Granular fragrance composition for clothing and method for producing same

Abstract

The present invention relates to a fragrance granule composition for clothing, comprising a core and a coating layer covering the core. The core comprises the following components in parts by weight: water-soluble granules, adsorbent, essence, fragrance, adhesive, and filler. The coating layer comprises the following components in parts by weight: excipient and auxiliary agent. The fragrance granule composition for clothing of the present invention has an embedded structure and contains specific fragrances and adsorbents, which allows the essence to be fixed and released gradually. The particle size of the fragrance granules can be adjusted, which can suppress fragrance dissipation and achieve sustained fragrance delivery from the fragrance granules. The fragrance granule composition for clothing of the present invention also has a series of advantages, such as good solubility of the fragrance granules, good stability, and uniform appearance.

Description

[Technical Field]

[0001] The present invention relates to the technical field of fabric cleaning care, and in particular to a fragranced granular composition for clothing and a method for making the same. [Background technology]

[0002] Scent Booster, a product first released in 2011 and developed by Downy, a subsidiary of the American P&G Group, was introduced to the Chinese market by P&G China in 2017. After undergoing domestic improvements in 2019, it was upgraded to Version 2.0. This version of Scent Booster combines three functions: sterilization, dust mite removal, and stain removal. Its core ingredients remain aroma oils and fragrance microcapsules. Currently, there are two main requirements for Scent Booster: the ability to select the scent of Scent Booster according to personal preference, and the long-lasting scent, meaning the fragrance effect must last and not irritate the nose.

[0003] There are three main technical solutions for scent booster products currently available on the market. The first, relatively traditional solution, as described in Patent Documents 1-3, uses PEG (polyethylene glycol) as a carrier and melts the essence and PEG at high temperatures. However, the fragrance changes during the manufacturing process, affecting the fragrance stability of the product. The second solution, as described in Patent Documents 4-6, uses water-soluble granules as a carrier and coats the essence on the surface of the water-soluble granules. However, the essence remains exposed on the surface, which may result in some fragrance loss during storage or fragrance change due to high temperatures. The third solution, as described in Patent Document 7, provides a method for producing laundry detergent pellets. This improves scent booster manufacturing, but the core lacks fragrance and the coating layer is too thick, resulting in a low overall essence content and significantly reduced fragrance effectiveness.

[0004] As described above, in order to solve the problems existing in the prior art, it is necessary to design a fragrance composition that has a rational process, good product stability, good solubility, suppresses fragrance dissipation, and ultimately has an excellent and long-lasting fragrance effect. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] China Patent Publication No. 109652215 [Patent Document 2] China Patent Publication No. 113913250 [Patent Document 3] China Patent Publication No. 111286414 [Patent Document 4] China Patent Publication No. 110760395 [Patent Document 5] China Patent Publication No. 112522040 [Patent Document 6] China Patent Publication No. 112522039 [Patent Document 7] China Patent Publication No. 111748426 Summary of the Invention [Problem to be solved by the invention]

[0006] In view of the above, the present invention provides a fragrance granule composition for clothing to overcome the shortcomings of the prior art. This fragrance granule composition has an embedded structure, with the essence component embedded in the core and containing specific fragrance agents and adsorbents, which allows the essence to be fixed and released gradually. The particle size of the fragrance granules can be adjusted, which can prevent fragrance dissipation and achieve sustained fragrance delivery. The fragrance granule composition for clothing of the present invention also has a series of advantages, such as good solubility of the fragrance granules, good stability, and uniform appearance. [Means for solving the problem]

[0007] One object of the present invention is to provide a fragrance granule composition for clothing, the fragrance granule composition comprising a core and a coating layer covering the core, The core comprises the following parts by weight of ingredients: 10~30 parts of water-soluble granules 5 to 30 parts of adsorbent Essence 2-15 parts Flavoring agent 0.1 to 10 parts 10 to 30 parts adhesive Filler 1 to 10 parts The coating layer comprises the following components in parts by weight: 1 to 10 parts excipient 0.01 to 5 parts adhesive Auxiliary agent 0.01 to 5 parts the flavoring agent is selected from acrylamide copolymers; The comonomers of the acrylamide copolymer include (3-acrylamidopropyl)trimethylammonium chloride, acrylamide, nonylphenol polyoxyethylene ether acrylate, and acrylic acid; The adsorbent is fatty acid modified silica.

