WO2024109460A1

WO2024109460A1 - Viscosity-controllable composition and use thereof

Info

Publication number: WO2024109460A1
Application number: PCT/CN2023/127669
Authority: WO
Inventors: 康静; 倪向梅
Original assignee: 上海家化联合股份有限公司
Priority date: 2022-11-24
Filing date: 2023-10-30
Publication date: 2024-05-30
Also published as: CN115813809A

Abstract

Disclosed herein is a composition comprising PEG-240/HDI copolymer bis-decyltetradeceth-20 ether, water and polyol. An inorganic and organic balance value (IOB) of the polyol is below 5. A weight ratio of the PEG-240/HDI copolymer bis-decyltetradeceth-20 ether to the sum of the water and the polyol is 1:2 to 1:30. A weight ratio of the water to the polyol is 1:29 to 29:1. The present invention also relates to use of the composition comprising the PEG-240/HDI copolymer bis-decyltetradeceth-20 ether, the water and the polyol in cosmetics.

Description

Viscosity controllable composition and its application

Technical Field

The invention relates to the field of cosmetics, and in particular to a viscosity-controllable composition containing PEG-240/HDI copolymer bis-decyltetradecanol polyether-20 ether, water and polyol.

Background technique

PEG-240/HDI copolymer bis-decyltetradecanol polyether-20 ether is a water-soluble nonionic polymer. Its thickener mechanism is that the hydrophobic groups at both ends of the molecular chain attract each other to form petal-shaped micelles, which make the macromolecular chain produce intramolecular or intermolecular association. When the concentration of micelles in aqueous solution exceeds a certain value, a three-dimensional network polymer chain will be formed, so it is also called an associative thickener. The micelle binding ability of PEG-240/HDI copolymer bis-decyltetradecanol polyether-20 ether is weak. Under the action of shear force, it can achieve association-disassociation equilibrium. The viscosity of the system only decreases slightly. When the external force is removed, the viscosity quickly recovers, and the effect of self-leveling can be achieved. At present, PEG-240/HDI copolymer bis-decyltetradecanol polyether-20 ether has been widely used in skin care cosmetics formulas such as creams, gels, essences, sprays, facial masks, hair masks, hair sprays, and makeup.

In the daily chemical industry, there are two main commercial raw materials with the corresponding ingredient name "PEG-240/HDI copolymer bis-decyl tetradecyl alcohol polyether-20 ether", one is GT-700 (trade name: ADEKA NOL GT-700), and the other is GT-730 (trade name: ADEKA NOL GT-730). Both raw materials come from ARKED. GT-700 was first launched in 2012, and then the company launched GT-730. GT-730 is a liquid composition composed of 30% GT-700, 50% butanediol, 19.94% water, 0.03% potassium laurate, and 0.03% tocopherol.

The processing technology of GT-700 is usually used in the field of daily chemicals. GT-700 is placed in the water phase, heated to 80-85°C, stirred and homogenized until the material is evenly dispersed. CN110711171A discloses a mirror cream with wrinkle removal and repairing effects. The preparation process of the wrinkle removal and repairing mirror cream is disclosed. GT-700 is placed in the water phase and put into the emulsifier to heat to 85°C, stir evenly, start the homogenization process at 2000rpm for 5 minutes, and keep warm and stir for 30 minutes. The water phase components include: water, disodium EDTA, sodium hyaluronate, Glycerin, propylene glycol, sodium polyacrylate, PEG-240/HDI copolymer bis-decyl tetradecanol polyether-20 ether, p-hydroxyacetophenone, 1,2-hexanediol. CN114617835A A two-dose DIY cream mask and its preparation method, and also proposes a two-dose DIY cream mask preparation process, GT-700 is placed in the water phase and put into the emulsifying pot, stirred and heated to 80℃-85℃, and then homogenized until the material is completely dispersed without particles, and kept warm for 20 minutes; its water phase components include: water, glycerin, butylene glycol, polyethylene glycol-8, methyl ester, acrylic acid (ester)/C10-30 alkyl acrylate cross-linked polymer, xanthan gum, PEG-240/HDI copolymer bis-decyl tetradecanol polyether-20 ether, allantoin, erythritol, etc. The preparation process of this type of product is a one-step heating method, that is, GT-700 is heated together with the water phase and other water phase raw materials to a relatively high temperature (80-85°C), supplemented by a long period of stirring or a high-energy homogenization process, which requires a lot of stirring time and heat and electricity. This not only increases production costs, but also goes against the energy conservation, emission reduction and low-carbon environmental protection concepts currently advocated by the country.

