CN108531298B - Washing powder containing fingered citron essential oil microcapsules and preparation method thereof - Google Patents

Washing powder containing fingered citron essential oil microcapsules and preparation method thereof Download PDF

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CN108531298B
CN108531298B CN201810315958.8A CN201810315958A CN108531298B CN 108531298 B CN108531298 B CN 108531298B CN 201810315958 A CN201810315958 A CN 201810315958A CN 108531298 B CN108531298 B CN 108531298B
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essential oil
fingered citron
citron essential
cyclodextrin
washing powder
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CN108531298A (en
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易封萍
朴栖西
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Shanghai Institute of Technology
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    • 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
    • C11D1/37Mixtures of compounds all of which are anionic
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    • 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
    • C11D17/00Detergent materials or soaps characterised by their shape or physical properties
    • C11D17/08Liquid soap, e.g. for dispensers; capsuled
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    • 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
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
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    • C11D3/046Salts
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    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
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    • C11D3/04Water-soluble compounds
    • C11D3/06Phosphates, including polyphosphates
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    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
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    • C11D3/08Silicates
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    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
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    • C11D3/10Carbonates ; Bicarbonates
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    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
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    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16Organic compounds
    • C11D3/20Organic compounds containing oxygen
    • C11D3/22Carbohydrates or derivatives thereof
    • C11D3/222Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
    • C11D3/225Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin etherified, e.g. CMC
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    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
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    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/29Sulfates of polyoxyalkylene ethers

Abstract

The invention provides washing powder containing fingered citron essence microcapsules, which comprises a step of preparing β -cyclodextrin aqueous solution, wherein β -cyclodextrin is dissolved in water to obtain β -cyclodextrin aqueous solution, the step of preparing fingered citron essential oil solution is also included, fingered citron essential oil is dissolved in an organic solvent to obtain the fingered citron essential oil solution, then the fingered citron essential oil microcapsules are prepared, the obtained fingered citron essential oil solution is added into the obtained β -cyclodextrin aqueous solution, embedding is carried out under the conditions of heating, shading and sealing, after the reaction is finished, reaction liquid is placed in a refrigerator for refrigeration, vacuum filtration is carried out, drying is carried out to constant weight, the fingered citron essential oil microcapsules are obtained, and the embedded microcapsules are applied to a washing powder formula to obtain the washing powder containing the fingered citron essence microcapsules.

Description

Washing powder containing fingered citron essential oil microcapsules and preparation method thereof
Technical Field
The invention belongs to the field of daily chemicals, and relates to washing powder, in particular to washing powder containing fingered citron essential oil microcapsules and a preparation method thereof.
Background
Essential oil belongs to volatile oil, some components can volatilize at room temperature or below, the stability is poor, the fragrance-retaining time is short, the quality of products is influenced, and the application of the essential oil is greatly limited. The embedding treatment of essential oil by microencapsulation technology is a research hotspot in recent years. Through microencapsulation, volatilization of the essential oil is inhibited due to the sealing effect of the capsule wall, and fragrance is completely retained, so that the storage time of the essential oil is prolonged and the use stability is improved. Therefore, research on the encapsulation embedding process of the fingered citron essential oil is needed to obtain a microcapsule product with good embedding effect and high stability. And with the gradual improvement of the industrial level of textiles, people no longer limit the consumption of washing powder to strong detergency, and pay more attention to the use feeling and the efficacy thereof. The green and environment-friendly concept of health and fashion makes the cleaning products which contain natural plant components and have the fragrance effect favored by consumers to be a necessary trend. The common washing powder consists of a surfactant, a builder, a filler, a fluorescent brightener and an anti-redeposition agent, and the problems of cleanness of washing, fragrance of the applied washing powder and storage time of the fragrance are not taken into consideration, so that the common washing powder is low in effect, low in fragrance intensity and low in application value.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides washing powder containing the fingered citron essential oil microcapsules and a preparation method thereof, aiming at solving the technical problem of small fragrance intensity of the washing powder in the existing product, the washing powder containing the fingered citron essential oil microcapsules and the preparation method thereof are in accordance with the concept of healthy and green, and simultaneously, the fragrance of the fingered citron on textile clothes is endowed, so that the washing powder is pleasant to the body and mind. The invention also provides a preparation method of the fingered citron essential oil microcapsule, which can solve the technical problems of volatilization of essential oil and short fragrance retention time.
