A modified solubilizer and alcohol-free perfume

Abstract

The present invention belongs to the technical field of functional polymers and cosmetics, and discloses a modified solubilizer and an alcohol-free perfume. The preparation method of the modified solubilizer comprises the following steps: adding cyclodextrin to an ethanol aqueous solution and stirring and dispersing it uniformly, then adding an alkaline solution for alkalization reaction, then dripping an alkyl epoxy polyether for substitution reaction, filtering the reaction mixture, washing and drying the filter cake, and obtaining a modified solubilizer. The alcohol-free perfume comprises the following components by weight percentage: 10-20% flavor, 1-10% modified solubilizer, 0.5-2% moisturizer, 0-0.2% thickener, 0.01-0.05% antioxidant, 0.01-0.05% chelating agent, 0.5-1% preservative, and the remainder is deionized water. The flavor in the alcohol-free perfume of the present invention: solubilizer ≥ 1, does not contain alcohol solvent, and has good product stability and lasting fragrance.

Description

Technical Field

[0001] The invention belongs to the technical field of functional polymers and cosmetics, and particularly relates to a modified solubilizer and an alcohol-free perfume. Background Art

[0002] In the perfume industry, alcohol has long been used as a solvent. Alcohol perfumes are flammable liquids because of their flammability. Therefore, they are classified as "Class 3 dangerous goods" during use and transportation, and have high safety risks and costs for transportation and storage. In addition, alcohol-containing cosmetics are in urgent need of finding a solvent to replace alcohol due to problems such as skin sensitivity and infant safety. In addition, alcohol-containing perfumes evaporate quickly, and the fragrance lasts for a relatively short time. In addition, alcohol will affect the original fragrance, and too much alcohol will produce a pungent alcohol smell, which will bring a bad experience to users.

[0003] Therefore, the perfume industry tries to develop alcohol-free perfume to meet the needs of users. At present, alcohol-free water-based perfume faces the problem of solubilizing efficiency of solubilizer (fragrance: solubilizer ≤ 1 / 3). If the perfume is to be transparent, the amount of fragrance added cannot be too high. If the amount is too high, the solubilizer is usually present in high doses, and the viscosity seriously affects the feeling of use. If the amount of fragrance added is too low, the perfume loses its meaning.

[0004] Cyclodextrin molecules have a slightly conical hollow cylindrical three-dimensional ring structure. Its hydrophobic inner cavity and hydrophilic outer properties enable it to form inclusion compounds and molecular assembly systems with many organic and inorganic molecules based on van der Waals forces, hydrophobic interactions, and matching effects between host and guest molecules, thus having a solubilizing effect. However, due to the hydrogen bonding and intermolecular effects of the high content of hydroxyl groups in cyclodextrin molecules, its viscosity-increasing effect in aqueous solutions is significant, making it difficult to be used in low-viscosity perfume formulas. Summary of the invention

[0005] In view of the shortcomings and deficiencies of the above prior art, the primary purpose of the present invention is to provide a method for preparing a modified solubilizing agent.

[0006] Another object of the present invention is to provide a modified solubilizing agent prepared by the above method.

[0007] Another object of the present invention is to provide an alcohol-free perfume containing the modified solubilizer.

[0008] Another object of the present invention is to provide a method for preparing the alcohol-free perfume.

[0009] The purpose of the present invention is achieved through the following technical solutions:

[0010] A method for preparing a modified solubilizing agent comprises the following preparation steps:

[0011] Cyclodextrin is added to an ethanol aqueous solution and stirred to disperse uniformly, then an alkaline solution is added to carry out an alkalization reaction, and then an alkyl epoxy polyether is added dropwise to carry out a substitution reaction, the reaction mixture is filtered, and the filter cake is washed and dried to obtain a modified solubilizer.

[0012] Preferably, the cyclodextrin is α-cyclodextrin, β-cyclodextrin or γ-cyclodextrin commonly used in the art; β-cyclodextrin is more preferred, as it has the advantages of good solubilization effect and low cost.

[0013] Preferably, the ethanol aqueous solution uses an ethanol aqueous solution with an ethanol volume content greater than 70%. The ethanol ratio ensures that the cyclodextrin will not be fully dissolved, so as to facilitate the subsequent filtration separation and washing of the product. The solid phase reaction can effectively reduce the viscosity of the system, the reaction efficiency and production efficiency are high, and the product is easy to purify with less impurity residues.

