CN113599305A - Walnut oil soap-based silicone oil-free shampoo and preparation method thereof - Google Patents

Walnut oil soap-based silicone oil-free shampoo and preparation method thereof Download PDF

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CN113599305A
CN113599305A CN202110842864.8A CN202110842864A CN113599305A CN 113599305 A CN113599305 A CN 113599305A CN 202110842864 A CN202110842864 A CN 202110842864A CN 113599305 A CN113599305 A CN 113599305A
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walnut oil
oil
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soap
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CN113599305B (en
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孟蕾
惠佳如
吴细文
徐子悟
葛清明
樊雨彤
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Hunan University of Chinese Medicine
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/365Hydroxycarboxylic acids; Ketocarboxylic acids
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/02Preparations for cleaning the hair
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/12Preparations containing hair conditioners
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/20Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/30Characterized by the absence of a particular group of ingredients
    • A61K2800/34Free of silicones
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/413Nanosized, i.e. having sizes below 100 nm
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

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Abstract

The invention provides a walnut oil soap-based silicone-oil-free shampoo and a preparation method thereof, wherein the shampoo does not contain polyorganosiloxane, and comprises the following components in parts by weight: 10-20 parts of walnut oil polyhydroxy stearic acid; 5-8 parts of soap base; 1-6 parts of a water softener; 0.06-0.15 parts of essence; 15-20 parts of nano cellulose; 3-8 parts of polyethylene glycol; 5-10 parts of cocamidopropyl betaine; 5-10 parts of sodium dodecyl sulfate; 0.25-0.45 part of sodium benzoate; 1-3 parts of sodium carbonate; 0.1-0.5 part of sodium chloride. The walnut oil polyhydroxy stearic acid adopted by the shampoo prepared by the invention is a novel modified soap base surfactant, walnut oil with various unsaturated fatty acids is adopted, and the walnut oil polyhydroxy stearic acid has the hard water resistance of a modified soap base and has good dissolubility and foaming performance under neutral conditions and low temperature from the natural oil of the extracted walnut oil.

Description

Walnut oil soap-based silicone oil-free shampoo and preparation method thereof
Technical Field
The invention belongs to the technical field of washing and caring products, and particularly relates to a walnut oil soap-based silicone-oil-free shampoo and a preparation method thereof.
Background
Walnut oil is rich in polyunsaturated fatty acids and monounsaturated fatty acids. It contains Omega-6, Omega-9 and Omega-3 fats. The oil contains b vitamins, vitamin E, zinc, selenium, calcium, magnesium and niacin. All of these vitamins and minerals promote hair health and growth.
The beneficial components of walnut oil, especially unsaturated fatty acid, vitamin E and zinc, make your hair strong and lustrous. The fat in the oil is easily absorbed by the hair follicle, strengthening the hair from the inside. The fatty acid moisturizes the hair without losing moisture. Vitamin E protects the hair from harmful effects and helps prevent the hair from whitening. Walnut oil is useful for treating scalp infections that cause hair loss. Some people use it to remove seborrheic dermatitis, which is a widely spread disease according to wikipedia. The effect is better if walnut oil is mixed with jojoba oil or tea tree oil. Black walnut oil is even more effective against skin diseases and is believed to kill lice.
Walnut skin is a good method for naturally dyeing hair. Walnut oil does not color hair when applied to hair, but is believed to brighten the color.
However, in the prior art, no shampoo which adopts walnut oil as a part of oil to synthesize a modified surfactant, replaces a conventional surfactant, and can utilize beneficial components of the walnut oil to nourish hair and replace silicone oil is available.
Disclosure of Invention
Aiming at the defects, the invention provides the walnut oil soap-based silicone-oil-free shampoo which adopts walnut oil as a part of synthetic modified surfactant of grease, can utilize beneficial components of the walnut oil to nourish hair and replace silicone oil while achieving the purpose of replacing the conventional surfactant, and the preparation method thereof.
The invention provides the following technical scheme: the walnut oil soap-based silicone-free shampoo does not contain polyorganosiloxane and comprises the following components in parts by weight:
Figure BDA0003179689400000021
further, the diameter of the nano-cellulose is 10 nm-30 nm.
