Essence microcapsule as well as preparation method and application thereof

Abstract

The invention discloses an essence microcapsule and a preparation method and application thereof, the essence microcapsule comprises the following raw materials by weight: 15-45 parts of essence, 3-15 parts of isocyanate, 3-15 parts of a hydrophobic organic phase change material, 10-35 parts of a stabilizer, 3-15 parts of a curing agent, 15-45 parts of organosilicon, 3-15 parts of a dispersant, and water; the hydrophobic organic phase change material comprises n-tetradecanol and liquid paraffin in a weight ratio of 1: (1-5); the stabilizer comprises polyvinyl chloride and lecithin. The heat stability of the essence microcapsule can be improved by using the hydrophobic organic phase-change material and the stabilizer of specific types.

Description

Technical Field

[0001] The present invention relates to the field of material technology, and more specifically, to a flavor microcapsule and a preparation method and application thereof. Background Art

[0002] Fragrance is a kind of artificially formulated substance with a certain aroma, which is mainly used to add a specific aroma to products such as food, beverages, cosmetics and daily necessities. In cosmetics and daily necessities, flavors can not only bring unique aromas, but also modify certain irritating odors, thereby improving the acceptance and user experience of the products. With the development of society and the improvement of living standards, consumers have put forward higher requirements on the quality of cosmetics and daily necessities, and the demand for fragrances in cosmetics and daily necessities has also been increasing. However, due to the low boiling point, small molecular weight, easy volatility and poor thermal stability of flavors, when flavors are directly added to daily chemical products, the fragrance retention time of the flavors is short and the fragrance retention period cannot be guaranteed.

[0003] Microencapsulation technology is a technology that uses film-forming materials to encapsulate substances that are easily affected by the environment, such as flavor molecules, and forms micron-sized particles. Using microencapsulation technology to encapsulate flavors can reduce the volatilization of active ingredients in flavors, making the flavors easy to store and not easily oxidized. At the same time, it can also improve the thermal stability of the flavors and achieve a long-lasting release of the flavors. At present, the flavor microcapsules prepared by microencapsulation technology have a certain degree of thermal stability, but they still cannot meet the actual needs of consumers and need to be improved.

[0004] Therefore, it is of great significance to develop a flavor microcapsule with high thermal stability. Summary of the invention

[0005] The purpose of the present invention is to solve the problem of poor thermal stability of essence microcapsules in the prior art, and to provide an essence microcapsule and a preparation method and application thereof.

[0006] To achieve the above object, the technical solution adopted by the present invention is:

[0007] In a first aspect, the present invention provides a flavor microcapsule, wherein the raw materials thereof include the following components in parts by weight:

[0008] 15-45 parts of flavor, 3-15 parts of isocyanate, 3-15 parts of hydrophobic organic phase change material, 10-35 parts of stabilizer, 3-15 parts of curing agent, 15-45 parts of silicone, 3-15 parts of dispersant, water;

[0009] The hydrophobic organic phase change material comprises n-tetradecanol and liquid paraffin (CAS No.: 8012-95-1) in a weight ratio of 1:(1-5);

[0010] The stabilizer includes polyvinyl chloride (CAS No.: 9002-86-2) and lecithin (CAS No.: 8002-43-5).

[0011] The present invention can improve the thermal stability of the fragrance microcapsules by using specific types of hydrophobic organic phase change materials and stabilizers.

[0012] Specifically, in the process of preparing the fragrance microcapsules of the present invention, using n-tetradecanol and liquid paraffin in specific proportions as the hydrophobic organic phase change materials can increase the contact and adhesion force between molecules in the system, and can promote the formation of a structurally stable microcapsule wall by isocyanate, curing agent, and silicone to firmly lock and encapsulate the fragrance, thereby improving the thermal stability of the fragrance microcapsules.

[0013] Using polyvinyl chloride and lecithin as the stabilizer can not only improve the structural stability of the microcapsule wall during the preparation process of the fragrance microcapsules of the present invention, but also maintain the structural stability of the microcapsule wall after the formation of the fragrance microcapsules, so it is beneficial to improve the thermal stability of the fragrance microcapsules.

[0014] In the present invention, the thermal stability of the fragrance microcapsules is characterized by the magnitude of the thermal weight loss rate of the fragrance microcapsules. A small thermal weight loss rate of the fragrance microcapsules indicates high thermal stability of the fragrance microcapsules.

[0015] Preferably, the hydrophobic organic phase change material includes n-tetradecanol and liquid paraffin in a weight ratio of 1:(2-3).

[0016] Preferably, the stabilizer includes polyvinyl chloride and lecithin in a weight ratio of 1:(0.5-4).

