CN114622412B - Method for preparing sericin finishing spunlaced non-woven fabric through thermal bonding - Google Patents

Method for preparing sericin finishing spunlaced non-woven fabric through thermal bonding Download PDF

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CN114622412B
CN114622412B CN202210199156.1A CN202210199156A CN114622412B CN 114622412 B CN114622412 B CN 114622412B CN 202210199156 A CN202210199156 A CN 202210199156A CN 114622412 B CN114622412 B CN 114622412B
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sericin
powder
solution
chitosan
thermal bonding
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CN114622412A (en
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张芸
施淑波
刘北壬
贺铁强
尹乾麟
严国庆
张军
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Hangzhou Luxian New Materials Technology Co.,Ltd.
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Hangzhou Advanced Nonwoven Co ltd
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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
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/15—Proteins or derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
    • C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
    • C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03—Polysaccharides or derivatives thereof
    • D—TEXTILES; PAPER
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    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02—Natural fibres, other than mineral fibres
    • D06M2101/04—Vegetal fibres
    • D06M2101/06—Vegetal fibres cellulosic
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    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
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    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments

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Abstract

The invention discloses a method for preparing a sericin finishing spunlaced nonwoven fabric by thermal bonding, which comprises the following steps: (1) Mixing sericin powder and hot melt adhesive powder to obtain mixed powder; (2) Applying the mixed powder to the surface of the spunlaced nonwoven fabric by a powder spraying method; (3) And combining the sericin with the spunlaced nonwoven fabric by thermal bonding. The invention uses the hot melt adhesive to bond the silk glue on the surface of the spunlaced non-woven fabric by a hot bonding method, the operation process is simple, the loading amount of the silk glue is easy to control, and the influence of aldehyde cross-linking agents on the health of human bodies is avoided.

Description

Method for preparing sericin finishing spunlaced non-woven fabric through thermal bonding
Technical Field
The invention relates to the field of spunlaced nonwovens, in particular to a method for preparing sericin finishing spunlaced nonwovens by thermal bonding.
Background
The silk mainly comprises an inner silk fibroin and an outer silk sericin, wherein the sericin accounts for 25-30wt% of the inner silk fibroin, and has the effects of protecting and bonding the silk fibroin wrapped in the inner silk fibroin. Sericin is a globular protein, has 18 amino acids composition, and shows good water solubility and water absorbability. For a long time, because of the requirements of silk making and textile technology, sericin is not effectively utilized, but is removed and discharged together with wastewater. However, in recent years, through intensive research on sericin, the sericin has excellent performances such as oxidation resistance, ultraviolet resistance, moisture retention, biocompatibility and the like, and has great application potential in the fields of textile printing and dyeing, chemistry and chemical industry, food, medicine and health, biological materials and the like.
Sericin is loaded on the textile, so that the performances of moisture absorption, moisture preservation, ultraviolet resistance, biocompatibility and the like of the textile can be improved, and the sericin is widely studied. Because the sericin has good solubility, how to improve the washing resistance of the textile after the sericin is finished and reduce the dissolution loss rate of the sericin is a difficult point for modifying the textile by the sericin. In the prior art, a textile is generally finished by sericin through a solution finishing method, and a cross-linking agent is added into finishing liquid, so that the water solubility of the sericin is reduced by utilizing the reaction of the cross-linking agent and sericin, and the sericin is fixed on the surface of the textile in a stable structure, so that the dissolution loss rate of the sericin is reduced.
However, when a solution finishing method is adopted, the loading capacity of the sericin is difficult to control, the raw material utilization rate is low, and the sericin waste is serious under the influence of the reaction capacity and the reaction speed of the crosslinking agent and the sericin; and the common formaldehyde cross-linking agents such as formaldehyde, glutaraldehyde and the like have great harm to human health, have influence on operators in the finishing process, and the finished textile is easy to influence human health in the using process.
