阅读说明：本技术 利用有机棉制备抗菌防螨襁褓用品的工艺 (Process for preparing antibacterial anti-mite swaddle article by using organic cotton ) 是由 张丽 马晓飞 张志成 于 2021-06-29 设计创作，主要内容包括：本发明公开了一种利用有机棉制备抗菌防螨襁褓用品的工艺,涉及有机棉加工技术领域,本发明以有机棉纤维作为原料,经抗菌和防螨处理后赋予有机棉优良的抗菌防螨性能,同时安全性高,解决了常规化学类抗菌剂和防螨剂所存在的安全隐患问题,并且耐水洗性强,经多次水洗后仍具有良好的抗菌防螨性能,抗菌防螨时效长。(The invention discloses a process for preparing an antibacterial anti-mite swaddling article by using organic cotton, which relates to the technical field of organic cotton processing.)

1. The process for preparing the antibacterial anti-mite swaddle article by using the organic cotton is characterized in that: the method comprises the following process steps:

(1) dissolving carboxymethyl chitosan and silicotungstic acid in water to prepare an antibacterial treatment solution, then soaking the organic cotton fiber in the antibacterial treatment solution, taking out the organic cotton fiber, and heating and drying the organic cotton fiber to obtain antibacterial modified organic cotton fiber;

(2) dissolving beta-cyclodextrin and potassium carbonate in hot water, adding a phase transfer catalyst, then dropwise adding chloromethyl pivalate dissolved in toluene, heating and reacting while stirring, continuing to react after the dropwise addition of the chloromethyl pivalate, recovering toluene after the reaction is finished, washing and distilling residues, drying in vacuum, crushing, and sieving to obtain modified cyclodextrin;

(3) dropwise adding eucalyptus essential oil dissolved in ethanol into the modified cyclodextrin prepared in the step (2) under stirring, uniformly mixing, then introducing into a granulator for granulation, and sieving to obtain an anti-mite microcapsule;

(4) adding acrylic resin emulsion and anti-mite microcapsules into water, uniformly mixing to obtain slurry, carding and lapping the antibacterial modified organic cotton fibers prepared in the step (1) to form a fiber web, spraying the slurry on the surface of the fiber web, drying and reinforcing to obtain non-woven fabric;

(5) and (4) processing the non-woven fabric prepared in the step (4) into an antibacterial anti-mite swaddling article.

2. The process for preparing an antibacterial anti-mite swaddling article using organic cotton as claimed in claim 1, wherein the process comprises the following steps: the mass concentration of the carboxymethyl chitosan contained in the steeping liquor in the step (1) is 0.5-2.5%.

3. The process for preparing an antibacterial anti-mite swaddling article using organic cotton as claimed in claim 1, wherein the process comprises the following steps: the dosage of the silicotungstic acid in the step (1) is 0.05-0.5 percent of the mass of the carboxymethyl chitosan.

4. The process for preparing an antibacterial anti-mite swaddling article using organic cotton as claimed in claim 1, wherein the process comprises the following steps: in the step (1), the dipping temperature is 40-60 ℃, and the heating and drying temperature is 80-100 ℃.

5. The process for preparing an antibacterial anti-mite swaddling article using organic cotton as claimed in claim 1, wherein the process comprises the following steps: the phase transfer catalyst in the step (2) is selected from any one of tetrabutylammonium chloride, tetrabutylammonium bromide, dodecyl trimethyl ammonium chloride, tetradecyl trimethyl ammonium chloride and benzyl triethyl ammonium chloride.

6. The process for preparing an antibacterial anti-mite swaddling article using organic cotton as claimed in claim 1, wherein the process comprises the following steps: in the step (2), the molar ratio of the chloromethyl pivalate, the potassium carbonate and the phase transfer catalyst is 1 (1-1.05) to 1% -5%, and the mass ratio of the beta-cyclodextrin to the chloromethyl pivalate is 1 (1.5-2).

7. The process for preparing an antibacterial anti-mite swaddling article using organic cotton as claimed in claim 1, wherein the process comprises the following steps: in the step (3), the mass ratio of the modified cyclodextrin to the eucalyptus essential oil is 1 (0.5-2), and the volume ratio of the eucalyptus essential oil to the ethanol is 1 (1-5).