[0008] Furthermore, the auxiliary agent is one or more selected from the group consisting of dyes, cationic polymers, and inorganic salts.

[0009] The acrylamide copolymer has the function of fixing and releasing fragrance slowly, and also forms unique flocks with the solid granules in the detergent, which adhere the essence and deposit it on the fabric, allowing the essence's fragrance effect on the fabric to last longer.

[0010] Furthermore, the water-soluble granules are one or more selected from sucrose, glucose, fructose, maltose, dextrin, PEG, and sodium carbonate.

[0011] Furthermore, the essence is one or more types selected from a liquid essence and a microcapsule essence.

[0012] Among them, liquid essences are usually designed by essence manufacturers to meet consumer needs, using a mixture of oils or oil-soluble substances as solvents and water or water-soluble substances as solvents. Based on market research, the essence blend is adjusted to express the top note, middle note, and base note of the essence. In the fragrance granule composition of the present invention, the liquid essence contains one or two compositions of a water-soluble essence and an oil-soluble essence.

[0013] Microencapsulated essences are made by encapsulating raw materials such as essences and plant essential oils in special materials using modern scientific and technological means to form a microencapsulated emulsion. The encapsulating material may be selected from polyurea, polyurethane, and / or polyurea-polyurethane, preferably polyoxymethylene urea. Such systems include, but are not limited to, urea-formaldehyde and / or melamine-formaldehyde. After a product is treated with a fragrance, the fragrance retention time of the product can be significantly extended. During washing, the microencapsulated essence remains on the fibers of the clothing, and with the friction of the clothing, the fragrance microcapsules burst like bubbles, continuously releasing the fragrance.

[0014] Furthermore, the amount of the microcapsule essence added is 1 to 10 parts.

[0015] Furthermore, the amount of the liquid essence added is 1 to 10 parts.

[0016] Furthermore, the excipient is one or more selected from titanium dioxide powder, calcium carbonate powder, sub-titanium powder, calcium silicate, silica, kaolin, montmorillonite powder, and mica powder.

[0017] Furthermore, the amount of the adsorbent added is 2 to 20 parts.

[0018] Furthermore, the auxiliary agent may be selected from one or more mixtures of pigments, cationic polymers, and neutral inorganic salts to diversify the appearance and function of the fragrance granules, where the inorganic salt is an anhydrous crystalline salt, and may be selected from, but is not limited to, sodium chloride, potassium chloride, magnesium chloride, calcium chloride, sodium sulfate, potassium sulfate, magnesium sulfate, calcium carbonate, and calcium bicarbonate.

[0019] The cationic polymer may be selected from, but is not limited to, guar hydroxypropyltrimethylammonium chloride, gum arabic, ammonium polyphosphate, polyquaternary ammonium salt-6, polyquaternary ammonium salt-7, polyquaternary ammonium salt-10, polyquaternary ammonium salt-39, and polyquaternary ammonium salt-67.

[0020] Furthermore, the fatty acid is one or more selected from caprylic acid, nonanoic acid, capric acid, lauric acid, myristic acid, palmitic acid, and stearic acid.

[0021] Furthermore, the filler is one or more selected from the group consisting of hydrogen carbonate, carbonate, sulfate, nitrate, chloride, citrate, tartrate, acetate, and formate.

[0022] Furthermore, the adhesive is one or more selected from the group consisting of bentonite, starch glue, dextrin, polyvinyl alcohol, and hydroxypropylmethylcellulose.

