CN110820325A - Preparation method and antibacterial finishing method of antibacterial sol for shoemaking - Google Patents
Preparation method and antibacterial finishing method of antibacterial sol for shoemaking Download PDFInfo
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- CN110820325A CN110820325A CN201911269284.3A CN201911269284A CN110820325A CN 110820325 A CN110820325 A CN 110820325A CN 201911269284 A CN201911269284 A CN 201911269284A CN 110820325 A CN110820325 A CN 110820325A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with organometallic compounds; with organic compounds containing boron, silicon, selenium or tellurium atoms
- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
Abstract
The invention provides a preparation method and an antibacterial finishing method of antibacterial sol for shoemaking, which comprises the following steps: TEOS is used as a precursor, EtOH is used as a solvent, and HNO is selected3Adding a certain amount of GPTMS and TH as a catalyst, electrically stirring for 5h at the hydrolysis temperature of 30 ℃, and standing for a period of time at room temperature to prepare transparent antibacterial sol; performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabrics in the transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a rod pressing mode, and removing redundant transparent antibacterial sol; compared with the prior art, the invention adopts a two-soaking two-rolling process with the rolling residual rate of 70-80 percent, under the conditions of the soaking time of 10s, the pre-drying temperature of 130 ℃, the pre-drying time of 2.5min, the baking temperature of 190 ℃ and the baking time of 40s,the shoe material has good bacteriostatic effect on candida albicans and trichophyton rubrum, and the bacteriostatic rate is more than 90%.
Description
Technical Field
The invention relates to the technical field of shoemaking antibiosis, in particular to a preparation method and an antibacterial finishing method of an antibacterial sol for shoemaking.
Background
Shoes are a necessity of daily life. Along with the development of society and the improvement of living standard of people, the requirements of people on the comfort and the sanitation of shoes and boots are higher and higher. In recent years, the industries of antibacterial agents and antibacterial fabrics gradually mature, and international and domestic scholars try to apply the antibacterial agents and the antibacterial fabrics to shoe and boot products, so that a batch of antibacterial agents and antibacterial shoe materials for shoes are also emerged in the market.
Although the shoe antibacterial materials are developed on the market at present, the application of the antibacterial agent in the shoe products still has many defects. For example, most of the existing antibacterial shoe materials show good antibacterial effect on typical bacteria such as escherichia coli, staphylococcus aureus and the like, but have no obvious effect on fungi which really cause foot diseases. The silver antibacterial agent easily causes the color change of the base material under the illumination condition, and influences the aesthetic feeling of the appearance of the shoe material. In addition, antimicrobial durability and antimicrobial washability are likewise unsolved challenges in antimicrobial footwear.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a preparation method and an antibacterial finishing method of the antibacterial sol for shoemaking starting from solving the problems of the stability of the antifungal sol and the production of the antifungal shoe material.
The invention provides a preparation method and an antibacterial finishing method of antibacterial sol for shoemaking, which comprises the following steps:
(1) TEOS (tetraethyl orthosilicate) is used as a precursor, EtOH (absolute ethyl alcohol) is used as a solvent, and HNO is selected3Adding a certain amount of GPTMS (gamma-glycidoxypropyltrimethoxysilane) and TH (terbinafine hydrochloride) as a catalyst, electrically stirring for 5 hours at the hydrolysis temperature of 30 ℃, and standing for a period of time at room temperature to prepare transparent antibacterial sol;
(2) the lining cloth for the shoes is subjected to antibacterial finishing by adopting a padding finishing process, the fabric is soaked in the transparent antibacterial sol for a certain time, the transparent antibacterial sol is pressed into gaps among the fabrics in a rod pressing mode, and meanwhile, the redundant transparent antibacterial sol is removed.
Further, the optimization process of the step (1) is as follows: according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; and secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving uniformly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred electrically for 5 hours in a water bath at the constant temperature of 30 ℃, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare the transparent antibacterial sol.
Further, the padding finishing process in the step (2) comprises the processes of pre-drying, baking, washing and hanging for airing.
Further, the padding finishing process can be divided into various forms of one-dipping one-rolling, one-dipping two-rolling, two-dipping two-rolling and more-dipping one-rolling.
Furthermore, the pre-drying temperature of the padding finishing process is 100-140 ℃, the pre-drying time is 2-4 min, the baking temperature is 180-220 ℃, the baking time is 10-50 s, and the dipping time is 5-25 s.