Another processing technology is to directly use GT-730 as a pre-dispersion liquid of GT-700. CN114191332A A hair mask with shape memory function and its preparation method, designed a hair mask with shape memory function, the preparation process of its aqueous phase is to add a thickener to water and stir evenly, while stirring, heat it to 80 ℃ ~ 95 ℃, add GT-730 and polyol, keep the temperature and stir evenly. There is also CN113784760A gel skin external composition, which discloses that the gel skin external use also directly uses GT-730 as a pre-dispersion liquid of GT-700. Although GT-730 is a pre-dispersion liquid of GT-700, its application flexibility in the formula is not high, which limits its application in other cosmetic formula systems. On the other hand, it also increases the cost of the enterprise. For example, a cosmetics company has already started using GT-700. In order to facilitate production, if it can only choose GT-730 instead of the original GT-700, this will undoubtedly increase the cost of the enterprise; if both are purchased, the pressure of raw material inventory will be increased. For example, the viscosity of GT-730 preparation is relatively high, which makes it inconvenient to pour when adding in actual production. In addition, there is no report on the effect of the ratio of GT-700 to water and polyol on rheology.

Scientific production methods and energy-saving and efficient processes are what enterprises pursue. On the one hand, they reduce energy loss, and on the other hand, they simplify production processes. This can not only reduce production costs and improve the economic benefits of the enterprise, but also promote the long-term development of daily chemical production processes.

The present invention unexpectedly found that the method of preparing a certain composition of GT-700 with polyol and water consumes significantly less time, heat energy and electric energy than the process of directly adding GT-700 into the water phase. In addition, the study found that the ratio of polyols with different IOB values to water also has a significant effect on the rheological properties of the composition, which means that it can meet the needs of different formulation systems and expand the application field of GT-700.

Summary of the invention

In one aspect, the present invention provides a composition comprising PEG-240/HDI copolymer bis-decyltetradecyl alcohol polyether-20 ether, water and a polyol,

wherein the inorganic-organic balance (IOB) value of the polyol is less than 5;

wherein the weight ratio of PEG-240/HDI copolymer bis-decyltetradecyl alcohol polyether-20 ether to the sum of water and polyol is 1:2 to 1:30;

Wherein, the weight ratio of water to polyol is 1:29 to 29:1.

In a preferred embodiment, the weight ratio of PEG-240/HDI copolymer bis-decyltetradecyl alcohol polyether-20 ether to the sum of water and polyol is 1:14 to 1:30, and the weight ratio of water to polyol is ≤1.

In a preferred embodiment, the weight ratio of water to polyol is 1:1 to 29:1.

In a preferred embodiment, the weight ratio of PEG-240/HDI copolymer bis-decyltetradecyl alcohol polyether-20 ether: water: polyol is 1:1:13 to 1:5:9.

In a preferred embodiment, the weight ratio of PEG-240/HDI copolymer bis-decyltetradecyl alcohol polyether-20 ether: water: polyol is 1:5:10.

In a preferred embodiment, the polyol is selected from diglycerol, propylene glycol, polyglycerol-3, methylpropanediol, ethanol, butylene glycol, PEG-6, PEG-8, glyceryl polyether-26, dipropylene glycol, 1,2-pentanediol, 1,2-hexanediol or a combination thereof.

In a preferred embodiment, the viscosity of the composition of the present invention is 1000-4000 mPa·s.

On the other hand, the present invention also relates to the use of a composition comprising PEG-240/HDI copolymer bis-decyltetradecyl alcohol polyether-20 ether, water and a polyol in cosmetics. In a preferred embodiment, the cosmetics are selected from: creams, gels, essences, lotions, sprays, facial masks, hair masks, hair sprays or makeup.

BRIEF DESCRIPTION OF THE DRAWINGS

FIG1 is a photograph of samples of Examples 1 to 7, which is taken after the samples are restored to room temperature (25° C.) for 72 hours.

FIG2 is a photograph of samples of Example 8 to Example 15, which is taken after the samples are restored to room temperature (25° C.) for 72 hours.

Figure 3 is a photo of samples of Comparative Examples 1 to 3, which were taken after the samples were restored to room temperature (25°C) for 72 hours and the PET sample bottles were inverted. Comparative Examples 1 and 2 are solid gels that do not flow when inverted; Comparative Example 3 is a fluid soft gel that flows when inverted.

Figure 4 is a photo of samples of Examples 16 to 18, which was taken after the samples were restored to room temperature (25°C) for 72 hours and the PET sample bottles were inverted. Examples 16 and 17 are clear transparent solutions that flow when inverted; Example 18 is a viscoelastic transparent gel that does not flow when inverted.

Figure 5 is a photo of samples of Examples 19 to 24, which were taken after the samples were restored to room temperature (25°C) for 72 hours and the PET sample bottles were inverted. Examples 19 and 22 are clear transparent solutions, Example 23 is a viscoelastic transparent gel that flows when inverted, and Example 24 is a solid gel that does not flow when inverted.

Figure 6 is a photo of samples of Examples 25 to 30, which were taken after the samples were restored to room temperature (25°C) for 72 hours and the PET sample bottles were inverted. Example 25 is a translucent solution, Examples 26 to 28 are clear transparent solutions, and Examples 29 to 30 are fluidized gels.

Figure 7 is a photo of samples of Examples 31 to 36, which were taken after the samples were restored to room temperature (25°C) for 72 hours and the PET sample bottles were inverted. Example 31 is a viscoelastic gel with a fluid state, and Examples 32 to 36 are clear transparent solutions.