Disclosure of Invention
The invention provides a method for preparing a sericin finishing spunlaced non-woven fabric by thermal bonding, which aims to solve the problems that the loading amount of sericin is difficult to control and common formaldehyde, glutaraldehyde and other aldehyde cross-linking agents have great harm to human health when a textile is finished by a solution finishing method in the prior art, and the sericin is adhered to the surface of the spunlaced non-woven fabric by the thermal bonding method.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method for preparing a sericin finishing spunlaced nonwoven fabric by thermal bonding comprises the following steps:
(1) Mixing insoluble sericin powder and hot melt adhesive powder to obtain mixed powder;
(2) Applying the mixed powder to the surface of the spunlaced nonwoven fabric by a powder spraying method;
(3) And combining the sericin with the spunlaced nonwoven fabric by thermal bonding.
The invention uses the hot melt adhesive to adhere the silk glue on the surface of the spunlaced non-woven fabric by the hot bonding method, so that the finished spunlaced non-woven fabric has good performances of moisture absorption, moisture preservation, ultraviolet resistance, biocompatibility and the like, and can be used as an excellent material of sanitary products such as wet tissues, cotton soft tissues, facial masks and the like. Compared with the traditional solution finishing method, the thermal bonding method has the advantages of simple operation process, easy control of the sericin load, high raw material utilization rate, less sericin waste and avoidance of the influence of aldehyde cross-linking agents on human health.
Preferably, the mass ratio of the insoluble sericin powder to the hot melt adhesive powder in the mixed powder in the step (1) is 2 to 8:8 to 2.
Preferably, the sericin powder is insoluble sericin powder modified by a modified aldehyde chitosan crosslinking agent, and the preparation method comprises the following steps:
a) Oxidizing chitosan by sodium periodate to obtain aldehyde chitosan;
b) Dissolving the aldehyde chitosan in an acetic acid solution to obtain a solution to be treated, carrying out low-temperature plasma treatment on the solution to be treated, regulating the pH value of the solution to be neutral after the treatment, adding absolute ethyl alcohol for precipitation, and separating, washing and drying a precipitation product to obtain a modified aldehyde chitosan crosslinking agent;
c) Dissolving the modified aldehyde chitosan cross-linking agent in water, adding sericin powder, stirring for reaction, freeze-drying, heating the freeze-dried product at 40-45 ℃ for 30-40 min, and grinding the product to obtain the insoluble sericin powder.
In order to reduce the dissolution rate of the sericin on the surface of the finished spun-laced non-woven fabric, the modified aldehyde chitosan is used for modifying the sericin, so that the water solubility of the sericin is reduced. The invention firstly uses sodium periodate to oxidize chitosan to obtain aldehyde chitosan, and introduces a group capable of carrying out crosslinking reaction with sericin into chitosan molecules. However, the research of the invention shows that the crosslinking effect of the aldehyde chitosan and the sericin is poor, and when the macromolecular aldehyde chitosan is directly used for modifying the sericin, the dissolution rate of the sericin on the surface of the spunlaced nonwoven fabric is still higher. Therefore, the invention carries out low-temperature plasma treatment on the aldehyde chitosan and depolymerizes and modifies the aldehyde chitosan. After the aldehyde chitosan is modified by the method in the invention by low-temperature plasma, the molecular weight of the aldehyde chitosan can be reduced, the oligomeric chitosan is obtained, the crosslinking effect of the crosslinking agent on the sericin is improved, the water solubility of the sericin is effectively reduced, the compatibility of the sericin and the hot melt adhesive is improved, and the washing resistance of the sericin on the surface of the spun-laced non-woven fabric after finishing is improved.
Preferably, the oxidation process in step a) is: adding chitosan into sodium periodate solution, adding glycol solution to terminate reaction after light-shielding reaction under nitrogen protection, adding acetone to filtrate for precipitation after filtration, and separating, washing and drying the precipitation product to obtain aldehyde chitosan; the concentration of the sodium periodate solution is 0.3-0.5 mol/L, the mass volume ratio of chitosan to the sodium periodate solution is 1 g:50-100 mL, the reaction temperature is 25-35 ℃, and the reaction time is 2-4 h; the mol ratio of the added glycol to the sodium periodate is 2:40-45.
