A kind of clothing fragrance particle composition and preparation method thereof

Abstract

The present invention relates to a composition of lingering fragrance particles for clothing, comprising: a pellet core and a coating layer that wraps the pellet core, characterized in that the pellet core comprises the following components in parts by mass: water-soluble particles, an adsorbent, a fragrance, a fragrance agent, a binder, and a filler; and the coating layer comprises the following components in parts by mass: an excipient and an adjuvant. The composition of lingering fragrance particles for clothing of the present invention has a coating structure and contains specific fragrance agents and adsorbents, which can stabilize and slowly release the fragrance of the fragrance. The particle size of the fragrance particles is controllable and can prevent the loss of fragrance, thereby achieving long-lasting fragrance retention of the fragrance particles. The composition of lingering fragrance particles for clothing of the present invention also has a series of advantages such as good solubility, good stability, and uniform appearance of the fragrance particles.

Description

Technical Field

[0001] The invention relates to the technical field of fabric washing and care, in particular to a clothing fragrance-retaining particle composition and a preparation method thereof. Background Art

[0002] Fragrance beads are a product developed by Downy, a subsidiary of the US Procter & Gamble Group, in 2011. P&G China introduced them to the Chinese market in 2017 and upgraded them to version 2.0 in 2019. This version of the beads eliminates bacteria, removes mites, and dissolves dirt. Its core ingredients remain fragrance oils and fragrance microcapsules. Current demand for fragrance beads is driven by two key factors: the ability to choose the scent to your liking and the ability to maintain a long-lasting, non-pungent fragrance.

[0003] There are three main technical solutions for fragrance-retaining products currently on the market. The first, more traditional technical solution, such as the technical solutions with patent numbers CN109652215A, CN113913250A, and CN111286414A, uses PEG polyethylene glycol as a carrier, allowing the flavor and PEG to blend at high temperatures, which can cause the aroma to change during the production process and affect the stability of the finished product's flavor. The second technical solution, such as the patents CN110760395A, CN112522040A, and CN112522039A, uses water-soluble particles as a carrier, and the flavor is coated on the surface of the water-soluble particles. The flavor is always exposed on the surface, and there is a risk of partial loss of the fragrance during storage and changes in the fragrance at high temperatures. The third technical solution, such as patent number CN111748426A, provides a method for preparing laundry detergent micropills, which improves the preparation of fragrance beads. However, the pill core does not contain fragrance agent, the coating layer wraps too much, the overall fragrance content is low, and the fragrance effect will be greatly reduced.

[0004] In summary, there is an urgent need to design a fragrance-retaining composition with a reasonable process flow, good product stability, good solubility, and the ability to prevent the loss of fragrance, thereby ultimately providing an excellent and lasting fragrance effect, in order to solve the problems existing in the prior art. Summary of the Invention

[0005] Based on this, the present invention provides a composition of lingering fragrance particles for clothing, overcoming the shortcomings of the prior art. This composition has an encapsulated structure, with a fragrance component encapsulated within a core. It also contains a specific fragrance agent and adsorbent, enabling a controlled and sustained release of the fragrance. The particles have a controllable particle size and can prevent the loss of fragrance, thereby achieving long-lasting fragrance. The composition also offers advantages such as good solubility, stability, and a uniform appearance.

[0006] One object of the present invention is to provide a fragrance-retaining particle composition for clothing, the fragrance-retaining particle composition comprising: a pellet core and a coating layer wrapping the pellet core;

[0007] The pellet core comprises the following components in parts by mass:

[0008]

[0009]

[0010] The coating layer comprises the following components in parts by weight:

[0011] 1-10 parts of excipients

[0012] Adhesive 0.01-5 parts

[0013] 0.01-5 parts of additives;

[0014] in,

[0015] The fragrance retaining agent is selected from acrylamide copolymer;

[0016] The comonomers of the acrylamide copolymer include (3-acrylamidopropyl)trimethylammonium chloride, acrylamide, nonylphenol polyoxyethylene ether acrylate, and acrylic acid;

[0017] The adsorbent is fatty acid-modified silica.