The invention provides washing powder containing a fingered citron essence microcapsule, which comprises the following components in percentage by mass:
Figure BDA0001623764920000011
Figure BDA0001623764920000021
the fingered citron essential oil microcapsule is prepared by the following method:
1) a step of preparing β -cyclodextrin aqueous solution, dissolving β -cyclodextrin in water to obtain β -cyclodextrin aqueous solution, wherein the material ratio of β -cyclodextrin to water is 1 g: 6ml-10ml, and the dissolving temperature is 70 ℃ to 80 ℃;
2) a step of preparing the solution of the fingered citron essential oil, which is to dissolve the fingered citron essential oil into an organic solvent to obtain the solution of the fingered citron essential oil; the organic solvent is absolute ethyl alcohol, and the volume ratio of the fingered citron essential oil to the absolute ethyl alcohol is 1: 15-25;
3) adding the obtained fingered citron essential oil solution into the obtained β -cyclodextrin aqueous solution, wherein the mass ratio of β -cyclodextrin to the fingered citron essential oil is 4g-7 g: 1g, embedding is carried out under the conditions of heating, shading and sealing, the embedding temperature is 45-55 ℃, the embedding time is 1.5h-2.5h, the reaction solution is placed into a refrigerator for refrigeration after the reaction is finished, the refrigeration temperature is 3-5 ℃, the refrigeration time is 22h-26h, drying is carried out after vacuum filtration until the constant weight is achieved, and the fingered citron essential oil microcapsule is obtained, wherein the drying temperature is 45-55 ℃.
Further, the surfactant is composed of sodium alkyl benzene sulfonate, fatty alcohol-polyoxyethylene ether sodium sulfate and sodium stearate, wherein the sodium alkyl benzene sulfonate, the fatty alcohol-polyoxyethylene ether sodium sulfate and the sodium stearate respectively account for (4-6%), (2-4%) in the washing powder according to mass percentage.
Furthermore, the builder consists of sodium tripolyphosphate, sodium carbonate and sodium silicate, and the sodium tripolyphosphate, the sodium carbonate and the sodium silicate are respectively (10-15%), (10-15%) and (10-20%) in the washing powder by mass percentage.
Furthermore, the filler is sodium sulfate, and the anti-redeposition agent is cellulose ether.
Further, the fluorescent whitening agent consists of 1, 2-stilbene and biphenyl distyryl derivatives, and the mass percentages of the 1, 2-stilbene (and the biphenyl distyryl derivatives in the washing powder are respectively (0.05-0.1%), (0.05-0.1%).
Further, the enzyme comprises a protease, an amylase, a lipase and a cellulase, wherein the protease, the amylase, the lipase and the cellulase are respectively (0.08-0.2%), (0.07-0.2%), (0.08-0.2%) and (0.08-0.2%) in the washing powder in percentage by mass.
