CN113338037B - Preparation method of two-layer structure noctilucent cotton cloth - Google Patents

Abstract

The invention discloses two-layer structure noctilucent cotton cloth and a preparation method thereof. Cotton cloth, water-resistant noctilucent powder and double-bond mixed silane coupling agent are used as main raw materials. The method comprises the following steps: preparation of cotton cloth containing an initiator, (2) preparation of double-bond mixed silane coupling agent grafted cotton cloth, and (3) preparation of noctilucent cotton cloth. The method has the advantages of simple process, easy operation, no need of expensive instruments and easy popularization, and the prepared two-layer structure noctilucent cotton cloth has very good noctilucent stability and washing fastness and has wide application value in the fields of noctilucent fabrics and the like.

Description

A kind of preparation method of two-layer structure luminous cotton cloth

technical field

The invention relates to the fields of material preparation and polymer modification, in particular to a preparation method of a two-layer structure luminous cotton cloth.

Background technique

At present, many countries mandate that some jobs need to wear clothes with luminous emission function. More and more people who like to exercise at night like to buy clothes with luminous effect, and the market for luminous clothing is growing. This kind of luminous light mainly comes from luminous fabrics made of luminous powder, so the development of luminous fabrics with excellent performance is the goal of some textile enterprises and has broad market prospects. According to domestic and foreign patents and luminous fabric market research, our team found that most of the luminous fabrics are melt-spun luminous powder and fibers to make luminous fibers and then blended or directly coated with luminous powder sauce on the fabric. Made, and most of them use polymer binders. The luminous fabrics prepared by such methods often have disadvantages such as not being washable, relatively hard to the touch, short service life, large differences in luminous performance between batches during mass production, etc., and fail to effectively meet market demand.

Aiming at the defects of luminous fabrics in the existing market, this invention cleverly forms a double-layer structure on the fiber surface through the innovative method of initiator adsorption-chemical grafting-luminous powder immobilization, so that the fabric can retain its original softness and hardness while endowing it with Excellent characteristics of washing resistance, uniform and stable luminescence.

Contents of the invention

The purpose of the present invention is to overcome some deficiencies in the prior art, and provides a preparation method of a two-layer structure luminous cotton cloth, which is simple in process, easy to operate, does not require expensive instruments, and is easy to popularize. The prepared two-layer structure luminous cotton cloth has Very good luminous stability and washing fastness, it has wide application value in luminous fabrics and other fields.

To achieve the above object, the present invention adopts the following technical solutions:

A method for preparing luminous cotton cloth with a two-layer structure, which uses cotton cloth, water-resistant luminous powder and a double bond-containing mixed silane coupling agent as main raw materials.

A preparation method of a two-layer structure luminous cotton cloth, comprising the following steps:

(1) Preparation of cotton cloth containing initiator

Immerse the cotton cloth in the organic solution containing the initiator, and finally take it out and dry it under vacuum to obtain the cotton cloth containing the initiator;

(2) Preparation of grafted cotton cloth containing double bond mixed silane coupling agent

Put the cotton cloth containing the initiator into the reactor with mixed solvent, add the double bond-containing mixed silane coupling agent monomer, remove the air, then raise the temperature to 60-75°C for 1-12h, then stir, wash, and dry After that, the cotton cloth surface-modified by the silane coupling agent is obtained;

(3) Preparation of luminous cotton cloth

Immerse the prepared cotton cloth surface-modified by the silane coupling agent into an aqueous solution of water-resistant luminous powder with a pH of 2-5 and stir at 70-90°C for reaction, and wash and vacuum-dry the obtained cotton cloth to obtain a two-layer structure luminous cotton cloth ( That is, luminous powder grafted cotton cloth).

In step (1), the initiator is azobisisobutyronitrile (AIBN) or dibenzoyl peroxide. The solvent of the organic solution containing the initiator is ethanol.

The immersion time is 20-60 minutes, preferably 30 minutes.

In step (2), the mixed solvent is prepared by using an organic solvent and water in a volume ratio of 7-11:1 (preferably a volume ratio of 9:1).

The organic solvent is one of ethanol, methanol, toluene or ethyl acetate.