[0018] Furthermore, the auxiliary agent is selected from one or more of pigments, cationic polymers, and inorganic salts.

[0019] The acrylamide copolymer mentioned above has the function of fixing and slow-releasing fragrance on one hand, and on the other hand, it can form a unique flocculent with the solid particles in the detergent, carrying the fragrance to be deposited on the fabric, making the fragrance effect of the fragrance on the fabric more lasting.

[0020] Furthermore, the water-soluble particles are selected from one or more of sucrose, glucose, fructose, maltose, dextrin, PEG, and soda ash.

[0021] Furthermore, the fragrance is selected from one or more of liquid fragrances and microcapsule fragrances.

[0022] Liquid fragrances are typically designed by fragrance companies based on consumer demand, using a mixture of oils or oil-soluble substances as solvents, or water or water-soluble substances as solvents. The fragrance formula is adjusted based on market research into the top, body, and base notes of the fragrance. The liquid fragrance in the fragrance-retaining granules described herein comprises a combination of one or both water-soluble and oil-soluble fragrances.

[0023] Microcapsule fragrances are made by wrapping essences, essential oils and other raw materials with special materials through modern scientific and technological means to form microcapsules in an emulsion. This wrapping material can be selected from polyurea, polyurethane and / or polyurea-polyurethane, preferably polyformaldehyde urea. Such systems include but are not limited to urea-formaldehyde and / or melamine-formaldehyde. After the product is treated with fragrance, the product's fragrance retention time can be greatly extended. During the washing process, the microcapsule fragrance remains in the clothing fibers. As the clothes rub, the fragrant microcapsules will burst like bubbles, continuously emitting fragrance.

[0024] Furthermore, the added amount of the microcapsule flavor is 1-10 parts.

[0025] Furthermore, the added amount of the liquid essence is 1-10 parts.

[0026] Furthermore, the excipient is selected from one or more of titanium dioxide, calcium carbonate powder, titanium dioxide powder, calcium silicate, silicon dioxide, kaolin, montmorillonite powder, and mica powder.

[0027] Furthermore, the adsorbent is added in an amount of 2-20 parts.

[0028] Furthermore, to diversify the appearance and functionality of the fragrance-retaining particles, the additives may include, but are not limited to, one or a mixture of pigments, cationic polymers, and neutral inorganic salts. The inorganic salts are anhydrous crystalline salts and may be selected from, but not limited to, sodium chloride, potassium chloride, magnesium chloride, calcium chloride, sodium sulfate, potassium sulfate, magnesium sulfate, calcium carbonate, and calcium bicarbonate.

[0029] The cationic polymer may be selected from, but not limited to, guar hydroxypropyltrimonium chloride, gum arabic, ammonium polyphosphate, polyquaternium-6, polyquaternium-7, polyquaternium-10, polyquaternium-39, and polyquaternium-67.

[0030] Furthermore, the fatty acid is selected from one or more of caprylic acid, nonanoic acid, capric acid, lauric acid, myristic acid, palmitic acid, and stearic acid.

[0031] Furthermore, the filler is selected from one or more of bicarbonate, carbonate, sulfate, nitrate, chloride, citrate, tartrate, acetate, and formates.

[0032] Furthermore, the binder is selected from one or more of bentonite, starch paste, dextrin, polyvinyl alcohol, and hydroxypropyl methylcellulose.

[0033] Another object of the present invention is to provide a method for preparing the above-mentioned clothing fragrance particle composition, comprising the following steps:

[0034] S1. Preparation of fragrance:

[0035] The comonomer is added into water, stirred until dissolved, the pH of the solution is adjusted, an initiator is added under the protection of nitrogen, heated for reaction, and purified to obtain a fragrance agent;

[0036] S2. Preparation of adsorbent:

[0037] Silicon dioxide is added to liquid fatty acid, and after ultrasonic treatment, the mixture is heated for reaction and purified to obtain an adsorbent.

