdin Chemicals.

In some preferred embodiments, the nanoparticle additive is a titanium sugar nanoparticle that has been modified in two steps.

In some preferred embodiments, the two-step modification of the titanium saccharide nanoparticles is a carboxylation modification and an imidazole backbone modification, respectively.

The titanium sugar after the two-step modification is added as a nano particle additive, so that the light resistance of the composite fiber can be effectively improved. The applicant speculates that: the heterojunction structure in the titanium sugar after the two-step modification effectively inhibits the backflow of electron-hole pairs, and improves the light absorption wavelength of the titanium sugar, so that the absorption effect of the titanium sugar on ultraviolet light and visible light is obviously improved.

The two-step modified titanium sugar is self-made, and comprises the following steps: (1) dissolving dihydro-2, 5-furandione (CAS number: 108-30-5) in DMF solution, heating and stirring at 40-50 deg.C in water bath for 1-2 hr; (2) adding a DMF solution containing titanium sugar (13463-67-7) into the DMF solution while stirring, uniformly stirring and dispersing, then dropwise adding N- (beta-aminoethyl) -alpha-aminopropyltrimethoxysilane (CAS number: 1760-24-3), and continuously stirring and reacting for 3-4 hours to obtain the first-step modified titanium sugar nanoparticles; (3) mixing the titanium sugar nanoparticles modified in the first step with a predetermined amount of dimethylimidazole (CAS number: 693-98-1) and zinc nitrate, adding a deionized water solvent, reacting at the temperature of 80-100 ℃ for 2-2.5 hours, washing and drying the obtained product, and obtaining the modified titanium sugar coordinated and combined with the imidazole skeleton.

In some preferred embodiments, the coagent is di-t-butyl-p-cresol and diphenylamine; the weight ratio of di-tert-butyl-p-cresol to diphenylamine is 1-3: 1 to 3.

The compounding of the phenol-based auxiliary agent and the amine-based auxiliary agent has more remarkable effect on reducing the phenomenon of atom electron loss in the fiber than the single use. The di-tert-butyl-p-cresol and the diphenylamine can simultaneously capture active free electrons, so that the active free electrons are changed into inactive electrons, continuous electron losing reactions are inhibited, the phenols are beneficial to the regeneration of amines so that the amines can work circularly, the atom electron losing reactions can be inhibited for a long time, the electron losing activity of the whole composite fiber is inhibited through the synergistic effect of the phenol and the amine, and the performance stability of the whole fiber is improved.

In some preferred embodiments, the additive is a yew extract (yew, a natural treasure anticancer plant belonging to the family taxaceae in the order taxotere, class piniperidae, the phylum gymnospermum), a black coumarins extract and a modified 3-aldehyde-7-diethylaminocoumarin; the weight ratio of the taxus chinensis extract to the black tonka bean extract to the modified 3-aldehyde-7-diethylaminocoumarin is 20-30: 1-2: 0.1 to 1.

The addition of the taxus chinensis extract, the black coumarins extract and the modified 3-aldehyde-7-diethylamino coumarin can effectively improve the functionality of the composite fiber and provide excellent glossiness and anti-inflammatory and antibacterial properties. The applicant speculates that: paclitaxel acts on the microtubule system of fungal cells to prevent microtubule depolymerization, which results in abnormal arrangement of vascular bundles; the taxol has excellent free radical scavenging activity and the synergistic effect of an auxiliary agent, and inhibits active free radicals and free electrons, thereby inhibiting the chain continuous electron losing reaction; the mutual interaction between the coumarin component and the modified 3-aldehyde-7-diethylamino coumarin molecule in the black coumarins extract and the energy transfer among multiple states improve the energy utilization rate and the transfer efficiency, convert harmful light, and reduce the damage of illumination to fibers under the synergistic effect with the two-step modified titanium sugar nanoparticles.

The modified 3-aldehyde-7-diethylamino coumarin is self-made, and the preparation method comprises the following steps: (1) dissolving indole modifier and 3-aldehyde-7-diethylaminocoumarin (CAS number: 54711-39-6) in diethyl ether; (2) dropwise adding nitric acid serving as a reaction catalyst into the solution until the pH value is 2.5-6, installing condensation reflux after the dropwise adding is finished, heating to 50-60 ℃, and continuously stirring for reacting for 2-3 hours; (3) and after the reaction solution generates a precipitate, filtering the product, and leaching a filter cake by using diethyl ether to obtain a final product.