Preferably, the working gas used in the low temperature plasma treatment in the step B) is argon and nitrogen with a volume ratio of 2-4:1. The working gas in the invention is used for low-temperature plasma treatment, so that the crosslinking effect of the aldehyde chitosan on the sericin can be effectively improved, the water solubility of the sericin is reduced, and the compatibility of the sericin and the hot melt adhesive is improved.
Preferably, the pressure is 25-35 Pa, the power is 600-1000W, and the treatment time is 1-2 h during the low temperature plasma treatment in the step B).
Preferably, the mass concentration of the acetic acid solution in the step B) is 1-3%, and the mass concentration of the aldehyde chitosan in the solution to be treated is 0.1-0.5%.
Preferably, the mass ratio of the modified aldehyde chitosan cross-linking agent to the sericin powder in the step C) is 1:1-2, the stirring reaction time is 20-30 min, and the freeze drying time is 2-3 h.
Preferably, the mixed powder in the step (2) is mixed with the spun-laced non-woven fabricThe surface dosage is 3-8 g/m 2 。
Preferably, the raw material of the spunlaced nonwoven fabric in the step (2) is one or more selected from polyester fiber, polypropylene fiber and cellulose fiber.
Preferably, the thermal bonding in the step (3) is hot roll thermal bonding or oven thermal bonding.
Preferably, the thermal bonding temperature in step (3) is 60 to 100 ℃.
Therefore, the invention has the following beneficial effects:
(1) The hot melt adhesive is used for bonding the silk glue on the surface of the spunlaced non-woven fabric by a hot bonding method, the operation process is simple, the loading amount of the silk glue is easy to control, and the influence of an aldehyde cross-linking agent on the health of a human body is avoided;
(2) The modified aldehyde chitosan is used for modifying the sericin, so that the water solubility of the sericin is reduced, the compatibility of the sericin and the hot melt adhesive is improved, and the washing resistance of the finished sericin on the surface of the spun-laced non-woven fabric is improved.
Detailed Description
The invention is further described below in connection with the following detailed description.
General examples:
a method for preparing a sericin finishing spunlaced nonwoven fabric by thermal bonding comprises the following steps:
(1) Mixing sericin powder and hot melt adhesive powder to obtain mixed powder; the mass ratio of the sericin powder to the hot melt adhesive powder in the mixed powder is 2-8:8-2; the sericin powder is insoluble sericin powder modified by a modified aldehyde chitosan crosslinking agent, and the preparation method comprises the following steps:
a) Adding chitosan into 0.3-0.5 mol/L sodium periodate solution, wherein the mass volume ratio of the chitosan to the sodium periodate solution is 1 g:50-100 mL, carrying out light-shielding reaction for 2-4 hours at 25-35 ℃ under the protection of nitrogen, and then adding glycol solution to terminate the reaction, wherein the mol ratio of the added glycol to the sodium periodate is 2:40-45; adding acetone into the filtrate for precipitation after filtration, and separating, washing and drying the precipitation product to obtain aldehyde chitosan;
b) Dissolving the aldehyde chitosan in an acetic acid solution with the mass concentration of 1-3% to obtain a solution to be treated, wherein the mass concentration of the aldehyde chitosan in the solution to be treated is 0.1-0.5%; carrying out low-temperature plasma treatment on the solution to be treated, wherein the working gas in the low-temperature plasma treatment is argon and nitrogen with the volume ratio of 2-4:1, the pressure is 25-35 Pa, the power is 600-1000W, and the treatment time is 1-2 h; after treatment, regulating the pH value of the solution to be neutral, adding absolute ethyl alcohol for precipitation, and separating, washing and drying a precipitation product to obtain the modified aldehyde chitosan crosslinking agent;
c) Dissolving the modified aldehyde chitosan cross-linking agent in water, adding sericin powder, stirring and reacting for 20-30 min, freeze-drying for 2-3 h, heating the freeze-dried product at 40-45 ℃ for 30-40 min, and grinding the product to obtain insoluble sericin powder;
(2) Applying the mixed powder to the surface of the spunlaced non-woven fabric by a powder spraying method, wherein the dosage of the mixed powder on the surface of the spunlaced non-woven fabric is 3-8 g/m 2 ；
(3) The sericin and the spunlaced nonwoven are combined and formed through hot roll thermal bonding or oven thermal bonding, and the thermal bonding temperature is 60-100 ℃.