[0038] Furthermore, the mass ratio of (3-acrylamidopropyl)trimethylammonium chloride, acrylamide, nonylphenol polyoxyethylene ether acrylate, and acrylic acid in the comonomer is 10-20:5-30:5-10:1-15.

[0039] Furthermore, the initiator is selected from one or more of ammonium persulfate and potassium persulfate.

[0040] Furthermore, the pH is 5-9.

[0041] Furthermore, in step S1, the temperature of the heating reaction is 45-75°C and the time is 24-40 hours; in step S2, the temperature of the heating reaction is 70-90°C and the time is 0.5-3 hours.

[0042] Furthermore, the method further comprises the following steps:

[0043] S3. Pour the water-soluble particles, adsorbent, binder, fragrance agent, and filler into the granulation device;

[0044] S4. The flavor and water are mixed to form a spray liquid, spray granulation, and dried to obtain pellet cores;

[0045] S5. Excipients, adhesives and adjuvants are prepared to form a coating liquid, which is sprayed on the surface of the pellet core to form a coating layer, and then dried to obtain the clothing fragrance granule composition.

[0046] The present invention has the following beneficial effects:

[0047] 1. The clothing fragrance granule composition prepared by the present invention has a core-shell structure, and the core structure contains a fragrance agent obtained by copolymerizing four monomers: (3-acrylamidopropyl)trimethylammonium chloride, acrylamide, nonylphenol polyoxyethylene ether acrylate, and acrylic acid. Using nonylphenol polyoxyethylene ether acrylate as a comonomer can reduce surface tension and enable the fragrance agent to better contact with the essence; acrylamide can thicken and improve adhesion, improve the wetting performance of the fragrance agent in the fabric, and prevent the volatilization and loss of fragrance molecules; and the acrylic acid monomer introduces a large number of carboxyl groups, further improving the polarity, having better compatibility with other ingredients in the composition, and more stably combining with components such as fragrance; nonylphenol polyoxyethylene ether acrylate has a long chain structure and contains more oxygen-containing functional groups, so it is easy to entangle and adsorb with the essence molecules in the formula, and intermolecular forces can be formed between multiple ingredients, thereby enhancing stability and binding strength, and effectively improving the performance of sustained release and fragrance retention. This tetrapolymer has the advantage of good water solubility, can improve the thermal stability of the composition, is not easily inactivated at high temperatures, and can form unique floccules with solid particles in the detergent, so that the fragrance is deposited on the fabric, achieving the effect of sustained fragrance release, ensuring that the fragrance in the fragrance beads can better enter the fiber, achieving a long-lasting fragrance effect.

[0048] 2. The present invention's fragrance-retaining particle composition for clothing uses fatty acid-modified silica as an adsorbent, which improves the dispersibility and thermal stability of the silica, allowing it to be more evenly dispersed throughout the composition. Furthermore, the porous surface of the modified silica allows for greater absorption of fragrance. Furthermore, the fatty acid-modified silica has improved lipophilicity and compatibility with fragrance retaining agents, further enhancing the stability of the composition. The fragrance-retaining particle composition for clothing of the present invention promotes the flocculation of more fragrance on the surface of fabric fibers, increasing the amount of fragrance deposited on clothing and significantly enhancing the fragrance-retaining effect. DETAILED DESCRIPTION

[0049] In order to more clearly illustrate the technical solutions of the present invention, the following examples are given. Unless otherwise stated, the raw materials, reactions and post-processing methods mentioned in the examples are common raw materials on the market and technical methods well known to those skilled in the art.

[0050] The terms "preferred," "preferably," "more preferred," and the like, used herein, refer to embodiments of the invention that may provide certain benefits under certain circumstances. However, other embodiments may also be preferred under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.

