阅读说明：本技术 一种留香颗粒组合物及其制备方法 (Fragrance-retaining particle composition and preparation method thereof ) 是由 王权威 王新权 王喜梅 李东华 于 2021-08-27 设计创作，主要内容包括：本发明涉及一种留香颗粒组合物,所述留香颗粒组合物具有核壳结构,所述核壳结构包括：核结构,所述核结构的成分,包括香精、吸附剂和填充剂；壳结构,所述壳结构的成分,包括粘合剂和包覆材料；其中,所述填充剂选自无机填充剂、有机填充剂的一种、多种或其混合物。本发明的留香颗粒组合物可以使得香精稳定均匀地向留香颗粒组合物的壳结构,以及其表面扩散,从而实现持久且均匀的留香效果。本发明的留香颗粒组合物还具有留香颗粒溶解性好、成本低、稳定性好、外观均一等一系列优点。(The invention relates to a fragrance-retaining particle composition, which has a core-shell structure, wherein the core-shell structure comprises: a core structure, the core structure comprising ingredients including a fragrance, an adsorbent, and a filler; a shell structure, the components of the shell structure including a binder and a coating material; wherein the filler is selected from one or more of inorganic filler and organic filler or a mixture thereof. The fragrance-retaining particle composition can ensure that the essence is stably and uniformly diffused to the shell structure and the surface of the fragrance-retaining particle composition, thereby realizing the lasting and uniform fragrance-retaining effect. The fragrance-retaining particle composition also has a series of advantages of good solubility of fragrance-retaining particles, low cost, good stability, uniform appearance and the like.)

1. A fragrance-retaining particulate composition, the fragrance-retaining particulate composition having a core-shell structure, the core-shell structure comprising:

a core structure, the core structure comprising ingredients including a fragrance, an adsorbent, and a filler;

a shell structure, the components of the shell structure including a binder and a coating material;

wherein the content of the first and second substances,

the filler is selected from one or more of inorganic filler and organic filler or a mixture thereof.

2. The flavor-retaining particle composition of claim 1, wherein the adsorbent is selected from one or more of white carbon black, bentonite, anhydrous sodium sulphate and zeolite.

3. The flavor-retaining particle composition according to claim 1, wherein the mass ratio of the inorganic filler to the organic filler in the filler is: 1:1-3:1.

4. A fragrance-retaining particulate composition according to claim 3, characterized in that the inorganic filler is selected from one or more of the group consisting of bicarbonate, carbonate, sulphate, nitrate, chloride, citrate, tartrate, acetate, formate; the organic filler is selected from polyols.

5. A fragrance-retaining particle composition according to claim 4, wherein the polyol has a melting point of not less than 40 ℃.

6. A fragrance-retaining granule composition according to claim 1, wherein the binder is selected from one or more of starch, dextrin, polyvinyl alcohol, hydroxypropylmethylcellulose.

7. The flavor-retaining particle composition of claim 1, wherein the coating material is selected from one or more of sucrose powder, glucose powder, kaolin, montmorillonite powder, and mica powder.

8. The aroma-retaining particle composition according to claim 1, wherein the aroma-retaining particle composition comprises a core structure and a shell structure, and the aroma-retaining particle composition comprises the following components in parts by mass:

9. a fragrance-retaining particle composition according to claim 8 wherein the adjuvants comprise one or more of pigments, cationic polymers, inorganic salts, water.

10. A process for the preparation of a perfume-retaining particle composition according to any of claims 1 to 9 comprising the steps of:

s1, preparation of a core structure: mixing essence and water, adding adsorbent and filler, stirring, and granulating;

s2, preparing a fragrance-retaining particle composition: the core structure, binder and coating material are mixed and then granulated.

Technical Field

The invention belongs to the field of fragrance retention of fabrics, and particularly relates to a fragrance retention particle composition and a preparation method thereof.