8. The process for preparing an antibacterial anti-mite swaddling article using organic cotton as claimed in claim 1, wherein the process comprises the following steps: in the step (4), the mass ratio of the acrylic resin emulsion to the anti-mite microcapsule is (2-10) to 1.

9. The process for preparing an antibacterial anti-mite swaddling article using organic cotton as claimed in claim 1, wherein the process comprises the following steps: the dosage of the anti-mite microcapsule in the step (4) is 1-5g per 100g of the antibacterial modified organic cotton fiber.

The technical field is as follows:

the invention relates to the technical field of organic cotton processing, in particular to a process for preparing an antibacterial anti-mite swaddling article by using organic cotton.

Background art:

organic Cotton, which is the term translated from Organic Cotton, is also called ecological Cotton or biological Cotton in other foreign languages. In the production of organic cotton, natural cultivation management for biological prevention and control of plant diseases and insect pests by organic fertilizer is mainly used, chemicals are not used, and all natural pollution-free production is carried out from seeds to agricultural products. And the content of toxic and harmful substances such as heavy metal nitrate harmful organisms (including microorganisms, parasitic ova and the like) in the cotton is controlled within a standard specified limit range by taking agricultural product safety quality standards issued by countries or WTO/FAO as a measurement scale, and the certified commodity cotton is obtained. In the production of organic cotton, not only the necessary conditions of light, heat, water, soil and the like for cultivating cotton are required, but also the cleanness of the farmland soil environment, irrigation water quality, air environment and the like is required to be specified.

In recent years, people have higher and higher requirements on the safety and comfort of infant textiles, and the organic cotton is selected as a processing raw material, but the antibacterial and anti-mite performance of the organic cotton is poor, and if the antibacterial and anti-mite finishing is not carried out on the organic cotton, the using effect of the organic cotton is directly influenced.

The invention content is as follows:

the invention aims to solve the technical problem of providing a process for preparing an antibacterial anti-mite swaddling article by using organic cotton, wherein the antibacterial treatment liquid and anti-mite microcapsules are used for carrying out antibacterial anti-mite finishing on the organic cotton to prepare an organic cotton product with excellent antibacterial and anti-mite performances, and the organic cotton product is suitable for processing infant fabrics.

The technical problem to be solved by the invention is realized by adopting the following technical scheme:

the process for preparing the antibacterial anti-mite swaddling article by using the organic cotton comprises the following process steps:

(1) dissolving carboxymethyl chitosan and silicotungstic acid in water to prepare an antibacterial treatment solution, then soaking the organic cotton fiber in the antibacterial treatment solution, taking out the organic cotton fiber, and heating and drying the organic cotton fiber to obtain antibacterial modified organic cotton fiber;

(2) dissolving beta-cyclodextrin and potassium carbonate in hot water, adding a phase transfer catalyst, then dropwise adding chloromethyl pivalate dissolved in toluene, heating and reacting while stirring, continuing to react after the dropwise addition of the chloromethyl pivalate, recovering toluene after the reaction is finished, washing and distilling residues, drying in vacuum, crushing, and sieving to obtain modified cyclodextrin;

(3) dropwise adding eucalyptus essential oil dissolved in ethanol into the modified cyclodextrin prepared in the step (2) under stirring, uniformly mixing, then introducing into a granulator for granulation, and sieving to obtain an anti-mite microcapsule;

(4) adding acrylic resin emulsion and anti-mite microcapsules into water, uniformly mixing to obtain slurry, carding and lapping the antibacterial modified organic cotton fibers prepared in the step (1) to form a fiber web, spraying the slurry on the surface of the fiber web, drying and reinforcing to obtain non-woven fabric;

(5) and (4) processing the non-woven fabric prepared in the step (4) into an antibacterial anti-mite swaddling article.

The mass concentration of the carboxymethyl chitosan contained in the steeping liquor in the step (1) is 0.5-2.5%.

The dosage of the silicotungstic acid in the step (1) is 0.05-0.5 percent of the mass of the carboxymethyl chitosan.

In the step (1), the dipping temperature is 40-60 ℃, and the heating and drying temperature is 80-100 ℃.