Described double bond-containing mixed silane coupling agent monomer is KH570 (gamma-methacryloxypropyltrimethoxysilane), KH-A172 (vinyltrimethoxysilane), A171 (vinyltri( b-Methoxyethoxy) silane) and A151 (vinyltriethoxysilane) are used in combination, and the mixing volume ratio is (V/V)2/8～8/2.

The ratio of the amount of the mixed solvent to the double bond-containing mixed silane coupling agent monomer is 10-50ml: 1-5g. The most preferred ratio is 30ml: 3g.

Exclude air with nitrogen or inert gas.

More preferably, the temperature is raised to 65-70° C. for 1-12 hours.

The conditions for stirring and cleaning are as follows: stirring and cleaning the cotton cloth 2-3 times at 65-75°C,

The agitation and cleaning uses deionized water.

Dry by air drying.

In step (3), the particle size (nm) of the luminous powder in the water-resistant luminous powder aqueous solution is 10-500, more preferably 220-420.

The reaction time of the stirring reaction is 1 to 6 hours.

Compared with prior art, the present invention has following advantage:

The invention uses cotton cloth, luminous powder of suitable size and silane coupling agent containing double bonds as main raw materials to prepare luminous cotton cloth of suitable size. The process of the invention is simple, easy to operate, does not require expensive instruments, and is easy to popularize. The prepared two-layer structure luminous cotton cloth has very good luminous stability and washing fastness, and has wide application value in the fields of luminous fabrics and the like.

The luminous powder immobilized with the silane coupling agent cotton cloth successfully prepared by the invention realizes the self-cleaning performance of the cotton cloth and improves the pollution resistance and stability of the cotton cloth. The two-layer structure luminous cotton cloth prepared by the method has the following advantages: (1) has a water resistance of more than 10 times and a stability of 90%; (2) has a luminous emitting ability of more than 3 hours; (3) has excellent stability; (4) The process is simple, easy to operate, cheap in equipment and easy to popularize.

Description of drawings

Fig. 1 is the weight gain (%) after grafting of the two-layer structure luminous cotton cloth of embodiment 1～6.

Fig. 2 is the weight gain (%) of the two-layered luminous cotton cloth luminous powder of Examples 1-6 after being immobilized.

Fig. 3 is the weight loss (%) of the two-layer structure luminescent cotton cloth of Examples 1-6 after 10 times of washing.

Detailed ways

The preparation method of luminous cotton cloth of the present invention comprises the following processes:

(1) Preparation of cotton cloth containing initiator

The cotton cloth is immersed in the ethanol solution containing the initiator, and finally taken out and dried in vacuum to obtain the cotton cloth containing the initiator.

(2) Preparation of silane coupling agent grafted cotton cloth

Put the cotton cloth containing the initiator into the reaction bottle containing the mixed solution of methanol and water, and add the mixed silane coupling agent; ventilate nitrogen to remove the air, then raise the temperature to 65-70°C for 1-12 hours; use deionized water Stir and wash the reacted cotton cloth for 2 to 3 times at 65-70° C., and dry to obtain the cotton cloth grafted with the silane coupling agent.

(3) Preparation of two-layer structure luminous cotton cloth

Immerse the prepared silane coupling agent grafted cotton cloth into a solution of suitable size luminous powder and stir for a certain period of time. The obtained cotton cloth is washed and vacuum-dried to obtain a luminous cotton cloth of suitable size.

The following are several specific examples of the present invention, which are further descriptions of the present invention.

Example 1

1) Preparation of cotton cloth containing AIBN initiator: take 4 g of cotton cloth and immerse it in the ethanol solution of AIBN for 30 minutes, take it out and dry it under vacuum at room temperature to obtain the cotton cloth containing initiator.

2) Graft coupling agent on the surface of cotton cloth: put 3 pieces of cotton cloth (3cm×3cm) containing AIBN into a three-necked flask filled with 30ml of ethanol and water mixed solution (9/1 volume ratio), and add 3g of KH570 and Mixed reagent of KH-A172 (2/8 volume ratio). Nitrogen was passed for 30 minutes to remove the air, and then the flask was moved into a 70° oil bath to react for 1 hour. Stir and wash the reacted cotton cloth with deionized water at 70° C. for 3 times, and dry to obtain the cotton cloth grafted with the coupling agent.

