CN113599305B - Walnut oil soap base silicone oil-free shampoo and preparation method thereof - Google Patents

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

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CN113599305B
CN113599305B CN202110842864.8A CN202110842864A CN113599305B CN 113599305 B CN113599305 B CN 113599305B CN 202110842864 A CN202110842864 A CN 202110842864A CN 113599305 B CN113599305 B CN 113599305B
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walnut oil
oil
weight
sodium
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CN113599305A (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 base silicone oil-free shampoo and a preparation method thereof, wherein the shampoo does not contain polyorganosiloxane, and the shampoo 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 water softener; 0.06-0.15 part of essence; 15-20 parts of nanocellulose; 3-8 parts of polyethylene glycol; 5-10 parts of cocamidopropyl betaine; 5-10 parts of sodium dodecyl sulfate; 0.25 to 0.45 portion of sodium benzoate; 1-3 parts of sodium carbonate; sodium chloride 0.1-0.5 parts. The walnut oil polyhydroxy stearic acid adopted by the shampoo prepared by the invention is a novel modified soap base surfactant, the walnut oil with various unsaturated fatty acids is adopted, and the modified soap base is good in dissolubility and foam performance under neutral conditions and low temperature from natural grease of the extracted walnut oil.

Description

Walnut oil soap base 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 shiny. Fat in the oil is easily absorbed by hair follicles, and the hair is reinforced from inside. Fatty acids can moisturize hair and not allow hair to lose moisture. Vitamin E protects the hair from deleterious effects and helps prevent the hair from whitening. Walnut oil helps treat scalp infections that lead to hair loss. Some people use it to remove seborrheic dermatitis, a widely spread disease according to wikipedia. The effect is better if the walnut oil is mixed with jojoba oil or tea tree oil. Black walnut oil is even more effective against skin disorders and is believed to kill lice.
Walnut skin is a good method for naturally dyeing hair. Walnut oil is applied to hair without coloring, but is believed to lighten the color.
However, in the prior art, walnut oil is not used as a part of grease to synthesize a modified surfactant, and meanwhile, the shampoo which can nourish hair and replace silicone oil by utilizing beneficial components of the walnut oil is achieved while replacing a conventional surfactant.
Disclosure of Invention
Aiming at the defects, the invention provides the walnut oil soap base silicone oil-free shampoo which adopts walnut oil as a part of grease to synthesize the modified surfactant, and can utilize the beneficial components of the walnut oil to nourish hair and replace silicone oil while simultaneously replacing the conventional surfactant, and the preparation method thereof.
The invention provides the following technical scheme: the walnut oil soap-based silicone oil-free shampoo does not contain polyorganosiloxane, and comprises the following components in parts by weight:
further, the diameter of the nanocellulose is 10 nm-30 nm.
Further, the nanocellulose is one or more of nanocrystallized ethyl hydroxyethyl cellulose, nanocrystallized methyl hydroxypropyl cellulose or nanocrystallized methyl carboxypropyl cellulose.
Further, the water softener is one or more of sodium silicate, sodium tripolyphosphate and sodium hexametaphosphate.
Further, the preparation raw materials of the walnut oil polyhydroxy stearic acid comprise the following components in parts by weight:
30-50 parts of walnut oil;
further, the preparation method of the walnut oil polyhydroxy stearic acid comprises the following steps:
1) Mixing the weight parts of sodium hydroxide with one half of the weight parts of absolute ethyl alcohol to obtain sodium hydroxide ethanol solution, dripping the sodium hydroxide ethanol solution into the weight parts of walnut oil, saponifying for 1-1.5 h at 55-65 ℃, and then cooling to room temperature to obtain a precipitation solution with a lower soap cake;
2) Acidifying the soap cake in the precipitate obtained in the step 1) by adopting 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 to be neutral by using saturated sodium chloride, standing for layering, taking an upper layer oil layer as a 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 rest half of the absolute ethyl alcohol 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 the enriched unsaturated fatty acid;
4) The enriched unsaturated fatty acid obtained in the step 3) is firstly mixed with the weight part of H 2 O 2 Mixing, reacting at 30-35 ℃ for 30min, placing in a sulfuric acid methanol solution, esterifying for 3-4 h in a water bath at 60-70 ℃, cooling to room temperature after the reaction is finished, adding 20-30 parts of water, equally dividing the petroleum ether into 3 parts, extracting with 1 part of petroleum ether each time, extracting for 3 times, and merging into petroleum etherRecovering petroleum ether under reduced pressure, and weighing to constant weight to obtain oleum Juglandis 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 in a volume ratio of 1:200-1:250.