Example 1:
a method for preparing a sericin finishing spunlaced nonwoven fabric by thermal bonding comprises the following steps:
(1) Mixing insoluble sericin powder and hot melt adhesive powder (German Korschun Bayer TPU 255) according to a mass ratio of 5:5 to obtain mixed powder; the preparation method of the insoluble sericin powder comprises the following steps:
a) Adding chitosan into 0.4mol/L sodium periodate solution, wherein the mass volume ratio of the chitosan to the sodium periodate solution is 1g to 80mL, adding ethylene glycol solution to terminate the reaction after light-shielding reaction for 3 hours at 30 ℃ under the protection of nitrogen, and the mol ratio of the added ethylene glycol to the sodium periodate is 2 to 43; adding acetone into the filtrate for precipitation after filtration, and separating, washing and drying the precipitation product to obtain aldehyde chitosan;
b) Dissolving aldehyde chitosan in an acetic acid solution with the mass concentration of 2% to obtain a solution to be treated, wherein the mass concentration of the aldehyde chitosan in the solution to be treated is 0.3%; carrying out low-temperature plasma treatment on the solution to be treated, wherein the working gas in the low-temperature plasma treatment is argon and nitrogen with the volume ratio of 3:1, the pressure is 30Pa, the power is 800W, and the treatment time is 1.5h; adjusting the pH value of the solution to be neutral by using a NaOH solution with the concentration of 1mol/L after the treatment, adding absolute ethyl alcohol for precipitation, and separating, washing and drying a precipitation product to obtain the aldehyde chitosan crosslinking agent;
c) Dissolving the modified aldehyde chitosan cross-linking agent in water to obtain a modified aldehyde chitosan solution with the mass concentration of 5%, adding sericin powder (SiAN you Biotechnology Co., ltd.) into the solution, stirring the mixture to react for 25min, freeze-drying the mixture for 2.5h, heating the freeze-dried product at 42 ℃ for 35min, and grinding the product to obtain insoluble sericin powder;
(2) The mixed powder was applied to a gram weight of 30g/m by the powder spraying method 2 The dosage of the mixed powder on the surface of the PET spunlaced non-woven fabric is 5g/m 2 ；
(3) And combining the sericin with the spunlaced nonwoven fabric by hot-roll thermal bonding, wherein the thermal bonding temperature is 80 ℃.