The indole modifier is self-made, and the preparation method comprises the following steps: under the protection of nitrogen, 5-chloro-2-methylindole (CAS number: 1075-35-0) is dissolved in toluene and heated to 50-60 ℃ for preheating, then 5-bromo-m-xylene glycol (CAS number: 51760-22-6) is dropwise added into a flask, the temperature is fixed at 60 ℃ with continuous stirring, after the reaction is finished, the mixture is refluxed for 3-4 hours, and then the reaction solution is dried in a spinning mode to obtain the final product.

The black tonka bean extract in the invention can be commercially available, for example, the black tonka bean extract product produced by Gansu Probiotics and Probiotics, Inc.

In some preferred embodiments, the powder filler is N- (. beta. -aminoethyl) -a-aminopropyltrimethoxysilane surface-modified spherical SiO₂(ii) a The fineness of the powder filler is 20-50 nm.

Spherical SiO surface-modified with N- (. beta. -aminoethyl) - α -aminopropyltrimethoxysilane₂As a powder filler, the composite fiber can effectively improve the waterproofness and tensile strength of the composite fiber, and improve the overall performance. The applicant speculates that: modified SiO₂Surface carboxyl groups being replaced, SiO₂The surface and the base polymer show good interfacial associativity, can be quickly and effectively dispersed in a polymer matrix when being added without adding an oleophilic suspension forming agent, eliminates the influence of the forming agent on the fiber performance, and simultaneously SiO under the fineness₂Can be effectively filled in the inner pores after the fiber is formed.

The invention relates to a spherical SiO after surface modification of N- (beta-aminoethyl) -alpha-aminopropyltrimethoxysilane (CAS number: 1760-24-3)₂The method is self-made and comprises the following steps: (1) n- (. beta. -aminoethyl) radical) The alpha-aminopropyl trimethoxy silane, deionized water and ethanol are subjected to reaction by 2-3: 2: 5, diluting, adding nitric acid to adjust the pH value to 4-4.5, stirring at room temperature for 3-3.5 hours, adding the diluent into an ethanol solution, and adding spherical SiO₂Slowly adding the mixture into the reaction kettle, heating to 90-100 ℃ with slight stirring, reacting for 5-6 hours, washing with ethanol, and drying at 70-80 ℃ for 12-24 hours to obtain surface-treated spherical SiO₂。

The second aspect of the invention provides a preparation method of the anti-oxidation fiber containing the taxus chinensis, which comprises the following steps: (1) heating the base polymer to 140-150 ℃ until the base polymer is molten, adding an additive, an auxiliary agent and a powder filler, and continuously stirring for 4-5 hours until the system is completely compatible; (2) heating to 160-170 ℃, adding a nanoparticle additive and an alcohol additive, rapidly stirring, and immediately introducing into a melting granulator for bubble removal granulation to obtain spinning granules; (3) and adding the spinning granules into a spinning machine at a constant speed for spinning, and quickly cooling and condensing the formed spinning granules into tow fibers through a low-temperature air box.

In some preferred embodiments, the spinning machine is a melt spinning twin-screw extruder, and the heating temperature of the spinning pellets in the spinning process is 160-165 ℃.

Examples

The technical solution of the present invention is described in detail by the following examples, but the scope of the present invention is not limited to all of the examples. The starting materials of the present invention are all commercially available unless otherwise specified.

Example 1

Embodiment 1 provides an anti-oxidation fiber containing taxus chinensis, which comprises the following raw materials in parts by weight: 60 parts of a copolymer of methyl formate and cyanoethylene, 30 parts of an additive (the weight ratio of the taxus chinensis extract, the black coumarone extract and the modified 3-aldehyde-7-diethylamino coumarin is 28: 2: 1), 5 parts of di-tert-butyl-p-cresol, 5 parts of diphenylamine, 8 parts of two-step modified titanium sugar, 8 parts of N- (beta-aminoethyl) -alpha-aminopropyl trimethoxy silane surface-modified spherical SiO₂5 parts (fineness of 30nm) and 10 parts of glycerol.