Further, the pressure of recovering petroleum ether under reduced pressure in the step 4) is 1.0 KPa-1.2 KPa, and the temperature is 105-115 ℃.
The invention also provides a preparation method of the walnut oil soap base silicone oil-free shampoo, which comprises the following steps:
s1: adding the sodium benzoate and the water softener in the weight parts into 50 parts of distilled water, and stirring for dissolution;
s2: under the stirring condition, placing the mixed solution obtained in the step S1 into a reaction kettle, adding the sodium carbonate, the sodium dodecyl sulfate, the walnut oil polyhydroxy stearic acid and the soap base in parts by weight into the reaction kettle, uniformly stirring, heating at 70-80 ℃, continuously stirring in the heating process, and preserving the temperature for 15-20 min;
s3: cooling to 40-60 ℃, adding the cocoamidopropyl betaine, the nanocellulose and the polyethylene glycol in parts by weight into the mixture obtained in the step S2, stirring until the components are completely dissolved, and preserving heat for 5-10 min;
s4: cooling to 30-35 ℃, adding the essence and the sodium chloride in parts by weight, adjusting the viscosity to 2000-3500 cp, and continuing stirring for 10-30min to obtain the walnut oil soap base silicone oil-free shampoo.
The beneficial effects of the invention are as follows:
1. the walnut oil in the walnut oil polyhydroxy stearic acid adopted by the shampoo is prepared by adopting a low-temperature extraction method, so that volatile nutritional ingredients in the walnut oil 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, the walnut oil with various unsaturated fatty acids is adopted, the fatty acids with different unsaturated degrees are obtained by hydrolysis from the natural oil of the extracted walnut oil, and then the polyhydroxy fatty acids with different hydroxyl numbers are obtained by oxidizing the double bonds of the unsaturated fatty acids, so that the modified soap base has the hard water resistance of modified soap base, has good solubility and foam performance under neutral conditions and low temperature, the defect of poor low-temperature solubility of common fatty acid sodium commonly used in the shampoo is avoided, and the defect of perishable rance of the walnut oil polyhydroxy stearic acid containing various unsaturated fatty acids is avoided due to urea.
3. The nano cellulose adopted by the shampoo prepared by the invention utilizes the self hydrophilic chemical characteristic, so that the shampoo has higher surface activity, and can effectively reduce the surface tension of an interface, thereby enhancing the foam stability of the shampoo in the use process.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The embodiment provides a walnut oil soap-based silicone oil-free shampoo, which does not contain polyorganosiloxane, and comprises the following components in parts by weight:
the walnut oil polyhydroxy stearic acid comprises the following raw materials in parts by weight:
the preparation method of the walnut oil polyhydroxy stearic acid comprises the following steps:
1) Mixing 20 parts of sodium hydroxide with 50 parts of absolute ethyl alcohol to obtain a sodium hydroxide ethanol solution, dripping the sodium hydroxide ethanol solution into the walnut oil of the weight parts, saponifying for 1.5 hours at 55 ℃, and then cooling to room temperature to obtain a precipitate with a lower soap cake;
2) Acidifying the soap cake in the precipitate obtained in the step 1) by adopting 12% hydrochloric acid, controlling the final pH of the reaction liquid to be 3.5 in the acidification process, then washing the mixture with saturated sodium chloride to neutral pH of 6.5, standing for layering, taking an upper layer 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 8 parts of urea into the rest 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, stirring uniformly, and refluxing in a water bath at 60 ℃ for 30min to obtain enriched unsaturated fatty acid;
4) The enriched unsaturated fatty acid obtained in the step 3) is firstly mixed with 30 parts of H 2 O 2 Mixing, reacting at 30deg.C for 30min, esterifying in water bath at 70deg.C for 3 hr, cooling to room temperature, adding 30 parts of water, equally dividing 30 parts of petroleum ether into 3 parts, extracting 1 part of petroleum ether (10 parts by weight per 1 part of petroleum ether) each time for 3 times, mixing to obtain petroleum ether phase, recovering petroleum ether under reduced pressure at 105deg.C and 1.2KPa, and weighing to constant weight to obtain oleum Juglandis polyhydroxyAnd (3) base stearic acid.