Detailed ways

The present invention unexpectedly found that the time, heat energy and electric energy consumed by the process operation of directly adding PEG-240/HDI copolymer bis-decyl tetradecanol polyether-20 ether to the water phase were significantly reduced when PEG-240/HDI copolymer bis-decyl tetradecanol polyether-20 ether was formulated with polyols and water. Therefore, the present invention provides a composition comprising PEG-240/HDI copolymer bis-decyl tetradecanol polyether-20 ether, water and polyols, which has the advantages of simplifying the cosmetic production process, green energy saving and reducing production costs. The composition comprising PEG-240/HDI copolymer bis-decyl tetradecanol polyether-20 ether, water and polyols can be used as an efficacy additive in cosmetics, significantly improving the processing time and energy consumption of conventional production processes.

In addition, the present invention unexpectedly found that the ratio of polyols with different IOB values to water has a significant effect on the rheological properties of the composition, which means that different formulation system requirements can be met, expanding the application field of PEG-240/HDI copolymer bis-decyltetradecyl alcohol polyether-20 ether.

PEG-240/HDI Copolymer Bis-Decyltetradecyl Alcohol Eth-20 Ether

GT-700, the corresponding ingredient name is "PEG-240/HDI copolymer bis-decyltetradecanol polyether-20 ether", which is a water-soluble non-ionic polymer. Its thickening mechanism is that the hydrophobic groups at both ends of the molecular chain attract each other to form petal-shaped micelles, causing the macromolecular chains to produce intramolecular or intermolecular associations. When the concentration of micelles in the aqueous solution exceeds a certain value, a three-dimensional network polymer chain will be formed, so it is also called an associative thickener. The micelle binding ability of PEG-240/HDI copolymer bis-decyltetradecanol polyether-20 ether is weak. Under the action of shear force, it can achieve an association-disassociation balance. The viscosity of the system only decreases slightly. When the external force is removed, the viscosity quickly recovers, and the effect of self-leveling can be achieved.

At present, PEG-240/HDI copolymer bis-decyltetradecyl alcohol polyether-20 ether has been widely used in skin care cosmetics formulas such as creams, gels, essences, sprays, facial masks, hair masks, hair sprays, and makeup.

This application is based on the following unexpected discovery: the combination of GT-700, polyol and water can significantly improve the disadvantages of the conventional production process, which is long processing time and consumes a lot of heat and electricity. Moreover, the use of different ratios of polyol to water also has a significant effect on the rheological properties of the composition containing GT-700, which means that different formulation system requirements can be met, greatly expanding the application field of GT-700.

Polyol

The present invention adopts a liquid polyol with an IOB value of less than 5. Chinese patent application CN201980051731.X discloses the definition of a liquid polyol with an IOB value of less than 5. IOB value refers to the abbreviation of Inorganic/Organic Balance, that is, "IOB value = inorganic value (IV) / organic value (OV)", which is an indicator of the polarity of an organic compound. In short, the larger the IOB value, the greater the polarity and the higher the hydrophilicity. The IOB values of some common polyols are shown in Table 1.

Table 1: Polyols with IOB values below 5

In a preferred embodiment, the selection of polyols includes but is not limited to glycerol, diglycerol, propylene glycol, methyl propanediol, ethanol, butylene glycol, PEG-6, PEG-8, pentanediol, hexanediol, etc. The present invention provides a new green and energy-saving process for producing products containing GT-700.

Compositions with controlled viscosity

The present invention provides a viscosity-controllable composition comprising GT-700, water and polyols. The composition is applied to the field of cosmetics, can simplify the production process operation, and can greatly save the time, electric energy and heat energy required for heat preservation, homogenization and stirring of the water phase in actual production.

In some embodiments, the weight ratio of GT-700 to the sum of water and polyol is 1:2 to 1:30.

In some embodiments, the weight portion of GT-700 is set to 1, and the weight ratio of water to polyol is 1: 1. The applicant has found that as the total weight portion of water and polyol gradually increases, the viscosity of the composition gradually decreases, and it is easier to obtain a clear and transparent solution with good fluidity, which is easy to prepare and transfer in actual production.

In some embodiments, the weight portion of GT-700 is set to 1, and the total weight portion of water and polyol is set to 4.

In some embodiments, the weight ratio of water to polyol is 1:7 to 3:1. In a preferred embodiment, the weight ratio of water to polyol is 1:7 to 1:1. In other embodiments, the weight ratio of water to polyol is 1:1 to 3:1. The applicant has found that the higher the relative proportion of water, the greater the viscosity of the composition. When the weight ratio of water to polyol is 3:1, the composition even forms a gel state. This gel state not only has self-leveling properties, but also exhibits obvious viscoelasticity. This may be because the interaction between hydrogen bonds between polyols and water molecules improves the brittleness of the physical network cross-linked structure formed by GT-700 macromolecules in water. On the contrary, if no polyol is present, the composition only exhibits the self-leveling properties and brittleness of the polymer.

In some embodiments, the weight of GT-700 is set to 1, and the total weight of water and polyol is Serving size: 14.

