阅读说明：本技术 一种添加香料的纺织品用整理剂 (Textile finishing agent added with spice ) 是由 王天义 梁立冬 张政 王毅 仝丹丹 于 2021-09-26 设计创作，主要内容包括：本发明涉及一种添加香料的纺织品用整理剂,属于日用化工产品技术领域,该纺织品用整理剂通过如下步骤制备：将香料添加剂、抗菌剂、柠檬酸、次磷酸钠和去离子水混合,得到一种添加香料的纺织品用整理剂。本发明制备的一种添加香料的纺织品用整理剂中加入了一种自制的抗菌剂,该抗菌剂是以壳聚糖为基体,壳聚糖本身具有抑菌作用,本发明中的抗菌剂上引入了异氰酸酯基团,异氰酸酯基团可以与棉纺织品纤维表面的羟基发生反应,以共价键进行接枝,提高了抗菌剂的稳定抗菌性；另外将紫外吸收剂也引入了抗菌剂的结构中,在洗衣、晾衣等程序后,减少彩色衣物褪色、黑色衣物变白的情况的发生。(The invention relates to a textile finishing agent added with spice, belonging to the technical field of daily chemical products, and the textile finishing agent is prepared by the following steps: and mixing the perfume additive, the antibacterial agent, citric acid, sodium hypophosphite and deionized water to obtain the textile finishing agent added with the perfume. The textile finishing agent added with the perfume is added with a self-made antibacterial agent, the antibacterial agent takes chitosan as a matrix, the chitosan has an antibacterial effect, isocyanate groups are introduced into the antibacterial agent, and can react with hydroxyl on the surface of cotton textile fibers to be grafted by covalent bonds, so that the stable antibacterial property of the antibacterial agent is improved; in addition, the ultraviolet absorbent is also introduced into the antibacterial agent structure, so that the color fading of colored clothes and the whitening of black clothes are reduced after the procedures of washing clothes, airing clothes and the like.)

1. A textile finishing agent added with perfume is prepared by uniformly mixing a perfume additive, an antibacterial agent, citric acid, sodium hypophosphite and deionized water; the antibacterial agent is characterized by being prepared by the following steps:

step S11, mixing chlorinated trimellitic anhydride and pyridine, adding dichloromethane, stirring for 10min, then adding chitosan, and stirring for reaction for 12h to obtain a solid a;

step S12, mixing the solid a with acetic acid, adding an ultraviolet absorption component, stirring and reacting for 1h at room temperature, then heating to 120 ℃, and stirring and reacting for 8h to obtain a solid b;

and step S13, mixing isophorone diisocyanate and tetrahydrofuran, then adding the solid b, stirring for 50min, adding dibutyltin dilaurate, and stirring to react for 2h at the temperature of 60 ℃ to obtain the antibacterial agent.

2. The finishing agent for textiles with added perfume as claimed in claim 1, wherein the ratio of the amounts of chlorinated trimellitic anhydride, chitosan, pyridine and dichloromethane in step S11 is 0.4 g: 10 g: 0.1 g: 100 mL; the amount ratio of the solid a, the ultraviolet absorbing component and the acetic acid in step S12 was 10 g: 1.8 g: 300 mL; in step S13, the amount ratio of isophorone diisocyanate, solid b, dibutyltin dilaurate, and tetrahydrofuran was 1.5 g: 4.4 g: 50 mg: 60 mL.

3. A fragrance-added textile finish according to claim 1, characterized in that the uv absorbing component is prepared by the following steps:

step S21, adding concentrated sulfuric acid, an ultraviolet absorbent and N-hydroxymethyl chloroacetamide into a flask, stirring and reacting for 3 hours at the temperature of 20-30 ℃, performing aftertreatment after the reaction is finished, dropping the obtained reaction liquid into an ice water mixture, and then stirring, standing, filtering and drying to obtain an intermediate 1;

and step S22, mixing the intermediate 1 with absolute ethyl alcohol, adding concentrated hydrochloric acid, heating and refluxing for reaction for 6 hours, maintaining the pH value of the reaction system to be less than 1 in the reaction process, decompressing and concentrating to remove the ethyl alcohol after the reaction is finished, then adjusting the pH value to be 8 by using a sodium hydroxide solution with the mass fraction of 20%, and decompressing and concentrating to remove the solvent to obtain the ultraviolet absorption component.

