CN101187164A - A kind of anti-wrinkle, antibacterial and anti-ultraviolet composite functional silk fabric and its preparation method - Google Patents

Abstract

The invention discloses a silk face material with compound functions of anti-wrinkle, antibiotic and anti-ultraviolet and the production method, which processes the product through the steps of processing silk nanometer anti-wrinkle, antibiotic and anti-violet finish and finishing the silk fabric, wherein the invention uses waste silk as material, which is helpful of resource regeneration; the waste silk belongs to natural green product and the silk face material with the compound functions of anti-wrinkle, anti-biotic and anti-ultraviolet meets the requirements of twenty-first century that the fabric functions should be oriented to develop based on comfort, cleanness and safety and cater for the consumption concept of green, health and fashion with easy process and low cost. The product passes the test with good anti-wrinkle, anti-biotic and anti-ultraviolet functions.

Description

A kind of anti-wrinkle, antibacterial and anti-ultraviolet composite functional silk fabric and its preparation method

Technical field:

The invention relates to a real silk fabric and a preparation method.

Background technique:

Silk fabric has many excellent properties, such as air permeability and moisture absorption, and also has excellent drapability, soft luster, special silky feeling, soft and comfortable to wear, and is deeply loved by people. With the continuous emergence of new chemical fibers in recent years, the inherent defects of silk itself have become more and more obvious, and traditional silk products have been severely challenged. Improving its anti-wrinkle performance and endowing it with various special functions, and improving the added value of silk is the key to silk. It is an urgent need for production enterprises to remain invincible. Existing waste silk, as the main by-product of the silk industry, has not been effectively utilized.

Invention content:

The object of the present invention is to provide a real silk fabric with anti-wrinkle, antibacterial and anti-ultraviolet composite functions and a preparation method.

Technical solution of the present invention is:

An anti-wrinkle, anti-bacterial, anti-ultraviolet composite functional silk fabric is characterized in that it is made by the following method:

(1) Preparation of silk fibroin nanosol anti-wrinkle antibacterial anti-ultraviolet finishing agent:

Preparation of liquid A: hydrolyzing waste silk with sodium hydroxide to obtain silk fibroin hydrolyzate;

Preparation of liquid B: Take butyl titanate, glacial acetic acid and deionized water, stir evenly, add to hydrochloric acid solution, after peptization, cool and age to obtain nano-titanium dioxide sol;

Compounding: adjust the pH of liquid A and liquid B to 3-5, and then mix and compound to obtain a stable anti-wrinkle, anti-bacterial, anti-ultraviolet finishing agent of silk fibroin nanosol;

(2) Finishing: Put the real silk fabric into the silk nano sol anti-wrinkle, anti-bacterial and anti-ultraviolet finishing agent for padding, and dry to obtain the product.

When liquid A and liquid B are mixed and compounded in step (1), the weight ratio of liquid A to liquid B is 6:4.

A method for preparing an anti-wrinkle, anti-bacterial and anti-ultraviolet composite functional silk fabric is characterized in that it comprises the following steps:

(1) Preparation of silk fibroin nanosol anti-wrinkle antibacterial anti-ultraviolet finishing agent:

Preparation of liquid A: hydrolyzing waste silk with sodium hydroxide to obtain silk fibroin hydrolyzate;

Preparation of liquid B: Take butyl titanate, glacial acetic acid and deionized water, stir evenly, add to hydrochloric acid solution, after peptization, cool and age to obtain nano-titanium dioxide sol;

Compounding: adjust the pH of liquid A and liquid B to 3-5, and then mix and compound to obtain a stable anti-wrinkle, anti-bacterial, anti-ultraviolet finishing agent of silk fibroin nanosol;

(2) Finishing: Put the real silk fabric into the silk nano sol anti-wrinkle, anti-bacterial and anti-ultraviolet finishing agent for padding, and dry to obtain the product.

