CN112205431A - Antibacterial composition, antibacterial infant clothes washing liquor and preparation method thereof - Google Patents

Antibacterial composition, antibacterial infant clothes washing liquor and preparation method thereof Download PDF

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Publication number
CN112205431A
CN112205431A CN202010963377.2A CN202010963377A CN112205431A CN 112205431 A CN112205431 A CN 112205431A CN 202010963377 A CN202010963377 A CN 202010963377A CN 112205431 A CN112205431 A CN 112205431A
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essential oil
stirring
plant
emulsion
bacteriostatic
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滕晖
姜惠敏
周航
孟君
蒋加拉
邹亚丽
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Zhuzhou Qianjin Pharmaceutical Co Ltd
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Zhuzhou Qianjin Pharmaceutical Co Ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/26Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
    • A01N25/28Microcapsules or nanocapsules
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/40Liliopsida [monocotyledons]
    • A01N65/42Aloeaceae [Aloe family] or Liliaceae [Lily family], e.g. aloe, veratrum, onion, garlic or chives
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D10/00Compositions of detergents, not provided for by one single preceding group
    • C11D10/04Compositions of detergents, not provided for by one single preceding group based on mixtures of surface-active non-soap compounds and soap
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/29Sulfates of polyoxyalkylene ethers
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/662Carbohydrates or derivatives
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/66Non-ionic compounds
    • C11D1/72Ethers of polyoxyalkylene glycols

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
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  • Agronomy & Crop Science (AREA)
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  • Dentistry (AREA)
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  • Pest Control & Pesticides (AREA)
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Abstract

The invention discloses an antibacterial composition, which is prepared by compounding piroctone olamine with specific plant essential oil, can ensure that the inhibition rate on escherichia coli, candida albicans and staphylococcus aureus is not lower than 50%, and further develops a weakly acidic antibacterial infant clothes washing liquid based on the antibacterial composition.

Description

Antibacterial composition, antibacterial infant clothes washing liquor and preparation method thereof
Technical Field
The invention relates to the technical field of daily chemicals, in particular to a bacteriostatic composition, bacteriostatic infant clothes washing liquor and a preparation method thereof.
Background
The skin of the infant and the skin of the adult have different physiological characteristics, the skin is more delicate and tender when the infant and the adult age are smaller, the thickness of the skin is only one tenth of that of the adult, the capability of resisting external stimulation is weak, the immune system is not complete, the body resistance is poor, the skin is protected only by a natural weak acid protective film of the skin after birth, and skin allergy easily occurs. With the improvement of living standard and the improvement of consumption consciousness of people, aiming at the infinite special products for infants, the infant clothes washing liquid is taken as the subdivision product of the laundry detergent, the market share is improved year by year in recent years, and the infant clothes washing liquid is highly concerned by mothers all the time, and cares clothes worn next to skin by babies 24 hours each day.
Infant's clothing lotion is protecting baby indirectly to a certain extent, especially when baby's sweat volume increases, if sweat stain, milk stain and other dirt that remain on the clothes can not get timely washing, breed the bacterium very easily, will harm baby's health and skin health at last, therefore infant's clothing lotion need reach to clothing stronger soil-removing power and lasting antibacterial effect.
Aiming at the characteristics of delicate skin and easy stimulation of infants, compared with the laundry detergent for adults, the laundry detergent for infants pays more attention to the performances in the aspects of safety, greenness, mildness, bacteriostasis, detergency and the like, because the anionic surfactant as the decontamination component in the laundry detergent is easy to inactivate under the weak acidic condition, the decontamination capability of the laundry detergent is reduced, therefore, most of the prior infant clothes washing liquor is neutral or weakly alkaline in order to realize better decontamination effect, for example, Chinese patent with publication number CN109957470A provides a natural amino acid surfactant concentrated infant clothing lotion and a preparation method thereof, the pH value of the laundry detergent is 6.5-7.5, the laundry detergent is weakly acidic, if residues exist after the laundry detergent is used, a certain stimulation effect can be caused on delicate skin of an infant, and when the stimulation times are too many, eczema can be more easily caused, and even red blood streak and the like can appear. In addition, chinese patent publication No. CN107541360A provides a green and environmentally friendly laundry detergent for infants, which has a strong detergency, but contains a high content of protease, and is also at risk of causing irritation to the skin of infants.
Therefore, the infant clothes washing liquor with weak acidity, strong decontamination capability and good bacteriostatic effect is urgently needed to be developed.
Disclosure of Invention
The invention aims to provide mild and non-irritant infant clothes washing liquor which has high detergency under a weak acid condition and is superstrong and lasting in bacteriostasis. The inventor firstly discovers that the bacteriostasis effect of the plant essential oil can be remarkably improved by compounding the piroctone olamine salt with the specific plant essential oil, and the bacteriostasis rate to escherichia coli, candida albicans and staphylococcus aureus is higher than 50 percent; based on the antibacterial composition, an infant clothes washing liquid is developed, and the clothes washing liquid keeps high detergency under a weak acid system, has an ultra-strong and lasting antibacterial effect, and is mild and non-irritant.