Further, the nano-cellulose is one or more of nano ethyl hydroxyethyl cellulose, nano methyl hydroxypropyl cellulose or nano methyl carboxypropyl cellulose.
Further, the water softener is one or more of sodium silicate, sodium tripolyphosphate and sodium hexametaphosphate.
Further, the raw materials for preparing the walnut oil polyhydroxy stearic acid comprise the following components in parts by weight:
Figure BDA0003179689400000022
further, the preparation method of the walnut oil polyhydroxy stearic acid comprises the following steps:
1) mixing the sodium hydroxide with half of the anhydrous ethanol by weight to obtain a sodium hydroxide ethanol solution with the mass fraction of 3% -5%, dripping the sodium hydroxide ethanol solution into the walnut oil by weight, saponifying at 55-65 ℃ for 1-1.5 h, and then cooling to room temperature to obtain a precipitation solution with a lower soap cake;
2) acidifying the soap cake in the precipitation liquid obtained in the step 1) by using hydrochloric acid with the mass fraction of 12%, controlling the final pH of the reaction liquid to be 2.5-3.5 in the acidification process, then washing the reaction liquid to be neutral by using saturated sodium chloride, standing and layering the reaction liquid, taking an upper oil layer as mixed fatty acid obtained by hydrolysis of walnut oil, and adding anhydrous sodium sulfate into the oil layer containing the mixed fatty acid for drying;
3) adding the urea in the weight part into the remaining half of the anhydrous ethanol in the weight part, heating and refluxing at 75-85 ℃, adding the dried mixture containing the mixed fatty acid obtained in the step 2) after the urea is completely dissolved, stirring uniformly, and refluxing in a water bath at 50-60 ℃ for 30min to obtain enriched unsaturated fatty acid;
4) mixing the enriched unsaturated fatty acid obtained in the step 3) with the weight part of H2O2Mixing, reacting at 30-35 ℃ for 30min, then placing in a methanol sulfate solution, performing water bath esterification at 60-70 ℃ for 3-4 h, cooling to room temperature after the reaction is finished, then adding 20-30 parts of water, equally dividing the petroleum ether by weight into 3 parts, extracting 1 part of petroleum ether for 3 times each time, combining into a petroleum ether phase, recovering the petroleum ether under reduced pressure, and weighing to constant weight to obtain the walnut oil polyhydroxy stearic acid.
Further, the unsaturated fatty acid obtained by hydrolyzing and enriching the walnut oil in the step 3) is one or more of oleic acid, linoleic acid, linolenic acid, arachidonic acid and palmitic acid.
Further, the sulfuric acid methanol solution in the step 4) is concentrated sulfuric acid and methanol which are mixed according to a volume ratio of 1: 200-1: 250.
Further, the pressure of the petroleum ether recovered by decompression in the step 4) is 1.0KPa to 1.2KPa, and the temperature is 105 ℃ to 115 ℃.
The invention also provides a preparation method of the walnut oil soap-based silicone oil-free shampoo, which comprises the following steps:
s1: adding the sodium benzoate and the water softener in parts by weight into 50 parts of distilled water, and stirring for dissolving;
s2: putting the mixed solution obtained in the step S1 into a reaction kettle under the condition of stirring, adding the sodium carbonate, the sodium dodecyl sulfate, the walnut oil polyhydroxy stearic acid and the soap base according to the parts by weight, uniformly stirring, heating at 70-80 ℃, continuously stirring in the heating process, and keeping the temperature for 15-20 min;
s3: after the temperature is reduced to 40-60 ℃, adding the cocamidopropyl betaine, the nanocellulose and the polyethylene glycol in parts by weight into the mixture obtained in the step S2, stirring until the nanocellulose and the polyethylene glycol are completely dissolved, and keeping the temperature for 5-10 min;
s4: cooling to 30-35 ℃, adding the essence in parts by weight and the sodium chloride in parts by weight, adjusting the viscosity to 2000-3500 cp, and continuously stirring for 10-30min to obtain the walnut oil soap base silicone oil-free shampoo.
