阅读说明：本技术 一种乳化产品及其制备工艺 (Emulsified product and preparation process thereof ) 是由 任玉惠 杨菲林 刘影 于 2021-10-28 设计创作，主要内容包括：本发明提供一种乳化产品及其制备工艺,包括以下重量百分比原料：油相5～25％、乳化剂1～7％、增稠剂0.1～2％、保湿剂5～15％、余量为去离子水；本发明将各原料科学配比,调整组成各个原料之间的比例,通过温度、控制搅拌和均质速度、时间,使其在反应体系中更分散,有效成分更加均匀,无需在产品制备前提前预处理增稠剂的预溶解、溶胀,最终实现一致的增稠效果,获得的乳化产品长期稳定,在作物表面的粘附力更强。(The invention provides an emulsified product and a preparation process thereof, wherein the emulsified product comprises the following raw materials in percentage by weight: 5-25% of an oil phase, 1-7% of an emulsifier, 0.1-2% of a thickener, 5-15% of a humectant and the balance of deionized water; according to the invention, the raw materials are scientifically proportioned, the proportion of the raw materials is adjusted, the raw materials are dispersed in a reaction system through temperature and control of stirring and homogenizing speed and time, the effective components are more uniform, pre-dissolving and swelling of the thickening agent are not required to be pre-treated before the preparation of the product, the consistent thickening effect is finally realized, the obtained emulsified product is stable for a long time, and the adhesion on the surface of crops is stronger.)

1. An emulsified product characterized by: comprises the following raw materials in percentage by weight: 5-25% of an oil phase, 1-7% of an emulsifier, 0.1-2% of a thickener, 5-15% of a humectant and the balance of deionized water;

the oil phase comprises one or more than two of natural oil, synthetic oil and silicone oil;

the emulsifier is one or more of polysorbate, sorbitan stearate, cetearyl alcohol, stearic acid, glyceryl stearate, cetyl alcohol, stearyl alcohol, glyceryl stearate PEG-100, behenyl alcohol, coco glucoside, sucrose esters, alkyl glucoside, fatty acid polyglycerol esters, and lecithin;

the thickening agent is one or the combination of more than two of xanthan gum, carbomer, 2-acrylamide-2-methyl propyl sulfonate sodium, acryloyl dimethyl taurate/VP copolymer, hydroxyethyl cellulose, hydroxyethyl acrylate/acryloyl dimethyl taurate copolymer, acrylate copolymer sodium and acrylate/C10-30 alkanol acrylate cross-linked copolymer;

the humectant is one or more of trehalose, propylene glycol, 1, 3-butanediol, glycerol, glyceryl polyether-26, biological polysaccharide gum, xylitol, panthenol, allantoin, sodium hyaluronate, and Tremella polysaccharide.

2. An emulsified product as claimed in claim 1, wherein: comprises the following raw materials in percentage by weight: 15% of oil phase, 3% of emulsifier, 1.2% of thickener, 10% of humectant and the balance of deionized water.

3. An emulsified product as claimed in claim 1, wherein: the natural oil is one or more of coconut oil, shea butter, hydrogenated vegetable oil, macadamia nut oil, jojoba seed oil, white Potentilla chinensis seed oil, sweet almond oil, sunflower seed oil, almond oil, corn germ oil and squalane.

4. An emulsified product as claimed in claim 1, wherein: the synthetic oil is one or more of white oil, caprylic/capric triglyceride, isododecane, glycerol, vaseline, dioctyl carbonate, propylene glycol, butanediol, isononyl isononanoate, cetyl ethyl hexanoate and isostearic acid ester.

5. An emulsified product as claimed in claim 1, wherein: the silicone oil is one or more of gel silicone elastomer, polydimethylsiloxane, cyclopentadimethylsiloxane and dimethiconol.