The phase transfer catalyst in the step (2) is selected from any one of tetrabutylammonium chloride, tetrabutylammonium bromide, dodecyl trimethyl ammonium chloride, tetradecyl trimethyl ammonium chloride and benzyl triethyl ammonium chloride.

In the step (2), the molar ratio of the chloromethyl pivalate, the potassium carbonate and the phase transfer catalyst is 1 (1-1.05) to 1% -5%, and the mass ratio of the beta-cyclodextrin to the chloromethyl pivalate is 1 (1.5-2).

In the step (3), the mass ratio of the modified cyclodextrin to the eucalyptus essential oil is 1 (0.5-2), and the volume ratio of the eucalyptus essential oil to the ethanol is 1 (1-5).

In the step (4), the mass ratio of the acrylic resin emulsion to the anti-mite microcapsule is (2-10) to 1.

The dosage of the anti-mite microcapsule in the step (4) is 1-5g per 100g of the antibacterial modified organic cotton fiber.

The principle of antibacterial modification is as follows: the silicotungstic acid is used as a catalyst of esterification reaction to catalyze the esterification reaction between carboxymethyl chitosan and organic cotton fiber, and the carboxymethyl chitosan is grafted to the surface of the organic cotton fiber. The silicotungstic acid is used as a catalyst, so that the problem of strong corrosivity of concentrated sulfuric acid can be solved, the esterification reaction rate can be accelerated, compared with a conventional physical doping mode, the mode of doping carboxymethyl chitosan into organic cotton fibers by adopting a chemical means has the advantage of good antibacterial stability, and the problem of obvious reduction of antibacterial performance after washing is solved.

The eucalyptus essential oil has good anti-mite effect and high safety, so that the eucalyptus essential oil can be used for anti-mite treatment of infant fabrics. However, the eucalyptus essential oil has volatility, and the anti-mite period is short because the eucalyptus essential oil is directly mixed in the fiber, so that the release rate of the eucalyptus essential oil needs to be controlled, and the anti-mite period is prolonged.

The cyclodextrin has the structural characteristics of hydrophilic outer edge and hydrophobic inner cavity, various organic compounds can be embedded into the hydrophobic inner cavity of the cyclodextrin to form an inclusion complex, and the physicochemical property of the inclusion complex is changed, so that the cyclodextrin is commonly used for including the drug with poor water solubility, the stability and the bioavailability of the drug are improved, and the sustained-release effect is achieved.

The invention aims to prepare the micro anti-mite capsule by taking eucalyptus essential oil as a core material and cyclodextrin as a wall material, and aims to control the release rate of the eucalyptus essential oil and play a role in lasting anti-mite. However, cyclodextrin has good hydrophilicity, so that the water washing resistance is poor, and the eucalyptus essential oil is quickly volatilized after the wall material structure is damaged, so that the anti-mite period is shortened. In order to solve the problem, the invention carries out chemical modification on the cyclodextrin, thereby not only ensuring the initial anti-mite effect of the fabric, but also ensuring the anti-mite effect of the fabric after being washed for multiple times.

The principle of anti-mite modification is as follows: by utilizing the structural characteristic that cyclodextrin contains hydroxyl, etherification reaction is carried out on cyclodextrin and chloromethyl pivalate, and tert-butyl, ester group and ether group are introduced into the cyclodextrin structure, so that the water solubility of the cyclodextrin is weakened, the inclusion effect of eucalyptus essential oil is ensured, the release rate of the eucalyptus essential oil is controlled, the anti-mite effect is enhanced, and the anti-mite time effect is prolonged. The acrylic resin emulsion is used as an adhesive, and aims to realize firm attachment of the anti-mite microcapsules on cotton fibers and improve the washing resistance of the anti-mite microcapsules.

The invention has the beneficial effects that: the organic cotton fiber is used as a raw material, and is endowed with excellent antibacterial and anti-mite performance after antibacterial and anti-mite treatment, meanwhile, the safety is high, the problem of potential safety hazards of conventional chemical antibacterial agents and anti-mite agents is solved, the water washing resistance is high, the organic cotton fiber still has good antibacterial and anti-mite performance after being washed for many times, and the antibacterial and anti-mite aging time is long.