The invention has the beneficial effects that:
1. the walnut oil in the walnut oil polyhydroxy stearic acid adopted by the shampoo prepared by the invention is prepared by a low-temperature extraction method, so that volatile nutritional ingredients in the walnut oil polyhydroxy stearic acid are reserved, the shampoo is beneficial to nourishing hair and skin, and the shampoo has the effects of growing and blackening hair after long-term use.
2. The walnut oil polyhydroxy stearic acid adopted by the shampoo prepared by the invention is a novel modified soap base surfactant, walnut oil with various unsaturated fatty acids is adopted, fatty acids with different unsaturation degrees are obtained by hydrolysis from natural grease of the extracted walnut oil, and polyhydroxy fatty acids with different hydroxyl numbers are obtained by oxidizing double bonds of the unsaturated fatty acids.
3. The nano-cellulose adopted by the shampoo prepared by the invention utilizes the hydrophilic chemical property of the nano-cellulose, so that the nano-cellulose has higher surface activity, and can effectively reduce the surface tension of an interface, thereby enhancing the foam stability of the shampoo in the using process.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
This example provides a walnut oil soap-based silicone-free shampoo, which does not contain polyorganosiloxane, and comprises the following components in parts by weight:
Figure BDA0003179689400000051
the walnut oil polyhydroxy stearic acid preparation raw material comprises the following components in parts by weight:
Figure BDA0003179689400000052
Figure BDA0003179689400000061
the preparation method of the walnut oil polyhydroxy stearic acid comprises the following steps:
1) mixing 20 parts of sodium hydroxide and 50 parts of absolute ethyl alcohol to obtain a sodium hydroxide ethanol solution with the mass fraction of 5%, dripping the sodium hydroxide ethanol solution into the walnut oil with the weight parts, saponifying at 55 ℃ for 1.5h, and then cooling to room temperature to obtain a precipitation solution with a lower soap cake;
2) acidifying the soap cake in the precipitation liquid obtained in the step 1) by using hydrochloric acid with the mass fraction of 12%, controlling the final pH of the reaction liquid to be 3.5 in the acidification process, then cleaning the soap cake by using saturated sodium chloride until the neutral pH is 6.5, standing and layering, taking an upper oil layer as mixed fatty acid obtained by hydrolysis from walnut oil, and adding anhydrous sodium sulfate into the oil layer containing the mixed fatty acid for drying;
3) adding 8 parts of urea into the remaining 50 parts of absolute ethyl alcohol, heating and refluxing at 75 ℃, adding the dried mixture containing the mixed fatty acid obtained in the step 2) after the urea is completely dissolved, uniformly stirring, and refluxing in a water bath at 60 ℃ for 30min to obtain enriched unsaturated fatty acid;
4) mixing the enriched unsaturated fatty acid obtained in the step 3) with 30 parts of H2O2Mixing, reacting at 30 ℃ for 30min, then placing in a sulfuric acid methanol solution obtained by concentrated sulfuric acid and methanol according to the volume ratio of 1:200, carrying out water bath esterification at 70 ℃ for 3h, cooling to room temperature after the reaction is finished, then adding 30 parts of water, equally dividing 30 parts of petroleum ether into 3 parts, extracting by 1 part of petroleum ether (namely 10 parts by weight of petroleum ether per 1 part) each time, carrying out co-extraction for 3 times, combining to obtain a petroleum ether phase, recovering the petroleum ether under reduced pressure at 105 ℃ and 1.2KPa, and weighing to constant weight to obtain the walnut oil polyhydroxy stearic acid.
Through detection, unsaturated fatty acids obtained by hydrolyzing and enriching the walnut oil in the step 3) are 92.38% of oleic acid, 3.5% of linoleic acid, 0.32% of linolenic acid and 3.8% of palmitic acid.