Example 1 alsoProvides a preparation method of anti-oxidation fiber containing taxus chinensis, which comprises the following steps (in parts by weight): (1) heating 60 parts of a copolymer of methyl methacrylate and cyanoethylene to 145 ℃ to be molten, adding 28 parts of a taxus chinensis extract, 1 part of a black coumarins extract, 1 part of indole-modified 3-aldehyde-7-diethylaminocoumarin, 5 parts of di-tert-butyl-p-cresol, 5 parts of diphenylamine and N- (beta-aminoethyl) -alpha-aminopropyltrimethoxysilane surface-modified spherical SiO₂5 parts of the mixture is continuously stirred for 4 hours until the system is completely compatible; (2) heating to 170 ℃, adding 8 parts of titanium sugar and 5 parts of glycerol which are modified in the two steps, quickly stirring, and immediately introducing into a melting granulator for bubble removal granulation to obtain spinning granules; (3) adding the spinning granules into a double-screw extruder for melt spinning, and quickly cooling and condensing the extruded and molded pellets into tow fibers by a low-temperature air box at 5 ℃.

The taxus extract in this example is a taxus extract product produced by shanxi Hao Chen Biotech limited.

The copolymer of methyl formate and cyanoethylene in this example was prepared by the following steps: (1) heating a water bath kettle to 55 ℃, measuring 100 parts of distilled water, adding the distilled water into a three-neck flask, and introducing N₂Protection; (2) weighing emulsifier OP-102.5 parts and SDS (CAS number: 151-21-3)2 parts, adding into a three-neck flask, stirring, and reflux-cooling with a condenser; (3) 60 parts of cyanoethylene (CAS number: 107-13-1) and 20 parts of methyl formate (CAS number: 80-62-6) are weighed and uniformly mixed, and 2 parts of n-dodecyl mercaptan (CAS number: 112-55-0) are added into a three-neck flask; (4) after reacting for 1 hour, adding 1 part of ammonium persulfate for the first time; mixing the cyanoethylene and the methyl ester uniformly, taking out 8 parts of mixed solution, and directly adding the mixed solution into a reaction system for reaction for 1 hour; (5) after the reaction is finished, adding 1 part of ammonium persulfate initiator for the second time, dropwise adding the rest of mixed solution into the three-neck flask, controlling the dropwise adding speed to be 2 drops/s, and reacting for 4 hours; (6) and after the reaction is finished, taking out the reaction liquid, adding 60 parts of anhydrous magnesium sulfate demulsifier for demulsification, and finally filtering and drying the demulsified product to obtain the final product.

In this example, the cyanoethylene product was an analytically pure cyanoethylene product produced by chemical Limited in south-east province, Aohne, Japan.

In this example, the methyl ester may be an analytically pure methyl ester product sold by alatin chemical company.

The two-step modified titanium sugar is self-made in the embodiment and comprises the following steps: (1) dissolving 2 parts of dihydro-2, 5-furandione (CAS number: 108-30-5) in 20 parts of DMF solution, and heating and stirring at 50 ℃ in a water bath for 1 hour; (2) adding 20 parts of DMF solution containing 3 parts of titanium sugar (13463-67-7) while stirring, stirring and dispersing uniformly, then dropwise adding 5 parts of N- (beta-aminoethyl) -alpha-aminopropyltrimethoxysilane (CAS number: 1760-24-3), and continuously stirring and reacting for 3 hours to obtain the first-step modified titanium sugar nanoparticles; (3) 5 parts of the first-step modified titanium sugar nanoparticles, 5 parts of dimethylimidazole (CAS number: 693-98-1) and 3 parts of zinc nitrate are mixed, 50 parts of deionized water solvent is added, the mixture reacts for 2 hours at the temperature of 80 ℃, and the obtained product is washed and dried to obtain the modified titanium sugar coordinated and combined with the imidazole skeleton.