[0014] Preferably, the alkaline solution is a sodium hydroxide solution or a potassium hydroxide solution.

[0015] Preferably, the alkalization reaction is carried out at a temperature of 20-80°C and for a time of 10-60 minutes.

[0016] Preferably, the molecular formula of the alkyl epoxy polyether is C n H 2n+1 O(CH 2 CH(CH 3 )O) a (CH 2 CH 2 O) b CH 2 (CHCH 2 )O, with an average molecular weight of 300-1500. It is a conventional raw material in this field.

[0017] Preferably, the added amount of the alkyl epoxy polyether is 10-60% of the mass of cyclodextrin.

[0018] Preferably, the temperature of the substitution reaction is 20-80° C. and the time is 1-6 h.

[0019] A modified solubilizing agent is prepared by the method.

[0020] An alcohol-free perfume containing the modified solubilizer, comprising the following components by weight percentage:

[0021] Fragrance 10-20%, modified solubilizer 1-10%, humectant 0.5-2%, thickener 0-0.2%, antioxidant 0.01-0.05%, chelating agent 0.01-0.05%, preservative 0.5-1%, and the balance is deionized water.

[0022] Preferably, the moisturizing agent is one or more of methylpropanediol, propylene glycol, butylene glycol and glycerin.

[0023] Preferably, the thickener is polyacrylate cross-linked polymer-6. This raw material is a self-thickening carbomer, does not need to be neutralized, and is electrolyte-resistant. In addition, since the modified solubilizer of the present application has solubilizing, stabilizing and thickening effects at the same time, in order to keep the perfume low in viscosity, the formula of the present application does not need to add an additional thickener.

[0024] Preferably, the antioxidant is one or more of BHT and tocopherol (vitamin E).

[0025] Preferably, the chelating agent is disodium EDTA.

[0026] Preferably, the preservative is one or more of Naturcare HL-09 (Shanghai Baijie Chemical Co., Ltd.) and LKCare BHC (LK Chemicals Co., Ltd).

[0027] Because the formulation system of the present invention is an aqueous formulation, some anti-inflammatory, anti-allergic and other conditioning components can be added according to actual conditions.

[0028] The preparation method of the above-mentioned alcohol-free perfume comprises the following preparation steps:

[0029] Step (1): Add the moisturizer, thickener, chelating agent and part of the deionized water into the manufacturing pot, and stir homogenously until all the components are fully mixed;

[0030] Step (2): Add the modified solubilizer to the remaining deionized water in a clean container to dissolve it, then add the flavor and antioxidant and mix and stir until completely dissolved, then add to the manufacturing pot of step (1) and stir evenly;

[0031] Step (3): Add preservatives to the pot prepared in step (2), stir evenly, and filter to obtain alcohol-free perfume.

[0032] Compared with the prior art, the present invention has the following beneficial effects:

[0033] (1) The ratio of flavor to solubilizer in the alcohol-free perfume of the present invention is ≥ 1, which solves the solubilization efficiency problem of the solubilizer in the current alcohol-free water-based transparent perfume (flavor to solubilizer ≤ 1 / 3), and the product has good stability and lasting fragrance.

[0034] (2) In order to ensure clarity and impurity-free during the production process, traditional alcohol perfumes need to be aged for 10 days and frozen at sub-zero temperatures to remove insoluble impurities. The modified solubilizer of the present invention has better compatibility with the essence and has a milky white texture. The above two steps can be omitted, greatly saving the production cycle and energy consumption. BRIEF DESCRIPTION OF THE DRAWINGS

[0035] Figure 1 This is a diagram showing the appearance of the alcohol-free perfume obtained in Example 2 of the present invention. DETAILED DESCRIPTION

[0036] The present invention is further described in detail below in conjunction with embodiments and drawings, but the embodiments of the present invention are not limited thereto.