The embodiment also provides a preparation method of the walnut oil soap-based silicone-free shampoo, which comprises the following steps:
s1: adding 0.25 part of sodium benzoate and 1 part of sodium tripolyphosphate into 50 parts of distilled water, and stirring for dissolving;
s2: putting the mixed solution obtained in the step S1 into a reaction kettle under the condition of stirring, adding 3 parts of sodium carbonate, 5 parts of sodium dodecyl sulfate, 20 parts of walnut oil polyhydroxy stearic acid and the soap base in parts by weight, uniformly stirring, heating at 70 ℃, continuously stirring in the heating process, and keeping the temperature for 20 min;
s3: cooling to 50 ℃, adding 10 parts of cocamidopropyl betaine, 20 parts of nano-methylhydroxypropylcellulose with the diameter of 10nm and 3 parts of polyethylene glycol into the mixture obtained in the step S2, stirring until the mixture is completely dissolved, and keeping the temperature for 7 min;
s4: cooling to 35 deg.C, adding 0.15 parts of essence and 0.1 parts of sodium chloride, adjusting viscosity to 2000cp, and stirring for 10min to obtain walnut oil soap base silicone-free shampoo.
Example 2
This example provides a walnut oil soap-based silicone-free shampoo, which does not contain polyorganosiloxane, and comprises the following components in parts by weight:
Figure BDA0003179689400000071
Figure BDA0003179689400000081
the walnut oil polyhydroxy stearic acid preparation raw material comprises the following components in parts by weight:
Figure BDA0003179689400000082
the preparation method of the walnut oil polyhydroxy stearic acid comprises the following steps:
1) mixing 15 parts of sodium hydroxide and 25 parts of absolute ethyl alcohol to obtain a sodium hydroxide ethanol solution with the mass fraction of 3%, dripping the sodium hydroxide ethanol solution into the walnut oil with the weight part, saponifying at 65 ℃ for 1.2h, and cooling to room temperature to obtain a precipitation solution with a lower soap cake;
2) acidifying the soap cake in the precipitation liquid obtained in the step 1) by using hydrochloric acid with the mass fraction of 12%, controlling the final pH of the reaction liquid to be 3.0 in the acidification process, then cleaning the reaction liquid to be neutral by using saturated sodium chloride, standing and layering the reaction liquid, taking an upper oil layer as mixed fatty acid obtained by hydrolyzing walnut oil, and adding anhydrous sodium sulfate into the oil layer containing the mixed fatty acid for drying;
3) adding 6.5 parts of urea into the remaining 25 parts of absolute ethyl alcohol, heating and refluxing at 80 ℃, adding the dried mixture containing the mixed fatty acid obtained in the step 2) after the urea is completely dissolved, uniformly stirring, and refluxing in a water bath at 50 ℃ for 30min to obtain enriched unsaturated fatty acid;
4) mixing the enriched unsaturated fatty acid obtained in the step 3) with 20 parts of H2O2Mixing, reacting at 35 ℃ for 30min, then placing in concentrated sulfuric acid and methanol-sulfuric acid methanol solution according to the volume ratio of 1:250, esterifying for 4h in water bath at 65 ℃, cooling to room temperature after the reaction is finished, then adding 20 parts of water, equally dividing 15 parts of petroleum ether into 3 parts (namely, 5 parts of petroleum ether in each part), extracting with 1 part of petroleum ether each time, co-extracting for 3 times, combining into a petroleum ether phase, recovering the petroleum ether under reduced pressure at 100 ℃ and 1.0KPa, and weighing to constant weight to obtain the walnut oil polyhydroxy stearic acid.
Through detection, unsaturated fatty acids obtained by hydrolyzing and enriching the walnut oil in the step 3) are 90.8% of oleic acid, 1.1% of linoleic acid, 0.3% of linolenic acid, 3.3% of arachidonic acid and 4.5% of palmitic acid.
The embodiment also provides a preparation method of the walnut oil soap-based silicone-free shampoo, which comprises the following steps:
s1: adding 0.45 part of sodium benzoate and 3.5 parts of sodium silicate into 50 parts of distilled water, and stirring for dissolving;
s2: placing the mixed solution obtained in the step S1 into a reaction kettle under the condition of stirring, adding 2 parts of sodium carbonate, 8 parts of sodium dodecyl sulfate, 15 parts of walnut oil polyhydroxy stearic acid and 8 parts of soap base, uniformly stirring, heating at 80 ℃, continuously stirring in the heating process, and keeping the temperature for 15 min;
s3: after the temperature is reduced to 60 ℃, adding 5 parts of cocamidopropyl betaine, 15 parts of nano methyl carboxypropyl cellulose with the diameter of 20nm and 8 parts of polyethylene glycol into the mixture obtained in the step S2, stirring until the nano methyl carboxypropyl cellulose and the polyethylene glycol are completely dissolved, and then keeping the temperature for 5 min;
s4: cooling to 32 ℃, adding the essence in parts by weight and the sodium chloride in parts by weight, adjusting the viscosity to 2500cp, and continuously stirring for 20min to obtain the walnut oil soap-based silicone-oil-free shampoo.