The invention aims to provide a bacteriostatic composition.
The invention also aims to provide the infant clothes washing lotion with weak acid bacteriostasis.
It is still another object of the present invention to provide a method for preparing the above laundry detergent liquid.
The above purpose of the invention is realized by the following technical scheme:
the invention provides a bacteriostatic composition, which is prepared from the following components in parts by mass of 0.1-0.3: 0.05-0.2: 0.05-0.1: 0.1-0.3: 0.05-0.1 of piroctone olamine salt, honeysuckle flower essential oil, aloe essential oil, folium artemisiae argyi essential oil and grapefruit essential oil.
Preferably, the bacteriostatic composition is prepared from the following components in a mass ratio of 0.2: 0.1: 0.08: 0.2: 0.08 of piroctone olamine salt, honeysuckle flower essential oil, aloe essential oil, argyi leaf essential oil and grapefruit essential oil.
The plant essential oil component has the property of inhibiting or killing certain microorganisms, and can be used as natural bacteriostatic agent. In order to develop a natural bacteriostatic agent for infant clothes lotion, an inventor preliminarily determines honeysuckle flower essential oil, aloe essential oil, folium artemisiae argyi essential oil, tea tree essential oil, grapefruit essential oil, eucalyptus essential oil, chamomile essential oil, marigold essential oil, pomegranate essential oil, sweet orange essential oil and grapefruit essential oil as main bacteriostatic essential oils through a large amount of research, but most of the essential oils have strong inhibitory action on escherichia coli and staphylococcus aureus, but have very small action on candida albicans, and based on the result that pure plant essential oil is difficult to meet the requirement on bacteriostatic rate due to bacteriostasis, the inventor continuously tries to compound various bacteriostatic components such as salicylic acid, propylene glycol, lauroyl arginine ethyl hydrochloride and the essential oils, but the effects are still not ideal. Then, the ingredients which can realize better antibacterial effect by compounding with the essential oil are continuously researched, and the combination of piroctone olamine salt (OCT), honeysuckle flower essential oil, aloe essential oil, folium artemisiae argyi essential oil and grapefruit essential oil according to a specific proportion is found, so that the antibacterial rate of escherichia coli, candida albicans and staphylococcus aureus can be ensured to be higher than 50%, and the antibacterial effect of the plant essential oil is remarkably improved.
Preferably, in the antibacterial composition, the honeysuckle essential oil, the aloe essential oil, the folium artemisiae argyi essential oil and the grapefruit essential oil are prepared into microcapsules wrapping 4 kinds of essential oil, and the microcapsules taking high polymer polyvinylpyrrolidone (PVP) and plant essential oil as carriers can completely retain effective active ingredients and enhance antibacterial action; the prepared essential oil microcapsule can permeate into the fiber of the clothes to achieve the effect of continuously slowly releasing and inhibiting bacteria.
Preferably, the preparation method of the microcapsule is as follows:
s1, preparation of plant essential oil emulsion
Adding span-80 into plant essential oil, adding tween-80 into deionized water, stirring for dissolving, mixing the two, and shearing and emulsifying with ultrasonic cell pulverizer to obtain plant essential oil emulsion; the mass ratio of the plant essential oil to the span-80 to the tween-80 is 8-12: 1-3: 1; the working conditions of the ultrasonic cell crushing instrument are as follows: working time is 2s, interval time is 3s, working frequency is 300W, and emulsification is carried out for 200 times;
s2, preparing wall material mixed liquor
Weighing octenyl succinate starch, polyvinylpyrrolidone and maltodextrin, adding into deionized water, and stirring to prepare a wall material mixed solution; the mass ratio of the octenyl succinate starch to the polyvinylpyrrolidone to the maltodextrin is 2-4: 2-4: 1; the stirring is carried out at the rotating speed of 400rpm for 2-5 min;
s3, preparation of core-wall mixed emulsion
Slowly dripping the prepared wall material mixed solution into a prepared plant essential oil emulsion, stirring at 8000rpm for 5-10 min for complex coacervation reaction, and finally dripping 0.1-2% glutaraldehyde for curing for 30min to prepare a plant bacteriostatic microcapsule core-wall mixed emulsion;
s4, preparation of microcapsule emulsion
Carrying out colloid milling on the prepared core-wall mixed emulsion, and homogenizing for 3 times under the pressure of 30MPA to obtain plant bacteriostatic microcapsule emulsion;
preferably, the mass ratio of the plant essential oil to the span-80 to the tween-80 is 10: 2: 1.
preferably, the mass ratio of the octenyl succinate starch to the polyvinylpyrrolidone to the maltodextrin is 3: 3: 1.
preferably, the glutaraldehyde is added in an amount of 1%.