In step (1), when liquid A is prepared, the concentration of sodium hydroxide is 1-5mol/L, the hydrolysis temperature is 70°C, the amount of waste silk is 1-5g, the amount of sodium hydroxide is 50-250ml, and the hydrolysis time is 1 ~2 hours; when preparing liquid B, take 3.5-35g of butyl titanate, 0.6-6ml of glacial acetic acid, add 10-100ml of deionized water and stir evenly with a magnetic stirrer, then add it dropwise to 40ml at a concentration of 0.1mol/L hydrochloric acid solution, at the same time at 20 ° C for 30 minutes under constant temperature magnetic stirring, then raised the temperature to 40 ° C and continued to stir for 40 minutes to make it peptized, took it out and naturally cooled and aged to obtain nano-titanium dioxide sol; when mixing liquid A and liquid B , The weight ratio of liquid A and liquid B is 6:4.

The specific method of step (2) is: put the real silk fabric into the silk nano sol anti-wrinkle, antibacterial and anti-ultraviolet finishing agent working solution for padding, the rolling rate is 85%, and the padding is two dipping and two rolling; Pre-bake for 2 minutes, then bake at 120-160°C for 3-4 minutes, then wash with water and dry to obtain the product.

The silk fibroin finishing agent made by degumming and hydrolyzing waste silk has a certain amount of free active groups, such as hydroxyl, amino, carboxyl, etc., which can form relatively stable chemical bonds with silk fiber molecules, or precipitate in the amorphous area of the fiber, Thereby improving the wrinkle resistance of real silk.

Titanium dioxide produced in nano-sol has good antibacterial and anti-ultraviolet functions; nano-materials can also be used as catalysts for silk fibroin anti-wrinkle finishing due to their large surface area, many surface active centers, and strong adsorption capacity.

The silk fibroin hydrolyzate and nano-sol are compounded into a stable finishing agent in a certain proportion under a certain pH condition, which has a synergistic effect and makes the finished silk fabric have better anti-wrinkle, anti-bacterial, anti-ultraviolet composite functions.

The invention uses waste silk as a raw material, which is beneficial to the regeneration of resources; waste silk belongs to natural green products, and the developed anti-wrinkle, anti-bacterial, anti-ultraviolet composite functional silk fabric meets the requirements of the functional finishing of textiles in the 21st century, which should be based on comfort, cleanliness and safety. Development direction, and cater to people's "environmental protection, health, fashion" consumption concept, convenient processing, low cost. After testing, the product has good anti-wrinkle, anti-bacterial and anti-ultraviolet composite functions, among which the anti-wrinkle performance is increased by 10-30%, the anti-ultraviolet UPF level is 40-50 ⁺ , and the antibacterial zone for Escherichia coli and Staphylococcus aureus is 1-10mm, and the hand feels Soft and comfortable to wear, meeting the requirements for taking.

The present invention will be further described below in conjunction with embodiment.

Detailed ways:

Example 1: Finishing silk fabrics with silk fibroin nano-sol composite functional finishing agent

(1) Prepare A liquid: hydrolyze waste silk with sodium hydroxide to obtain silk fibroin hydrolyzate; wherein the concentration of sodium hydroxide is 2mol/L, the consumption of waste silk is 2g, the consumption of sodium hydroxide is 50ml, and the hydrolysis temperature is 70 ℃, the hydrolysis time is 2 hours.

(2) Preparation of liquid B: Take 3.5g of butyl titanate and 3ml of glacial acetic acid, add 10ml of deionized water and stir evenly with a magnetic stirrer, then add them dropwise to 40ml of 0.1mol/L hydrochloric acid solution, and at the same time After 30 minutes of magnetic stirring at constant temperature at 20°C, the temperature was raised to 40°C and continued to stir for 40 minutes to make it peptized, and then it was taken out and naturally cooled and aged to obtain nano-titanium dioxide sol;

(3) Preparation of silk fibroin nanosol anti-wrinkle, antibacterial and anti-ultraviolet finishing agent: adjust the pH of liquid A and liquid B to 4 respectively, and compound according to a certain proportion to form a stable finishing agent. Wherein the weight ratio of silk fibroin to nano sol is 6:4.