Compared with the prior art, the preparation method and the antibacterial finishing method of the antibacterial sol for shoemaking provided by the invention have the advantages that when n (TEOS): n (H)2O): n (etoh) ═ 1: 30: 10, n (teos): n (gptms) ═ 6: 1, the prepared sol has good transparency and is stable, and the lower the aging temperature is, the smaller and more stable the viscosity change of the sol is; by adopting a two-dipping two-rolling process with the rolling residual rate of 70-80%, under the conditions of 10s of dipping time, 130 ℃ of pre-drying temperature, 2.5min of pre-drying time, 190 ℃ of baking temperature and 40s of baking time, the shoe material has good bacteriostatic effect on candida albicans and trichophyton rubrum, and the bacteriostatic rate is more than 90%.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
Example one
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for even dissolution, the mixture is added into the mixed solution prepared in the previous step, and the mixture is stirred electrically for 5 hours in a water bath at the constant temperature of 30 DEG CPlacing the mixture at 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) the method comprises the steps of performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 110 ℃, the pre-drying time is 3min, the baking temperature is 190 ℃, the baking time is 30s, and the soaking time is 15 s.
Example two
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving evenly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred for 5 hours in a water bath at the constant temperature of 30 ℃ and in an electric mode, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) the method comprises the steps of performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 120 ℃, the pre-drying time is 3min, the baking temperature is 190 ℃, the baking time is 30s, and the soaking time is 15 s.
EXAMPLE III
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting the pH to 2, 30Stirring at deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving evenly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred for 5 hours in a water bath at the constant temperature of 30 ℃ and in an electric mode, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) the method comprises the steps of performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the prebaking temperature is 130 ℃, the prebaking time is 3min, the baking temperature is 190 ℃, the baking time is 30s, and the soaking time is 15 s.
Example four
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving evenly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred for 5 hours in a water bath at the constant temperature of 30 ℃ and in an electric mode, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) the method comprises the steps of performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 140 ℃, the pre-drying time is 3min, the baking temperature is 190 ℃, the baking time is 30s, and the soaking time is 15 s.
EXAMPLE five
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O)：n(EtOH): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving evenly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred for 5 hours in a water bath at the constant temperature of 30 ℃ and in an electric mode, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) the method comprises the steps of performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 120 ℃, the pre-drying time is 3.5min, the baking temperature is 190 ℃, the baking time is 30s, and the soaking time is 15 s.
EXAMPLE six
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving evenly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred for 5 hours in a water bath at the constant temperature of 30 ℃ and in an electric mode, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) the method comprises the steps of performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 120 ℃, the pre-drying time is 4min, the baking temperature is 190 ℃, the baking time is 30s, and the soaking time is 15 s.
EXAMPLE seven
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving evenly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred for 5 hours in a water bath at the constant temperature of 30 ℃ and in an electric mode, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) the method comprises the steps of performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 120 ℃, the pre-drying time is 3min, the baking temperature is 180 ℃, the baking time is 30s, and the soaking time is 15 s.
Example eight
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving evenly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred for 5 hours in a water bath at the constant temperature of 30 ℃ and in an electric mode, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) carrying out antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics by adopting a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 120 ℃, the pre-drying time is 3min, the baking temperature is 200 ℃, the baking time is 30s, and the soaking time is 15 s.
Example nine
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving evenly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred for 5 hours in a water bath at the constant temperature of 30 ℃ and in an electric mode, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) the method comprises the steps of performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 120 ℃, the pre-drying time is 3min, the baking temperature is 190 ℃, the baking time is 20s, and the soaking time is 15 s.
Example ten
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving evenly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred for 5 hours in a water bath at the constant temperature of 30 ℃ and in an electric mode, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) the method comprises the steps of performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 120 ℃, the pre-drying time is 3min, the baking temperature is 190 ℃, the baking time is 10s, and the soaking time is 15 s.
EXAMPLE eleven
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving evenly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred for 5 hours in a water bath at the constant temperature of 30 ℃ and in an electric mode, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) the method comprises the steps of performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 120 ℃, the pre-drying time is 3min, the baking temperature is 190 ℃, the baking time is 40s, and the soaking time is 15 s.
Example twelve
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for even dissolution, the mixture is added into the mixed solution prepared in the previous step, and the mixture is stirred electrically in a water bath at the constant temperature of 30 DEG C5h, placing the mixture at 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) the method comprises the steps of performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 120 ℃, the pre-drying time is 3min, the baking temperature is 190 ℃, the baking time is 30s, and the soaking time is 5 s.
EXAMPLE thirteen
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving evenly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred for 5 hours in a water bath at the constant temperature of 30 ℃ and in an electric mode, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) the method comprises the steps of performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 120 ℃, the pre-drying time is 3min, the baking temperature is 190 ℃, the baking time is 30s, and the soaking time is 10 s.
