CN111035580B - Preparation method of liquid medicine system of low-permeability wet tissue - Google Patents
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/731—Cellulose; Quaternized cellulose derivatives
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- A—HUMAN NECESSITIES
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- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/0208—Tissues; Wipes; Patches
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/29—Titanium; Compounds thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/736—Chitin; Chitosan; Derivatives thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/10—Washing or bathing preparations
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/52—Stabilizers
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- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/84—Products or compounds obtained by lyophilisation, freeze-drying
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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Abstract
The invention relates to the technical field of wet tissues, in particular to a preparation method of a low-seepage wet tissue liquid medicine system, which comprises wet tissue liquid medicine and nano-scale cellulose accounting for 0.04-0.2% of the mass fraction of the wet tissue liquid medicine, wherein after the nano-scale cellulose is added into the wet tissue liquid medicine, triethanolamine is used for adjusting the pH value of the liquid medicine system to be 9.0-9.5 at normal temperature, so that the nano-scale cellulose can be uniformly dispersed and can not generate agglomeration, citric acid is used for adjusting the pH value of the liquid medicine system to be 4.5-5.5 to form a stable low-seepage liquid medicine system, and the rotational viscosity of the system is controlled to be 200-Pa.s and 300 Pa.s. The nano-cellulose is utilized to effectively improve the viscosity of the wet tissue liquid medicine, reduce the fluidity of the wet tissue liquid medicine, reduce the infiltration condition of the wet tissue liquid medicine, simultaneously have fresh hand feeling, do not have the sticky hand feeling problem of the conventional thickening agent, can be compounded with most of antiseptic and bactericidal agents for use, and has wide application range.
Description
Technical Field
The invention relates to the technical field of wet tissues, in particular to a preparation method of a liquid medicine system of a low-permeability wet tissue.
Background
At present, due to the fact that a cleaning agent and an anticorrosive bactericide are added into a liquid medicine system of 80 large-package wet tissues, the surface tension of liquid medicine is greatly reduced, the liquidity of the liquid medicine is increased, infiltration is easy to generate, the upper-layer wet tissues in the same package are dry, the bottom-layer wet tissues are wet, the liquid content of the upper-layer wet tissues is even different by more than one time, and the use of consumers is inconvenient. The conventional method is to use cellulose or carbomer thickener to increase the viscosity of the liquid medicine and reduce the fluidity of the liquid medicine to reduce the infiltration of the liquid medicine. However, the use experience of consumers is affected due to sticky hand feeling of cellulose, and carbomer is difficult to use due to the fact that carbomer collides with most of antiseptic bactericides in an ionic manner.
Disclosure of Invention
The invention aims to overcome the defects and provide a preparation method of a liquid medicine system of a low-permeability wet towel.
In order to achieve the purpose, the technical solution of the invention is as follows:
a preparation method of a liquid medicine system of a low-permeability wet tissue comprises a wet tissue liquid medicine and nano-scale cellulose accounting for 0.04-0.2% of the mass fraction of the wet tissue liquid medicine, wherein after the nano-scale cellulose is added into the wet tissue liquid medicine, triethanolamine is used for adjusting the pH value of the liquid medicine system to be within a range of 9.0-9.5 at normal temperature, so that the nano-scale cellulose can be uniformly dispersed and cannot generate agglomeration, citric acid is used for adjusting the pH value of the liquid medicine system to be within a range of 4.5-5.5 to form a stable low-permeability liquid medicine system, and the rotational viscosity of the system is controlled to be 200-300 Pa.s.
Preferably, the preparation of the nano-scale cellulose comprises the following specific steps:
1) mixing cellulose powder with water to obtain a cellulose aqueous solution with the concentration of 0.01mol/L, adding nano titanium dioxide with one mass percent of the cellulose aqueous solution in a stirring state, and performing oxidative degradation for 2-3h under the irradiation of 200W ultrasonic wave radiation by a 300W xenon lamp under a vacuum condition to obtain a cellulose precursor;
2) adding sodium cyclamate into the fiber precursor in the step 1, reacting at 60-80 ℃ for 40-60min, gradually adding chitosan, and stirring at 90-100 ℃ for reacting for 2-4h to obtain a fiber suspension;
3) and (3) freeze-drying and powder grinding the cellulose suspension obtained in the step (2) to obtain the nano-cellulose.