[0017] More preferably, the stabilizer includes polyvinyl chloride and lecithin in a weight ratio of 1:(0.5-3).

[0018] Even more preferably, the stabilizer includes polyvinyl chloride and lecithin in a weight ratio of 1:(1-2).

[0019] Common fragrances in the art can be used in the present invention, such as at least one of eucalyptus oil, blue gum oil, rose oil, sweet orange oil, Michelia alba oil, lemon oil, agarwood oil, tangerine peel oil, clove oil, rosemary oil, citronella oil, and gardenia oil.

[0020] Preferably, the isocyanate is at least one of isophorone diisocyanate, 2,4-toluene diisocyanate, 2,6-toluene diisocyanate, and dicyclohexylmethane diisocyanate.

[0021] Preferably, the curing agent is at least one of ethylenediamine, tetraethylenepentamine, and hexamethylenediamine.

[0022] Preferably, the silicone is at least one of methyltrimethoxysilane, vinyl silane, and silicone oil.

[0023] Preferably, the dispersant is at least one of styrene-maleic anhydride copolymer (CAS No.: 9011-13-6), polyethylene glycol (CAS No.: 25322-68-3), and glyceryl tristearate (CAS No.: 555-43-1).

[0024] Preferably, the weight parts of water are 20 - 50 parts.

[0025] More preferably, the weight parts of water are 20 - 30 parts.

[0026] Preferably, the average particle size of the flavor microcapsules is 20 - 80 μm.

[0027] More preferably, the average particle size of the flavor microcapsules is 20μm, 22μm, 25μm, 27μm, 30μm, 31μm, 32μm, 33μm, 34μm, 35μm, 36μm, 37μm, 38μm, 39μm, 40μm, 41μm, 42μm, 43μm, 44μm, 45μm, 46μm, 47μm, 48μm, 49μm, 50μm, 51μm, 52μm, 53μm, 54μm, 55μm, 56μm, 57μm, 58μm, 59μm, 60μm, 62μm, 65μm, 67μm, 70μm, 72μm, 75μm, 77μm, 80μm or the range composed of any two of these values.

[0028] Even more preferably, the average particle size of the flavor microcapsules is 30 - 60 μm, specifically 35 - 60 μm or 38 - 60 μm.

[0029] Even more preferably, the average particle size of the flavor microcapsules is 48 - 52 μm.

[0030] Preferably, for the flavor microcapsules, calculated by weight parts, its raw materials include the following components:

[0031] 20 - 40 parts of flavor, 5 - 10 parts of isocyanate, 5 - 10 parts of hydrophobic organic phase change material, 15 - 30 parts of stabilizer, 5 - 10 parts of curing agent, 20 - 40 parts of silicone, 5 - 10 parts of dispersant, and water.

[0032] In a second aspect, the present invention provides a method for preparing flavor microcapsules, comprising the following steps:

[0033] S1. Mix the flavor, isocyanate, and hydrophobic organic phase change material to obtain an organic phase;

[0034] S2. Mix the stabilizer and water to obtain an aqueous phase;

[0035] S3. Mix the organic phase, the aqueous phase, the curing agent, the silicone and the dispersant to react, and then the microcapsules of essence can be obtained.

[0036] Preferably, in step S3, the temperature of the reaction is 40 - 50 °C.

[0037] Preferably, after the reaction in step S3, centrifugation, washing and drying are further included.

[0038] Preferably, step S3 is specifically: first mix the organic phase and the aqueous phase, and perform homogenization, then add the curing agent, the silicone and the dispersant to react, and then the microcapsules of essence can be obtained.

[0039] Preferably, the rate of the homogenization is 1500 - 3000 rpm.

[0040] In the third aspect, the present invention provides an application of the microcapsules of essence in cosmetics and / or daily necessities.

[0041] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0042] The present invention can improve the thermal stability of the microcapsules of essence by using specific types of hydrophobic organic phase change materials and stabilizers.

[0043] Specifically, in the process of preparing the microcapsules of essence in the present invention, using specific proportions of n - tetradecanol and liquid paraffin as the hydrophobic organic phase change materials can increase the contact and adhesion force between molecules in the system, and can promote the formation of a microcapsule wall with stable structure by isocyanate, curing agent and silicone to firmly lock and encapsulate the essence, thereby improving the thermal stability of the microcapsules of essence.

[0044] Using polyvinyl chloride and lecithin as stabilizers can not only improve the structural stability of the microcapsule wall in the process of preparing the microcapsules of essence in the present invention, but also maintain the structural stability of the microcapsule wall after the microcapsules of essence are formed, so it is beneficial to improve the thermal stability of the microcapsules of essence. Description of the Drawings

[0045] Figure 1 It is the optical microscope morphology diagram of the microcapsules of essence in Example 1.