Background

As the living standard of people is gradually improved, consumers have higher requirements on fabric care, namely, the requirements on cleanness and tidiness of clothes are met, and the clothes after washing are expected to release pleasant faint scent, so that the clothes have the effects of lasting fragrance on the clothes and resisting peculiar smells such as chafing dish materials, barbecue materials and the like. However, the detergent powder or the laundry detergent has less essence which can be used in the formula due to the compatibility problem and the stability concern, and the dosage is limited, so the effect of lasting fragrance can not be achieved. The fabric fragrance-retaining products are designed to meet the unique requirements of different consumers on fragrance-retaining strength and fragrance-retaining smell. The product is directly added with the laundry detergent at the washing stage without being additionally added at the rinsing stage, so that the addition operation is more convenient than that of the softener at the rinsing stage on the one hand, and no chemical residue is ensured on the other hand.

The aroma-retaining products appearing in the current market mainly have two technical schemes. One, for example, the technical scheme of patent numbers CN109234043A, CN111518637A and CN111286414A, uses PEG polyethylene glycol as a carrier, blends with essence under melting, and then cools and granulates to obtain the product. Obviously, the essences are volatile substances, and when the essences are melted together at high temperature, partial volatilization can be caused, so that the fragrance and the odor type are changed, and the stability of a finished product is even affected. In addition, the production equipment investment is large, the process is complex, and different product appearances and aroma expressions can be generated due to slight change of process parameters. In another technical scheme, as described in patent nos. CN110760395A, CN112522040A and CN112522039A, a water-soluble substance is used as a carrier, and a liquid essence or a microcapsule essence is adsorbed on the surface of the water-soluble substance to achieve the effect of retaining fragrance of fabric. However, in the product prepared by the method, only the shell is provided with essence, and the essence is rapidly lost along with the prolonging of the storage time, so that the lasting fragrance retaining capability is reduced; and the preparation process is complex to control, and the particle size in the production process is difficult to control uniformly.

In view of the above, it is desirable to design a fragrance-retaining composition with simple process, easily controllable particle size, good product stability, good solubility, and fragrance barrier layer to slow down fragrance loss and finally provide excellent and sustained fragrance-retaining effect.

Disclosure of Invention

The invention aims at the technical problems and discloses a fragrance-retaining particle composition which has a core-shell structure, essence components are coated in the core structure, and the essence can be stably and uniformly diffused to the shell structure and the surface of the fragrance-retaining particle composition by adding an adhesive and a filling material, so that a lasting and uniform fragrance retaining effect is realized. The fragrance-retaining particle composition also has a series of advantages of good solubility of fragrance-retaining particles, low cost, good stability, uniform appearance and the like.

As used herein, unless otherwise indicated, "fragrance-retaining granules" also refers to "fragrance-retaining particles".

One object of the present invention is to disclose a fragrance-retaining particle composition having a core-shell structure comprising:

a core structure, the core structure comprising ingredients including a fragrance, an adsorbent, and a filler;

a shell structure, the components of the shell structure including a binder and a coating material;

wherein the filler is selected from a mixture of inorganic fillers and organic fillers.

The essence can be liquid essence and/or microcapsule essence.

The liquid essence is prepared by taking mixed oil or oil-soluble substances designed by essence companies as solvents and water or water-soluble substances as solvents according to the requirements of consumers. The formula of the essence is adjusted according to the expression of the top note, the body note and the tail note of the essence researched and researched by the market. In the composition of the fragrance-retaining particles, the liquid essence comprises one or two of water-soluble essence and oil-soluble essence. The addition amount of the liquid essence is preferably 1-10 wt%.

The microcapsule essence is prepared by wrapping raw materials such as essence, plant essential oil and the like with special materials by a modern technological means to form microcapsule emulsion. The wrapping material may be selected from polyurea, polyurethane and/or polyureaurethane, preferably polyoxymethylene urea, such systems including but not limited to urea-formaldehyde and/or melamine-formaldehyde. After the product is treated by the aromatic, the fragrance retention time of the product can be greatly prolonged. During the washing process, the microcapsule essence is retained in the clothes fiber, and along with the friction of clothes, the microcapsules retaining the fragrance explode like foam to continuously emit the fragrance. The amount of microencapsulated flavour in the composition of the flavour-retaining particles described herein is preferably 1-10 wt%.

The essence is preferably a composition of the two essences.

The adsorbent is selected from inorganic salt compounds, has loose and porous surface, and can adsorb essence to the maximum extent. The adsorbent disclosed by the invention has good hydrophilicity, so that the adsorbent can be conveniently granulated, and can be quickly dispersed in the washing process without being adsorbed on fabrics. In the composition of the fragrance-retaining particles of the present invention, the addition amount of the adsorbent is preferably 20 to 50 wt%.