[0037] Example 1

[0038] A method for preparing a modified solubilizing agent comprises the following preparation steps:

[0039] β-cyclodextrin was added to 85vt.% ethanol aqueous solution and stirred to disperse evenly, and then heated to 60°C, and then sodium hydroxide aqueous solution was added to adjust the pH value of the system to 12 for alkalization reaction for 30 minutes, and then alkyl epoxy polyether (average molecular weight of 1000, Wuhan Maikairui Chemical Co., Ltd.) with a mass of 25% of cyclodextrin was added dropwise for substitution reaction for 3 hours. After the reaction was completed, the temperature was lowered to room temperature, the reaction mixture was filtered, the filter cake was washed with ethanol, and vacuum rotary dried at 80°C to obtain a modified solubilizer. The average degree of substitution DS of the product was determined to be 4.95.

[0040] Example 2

[0041] An alcohol-free perfume comprising the following components by weight percentage:

[0042] Fragrance 15%;

[0043] 5% of the modified solubilizing agent of Example 1;

[0044] Moisturizer: Methylpropanediol 1%;

[0045] Thickener Polyacrylate Crosspolymer-6 0.05%;

[0046] Antioxidant tocopherol 0.05%;

[0047] Chelating agent: disodium EDTA 0.05%;

[0048] Preservative Naturcare HL-09 0.8%;

[0049] The balance was deionized water.

[0050] The preparation method of the above-mentioned alcohol-free perfume comprises the following preparation steps:

[0051] (1) Take the raw material components according to the above weight percentages, add the moisturizing agent methylpropanediol, the thickening agent polyacrylate cross-linked polymer-6, the chelating agent EDTA disodium, and 60% of the total amount of deionized water into the manufacturing pot, and stir homogenously for more than 5 minutes until the components are fully mixed.

[0052] (2) Use a clean container to add the modified solubilizer to the remaining 40% deionized water to dissolve, then add the flavor and antioxidant tocopherol and mix until completely dissolved. Then add to the manufacturing pot of step (1) and stir evenly.

[0053] (3) Add the preservative Naturcare HL-09 to the production pot in step (2), stir for 5 minutes to mix evenly, and filter to obtain the alcohol-free perfume.

[0054] The appearance of the alcohol-free perfume obtained in this embodiment is shown in the figure Figure 1 It can be seen that the alcohol-free perfume obtained by the present invention is a uniform milky white stable system.

[0055] Example 3

[0056] An alcohol-free perfume comprising the following components by weight percentage:

[0057] Fragrance 15%;

[0058] 2% of the modified solubilizing agent of Example 1;

[0059] Humectant: propylene glycol 1%;

[0060] Thickener Polyacrylate Crosspolymer-6 0.10%;

[0061] Antioxidant tocopherol 0.05%;

[0062] Chelating agent: disodium EDTA 0.05%;

[0063] Preservative Naturcare HL-09 0.8%;

[0064] The balance was deionized water.

[0065] The preparation method of the above-mentioned alcohol-free perfume is the same as that of Example 1.

[0066] Example 4

[0067] An alcohol-free perfume comprising the following components by weight percentage:

[0068] Fragrance 15%;

[0069] The modified solubilizer of Example 1 7.5%;

[0070] Moisturizer Butylene Glycol 1%;

[0071] Antioxidant tocopherol 0.05%;

[0072] Chelating agent: disodium EDTA 0.05%;

[0073] Preservative Naturcare HL-09 0.8%;

[0074] The balance was deionized water.

[0075] The preparation method of the above-mentioned alcohol-free perfume is the same as that of Example 1.

[0076] Comparative Example 1

[0077] Use an ordinary alcohol-containing perfume containing the same fragrance and the same fragrance addition amount (15%).

[0078] Using the common alcohol-containing perfume of Comparative Example 1 and the alcohol-free perfumes of Examples 2-4 of the present invention, under the same environment, the fragrance was manually scored with fragrance test papers at 0h, 4h, 8h, and 12h (0-5 points, 5 points for full smell, 0 points for no smell), and the relationship between fragrance concentration score and time as shown in Table 1 below was obtained.