Through detection, unsaturated fatty acid obtained by hydrolyzing and enriching the walnut oil in the step 3) is 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 base silicone oil-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, stirring and dissolving;
s2: under the stirring condition, placing the mixed solution obtained in the step S1 into a reaction kettle, adding 3 parts of sodium carbonate, 5 parts of sodium dodecyl sulfate, 20 parts of walnut oil polyhydroxy stearic acid and the soap base, uniformly stirring, heating at 70 ℃, continuously stirring in the heating process, and preserving heat for 20min;
s3: cooling to 50 ℃, adding 10 parts of cocamidopropyl betaine, 20 parts of 10 nm-diameter nanometer methyl hydroxypropyl cellulose and 3 parts of polyethylene glycol into the mixture obtained in the step S2, stirring until the mixture is completely dissolved, and preserving heat for 7min;
s4: cooling to 35 ℃, adding 0.15 part of essence and 0.1 part of sodium chloride, adjusting the viscosity to 2000cp, and continuously stirring for 10min to obtain the walnut oil soap base silicone oil-free shampoo.
Example 2
The embodiment provides a walnut oil soap-based silicone oil-free shampoo, which does not contain polyorganosiloxane, and comprises the following components in parts by weight:
the walnut oil polyhydroxy stearic acid comprises the following raw materials in parts by weight:
the preparation method of the walnut oil polyhydroxy stearic acid comprises the following steps:
1) Mixing 15 parts of sodium hydroxide with 25 parts of absolute ethyl alcohol to obtain sodium hydroxide ethanol solution, dripping the sodium hydroxide ethanol solution into the walnut oil of the weight parts, saponifying for 1.2 hours at 65 ℃, and then cooling to room temperature to obtain a precipitate with a lower soap cake;
2) Acidifying the soap cake in the precipitate obtained in the step 1) by adopting 12% hydrochloric acid, controlling the final pH of the reaction liquid to be 3.0 in the acidification process, then washing to be neutral by using saturated sodium chloride, standing for layering, taking an upper oil layer as a 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 6.5 parts of urea into the rest 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, stirring uniformly, and refluxing in a water bath at 50 ℃ for 30min to obtain enriched unsaturated fatty acid;
4) The enriched unsaturated fatty acid obtained in the step 3) is firstly mixed with 20 parts of H 2 O 2 After mixing, reacting for 30min at 35 ℃, then placing in a concentrated sulfuric acid and methanol sulfuric acid methanol solution in a volume ratio of 1:250, esterifying for 4h 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 by weight of each part of petroleum ether), extracting by 1 part of petroleum ether each time for 3 times, merging into petroleum ether phase, recovering 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 acid obtained by hydrolyzing and enriching the walnut oil in the step 3) is 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 base silicone oil-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, stirring and dissolving;
s2: under the stirring condition, placing the mixed solution obtained in the step S1 into a reaction kettle, 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, heating at 80 ℃ after uniformly stirring, continuously stirring in the heating process, and preserving the temperature for 15min;
s3: cooling 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 mixture is completely dissolved, and preserving the heat for 5min;
s4: cooling to 32 ℃, adding the essence and the sodium chloride in parts by weight, adjusting the viscosity to 2500cp, and continuously stirring for 20min to obtain the walnut oil soap base silicone oil-free shampoo.