The adhesive is water soluble so as to be dissolved in water quickly. The adhesive is mainly used for adjusting the strength and the size of the granulated particles to obtain the particles with uniform appearance and moderate strength. The addition amount of the clothes fragrance-retaining particle composition is 1-5 wt%.

Further, the adsorbent is selected from one or more of white carbon black, bentonite, anhydrous sodium sulphate and zeolite.

Further, the filler is selected from one or more of inorganic filler, organic filler or a mixture thereof;

in the filler, the mass ratio of the inorganic filler to the organic filler is as follows: 1:1-3:1.

Further, the inorganic filler is selected from one or more of bicarbonate, carbonate, sulfate, nitrate, chloride, citrate, tartrate, acetate and formate; the organic filler is selected from polyols.

Further, the melting point of the polyhydric alcohol is more than or equal to 40 ℃;

wherein

The polyol can be, but is not limited to, a polyol small molecule or a polyol polymer;

wherein, the molecular structure of the polyol small molecule at least contains 4 hydroxyl groups, and the molecular weight of the polyol small molecule is preferably more than 100;

the polyol polymer is selected from one of polyethylene glycol and polyvinyl alcohol, and the molecular weight of the polyol polymer is preferably more than 1000.

Further, the adhesive is selected from one or more of starch, dextrin, polyvinyl alcohol and hydroxypropyl methyl cellulose.

Further, the coating material is one or more of sucrose powder, glucose powder, kaolin, montmorillonite powder and mica powder.

Further, the aroma-retaining particle composition comprises a core structure and a shell structure, and comprises the following components in percentage by mass:

further, the auxiliary agent comprises one or more of pigment, cationic polymer, inorganic salt and water.

Auxiliary agents in order to diversify the appearance and function of the fragrance-retaining particles, the following substances can be optionally added: pigment, cationic polymer, neutral inorganic salt and/or water. Wherein the inorganic salt is anhydrous crystalline salt selected from the group consisting of but not limited to sodium chloride, potassium chloride, magnesium chloride, calcium chloride, sodium sulfate, potassium sulfate, magnesium sulfate, calcium carbonate, and calcium bicarbonate. The cationic polymer may be selected from, but is not limited to, guar hydroxypropyltrimonium chloride, gum arabic, ammonium polyphosphate, polyquaternium-6, polyquaternium-7, polyquaternium-10, polyquaternium-39, polyquaternium-67.

Another object of the present invention is to disclose a method for preparing the above perfume particle composition, which comprises the steps of:

s1, preparation of a core structure: mixing essence and water, adding adsorbent and filler, stirring, and granulating;

s2, preparing a fragrance-retaining particle composition: the core structure, binder and coating material are mixed and then granulated.

Further, the grain diameter of the fragrance-retaining particle composition is 2-20 mm.

The invention has the following beneficial effects:

1. on one hand, the fragrance-retaining particle composition disclosed by the invention has a core-shell structure, essence components are coated in the core structure, and the essence can be stably and uniformly diffused to the shell structure and the surface of the fragrance-retaining particle composition by adding the adhesive and the coating material; on the other hand, the aroma-retaining particle composition disclosed by the invention adopts a normal-temperature preparation process flow, so that the problem of essence volatilization at a high temperature is avoided, and a lasting and uniform aroma-retaining effect is realized.

2. The fragrance-retaining particle composition disclosed by the invention is good in stability and solubility and simple in preparation method, and fragrance-retaining particles with uniform particles, moderate strength and attractive shape can be obtained by adding the adhesive.

Detailed Description

In order to more clearly illustrate the technical solution of the present invention, the following examples are given. The starting materials, reactions and work-up procedures which are given in the examples are, unless otherwise stated, those which are customary on the market and are known to the person skilled in the art.

The liquid essence in the examples and comparative examples of the present invention was purchased from Qiwashington; the brand is 'flower and fruit fragrance-fresh summer';

the microcapsule essence in the embodiment of the invention is purchased from Qiwashington; the brand is 'flower and fruit fragrance-beautiful appearance';

the strength test of the fragrance-retaining particles in the examples and the comparative examples is carried out by adopting an HG2224-91 particle flexural strength test method.