[0023] Another object of the present invention is to provide a method for producing the fragrance granule composition for clothing, the method comprising the steps of: a fragrance preparation step S1 in which a comonomer is added to water, stirred until dissolved, the pH of the solution is adjusted, an initiator is added in a nitrogen gas atmosphere, the mixture is heated to react, and the resulting mixture is purified to obtain a fragrance; an adsorbent preparation step S2 in which silica is added to liquid fatty acid, ultrasonically treated, heated to react, and purified to obtain an adsorbent; Includes.

[0024] Furthermore, the comonomers are (3-acrylamidopropyl)trimethylammonium chloride, acrylamide, nonylphenol polyoxyethylene ether acrylate, and acrylic acid in a mass ratio of 10-20:5-30:5-10:1-15.

[0025] Furthermore, the initiator is one or more selected from ammonium persulfate and potassium persulfate.

[0026] Furthermore, the pH is 5 to 9.

[0027] Furthermore, in step S1, the reaction is carried out by heating at a temperature of 45 to 75°C for 24 to 40 hours, and in step S2, the reaction is carried out by heating at a temperature of 70 to 90°C for 0.5 to 3 hours.

[0028] moreover, Step S3: Putting the water-soluble granules, adsorbent, adhesive, flavoring agent, and filler into a granulation device; Step S4: Mixing the essence with water to form a spray liquid, spray granulating, and drying to obtain cores; Step S5: preparing a coating liquid containing excipients, adhesives, and auxiliaries, spraying the coating liquid on the surface of the core to form a coating layer, and drying the coating liquid to obtain the fragrance granule composition for clothing; Includes. [Effects of the Invention]

[0029] The effects of the present invention are as follows.

[0030] 1. The fragrance granule composition for clothing obtained by the present invention has a core-shell structure, and the core structure contains a fragrance obtained by copolymerizing four monomers: (3-acrylamidopropyl)trimethylammonium chloride, acrylamide, nonylphenol polyoxyethylene ether acrylate, and acrylic acid. The use of nonylphenol polyoxyethylene ether acrylate as a comonomer reduces surface tension, allowing for better contact between the fragrance and essence. Acrylamide can thicken the composition, improve adhesion, and increase the wetting of the fragrance in the fabric, preventing the evaporation and loss of fragrance molecules. The acrylic acid monomer introduces many carboxyl groups, further improving polarity, providing better compatibility with other components in the composition and more stable bonding with ingredients such as essence. Nonylphenol polyoxyethylene ether acrylate has a long chain structure and contains many oxygen-containing functional groups, making it easy to entangle and adsorb with essence molecules in the formulation and forming intermolecular forces between multiple components, thereby increasing stability and bonding strength and effectively improving sustained-release and fragrance performance. This quaternary copolymer has excellent water solubility and can improve the thermal stability of the composition, making it less likely to be deactivated at high temperatures. It can form unique flocks with the solid granules in the detergent, thereby depositing the essence on the fabric and achieving the effects of fragrance and sustained release. This allows the essence in the scent booster to penetrate well into the fibers, ensuring a sustained fragrance effect.

[0031] 2. The fragrance granule composition for clothing of the present invention uses fatty acid-modified silica as an adsorbent, which improves the dispersibility of silica, improves its thermal stability, and allows it to be dispersed more uniformly throughout the composition. Furthermore, the modified silica has a porous surface, allowing it to adsorb more essence. Furthermore, fatty acid-modified silica has better lipophilicity and is more compatible with fragrances, further improving the stability of the composition. The fragrance granule composition for clothing of the present invention promotes the aggregation of more essence on the surface of textile fibers, increasing the amount of essence deposited on clothing and significantly enhancing the fragrance effect. DETAILED DESCRIPTION OF THE INVENTION

[0032] In order to more clearly explain the technical solution of the present invention, the following examples are given. Unless otherwise specified, the raw materials, reaction and post-treatment means shown in the examples are all common raw materials on the market and technical means well known to those skilled in the art.

[0033] As used herein, the terms "preferred," "preferably," "more preferred," and the like refer to embodiments of the invention that may, in some circumstances, provide certain beneficial effects. However, other embodiments may also be preferred, under the same or other circumstances. Furthermore, the description of one or more preferred embodiments does not imply that other embodiments cannot be utilized, nor is it intended to exclude other embodiments from the scope of the invention.