Example 2:
a method for preparing a sericin finishing spunlaced nonwoven fabric by thermal bonding comprises the following steps:
(1) Mixing insoluble sericin powder and hot melt adhesive powder (German Korschun Bayer TPU 255) according to a mass ratio of 2:8 to obtain mixed powder; the preparation method of the insoluble sericin powder comprises the following steps:
a) Adding chitosan into 0.3mol/L sodium periodate solution, wherein the mass volume ratio of the chitosan to the sodium periodate solution is 1g to 100mL, adding ethylene glycol solution after light-shielding reaction for 4 hours at 25 ℃ under the protection of nitrogen to terminate the reaction, and the mol ratio of the added ethylene glycol to the sodium periodate is 2 to 40; adding acetone into the filtrate for precipitation after filtration, and separating, washing and drying the precipitation product to obtain aldehyde chitosan;
b) Dissolving aldehyde chitosan in an acetic acid solution with the mass concentration of 1% to obtain a solution to be treated, wherein the mass concentration of the aldehyde chitosan in the solution to be treated is 0.1%; carrying out low-temperature plasma treatment on the solution to be treated, wherein the working gas in the low-temperature plasma treatment is argon and nitrogen with the volume ratio of 2:1, the pressure is 25Pa, the power is 1000W, and the treatment time is 1h; adjusting the pH value of the solution to be neutral by using a NaOH solution with the concentration of 1mol/L after the treatment, adding absolute ethyl alcohol for precipitation, and separating, washing and drying a precipitation product to obtain the aldehyde chitosan crosslinking agent;
c) Dissolving the modified aldehyde chitosan cross-linking agent in water to obtain a modified aldehyde chitosan solution with the mass concentration of 2%, adding sericin powder (SiAN you Biotechnology Co., ltd.) into the modified aldehyde chitosan cross-linking agent, stirring and reacting for 30min, freeze-drying for 2h, heating the freeze-dried product at 40 ℃ for 40min, and grinding the product to obtain the insoluble sericin powder;
(2) The mixed powder was applied to a gram weight of 30g/m by the powder spraying method 2 The dosage of the mixed powder on the surface of the PET spunlaced non-woven fabric is 8g/m 2 ；
(3) And combining the sericin with the spunlaced nonwoven fabric by hot-roll thermal bonding, wherein the thermal bonding temperature is 100 ℃.
Example 3:
a method for preparing a sericin finishing spunlaced nonwoven fabric by thermal bonding comprises the following steps:
(1) Mixing insoluble sericin powder and hot melt adhesive powder (German Korschun Bayer TPU 255) according to a mass ratio of 8:2 to obtain mixed powder; the preparation method of the insoluble sericin powder comprises the following steps:
a) Adding chitosan into 0.5mol/L sodium periodate solution, wherein the mass volume ratio of the chitosan to the sodium periodate solution is 1g to 50mL, adding ethylene glycol solution to terminate the reaction after light-shielding reaction for 2 hours at 35 ℃ under the protection of nitrogen, and the mol ratio of the added ethylene glycol to the sodium periodate is 2 to 45; adding acetone into the filtrate for precipitation after filtration, and separating, washing and drying the precipitation product to obtain aldehyde chitosan;
b) Dissolving aldehyde chitosan in an acetic acid solution with the mass concentration of 3% to obtain a solution to be treated, wherein the mass concentration of the aldehyde chitosan in the solution to be treated is 0.5%; carrying out low-temperature plasma treatment on the solution to be treated, wherein the working gas in the low-temperature plasma treatment is argon and nitrogen with the volume ratio of 4:1, the pressure is 35Pa, the power is 600W, and the treatment time is 2h; adjusting the pH value of the solution to be neutral by using a NaOH solution with the concentration of 1mol/L after the treatment, adding absolute ethyl alcohol for precipitation, and separating, washing and drying a precipitation product to obtain the aldehyde chitosan crosslinking agent;
c) Dissolving the modified aldehyde chitosan cross-linking agent in water to obtain a modified aldehyde chitosan solution with the mass concentration of 5%, adding sericin powder (SiAN you Biotechnology Co., ltd.) into the solution, stirring the mixture to react for 20min, freeze-drying the mixture for 3h, heating the freeze-dried product at 45 ℃ for 30min, and grinding the product to obtain the insoluble sericin powder;
(2) The mixed powder was applied to a gram weight of 30g/m by the powder spraying method 2 The dosage of the mixed powder on the surface of the PET spunlaced non-woven fabric is 3g/m 2 ；
(3) And combining the sericin with the spunlaced nonwoven fabric by hot-roll thermal bonding, wherein the thermal bonding temperature is 60 ℃.