The specific implementation mode is as follows:

in order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.

Example 1

(1) Firstly, dissolving carboxymethyl chitosan and silicotungstic acid in water to prepare an antibacterial treatment solution, wherein the mass concentration of the carboxymethyl chitosan contained in the impregnation solution is 2%, and the dosage of the silicotungstic acid is 0.25% of the mass of the carboxymethyl chitosan, then impregnating the organic cotton fiber in the antibacterial treatment solution for 1.5h at the temperature of 40 ℃, taking out the organic cotton fiber, and heating and drying the organic cotton fiber at the temperature of 80 ℃ to obtain the antibacterial modified organic cotton fiber. By monitoring the reaction progress by IR, the hydroxyl group content in the system decreased, indicating that the hydroxyl group participated in the reaction.

(2) Dissolving beta-cyclodextrin and potassium carbonate in hot water at 80 ℃, adding dodecyl trimethyl ammonium chloride, then dropwise adding chloromethyl pivalate dissolved in toluene, wherein the molar ratio of the chloromethyl pivalate to the potassium carbonate to the dodecyl trimethyl ammonium chloride is 1:1: 3%, the mass ratio of the beta-cyclodextrin to the chloromethyl pivalate is 1:1.5, heating to 80 ℃ under stirring for reaction, continuing the reaction until the chloromethyl pivalate is completely reacted after the chloromethyl pivalate is dropwise added, ending the reaction, carrying out reduced pressure distillation to recover toluene, washing distillation residues, carrying out vacuum drying, crushing, and sieving to obtain the modified cyclodextrin. The progress of the reaction was monitored by TLC until all chloromethyl pivalate had reacted.

(3) Dropwise adding eucalyptus essential oil dissolved in ethanol into the modified cyclodextrin prepared in the step (2) under stirring, wherein the mass ratio of the modified cyclodextrin to the eucalyptus essential oil is 1:1, and the volume ratio of the eucalyptus essential oil to the ethanol is 1:3, uniformly mixing, introducing into a granulator, granulating, and sieving to obtain the anti-mite microcapsule.

(4) Adding acrylic resin emulsion MSDS and anti-mite microcapsules into water, wherein the mass ratio of the acrylic resin emulsion MSDS to the anti-mite microcapsules is 10:1, the dosage of the anti-mite microcapsules is 5g per 100g of antibacterial modified organic cotton fibers, uniformly mixing to obtain slurry, carding and lapping the antibacterial modified organic cotton fibers prepared in the step (1) to form a fiber web, spraying the slurry on the surface of the fiber web, drying and reinforcing to obtain the non-woven fabric.

(5) And (4) processing the non-woven fabric prepared in the step (4) into an antibacterial anti-mite swaddling article.

Example 2

(1) Firstly, dissolving carboxymethyl chitosan and silicotungstic acid in water to prepare an antibacterial treatment solution, wherein the mass concentration of the carboxymethyl chitosan contained in the impregnation solution is 2.5%, and the dosage of the silicotungstic acid is 0.25% of the mass of the carboxymethyl chitosan, then impregnating the organic cotton fiber in the antibacterial treatment solution for 1h at the temperature of 50 ℃, taking out the organic cotton fiber, and heating and drying the organic cotton fiber at the temperature of 85 ℃ to obtain the antibacterial modified organic cotton fiber.

(2) Dissolving beta-cyclodextrin and potassium carbonate in hot water at 80 ℃, adding dodecyl trimethyl ammonium chloride, then dropwise adding chloromethyl pivalate dissolved in toluene, wherein the molar ratio of the chloromethyl pivalate to the potassium carbonate to the phase transfer catalyst is 1:1.05: 5%, the mass ratio of the beta-cyclodextrin to the chloromethyl pivalate is 1:1.5, heating to 80 ℃ under stirring for reaction, continuing to react until the chloromethyl pivalate is completely reacted after the chloromethyl pivalate is dropwise added, recovering toluene by reduced pressure distillation after the reaction is finished, washing distillation residues with water, drying in vacuum, crushing and sieving to obtain the modified cyclodextrin.