The modified 3-formyl-7-diethylaminocoumarin is prepared by a self-made method, and the preparation method comprises the following steps: (1) dissolving 3 parts of indole modifier and 5 parts of 3-aldehyde-7-diethylamino coumarin (CAS number: 54711-39-6) in 20 parts of diethyl ether; (2) dropwise adding 2 parts of nitric acid serving as a reaction catalyst into the solution until the pH value is 5, installing condensation reflux after the dropwise adding is finished, and heating to 60 ℃ to continuously stir for reaction for 2 hours; (3) and after the reaction solution generates a precipitate, filtering the product, and leaching a filter cake by using diethyl ether to obtain a final product.

The black tonka bean extract in the embodiment is a black tonka bean extract product produced by Gansu Probiotics and Reineckia Carneae biotechnology company.

N- (. beta. -aminoethyl) - α -aminopropyltrimethoxysilane in this example(CAS number: 1760-24-3) surface-modified spherical SiO₂The method is self-made and comprises the following steps: (1) n- (β -aminoethyl) - α -aminopropyltrimethoxysilane reacted with deionized water and ethanol over a 30: 20: diluting 50 parts by weight, adding 10 parts of nitric acid to adjust the pH to 4, stirring at room temperature for 3 hours, adding the diluent into an ethanol solution, and adding 5 parts of spherical SiO₂Slowly adding into the mixture, heating to 100 deg.C with slight stirring, reacting for 5 hr, washing with ethanol, and drying at 80 deg.C for 24 hr to obtain surface-treated spherical SiO₂。

The fiber produced in this example was designated X1.

Example 2

The embodiment of the present invention is different from embodiment 1 in that: the content of the cyanoethylene is 80 parts.

The fiber produced in this example was designated X2.

Example 3

The embodiment of the present invention is different from embodiment 1 in that: 6 parts of di-tert-butyl-p-cresol and 3 parts of diphenylamine.

The fiber produced in this example was designated X3.

Comparative example 1

The embodiment of this comparative example is the same as example 1 except that: methyl ester is 10 parts, and cyanoethylene is 80 parts.

The fiber produced in this comparative example was designated as D1.

Comparative example 2

The embodiment of this comparative example is the same as example 1 except that: the unmodified titanose is added.

The fiber produced in this comparative example was designated as D2.

Comparative example 3

The embodiment of this comparative example is the same as example 1 except that: 9 portions of di-tert-butyl-p-cresol and 1 portion of diphenylamine.

The fiber produced in this comparative example was designated as D3.

Comparative example 4

The embodiment of this comparative example is the same as example 1 except that: the weight ratio of the taxus chinensis extract to the black tonka bean extract to the modified 7-diethylaminocoumarin is 1: 1: 1.

the fiber produced in this comparative example was designated as D4.

Comparative example 5

The embodiment of this comparative example is the same as example 1 except that: n- (beta-aminoethyl) -alpha-aminopropyltrimethoxysilane modified spherical SiO₂Has a fineness of 200 nm.

The fiber produced in this comparative example was designated as D5.

Evaluation of Performance

1.24-hour smoke adsorption: the sample fibers were woven into a cloth, placed in a closed, smoke-filled container for 24 hours, taken out and tested for the smoke smell associated with it, 5 samples were tested for each example, and the measured values were averaged and reported in table 1.

2. Tensile strength: the sample fibers were woven into a fabric and measured with an electronic universal tester with reference to the standard GB/T528-.

3. Water contact angle: the sample fibers were woven into a cloth, and the hydrophilicity in air was measured on the sample using a sessile drop method water contact angle tester, 5 samples were tested for each example, and the measured water contact angle values were averaged and reported in table 1.

TABLE 1

Examples	Water contact angle	24 hours smoke adsorption	Tensile Strength (MPa)
				X1	150°	No smoke smell	47
X2	147°	No smoke smell	42
				X3	148°	No smoke smell	45
D1	101°	Extremely strong smoke flavor	31
				D2	105°	Extremely strong smoke flavor	29
D3	106°	Extremely strong smoke flavor	28
				D4	99°	Extremely strong smoke flavor	30
D5	91°	Extremely strong smoke flavor	25

Through the embodiments 1-3 and the comparative examples 1-5, the anti-oxidation fiber containing the taxus chinensis and the preparation method thereof provided by the invention have the advantages that the prepared fabric has excellent waterproofness, tensile strength and decontamination and odor removal properties, is suitable for popularization in the field of fabric fibers, and has a wide development prospect. Wherein, the example 1 obtains the best performance index under the factors of the best raw material weight ratio, the best modification condition, the best spinning process and the like.