3) Preparation of luminous cotton cloth: immerse the prepared coupling agent-grafted cotton cloth into a solution of green luminous powder with an average particle size of 420nm and a pH of 2.0, stir at 80°C for 4 hours, take it out, wash and dry it several times, and test the solidity of the luminous powder. Weight gain of cotton cloth after loading.

4) Excite the obtained luminous cotton cloth under the ultraviolet light and turn off the ultraviolet light to take pictures of the uniformity of the luminous emission and record the luminous duration. Calculate the weight loss of cotton cloth after 10 standard washings of luminous cloth.

After the silane modification, the weight of the cotton cloth increased by 4.53%, and after the luminous powder was immobilized, the weight of the grafted cotton cloth increased by 19.45%, and the luminous power lasted for 3.5 hours. After 10 times of washing, the weight of the cotton cloth was reduced by 2.61%, and the luminous duration remained at 3.5 hours.

Example 2

1) Preparation of cotton cloth containing AIBN initiator: take 4 g of cotton cloth and immerse it in the ethanol solution of AIBN for 30 minutes, take it out and dry it under vacuum at room temperature to obtain the cotton cloth containing initiator.

2) Graft coupling agent on the surface of cotton cloth: put 3 pieces of cotton cloth (3cm×3cm) containing AIBN into a three-necked flask filled with 30ml of ethanol and water mixed solution (9/1 volume ratio), and add 3g of KH- A mixed reagent of A172 and KH570 (3/7 volume ratio). Nitrogen was passed for 30 minutes to remove the air, and then the flask was moved into a 70° oil bath to react for 1 hour. Stir and wash the reacted cotton cloth with deionized water at 70° C. for 3 times, and dry to obtain the cotton cloth grafted with the coupling agent.

3) Preparation of luminous cotton cloth: immerse the prepared coupling agent-grafted cotton cloth into a solution of green luminous powder with an average particle size of 420nm and a pH of 3.0, stir at 80°C for 4 hours, take it out, wash and dry it several times, and test the solidity of the luminous powder. Weight gain of cotton cloth after loading.

4) Excite the obtained luminous cotton cloth under the ultraviolet light and turn off the ultraviolet light to take pictures of the uniformity of the luminous emission and record the luminous duration. Test the wash fastness of the luminous cloth after 10 standard washes.

The weight gain of cotton cloth after silane modification was 5.12%, and the weight gain of grafted cotton cloth after luminous powder was fixed was 17.59%. After 10 times of washing, the cotton cloth lost 3.98% of its weight, and the luminous duration remained at 3.5 hours.

Example 3

1) Preparation of cotton cloth containing AIBN initiator: take 4 g of cotton cloth and immerse it in the ethanol solution of AIBN for 30 minutes, take it out and dry it under vacuum at room temperature to obtain the cotton cloth containing initiator.

2) Graft coupling agent on the surface of cotton cloth: put 3 pieces of cotton cloth (3cm×3cm) containing AIBN into a three-necked flask filled with 30ml of ethanol and water mixed solution (9/1 volume ratio), and add 3g of A171 and Mixed reagent of KH-A172 (5/5 volume ratio). Nitrogen was passed for 30 minutes to remove the air, and then the flask was moved into a 70° oil bath to react for 1 hour. Stir and wash the reacted cotton cloth with deionized water at 70° C. for 3 times, and dry to obtain the cotton cloth grafted with the coupling agent.

3) Preparation of luminous cotton cloth: immerse the prepared coupling agent-grafted cotton cloth into a solution of green luminous powder with an average particle size of 420nm and a pH of 2.5, stir at 80°C for 4 hours, take it out, wash and dry it several times, and test the solidity of the luminous powder. Weight gain of cotton cloth after loading.

4) Excite the obtained luminous cotton cloth under the ultraviolet light and turn off the ultraviolet light to take pictures of the uniformity of the luminous emission and record the luminous duration. Test the wash fastness of the luminous cloth after 10 standard washes.