The ingredients and the corresponding mass fractions of the compositions of the fragrance retaining granules of the examples of the invention are shown in table 1. It should be noted that the mass fractions of all the components in the core structure or the shell structure in the present invention refer to the mass fractions of the components in the flavor-retaining granule composition.

Table 1 individual ingredients and corresponding mass fractions in the perfume particle compositions of the individual examples

The preparation of the fragrance-retaining granule compositions of examples 1-6 above was as follows:

s1, respectively weighing the mass of each component according to the mass fraction for later use;

s2, preparation of a core structure: at normal temperature, uniformly mixing liquid essence, microcapsule essence and water, then adding the adsorbent component and the filler component according to the table 1, and uniformly stirring to obtain a mixture; adding pigment, water and other auxiliaries into the mixture, uniformly stirring, and then granulating by using a granulator to obtain the particle size of the core structure, wherein examples 1 to 6 sequentially comprise; 6mm, 4mm, 5mm and 3 mm.

S3, preparing a fragrance-retaining particle composition: finally, the core structure, the binder and the coating material according to table 1 are prepared into particles with uniform (about 8mm) diameter and moderate (about 500N) strength, and the product is obtained. The resulting granules were either pure round or slightly olive shaped.

Obviously, in the above granulation coating process, the essence component exists in the interior of the granule, but not in the surface layer of the granule.

Comparative example 1

The prior common clothing aroma-enhancing particle structure based on PEG as a carrier adopted in the comparative example 1 does not have a core-shell structure, and comprises the following components:

7 wt% of liquid essence

PEG8000 93wt％。

The preparation process comprises the following steps: heating PEG8000 to 70-80 deg.C to melt into liquid, adding essence, stirring, and granulating to obtain granule with uniform size (about 8mm) and moderate strength (about 800N). The resulting particles were oblate.

Obviously, the above process adopts a eutectic granulation process, and the inside of the granules and the surface layer of the granules have essence components.

Comparative example 2

The clothing aroma-enhancing particle structure based on silicon dioxide as an adsorbent adopted in the comparative example 2 also has a core-shell structure and comprises the following components:

core structure:

glucose granules (diameter 7mm) 90 wt%

Shell structure:

7 wt% of liquid essence

Silica 3% by weight

The preparation process comprises the following steps: at normal temperature, glucose granules are added into a stirring pot to serve as a core structure, then liquid essence and silicon dioxide are added, the mixture is stirred uniformly, and a granulator is used for forming uniform (about 8mm) granules with moderate strength (about 800N).

Obviously, the liquid essence of the granules obtained by the above process is only adsorbed on the surface layer of the granules, and the essence component does not exist in the glucose granules in the core structure.

Test example

(1) Fragrance retention test

15g of each of the fragrance-retaining particle compositions of examples 1 and 6 and comparative examples 1 to 2 was poured into a washing machine, and then placed on pure cotton towels of the same specification individually and placed in the washing machine, and the washing machine was adjusted to a mixed washing mode to wash each of the above towels for 60 min. After washing, 10 trained evaluators evaluated the fragrance concentration of the towel, and the fragrance concentration was scored according to 1-5 points, with higher points indicating better fragrance retention intensity of the product. The evaluation staff respectively sets the towel which is just washed as a fragrance-retention effect evaluation point 1, the towel which is dried as a fragrance-retention effect evaluation point 2, and the towel which is stored for two weeks as a fragrance-retention effect evaluation point 3, and carries out fragrance-retention effect evaluation on the three evaluation points. The final test results were all averaged over 10 panelists and are shown in table 2 below.

Table 2 fragrance leave effect scores for different fragrance leave effect evaluation points for samples of example 1 and example 6, and comparative examples 1-2

The experimental results in table 2 show that the addition amounts and types of the liquid essences in example 1 and example 6 are the same as those in comparative examples 1-2, but the fragrance retention effects of the different fragrance retention effect evaluation points in example 1 and example 6 are obviously better than those in comparative example 1 and comparative example 2. This is because: the co-melting granulation process adopted in comparative example 1 causes partial volatilization of the liquid essence during the preparation process, so the fragrance retention effect is affected. The essence of comparative example 2 is retained in the shell structure of the particle rather than the core structure, so that the volatility is strong, resulting in a decrease in the fragrance retaining effect. In addition, the addition of the binder in examples 1 and 6 is more beneficial to the polymerization of the perfume, thereby preventing the loss of the perfume in the production process.