Preferably, the preparation of the cellulose powder comprises the following specific steps:
1) pulverizing natural herba Meliloti Nudiflorae plant to 3-5 cm, mixing with 2-5 wt% sulfuric acid solution, hydrolyzing, and filtering to obtain filter residue;
2) mixing the filter residue obtained in the step 1 with 5-8 wt% of sodium hydroxide, reacting at the constant temperature of 110-130 ℃ for 1-2 h, and filtering to obtain a delignification product;
3) and (3) soaking the delignified product obtained in the step (2) into 40-70% zinc chloride aqueous solution at normal temperature, wherein the liquid ratio is 1: 25, stirring for 30-50min, filtering, washing with water to neutrality, replacing with acetone, drying, and pulverizing to obtain cellulose powder.
Preferably, the nano titanium dioxide is in a rutile type.
Preferably, the liquid medicine system at least comprises antiseptic bactericide, water, humectant and surfactant.
Preferably, the antiseptic bactericide is one or more of thiabendazole, triadimenol, miamide, morpholine derivatives and triazine compounds.
Preferably, the humectant is one or more of a polyol humectant, a hyaluronic acid humectant, an amino acid humectant, sodium pyrrolidone carboxylate, an amide humectant, a glucose ester humectant, a lactic acid or sodium lactate humectant, and a collagen humectant.
Preferably, the surfactant is one or more of an anionic surfactant, a nonionic surfactant and a zwitterionic surfactant.
By adopting the technical scheme, the invention has the beneficial effects that:
compared with common cellulose, the nano-cellulose has larger surface area, smaller volume, better adsorption property, thixotropy, rheological property and high dispersibility. The nano-cellulose is utilized to effectively improve the viscosity of the wet tissue liquid medicine, reduce the fluidity of the wet tissue liquid medicine, reduce the infiltration condition of the wet tissue liquid medicine, simultaneously have fresh hand feeling, do not have the sticky hand feeling problem of the conventional thickening agent, can be compounded with most of antiseptic and bactericidal agents for use, and has wide application range.
The crystallinity of the cellulose is reduced through zinc chloride pretreatment, a non-crystallization area is increased, and the accessibility is increased, so that the cellulose is easier to react and degrade. The cellulose is further degraded into nanoscale units by microwave-assisted photocatalytic degradation, so that the degradation rate is high, and the process is simple; crosslinking and reforming the degradation product and sodium cyclamate, and adjusting the rheological property, dispersion and other effects of the nano-cellulose; the method effectively utilizes renewable biomass resource cellulose as a raw material, has the advantages of easily obtained raw material, low cost and higher social, economic and environmental protection significance.
Detailed Description
The invention is further illustrated by the following specific examples.
Preparing nano-grade cellulose:
pulverizing natural herba Meliloti Nudiflorae plant to 3-5 cm, mixing with 2-5 wt% sulfuric acid solution, hydrolyzing, and filtering to obtain filter residue; mixing the filter residue with 5-8 wt% of sodium hydroxide, reacting at 110-; soaking the delignified product into 40-70% zinc chloride aqueous solution at normal temperature, wherein the liquid ratio is 1: 25, stirring for 30-50min, filtering, washing with water to neutrality, replacing with acetone, drying, and pulverizing to obtain cellulose powder; mixing cellulose powder with water to obtain a cellulose aqueous solution with the concentration of 0.01mol/L, adding rutile type nano titanium dioxide with one mass percent of the cellulose aqueous solution under the stirring state, and performing oxidative degradation for 2-3h under the irradiation of 200W ultrasonic radiation by a 300W xenon lamp under the vacuum condition to obtain a cellulose precursor; adding sodium cyclamate into fiber precursor, reacting at 60-80 deg.C for 40-60min, gradually adding chitosan, stirring at 90-100 deg.C, and reacting for 2-4 hr to obtain fiber suspension; and (3) freeze-drying the cellulose suspension, and grinding the powder to obtain the nano-cellulose.