[0046] Figure 2 It is the optical microscope morphology diagram of the microcapsules of essence in Example 10. Detailed Embodiments

[0047] To better illustrate the purpose, technical solution and advantages of the present invention, the present invention will be further described below in conjunction with specific embodiments.

[0048] The experimental methods in the following examples without specifying specific conditions are generally carried out according to conventional conditions in the art or according to conditions recommended by the manufacturer; the raw materials, reagents, etc. used, unless otherwise specified, are all raw materials and reagents that can be obtained from commercial channels such as conventional markets.

[0049] In each embodiment and comparative example of the present invention, the use of reagents is as follows:

[0050] Liquid paraffin (CAS No.: 8012-95-1), AR, Foshan Xilong Chemical Co., Ltd.;

[0051] Polyvinyl chloride (CAS No.: 9002-86-2), P107106, Shanghai Aladdin Biochemical Technology Co., Ltd.;

[0052] Lecithin (CAS No.: 8002-43-5), L105732, Shanghai Aladdin Biochemical Technology Co., Ltd.;

[0053] Styrene-maleic anhydride copolymer (CAS No.: 9011-13-6, dispersant), S909954, Shanghai MacLean Biochemical Technology Co., Ltd.;

[0054] Polyethylene glycol (CAS No.: 25322-68-3, dispersant), P815611, Shanghai MacLean Biochemical Technology Co., Ltd.;

[0055] Glyceryl tristearate (CAS No. 555-43-1, dispersant), G109097, Shanghai Aladdin Biochemical Technology Co., Ltd.;

[0056] Silicone oil, dimethyl silicone oil, D493241, Shanghai Aladdin Biochemical Technology Co., Ltd.

[0057] Example 1

[0058] This embodiment provides a flavor microcapsule, and its raw materials include the following components by weight:

[0059] 40 parts of flavor (eucalyptus oil, rose oil and sweet orange oil in a weight ratio of 1:1:2), 10 parts of isocyanate (isophorone diisocyanate), 10 parts of hydrophobic organic phase change material, 20 parts of stabilizer, 8 parts of curing agent (ethylenediamine), 25 parts of organosilicon (vinyl silane), 10 parts of dispersant (styrene-maleic anhydride copolymer), and 20 parts of water;

[0060] The hydrophobic organic phase change material is n-tetradecanol and liquid paraffin (CAS No.: 8012-95-1) in a weight ratio of 1:3;

[0061] The stabilizer comprises polyvinyl chloride and lecithin (CAS No.: 8002-43-5) in a weight ratio of 1:1;

[0062] The preparation method of the above-mentioned essence microcapsules comprises the following steps:

[0063] S1. Mix the essence, isocyanate, and hydrophobic organic phase change material to obtain an organic phase;

[0064] S2. Mix the stabilizer and water to obtain an aqueous phase;

[0065] S3. First, mix the organic phase and the aqueous phase, and homogenize at a rate of 2000 rpm for 10 min, then add the curing agent, silicone, and dispersant, react at 50 °C for 2 h, centrifuge, wash with water, and dry at 50 °C to obtain the essence microcapsules.

[0066] Examples 2-4 and Comparative Examples 1-3

[0067] Examples 2-4 and Comparative Examples 1-3 provide different essence microcapsules, which are different from Example 1 in that the weight ratio of n-tetradecanol and liquid paraffin (CAS No.: 8012-95-1) is different, and the rest are the same as Example 1, as shown in the following table:

[0068] Table 1 Weight ratio of n-tetradecanol and liquid paraffin in Examples 1-4 and Comparative Examples 1-3

[0069] Weight ratio of tetradecanol and liquid paraffin Example 1 1:3 Example 2 1:2 Example 3 1:5 Example 4 1:1 Comparative Example 1 1:10 Comparative Example 2 1:0 Comparative Example 3 0:1

[0070] Examples 5 and Comparative Example 4

[0071] Examples 5 and Comparative Example 4 provide different essence microcapsules, which are different from Example 1 in that the weight parts of the hydrophobic organic phase change material are different, and the rest are the same as Example 1, as shown in the following table:

[0072] Table 2 Weight parts of the hydrophobic organic phase change material in Examples 1, 5 and Comparative Example 4

[0073] Weight parts of hydrophobic organic phase change material / part Example 1 10 Example 5 5 Comparative Example 4 0