Comparative example 1:
a method for preparing a sericin finishing spunlaced nonwoven fabric by thermal bonding comprises the following steps:
(1) Mixing sericin powder (Sian you Shuo biotechnology Co., ltd.) with hot melt adhesive powder (German Korschwan Bayer TPU 255) according to a mass ratio of 5:5 to obtain mixed powder;
(2) The mixed powder was applied to a gram weight of 30g/m by the powder spraying method 2 The dosage of the mixed powder on the surface of the PET spunlaced non-woven fabric is 5g/m 2 ；
(3) And combining the sericin with the spunlaced nonwoven fabric by hot-roll thermal bonding, wherein the thermal bonding temperature is 80 ℃.
Comparative example 2:
the preparation method of the insoluble sericin powder in comparative example 2 comprises the following steps:
a) Adding chitosan into 0.4mol/L sodium periodate solution, wherein the mass volume ratio of the chitosan to the sodium periodate solution is 1g to 80mL, adding ethylene glycol solution to terminate the reaction after light-shielding reaction for 3 hours at 30 ℃ under the protection of nitrogen, and the mol ratio of the added ethylene glycol to the sodium periodate is 2 to 43; adding acetone into the filtrate for precipitation after filtration, and separating, washing and drying the precipitation product to obtain aldehyde chitosan;
b) Dissolving aldehyde chitosan in an acetic acid solution with the mass concentration of 2% to obtain an aldehyde chitosan solution with the mass concentration of 5%, adding sericin powder (SiAnyou Biotechnology Co., ltd.) into the aldehyde chitosan solution, stirring the mixture to react for 25min, freeze-drying the mixture for 2.5h, heating the freeze-dried product at 42 ℃ for 35min, and grinding the product to obtain insoluble sericin powder;
the remainder was the same as in example 1.
Comparative example 3:
the preparation method of the insoluble sericin powder in comparative example 3 comprises the following steps:
a) Adding chitosan into 0.4mol/L sodium periodate solution, wherein the mass volume ratio of the chitosan to the sodium periodate solution is 1g to 80mL, adding ethylene glycol solution to terminate the reaction after light-shielding reaction for 3 hours at 30 ℃ under the protection of nitrogen, and the mol ratio of the added ethylene glycol to the sodium periodate is 2 to 43; adding acetone into the filtrate for precipitation after filtration, and separating, washing and drying the precipitation product to obtain aldehyde chitosan;
b) Dissolving aldehyde chitosan in an acetic acid solution with the mass concentration of 2% to obtain a solution to be treated, wherein the mass concentration of the aldehyde chitosan in the solution to be treated is 0.3%; carrying out low-temperature plasma treatment on the solution to be treated, wherein the working gas in the low-temperature plasma treatment is argon and nitrogen with the volume ratio of 3:1, the pressure is 30Pa, the power is 800W, and the treatment time is 30min; adjusting the pH value of the solution to be neutral by using a NaOH solution with the concentration of 1mol/L after the treatment, adding absolute ethyl alcohol for precipitation, and separating, washing and drying a precipitation product to obtain the aldehyde chitosan crosslinking agent;
c) Dissolving the modified aldehyde chitosan cross-linking agent in water to obtain a modified aldehyde chitosan solution with the mass concentration of 5%, adding sericin powder (SiAN you Biotechnology Co., ltd.) into the solution, stirring the mixture to react for 25min, freeze-drying the mixture for 2.5h, heating the freeze-dried product at 42 ℃ for 35min, and grinding the product to obtain insoluble sericin powder;
the remainder was the same as in example 1.