Further, comparing the fragrance of the towel after storing for two weeks, it can be seen that the fragrance retaining effect of the comparative examples 1-2 is much worse than that of the examples 1 and 6, because the core structure and the shell structure of the preparation process of the examples 1 and 6 have the essence, so that more essence is adsorbed on the fabric during washing, thereby achieving the long-term fragrance retaining effect.

(2) Dissolution Rate test

In a parallel experiment, a 1L beaker was filled with water, 0.2g of each of the samples of examples 1 to 6 and comparative examples 1 to 2 was weighed, and each was separately put into water, and the time for the sample to completely dissolve was observed at a rotation speed of 1000rpm, and the results were as shown in Table 3.

TABLE 3 dissolution times of samples of examples 1-6 and comparative examples 1-2

Sample (I)	Dissolution time (min)
		Example 1	<1
Example 2	<1
		Example 3	<1
Example 4	<1
		Example 5	<1
Example 6	<1
		Comparative example 1	8
Comparative example 2	6

Table 3 the results of the experiments show that the inventive samples have better solubility than the samples of comparative examples 1-2. This is relevant to the perfume carrier and the process of preparation. The PEG used in the sample of comparative example 1 as a carrier usually tends to be biased toward the use of PEG with a higher degree of polymerization to ensure the stability of the fragrance-retaining particles, resulting in a deviation in the solubility of the sample of comparative example 1; in the core-shell structure adopted in comparative example 2, the carbohydrate generally adopted in the core structure is repeatedly coated, so that the solubility is poor, and the overall solubility is reduced. In contrast, the core-shell prepared by the sample of the present invention is a substance having better water solubility, and is easily dispersed, so the solubility is better than that of the sample of comparative example 1-2.

(3) Product stability testing

The samples of examples 1 to 6 and comparative examples 1 to 2 were placed in an oven at 0 c, a constant temperature at 25 c and an oven at 45 c, respectively, for 1 month, and then the samples were taken out and the color difference change of the samples was visually observed. The results of the experiments are reported below.

TABLE 4 color difference recordings for samples of examples 1-6, comparative examples 1-2

Table 4 shows that, in comparative example 1, when PEG is used as the matrix, the liquid essence itself is easily discolored at high temperature; on the other hand, the essence is added into different matrixes, and the compatibility with the matrixes is different. The PEG matrix can undergo side reactions during the synthesis process, producing certain intermediate by-products, which can lead to discoloration. In comparative example 2, the perfume was adsorbed on the surface of the particles and was easily affected by the external environment, such as oxidation, temperature, volatilization of the perfume, etc., which resulted in the color change of the beads at normal and high temperatures. The perfume particles of examples 1-6, however, delayed the release of perfume due to the presence of the shell structure, resulting in no significant color change.

(4) Aroma leaving granule strength test

In a parallel experiment, 6 50ml small beakers with the same specification are prepared, 200g of the samples of examples 7-11 and comparative example 3 are weighed, a cover glass is flatly placed on each sample, 50g of weights with the same size are placed, the samples are placed at room temperature for 24 hours, and the deformation condition of the fragrance retaining particles of each sample is observed. The compositions and mass fractions of the samples of examples 7 to 11 and comparative example 3 are shown in Table 5. It should be noted that the mass fractions of all the components in the core structure or the shell structure in the present invention refer to the mass fractions of the components in the flavor-retaining granule composition.

The deformation of the flavor-retaining particles of examples 7 to 11 and comparative example 3 is shown in Table 6.

Table 5 ingredients and corresponding mass fractions for examples 7 to 11, comparative example 3

TABLE 6 deformation for 24h of the samples of examples 7-11, comparative example 3

The results of the experiments in tables 5 and 6 show that the comparative examples 7 to 11 and the comparative example 3 show that the morphology of the fragrance retaining particles is greatly affected by the addition of the binder, and the fragrance retaining particles without the addition of the binder are remarkably deformed. This indicates that the binder has a large effect on the strength of the flavor-retaining granule particles.

It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.

Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.