In some embodiments, the weight ratio of water to polyol is 1:13 to 13:1. In a preferred embodiment, the weight ratio of water to polyol is 1:13 to 1:1. In other embodiments, the weight ratio of water to polyol is 1:1 to 13:1. The applicant found that when the weight ratio of water to polyol is less than 1, the GT-700 macromolecule is mainly based on intramolecular association, the macromolecular chain curls, the fluid dynamics volume decreases, and the intrinsic viscosity decreases. As the relative proportion of water gradually increases, the viscosity of the composition increases. When the weight ratio of water to polyol is greater than 1, the solvent is mainly water, and the GT-700 macromolecular chains aggregate through hydrophobic association to form a supramolecular structure dominated by intermolecular association-a dynamic physical cross-linked network structure, the fluid dynamics volume increases, and the solution viscosity increases significantly. When the weight ratio of water to polyol is 11:3, the composition forms a gel with viscoelasticity. When the weight ratio of water to polyol increases to 13:1, the composition forms a soft gel.

In some embodiments, the weight ratio of water to polyol is 1:13 to 5:9. In a preferred embodiment, the weight ratio of GT-700:water:polyol is 1:1:13 to 1:5:9, so that the viscosity of the composition obtained is close to that of essence and emulsion, and is easy to disperse and transfer in actual production.

In some embodiments, the weight portion of GT-700 is set to 1, and the total weight portion of water and polyol is set to 30.

In some embodiments, the weight ratio of water to polyol is from 1:29 to 29: 1. In preferred embodiments, the weight ratio of water to polyol is from 1:29 to 1: 1. In other embodiments, the weight ratio of water to polyol is from 1: 1 to 29: 1.

By selecting a polyol with an IOB value below 5, a uniformly dispersed GT-700 composition can be obtained. By adjusting the ratio of water to polyol, a GT-700 composition with an ideal viscosity requirement can be obtained to meet the requirements of different formulation systems and expand its application field.

In some embodiments, the weight ratio of GT-700:water:polyol is set to 1:5:10.

In some embodiments, when the weight portion of GT-700 in the composition is 1, the weight ratio of water to the polyol having an IOB value less than 5 is ≤1, and the total weight portion of water to the polyol is within the range of 14-30. By adjusting the weight ratio of water to the polyol, we can obtain a GT-700 composition with an ideal viscosity (1000-4000 mPa·s).

Example

The present invention is further described below in conjunction with specific examples. It is necessary to point out that the examples are only used to further illustrate the present invention and cannot be construed as limiting the scope of the present invention. Those skilled in the art can make some non-essential improvements and adjustments based on the content of the present invention described above. The test methods in the following examples that do not specify specific conditions are usually based on conventional conditions or the conditions recommended by the manufacturer. Unless otherwise specified, all percentages and parts are by weight.

Experimental Materials

PEG-240/HDI copolymer bis-decyltetradecanol polyether-20 ether, purchased from Shanghai Zhaoheng Industrial Co., Ltd.;

1,3-Butanediol, purchased from Jiexitong (Shanghai) Trading Co., Ltd.;

Glycerol was purchased from Wilmar Oil & Fats Technology Co., Ltd.;

1,3-Propanediol, purchased from Cosfa International Trading (Shanghai) Co., Ltd.;

PEG-8, purchased from Shanghai Youwen Chemical Co., Ltd.;

1,2-Pentanediol, purchased from Shanghai Yuanshang Science and Trade Co., Ltd.;

1,2-Hexanediol was purchased from Shanghai Yuanshang Science and Trade Co., Ltd.;

Deionized water, homemade in the laboratory.

laboratory apparatus

Weighing balance: METTLER TOLEDO PB4002-N

Viscosity Tester: Brookfield RVDV-C

Mixer: IKA RW20 D S25 (72W, 220-240V)

Homogenizing emulsifier: Mizhiga VTU-1-1000

Embodiment 1-7:

Weigh GT-700, water, and 1,3-butanediol according to the weight parts shown in Table 2, add them into a 250ml beaker, place it in a constant temperature water bath at 70-80℃, disperse it evenly at 600-700rpm for 6-10min, observe and record the appearance of the material; then stop stirring, cool to room temperature for use, observe and record the appearance of the material again, and photograph the sample.

Embodiment 8-15:

Weigh GT-700, water and 1,3-butanediol according to the weight parts shown in Table 2, add them into a 250ml beaker, place it in a constant temperature water bath at 70-80℃, disperse it evenly under the conditions of 500-600r/min, 3-6min, observe and record the appearance of the material; then stop stirring, cool to room temperature for use, observe and record the appearance of the material again, and take pictures of the samples.

Table 2: Properties of GT-700-water-1,3-butanediol at different weight ratios

Table 2: Properties of GT-700-water-1,3-butanediol at different weight ratios (continued)

As shown in Table 2, in this series of experiments, according to the actual production of GT-700, water and 1,3-butanediol as a single-phase composition, the weight of GT-700 was set to 1, and the weight ratio of water to 1,3-butanediol was set to 1:1.