(4) Finishing: put the real silk fabric into silk nano sol anti-wrinkle antibacterial and anti-ultraviolet finishing agent working solution (3) for padding, the rolling rate is 85%, and the padding is two dipping and two rolling; Bake for 2 minutes, then bake at 150°C for 3 minutes, then wash with water and dry to obtain the product.

Comparative Example 1: Finishing silk fabrics with silk fibroin hydrolyzate

(1) Preparation of silk fibroin hydrolyzate (liquid A): hydrolyze waste silk with sodium hydroxide to obtain silk fibroin hydrolyzate; wherein the concentration of sodium hydroxide is 2mol/L, the consumption of waste silk is 2g, and the consumption of sodium hydroxide is 50ml, the hydrolysis temperature is 70°C, the hydrolysis time is 2 hours, and the pH is adjusted to 7.

(2) Finishing: put the silk fabric into the silk fibroin working solution (liquid A) for padding, the rolling rate is 85%, and the padding is two dipping and two rolling; then pre-baking at 90°C for 2 minutes, ℃ for 3 minutes, then washed with water and dried to obtain the product.

Comparative example 2: nano sol finishing silk fabric

(1) Preparation of nano-sol (B solution): Take 3.5g of butyl titanate and 3ml of glacial acetic acid, add 10ml of deionized water and stir evenly with a magnetic stirrer, then add it dropwise to 40ml of 0.1mol/L hydrochloric acid solution At the same time, after 30 minutes of magnetic stirring at a constant temperature at 20 ° C, the temperature was raised to 40 ° C and continued to stir for 40 minutes to make it peptized, and it was taken out and naturally cooled and aged to obtain a nano-titanium dioxide sol, and the pH was adjusted to 3;

(2) Finishing: Put the real silk fabric into the nano sol working solution (B liquid) for padding, wherein the nano sol compound working solution is made of silk fibroin and nano sol, and the weight ratio of silk fibroin and nano sol is 6 : 4, the liquid rolling rate is 85%, and the padding is two dipping and two rolling; then pre-baking at 90° C. for 2 minutes, and then washing at 150° C. for 3 minutes, then washing and drying to obtain the product.

Anti-wrinkle anti-bacterial anti-ultraviolet test report of the above example

            Anti-wrinkle properties   Antibacterial properties   Anti-ultraviolet properties example Wrinkle recovery angle/° Anti-wrinkle improvement rate/% Staphylococcus aureus inhibition zone/mm UPF value TUVA/% TUVB/% UPF rating As-is Example 1 Comparative Example 1 Comparative Example 2   252304279260 20.6310.713.17 08.54.51.0 22.0253.7232.1842.78 11.925.868.857.76 2.161.081.651.39 20503045

Test Methods:

1. Determination of fabric wrinkle resistance (wrinkle recovery angle):

Referring to the GB/T3819-83 standard, cut the finished fabric into five convex samples in the warp and five weft directions, and measure it on the YG(B)541D-II automatic digital fabric crease elasticity meter. Measure the longitude and latitude five times, and take the average value.

2. Fabric anti-ultraviolet effect (ultraviolet transmittance) test:

According to the Australian/New Zealand standard (AS/NZS 4399), it is tested by the US Labsphere UV transmission and protection performance tester.