Further, the washing powder containing gold and fingered citron essence microcapsules comprises the following components in percentage by mass:
Figure BDA0001623764920000022
Figure BDA0001623764920000031
further, the washing powder containing gold and fingered citron essence microcapsules comprises the following components in percentage by mass:
Figure BDA0001623764920000032
the invention also provides a preparation method of the fingered citron microcapsule washing powder, which comprises the following steps:
1) weighing the raw materials according to the mass percentage, placing the raw materials into a container, sieving sodium carbonate, and uniformly mixing the sieved sodium carbonate with the raw materials except water, wherein the mass of the sodium carbonate is 12 percent of the total mass of the raw materials;
2) uniformly mixing the solid powder obtained in the step 1), spraying water into the powder in a spray drying mode, and stirring while spraying water to enable the water to be uniformly soaked into the powder;
3) continuing to stir the step 2), and then granulating;
4) drying the granules obtained in the step 3), sieving the dried granules with a 10-20-mesh sieve, and packaging the sieved granules to obtain a finished product. The invention also provides a preparation method of the fingered citron essential oil microcapsule, which comprises the following steps:
1) a step of preparing β -cyclodextrin aqueous solution, dissolving β -cyclodextrin in water to obtain β -cyclodextrin aqueous solution, wherein the material ratio of β -cyclodextrin to water is 1 g: 6ml-10ml, and the dissolving temperature is 70 ℃ to 80 ℃;
2) a step of preparing the solution of the fingered citron essential oil, which is to dissolve the fingered citron essential oil into an organic solvent to obtain the solution of the fingered citron essential oil; the organic solvent is absolute ethyl alcohol, and the volume ratio of the fingered citron essential oil to the absolute ethyl alcohol is 1: 15-25;
3) adding the obtained fingered citron essential oil solution into the obtained β -cyclodextrin aqueous solution, wherein the mass ratio of β -cyclodextrin to the fingered citron essential oil is 4g-7 g: 1g, embedding is carried out under the conditions of heating, shading and sealing, the embedding temperature is 45-55 ℃, the embedding time is 1.5h-2.5h, the reaction solution is placed into a refrigerator for refrigeration after the reaction is finished, the refrigeration temperature is 3-5 ℃, the refrigeration time is 22h-26h, drying is carried out after vacuum filtration until the constant weight is achieved, and the fingered citron essential oil microcapsule is obtained, wherein the drying temperature is 45-55 ℃.
The invention provides a preparation method of a fingered citron essential oil-containing microcapsule washing powder, which comprises the steps of preparing β -cyclodextrin aqueous solution, dissolving β -cyclodextrin in water to obtain β -cyclodextrin aqueous solution, then preparing fingered citron essential oil solution, dissolving fingered citron essential oil in an organic solvent to obtain the fingered citron essential oil solution, then preparing fingered citron essential oil microcapsules, adding the obtained fingered citron essential oil solution into the obtained β -cyclodextrin aqueous solution, embedding under the conditions of heating, shading and sealing, after the reaction is finished, placing reaction liquid in a refrigerator for refrigeration, performing vacuum filtration, drying to constant weight to obtain the fingered citron essential oil microcapsules, and applying the embedded microcapsules to a washing powder formula.
Compared with the prior art, the invention has remarkable technical progress. The method can enhance the mechanical strength of the microcapsule and the slow release performance of the fingered citron essence, and has great positive significance on the uniformity, the slow release performance and the stability of the overall particle size of the fingered citron essence microcapsule product. The preparation method of the fingered citron essential oil microcapsule has the advantages of good embedding effect, high stability, good economy and the like. According to the invention, the fingered citron essential oil is embedded and then applied to the washing powder, so that the essential oil can play a long-lasting fragrance characteristic in the product, and meanwhile, the product brings pleasant sensory experience of faint scent.
Detailed Description
The invention is further illustrated, but not limited, by the following specific examples.
Specifically, in the present invention:
the fingered citron essential oil is prepared according to the method in Chinese patent application 201610979286.1, and the fingered citron is provided by Zhejiang Jinshoubao Biotechnology Co.