4. The finishing agent for textile added with perfume of claim 3, wherein the mass fraction of concentrated sulfuric acid in step S21 is 98%, and the ultraviolet absorbent is one of 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole and 2- (5-tert-butyl-2-hydroxyphenyl) benzotriazole; the dosage molar ratio of the ultraviolet absorbent to the N-hydroxymethyl chloroacetamide is 1: 1; the mass ratio of the concentrated sulfuric acid to the ultraviolet absorbent is 140: 30-33 parts of; in the step S22, the mass fraction of the concentrated hydrochloric acid is 36%, and the dosage ratio of the intermediate 1 to the absolute ethyl alcohol is 1 g: 10 mL; the molar ratio of the intermediate 1 to the concentrated hydrochloric acid is 1: 1.

5. a perfume-added textile finish according to claim 1, wherein the amount ratio of the perfume additive, the antibacterial agent, the citric acid, the sodium hypophosphite and the deionized water is 0.2 g: 4-5 g: 20-30 g: 5-6 g: 1000 mL.

6. A perfumed textile finish according to claim 1, characterised in that the perfume additive is one of rhodinol and α -ionone.

Technical Field

The invention belongs to the technical field of daily-use chemical products, and particularly relates to a textile finishing agent added with spices.

Background

With the improvement of living standard of people, people not only pay more and more attention to the aesthetic feeling of the appearance of the textile, but also pursue the comfort and the safety of the textile.

Many microorganisms live in the daily used fabrics of people, such as socks, underwear, underpants, quilts, bedsheets, towels, etc., which can cause abnormal stimulation to the skin of human body, induce various skin diseases, even can spread various diseases, such as venereal diseases, skin diseases, etc., and affect health. The existence of microorganisms can also cause the degradation of macromolecules of fabric fibers, so that the fabric has the phenomena of brittle damage, color change, mildew and the like, and the appearance and color of clothes and ornaments are influenced; in addition, after washing clothes, drying clothes and other procedures, the problems of color clothes fading, black clothes whitening and the like are often found.

Disclosure of Invention

In order to solve the technical problems mentioned in the background art, the invention provides a textile finishing agent added with perfume.

The purpose of the invention can be realized by the following technical scheme:

a textile finishing agent added with perfume is prepared by the following steps:

and mixing the perfume additive, the antibacterial agent, citric acid, sodium hypophosphite and deionized water to obtain the textile finishing agent added with the perfume.

Further, the antibacterial agent is prepared by the steps of:

step S11, mixing chlorinated trimellitic anhydride and pyridine, adding dichloromethane, stirring for 10min, then adding chitosan, stirring and reacting for 12h, decompressing and filtering after the reaction is finished, washing the obtained filter cake with absolute ethyl alcohol, and drying at 40 ℃ under vacuum condition to constant weight after the washing is finished to obtain a solid a; acylation reaction is carried out on amino on chitosan molecules and acyl chloride groups on chlorinated trimellitic anhydride;

step S12, mixing the solid a with acetic acid, adding an ultraviolet absorption component, stirring and reacting for 1h at room temperature, heating to 120 ℃, stirring and reacting for 8h, cooling to room temperature after the reaction is finished, filtering, washing a filter cake with deionized water until a washing liquid is neutral, and obtaining a solid b; reacting the solid a with an ultraviolet absorption component, and introducing the ultraviolet absorption component into the solid a;

and step S13, mixing isophorone diisocyanate and tetrahydrofuran, then adding the solid b, stirring for 50min, adding dibutyltin dilaurate, and stirring to react for 2h at the temperature of 60 ℃ to obtain the antibacterial agent. The isocyanate group is introduced by reacting isophorone diisocyanate with the hydroxyl group on solid a.

Further, the use amount ratio of the chlorinated trimellitic anhydride, chitosan, pyridine and methylene chloride in step S11 was 0.4 g: 10 g: 0.1 g: 100 mL; the amount ratio of the solid a, the ultraviolet absorbing component and the acetic acid in step S12 was 10 g: 1.8 g: 300 mL; in step S13, the amount ratio of isophorone diisocyanate, solid b, dibutyltin dilaurate, and tetrahydrofuran was 1.5 g: 4.4 g: 50 mg: 60 mL.

Further, the ultraviolet absorbing component is prepared by the steps of:

step S21, adding concentrated sulfuric acid, an ultraviolet absorbent and N-hydroxymethyl chloroacetamide into a flask, stirring and reacting for 3 hours at the temperature of 20-30 ℃, performing aftertreatment after the reaction is finished, dropping the obtained reaction liquid into an ice water mixture, and then stirring, standing, filtering and drying to obtain an intermediate 1; reacting N-hydroxymethyl chloroacetamide with an ultraviolet absorbent, and reacting the N-hydroxymethyl chloroacetamide with the ortho position of a hydroxyl on the ultraviolet absorbent to prepare an intermediate 1, wherein the intermediate 1 still contains amide bond;

and step S22, mixing the intermediate 1 with absolute ethyl alcohol, adding concentrated hydrochloric acid, heating and refluxing for 6 hours, supplementing a hydrochloric acid solution in the reaction process, maintaining the pH value of the reaction system to be less than 1, decompressing and concentrating to remove the ethyl alcohol after the reaction is finished, adjusting the pH value to be 8 by using a sodium hydroxide solution with the mass fraction of 20%, decompressing and concentrating to remove the solvent to obtain the ultraviolet absorption component. In the step, the intermediate 1 is subjected to amide hydrolysis, and the obtained ultraviolet absorption component contains amino groups, so that the ultraviolet absorption component can conveniently participate in subsequent reactions and is introduced into an ultraviolet absorption structure.