Example fourteen
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting the pH toStirring at 2, 30 ℃ electrically to prepare a mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving evenly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred for 5 hours in a water bath at the constant temperature of 30 ℃ and in an electric mode, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) the method comprises the steps of performing antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, pressing the transparent antibacterial sol into gaps among the fabrics in a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 120 ℃, the pre-drying time is 3min, the baking temperature is 190 ℃, the baking time is 30s, and the soaking time is 20 s.
Example fifteen
A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving evenly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred for 5 hours in a water bath at the constant temperature of 30 ℃ and in an electric mode, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare transparent antibacterial sol;
(2) carrying out antibacterial finishing on the lining cloth for the shoes by adopting a padding finishing process, soaking the fabric in transparent antibacterial sol for a certain time, then padding once again, pressing the transparent antibacterial sol into gaps among the fabrics by adopting a stick pressing mode, removing redundant transparent antibacterial sol, and finally detecting the antibacterial performance of a sample, wherein the pre-drying temperature is 120 ℃, the pre-drying time is 3min, the baking temperature is 190 ℃, the baking time is 30s, and the soaking time is 15 s.
The first, second, third and fourth examples show that the antibacterial effect of the fabric is greatly influenced in the pre-drying process. The pre-baking can diffuse the antibacterial sol into the fiber on one hand, and evaporate the water in the fiber on the other hand, thereby being beneficial to subsequent processing. After the fabric is soaked in the antibacterial sol for a certain time, part of the antibacterial sol permeates into the fibers and part of the antibacterial sol is distributed among the fibers, and the antibacterial sol can be better diffused into the fibers in the pre-drying process. The pre-baking can prevent the phenomena that the antibacterial sol absorbed by the fabric fiber migrates to the surface of the fabric at an excessively high baking temperature, so that the antibacterial sol is gathered and cannot be well attached to a shoe material, and the antibacterial rate is low and the antibacterial durability is not enough. When the pre-drying temperature is 120 ℃, the bacteriostatic rate of the shoe material on candida albicans is the highest, and then the bacteriostatic rate is balanced after being sharply reduced along with the rise of the temperature. The reason is that when the pre-drying temperature is lower and the same time is used, the antibacterial sol soaked on the shoe material cannot be completely deposited in the fiber, and when the high-temperature baking is carried out, part of the sol migrates to the surface of the fabric, so that the bacteriostasis rate is not high; when the pre-drying temperature is higher than 120 ℃, the antibacterial sol can rapidly migrate to the surface of the fabric along with moisture to generate accumulation, so that the antibacterial sol attached to the shoe material is less, and then the sol migrated to the surface is washed by water to fall off, so that the bacteriostasis rate is reduced.
The second, fifth and sixth embodiments show that the pre-drying process can promote the antibacterial sol to enter the fiber on one hand, and can also make part of the sol migrate to the surface of the fiber on the other hand. At the same pre-drying temperature, the more water on the fabric evaporates with the increase of time, the more and more antibacterial sol migrates to the surface of the fabric along with the water, so that a large amount of sol is aggregated to form gel on the surface of the fiber and falls off in the washing process, thereby reducing the bacteriostasis rate of the antibacterial sol. At the pre-drying temperature of 120 ℃, the pre-drying time is before 3.5min, the bacteriostasis rate continuously rises, and reaches the maximum value at 3.5min, and then the bacteriostasis rate sharply drops, which shows that more and more antibacterial sol enters the fiber before 3.5min, and when the time exceeds 3.5min, the antibacterial sol migrates and gathers to the fiber surface along with the volatilization amount of the water in the fabric, so that the amount of the antibacterial sol gathered on the fiber surface is gradually larger than the amount of the antibacterial sol entering the fiber, and the bacteriostasis rate of the fabric sharply drops.
The second, seventh and eighth embodiments show that the baking can make the fiber expand by heating, accelerate the diffusion of part of the ungelled antibacterial sol to the fiber, and make the antibacterial sol and the fiber generate chemical crosslinking reaction, so that the antibacterial sol and the cotton fiber are combined in a chemical bond manner, thereby improving the combining fastness between the antibacterial sol and the fiber. When the baking temperature reaches 190 ℃, the bacteriostasis rate of the shoe material reaches the maximum, which shows that the antibacterial sol and the cotton fiber are subjected to stable chemical crosslinking at 190 ℃. With the rise of the baking temperature, the bacteriostasis rate of the shoe material is sharply reduced, and DSC experiments show that the antibacterial component is sharply decomposed at the high temperature of 200 ℃. As the cotton fabric is easy to yellow under the condition of high temperature, when the shoe material is baked at the temperature of 200 ℃, the material is seriously yellow and not beautiful, and the subsequent use is influenced.