6. A process for the preparation of an emulsified product according to claim 1, wherein: the method comprises the following steps:

s1, adding the humectant into deionized water, stirring at 20-80 rpm while heating to 80 +/-5 ℃, and uniformly mixing to obtain a phase A;

s2, placing 30-60% of the total weight of the oil phase and the thickening agent into an oil pan, stirring and heating to 70-85 ℃ at 20-80 rpm, preserving heat for 10-30 min, and uniformly stirring to obtain a phase B;

s3, adding the phase B into the phase A while stirring, homogenizing and emulsifying for 5-10 min under the conditions of 1000-4000 rpm and 85 +/-2 ℃, continuously stirring for 10-20 min at 20-80 rpm, and preserving heat;

s4, adding the rest of thickening agent into the feed liquid obtained in the step S3, homogenizing at 1000-4000 rpm for 1-5 min, and then continuously stirring at 20-80 rpm for 5-30 min; cooling to 35-45 ℃, homogenizing at 500-2000 rpm for 1-10 min, stirring at 10-80 rpm for 10-30 min, and filtering to obtain a finished product.

Technical Field

The invention relates to the technical field of cosmetics, in particular to an emulsified product and a preparation process thereof.

Background

Along with the improvement of living standard of people, people pay more and more attention to the maintenance and care of skin, various functional products such as emulsified products on the market, moisture preservation, sun protection, aging resistance and the like are endless, but the emulsifying effect in the preparation process is poor, so that functional factors in the emulsified products cannot be well utilized, the absorption effect of the products is poor, the cost is wasted, and further, many merchants optimize from the direction of emulsifying process and thickening agent adjustment, but the existing emulsifying agents and thickening agents are various, when powdery emulsified thickening agents are selected, the subsequent dissolution is assisted by means of sufficient pre-dissolution, swelling and the like, and the conventional thickening agents are added into a water phase or an oil phase, but the emulsified products belong to a high-oil system, the water content is low, and the powdery thickening agents cannot be fully pre-dissolved, the problems of process failure, poor product stability and the like are easily caused.

Disclosure of Invention

In view of the above, the present invention provides an emulsified product and a preparation process thereof, which solve the above problems.

The technical scheme of the invention is realized as follows: an emulsified product comprises the following raw materials in percentage by weight: 5-25% of an oil phase, 1-7% of an emulsifier, 0.1-2% of a thickener, 5-15% of a humectant and the balance of deionized water;

the oil phase comprises one or more than two of natural oil, synthetic oil and silicone oil;

the emulsifier is one or more of polysorbate, sorbitan stearate, cetearyl alcohol, stearic acid, glyceryl stearate, cetyl alcohol, stearyl alcohol, glyceryl stearate PEG-100, behenyl alcohol, coco glucoside, sucrose esters, alkyl glucoside, fatty acid polyglycerol esters, and lecithin;

the thickening agent is one or the combination of more than two of xanthan gum, carbomer, 2-acrylamide-2-methyl propyl sulfonate sodium, acryloyl dimethyl taurate/VP copolymer, hydroxyethyl cellulose, hydroxyethyl acrylate/acryloyl dimethyl taurate copolymer, acrylate copolymer sodium and acrylate/C10-30 alkanol acrylate cross-linked copolymer;

the humectant is one or more of trehalose, propylene glycol, 1, 3-butanediol, glycerol, glyceryl polyether-26, biological polysaccharide gum, xylitol, panthenol, allantoin, sodium hyaluronate, and Tremella polysaccharide.

Further, the emulsified product also comprises 0.3-1% of active matters and 0.5-4% of preservatives, wherein the active matters are yeast fermentation product filtrate and lactic acid fermentation product filtrate which are commercially available; the antiseptic is one of caprylyl hydroximic acid, 1, 2-pentanediol, 1, 2-hexanediol, and caprylyl glycol.

Further, the emulsified product comprises the following raw materials in percentage by weight: 15% of oil phase, 3% of emulsifier, 1.2% of thickener, 10% of humectant, 0.7% of active matter, 2% of preservative and the balance of deionized water.