The invention also provides weakly acidic bacteriostatic infant clothing washing liquor which comprises the following components in percentage by mass: 21-32.5% of surfactant, 1.5-5% of plant detergent, 0.3-0.8% of protease, 0.1-0.5% of saponifier, 0.25-1.0% of antibacterial composition, 0.05-0.1% of preservative, 0.1-0.5% of calcium-magnesium ion chelating agent, pH regulator for regulating the pH value to 5-7 and the balance of water;
the surfactant comprises the following components in a mass ratio of 2-4.5: 13-18: 6-10 of coconut oil fatty acid diethanolamide, Texapon N70 and AEO 9.
Coconut oil diethanolamide in the formula of the infant clothing washing liquid belongs to a nonionic surfactant, and is compounded with Texapon N70 and AEO9, and vegetable detergents, namely coconut oil acid, lauryl glucoside and protease are used, so that the decontamination effect is enhanced; the infant clothing washing liquid is matched with a specific surfactant, a natural plant detergent, protease and a saponifier, namely potassium hydroxide to serve as a decontamination formula, and the decontamination capability of the infant clothing washing liquid is equivalent to that of the infant clothing washing liquid under a weak alkaline condition under the weak acidic condition of the system; the specific natural plant essential oil formula is added into the antibacterial formula, compared with other plant essential oil formulas, the antibacterial effect of the clothes washing liquid system is better, the components of the whole formula system have strong detergency, are natural, mild and non-irritant, have good antibacterial effect, and are easy to clean, clean and free of residues on the decontamination components.
Preferably, the plant detergent comprises the following components in a mass ratio of 0.5-2: 1-3 of coconut oleic acid and lauryl glucoside.
Preferably, the protease is Medley Advance 300L.
Preferably, the saponifier is potassium hydroxide.
Further preferably, the dosage ratio of the saponifier potassium hydroxide to the coconut oil acid is 0.1-0.5: 0.5 to 2.
Preferably, the preservative is morsop K15.
Preferably, the calcium and magnesium ion chelating agent is disodium edetate.
Preferably, the pH adjusting agent is citric acid or sorbic acid. Citric acid is most preferred, and is used as a pH regulator of the system, and deionized water is used for preparing a solution when the citric acid is used, so that calcium and magnesium ions in hard water can be dissolved, and the citric acid can be used as a chelating agent and the pH regulator.
Preferably, the pH is adjusted to 5-6.8.
Most preferably, the pH is adjusted to 6.5.
The invention also provides a preparation method of the laundry detergent, which is characterized by comprising the following steps:
s1, putting deionized water, a chelating agent, coconut oil fatty acid diethanolamide, Texapon N70 and coconut oil acid into an emulsifying pot, starting stirring at the stirring speed of 30rpm, heating the emulsifying pot to 80-85 ℃, and preserving heat for 15-20 min;
s2, cooling to 65-70 ℃, sequentially adding AEO9 and lauryl glucoside, continuously stirring at a stirring speed of 30rpm until the mixture is completely uniform and has no particles, and keeping the temperature for 15-20 min;
s3, cooling to 55-60 ℃, putting the potassium hydroxide into an emulsifying pot, vacuumizing and stirring until the potassium hydroxide is completely and uniformly dissolved, and continuing stirring for 10-20 min under heat preservation;
s4, cooling to 40-48 ℃, adding protease Medley Advance 300L and preservative Morpu K15, and uniformly stirring;
s5, adding piroctone olamine salt and plant essential oil microcapsules, and stirring the emulsion uniformly;
s6, cooling to 35-40 ℃, and adding a pH regulator to regulate the pH.
The bacteriostasis of the invention refers to inhibiting escherichia coli and/or candida albicans and/or staphylococcus aureus.
The honeysuckle essential oil, the aloe essential oil and the folium artemisiae argyi essential oil can be purchased from the market and can also be prepared by self.
Compared with the prior art, the invention has the following beneficial effects:
(1) the piroctone olamine salt is compounded with the specific plant essential oil, so that the bacteriostasis rate of the piroctone olamine salt to escherichia coli, candida albicans and staphylococcus aureus is not lower than 50%.
(2) According to the weakly acidic bacteriostatic infant clothing washing liquid developed by the invention, a specific surfactant, a natural plant detergent and protease are matched as a decontamination formula, and under the condition that the system is weakly acidic, the detergency of the washing liquid is equivalent to that of the washing liquid under the weak alkaline condition, so that the washing liquid is more suitable for delicate skin of an infant; and a specific natural plant essential oil formula is added into the bacteriostatic formula, so that compared with other plant essential oil formulas, the bacteriostatic effect of the clothing washing lotion system is better, and the bacteriostatic effect of the clothing washing lotion system is especially good for inhibiting escherichia coli, staphylococcus aureus and candida albicans; the plant bacteriostatic formula is further prepared into a microcapsule form and added into a clothes washing liquid system, and the essential oil microcapsule can permeate into clothes fibers to achieve the effect of continuously slowly releasing and inhibiting bacteria. The components of the whole formula system have strong detergency, weak acidity, mildness, no irritation and strong bacteriostatic effect, and the decontamination components in the clothes washing liquor product are easy to clean, clean and free of residues.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1 study of bacteriostatic formulations
1. The bacteriostasis detection is carried out on different plant essential oil combinations according to QB/T2850-2007 standard, as shown in Table 1.