Example 3
This example provides a walnut oil soap-based silicone-free shampoo, which does not contain polyorganosiloxane, and comprises the following components in parts by weight:
Figure BDA0003179689400000091
Figure BDA0003179689400000101
the walnut oil polyhydroxy stearic acid preparation raw material comprises the following components in parts by weight:
Figure BDA0003179689400000102
the preparation method of the walnut oil polyhydroxy stearic acid comprises the following steps:
1) mixing 10 parts of sodium hydroxide and 40 parts of absolute ethyl alcohol to obtain a sodium hydroxide ethanol solution with the mass fraction of 4%, dripping the sodium hydroxide ethanol solution into the walnut oil with the weight parts, saponifying at 60 ℃ for 1h, and cooling to room temperature to obtain a precipitation solution with a lower soap cake;
2) acidifying the soap cake in the precipitation liquid obtained in the step 1) by using hydrochloric acid with the mass fraction of 12%, controlling the final pH of the reaction liquid to be 2.5 in the acidification process, then cleaning the reaction liquid to be neutral by using saturated sodium chloride, standing and layering the reaction liquid, taking an upper oil layer as mixed fatty acid obtained by hydrolyzing walnut oil, and adding anhydrous sodium sulfate into the oil layer containing the mixed fatty acid for drying;
3) adding 5 parts of urea into the remaining 40 parts of absolute ethyl alcohol, heating and refluxing at 85 ℃, adding the dried mixture containing the mixed fatty acid obtained in the step 2) after the urea is completely dissolved, uniformly stirring, and performing water bath reflux at 55 ℃ for 30min to obtain enriched unsaturated fatty acid;
4) mixing the enriched unsaturated fatty acid obtained in the step 3) with 25 parts of H2O2Mixing, reacting at 33 deg.C for 30min, and standingPerforming water bath esterification for 3.5 hours at 60 ℃ in a sulfuric acid methanol solution of concentrated sulfuric acid and methanol according to the volume ratio of 1:220, cooling to room temperature after the reaction is finished, then adding 25 parts of water, equally dividing 21 parts of petroleum ether into 3 parts (namely, 7 parts of petroleum ether in each part), extracting 1 part of petroleum ether for 3 times each time, combining the petroleum ether phases, selecting and recovering petroleum ether under reduced pressure at 110 ℃ and 1.1KPa, and weighing to constant weight to obtain the walnut oil polyhydroxy stearic acid.
Through detection, unsaturated fatty acids obtained by hydrolyzing and enriching the walnut oil in the step 3) are 82.6% of oleic acid, 2.4% of linoleic acid, 7.6% of linolenic acid, 1.8% of arachidonic acid and 5.6% of palmitic acid.
The embodiment also provides a preparation method of the walnut oil soap-based silicone-free shampoo, which comprises the following steps:
s1: adding 0.35 part of sodium benzoate and 6 parts of sodium hexametaphosphate into 50 parts of distilled water, and stirring for dissolving;
s2: putting the mixed solution obtained in the step S1 into a reaction kettle under the stirring condition, adding 1 part of sodium carbonate, 10 parts of sodium dodecyl sulfate, 10 parts of walnut oil polyhydroxy stearic acid and 6 parts of soap base, uniformly stirring, heating at 75 ℃, continuously stirring in the heating process, and keeping the temperature for 17 min;
s3: after the temperature is reduced to 40 ℃, adding 7.5 parts of cocamidopropyl betaine, 18 parts of nano ethyl hydroxyethyl cellulose with the diameter of 30nm and 5 parts of polyethylene glycol into the mixture obtained in the step S2, stirring until the nano ethyl hydroxyethyl cellulose and the polyethylene glycol are completely dissolved, and then keeping the temperature for 10 min;
s4: cooling to 30 deg.C, adding 0.10 parts of essence and 0.5 parts of sodium chloride, adjusting viscosity to 3500cp, and stirring for 30min to obtain walnut oil soap base silicone-free shampoo.