Comparative example 4:
the preparation method of the insoluble sericin powder in comparative example 4 comprises the following steps:
a) Adding chitosan into 0.4mol/L sodium periodate solution, wherein the mass volume ratio of the chitosan to the sodium periodate solution is 1g to 80mL, adding ethylene glycol solution to terminate the reaction after light-shielding reaction for 3 hours at 30 ℃ under the protection of nitrogen, and the mol ratio of the added ethylene glycol to the sodium periodate is 2 to 43; adding acetone into the filtrate for precipitation after filtration, and separating, washing and drying the precipitation product to obtain aldehyde chitosan;
b) Dissolving aldehyde chitosan in an acetic acid solution with the mass concentration of 2% to obtain a solution to be treated, wherein the mass concentration of the aldehyde chitosan in the solution to be treated is 0.3%; carrying out low-temperature plasma treatment on the solution to be treated, wherein the working gas is argon gas in the low-temperature plasma treatment, the pressure is 30Pa, the power is 800W, and the treatment time is 1.5h; adjusting the pH value of the solution to be neutral by using a NaOH solution with the concentration of 1mol/L after the treatment, adding absolute ethyl alcohol for precipitation, and separating, washing and drying a precipitation product to obtain the aldehyde chitosan crosslinking agent;
c) Dissolving the modified aldehyde chitosan cross-linking agent in water to obtain a modified aldehyde chitosan solution with the mass concentration of 5%, adding sericin powder (SiAN you Biotechnology Co., ltd.) into the solution, stirring the mixture to react for 25min, freeze-drying the mixture for 2.5h, heating the freeze-dried product at 42 ℃ for 35min, and grinding the product to obtain insoluble sericin powder;
the remainder was the same as in example 1.
Comparative example 5:
the preparation method of the insoluble sericin powder in comparative example 5 comprises the following steps:
a) Adding chitosan into 0.4mol/L sodium periodate solution, wherein the mass volume ratio of the chitosan to the sodium periodate solution is 1g to 80mL, adding ethylene glycol solution to terminate the reaction after light-shielding reaction for 3 hours at 30 ℃ under the protection of nitrogen, and the mol ratio of the added ethylene glycol to the sodium periodate is 2 to 43; adding acetone into the filtrate for precipitation after filtration, and separating, washing and drying the precipitation product to obtain aldehyde chitosan;
b) Dissolving aldehyde chitosan in an acetic acid solution with the mass concentration of 2% to obtain a solution to be treated, wherein the mass concentration of the aldehyde chitosan in the solution to be treated is 0.3%; carrying out low-temperature plasma treatment on the solution to be treated, wherein the working gas is nitrogen in the low-temperature plasma treatment, the pressure is 30Pa, the power is 800W, and the treatment time is 1.5h; adjusting the pH value of the solution to be neutral by using a NaOH solution with the concentration of 1mol/L after the treatment, adding absolute ethyl alcohol for precipitation, and separating, washing and drying a precipitation product to obtain the aldehyde chitosan crosslinking agent;
c) Dissolving the modified aldehyde chitosan cross-linking agent in water to obtain a modified aldehyde chitosan solution with the mass concentration of 5%, adding sericin powder (SiAN you Biotechnology Co., ltd.) into the solution, stirring the mixture to react for 25min, freeze-drying the mixture for 2.5h, heating the freeze-dried product at 42 ℃ for 35min, and grinding the product to obtain insoluble sericin powder;
the remainder was the same as in example 1.
The sericin-finished spunlaced nonwoven fabrics prepared in the above examples and comparative examples were tested for their water-washing resistance, and the results are shown in table 1.
Weight gain rate= (m 1 -m 0 )/m 0 X 100%, where m 0 For dry mass of sample before loading sericin, m 1 The dry mass of the sample after sericin loading;
the dissolution rate= (M-M)/mx100%, where M is the dry mass of the sample before water washing and M is the dry mass of the sample after water washing.
Table 1: sericin adhesion performance test results.