Example 1
A preparation method of the gold fingered citron essential oil microcapsule comprises the steps of taking gold fingered citron essential oil as a core material, taking β -cyclodextrin as a wall material, weighing β -cyclodextrin 10.00g, adding 80ml of water according to the volume mass ratio of deionized water to β -cyclodextrin of 8: 1, stirring in a water bath at 80 ℃ to dissolve the gold fingered citron essential oil to obtain β -cyclodextrin aqueous solution, cooling to 50 ℃ and keeping the temperature for later use, obtaining 2g of gold fingered citron essential oil, adding ethanol according to the volume ratio of 20: 1 of ethanol to essential oil, dissolving with absolute ethanol, adding dropwise into β -cyclodextrin aqueous solution at a constant speed while stirring, carrying out light-proof sealing embedding at the water bath temperature of 50 ℃ for 2 hours, taking out reaction liquid, cooling the reaction liquid to room temperature, standing in a refrigerator at 4 ℃ for 24 hours, carrying out vacuum filtration, and drying in a drying oven at 50 ℃ to a constant weight to obtain white solid particles, namely the gold fingered citron essential oil microcapsule.
Determination of the encapsulation efficiency of the microcapsules:
the fingered citron essential oil microcapsule W of the embodiment is weighed1Placing in a small beaker with dry weight, adding 20ml of hot water, stirring to dissolve, adding 30ml of petroleum ether, shaking for extraction, extracting twice, filtering the sample, and drying the sample to constant weight W2The embedding rate was calculated according to the following formula:
Figure BDA0001623764920000051
determination of microcapsule embedding yield:
Figure BDA0001623764920000052
in the formula:
m1- -mass of fructus Citri Sarcodactylis essential oil, g;
m 2- β -cyclodextrin mass, g;
m 3-the mass of the obtained fingered citron essential oil microcapsule after drying, g;
through measurement and calculation, the embedding rate of the embodiment is 61.2%, and the embedding yield is 88.9%.
Example 2
The fingered citron essential oil microcapsule and the fingered citron essential oil prepared in the example 1 are heated to measure the slow release performance, and the specific data are shown in the following table 1:
TABLE 1 influence of Sedum Sarcodactylis essential oil microencapsulation on essential oil volatility
Heating time/h Fructus Citri Sarcodactylis essential oil volatility (%) Fructus Citri Sarcodactylis essential oil microcapsule volatility (%)
0 0 0
6 21.1 3.2
12 40.5 3.3
18 51.7 7.8
24 55.9 9.5
30 60.1 11.7
It can be seen from the above table that as the heating time is prolonged, part of the essential oil volatilizes from the fingered citron essential oil and the microcapsule, but the volatilization rates of the essential oil and the microcapsule are different, and the sustained release effect of the essential oil of the fingered citron microcapsule is far better than that of the non-embedded essential oil.
Example 3
The bergamot essential oil microcapsule is tested for fragrance retention effect, and specific data are shown in the following table 2:
TABLE 2 variation of essence Mass concentration at different drying times
Drying time/h Fructus Citri Sarcodactylis essential oil Microcapsule of essential oil of fingered citron
0 3.5 3.4
1 1.7 2.5
3 0.4 1.6
7 0.2 1.2
15 0 1.1
It can be seen from the above table that the mass concentration of the fingered citron microcapsule essential oil is far stronger than that of the non-embedded essential oil along with the extension of the drying time.
Example 4
The fingered citron essential oil microcapsule washing powder comprises the following components in percentage by mass:
TABLE 3 formulation of fructus Citri Sarcodactylis essential oil microcapsule detergent
Figure BDA0001623764920000061
Figure BDA0001623764920000071
A preparation method of the fingered citron microcapsule washing powder comprises the following steps:
1) weighing the amount of each raw material according to a designed formula, placing the raw materials in a container, sieving sodium carbonate, and uniformly mixing the sodium carbonate with the mixed powder, wherein the mass of the sodium carbonate is 12% of the total mass of the raw materials;
2) uniformly mixing the solid powder in the step 1), spraying water into the powder in a spray drying mode, and stirring while spraying water to enable the water to be uniformly soaked into the powder.
3) Continuing to stir step 2), and then granulating.
4) Drying the granules obtained in the step 3) to a certain temperature, sieving the granules by a sieve with 10-20 meshes, and packaging the sieved granules into finished products.