Example 1
The formula of the wet tissue liquid medicine system is as follows: 3.5 percent of sodium alkyl benzene sulfonate, 1.5 percent of fatty alcohol-polyoxyethylene ether sulfuric acid, 3.5 percent of glycerol, 0.06 percent of triadimenol, 0.8 percent of nano-grade cellulose, 0.01 percent of essence and the balance of pure water.
The components of the wet tissue liquid medicine are physically mixed together, wherein after the nano-scale cellulose is added, triethanolamine is used for adjusting the pH value of a liquid medicine system to be within the range of 9.0-9.5 at normal temperature, so that the nano-scale cellulose can be uniformly dispersed and can not generate agglomeration, citric acid is used for adjusting the pH value of the liquid medicine system to be within the range of 4.5-5.5 to form a stable low-seepage liquid medicine system, and the rotational viscosity of the system is controlled to be 200-300 Pa.s.
Example 2
The formula of the wet tissue liquid medicine system is as follows: 2.5 percent of coconut oil acid monoisopropanolamide, 1.5 percent of alkyl glycoside, 0.8 percent of bisabolol, 0.5 percent of 1, 2-hexanediol, 1.2 percent of thiabendazole, 0.1 percent of nano-grade cellulose, 0.01 percent of essence and the balance of pure water.
In the present example, a wet towel solution system was prepared in the same manner as in example 1.
Example 3
The formula of the wet tissue liquid medicine system is as follows: 3.5 percent of sodium lauroyl sarcosinate, 0.7 percent of betaine, 0.5 percent of hyaluronic acid, 0.3 percent of propylene glycol, 0.5 percent of potassium sorbate, 0.5 percent of imidazole amide, 0.1 percent of nano-grade cellulose, 0.01 percent of essence and the balance of pure water.
In the present example, the wet towel solution system was prepared in the same manner as in example 1.
Example 4
The formula of the wet tissue liquid medicine system is as follows: 3.5 percent of sodium alkyl benzene sulfonate, 1.5 percent of fatty alcohol-polyoxyethylene ether sulfuric acid, 3.5 percent of glycerol, 0.06 percent of triadimenol, 0.8 percent of cellulose, 0.01 percent of essence and the balance of pure water.
In the present example, a wet towel solution system was prepared in the same manner as in example 1.
Example 5
The formula of the wet tissue liquid medicine system is as follows: 3.5 percent of sodium alkyl benzene sulfonate, 1.5 percent of fatty alcohol-polyoxyethylene ether sulfuric acid, 3.5 percent of glycerol, 0.06 percent of triadimenol, 0.01 percent of essence and the balance of pure water.
The wet tissue liquid medicine obtained in the above embodiments is subjected to a human body contact test, an anticorrosion test and a permeability test respectively, and the specific test results are shown in the following table:
examples | Human body contact test | Test for Corrosion resistance | Permeability ofAbility to test |
Example 1 | Is free of | Is free of | <5% |
Example 2 | Is composed of | Is free of | <5% |
Example 3 | Is free of | Is free of | <5% |
Example 4 | Has sticky feeling | Has mildew spot | >10% |
Example 5 | Is free of | Has mildew spot | >50% |
In the human body contact test, 30 subjects touched the nonwoven fabric cut pieces impregnated with the wet tissue solution of the present invention, respectively, and evaluation information of the subjects was collected.
The anticorrosion performance test is to carry out an outdoor exposure test on the non-woven fabric cut pieces soaked with the wet tissue liquid medicine, and the exposure standing time is 1 month.
Permeability test method: the non-woven fabric cut pieces containing 50% of viscose fibers and having the gram weight of 75gsm and the thickness of 2.5 mm are saturated and impregnated in the wet tissue liquid medicine, and after the impregnation, the non-woven fabric cut pieces are stacked in a box-packed mode, sealed and packaged, wherein the number of the stacked non-woven fabric cut pieces is 80, and the saturated weight of the liquid medicine of the single non-woven fabric cut piece is recorded. After packaging, the package was left to stand at room temperature for 30 days, and then the package was removed, and the top sheet of the nonwoven fabric cut piece was weighed to obtain the weight after standing, and the chemical loss rate (saturated weight-weight after standing)/(saturated weight-dry weight of nonwoven fabric cut piece) X100%.