TABLE 1
Figure BDA0002681375200000051
Figure BDA0002681375200000061
The results in Table 1 show that the formula of each group of essential oils has strong inhibitory effect on Escherichia coli and Staphylococcus aureus, but has little effect on Candida albicans. Therefore, the pure essential oil bacteriostasis system cannot simultaneously achieve the bacteriostasis rate of at least 50 percent on escherichia coli, candida albicans and staphylococcus aureus.
2. Based on the fact that pure essential oil cannot meet the requirement on the bacteriostasis rate, the cooperation of piroctone olamine salt (OCT) and plant essential oil is discovered through exploration, the bacteriostasis rate of escherichia coli, candida albicans and staphylococcus aureus can be guaranteed to be not less than 50%, and the bacteriostasis effect can be remarkably improved by compounding with the essential oil. The bacteriostasis experiment is carried out according to the QB/T2850-2007 standard, and the specific data are shown in the table 2.
TABLE 2
Figure BDA0002681375200000071
Figure BDA0002681375200000081
From the bacteriostatic results in table 2, it can be seen that the combination of piroctone olamine salt, honeysuckle essential oil, aloe essential oil, artemisia leaf essential oil and grapefruit essential oil can achieve better bacteriostatic effect.
2. The mass ratio of piroctone olamine salt to honeysuckle essential oil, aloe essential oil, artemisia leaf essential oil and grapefruit essential oil was further optimized by a single factor experiment and an orthogonal experiment, as shown in table 3.
TABLE 3
Figure BDA0002681375200000082
Figure BDA0002681375200000091
From the bacteriostatic effect of table 3, the mass ratio of the piroctone olamine salt to the honeysuckle essential oil, the aloe essential oil, the folium artemisiae argyi essential oil and the grapefruit essential oil can be controlled to be 0.1-0.3: 0.05-0.2: 0.05-0.1: 0.1-0.3: 0.05 to 0.1; wherein the optimal mass ratio is 0.2: 0.1: 0.08: 0.2: 0.08.
example 2 plant essential oil microcapsule study
1. Material
(1) Core material: the optimal mass ratio is 0.2: 0.1: 0.08: 0.2: taking four plant essential oils in the bacteriostatic group of 0.08 as an example for experiment;
(2) the wall materials are octenyl succinate starch, polyvinylpyrrolidone and maltodextrin;
(3) the emulsifier is span-80 and tween-80;
(4) the curing agent is glutaraldehyde.
2. Preparation method (1) preparation of plant essential oil emulsion
Adding span-80 into plant essential oil, adding tween-80 into deionized water, stirring for dissolving, mixing the two, and shearing and emulsifying with ultrasonic cell pulverizer to obtain plant essential oil emulsion;
(2) preparation of wall material mixed liquid
Weighing octenyl succinate starch, polyvinylpyrrolidone and maltodextrin, adding into deionized water, and stirring to prepare a wall material mixed solution;
(3) preparation of core-wall mixed emulsion
Slowly dripping the prepared wall material mixed solution into the prepared plant essential oil emulsion, stirring for complex coacervation reaction, and finally dripping glutaraldehyde for curing to prepare the deodorant microcapsule core wall mixed emulsion;
(4) preparation of plant bacteriostatic microcapsule emulsion
Carrying out colloid milling on the prepared core-wall mixed emulsion, and homogenizing to obtain a preparation antibacterial microcapsule emulsion;
3. preparation optimization of plant bacteriostatic essential oil microcapsules
(1) Effect of emulsifiers on stability of vegetable oil emulsions
1) Experimental methods
Respectively using span-80 and tween-80 in different mass ratios to prepare the plant bacteriostatic essential oil emulsion, calculating hydrophilic-lipophilic balance value HLB of different mass ratios of the plant bacteriostatic essential oil compound emulsifier according to a formula, and then observing the stability of the emulsion to determine the optimal HLB value.
Wherein the stability is divided into standing stability and centrifugal stability, namely, whether the emulsion is layered or not is observed under the conditions of standing for a day and a night and centrifugation for 5min at the rotation speed of a centrifugal machine of 4000 r/min.
The formula for calculating the mixed HLB value of the compound emulsifier is as follows:
HLBa,b=HLBa×A%+HLBb×B%。
in the above formula: HLBa, b — HLB value of mixed emulsifier; HLBa — HLB value of emulsifier a; HLBb — HLB value of emulsifier b; a% -the mass fraction thereof in the mixture; b% -the mass fraction thereof in the mixture. Mixture refers to a mixture of emulsifiers. (the HLB of span-80 is 4.3, and the HLB of Tween-80 is 15.)