A method for testing fingered citron essential oil microcapsule washing powder, wherein a Peroxide Value (PV) is an important index, comprises the following steps:
1) according to the test method of GB/T5538-1995, the influence of the fingered citron essential oil microcapsule washing powder prepared in the embodiment 3 of the invention on the stability of animal and vegetable oil is tested, and firstly, a mixed solution of acetic acid and isooctane (1 ml: 1ml) of the solution, 15ml of each solution was taken.
2) A saturated solution of potassium iodide (1ml) was prepared and added to step 1 above, kept in the dark for 3min and 30ml of deionized water was added.
3) Titration was started with sodium thiosulfate (0.01mol/L) and 0.5ml of starch solution (1%) was used as indicator until the blue color disappeared. The specific data are shown in Table 4.
TABLE 4 Effect of microencapsulated Sedum Sarcodactylis essential oil on oil stability
Figure BDA0001623764920000072
Figure BDA0001623764920000081
The above table shows that the fingered citron microcapsule has strong antioxidation in the application of the washing powder.
It will be apparent to those skilled in the art that appropriate modifications and variations can be made in the above processes and materials and in the above teachings and these modifications and variations are within the scope of the invention as defined in the appended claims. The scope of the invention is to be determined by all claims.
In conclusion, the preparation method of the fingered citron essential oil microcapsule and the preparation method of the fingered citron essential oil microcapsule washing powder can effectively embed the fingered citron essential oil, so that the volatilization rate of the essential oil is reduced, the prepared fingered citron essential oil microcapsule washing powder has good fragrance endowing effect, complete and fine fragrance and long fragrance retention time, and has strong antioxidation effect.
The above description is only a basic description of the present invention, and any equivalent changes made according to the technical solution of the present invention should fall within the protection scope of the present invention.

Claims (1)

1. The washing powder containing the fingered citron essence microcapsules is characterized by comprising the following components in percentage by mass:
Figure FDA0002426405740000011
the sodium sulfate is a filler, and the cellulose ether is an anti-redeposition agent;
the fingered citron essential oil microcapsule is prepared by the following method:
1) a step of preparing β -cyclodextrin aqueous solution, dissolving β -cyclodextrin in water to obtain β -cyclodextrin aqueous solution, wherein the material ratio of β -cyclodextrin to water is 1 g: 6ml-10ml, and the dissolving temperature is 70 ℃ to 80 ℃;
2) a step of preparing the solution of the fingered citron essential oil, which is to dissolve the fingered citron essential oil into an organic solvent to obtain the solution of the fingered citron essential oil; the organic solvent is absolute ethyl alcohol, and the volume ratio of the fingered citron essential oil to the absolute ethyl alcohol is 1: 15-25;
3) adding the obtained fingered citron essential oil solution into the obtained β -cyclodextrin aqueous solution, wherein the mass ratio of β -cyclodextrin to the fingered citron essential oil is 4g-7 g: 1g, embedding is carried out under the conditions of heating, shading and sealing, the embedding temperature is 45-55 ℃, the embedding time is 1.5h-2.5h, the reaction solution is placed in a refrigerator for refrigeration after the reaction is finished, the refrigeration temperature is 3-5 ℃, the refrigeration time is 22h-26h, drying is carried out after vacuum filtration until the constant weight is achieved, and the fingered citron essential oil microcapsule is obtained, wherein the drying temperature is 45-55 ℃;
the preparation method of the fingered citron microcapsule washing powder comprises the following steps:
1) weighing the raw materials according to the mass percentage, placing the raw materials into a container, sieving sodium carbonate, and uniformly mixing the sieved sodium carbonate with the raw materials except water;
2) uniformly mixing the solid powder obtained in the step 1), spraying water into the powder in a spray drying mode, and stirring while spraying water to enable the water to be uniformly soaked into the powder;
3) continuing to stir the step 2), and then granulating;
4) drying the granules obtained in the step 3), sieving the dried granules with a 10-20-mesh sieve, and packaging the sieved granules to obtain a finished product.
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