3. Antibacterial performance test

Bacteria: Staphylococcus aureus

The standard formulation of the culture medium:

Beef extract 0.3g

Peptone 1.0g

Sodium chloride 0.5g

Agar 3g

Water 100mL

pH 7.6

Wash the Petri dishes, pipettes and test tubes, wrap them in newspaper and sterilize them in an oven at 160°C for two hours. Accompany the medium according to the standard formula, heat to dissolve, and stir constantly, and then sterilize it in a high-temperature and high-pressure sterilizer for 20 minutes. Cool the culture medium to 50°C, divide it into petri dishes, and ensure that the culture medium covers the bottom of the culture dish. Pipette the diluted bacteria on the culture medium in a sterile environment to ensure that the bacteria cover the culture medium. The finished silk fabric was cut into a circle with a diameter of 10 mm, placed on the bacterial culture medium, and the petri dish was placed in an incubator at 37° C. for 24 hours.

Claims (5)

1. anti-creasing anti-bacterial anti-violet composite function silk fabric is characterized in that: adopt following method to make:

(1) preparation fibroin Nano sol creasing anti-bacterial anti UV finishing agent:

A liquid preparation:, make the fibroin hydrolyzate with the useless silk of sodium hydroxide hydrolysis;

B liquid preparation: get butyl titanate, glacial acetic acid adds deionized water, be added in the hydrochloric acid solution after stirring, behind the peptization, cooling and aging, nano titanic oxide sol;

Composite: it is 3～5 that A liquid and B liquid are regulated pH respectively, mix again composite, fibroin Nano sol creasing anti-bacterial anti UV finishing agent that must be stable;

(2) arrangement: silk fabric is put into the agent of fibroin Nano sol creasing anti-bacterial anti UV finishing pad, get product after the drying.

2. anti-creasing anti-bacterial anti-violet composite function silk fabric according to claim 1 is characterized in that: A liquid and B liquid mix when composite in the step (1), and the weight ratio of A liquid and B liquid is 6: 4.

3. the preparation method of an anti-creasing anti-bacterial anti-violet composite function silk fabric is characterized in that: comprise the following steps:

(1) preparation fibroin Nano sol creasing anti-bacterial anti UV finishing agent:

A liquid preparation:, make the fibroin hydrolyzate with the useless silk of sodium hydroxide hydrolysis;

B liquid preparation: get butyl titanate, glacial acetic acid adds deionized water, be added in the hydrochloric acid solution after stirring, behind the peptization, cooling and aging, nano titanic oxide sol;

Composite: it is 3～5 that A liquid and B liquid are regulated pH respectively, mix again composite, fibroin Nano sol creasing anti-bacterial anti UV finishing agent that must be stable;

(2) arrangement: silk fabric is put into the agent of fibroin Nano sol creasing anti-bacterial anti UV finishing pad, get product after the drying.

4. the preparation method of a kind of anti-creasing anti-bacterial anti-violet composite function silk fabric according to claim 3, it is characterized in that: in the step (1), when A liquid prepares, concentration sodium hydroxide is 1～5mol/L, the waste silk consumption is 1～5g, sodium hydroxide concentration is 50～250ml, and hydrolysis temperature is 70 ℃, and hydrolysis time is 1～2 hour; When B liquid prepares, get butyl titanate 3.5-35g, glacial acetic acid 0.6-6ml, add the 10-100ml deionized water with magnetic stirrer evenly after, it is added drop-wise in the hydrochloric acid solution of 40ml0.1mol/L concentration, simultaneously 20 ℃ of following constant temperature magnetic agitation after 30 minutes, be warming up to 40 ℃ of continuation stirrings and made it peptization in 40 minutes, take out the nature cooling and aging, get nano titanic oxide sol; When composite, the weight ratio of A liquid and B liquid is 6: 4 with A liquid and B liquid.

5. according to the preparation method of claim 3 or 4 described a kind of anti-creasing anti-bacterial anti-violet composite function silk fabrics, it is characterized in that: the concrete grammar of step (2) is: silk fabric is put into fibroin Nano sol creasing anti-bacterial anti UV finishing agent working solution pad, pick-up rate is 85%, and padding is two to soak two and roll; 90 ℃ of following preliminary dryings 2 minutes, under 120～160 ℃, bake again and handled 3～4 minutes then, wash then, dry product.