[0051] It should be understood that, except in any operating examples, or where otherwise indicated, all numbers expressing, for example, quantities of ingredients used in the specification and claims are to be understood as being modified in all instances by the term "about." Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and appended claims are approximations that may vary depending upon the desired properties to be obtained by the present invention.

[0052] It should be noted that, in the specific implementation process, the granulation device mentioned adopts a relatively mature device currently available on the market.

[0053] The glucose in the embodiment of the present invention is water-soluble granules purchased from Shandong Liang New Material Technology Co., Ltd.

[0054] The liquid flavors in the examples and comparative examples of the present invention were purchased from Givaudan; the brand is "Flower and Fruit Fragrance - Fresh Summer".

[0055] The microcapsule essence in the embodiment of the present invention is purchased from Givaudan; the brand is "Flower and Fruit Fragrance - Graceful and Beautiful".

[0056] The light calcium carbonate in the embodiment of the present invention is a filler purchased from Jiangxi Polysilicon Mining Co., Ltd.

[0057] The starch paste in the embodiment of the present invention is an adhesive purchased from Wanruida.

[0058] The bentonite used in the embodiment of the present invention is an adhesive and is purchased from Xinyang Junxin Industrial Co., Ltd.

[0059] The titanium dioxide used in the examples of the present invention is an excipient purchased from Jiangxi Tuoan New Materials Co., Ltd.

[0060] The calcium carbonate powder in the embodiment of the present invention is an excipient purchased from Jiangxi Tuobang New Materials Co., Ltd.

[0061] The water-soluble pigment in the embodiment of the present invention is BLUE HP, purchased from Lincoln, USA.

[0062] In the examples of the present invention, (3-acrylamidopropyl)trimethylammonium chloride was purchased from Shanghai Yien Chemical Technology Co., Ltd.

[0063] Acrylamide in the examples of the present invention was purchased from Tokyo Chemical Industry Development Co., Ltd. (Shanghai).

[0064] The nonylphenol polyoxyethylene ether acrylate in the embodiment of the present invention is prepared by itself, and the preparation method is referenced by Zhang Fusheng, Liu Guoliang, Xu Xiaofang, etc. Synthesis of nonylphenol polyoxyethylene ether acrylate polymer and its surface activity and heavy oil viscosity reduction performance [J]. Journal of Donghua University (Natural Science Edition), 2020, 46(05): 747-753.

[0065] Acrylic acid, lauric acid, silicon dioxide, and caproic acid in the examples of the present invention were all purchased from Tokyo Chemical Industry (Shanghai) Co., Ltd.

[0066] In the embodiments of the present invention, PVA is an adhesive, which is purchased from Tokyo Chemical Industry (Shanghai) Development Co., Ltd.

[0067] The ingredients and corresponding parts by mass in the clothing fragrance granule compositions of Examples 1-3 and Comparative Examples 1-3 of the present invention are shown in Table 1.

[0068] Table 1 Components and their mass fractions in Examples 1-3 and Comparative Examples 1-3

[0069]

[0070]

[0071] The preparation method of the clothing fragrance particle composition of Examples 1-3 comprises the following steps:

[0072] S1. Preparation of fragrance agent (acrylamide copolymer):

[0073] 15 g (3-acrylamidopropyl)trimethylammonium chloride, 25 g acrylamide, 7 g nonylphenol polyoxyethylene ether acrylate, and 5.7 g acrylic acid were added to 600 mL of water in sequence and stirred until dissolved. The pH of the solution was adjusted to 7 with a 30% sodium hydroxide solution. Under nitrogen protection, 14 mL of a 0.05 mol / L potassium persulfate solution was added. The mixture was heated to 65° C. and reacted for 30 h. The mixture was washed and filtered to obtain a fragrance agent.