Comparative example 1
This example differs from example 1 only in that the same amount by weight of the same amount of cocamidopropyl betaine as in example 1 was replaced by the same amount by weight of the polyorganosiloxane as cocamidopropyl betaine, which had the same lubricating and softening effect.
Comparative example 2
The difference between the embodiment and the embodiment 1 is that sodium laureth sulfate with surfactant effect is used to replace walnut oil polyhydroxy stearic acid in the embodiment, and the weight portion of the sodium laureth sulfate is the same as that of the walnut oil polyhydroxy stearic acid.
Comparative example 3
This example differs from example 1 only in that the shampoo was prepared without using nano-methylhydroxypropylcellulose having a diameter of 10 nm.
Experimental example 1
The shampoos of examples 1 to 3 and comparative examples 1 to 3 according to the present invention were prepared into a solution with a mass fraction of 1%, slowly heated or cooled, and when the critical temperature at which the solution suddenly changed from turbid to clear was its Krafft Point, the measurement was repeated three times, and the average value was taken. The results are shown in Table 1.
Experimental example 2
At a certain temperature, respectively measuring 10mL of the shampoos of examples 1-3 and comparative examples 1-3 of the present invention to prepare 0.1% by mass of solution, placing the solution in a 100mL measuring cylinder with a plug, adding a buffer solution to dilute the solution to 30mL, shaking the solution for 10 times after the plug is formed, standing the solution for 30s, recording a bubble volume H0, recording a foam stabilizing volume H1 after 5min, and taking the average value of the bubble volumes of 5 parallel experiments as the foaming power, wherein the larger the bubble volume is, the better the foaming power is. The results are shown in Table 1.
TABLE 1
Kraff point Volume of bubbles
Example 1 <0 93.6
Example 2 <0 92.5
Example 3 <0 93.0
Comparative example 1 <0 79.7
Comparative example 2 16 39.6
Comparative example 3 <0 68.6
Experimental example 3
The shampoos of examples 1 to 3 and comparative examples 1 to 3 of the present invention were taken, 100g of water was added, and after stirring for 10 seconds with a stirrer, the foam height was recorded for evaluating foamability/initial foam height, and after standing for 5min, the height of the water surface (drainage height) of the lower layer of foam was recorded for evaluating the stability of foam. The results are shown in Table 2.
TABLE 2
Height of foam Height of water discharge
Example 1 10.8cm 0.67cm
Example 2 10.3cm 0.72cm
Example 3 9.8cm 0.75cm
Comparative example 1 8.6cm 0.68cm
Comparative example 2 8.7cm 0.73cm
Comparative example 3 6.3cm 1.43cm
As can be seen from Table 2, the addition of nanocellulose having a diameter of 10nm to 30nm effectively increased the foam height of the shampoo and effectively decreased the height of the water outlet below the foam, meaning that the stability of the foam was enhanced, while in comparative example 3, the height of the water outlet was greatly increased due to the absence of nanocellulose, indicating that the stability was poor.
Through Ames test detection, the shampoo prepared by the invention is specified in national standard GB7919-1987 cosmetic safety evaluation program and method
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features included in other embodiments, rather than other features, combinations of features of different embodiments are meant to be within the scope of the invention and form different embodiments. For example, in the claims above, any of the claimed embodiments may be used in any combination. The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.

Claims (10)

1. The walnut oil soap-based silicone-free shampoo is free of polyorganosiloxane and is characterized by comprising the following components in parts by weight:
Figure FDA0003179689390000011
2. the walnut oil soap-based silicone oil-free shampoo of claim 1 wherein the nanocellulose has a diameter of 10nm to 30 nm.
3. The walnut oil soap-based silicone-free shampoo of claim 1, wherein the nanocellulose is one or more of nanoethylhydroxyethylcellulose, nanomethylhydroxypropylcellulose, or nanomethylcarboxypropylcellulose.
4. The walnut oil soap-based silicone-free shampoo of claim 1 wherein the water softener is one or more of sodium silicate, sodium tripolyphosphate, and sodium hexametaphosphate.