As can be seen from Table 1, when the spun-laced nonwoven fabrics were subjected to sericin finishing by the method of the present invention in examples 1 to 3, the sericin had good water-washing resistance on the surface of the spun-laced nonwoven fabrics and the dissolution rate after washing was low. In contrast, the comparative example 1 did not modify the sericin, the water solubility of the sericin was good, and the dissolution rate after washing was significantly improved as compared with that in example 1. In comparative example 2, the aldehyde chitosan which is not treated by low-temperature plasma is adopted to modify the sericin, and in comparative example 3, the low-temperature plasma treatment time is too short, and the washing resistance of the sericin after finishing is obviously reduced compared with that of example 1, which shows that the water-solubility modification effect of macromolecular aldehyde chitosan on the sericin is inferior to that of the oligomeric aldehyde chitosan after depolymerization. The low temperature plasma treatment atmosphere of the aldehyde chitosan solution was changed in comparative example 3 and comparative example 4, and the washing resistance after sericin finishing was also lowered as compared with that in example 1, indicating that the kind of the working gas during the low temperature plasma treatment had an influence on the modifying effect of the modified aldehyde chitosan on sericin.
The untreated PET spunlaced nonwoven fabric and the sericin-finished spunlaced nonwoven fabric obtained in example 1 were tested for hygroscopicity and antibacterial properties, and the results are shown in table 2. Wherein, the test method of the moisture regain refers to GB/T9995-1997; the antibacterial test method is referred to GB/T20944.2-2008.
Table 2: and (5) testing the hygroscopicity and the antibacterial performance of the spunlaced nonwoven fabric.
As can be seen from table 2, after finishing with sericin, the hygroscopicity and the antibacterial property of the spun-laced nonwoven fabric are remarkably improved, and the spun-laced nonwoven fabric is beneficial to the application in sanitary products such as wet tissues, cotton soft tissues, facial masks and the like.

Claims (8)

1. The method for preparing the sericin finishing spunlaced non-woven fabric by thermal bonding is characterized by comprising the following steps of:
(1) Mixing sericin powder and hot melt adhesive powder to obtain mixed powder;
(2) Applying the mixed powder to the surface of the spunlaced nonwoven fabric by a powder spraying method;
(3) Combining the sericin with the spunlaced nonwoven fabric through thermal bonding;
the sericin powder is insoluble sericin powder modified by a modified aldehyde chitosan crosslinking agent, and the preparation method comprises the following steps:
a) Oxidizing chitosan by sodium periodate to obtain aldehyde chitosan;
b) Dissolving the aldehyde chitosan in an acetic acid solution to obtain a solution to be treated, carrying out low-temperature plasma treatment on the solution to be treated, regulating the pH value of the solution to be neutral after the treatment, adding absolute ethyl alcohol for precipitation, and separating, washing and drying a precipitation product to obtain a modified aldehyde chitosan crosslinking agent; the working gas in the low-temperature plasma treatment is argon and nitrogen with the volume ratio of 2-4:1;
c) And dissolving the modified aldehyde chitosan cross-linking agent in water, adding sericin powder, stirring for reaction, freeze-drying, heating the freeze-dried product at 40-45 ℃ for 30-40 min, and grinding the product to obtain the insoluble sericin powder.
2. The method of claim 1, wherein the mass ratio of the sericin powder to the hot melt adhesive powder in the mixed powder in the step (1) is 2-8:8-2.
3. The method according to claim 1, wherein the pressure is 25-35 Pa, the power is 600-1000W, and the treatment time is 1-2 hours during the low temperature plasma treatment in the step B).
4. The method according to claim 1, wherein the mass concentration of the acetic acid solution in the step B) is 1-3%, and the mass concentration of the aldehyde chitosan in the solution to be treated is 0.1-0.5%.
5. The method of claim 1, wherein the mass ratio of the modified aldehyde chitosan cross-linking agent to the sericin powder in the step C) is 1:1-2, the stirring reaction time is 20-30 min, and the freeze drying time is 2-3 h.
6. The method according to claim 1, wherein the amount of the mixed powder in the step (2) used on the surface of the spun-laced nonwoven fabric is 3-8 g/m 2 。
7. The method of claim 1, wherein the thermal bonding in step (3) is a hot roll thermal bonding or an oven thermal bonding.
8. The method according to claim 1 or 7, wherein the thermal bonding temperature in step (3) is 60 to 100 ℃.
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