Further, the natural oil is one or more of coconut oil, shea butter, hydrogenated vegetable oil, macadamia nut oil, jojoba seed oil, white pond flower seed oil, sweet almond oil, sunflower seed oil, almond oil, corn germ oil and squalane.

Further, the synthetic oil and fat is one or more of white oil, caprylic/capric triglyceride, isododecane, glycerol, vaseline, dioctyl carbonate, propylene glycol, butylene glycol, isononyl isononanoate, cetyl ethylhexanoate and isostearic acid ester.

Further, the silicone oil is one or more of gel silicone elastomer, polydimethylsiloxane, cyclopentadimethylsiloxane and dimethiconol.

Further, the preparation process of the emulsified product comprises the following steps:

s1, adding the humectant into deionized water, stirring at 20-80 rpm while heating to 80 +/-5 ℃, and uniformly mixing to obtain a phase A;

s2, placing 30-60% of the total weight of the oil phase and the thickening agent into an oil pan, stirring and heating to 70-85 ℃ at 20-80 rpm, preserving heat for 10-30 min, and uniformly stirring to obtain a phase B;

s3, adding the phase B into the phase A while stirring, homogenizing and emulsifying for 5-10 min under the conditions of 1000-4000 rpm and 85 +/-2 ℃, continuing stirring for 10-20 min at 20-80 rpm, and keeping the temperature;

s4, adding the rest of thickening agent into the feed liquid obtained in the step S3, homogenizing at 1000-4000 rpm for 1-5 min, and then continuously stirring at 20-80 rpm for 5-30 min; cooling to 35-45 ℃, adding the active substance and the preservative, homogenizing at 500-2000 rpm for 1-10 min, stirring at 10-80 rpm for 10-30 min, and filtering to obtain a finished product.

Compared with the prior art, the invention has the beneficial effects that:

(1) the invention reasonably selects each raw material, scientifically mixes the oil phase, the humectant, the thickener, the emulsifier and other raw materials, combines the preparation process, and uniformly disperses the system by controlling the temperature, the stirring speed, the homogenizing speed and the time.

(2) According to the preparation process, the thickening agent is added through a two-step method, part of the thickening agent is added into the oil phase, and the rest of the thickening agent is added into the water phase, so that the powdery thickening agent is effectively dispersed, aggregation and agglomeration are avoided, uniform and consistent thickening effect is realized, pre-dissolution and swelling of the thickening agent are not required to be pre-treated before preparation of a product, and other adverse factors in the pre-treatment process can be avoided to cause viscosity difference among batches.

(3) The emulsified product has good skin feel, stable appearance in stability investigation, no oil-water separation, stable viscosity, stable and expected viscosity, stable emulsifying system and excellent skin feel.

Detailed Description

In order to better understand the technical content of the invention, specific examples are provided below to further illustrate the invention.

The experimental methods used in the examples of the present invention are all conventional methods unless otherwise specified.

The materials, reagents and the like used in the examples of the present invention can be obtained commercially without specific description.

Example 1

An emulsified product comprises the following raw materials in percentage by weight: 5% of oil phase, 1% of emulsifier, 0.1% of thickener, 5% of humectant, 0.3% of active matter, 0.5% of preservative and the balance of deionized water; the oil phase is white oil, caprylic/capric triglyceride, gel silicone shell and squalane in a volume ratio of 3:5:3: 3; the emulsifier is prepared from the following components in a volume ratio of 0.6: 0.4: 0.5 polysorbate, sorbitan stearate, cetearyl alcohol; the thickening agent is hydroxyethyl acrylate/sodium acryloyl dimethyl sulfonate copolymer; the humectant is 1, 3-butanediol, propylene glycol and glycerol in a volume ratio of 3:3: 5; the active substances are yeast fermentation product filtrate and lactic acid fermentation product filtrate in a volume ratio of 2:1, and the preservative is caprylyl hydroximic acid.