After silane modification, the weight of the cotton cloth increased by 3.4%, and after the luminous powder was immobilized, the weight of the grafted cotton cloth increased by 18.67%. After 10 times of washing, the weight of the cotton cloth is reduced by 2.9%, and the luminous duration remains at 3.5 hours.

Example 4

1) Preparation of cotton cloth containing AIBN initiator: Take 4 g of cotton cloth and immerse it in the ethanol solution of azobisisoheptane for 30 minutes, take it out and dry it under vacuum at room temperature to obtain the cotton cloth containing the initiator.

2) Graft coupling agent on the surface of cotton cloth: put 3 pieces of cotton cloth (3cm×3cm) containing AIBN into a three-necked flask filled with 30ml of ethanol and water mixed solution (9/1 volume ratio), and add 3g of A151 and Mixed reagent of KH570 (6/4 volume ratio). Nitrogen was passed for 30 minutes to remove the air, and then the flask was moved into a 65° oil bath to react for 1 hour. Stir and wash the reacted cotton cloth with deionized water at 70° C. for 3 times, and dry to obtain the cotton cloth grafted with the coupling agent.

3) Preparation of luminous cotton cloth: immerse the prepared coupling agent-grafted cotton cloth into a solution of green luminous powder with an average particle size of 420nm and a pH of 3.0, stir at 80°C for 4 hours, take it out, wash and dry it several times, and test the solidity of the luminous powder. Weight gain of cotton cloth after loading.

4) Excite the obtained luminous cotton cloth under the ultraviolet light and turn off the ultraviolet light to take pictures of the uniformity of the luminous emission and record the luminous duration. Test the wash fastness of the luminous cloth after 10 standard washes.

The weight gain of cotton cloth after silane modification was 6.13%, and the weight gain of grafted cotton cloth after luminous powder was fixed was 20.12%. After 10 times of washing, the weight of the cotton cloth is reduced by 1.46%, and the luminous duration remains at 4 hours.

Example 5

1) Preparation of cotton cloth containing azobisisoheptane hair agent: take 4 g of cotton cloth and immerse it in the ethanol solution of azobisisoheptane for 30 minutes, take it out and dry it under vacuum at room temperature to obtain the cotton cloth containing initiator.

2) Graft coupling agent on the surface of cotton cloth: put 3 pieces of cotton cloth (3cm×3cm) containing azobisisoheptane into a three-necked flask containing 30ml of ethanol and water mixed solution (9/1 volume ratio), and Add 3g of KH570 and A151 mixed reagent (5/5 volume ratio). Nitrogen was passed for 30 minutes to remove the air, and then the flask was moved into a 70° oil bath to react for 1 hour. Stir and wash the reacted cotton cloth with deionized water at 70° C. for 3 times, and dry to obtain the cotton cloth grafted with the coupling agent.

3) Preparation of luminous cotton cloth: immerse the prepared coupling agent-grafted cotton cloth into a solution of green luminous powder with an average particle size of 220nm and a pH of 3.0, stir at 85°C for 4 hours, take it out, wash and dry it several times, and test the solidity of the luminous powder. Weight gain of cotton cloth after loading.

4) Excite the obtained luminous cotton cloth under the ultraviolet light and turn off the ultraviolet light to take pictures of the uniformity of the luminous emission and record the luminous duration. Test the wash fastness of the luminous cloth after 10 standard washes.

The weight gain of cotton cloth after silane modification was 5.63%, and the weight gain of grafted cotton cloth after luminous powder was fixed was 24.59%. After 10 times of washing, the weight of the cotton cloth is reduced by 4.22%, and the luminous duration remains at 3.5 hours.

Example 6

1) Preparation of cotton cloth containing azobisisoheptane initiator: Take 4 g of cotton cloth and immerse it in the ethanol solution of azobisisoheptane for 30 minutes, take it out and dry it under vacuum at room temperature to obtain the cotton cloth containing the initiator.