Further, in step S21, the mass fraction of the concentrated sulfuric acid is 98%, and the ultraviolet absorbent is one of 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole and 2- (5-tert-butyl-2-hydroxyphenyl) benzotriazole; the dosage molar ratio of the ultraviolet absorbent to the N-hydroxymethyl chloroacetamide is 1: 1; the mass ratio of the concentrated sulfuric acid to the ultraviolet absorbent is 140: 30-33 parts of; in the step S22, the mass fraction of the concentrated hydrochloric acid is 36%, and the dosage ratio of the intermediate 1 to the absolute ethyl alcohol is 1 g: 10 mL; the molar ratio of the intermediate 1 to the concentrated hydrochloric acid is 1: 1.

further, the dosage ratio of the perfume additive, the antibacterial agent, the citric acid, the sodium hypophosphite and the deionized water is 0.2 g: 4-5 g: 20-30 g: 5-6 g: 1000 mL;

further, the perfume additive is one of rhodinol and alpha-ionone.

When in use, the fabric is immersed into the finishing agent, impregnated or padded and then dried.

The invention has the beneficial effects that:

the textile finishing agent added with the perfume is added with a self-made antibacterial agent, the antibacterial agent takes chitosan as a matrix, the chitosan has an antibacterial effect, isocyanate groups are introduced into the antibacterial agent, and can react with hydroxyl on the surface of cotton textile fibers to be grafted by covalent bonds, so that the stable antibacterial property of the antibacterial agent is improved; in addition, the ultraviolet absorbent is also introduced into the antibacterial agent structure, so that the fading of colored clothes and the whitening of black clothes are reduced after the procedures of washing clothes, airing clothes and the like.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

Preparing an ultraviolet absorption component:

step S21, adding concentrated sulfuric acid, an ultraviolet absorbent and N-hydroxymethyl chloroacetamide into a flask, stirring and reacting for 3 hours at the temperature of 20 ℃, performing aftertreatment after the reaction is finished, dropping the obtained reaction liquid into an ice-water mixture, and then stirring, standing, filtering and drying to obtain an intermediate 1; wherein the mass fraction of concentrated sulfuric acid is 98%, and the ultraviolet absorbent is 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole; the dosage molar ratio of the ultraviolet absorbent to the N-hydroxymethyl chloroacetamide is 1: 1; the mass ratio of the concentrated sulfuric acid to the ultraviolet absorbent is 140: 30, of a nitrogen-containing gas;

step S22, mixing the intermediate 1 with absolute ethyl alcohol, adding concentrated hydrochloric acid, heating and refluxing for 6 hours, supplementing a hydrochloric acid solution in the reaction process, maintaining the pH value of the reaction system to be less than 1, removing the ethyl alcohol by vacuum concentration after the reaction is finished, adjusting the pH value to be 8 by using a sodium hydroxide solution with the mass fraction of 20%, and then removing the solvent by vacuum concentration to obtain an ultraviolet absorption component; wherein the mass fraction of the concentrated hydrochloric acid is 36%, and the dosage ratio of the intermediate 1 to the absolute ethyl alcohol is 1 g: 10 mL; the molar ratio of the intermediate 1 to the concentrated hydrochloric acid is 1: 1.

example 2

Preparing an ultraviolet absorption component:

step S21, adding concentrated sulfuric acid, an ultraviolet absorbent and N-hydroxymethyl chloroacetamide into a flask, stirring and reacting for 3 hours at the temperature of 30 ℃, performing aftertreatment after the reaction is finished, dropping the obtained reaction liquid into an ice-water mixture, and then stirring, standing, filtering and drying to obtain an intermediate 1; wherein the mass fraction of the concentrated sulfuric acid is 98%, and the ultraviolet absorbent is 2- (5-tert-butyl-2-hydroxyphenyl) benzotriazole; the dosage molar ratio of the ultraviolet absorbent to the N-hydroxymethyl chloroacetamide is 1: 1; the mass ratio of the concentrated sulfuric acid to the ultraviolet absorbent is 140: 33;