Example 2

An emulsified product comprises the following raw materials in percentage by weight: 25% of oil phase, 7% of emulsifier, 2% of thickener, 15% of humectant, 1% of active matter, 4% of preservative and the balance of deionized water; the oil phase is white oil, caprylic/capric triglyceride, gel silicone shell and squalane in a volume ratio of 3:5:3: 3; the emulsifier is prepared from the following components in a volume ratio of 0.6: 0.4: 0.5 polysorbate, sorbitan stearate, cetearyl alcohol; the thickening agent is hydroxyethyl acrylate/sodium acryloyl dimethyl sulfonate copolymer; the humectant is 1, 3-butanediol, propylene glycol and glycerol in a volume ratio of 3:3: 5; the active substances are yeast fermentation product filtrate and lactic acid fermentation product filtrate in a volume ratio of 2:1, and the preservative is 1, 2-pentanediol.

Example 3

An emulsified product comprises the following raw materials in percentage by weight: 15% of oil phase, 3% of emulsifier, 1.2% of thickener, 10% of humectant, 0.7% of active matter, 2% of preservative and the balance of deionized water; the oil phase is white oil, caprylic/capric triglyceride, gel silicone shell and squalane in a volume ratio of 3:5:3: 3; the emulsifier is prepared from the following components in a volume ratio of 0.6: 0.4: 0.5 polysorbate, sorbitan stearate, cetearyl alcohol; the thickening agent is hydroxyethyl acrylate/sodium acryloyl dimethyl sulfonate copolymer; the humectant is 1, 3-butanediol, propylene glycol and glycerol in a volume ratio of 3:3: 5; the active substances are yeast fermentation product filtrate and lactic acid fermentation product filtrate in a volume ratio of 2:1, and the preservative is caprylyl glycol;

the emulsified products of the above examples 1 to 3 were prepared by the following preparation methods:

s1, adding the humectant into deionized water, stirring and heating to 80 ℃ at 50rpm, and uniformly mixing to obtain a phase A;

s2, placing 50% of the total mass of the oil phase and the thickening agent into an oil pan, heating to 80 ℃ under stirring at 50rpm, preserving heat for 20min, and uniformly stirring to obtain a phase B;

s3, adding the phase B into the phase A while stirring, homogenizing and emulsifying for 8min at 2000rpm and 85 ℃, continuing stirring for 15min at 50rpm, and keeping the temperature;

s4, adding the rest thickening agent into the feed liquid obtained in the step S3, homogenizing at 3000rpm for 3min, continuously stirring at 50rpm for 13min, and cooling to 40 ℃; adding antiseptic and active substance, homogenizing at 1200rpm for 6min, stirring at 50rpm for 20min, filtering, discharging, and storing in a designated container to obtain the final product

Example 4

The difference between the embodiment and the embodiment 3 is that an emulsified product comprises the following raw materials in percentage by weight: 5% of oil phase, 1% of emulsifier, 0.1% of thickener, 5% of humectant, 0.3% of active matter, 0.5% of preservative and the balance of deionized water; the oil phase is white oil, caprylic/capric triglyceride, gel silicone shell and squalane in a volume ratio of 3:5:3: 3; the emulsifier is prepared from the following components in a volume ratio of 0.6: 0.4: 0.5 polysorbate, sorbitan stearate, cetearyl alcohol; the thickening agent is hydroxyethyl acrylate/sodium acryloyl dimethyl sulfonate copolymer; the humectant is 1, 3-butanediol, propylene glycol and glycerol in a volume ratio of 3:3: 5; the active substances are yeast fermentation product filtrate and lactic acid fermentation product filtrate in a volume ratio of 2:1, and the preservative is caprylyl glycol;

the emulsified product is prepared by the following preparation method:

s1, adding the humectant into deionized water, stirring and heating to 80 ℃ at 20rpm, and uniformly mixing to obtain a phase A;