2) Graft coupling agent on the surface of cotton cloth: put 3 pieces of cotton cloth (3cm×3cm) containing azobisisoheptane into a three-necked flask containing 30ml of ethanol and water mixed solution (9/1 volume ratio), and Add 3 g of KH570 and A151 mixed reagent (7/3 volume ratio). Nitrogen was passed for 30 minutes to remove the air, and then the flask was moved into a 70° oil bath to react for 1 hour. Stir and wash the reacted cotton cloth with deionized water at 70° C. for 3 times, and dry to obtain the cotton cloth grafted with the coupling agent.

3) Preparation of luminous cotton cloth: immerse the prepared coupling agent-grafted cotton cloth into a solution of green luminous powder with an average particle size of 220nm and a pH of 4.0, stir at 75°C for 4 hours, take it out, wash and dry it several times, and test the solidity of the luminous powder. Weight gain of cotton cloth after loading.

4) Excite the obtained luminous cotton cloth under the ultraviolet light and turn off the ultraviolet light to take pictures of the uniformity of the luminous emission and record the luminous duration. Test the wash fastness of the luminous cloth after 10 standard washes.

After silane modification, the weight of cotton cloth increased by 4.37%, and after the luminous powder was immobilized, the weight of grafted cotton cloth increased by 22.1%. After 10 times of washing, the cotton cloth lost 2.4% of its weight, and the luminous duration remained at 4 hours.

The above descriptions are only preferred embodiments of the present invention, and all equivalent changes and modifications made according to the scope of the patent application of the present invention shall fall within the scope of the present invention.

Claims (8)

1. A preparation method of two-layer structure noctilucent cotton cloth is characterized by comprising the following steps:

(1) Soaking cotton cloth into organic solution containing initiator, and vacuum drying to obtain cotton cloth containing initiator;

the initiator is azobisisobutyronitrile or dibenzoyl peroxide;

(2) Placing cotton cloth containing an initiator into a reactor filled with a mixed solvent, adding a double-bond-containing mixed silane coupling agent monomer, removing air, heating to 60-75 ℃ for reaction for 1-12h, stirring, cleaning, and drying to obtain the cotton cloth with the surface modified by the silane coupling agent;

the double-bond mixed silane coupling agent monomer is two of gamma-methacryloxypropyltrimethoxysilane, vinyl trimethoxysilane, vinyl tri (b-methoxyethoxy) silane and vinyl triethoxysilane which are mixed for use, and the volume ratio of the mixture is 2/8-8/2;

(3) Soaking the prepared cotton cloth with the surface modified by the silane coupling agent into a noctilucent powder aqueous solution with the pH value of 2-5, stirring and reacting at 70-90 ℃, and washing and vacuum drying the obtained cotton cloth to obtain the noctilucent cotton cloth with the two-layer structure;

the grain diameter of the noctilucent powder in the noctilucent powder aqueous solution is 10-500 nm.

2. The method for preparing the two-layer noctilucent cotton cloth according to claim 1, wherein in the step (1), the solvent of the organic solution containing the initiator is ethanol.

3. The method for preparing the two-layer noctilucent cotton cloth according to claim 1, wherein in the step (1), the immersion time is 20-60 min.

4. The preparation method of the two-layer noctilucent cotton cloth according to claim 1, wherein in the step (2), the volume ratio of the mixed solvent is 7-11: 1 and water;

the organic solvent is one of ethanol, methanol, toluene or ethyl acetate.

5. The preparation method of two-layer noctilucent cotton cloth according to claim 1, wherein in the step (2), the ratio of the amount of the mixed solvent to the amount of the double-bond-containing mixed silane coupling agent monomer is 10-50 ml: 1-5 g.

6. The method for preparing the two-layer noctilucent cotton cloth according to claim 1, wherein in the step (2), the temperature is raised to 65-70 ℃ for reaction for 1-12h.

7. The method for preparing the two-layer noctilucent cotton cloth according to claim 1, wherein in the step (2), the stirring and cleaning conditions are as follows: and stirring and cleaning the cotton cloth after reaction for 2-3 times at 65-75 ℃, wherein deionized water is adopted for stirring and cleaning.

8. The method for preparing the two-layer noctilucent cotton cloth according to claim 1, wherein in the step (3), the reaction time of the stirring reaction is 1-6 hours.

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