From the experimental data obtained in the table above, it can be seen that: the examples 1 to 3 were excellent in touch, corrosion resistance and permeation resistance, and satisfied the production requirements.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. A preparation method of a liquid medicine system of a low-permeability wet tissue is characterized by comprising the following steps: the low-permeability liquid medicine system comprises a wet tissue liquid medicine and nano-level cellulose accounting for 0.04-0.2% of the mass fraction of the wet tissue liquid medicine, wherein after the nano-level cellulose is added into the wet tissue liquid medicine, triethanolamine is used for adjusting the pH value of the liquid medicine system to be within a range of 9.0-9.5 at normal temperature, so that the nano-level cellulose can be uniformly dispersed and cannot generate agglomeration, citric acid is used for adjusting the pH value of the liquid medicine system to be within a range of 4.5-5.5 to form a stable low-permeability liquid medicine system, and the rotational viscosity of the system is controlled to be 200-300 Pa.s.
2. The method for preparing a liquid medicine system of a low-permeability wet tissue according to claim 1, which is characterized in that: the preparation of the nano-scale cellulose comprises the following specific steps:
1) mixing cellulose powder with water to obtain a cellulose aqueous solution with the concentration of 0.01mol/L, adding nano titanium dioxide with one mass percent of the cellulose aqueous solution in a stirring state, and performing oxidative degradation for 2-3h under the irradiation of 200W ultrasonic wave radiation by a 300W xenon lamp under a vacuum condition to obtain a cellulose precursor;
2) adding sodium cyclamate into the fiber precursor in the step 1, reacting at 60-80 ℃ for 40-60min, gradually adding chitosan, and stirring at 90-100 ℃ for reacting for 2-4h to obtain a fiber suspension;
3) and (3) freeze-drying and powder grinding the cellulose suspension obtained in the step (2) to obtain the nano-cellulose.
3. The method for preparing a liquid medicine system of a low-permeability wet tissue according to claim 2, which is characterized in that: the preparation of the cellulose powder comprises the following specific steps:
1) pulverizing natural herba Meliloti Nudiflorae plant to 3-5 cm, mixing with 2-5 wt% sulfuric acid solution, hydrolyzing, and filtering to obtain filter residue;
2) mixing the filter residue obtained in the step 1 with 5-8 wt% of sodium hydroxide, reacting at the constant temperature of 110-130 ℃ for 1-2 h, and filtering to obtain a delignification product;
3) and (3) soaking the delignified product obtained in the step (2) into 40-70% of zinc chloride aqueous solution at normal temperature, wherein the liquid ratio is 1: 25, stirring for 30-50min, filtering, washing with water to neutrality, replacing with acetone, drying, and pulverizing to obtain cellulose powder.
4. The method for preparing a liquid medicine system of a low-permeability wet tissue according to claim 2, which is characterized in that: the nano titanium dioxide is in a rutile type.
5. The method for preparing a liquid medicine system of a low-permeability wet tissue according to claim 1, which is characterized in that: the liquid medicine system at least comprises antiseptic bactericide, water, humectant and surfactant.
6. The method for preparing a liquid medicine system of a low-permeability wet tissue according to claim 5, which is characterized in that: the antiseptic bactericide is one or more of thiabendazole, triadimenol, miamide, morpholine derivatives and triazine compounds.
7. The method for preparing a liquid medicine system of a low-permeability wet tissue according to claim 5, which is characterized in that: the humectant is one or more of polyalcohol humectant, hyaluronic acid humectant, amino acids humectant, sodium pyrrolidone carboxylate, amide humectant, glucose esters humectant, lactic acid or sodium lactate humectant, and collagen humectant.
8. The method for preparing a liquid medicine system of a low-permeability wet tissue according to claim 5, which is characterized in that: the surfactant is one or more of anionic surfactant, nonionic surfactant and zwitterionic surfactant.
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