[0074] S2. Preparation of adsorbent (fatty acid modified silica):

[0075] 1 g of silica was immersed in sufficient liquid lauric acid, ultrasonicated for 30 min, reacted at 80 °C for 1 h, centrifuged, washed, and dried at room temperature to obtain an adsorbent;

[0076] S3 according to the above parts by mass, the water-soluble particles, adsorbent, binder, flavoring agent, filler poured into the granulation device;

[0077] S4. The flavor and sufficient water are mixed to form a spray liquid, spray granulation, to obtain a pellet core, and drying;

[0078] S5. Prepare a coating liquid with excipients, adhesives, adjuvants and water, spray it on the surface of the pill core to form a coating layer, and then dry it to obtain a fragrance-retaining granule composition.

[0079] The difference between the comparative example and embodiment 2 is:

[0080] In Comparative Example 1, the acrylamide copolymer was replaced with acrylamide copolymer A, which was a binary copolymer of (3-acrylamidopropyl)trimethylammonium chloride and acrylamide (i.e., nonylphenol polyoxyethylene ether acrylate and acrylic acid were deleted from the acrylamide copolymer monomers in the embodiment, and the other components remained unchanged). The other components and preparation methods were the same. In Comparative Example 2, the fatty acid-modified silica was replaced with an equal mass of hexanoic acid-modified silica. The other components and preparation methods were the same. In Comparative Example 3, the coating layer was deleted, and only the pellet core structure was contained. The other components and preparation methods were the same.

[0081] Test Example 1

[0082] Fragrance retention test

[0083] 15 g of each of the fragrance-retaining particle compositions of Example 2 and Comparative Examples 1-3 were placed on pure cotton towels of the same specifications and put into a washing machine. The washing machine was adjusted to a mixed washing mode, and each of the towels was washed for 60 minutes.

[0084] After washing, 10 trained testers evaluated the fragrance concentration of the towels, with the fragrance concentration rated on a scale of 1-5. The higher the score, the better the fragrance retention of the product.

[0085] The testers scored the fragrance retention effect at each of the three evaluation points: freshly washed towels (point 1), dried towels (point 2), and two-week-old towels after rubbing them (point 3). The final test results were the average of the 10 testers' scores, as shown in Table 2 below.

[0086] Table 2 Fragrant effect scores of the samples of Example 2 and Comparative Examples 1-3 at different fragrance effect evaluation points

[0087]

[0088] The experimental results in Table 2 show that Example 2 scored significantly better than Comparative Examples 1-3. This demonstrates that the acrylamide copolymer used in Example 2, as a fragrance retention agent, can stabilize and slow the release of the fragrance, enhancing the fragrance's long-lasting aroma. In contrast, the fragrance in Comparative Example 1, which replaced the acrylamide copolymer, is highly volatile, resulting in a less persistent fragrance that gradually weakens over time. Comparative Example 2 uses caproic acid-modified silica as an adsorbent, which reduces its dispersion and adsorption properties, resulting in a decreased fragrance retention. Furthermore, Comparative Example 3 lacks a coating layer, resulting in the worst fragrance retention.

[0089] Test Example 2

[0090] Dissolution rate test

[0091] In a parallel experiment, a 1 L beaker was filled with water, and then 0.2 g of each sample of Example 2 and Comparative Examples 1-3 was weighed and placed in water separately. The time it took for the sample to completely dissolve was observed at a rotation speed of 1000 rpm. The results are shown in Table 3.

[0092] Table 3 Dissolution time of samples of Example 2 and Comparative Examples 1-3

[0093] sample Dissolution time (min) Example 2 4 Comparative Example 1 6 Comparative Example 2 6 Comparative Example 3 1

[0094] The experimental results in Table 3 show that Example 2 of the present invention has better solubility than the samples in the comparative examples. The substitution of the acrylamide copolymer in Comparative Example 1 reduced the solubility of the composition and prolonged the dissolution time of the fragrance beads. The substitution of modified silica in Comparative Example 2 also reduced its solubility. Comparative Example 3, lacking a coating layer, had the shortest dissolution time.

[0095] Test Example 3

[0096] Product stability testing

[0097] The samples of Example 2 and Comparative Examples 1-3 were placed in an oven at 0°C, a constant temperature of 25°C, and an oven at 45°C for one month, and then the samples were taken out and the color difference of the samples was observed with the naked eye. The experimental results are recorded as follows.