The experiment found that as the total weight of water and 1,3-butanediol gradually increased, the viscosity, stirring speed and time of the examples all changed. As shown in Table 2, when Example 1-Example 7 was stirred and dispersed, 600-700rpm and 6-10min were required to disperse evenly. The composition had a high viscosity and was accompanied by a large number of bubbles. After cooling to room temperature, it was a clear and transparent solution with a high viscosity. When Example 8-Example 15 was stirred and dispersed, it was possible to disperse evenly by stirring at a low speed for 3-6min. After cooling to room temperature, it was a clear and transparent solution with good fluidity, which was easy to prepare and transfer in actual production. Figure 1-2 is a sample photo of Example 1-Example 15. As can be seen from the figure, after the sample returned to room temperature (25°C) for 72h, Example 1-Example 15 were all clear and transparent solutions in the PET bottle.

Test Example 1: Viscosity Test

After the sample returns to room temperature (25°C) for 72 hours, weigh 150 g of the composition of Example 1 to Example 15, and use a viscosity tester (model: Brookfield RVDV-C) to measure the viscosity of the composition. The test conditions are: select a suitable rotor (S03, S04, S91, S92, S93, S95), the speed range is 10-50rpm, the test time is 60s, and the torque is controlled in the range of 30%-80%.

Table 3: Viscosity of samples from Examples 1 to 15

As shown in Table 3, as the amount of water and 1,3-butanediol gradually increased in Examples 1 to 15, the viscosity gradually decreased. The viscosity of Examples 9 to 15 was similar to that of emulsions and essences, and the fluidity was good. This is because the relative concentration of GT-700 gradually decreased, the GT-700 macromolecules were mainly intramolecularly associated, the macromolecular chains curled, the fluid dynamics volume decreased, and the characteristic viscosity decreased. The above results show that GT-700 can be quickly dispersed by a composition composed of different proportions of GT-700-water-1,3-butanediol, and a composition with good fluidity can be obtained when the concentration of GT-700 is low.

Comparative Examples 1-3

Weigh an appropriate amount of GT-700 and water as shown in Table 4, add them into a 250ml beaker, place in a constant temperature water bath at 70-80°C, disperse evenly at 550-700rpm for 6-10min, observe and record the appearance of the material; then stop stirring, cool to room temperature for use, observe and record the appearance of the material again, and photograph the sample.

Table 4: Properties of GT-700-water at different weight ratios

From Table 4, we found that Comparative Example 1 (the weight ratio of GT-700 to water is 1:4) is a hard solid gel when cooled to room temperature. As the amount of water increases, Comparative Example 3 (the weight ratio of GT-700 to water is 1:30) cooled to room temperature to form a soft gel with a broken texture. Combined with Figure 3, we can see that Comparative Examples 1 and 2 are solid gels that do not flow when inverted; Comparative Example 3 is a fluid soft gel that flows when inverted. In the comparative examples, as the concentration of GT-700 decreases, the transparency of the gel increases. The opacity of the gel in Comparative Example 1 is relatively high. This is because the concentration of GT-700 reaches 20% at this time, and the GT-700 polymer chains in the formed three-dimensional network structure are mainly intramolecular and intermolecular association. The concentration of petal-shaped micelles formed by association is relatively high, and the fluid dynamics volume is increased, showing an opaque appearance of the gel through light scattering. As the concentration of GT-700 decreases, the viscosity of the composition system gradually decreases, and the transparency of the gel increases.

Embodiment 16-18:

Weigh appropriate amounts of GT-700, water, and 1,3-butanediol according to the weight ratio shown in Table 5, add them into a 250ml beaker, place in a constant temperature water bath at 70-80°C, disperse evenly at 500-600r/min, 3-6min, observe and record the appearance of the material; then stop stirring, cool to room temperature for use, observe and record the appearance of the material again, and photograph the sample.

Table 5: GT-700-water-1,3-butanediol at different weight ratios

In Table 5, Example 16 to Example 18, the total weight of water and 1,3-butanediol was set to 4 parts by weight, and the relative ratio of water to 1,3-butanediol was changed. Combined with Figure 4, we can see that the compositions of Example 16 and Example 17 are clear and transparent solutions when finally cooled to room temperature, and flow when inverted; Example 18 is a transparent gel with a certain viscoelasticity, and does not flow when inverted.

Test Example 2: Viscosity Test

After the sample has returned to room temperature (25°C) for 72 hours, 150 g of the composition of Example 16-Example 18 is weighed, and the viscosity of the composition is measured using a viscosity tester (model: Brookfield RVDV-C). The test conditions are: select rotor S04, speed range 12-20 rpm, test time 60 s, and torque control within the range of 30%-80%.