(3) Dropwise adding eucalyptus essential oil dissolved in ethanol into the modified cyclodextrin prepared in the step (2) under stirring, wherein the mass ratio of the modified cyclodextrin to the eucalyptus essential oil is 1:1, and the volume ratio of the eucalyptus essential oil to the ethanol is 1:5, uniformly mixing, introducing into a granulator, granulating, and sieving to obtain the anti-mite microcapsule.

(4) Adding acrylic resin emulsion MSDS and anti-mite microcapsules into water, wherein the mass ratio of the acrylic resin emulsion MSDS to the anti-mite microcapsules is 5:1, the dosage of the anti-mite microcapsules is 3g per 100g of antibacterial modified organic cotton fibers, uniformly mixing to obtain slurry, carding and lapping the antibacterial modified organic cotton fibers prepared in the step (1) to form a fiber web, spraying the slurry on the surface of the fiber web, drying and reinforcing to obtain the non-woven fabric.

(5) And (4) processing the non-woven fabric prepared in the step (4) into an antibacterial anti-mite swaddling article.

Example 3

(1) Firstly, dissolving carboxymethyl chitosan and silicotungstic acid in water to prepare an antibacterial treatment solution, wherein the mass concentration of the carboxymethyl chitosan contained in the impregnation solution is 2.5%, and the dosage of the silicotungstic acid is 0.5% of the mass of the carboxymethyl chitosan, then impregnating the organic cotton fiber in the antibacterial treatment solution for 1h at the temperature of 50 ℃, taking out the organic cotton fiber, and heating and drying the organic cotton fiber at the temperature of 90 ℃ to obtain the antibacterial modified organic cotton fiber.

(2) Dissolving beta-cyclodextrin and potassium carbonate in hot water at 80 ℃, adding dodecyl trimethyl ammonium chloride, then dropwise adding chloromethyl pivalate dissolved in toluene, wherein the molar ratio of the chloromethyl pivalate to the potassium carbonate to a phase transfer catalyst is 1:1: 5%, the mass ratio of the beta-cyclodextrin to the chloromethyl pivalate is 1:2, heating to 80 ℃ under stirring for reaction, continuing to react until the chloromethyl pivalate is completely reacted after the chloromethyl pivalate is dropwise added, ending the reaction, carrying out reduced pressure distillation to recover toluene, washing distillation residues, carrying out vacuum drying, crushing, and sieving to obtain the modified cyclodextrin.

(3) Dropwise adding eucalyptus essential oil dissolved in ethanol into the modified cyclodextrin prepared in the step (2) under stirring, wherein the mass ratio of the modified cyclodextrin to the eucalyptus essential oil is 1:2, and the volume ratio of the eucalyptus essential oil to the ethanol is 1:4, uniformly mixing, introducing into a granulator, granulating, and sieving to obtain the anti-mite microcapsule.

(4) Adding acrylic resin emulsion MSDS and anti-mite microcapsules into water, wherein the mass ratio of the acrylic resin emulsion MSDS to the anti-mite microcapsules is 8:1, the dosage of the anti-mite microcapsules is 4g per 100g of antibacterial modified organic cotton fiber, uniformly mixing to obtain slurry, carding and lapping the antibacterial modified organic cotton fiber prepared in the step (1) to form a fiber web, spraying the slurry on the surface of the fiber web, drying and reinforcing to obtain the non-woven fabric.

(5) And (4) processing the non-woven fabric prepared in the step (4) into an antibacterial anti-mite swaddling article.

Comparative example 1

Comparative example 1 is the same as example 1 except that silicotungstic acid in example 1 is removed.

(1) Firstly, dissolving carboxymethyl chitosan in water to prepare an antibacterial treatment solution, wherein the mass concentration of the carboxymethyl chitosan contained in the impregnation solution is 2%, then impregnating the organic cotton fiber in the antibacterial treatment solution for 1.5h at the temperature of 40 ℃, taking out the organic cotton fiber, and heating and drying the organic cotton fiber at the temperature of 80 ℃ to obtain the antibacterial modified organic cotton fiber.