[0079] Table 1 Relationship between aroma concentration score and time

[0080]

[0081] Referring to the relationship table between the fragrance concentration score and time in Table 1, it can be seen that the fragrance of the alcohol-free perfume of the present invention is retained longer than that of the alcohol-containing perfume of the same proportion, mainly because the solvent water evaporates relatively slowly relative to the alcohol, so the fragrance is retained longer; wherein the fragrance retention effect of the alcohol-free perfumes in Examples 2 to 4 is equivalent, mainly because the proportion of raw materials such as solubilizers has little effect on the fragrance; wherein the alcohol-containing perfume in Comparative Example 1 has a worse fragrance retention effect than that of the alcohol-free perfumes in Examples 2 to 4 when first smelled, mainly because the volatilization of the solvent alcohol interferes with the original fragrance.

[0082] Comparative Example 2

[0083] An alcohol-free perfume, compared with Example 2, uses an equal amount of unmodified β-cyclodextrin to replace the modified solubilizer, and the rest is the same.

[0084] The alcohol-free perfumes of Comparative Example 2 and Examples 2-4 of the present invention were used to test the spray performance (using a conventional perfume spray nozzle) and the cold and hot cycle stability test (stored in a -10°C thermostat for 12 hours, taken out and stored at room temperature for 12 hours, then placed in a 45°C thermostat for 12 hours, and the emulsion stratification was observed after 15 cycles). The results shown in Table 2 are as follows.

[0085] Table 2 Spray performance and hot and cold cycle stability test results

[0086] Test sample / performance Spray performance Thermal cycle stability Comparative Example 2 Difficult to atomize Obvious stratification Example 2 Good atomization No stratification Example 3 Good atomization No stratification Example 4 Good atomization No stratification

[0087] Referring to the results in Table 2, it can be seen that the present invention uses alkyl epoxy polyether to modify cyclodextrin, which can significantly reduce its viscosity-increasing properties and enhance its solubilizing properties in the alcohol-free perfume formula of the present invention.

[0088] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be equivalent replacement methods and are included in the protection scope of the present invention.

Claims

1. An alcohol-free perfume, characterized in that: The composition comprises the following components by weight percentage: Fragrance 10-20%, modified solubilizer 1-10%, humectant 0.5-2%, thickener 0-0.2%, antioxidant 0.01-0.05%, chelating agent 0.01-0.05%, preservative 0.5-1%, the balance is deionized water; The modified solubilizing agent is prepared by the following method: Add β-cyclodextrin to an ethanol aqueous solution and stir to disperse it uniformly, then add an alkaline solution to carry out an alkalization reaction, then drop an alkyl epoxy polyether to carry out a substitution reaction, filter the reaction mixture, take the filter cake, wash it, and dry it to obtain a modified solubilizer; The molecular formula of the alkyl epoxy polyether is C n H 2n+1 O(CH2CH(CH3)O) a (CH2CH2O) b CH2(CHCH2)O, the average molecular weight is 300-1500; the addition amount of the alkyl epoxy polyether is 10-60% of the mass of cyclodextrin.

2. An alcohol-free perfume according to claim 1, characterized in that: The ethanol aqueous solution adopts an ethanol aqueous solution with an ethanol volume content greater than 70%.

3. The alcohol-free perfume according to claim 1, characterized in that: The alkaline solution is a sodium hydroxide solution or a potassium hydroxide solution; the temperature of the alkalization reaction is 20-80° C. and the time is 10-60 minutes.

4. The alcohol-free perfume according to claim 1, characterized in that: The temperature of the substitution reaction is 20-80° C. and the time is 1-6 hours.

5. The alcohol-free perfume according to claim 1, characterized in that The moisturizer is one or more of methyl propanediol, propylene glycol, butylene glycol, and glycerin; the thickener is polyacrylate cross-linked polymer-6; the antioxidant is one or more of BHT and tocopherol; and the chelating agent is disodium EDTA.

6. The method for preparing an alcohol-free perfume according to any one of claims 1 to 5, characterized in that: The method comprises the following preparation steps: (1) Add the moisturizer, thickener, chelating agent and part of the deionized water into the manufacturing pot and stir homogenously until all the components are fully mixed; (2) Add the modified solubilizer to the remaining deionized water in a clean container and dissolve it. Then add the flavor and antioxidant and mix and stir until they are completely dissolved. Then add them to the manufacturing pot in step (1) and stir evenly. (3) Add preservatives to the pot prepared in step (2), stir evenly, and filter to obtain the alcohol-free perfume.

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