[0034] Unless otherwise indicated, in any operating examples or otherwise, all numbers expressing quantities of ingredients and the like used in the specification and claims are to be understood as being modified in all instances by the term "about." Accordingly, the numerical parameters set forth in the following specification and appended claims are approximations that may vary depending upon the desired performance sought by the present invention, unless expressly indicated to the contrary.

[0035] In the specific implementation process, the granulation equipment mentioned is a relatively mature equipment available on the market.

[0036] The glucose used in the examples of the present invention is water-soluble granules, which was purchased from Shandong Liang New Materials Science and Technology Co., Ltd.

[0037] The liquid essence in the examples and comparative examples of the present invention was purchased from Chihuatong, and the brand was "Flower and Fruit Fragrance - Fresh Summer."

[0038] The microcapsule essence in the examples of the present invention was purchased from Chihuatong, and the brand was "Hanakakukou ~ Manmiao Shengzi".

[0039] In the examples of the present invention, precipitated calcium carbonate was purchased from Jiangxi Juxi Mining Co., Ltd. as a filler.

[0040] The starch paste in the examples of the present invention was purchased from Wanruida as an adhesive.

[0041] The bentonite used in the examples of the present invention was purchased from Xinyang Junxin Industrial Co., Ltd. as an adhesive.

[0042] In the examples of the present invention, titanium dioxide powder was purchased as an excipient from Jiangxi Tuoan New Materials Co., Ltd.

[0043] In the examples of the present invention, calcium carbonate powder was purchased as an excipient from Jiangxi Tuobang New Materials Co., Ltd.

[0044] The water-soluble dye in the examples of the present invention was BLUE HP and was purchased from Milliken.

[0045] In the examples of the present invention, (3-acrylamidopropyl)trimethylammonium chloride was purchased from Shanghai Yi'en Chemical Technology Co., Ltd.

[0046] The acrylamide in the examples of the present invention was purchased from TCI (Shanghai) Chemical Industry Development Co., Ltd.

[0047] The nonylphenol polyoxyethylene ether acrylate in the examples of the present invention is self-prepared, and the preparation method can be referred to the following literature: Zhang Fusheng, Liu Guoliang, Xu Xiaofang et al., Synthesis of Nonylphenol Polyoxyethylene Ether Acrylate Polymer and Its Interfacial Activity and Heavy Oil Viscosity Reducing Performance [J]. Journal of Donghua University [Natural Science Edition], 2020, 46(05): 747-753.

[0048] The acrylic acid, lauric acid, silica, and caproic acid used in the examples of the present invention were all purchased from TCI (Shanghai) Chemical Industry Development Co., Ltd.

[0049] The PVA adhesive in the examples of the present invention was purchased from TCI (Shanghai) Chemical Industry Development Co., Ltd.

[0050] Table 1 shows the components of the fragrance granule compositions for clothing of Examples 1 to 3 of the present invention and Comparative Examples 1 to 3 and the corresponding parts by mass.

[0051] [Table 1]

[0052] The method for producing the fragrance granule compositions for clothing according to Examples 1 to 3 includes the following steps. Flavoring agent (acrylamide copolymer) preparation step S1: 15 g of (3-acrylamidopropyl)trimethylammonium chloride, 25 g of acrylamide, 7 g of nonylphenol polyoxyethylene ether acrylate, and 5.7 g of acrylic acid were added sequentially to 600 mL of water and stirred until dissolved. The pH of the solution was adjusted to 7 with a 30% by mass sodium hydroxide solution, and 14 mL of a 0.05 mol / L potassium persulfate solution was added in a nitrogen gas atmosphere. The mixture was heated to 65°C and reacted for 30 hours, washed, and filtered to obtain a fragrance. Adsorbent (fatty acid modified silica) preparation step S2: 1 g of silica was immersed in a sufficient amount of liquid lauric acid, ultrasonicated for 30 minutes, reacted at 80°C for 1 hour, centrifuged, washed, and then dried at room temperature to obtain an adsorbent. Step S3: According to the above mass parts, the water-soluble granules, adsorbent, adhesive, flavoring agent, and filler were placed in a granulator. Step S4: The essence was mixed with a sufficient amount of water to form a spray liquid, and spray granulation was carried out to obtain cores, which were then dried. Step S5: A coating liquid containing excipients, adhesives, auxiliaries and water was prepared, sprayed onto the surface of the core to form a coating layer, and dried to obtain a scent booster granule composition.