Table 6: Viscosity of samples in Examples 16-18

Through the viscosity test of Example 16-Example 18 in Table 6, we found that the weight ratio of water to 1,3-butanediol has a significant effect on the properties of the composition. The higher the relative proportion of water, the greater the viscosity of the composition. It is particularly noteworthy that the viscosity of Example 2 (124000mPa·s) is 14.2 times that of Example 17 (viscosity 8730mPa·s); when the weight ratio of water to 1,3-butanediol in Example 18 is 3:1, a gel state is formed. We found that Example 18 not only has the characteristics of self-leveling but also exhibits obvious viscoelasticity. This may be because the interaction between hydrogen bonds between 1,3-butanediol and water molecules improves the brittleness of the physical network cross-linked structure formed by GT-700 macromolecules in water, so Example 18 exhibits certain viscoelasticity and self-leveling properties. Since Comparative Example 1 does not contain 1,3-butanediol, it only exhibits the self-leveling properties and brittleness of the polymer. The above experimental results show that the rheological properties of the composition can be significantly improved by changing the weight ratio of water to 1,3-butanediol.

Embodiment 19-22:

Weigh appropriate amounts of GT-700, water, and 1,3-butanediol according to the weight ratio shown in Table 7, add them into a 250ml beaker, place in a constant temperature water bath at 70-80°C, disperse evenly at 500-600r/min, 3-6min, observe and record the appearance of the material; then stop stirring, cool to room temperature for use, observe and record the appearance of the material again, and photograph the sample.

Embodiment 23-24:

According to the weight ratio shown in Table 7, weigh appropriate amounts of GT-700, water, and 1,3-butanediol, add 250 ml Put the mixture into a beaker of a certain specification, place it in a constant temperature water bath at 70-80℃, disperse it evenly at 650-700r/min, 6-10min, observe and record the appearance of the material; then stop stirring, cool it to room temperature for use, observe and record the appearance of the material again, and take pictures of the samples.

Table 7: Properties of GT-700-water-1,3-butanediol at different weight ratios

In Table 7, Example 19 to Example 24, the total mass of water and 1,3-butanediol was set to 14 parts by weight, and the relative proportion of water and 1,3-butanediol was changed. Combined with the sample photos in Figure 5, Example 19 to Example 22 were finally cooled to room temperature to be clear and transparent solutions, Example 23 was a transparent gel with a certain viscoelasticity, and both flowed when inverted; Example 24 was a solid gel that did not flow when inverted.

Test Example 3: Viscosity Test

After the sample returns to room temperature (25°C) for 72 hours, weigh 150 g of the composition of Example 19 to Example 24, and use a viscosity tester (model: Brookfield RVDV-C) to measure the viscosity of the composition. The test conditions are: select a suitable rotor (S02, S03, S95), the speed range is 12-30rpm, the test time is 60s, and the torque is controlled in the range of 30%-80%.

Table 8: Viscosity of samples in Examples 19-24

Through the viscosity test in Table 8, we found that when the weight ratio of water:1,3-butanediol is less than 1, the viscosity of Example 19 is 441 mPa·s, the viscosity of Example 20 is 649 mPa·s, and the viscosity of Example 21 is 1367 mPa·s. When the weight ratio of water:1,3-butanediol is 1, the viscosity of Example 7 is 6880 mPa·s. When the weight ratio of water:1,3-butanediol is greater than 1, the viscosity of Example 22 is 76300 mPa·s. Example 23 (water:1,3-butanediol weight ratio=11:3) is a gel with certain viscoelasticity, and Example 24 is a soft gel that is easily broken.

Combined with Example 16 to Example 22, we can find that when the weight ratio of water: 1,3-butanediol is less than 1, the solvent is mainly 1,3-butanediol, the proportion of water is less, and the GT-700 macromolecule is mainly based on intramolecular association, which will cause the macromolecular chain to curl, the fluid dynamics volume to decrease, and the intrinsic viscosity to decrease; as the relative proportion of water gradually increases, the viscosity of the composition increases. When the weight ratio of water: 1,3-butanediol is greater than 1, the solvent is mainly water, and the GT-700 macromolecular chain aggregates through hydrophobic association to form a supramolecular structure dominated by intermolecular association-a dynamic physical cross-linked network structure, the fluid dynamics volume increases, and the solution viscosity increases significantly. The above experimental results show that the viscosities of Example 19 to Example 21 (GT-700-water-1,3-butanediol weight ratio from 1:1:13 to 1:5:9) are relatively close to the viscosity of essences and emulsions, and are easy to disperse and transfer in actual production, meeting our needs.

Embodiment 25-30:

Weigh appropriate amounts of GT-700, water, and 1,3-butanediol according to the weight ratio shown in Table 9, add them into a 250ml beaker, place in a constant temperature water bath at 70-80°C, disperse evenly at 500-600r/min, 3-6min, observe and record the appearance of the material; then stop stirring, cool to room temperature for use, observe and record the appearance of the material again, and photograph the sample.

Table 9: Properties of GT-700-water-1,3-butanediol at different weight ratios

In Table 9, the total mass of water and 1,3-butanediol is set to 30 parts by weight, and the relative proportion of water and 1,3-butanediol is changed. Combined with the sample photos of Examples 25 and 30 in Figure 6, Example 25 is finally cooled to room temperature to be a translucent solution, Examples 26 to 28 are clear and transparent solutions, and Examples 29 and 30 are gels with certain fluidity and viscoelasticity.