From the second, ninth, tenth and eleventh examples, when the baking time is less than 30s, the bacteriostasis rate is significantly increased with the extension of the baking time, which indicates that the efficiency of the antibacterial sol is gradually increased, and then, the bacteriostasis rate is sharply decreased with the extension of the baking time, because the antibacterial component is decomposed in part of the sol under the condition of high temperature for a long time.
The second, twelfth, thirteenth and fourteenth embodiments show that the bacteriostasis rate is gradually increased along with the increase of the dipping time, but the difference is not great, and the bacteriostasis rate is gradually increased when the dipping time is between 5s and 15s, because the shoe material is gradually soaked in the antibacterial sol along with the increase of the dipping time; when the dipping time is more than 15s, the bacteriostasis rate is basically consistent, because when the dipping time is 15s, the shoe material is basically soaked, the antibacterial sol in the fiber is basically saturated, and the antibacterial sol is not more attached to the shoe material along with the extension of the dipping time, so the bacteriostasis rate is basically kept unchanged. In addition, industrial production requires that the process flow is simplified as much as possible, the processing time is shortened, and the maximization of production benefit is achieved, so that the optimal soaking time is 10 s.
From the second and fifteenth examples, the bacteriostatic ratio of the candida albicans by the sample prepared by the one-dip one-roll method is 62.76%, and the bacteriostatic ratio of the candida albicans by the sample prepared by the two-dip two-roll method is 96.15%. This is because two-pad padding has a better fabric wetting effect than one-pad padding, and multiple padding allows more finishing liquor to be squeezed into the interstices of the fibers.
The foregoing has described preferred embodiments of the present invention and is not to be construed as limiting the claims. The present invention is not limited to the above embodiments, and the specific structure thereof is allowed to vary, and various changes made within the scope of the independent claims of the present invention are within the scope of the present invention.
Claims (5)
1. A preparation method and an antibacterial finishing method of antibacterial sol for shoemaking comprise the following steps:
(1) TEOS is used as a precursor, EtOH is used as a solvent, and HNO is selected3Adding a certain amount of GPTMS and TH as a catalyst, electrically stirring for 5h at the hydrolysis temperature of 30 ℃, and standing for a period of time at room temperature to prepare transparent antibacterial sol;
(2) the lining cloth for the shoes is subjected to antibacterial finishing by adopting a padding finishing process, the fabric is soaked in the transparent antibacterial sol for a certain time, the transparent antibacterial sol is pressed into gaps among the fabrics in a rod pressing mode, and meanwhile, the redundant transparent antibacterial sol is removed.
2. The preparation method and the antibacterial finishing method of the antibacterial sol for shoemaking according to claim 1, wherein the optimization process of step (1) is as follows: according to n (TEOS): n (H)2O): n (etoh): n (GPTMS) ═ 4 to 8: (150-200): (40-80): (1-5), wherein the EtOH is added in two steps, 2/3 which is the total content of the EtOH is added in the first step, and 65% of HNO is used3Adjusting pH to 2, and stirring at 30 deg.C to obtain mixed solution; and secondly, 0.1mol of TEOS is taken, 0.1g of TH is added, the rest 1/3 of EtOH is used for dissolving uniformly, the mixture is added into the mixed solution prepared in the previous step, the mixture is stirred electrically for 5 hours in a water bath at the constant temperature of 30 ℃, and the mixture is placed at the temperature of 15 ℃ for a period of time to prepare the transparent antibacterial sol.
3. The method for preparing the antibacterial sol for shoemaking and the antibacterial finishing method according to claim 1, wherein the padding finishing process in step (2) comprises pre-baking, washing and hanging and airing processes.
4. The method for preparing the antibacterial sol and the antibacterial finishing method for the shoemaking according to claim 3, wherein the padding finishing process can be divided into a plurality of forms including one-dipping-one-rolling, one-dipping-two-rolling, two-dipping-two-rolling and more-dipping-one-rolling.
5. The preparation method and the antibacterial finishing method of the antibacterial sol for shoemaking according to claim 4, wherein the pre-drying temperature of the padding finishing process is 100-140 ℃, the pre-drying time is 2-4 min, the baking temperature is 180-220 ℃, the baking time is 10-50 s, and the dipping time is 5-25 s.
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| CN112175222A (en) * | 2020-10-13 | 2021-01-05 | 张家港世恒实业有限公司 | Antibacterial processing technology of degradable disposable gloves |
| CN113774670A (en) * | 2021-08-20 | 2021-12-10 | 南通帝沙纺织有限公司 | Preparation method of antibacterial warm-keeping fabric |
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