[0053] The differences between the comparative example and Example 2 are as follows.

[0054] 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 removed from the monomers of the acrylamide copolymer in the Examples, and the remaining components were unchanged), but the other components and manufacturing method were the same. In Comparative Example 2, the fatty acid-modified silica was replaced with the same mass of caproic acid-modified silica, but the other components and manufacturing method were the same. In Comparative Example 3, the coating layer was removed, leaving only a core, but the other components and manufacturing method were the same.

[0055] Test example 1

[0056] Fragrance test

[0057] 15 g of each of the scented granule compositions of Example 2 and Comparative Examples 1 to 3 was placed on a pure cotton towel of the same specifications, which was then placed in a washing machine. The washing machine was set to a mixed wash mode and each towel was washed for 60 minutes.

[0058] After washing, 10 trained panelists rated the scent intensity of the towels on a scale of 1 to 5, with higher scores indicating stronger fragrance.

[0059] The evaluators rated the fragrance effect for each of the three evaluation items: freshly washed towels were rated as fragrance effect evaluation item 1, dried towels were rated as fragrance effect evaluation item 2, and towels that had been stored for two weeks and then rubbed were rated as fragrance effect evaluation item 3. The final test results were all average scores from the 10 evaluators, and the test results are shown in Table 2 below.

[0060] [Table 2]

[0061] From the experimental results in Table 2, Example 2 scores are clearly superior to Comparative Examples 1 to 3. This proves that by using an acrylamide copolymer as a fragrance in Example 2, the essence can be fixed and released gradually, enhancing the sustained fragrance effect of the essence. On the other hand, the essence in Comparative Example 1, in which an acrylamide copolymer was used instead, is highly volatile, and the fragrance of the fragrance does not last long and gradually weakens over time. When caproic acid-modified silica is used as an adsorbent as in Comparative Example 2, the dispersion and adsorption effects are reduced, resulting in a decrease in the fragrance effect of the fragrance. Comparative Example 3 does not include a coating layer, resulting in the lowest fragrance effect.

[0062] Test example 2

[0063] Dissolution Rate Test

[0064] In a parallel experiment, a 1 L beaker was filled with water, and then 0.2 g of each of the samples from Example 2 and Comparative Examples 1 to 3 was taken and placed in water alone at a rotation speed of 1000 rpm. The time it took for the sample to completely dissolve was observed. The results are shown in Table 3.

[0065] [Table 3]

[0066] The experimental results in Table 3 show that the sample of Example 2 of the present invention has better solubility than the comparative examples. Comparative Example 1, which replaced the acrylamide copolymer, reduced the solubility of the composition and extended the dissolution time of the scent booster. Comparative Example 2, which replaced modified silica, also reduced the dissolution ability. Comparative Example 3, which does not include a coating layer, had the shortest dissolution time.

[0067] Test example 3

[0068] Product Stability Testing

[0069] The samples of Example 2 and Comparative Examples 1 to 3 were left in a 0°C oven, a 25°C constant temperature oven, and a 45°C oven for one month, and then the samples were taken out and observed with the naked eye for changes in chromatic aberration. The experimental results are as follows:

[0070] [Table 4]

[0071] As can be seen from the experimental results in Table 4, Example 2 had excellent stability and did not undergo significant color change, but Comparative Example 1 replaced acrylamide copolymer, and Comparative Example 2 replaced modified silica, which reduced the compatibility, dispersibility, and stability between the components. Comparative Example 3 did not include a coating layer, and was therefore susceptible to environmental conditions such as outside temperature and prone to oxidation, making the product prone to discoloration at room temperature and high temperatures.