[0074] Examples 6-9 and Comparative Examples 5-6

[0075] Examples 6-9 and Comparative Examples 5-6 provide different essence microcapsules, which are different from Example 1 in that the weight ratio of polyvinyl chloride and lecithin (CAS No.: 8002-43-5) is different, and the rest are the same as Example 1, as shown in the following table:

[0076] Table 3 Weight ratio of polyvinyl chloride and lecithin in Examples 1, 6-9 and Comparative Examples 5-6

[0077] Weight ratio of polyvinyl chloride and lecithin Example 1 1:1 Example 6 1:2 Example 7 1:0.5 Example 8 1:3 Example 9 1:4 Comparative Example 5 1:0 Comparative Example 6 0:1

[0078] Examples 10-11 and Comparative Example 7

[0079] Examples 10 - 11 and Comparative Example 7 provide different fragrance microcapsules, which are different from Example 1 in that the weight parts of the stabilizer are different, and the rest are the same as Example 1. The specific details are shown in the following table:

[0080] Table 4 Weight Parts of the Stabilizer in Example 1, Examples 10 - 11 and Comparative Example 7

[0081]

[0082]

[0083] Example 12

[0084] This example provides a fragrance microcapsule, and calculated by weight parts, its raw materials include the following components:

[0085] Fragrance (eucalyptus oil, rose oil and sweet orange oil with a weight ratio of 1:2:2) 20 parts, isocyanate (2,4-toluene diisocyanate) 5 parts, hydrophobic organic phase change material 5 parts, stabilizer 15 parts, curing agent (tetraethylenepentamine) 5 parts, silicone (methyltrimethoxysilane) 20 parts, dispersant (polyethylene glycol) 5 parts, water 30 parts;

[0086] The hydrophobic organic phase change material is n - tetradecanol and liquid paraffin (CAS No.: 8012 - 95 - 1) with a weight ratio of 1:3;

[0087] The stabilizer includes polyvinyl chloride and lecithin (CAS No.: 8002 - 43 - 5) with a weight ratio of 1:1;

[0088] The preparation method of the above - mentioned fragrance microcapsule is the same as that of Example 1.

[0089] Example 13

[0090] This example provides a fragrance microcapsule, and calculated by weight parts, its raw materials include the following components:

[0091] Fragrance (eucalyptus oil and sweet orange oil with a weight ratio of 1:2) 40 parts, isocyanate (dicyclohexylmethane diisocyanate) 5 parts, hydrophobic organic phase change material 5 parts, stabilizer 30 parts, curing agent (hexamethylenediamine) 10 parts, silicone (silicone oil) 40 parts, dispersant (glycerol tristearate) 10 parts, water 20 parts;

[0092] The hydrophobic organic phase change material is n - tetradecanol and liquid paraffin (CAS No.: 8012 - 95 - 1) with a weight ratio of 1:3;

[0093] The stabilizer includes polyvinyl chloride and lecithin (CAS No.: 8002 - 43 - 5) with a weight ratio of 1:1;

[0094] The preparation method of the above-mentioned flavor microcapsules is the same as that of Example 1.

[0095] Comparative Example 8

[0096] This comparative example provides a flavor microcapsule, which is different from Example 1 in that paraffin wax (CAS No.: 8002-74-2, P100933, Shanghai Aladdin Biochemical Technology Co., Ltd.) is used instead of liquid paraffin, and the rest are the same as those in Example 1.

[0097] Comparative Example 9

[0098] This comparative example provides a flavor microcapsule, which is different from Example 1 in that n-eicosane is used instead of liquid paraffin, and the rest are the same as those in Example 1.

[0099] Comparative Example 10

[0100] This comparative example provides a flavor microcapsule, which is different from Example 1 in that gum arabic (CAS No.: 9000-01-5, A108975, Shanghai Aladdin Biochemical Technology Co., Ltd.) is used instead of lecithin, and the rest are the same as those in Example 1.

[0101] Performance test

[0102] The performance of the flavor microcapsules of each example and comparative example was tested, and the specific details are as follows:

[0103] 1. Thermogravimetric rate test:

[0104] Using a thermogravimetric analyzer, at a nitrogen temperature of 25°C - 800°C, the flavor microcapsule samples (about 10 mg) of each example or comparative example were sealed in an alumina crucible, and the thermogravimetric rate test was carried out at a heating rate of 10°C / min;

[0105] In the present invention, the thermostability of the flavor microcapsule is characterized by the magnitude of the thermogravimetric rate of the flavor microcapsule. A small thermogravimetric rate of the flavor microcapsule indicates high thermostability of the flavor microcapsule;

[0106] 2. Average particle size test

[0107] Using a laser particle size analyzer, about 5 mg of the flavor microcapsule samples of each example or comparative example were dissolved in 10 mL of ethanol, diluted 5 times in a test tube, and then placed in a cuvette to measure the average particle size of the flavor microcapsules;

[0108] The experimental results are as follows:

[0109] Table 5 Performance test results of the flavor microcapsules of each example and comparative example

[0110]

[0111]

[0112] Figure 1 Optical microscope morphology diagram of the flavor microcapsules in Example 1. Figure 2 Optical microscope morphology diagram of the flavor microcapsules in Example 10.