5. The walnut oil soap-based silicone-oil-free shampoo as claimed in claim 1, wherein the walnut oil polyhydroxystearic acid is prepared from the following raw materials in parts by weight:
Figure FDA0003179689390000012
Figure FDA0003179689390000021
6. the walnut oil soap-based silicone oil-free shampoo according to claim 5, wherein the preparation method of the walnut oil polyhydroxystearic acid comprises the following steps:
1) mixing the sodium hydroxide with half of the anhydrous ethanol by weight to obtain a sodium hydroxide ethanol solution with the mass fraction of 3% -5%, dripping the sodium hydroxide ethanol solution into the walnut oil by weight, saponifying at 55-65 ℃ for 1-1.5 h, and then cooling to room temperature to obtain a precipitation solution with a lower soap cake;
2) acidifying the soap cake in the precipitation liquid obtained in the step 1) by using hydrochloric acid with the mass fraction of 12%, controlling the final pH of the reaction liquid to be 2.5-3.5 in the acidification process, then washing the reaction liquid to be neutral by using saturated sodium chloride, standing and layering the reaction liquid, taking an upper oil layer as mixed fatty acid obtained by hydrolysis of walnut oil, and adding anhydrous sodium sulfate into the oil layer containing the mixed fatty acid for drying;
3) adding the urea in the weight part into the remaining half of the anhydrous ethanol in the weight part, heating and refluxing at 75-85 ℃, adding the dried mixture containing the mixed fatty acid obtained in the step 2) after the urea is completely dissolved, stirring uniformly, and refluxing in a water bath at 50-60 ℃ for 30min to obtain enriched unsaturated fatty acid;
4) mixing the enriched unsaturated fatty acid obtained in the step 3) with the weight part of H2O2Mixing, reacting at 30-35 ℃ for 30min, then placing in a methanol sulfate solution, performing water bath esterification at 60-70 ℃ for 3-4 h, cooling to room temperature after the reaction is finished, then adding 20-30 parts of water, equally dividing the petroleum ether by weight into 3 parts, extracting 1 part of petroleum ether for 3 times each time, combining into a petroleum ether phase, recovering the petroleum ether under reduced pressure, and weighing to constant weight to obtain the walnut oil polyhydroxy stearic acid.
7. The walnut oil soap-based silicone oil-free shampoo according to claim 6, wherein the unsaturated fatty acid obtained by hydrolysis and enrichment of the walnut oil in step 3) is one or more of oleic acid, linoleic acid, linolenic acid, arachidonic acid, and palmitic acid.
8. The walnut oil soap-based silicone oil-free shampoo as claimed in claim 6, wherein the methanol sulfate solution in step 4) is concentrated sulfuric acid and methanol at a volume ratio of 1:200 to 1: 250.
9. The walnut oil soap-based silicone oil-free shampoo as claimed in claim 6 wherein the pressure of the petroleum ether recovered under reduced pressure in step 4) is 1.0KPa to 1.2KPa and the temperature is 105 ℃ to 115 ℃.
10. The method of preparing a walnut oil soap-based silicone free shampoo according to any of claims 1-9 comprising the steps of:
s1: adding the sodium benzoate and the water softener in parts by weight into 50 parts of distilled water, and stirring for dissolving;
s2: putting the mixed solution obtained in the step S1 into a reaction kettle under the condition of stirring, adding the sodium carbonate, the sodium dodecyl sulfate, the walnut oil polyhydroxy stearic acid and the soap base according to the parts by weight, uniformly stirring, heating at 70-80 ℃, continuously stirring in the heating process, and keeping the temperature for 15-20 min;
s3: after the temperature is reduced to 40-60 ℃, adding the cocamidopropyl betaine, the nanocellulose and the polyethylene glycol in parts by weight into the mixture obtained in the step S2, stirring until the nanocellulose and the polyethylene glycol are completely dissolved, and keeping the temperature for 5-10 min;
s4: cooling to 30-35 ℃, adding the essence in parts by weight and the sodium chloride in parts by weight, adjusting the viscosity to 2000-3500 cp, and continuously stirring for 10-30min to obtain the walnut oil soap base silicone oil-free shampoo.
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