2) Results of the experiment
TABLE 4 influence of the mass ratio of emulsifiers on the emulsion stability
Span-80: tween-80 1:2 1:1.5 1:1 1.5:1 2:1 2.5:1
Mixed HLB value 11.5 10.7 9.6 8.6 7.9 7.4
Stability of standing Not layering Not layering Not layering Not layering Not layering Not layering
Centrifugal stability Layering Layering Not layering Not layering Not layering Slightly delaminated
As a result, as shown in Table 4, when the HLB value of the mixture was less than 7.9, the emulsion was free from the phenomenon of separation after standing for one day and night, and had good stability and oil droplets on the surface after centrifugation; when the HLB value is more than 9.6, the emulsion has no layering phenomenon after standing for a day and a night, the emulsion has layering of different degrees after centrifugation, and the centrifugal stability is increasingly poor along with the increase of the HLB value: when the HLB value is 7.9-9.6, no layering phenomenon occurs in the emulsion after standing and centrifuging, so that the HLB value of the plant mixed essential oil is determined to be 7.9-9.6, and the stability of the essential oil emulsion is optimal, namely span-80: the mass ratio of the tween-80 is 1-2: 1, the stability is the best.
(2) Embedding rate of plant bacteriostatic essential oil microcapsule emulsion prepared from wall material mixed solution consisting of different mass ratios
1) Method for measuring embedding rate of microcapsules
And (3) microcapsule surface oil determination: accurately weighing 2g of sample (accurately to 0.001g) m to a triangular flask m1 with constant weight, adding 15mL of petroleum ether (boiling range of 30-60 ℃), oscillating at intervals, extracting for 10min, filtering the sample by using filter paper, leaching for 3 times, washing the triangular flask and the filter paper by using 10mL of petroleum ether, combining filtrates, placing the filtrates in a dried and weighed heart-shaped flask, carrying out vacuum spin-drying at 30 ℃, cooling and weighing m 2.
Surface oil content%
And (3) total oil determination: accurately weighing 2g of sample, dissolving in 10mL of 60 ℃ hot water, adding alpha-amylase, carrying out water bath at 60 ℃ for 10min, hydrolyzing starch in microcapsule wall materials, and releasing essential oil. After cooling, adding chloroform/methanol (15/30mL) mixture, shaking for 10min, adding 15mL chloroform, shaking for 2min, adding 15mL deionized water, shaking for 5min, pouring into a centrifuge cup, centrifuging at 4200r/min for 5min, taking the lower layer liquid, placing in a dried and weighed round bottom flask, and vacuum-drying at 30 ℃.
The inclusion rate%
Scanning the prepared plant bacteriostatic essential oil microcapsule emulsion by adopting an electron scanning microscope, and observing the microscopic morphology of the plant bacteriostatic essential oil microcapsule.
2) Results of the experiment
Octenyl succinated starch, polyvinylpyrrolidone, maltodextrin were selected for testing in various ratios, with a total mass of about 50g, as shown in table 5:
TABLE 5
Ratio of Embedding rate
4:4:1 97.3
3:3:1 98.6
2:2:1 96.2
1:1:2 92.7
1:1:4 71.6
1:1:8 58.4
The results are shown in table 5, with an octenyl succinated starch, polyvinylpyrrolidone, maltodextrin ratio of 4: 4: 1,3: 3: 1,2: 2: 1,1: 1: 2, the embedding rate is more than 90%, respectively 97.3%, 98.6%, 96.2% and 92.7%, wherein the proportion is 3: 3: the embedding rate is higher when 1 hour is used, and is obviously larger than the rate of 1: 1: 2 (92.7%), 1: 1: 4 (71.6%), 1: 1: embedding rate at 8 (58.4%). Thus, the mass ratio of the octenyl succinate starch to the polyvinylpyrrolidone to the maltodextrin wall material is determined to be 2-4: 2-4: 1, most preferably 3: 3: 1. the reason may be that octenyl succinate starch and polyvinylpyrrolidone are amphiphilic macromolecules, and a certain proportion of micromolecular maltodextrin is added to fill macromolecular cross-linking gaps so as to improve the embedding rate, but when the micromolecules are excessive, the embedding rate is reduced because the micromolecules do not have amphipathy and cannot form a macromolecular framework wall capsule structure.
(4) Embedding rate of plant bacteriostatic essential oil microcapsule emulsion prepared from curing agents with different mass ratios and particle size distribution of microcapsules
The plant bacteriostatic essential oil microcapsule emulsions were prepared with the addition amounts of glutaraldehyde curing agent (mass ratio of glutaraldehyde to the total amount of the wall material mixture and the plant bacteriostatic essential oil emulsion) of 0.1%, 0.2%, 0.3%, 0.4%, 1%, 2%, 3%, and 4%, respectively, and the results are shown in table 6.