[0072] It will be apparent to those skilled in the art that the present invention is not limited to the details of the illustrative embodiments set forth above, and that the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. Therefore, in all respects, the embodiments are to be considered illustrative and not restrictive. The scope of the present invention is limited by the appended claims, rather than the foregoing description, and all changes that come within the meaning and range of equivalency of the claims are intended to be embraced therein.

[0073] Although this specification is described according to the embodiments, each embodiment does not necessarily include only one independent technical means. This description in this specification is for the purpose of clarity, and those skilled in the art should understand the specification as a whole, and the technical means in each embodiment may be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A fragrance granule composition for clothing comprising a core and a coating layer covering the core, The core comprises the following parts by weight of ingredients: 10-30 parts of water-soluble granules 5 to 30 parts adsorbent Essence 2 to 15 parts Flavoring agent 0.1 to 10 parts 10 to 30 parts adhesive Filler 1 to 10 parts The coating layer comprises the following components in parts by weight: 1 to 10 parts of excipient Adhesive 0.01 to 5 parts Auxiliary agent 0.01 to 5 parts the flavoring agent is an acrylamide copolymer; The comonomer of the acrylamide copolymer is (3-acrylamidopropyl)trimethyl Ammonium chloride, acrylamide, nonylphenol polyoxyethylene ether Contains teracrylate, acrylic acid, The adsorbent is fatty acid-modified silica, and the fatty acid is lauric acid; The fragrance granule composition for clothing, wherein the auxiliary is one or more selected from the group consisting of a dye, a cationic polymer, and an inorganic salt.

2. The essence is one selected from a liquid essence and a microcapsule essence. The fragrance granule composition for clothing according to claim 1, characterized in that it contains a plurality of types of fragrance.

3. The excipient may be selected from the group consisting of titanium dioxide powder, calcium carbonate powder, calcium silicate, silica, kaolin, montmorillonite powder, and mica powder. The fragrance granules for clothing according to claim 1, characterized in that the fragrance granules are one or more selected from the group consisting of: composition.

4. A method for producing the fragrance granule composition for clothing according to any one of claims 1 to 3, comprising: The comonomer was added to water and stirred until dissolved, the pH of the solution was adjusted, and the mixture was heated under a nitrogen gas atmosphere. a fragrance preparation step S1 in which an initiator is added, heated to react, and purified to obtain a fragrance; Silica is added to liquid fatty acid, ultrasonicated, heated to react, and purified to produce an adsorbent. an adsorbent preparation step S2; Including, A method for producing a fragrance granule composition for clothing, characterized in that the fatty acid is lauric acid.

5. The comonomer is (3-acrylamidopropyl)trimethylammonium chloride , acrylamide, nonylphenol polyoxyethylene ether acrylate, acrylate The mass ratio of the carboxylic acid to the carboxylic acid is 10-20:5-30:5-10:1-15. A method for producing the fragrance granule composition for clothing according to claim 4.

6. The initiator is one or more selected from ammonium persulfate and potassium persulfate.

5. A method for producing the fragrance granule composition for clothing according to claim 4,

7. In step S1, the temperature for the reaction by heating is 45 to 75°C, and the time is 24 to 40 h, and in step S2, the temperature for the reaction by heating is 70 to 90°C, and the time is The method for producing the fragrance granule composition for clothing according to claim 4, characterized in that the drying time is 0.5 to 3 hours. Law.

8. Step S3: Putting the water-soluble granules, adsorbent, adhesive, flavoring agent, and filler into a granulation device; The essence is mixed with water to form a spray solution, which is spray granulated and dried to form the cores. Step S4 of obtaining A coating liquid containing excipients, adhesives, and auxiliary agents is prepared and sprayed onto the surface of the core. Step S5 of forming a coating layer and drying it to obtain the fragrance granule composition for clothing; further comprising 5. The method for producing a fragrance granule composition for clothing according to claim 4, wherein the auxiliary is one or more selected from the group consisting of a dye, a cationic polymer, and an inorganic salt.

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