[0113] As can be seen from Table 5, the present invention can improve the thermal stability of flavor microcapsules by using specific types of hydrophobic organic phase change materials and stabilizers.

[0114] Specifically, in the process of preparing flavor microcapsules in the present invention, using a specific proportion of n-tetradecanol and liquid paraffin as the hydrophobic organic phase change material can increase the contact and adhesion force between molecules in the system, and can promote the formation of a microcapsule wall with a stable structure by isocyanate, curing agent, and silicone to firmly lock and encapsulate the flavor, thereby improving the thermal stability of the flavor microcapsules.

[0115] Using polyvinyl chloride and lecithin as stabilizers can not only improve the structural stability of the microcapsule wall during the preparation process of the flavor microcapsules in the present invention, but also maintain the structural stability of the microcapsule wall after the formation of the flavor microcapsules. Therefore, it is beneficial to improve the thermal stability of the flavor microcapsules.

[0116] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit the protection scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those of ordinary skill in the art should understand that the technical solutions of the present invention can be modified or equivalently replaced without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A flavor microcapsule, characterized in that: Calculated by weight, the raw materials include the following ingredients: 15-45 parts of flavor, 3-15 parts of isocyanate, 3-15 parts of hydrophobic organic phase change material, 10-35 parts of stabilizer, 3-15 parts of curing agent, 15-45 parts of silicone, 3-15 parts of dispersant, water; The hydrophobic organic phase change material comprises n-tetradecanol and liquid paraffin in a weight ratio of 1:(1-5); The stabilizers include polyvinyl chloride and lecithin.

2. The flavor microcapsule according to claim 1, characterized in that: The hydrophobic organic phase change material comprises n-tetradecanol and liquid paraffin in a weight ratio of 1:(2-3).

3. The flavor microcapsule according to claim 1, characterized in that: The stabilizer comprises polyvinyl chloride and lecithin in a weight ratio of 1:(0.5-4).

4. The flavor microcapsule according to claim 3, characterized in that: The stabilizer comprises polyvinyl chloride and lecithin in a weight ratio of 1:(0.5-3).

5. The flavor microcapsule according to claim 4, characterized in that: The stabilizer includes polyvinyl chloride and lecithin in a weight ratio of 1:(1-2).

6. The flavor microcapsule according to claim 1, characterized in that: Including at least one of the following (1)-(5): (1) The isocyanate is at least one of isophorone diisocyanate, 2,4-toluene diisocyanate, 2,6-toluene diisocyanate, and dicyclohexylmethane diisocyanate; (2) The curing agent is at least one of ethylenediamine, tetraethylenepentamine, and hexamethylenediamine; (3) The organosilicon is at least one of methyltrimethoxysilane, vinyl silane and silicone oil; (4) The dispersant is at least one of styrene-maleic anhydride copolymer, polyethylene glycol, and tristearic acid glyceryl; (5) The essence is at least one of eucalyptus oil, eucalyptus globulus oil, rose oil, sweet orange oil, white jasmine oil, lemon oil, agarwood oil, tangerine peel oil, clove oil, rosemary oil, citronella oil, and gardenia oil.

7. The flavor microcapsule according to claim 1, characterized in that: The average particle size of the essence microcapsule is 20-80 μm.

8. The flavor microcapsule according to claim 1, characterized in that: The raw materials of the essence microcapsules include the following components by weight: 20-40 parts of flavor, 5-10 parts of isocyanate, 5-10 parts of hydrophobic organic phase change material, 15-30 parts of stabilizer, 5-10 parts of curing agent, 20-40 parts of silicone, 5-10 parts of dispersant, and water.

9. A method for preparing the flavor microcapsule according to any one of claims 1 to 8, characterized in that: The steps include: S1. Mixing flavor, isocyanate, and hydrophobic organic phase change material to obtain an organic phase; S2. Mixing stabilizer and water to obtain an aqueous phase; S3. Mix the organic phase, aqueous phase, curing agent, organosilicon and dispersant to react and obtain the fragrance microcapsules.

10. Use of the essence microcapsule according to any one of claims 1 to 7 in cosmetics and / or daily necessities.

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