Finally, it should be understood that the above-described embodiments are merely preferred embodiments of the present invention, and not intended to limit the present invention, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. An anti-oxidation fiber containing taxus chinensis, which is characterized in that: the raw materials comprise the following components in parts by weight: 60-80 parts of a base polymer, 20-40 parts of an additive, 5-10 parts of an auxiliary agent, 3-8 parts of a nanoparticle additive, 2-5 parts of a powder filler and 6-10 parts of an alcohol additive.

2. The oxidation resistant taxus chinensis-containing fiber as claimed in claim 1, wherein: the basic polymer is at least one of ester polymer, amide polymer, vinyl alcohol polymer, nitrile polymer and vinyl chloride polymer; the additive is at least one of taxus chinensis extract, black tonka bean extract, aloe leaf extract, camphor leaf extract, chamomile extract, chlorella extract and modified 3-aldehyde-7-diethylamino coumarin; the auxiliary agent is ditertiary butyl p-cresol, phenyl-alpha-aniline, o-xylylenediamine, methylphenol and diphenylamineAnd at least one of p-diphenol; the nano particle additive is at least one of titanium sugar, cerium dioxide, polyacrylonitrile and perovskite; the powder filler is SiO₂At least one of DE-FLUON, boron nitride and Al powder; the alcohol additive is at least one of glycerol, polyethylene glycol, methyl glycol and triethanolamine.

3. The oxidation resistant taxus chinensis-containing fiber as claimed in claim 1, wherein: the base polymer is a copolymer of methyl ester and cyanoethylene; the weight ratio of methyl formate to cyanoethylene is 1: 3 to 4.

4. The oxidation resistant taxus chinensis-containing fiber as claimed in claim 1, wherein: the nano particle additive is titanium sugar nano particles modified by two steps.

5. The oxidation resistant taxus chinensis-containing fiber as claimed in claim 4, wherein: the two-step modification of the titanium sugar nano particles is carboxylation modification and imidazole skeleton modification respectively.

6. The oxidation resistant taxus chinensis-containing fiber as claimed in claim 1, wherein: the auxiliary agent is di-tert-butyl-p-cresol and diphenylamine; the weight ratio of di-tert-butyl-p-cresol to diphenylamine is 1-3: 1 to 3.

7. The oxidation resistant taxus chinensis-containing fiber as claimed in claim 1, wherein: the additive is a taxus chinensis extract, a black coumarins extract and modified 3-aldehyde-7-diethylaminocoumarin; the weight ratio of the taxus chinensis extract to the black tonka bean extract to the modified 3-aldehyde-7-diethylaminocoumarin is 20-30: 1-2: 0.1 to 1.

8. The oxidation resistant taxus chinensis-containing fiber as claimed in claim 1, wherein: the powder filler is N- (beta-aminoethyl) -alpha-aminopropyl trimethyl oxysilane surface modified ballType SiO₂(ii) a The fineness of the powder filler is 20-50 nm.

9. A method of preparing an oxidation resistant taxus chinensis containing fiber according to claim 1, wherein: comprises the following steps: (1) heating the base polymer to 140-150 ℃ until the base polymer is molten, adding an additive, an auxiliary agent and a powder filler, and continuously stirring for 4-5 hours until the system is completely compatible; (2) heating to 160-170 ℃, adding a nanoparticle additive and an alcohol additive, rapidly stirring, and immediately introducing into a melting granulator for bubble removal granulation to obtain spinning granules; (3) and adding the spinning granules into a spinning machine at a constant speed for spinning, and quickly cooling and condensing the formed spinning granules into tow fibers through a low-temperature air box.

10. The method of preparing oxidation resistant taxus chinensis containing fiber as claimed in claim 9, wherein: the spinning machine is a melt spinning double-screw extruder, and the heating temperature of the spinning granules in the spinning process is 160-165 ℃.