Test Example 4: Viscosity Test

After the sample returns to room temperature (25°C) for 72 hours, weigh 150 g of the composition of Example 25-Example 30, and use a viscosity tester (model: Brookfield RVDV-C) to measure the viscosity of the composition. The test conditions are: select a suitable rotor (S02, S94), the speed range is 12-50rpm, the test time is 60s, and the torque is controlled in the range of 30%-80%.

Table 10: Viscosity of samples in Examples 25-30

From the viscosity test in Table 10, we found that when the weight ratio of water to 1,3-butanediol is less than 1, the viscosity changes of Examples 25 to 27 are small; when the weight ratio of water to 1,3-butanediol is 1, the viscosity changes of Examples 15 to 27 are small. The viscosity is 1120 mPa·s. When the weight ratio of water to 1,3-butanediol is greater than 1, the viscosity of Example 28 is 15400 mPa·s, and Examples 29 and 30 are gel structures, and the viscosity is also significantly increased.

This may be because, when the mass percentage of water in the solvent of Example 25-Example 27 is 3.2%-32.2%, the GT-700 macromolecular chain is curled in the solvent, so the viscosity of the composition is relatively low. Example 25 presents a translucent appearance. At this time, the solvent is mainly 1,3-butanediol, the degree of polymer association is low, and the macromolecular chain is curled and dispersed in the solvent, which may affect the processing technology of the composition dispersed in the water phase. The viscosity is significantly increased when the weight ratio of water to 1,3-butanediol is 1; as the relative proportion of water gradually increases, the final composition forms a gel structure. Compared with Comparative Example 3, Examples 29 and 30 still retain some viscoelasticity due to the hydrogen bonding between 1,3-butanediol and water in the composition. However, due to the high percentage of water in Example 30 (93.5% water), it also exhibits obvious brittle characteristics.

Examples 31-36:

According to the weight ratio shown in Table 11, appropriate amounts of GT700, water, glycerol, propylene glycol, butylene glycol, PEG-8, pentanediol and hexylene glycol were weighed, added into a 250 ml beaker, placed in a constant temperature water bath at 70-80 ° C, dispersed evenly under the conditions of 500-600r/min, 3-6min, and observed and recorded the appearance of the material; then stopped stirring, cooled to room temperature for use, observed and recorded the appearance of the material again, and photographed the sample.

Table 11: Properties of GT-700-water-1,3-polyol at different weight ratios

In Table 11, Example 31 to Example 36, the weight ratio of GT-700: water: polyol was set to 1: 5: 10, and the dispersibility of GT-700 in different polyol systems was investigated. FIG7 is a sample photo of Example 31 to Example 36. Example 31 was finally cooled to room temperature to be a viscoelastic gel with a fluid state, and Example 32 to Example 36 were clear transparent solutions.

Test Example 5: Viscosity Test

After the sample returned to room temperature (25°C) for 72 hours, 150 g of the composition of Example 31 to Example 36 was weighed, and the viscosity of the composition was measured using a viscosity tester (model: Brookfield RVDV-C). The test conditions were: select a suitable rotor (S91, S95, S02), speed range 12-50 rpm, test time 60 s, and torque control within the range of 30%-80%.

Table 12: Viscosity of samples in Examples 30-36

From the viscosity test in Table 12, we found that the viscosity of the compositions of different polyols varies greatly. According to Table 1, we can see that the IOB values of glycerol, propylene glycol, butylene glycol, PEG-8, pentanediol, and hexanediol gradually decrease, and the viscosity of the corresponding compositions also gradually decreases. In particular, we found that the viscosity of Example 34 (GT-700: water: PEG-8) is 6900 mPa·s, which is significantly higher than that of Example 33 (GT-700: water: 1,3-butanediol). From Table 1, we know that the IOB value of 1,3-butanediol is 2.5, and the IOB value of PEG-8 is 2.27. The difference in the IOB values of the two is not large, but the viscosity of the composition is significantly different. This is because the molecular chain of PEG-8 is longer, the entanglement between the molecular chains, and the steric hindrance effect caused by the hydrogen bonds formed with water molecules are conducive to the formation of a denser three-dimensional The network structure, therefore, the viscosity of the composition is also significantly higher than that of Example 33. Therefore, we conclude that a uniformly dispersed GT-700 composition can be obtained by selecting a polyol with an IOB value lower than 5. Based on the previous experimental results, we can also infer that a GT-700 composition with an ideal viscosity requirement can be obtained by adjusting the ratio of water to polyol, thereby meeting the requirements of different formulation systems and expanding its application field.

Based on the above results, we can conclude that when the weight portion of GT-700 in the composition is 1, the weight ratio of water to polyol with an IOB value lower than 5 is ≤1, and the total weight portion of water to polyol is within the range of 14-30. By adjusting the weight ratio of water to polyol, we can obtain a GT-700 composition with an ideal viscosity (1000-4000 mPa·s).