TABLE 6
Glutaraldehyde addition amount% The embedding rate% Average particle diameter of nm
0.1 96.9 280
0.2 97.4 270
0.3 97.2 260
0.4 96.8 250
1 98.2 200
2 95.8 300
3 81.7 500
4 78.6 800
As shown in Table 6, the embedding rate of the microcapsules decreased gradually as the amount of glutaraldehyde added increased, and the embedding rate was 95.8% or more for each of the 0.1% to 2% amounts, and was significantly decreased (81.7% and 78.6%) for each of the 3% and 4% amounts. The average particle size of the emulsion is firstly reduced and then increased along with the increase of the addition amount of the glutaraldehyde, and when the addition amount is 1%, the average particle size of the emulsion is the smallest, the dispersion is the most uniform, and the stability of the emulsion is the highest. It can be concluded from the table that the smaller the average particle size of the emulsion, the more stable the emulsion and the higher the embedding rate of the obtained microcapsules, because too little glutaraldehyde has poor curability and cannot form a stable emulsion; excessive glutaraldehyde causes excessive aggregation of macromolecular wall materials, flocculation is formed, and the stability of the emulsion is reduced. Therefore, the addition amount of glutaraldehyde is 0.1 to 2%, and the optimum addition amount is 1%.
(5) Embedding rate of plant bacteriostatic essential oil microcapsule emulsion and particle size distribution of microcapsules under action of colloid rods with different homogenization pressures and different homogenization times
In the preparation of microcapsule emulsions, when the homogenization pressure was 20, 25, 30, 35, 40 and the number of homogenization times was 1, 2, 3, 4, the embedding rate and the particle size distribution of the prepared microcapsule emulsion liquid were as shown in table 7.
TABLE 7
Figure BDA0002681375200000131
As shown in Table 7, the homogeneous pressure was 20 to 40mPa, the embedding rate increased with increasing pressure, and the embedding rate decreased with increasing pressure and higher than 35 mPa. The embedding rate is highest (98.2%) at 30mPa, and only 94.8% at 20mPa homogenization. This phenomenon occurs in relation to the degree of shear break of the emulsion.
The embedding rate is obviously increased along with the increase of the homogenization times. At 30mPa, the embedding rate of 3 and 4 homogenizations is 98.2% and 97.3%, respectively, which is significantly higher than that of 1 and 2 homogenizations (87.6% and 94.6%). The homogenizing times are increased, the shearing and crushing degree of the emulsion is higher, the combination of the wall material and the core material is firmer, the embedding rate is higher, and the homogenizing is selected for 3 times.
Examples 3-7 study of bacteriostatic laundry detergent for infant clothes
1. In table 8 are different formulations of laundry lotion.
TABLE 8
Figure BDA0002681375200000141
The honeysuckle essential oil, the aloe essential oil, the wormwood essential oil and the grapefruit essential oil in the antibacterial formula are prepared into microcapsules wrapping the four essential oils. The preparation method of the microcapsule comprises the following steps:
s1, preparation of plant essential oil emulsion
Adding 20g of span-80 into 100g of plant essential oil, adding 10g of tween-80 into 30g of deionized water, stirring to fully dissolve the two, uniformly mixing the two, and shearing and emulsifying by an ultrasonic cell crusher to form plant essential oil emulsion; the working conditions of the ultrasonic cell crushing instrument are as follows: working time is 2s, interval time is 3s, working frequency is 300W, and emulsification is carried out for 200 times;
s2, preparing wall material mixed liquor
Weighing 10.8g of octenyl succinate starch, 10.8g of polyvinylpyrrolidone and 3.6g of maltodextrin, adding into 25g of deionized water, and stirring at the rotating speed of 400rpm for 4min to prepare a wall material mixed solution;
s3, preparation of core-wall mixed emulsion
Slowly dripping the prepared wall material mixed solution into a prepared plant essential oil emulsion, stirring at 8000rpm for 5-10 min for complex coacervation reaction, and finally dripping 2.1g of glutaraldehyde for curing for 30min to prepare a plant bacteriostatic microcapsule core-wall mixed emulsion;
s4, preparation of plant bacteriostatic microcapsule emulsion
And (3) carrying out colloid milling on the prepared core-wall mixed emulsion, and homogenizing for 3 times under the pressure of 30mPa to obtain the plant bacteriostatic microcapsule emulsion.
2. Preparation of laundry lotion
(1) EXAMPLE 3 preparation of laundry detergent
S1, putting deionized water, a chelating agent, coconut oil fatty acid diethanolamide, Texapon N70 and coconut oil acid into an emulsifying pot, starting stirring at the stirring speed of 30rpm, heating the emulsifying pot to 80 ℃, preserving heat for 15min, and beginning cooling;
s2, cooling to 70 ℃, sequentially adding AEO9 and lauryl glucoside, continuously stirring at the stirring speed of 30rpm until the mixture is completely uniform and has no particles, preserving the heat for 15min, and beginning to cool;
s3, cooling to 60 ℃, putting the potassium hydroxide into an emulsifying pot, vacuumizing and stirring until the potassium hydroxide is completely and uniformly dissolved, continuing to keep the temperature and stirring for 10min, and then cooling;
s4, cooling to 48 ℃, adding protease Medley Advance 300L and preservative Morpu K15, and stirring uniformly;
s5, adding piroctone olamine salt, plant essential oil microcapsules and essence, and uniformly stirring;
s6, cooling to 40 ℃, and adjusting the pH to 6.5 by using citric acid to obtain the clothes washing liquid.