[0098] Table 4 Color difference records of samples of Example 2 and Comparative Examples 1-3

[0099] sample Samples at 0°C Samples at 25°C Samples at 45°C Example 2 No yellowing No yellowing Slight yellowing Comparative Example 1 Slight yellowing Slight yellowing Obvious yellowing Comparative Example 2 No yellowing Slight yellowing Slight yellowing Comparative Example 3 Slight yellowing Obvious yellowing Severe yellowing

[0100] The experimental results in Table 4 show that Example 2 has excellent stability and does not produce serious color changes. However, Comparative Example 1 replaces the acrylamide copolymer and Comparative Example 2 replaces the modified silica, resulting in reduced compatibility, dispersibility, and stability between the components. Comparative Example 3 does not contain a coating layer and is more susceptible to environmental conditions such as external temperature and is easily oxidized, resulting in the product being easily discolored at room temperature and high temperature.

[0101] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations that come within the meaning and range of equivalents of the claims be embraced therein.

[0102] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A clothing fragrance particle composition, characterized in that: The fragrance-retaining particle composition comprises: a pellet core and a coating layer wrapping the pellet core; The pellet core comprises the following components in parts by mass: 10-30 parts water-soluble granules 5-30 parts of adsorbent 2-15 parts of flavor 0.1-10 parts of fragrance 10-30 parts of adhesive 1-10 parts of filler; The coating layer comprises the following components in parts by weight: 1-10 parts of excipients Adhesive 0.01-5 parts 0.01-5 parts of additives; in, The fragrance retaining agent is an acrylamide copolymer; The comonomers of the acrylamide copolymer include (3-acrylamidopropyl)trimethylammonium chloride, acrylamide, nonylphenol polyoxyethylene ether acrylate, and acrylic acid; The adsorbent is lauric acid modified silica; The preparation method of the clothing fragrance particle composition comprises the following steps: S1. Preparation of fragrance: The comonomer is added into water, stirred until dissolved, the pH of the solution is adjusted, an initiator is added under the protection of nitrogen, heated for reaction, and purified to obtain a fragrance agent; S2. Preparation of adsorbent: Adding silica to liquid lauric acid, ultrasonically treating the solution, heating the solution for reaction, and purifying the solution to obtain an adsorbent; The mass ratio of (3-acrylamidopropyl)trimethylammonium chloride, acrylamide, nonylphenol polyoxyethylene ether acrylate, and acrylic acid in the comonomer is 10-20:5-30:5-10:1-15; The initiator is selected from one or more of ammonium persulfate and potassium persulfate; In step S1, the heating reaction temperature is 45-75°C and the time is 24-40 hours; in step S2, the heating reaction temperature is 70-90°C and the time is 0.5-3 hours.

2. The clothing fragrance particle composition according to claim 1, characterized in that The auxiliary agent is selected from one or more of pigments, cationic polymers and inorganic salts.

3. The clothing fragrance particle composition according to claim 1, characterized in that The fragrance is selected from one or more of liquid essences and microcapsule essences.

4. The clothing fragrance particle composition according to claim 1, characterized in that The excipient is selected from one or more of titanium dioxide, calcium carbonate powder, titanium dioxide powder, calcium silicate, silicon dioxide, kaolin, montmorillonite powder, and mica powder.

5. The clothing fragrance particle composition according to claim 1, characterized in that The preparation method of the clothing fragrance particle composition further comprises the following steps: S3. Pour the water-soluble particles, adsorbent, binder, fragrance agent, and filler into the granulation device; S4. The flavor and water are mixed to form a spray liquid, spray granulation, and dried to obtain pellet cores; S5. Excipients, adhesives and adjuvants are prepared to form a coating liquid, which is sprayed on the surface of the pellet core to form a coating layer, and then dried to obtain the clothing fragrance granule composition.

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