Example 3
The embodiment provides a walnut oil soap-based silicone oil-free shampoo, which does not contain polyorganosiloxane, and comprises the following components in parts by weight:
the walnut oil polyhydroxy stearic acid comprises the following raw materials in parts by weight:
the preparation method of the walnut oil polyhydroxy stearic acid comprises the following steps:
1) 10 parts of sodium hydroxide and 40 parts of absolute ethyl alcohol are mixed to obtain sodium hydroxide ethanol solution, the sodium hydroxide ethanol solution is dripped into the walnut oil with the weight parts, saponification is carried out for 1h at 60 ℃, and then the mixture is cooled to room temperature to obtain a precipitation solution with a lower soap cake;
2) Acidifying the soap cake in the precipitate obtained in the step 1) by adopting 12% hydrochloric acid, controlling the final pH of the reaction liquid to be 2.5 in the acidification process, then washing to be neutral by using saturated sodium chloride, standing for layering, taking an upper oil layer as a 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 5 parts of urea into the rest 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, stirring uniformly, and refluxing in a water bath at 55 ℃ for 30min to obtain enriched unsaturated fatty acid;
4) The enriched unsaturated fatty acid obtained in the step 3) is firstly mixed with 25 parts of H 2 O 2 After mixing, reacting for 30min at 33 ℃, then placing in a sulfuric acid methanol solution of concentrated sulfuric acid and methanol according to a volume ratio of 1:220, esterifying for 3.5h in a water bath at 60 ℃, 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 by weight of each part of petroleum ether), extracting by 1 part of petroleum ether each time for 3 times, merging into petroleum ether phase, 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 acid obtained by hydrolysis and enrichment of walnut oil in the step 3) is 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 base silicone oil-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, stirring and dissolving;
s2: under the stirring condition, placing the mixed solution obtained in the step S1 into a reaction kettle, 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, heating at 75 ℃ after uniformly stirring, continuously stirring in the heating process, and preserving the temperature for 17min;
s3: cooling 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 mixture is completely dissolved, and preserving heat for 10min;
s4: cooling to 30 ℃, adding 0.10 part of essence and 0.5 part of sodium chloride, adjusting the viscosity to 3500cp, and continuously stirring for 30min to obtain the walnut oil soap base silicone oil-free shampoo.
Comparative example 1
This example differs from example 1 only in that a polyorganosiloxane was used instead of cocamidopropyl betaine having the same lubricating and softening effects, the polyorganosiloxane being present in the same parts by weight as the cocamidopropyl betaine in example 1.
Comparative example 2
The difference between this example and example 1 is that the walnut oil polyhydroxy stearic acid in the example was replaced with sodium laureth sulfate having the efficacy of a surfactant, and the weight part of sodium laureth sulfate was the same as that of the walnut oil polyhydroxy stearic acid.
Comparative example 3
This example differs from example 1 only in that no shampoo was prepared using 10nm diameter nano methyl hydroxypropyl cellulose.
Experimental example 1
The shampoos of examples 1 to 3 and comparative examples 1 to 3 of the present invention were prepared as solutions having a mass fraction of 1%, and the solutions were slowly heated or cooled, and the critical temperature at which the solutions suddenly changed from cloudiness to clarification was the Krafft Point (Krafft Point), and the measurements were repeated three times to obtain the average value. The results are shown in Table 1.
Experimental example 2
At a certain temperature, 10mL of the shampoo of the invention examples 1-3 and comparative examples 1-3 is respectively measured and prepared into a solution with the mass fraction of 0.1%, the solution is placed in a 100mL measuring cylinder with a plug, the buffer solution is added for dilution to 30mL, the shaking is violently carried out for 10 times after the plug is arranged, the bubble volume H0 is recorded after standing for 30 seconds, the bubble stabilizing volume H1 is recorded after 5 minutes, and the average value of the bubble volumes of 5 parallel experiments is taken as the foaming force, wherein the larger the bubble volume is, the better the foaming force is. The results are shown in Table 1.
TABLE 1
Kraff point Bubble volume
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 with a stirrer for 10 seconds, the foam height was recorded for evaluation of foamability/initial foam height, and after standing for 5 minutes, the height of the water surface under the foam (drainage height) was recorded for evaluation of foam stability. The results are shown in Table 2.
TABLE 2
Foam height Drainage height
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 with a diameter of 10nm to 30nm can effectively increase the foam height of the shampoo and effectively reduce the water outlet height below the foam, meaning that the stability of the foam is enhanced, and the comparative example 3 shows that the stability is poor because nanocellulose is not added, the water outlet height is greatly increased.