(2) EXAMPLE 4 preparation of laundry detergent
The preparation method of example 4 is the same as example 3, except that the temperature is raised to 85 ℃ in the step of S1 in the preparation of the laundry detergent solution, and the temperature is maintained for 20 min.
(3) EXAMPLE 5 preparation of laundry detergent
The preparation method of example 5 is the same as example 3, except that the temperature is reduced to 65 ℃ in the step of S2 in the preparation of the laundry detergent solution, and the temperature is kept for 20 min.
(4) EXAMPLE 6 preparation of laundry detergent
The preparation method of example 6 is the same as example 3, except that in the preparation of the laundry detergent solution, the temperature is reduced to 55 ℃ in the step S3, and the temperature is kept and the stirring is carried out for 20 min.
(5) EXAMPLE 7 preparation of laundry detergent
The preparation method of example 7 is the same as that of example 3, except that the temperature is decreased to 40 ℃ in the step S4 and to 35 ℃ in the step S6 in the preparation of the laundry detergent.
Comparative example 1
Comparative example 1 the laundry detergent formulation was used as in example 5 except that the pH was 7.5 and the preparation method was the same as in example 5.
Comparative example 2
Comparative example 2 the laundry detergent formulation was used in the same manner as in example 5 except that the protease Medley Advance 300L was replaced with Medley Advance 200L and the preparation was the same as in example 5.
Comparative examples 3 to 6
Comparative examples 3-6 laundry detergent formulations are shown in table 9 below, prepared according to the same method as example 5.
TABLE 9
Figure BDA0002681375200000161
Figure BDA0002681375200000171
Example 12
1. Determination of detergency of laundry detergent
Taking examples 3-7 and comparative examples 1-6 as examples, the prepared antibacterial infant laundry detergent is subjected to detergency measurement by referring to a detergency measurement method in a QB/T1224-. The washing method comprises the following steps: the dirty cloth is soaked in clean water for 3 minutes, and then is scrubbed by hands for 1 minute, and the dirty cloth is washed by direct current water. The results are given in Table 10 below.
Watch 10
Figure BDA0002681375200000172
As shown in table 10, the tomato stain (stain removal ratio), pumpkin soup stain (stain removal ratio) and oil stain (stain removal ratio) of examples 3 to 7 were higher than the stain removal ratios of the standard laundry detergent and comparative examples 2, 3 and 4, and comparative examples 1, 5 and 6 were equivalent to the stain removal effects of the examples, but the PH of comparative example 1 was 7.5, was not close to the PH of the skin of a baby, was not mild enough, and was easy to hurt hands; comparative examples 5 and 6 are similar to the examples, but the economic cost is higher than that of the examples (the cost is higher due to the large amount of the catalyst used).
2. Laundry detergent bacteriostatic ability determination
The bacteriostatic experiments of examples 3-7 and comparative examples 1-6 were carried out according to the QB/T2850-2007 standard, and the bacteriostatic results are shown in the following table 11.
TABLE 11
Figure BDA0002681375200000181
Figure BDA0002681375200000191
The results are shown in table 11, the bacteriostatic ability of examples 3-7 and comparative examples 1, 2, 5 and 6 on escherichia coli, candida albicans and staphylococcus aureus are equivalent, the bacteriostatic effect of the laundry detergent for infant clothes is affected by different pH values of comparative example 1 and different protease types of comparative example 2, the bacteriostatic effect of the laundry detergent for infant clothes is affected by different bacteriostatic formula ratios and small addition amount of comparative examples 3 and 4, and the bacteriostatic effect of the laundry detergent for infant clothes is severe due to the fact that the comparative examples 5 and 6 are equivalent to the effects of the examples, but the dosage is large and the economic cost is high.
3. Laundry detergent bacteriostatic effect stability test
The laundry detergent of example 5 was placed at 37 ℃ for three months and then tested for its bacteriostatic effect, which was tested according to QB/T2850-2007 standard, and the bacteriostatic results are shown in Table 12.
TABLE 12
Figure BDA0002681375200000192
The result shows that after the bacteriostatic infant clothes laundry detergent disclosed by the invention is placed for three months, the bacteriostatic rate is still up to 99.9%.
4. The laundry detergent of example 5 was used as an example to test safety and stability.
(1) The safety test results are shown in Table 13
Watch 13
Figure BDA0002681375200000201
(2) Laundry detergent skin irritation test of examples 3-7
Entrusted testing organization: hunan mountain and water detection Co Ltd
And (3) detection results: according to the skin irritation strength grading standard in the 'disinfection technical specification' 2002 edition, the result of the repeated complete skin irritation test of the laundry detergent on rabbits is as follows: has no irritation, and meets the requirement of 'Disinfection technical Specification' 2002 edition 2.3.13.1.
It should be finally noted that the above examples are only intended to illustrate the technical solutions of the present invention, and not to limit the scope of the present invention, and that other variations and modifications based on the above description and thought may be made by those skilled in the art, and that all embodiments need not be exhaustive. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.