s2, placing 30% of the total mass of the oil phase and the thickening agent into an oil pan, heating to 70 ℃ under stirring at 20rpm, preserving heat for 10min, and uniformly stirring to obtain a phase B;

s3, adding the phase B into the phase A while stirring, homogenizing and emulsifying for 5min at 1000rpm and 85 ℃, continuously stirring for 10min at 20rpm, and keeping the temperature;

s4, adding the rest thickening agent into the feed liquid obtained in the step S3, homogenizing at 1000rpm for 1min, and then continuing stirring at 20rpm for 5 min; cooling to 35 deg.C, adding antiseptic and active substance, homogenizing at 500rpm for 1min, stirring at 10rpm for 10min, and filtering to obtain the final product.

Example 5

The difference between the embodiment and the embodiment 3 is that an emulsified product comprises the following raw materials in percentage by weight: 25% of oil phase, 7% of emulsifier, 2% of thickener, 15% of humectant, 1% of active matter, 4% of preservative and the balance of deionized water; the oil phase is white oil, caprylic/capric triglyceride, gel silicone shell and squalane in a volume ratio of 3:5:3: 3; the emulsifier is prepared from the following components in a volume ratio of 0.6: 0.4: 0.5 polysorbate, sorbitan stearate, cetearyl alcohol; the thickening agent is hydroxyethyl acrylate/sodium acryloyl dimethyl sulfonate copolymer; the humectant is 1, 3-butanediol, propylene glycol and glycerol in a volume ratio of 3:3: 5; the active matter is yeast fermentation product filtrate and lactic acid fermentation product filtrate in a volume ratio of 2:1, and the preservative is caprylyl glycol.

The emulsified product is prepared by the following preparation method:

s1, adding the humectant into deionized water, stirring and heating to 85 ℃ at 80rpm, and uniformly mixing to obtain a phase A;

s2, placing 60% of the total weight of the oil phase and the thickening agent into an oil pan, heating to 85 ℃ under stirring at 80rpm, preserving heat for 30min, and uniformly stirring to obtain a phase B;

s3, adding the phase B into the phase A while stirring, homogenizing and emulsifying for 10min at 4000rpm and 87 ℃, continuing stirring for 20min at 80rpm, and keeping the temperature;

s4, adding the rest thickening agent into the feed liquid obtained in the step S3, homogenizing at 4000rpm for 5min, and continuing stirring at 80rpm for 30 min; cooling to 45 ℃, adding the preservative and the active substance, homogenizing at 2000rpm for 1-10 min, stirring at 80rpm for 30min, and filtering to obtain a finished product.

Comparative example 1

The comparative example differs from example 3 in that an emulsified product comprises the following raw materials in percentage by weight: 3% of an oil phase, 8% of an emulsifier, 0.3% of a thickener, 20% of a humectant, 1.5% of an active substance, 5% of a preservative and the balance of deionized water, wherein the oil phase comprises white oil, caprylic/capric triglyceride, gel silicone elastomer and squalane in a volume ratio of 3:5:3: 3; the emulsifier is prepared from the following components in a volume ratio of 0.6: 0.4: 0.5 polysorbate, sorbitan stearate, cetearyl alcohol; the thickening agent is hydroxyethyl acrylate/sodium acryloyl dimethyl sulfonate copolymer; the humectant is 1, 3-butanediol, propylene glycol and glycerol in a volume ratio of 3:3: 5; the active matter is yeast fermentation product filtrate and lactic acid fermentation product filtrate in a volume ratio of 2:1, and the preservative is caprylyl glycol.