step S22, mixing the intermediate 1 with absolute ethyl alcohol, adding concentrated hydrochloric acid, heating and refluxing for 6 hours, supplementing a hydrochloric acid solution in the reaction process, maintaining the pH value of the reaction system to be less than 1, removing the ethyl alcohol by vacuum concentration after the reaction is finished, adjusting the pH value to be 8 by using a sodium hydroxide solution with the mass fraction of 20%, and then removing the solvent by vacuum concentration to obtain an ultraviolet absorption component; wherein the mass fraction of the concentrated hydrochloric acid is 36%, and the dosage ratio of the intermediate 1 to the absolute ethyl alcohol is 1 g: 10 mL; the molar ratio of the intermediate 1 to the concentrated hydrochloric acid is 1: 1.

example 3

Preparing an antibacterial agent:

step S11, mixing chlorinated trimellitic anhydride and pyridine, adding dichloromethane, stirring for 10min, then adding chitosan, stirring and reacting for 12h, decompressing and filtering after the reaction is finished, washing the obtained filter cake with absolute ethyl alcohol, and drying at 40 ℃ under vacuum condition to constant weight after the washing is finished to obtain a solid a; wherein the dosage ratio of the chlorinated trimellitic anhydride to the chitosan to the pyridine to the dichloromethane is 0.4 g: 10 g: 0.1 g: 100 mL;

step S12, mixing the solid a with acetic acid, adding an ultraviolet absorption component, stirring and reacting for 1h at room temperature, heating to 120 ℃, stirring and reacting for 8h, cooling to room temperature after the reaction is finished, filtering, washing a filter cake with deionized water until a washing liquid is neutral, and obtaining a solid b; wherein the dosage ratio of the solid a, the ultraviolet absorption component and the acetic acid is 10 g: 1.8 g: 300 mL; the uv absorbing component was prepared as in example 2;

step S13, mixing isophorone diisocyanate and tetrahydrofuran, then adding the solid b, stirring for 50min, adding dibutyltin dilaurate, and stirring to react for 2h at the temperature of 60 ℃ to obtain an antibacterial agent; wherein the dosage ratio of isophorone diisocyanate, solid b, dibutyltin dilaurate and tetrahydrofuran is 1.5 g: 4.4 g: 50 mg: 60 mL.

Example 4

A textile finishing agent added with perfume is prepared by the following steps:

and mixing the perfume additive, the antibacterial agent, citric acid, sodium hypophosphite and deionized water to obtain the textile finishing agent added with the perfume.

Wherein the dosage ratio of the perfume additive, the antibacterial agent, the citric acid, the sodium hypophosphite and the deionized water is 0.2 g: 4 g: 20 g: 5 g: 1000 mL; the perfume additive is rose alcohol; the antimicrobial was prepared as in example 3.

Example 5

A textile finishing agent added with perfume is prepared by the following steps:

and mixing the perfume additive, the antibacterial agent, citric acid, sodium hypophosphite and deionized water to obtain the textile finishing agent added with the perfume.

Wherein the dosage ratio of the perfume additive, the antibacterial agent, the citric acid, the sodium hypophosphite and the deionized water is 0.2 g: 4.5 g: 25g of: 5.5 g: 1000 mL; the perfume additive is one of rhodinol and alpha-ionone; the antimicrobial was prepared as in example 3.

Example 6

A textile finishing agent added with perfume is prepared by the following steps:

and mixing the perfume additive, the antibacterial agent, citric acid, sodium hypophosphite and deionized water to obtain the textile finishing agent added with the perfume.

Wherein the dosage ratio of the perfume additive, the antibacterial agent, the citric acid, the sodium hypophosphite and the deionized water is 0.2 g: 5 g: 30g of: 6 g: 1000 mL; the perfume additive is alpha-ionone; the antimicrobial was prepared as in example 3.

Comparative example 1

The UV absorbing component of comparative example 3 was removed and the remaining raw materials and preparation process remained the same.

Comparative example 2

The antibacterial agent of example 5 was replaced with the sample prepared in comparative example 1, and the remaining raw materials and preparation process were maintained.

Comparative example 3

The antibacterial agent in example 5 was replaced with chitosan, and the remaining raw materials and preparation process were kept unchanged.

The samples prepared in examples 4 to 6 and comparative examples 2 to 3 were subjected to the test;

and (3) antibacterial property test: after the fabrics finished in the examples 4-6 and the comparative examples 2-3 are washed for five times, an antibacterial performance test is carried out according to GB/T20944.3-2008 evaluation of antibacterial performance of textiles; the test results are shown in table 1 below:

TABLE 1

As can be seen from the above table 1, the finishing agent for textiles prepared by the invention has good bacteriostatic rate maintaining effect after washing.

In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.