Claims (10)

1. The antibacterial composition is characterized by comprising the following components in percentage by mass of 0.1-0.3: 0.05-0.2: 0.05-0.1: 0.1-0.3: 0.05-0.1 of piroctone olamine salt, honeysuckle flower essential oil, aloe essential oil, folium artemisiae argyi essential oil and grapefruit essential oil.
2. The bacteriostatic composition according to claim 1, which is prepared from the following components in a mass ratio of 0.2: 0.1: 0.08: 0.2: 0.08 of piroctone olamine salt, honeysuckle flower essential oil, aloe essential oil, argyi leaf essential oil and grapefruit essential oil.
3. The bacteriostatic composition according to claim 1 or 2, wherein the honeysuckle essential oil, the aloe essential oil, the folium artemisiae argyi essential oil and the grapefruit essential oil in the bacteriostatic composition are prepared into microcapsule emulsions wrapping 4 essential oils, and the microcapsule emulsions are prepared by the following steps:
s1, preparation of plant essential oil emulsion
Adding span-80 into plant essential oil, adding tween-80 into deionized water, stirring for dissolving, mixing, and shearing and emulsifying with ultrasonic cell pulverizer to obtain plant essential oil emulsion; the mass ratio of the plant essential oil to the span-80 to the tween-80 is 8-12: 1-3: 1; the working conditions of the ultrasonic cell crushing instrument are as follows: working time is 2s, interval time is 3s, working frequency is 300W, and emulsification is carried out for 200 times;
s2, preparing wall material mixed liquor
Weighing octenyl succinate starch, polyvinylpyrrolidone and maltodextrin, adding into deionized water, and stirring to prepare a wall material mixed solution; the mass ratio of the octenyl succinate starch to the polyvinylpyrrolidone to the maltodextrin is 2-4: 2-4: 1; the stirring is carried out at the rotating speed of 400rpm for 2-5 min;
s3, preparation of core-wall mixed emulsion
Slowly dripping the prepared wall material mixed solution into a prepared plant essential oil emulsion, stirring at 8000rpm for 5-10 min for complex coacervation reaction, and finally dripping 0.1-2% glutaraldehyde for curing for 30min to prepare a plant bacteriostatic microcapsule core-wall mixed emulsion;
s4, preparation of microcapsule emulsion
And (3) carrying out colloid milling on the prepared core-wall mixed emulsion, and homogenizing for 3 times under the pressure of 30MPA to obtain the plant bacteriostatic microcapsule emulsion.
4. The weakly acidic bacteriostatic infant clothing washing liquid is characterized by comprising the following components in percentage by mass: 21-32.5% of surfactant, 1.5-5% of plant detergent, 0.3-0.8% of protease, 0.1-0.5% of saponifier, 0.25-1.0% of bacteriostatic composition according to claim 3, 0.05-0.1% of preservative, 0.1-0.5% of calcium-magnesium ion chelating agent, pH regulator for regulating pH to 5-7, and the balance of water.
5. The infant laundry lotion according to claim 4, wherein the surfactant comprises a surfactant in a mass ratio of 2-4.5: 13-18: 6-10 of coconut oil fatty acid diethanolamide, Texapon N70 and AEO 9.
6. The infant laundry lotion according to claim 4, wherein the plant detergent comprises the components in a mass ratio of 0.5-2: 1-3 of coconut oleic acid and lauryl glucoside.
7. The infant laundry lotion according to claim 4, wherein the protease is Medley Advance 300L; the saponifier is potassium hydroxide; the preservative is mulberry common K15; the calcium and magnesium ion chelating agent is disodium ethylene diamine tetraacetate.
8. The infant laundry lotion according to claim 4, wherein the pH-adjusting agent is citric acid or sorbic acid.
9. The infant laundry lotion according to claim 4, wherein the pH is adjusted to 5 to 6.8.
10. A method of preparing a baby laundry lotion according to any one of claims 4 to 9, comprising the steps of:
s1, putting deionized water, a chelating agent, coconut oil fatty acid diethanolamide, Texapon N70 and coconut oil acid into an emulsifying pot, starting stirring at the stirring speed of 30rpm, heating the emulsifying pot to 80-85 ℃, and preserving heat for 15-20 min;
s2, cooling to 65-70 ℃, sequentially adding AEO9 and lauryl glucoside, continuously stirring at a stirring speed of 30rpm until the mixture is completely uniform and has no particles, and keeping the temperature for 15-20 min;
s3, cooling to 55-60 ℃, putting the potassium hydroxide into an emulsifying pot, vacuumizing and stirring until the potassium hydroxide is completely and uniformly dissolved, and continuing stirring for 10-20 min under heat preservation;
s4, cooling to 40-48 ℃, adding protease Medley Advance 300L and preservative Morpu K15, and uniformly stirring;
s5, adding piroctone olamine salt and the plant essential oil microcapsule emulsion and uniformly stirring;
s6, cooling to 35-40 ℃, and adding a pH regulator to regulate the pH.
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