Comparative example 2

This comparative example differs from example 3 in that the whole thickener was added to the oil phase in the step S2, the step S4 was carried out without adding the thickener, and the other steps were not changed,

the method comprises the following specific steps:

an emulsified product comprises the following raw materials in percentage by weight: 15% of oil phase, 3% of emulsifier, 1.2% of thickener, 10% of humectant, 0.7% of active matter, 2% of preservative and the balance of deionized water; the oil phase is white oil, caprylic/capric triglyceride, gel silicone shell and squalane in a volume ratio of 3:5:3: 3; the emulsifier is prepared from the following components in a volume ratio of 0.6: 0.4: 0.5 polysorbate, sorbitan stearate, cetearyl alcohol; the thickening agent is hydroxyethyl acrylate/sodium acryloyl dimethyl sulfonate copolymer; the humectant is 1, 3-butanediol, propylene glycol and glycerol in a volume ratio of 3:3: 5; the active substances are yeast fermentation product filtrate and lactic acid fermentation product filtrate in a volume ratio of 2:1, and the preservative is caprylyl glycol;

the emulsified product is prepared by the following preparation method:

s1, adding the humectant into deionized water, stirring and heating to 80 ℃ at 50rpm, and uniformly mixing to obtain a phase A;

s2, placing the oil phase and the thickening agent into an oil pan, heating to 80 ℃ under stirring at 50rpm, preserving heat for 20min, and uniformly stirring to obtain a phase B;

s3, adding the phase B into the phase A while stirring, homogenizing and emulsifying for 8min at 2000rpm and 85 ℃, continuing stirring for 15min at 50rpm, and keeping the temperature;

s4, cooling the feed liquid obtained in the step S3 to 45 ℃, adding the preservative and the active substances, homogenizing at 1200rpm for 6min, then stirring at 50rpm for 20min, filtering, and discharging to obtain a finished product.

First, performance test

(1) Measurement of viscosity, surface tension and osmotic force

The emulsified products obtained in the above examples 1 to 5 and comparative examples 1 to 3 were tested for viscosity, surface tension, and permeability, and the results were as follows:

as can be seen from the above table, the emulsified products obtained in the embodiments 1 to 5 of the present invention have significantly higher viscosity and permeability than the comparative examples, and the surface tension is significantly reduced compared to the comparative examples; comparing examples 1-5 with comparative example 1, it is shown that each raw material component can achieve better performance effect under a specific proportion; compared with the comparative example 2, the method shows that the powdery thickening agent can be effectively dispersed by adding the thickening agent step by step, uniform thickening effect is realized, and the expected viscosity is finally reached; examples 1 to 3 show that, by controlling the temperature, stirring speed, homogenizing speed and time, better emulsifying performance can be achieved, as compared with examples 4 and 5.

(2) Stability test

The emulsified products prepared in examples 1 to 5 of the present invention and comparative examples 1 to 2 were separately packaged in commercially available sample bottles and placed in thermostats having different temperature settings, the thermostats having temperatures of 4 ℃, 25 ℃, 40 ℃, 45 ℃ and 50 ℃ and a relative humidity of 75%, respectively, and were sampled at 1 week (1W), 1 month (1M) and 3 months (3M), and the stability of the emulsified products was observed, and the results are shown in table 2:

note: the expression indicates separated oil content, the expression ^ indicates separated water, the expression indicates layering, and the expression indicates no layering and oil-separated water phenomenon.

Viscosity stability:

the emulsified products prepared using example 3 and comparative example 2 of the present invention were separately packaged in commercially available sample bottles and placed in thermostats set at-18 ℃, 4 ℃, 25 ℃, 40 ℃, 45 ℃ and 50 ℃ with a relative humidity of 75% for immediate, 7, 30 and 90 days, and the viscosity was measured at 10S according to GB/T15357 using an NDJ-5S viscometer, spindle # 3, at a rotation speed of 12rpm, with the results as follows:

the results show that:

example 3 at-18 ℃, 4 ℃, 25 ℃, 45 ℃, 50 ℃ the product appearance shape is stable, the viscosity can be continuously maintained within +/-10% of the initial value, but the preparation method of comparative example 2, the product character appears unstable, the viscosity change is very large, even the viscosity reaches 13% of the expected viscosity in 90 days of detection, and the emulsified product performance is extremely unstable.

The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.