Notes on energy consumption

Based on the GT-700 composition proposed in the present invention, the energy consumption level of its production process is further evaluated. Taking the actual production of 800L of jelly essence as an example, a conventional production process is adopted, 1% GT-700 is placed in the water phase, put into the emulsifying pot and heated to 80℃-85℃, stirred evenly, turned on 2000rpm for homogenization for 5min, and kept warm and stirred for 20-30min. Among them, the rated power of the homogenization motor of the emulsifying pot is 11kW, and the rated power of the stirring motor is 5.5kW. After calculation, the power consumption for homogenization is: 0.9167kW·h; the power consumption for stirring is: 1.83kW·h-2.75kW·h. In addition, the heat energy required for the water phase is: 2.016×10 ⁸ J (Q _heat = c _water mΔt). Compared with the improved process proposed in the present invention, the GT-700-water-polyol composition is added to the emulsifying pot at 40-45°C after emulsification, and stirred for 3-6 minutes to disperse evenly. The power consumption is calculated to be: 0.275kW·h-0.55kW·h, which saves about 85% of energy consumption compared with the conventional production process. We can conclude that the GT-700-water-polyol composition simplifies the production process operation, and can greatly save the time, electricity and heat energy required for the insulation, homogenization and stirring of the water phase in actual production.

Application example 1-6: Application in gel essence system

Table 13: Raw material feed ratios in various application examples

Table 13 shows the compositions of Example 21, Example 24, Example 15, Example 27, Example 31, and Example 33. Add the raw materials of phase A to a 1000mL glass beaker in the amounts shown in Table 13, and stir at room temperature until they are completely dissolved into a clear and transparent solution. Add the raw materials of phase B to phase A (add for 1 min), and continue stirring at a speed of 500 rpm until the material is uniform and clear. Continue to add phase C in sequence and stir for 2-3 minutes until it is clear and transparent. Seal the beaker with plastic wrap and use it to obtain the sample to be tested. A gel essence with self-recovery properties can be obtained through a cold processing technology. The skin feels moisturizing, light and non-greasy. The formula preparation process is simple and can be completed by stirring and dispersing.

Application example 7-12: Application in gel emulsion system

Table 14: Raw material feed ratios in various application examples

Table 14 shows the compositions of Example 21, Example 24, Example 15, Example 27, Example 31, and Example 33. The raw materials of phase A were added to 1000 mL of the mixture in the amounts shown in Table 14. In a glass beaker, stir at 80℃-85℃ until completely dissolved into a clear and transparent solution. Add the raw materials of phase B to a 500ml glass beaker in sequence and heat at 80℃-85℃ to dissolve. Add phase B to phase A and emulsify at 80℃-85℃, 3000rpm for 5-6min. Add phase C and phase D in sequence at 40-45℃ and stir for 3-6min to disperse evenly. After the material is cooled to room temperature, seal the beaker with plastic wrap for standby use to obtain the sample to be tested. The above simple preparation process can produce a gel emulsion with self-recovering properties, which feels moisturizing and nourishing on the skin. The GT-700 composition is added at 40℃-45℃ after emulsification, which can save the time, heat energy and electricity consumed by heating and homogenizing GT-700 in phase A in the conventional method. It is an energy-saving and green sustainable production processing method.

Claims

A composition comprising PEG-240/HDI copolymer bis-decyltetradecyl alcohol polyether-20 ether, water and a polyol,

wherein the inorganic-organic balance (IOB) value of the polyol is less than 5;

wherein the weight ratio of PEG-240/HDI copolymer bis-decyltetradecyl alcohol polyether-20 ether to the sum of water and polyol is 1:2 to 1:30;

Wherein, the weight ratio of water to polyol is 1:29 to 29:1.
The composition of claim 1, wherein the weight ratio of PEG-240/HDI copolymer bis-decyltetradecyl alcohol polyether-20 ether to the sum of water and polyol is 1:14 to 1:30, and the weight ratio of water to polyol is ≤1.
The composition of claim 1, wherein the weight ratio of water to polyol is 1:1 to 29:1.
The composition of claim 1, wherein the weight ratio of PEG-240/HDI copolymer bis-decyltetradecyl alcohol polyether-20 ether: water: polyol is 1:1:13 to 1:5:9.
The composition of claim 1, wherein the weight ratio of PEG-240/HDI copolymer bis-decyltetradecyl alcohol polyether-20 ether: water: polyol is 1:5:10.
The composition of claim 1, wherein the polyol is selected from diglycerol, propylene glycol, polyglycerol-3, methyl propanediol, ethanol, butylene glycol, PEG-6, PEG-8, glyceryl polyether-26, dipropylene glycol, 1,2-pentanediol, 1,2-hexanediol or a combination thereof.
The composition according to claim 1, wherein the viscosity of the composition is 1000-4000 mPa·s.
Use of the composition according to any one of claims 1 to 7 in cosmetics.
The use according to claim 8, wherein the cosmetic is selected from the group consisting of: cream, gel, essence, lotion, spray, facial mask, hair mask, hair spray or makeup.
The use according to claim 8, wherein the use reduces the time, heat energy and electrical energy consumed in heating and homogenizing the PEG-240/HDI copolymer bis-decyltetradecyl polyether-20 ether.