(2) Dissolving beta-cyclodextrin and potassium carbonate in hot water at 80 ℃, adding dodecyl trimethyl ammonium chloride, then dropwise adding chloromethyl pivalate dissolved in toluene, wherein the molar ratio of the chloromethyl pivalate to the potassium carbonate to the dodecyl trimethyl ammonium chloride is 1:1: 3%, the mass ratio of the beta-cyclodextrin to the chloromethyl pivalate is 1:1.5, heating to 80 ℃ under stirring for reaction, continuing the reaction until the chloromethyl pivalate is completely reacted after the chloromethyl pivalate is dropwise added, ending the reaction, carrying out reduced pressure distillation to recover toluene, washing distillation residues, carrying out vacuum drying, crushing, and sieving to obtain the modified cyclodextrin.

(3) Dropwise adding eucalyptus essential oil dissolved in ethanol into the modified cyclodextrin prepared in the step (2) under stirring, wherein the mass ratio of the modified cyclodextrin to the eucalyptus essential oil is 1:1, and the volume ratio of the eucalyptus essential oil to the ethanol is 1:3, uniformly mixing, introducing into a granulator, granulating, and sieving to obtain the anti-mite microcapsule.

(4) Adding acrylic resin emulsion MSDS and anti-mite microcapsules into water, wherein the mass ratio of the acrylic resin emulsion MSDS to the anti-mite microcapsules is 10:1, the dosage of the anti-mite microcapsules is 5g per 100g of antibacterial modified organic cotton fibers, uniformly mixing to obtain slurry, carding and lapping the antibacterial modified organic cotton fibers prepared in the step (1) to form a fiber web, spraying the slurry on the surface of the fiber web, drying and reinforcing to obtain the non-woven fabric.

(5) And (4) processing the non-woven fabric prepared in the step (4) into an antibacterial anti-mite swaddling article.

Comparative example 2

Comparative example 2 was the same as example 1 except that the modified cyclodextrin in example 1 was replaced with cyclodextrin which was not modified.

(1) Firstly, dissolving carboxymethyl chitosan and silicotungstic acid in water to prepare an antibacterial treatment solution, wherein the mass concentration of the carboxymethyl chitosan contained in the impregnation solution is 2%, and the dosage of the silicotungstic acid is 0.25% of the mass of the carboxymethyl chitosan, then impregnating the organic cotton fiber in the antibacterial treatment solution for 1.5h at the temperature of 40 ℃, taking out the organic cotton fiber, and heating and drying the organic cotton fiber at the temperature of 80 ℃ to obtain the antibacterial modified organic cotton fiber.

(2) Dropwise adding eucalyptus essential oil dissolved in ethanol into the cyclodextrin under stirring, wherein the mass ratio of the cyclodextrin to the eucalyptus essential oil is 1:1, and the volume ratio of the eucalyptus essential oil to the ethanol is 1:3, uniformly mixing, introducing into a granulator, granulating, and sieving to obtain the anti-mite microcapsule.

(3) Adding acrylic resin emulsion MSDS and anti-mite microcapsules into water, wherein the mass ratio of the acrylic resin emulsion MSDS to the anti-mite microcapsules is 10:1, the dosage of the anti-mite microcapsules is 5g per 100g of antibacterial modified organic cotton fibers, uniformly mixing to obtain slurry, carding and lapping the antibacterial modified organic cotton fibers prepared in the step (1) to form a fiber web, spraying the slurry on the surface of the fiber web, drying and reinforcing to obtain the non-woven fabric.

(4) And (4) processing the non-woven fabric prepared in the step (3) into an antibacterial anti-mite swaddling article.

The antibacterial anti-mite swaddling articles prepared in the examples and the comparative examples were subjected to antibacterial anti-mite performance tests.

The test of the antibacterial performance conforms to the standard GB/T20944.3-2008, and the test of the anti-mite performance conforms to the standard GB/T24253-2009. Wherein, the water washing method refers to the standard GB/T3921.3-1997.

The test results are shown in the following table.

As can be seen from the data in the above table, the water washing resistance of the antibacterial effect can be enhanced by fixing carboxymethyl chitosan on cotton fiber through chemical bonds, and the water washing resistance of the anti-mite effect can be enhanced by chemically modifying cyclodextrin with chloromethyl pivalate.

The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.