Ames test shows that the shampoo prepared by the invention has the specification of composite national standard GB7919-1987 (cosmetic safety evaluation procedure and method)
The above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Furthermore, those skilled in the art will appreciate that while some embodiments herein include some features but not others included in other embodiments, 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 below, 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 (8)

1. A walnut oil soap-based silicone oil-free shampoo, which does not contain polyorganosiloxane, and is characterized by comprising the following components in parts by weight:
the preparation raw materials of the walnut oil polyhydroxy stearic acid comprise the following components in parts by weight:
the preparation method of the walnut oil polyhydroxy stearic acid comprises the following steps:
1) Mixing the weight parts of sodium hydroxide with one half of the weight parts of absolute ethyl alcohol to obtain sodium hydroxide ethanol solution, dripping the sodium hydroxide ethanol solution into the weight parts of walnut oil, saponifying for 1-1.5 h at 55-65 ℃, and then cooling to room temperature to obtain a precipitation solution with a lower soap cake;
2) Acidifying the soap cake in the precipitate obtained in the step 1) by adopting 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 to be neutral by using saturated sodium chloride, standing for layering, taking an upper layer oil layer as a 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 rest half of the absolute ethyl alcohol 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 the enriched unsaturated fatty acid;
4) The enriched unsaturated fatty acid obtained in the step 3) is firstly mixed with the weight part of H 2 O 2 After mixing, reacting for 30min at 30-35 ℃, then placing in a sulfuric acid methanol solution, esterifying for 3-4 h at 60-70 ℃ in a water bath, cooling to room temperature after the reaction is finished, then adding 20-30 parts of water, equally dividing the petroleum ether into 3 parts, extracting by 1 part of petroleum ether each time for 3 times, merging 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.
2. The walnut oil soap-based silicone-oil-free shampoo according to claim 1, wherein the diameter of the nanocellulose is 10 nm-30 nm.
3. The walnut oil soap-based silicone oil-free shampoo according to claim 1, wherein the nanocellulose is one or more of nanocylethyl hydroxyethyl cellulose, nanocymethyl hydroxypropyl cellulose or nanocymethyl carboxypropyl cellulose.
4. The walnut oil soap-based silicone-oil-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 according to claim 1, wherein 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.
6. The walnut oil soap-based silicone oil-free shampoo according to claim 1, wherein the sulfuric acid methanol solution in the step 4) is concentrated sulfuric acid and methanol in a volume ratio of 1:200-1:250.
7. The walnut oil soap-based silicone oil-free shampoo according to claim 1, wherein the pressure of recovering petroleum ether under reduced pressure in the step 4) is 1.0KPa to 1.2KPa, and the temperature is 105 ℃ to 115 ℃.
8. A method for preparing the walnut oil soap-based silicone oil-free shampoo according to any one of claims 1 to 7, which is characterized by comprising the following steps:
s1: adding the sodium benzoate and the water softener in the weight parts into 50 parts of distilled water, and stirring for dissolution;
s2: under the stirring condition, placing the mixed solution obtained in the step S1 into a reaction kettle, adding the sodium carbonate, the sodium dodecyl sulfate, the walnut oil polyhydroxy stearic acid and the soap base in parts by weight into the reaction kettle, uniformly stirring, heating at 70-80 ℃, continuously stirring in the heating process, and preserving the temperature for 15-20 min;
s3: cooling to 40-60 ℃, adding the cocoamidopropyl betaine, the nanocellulose and the polyethylene glycol in parts by weight into the mixture obtained in the step S2, stirring until the components are completely dissolved, and preserving heat for 5-10 min;
s4: cooling to 30-35 ℃, adding the essence and the sodium chloride in parts by weight, adjusting the viscosity to 2000-3500 cp, and continuing stirring for 10-30min to obtain the walnut oil soap base silicone oil-free shampoo.
CN202110842864.8A 2021-07-26 2021-07-26 Walnut oil soap base silicone oil-free shampoo and preparation method thereof Active CN113599305B (en)

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