A long-lasting fragrance, a laundry composition containing the same and a method of preparation

Abstract

The present application relates to a kind of long-lasting fragrance, the laundry composition containing the fragrance and preparation method, belong to the technical field of laundry fragrance.Laundry composition includes the following components: surfactant, propylene glycol, glycerol, triethanolamine, ethylenediaminetetraacetic acid disodium, polyethylene glycol double stearate, citric acid, antibacterial agent, preservative, enzyme agent and fragrance.The present application is formed by modifying network structure of Chinese orange shrub fiber and chitosan, and the prepared adsorption particles can adsorb more fragrance, and the adsorption particles are formed by copolymerization with methyl acrylate and eugenol, forming a coating structure, which can well protect the fragrance, and the coating layer is slowly decomposed, has long-term stability, so that the laundry composition can last long.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of essence, and relates to a long-lasting fragrance essence, a laundry composition containing the essence and a preparation method. BACKGROUND

[0002] There are various types of laundry essence, including floral essence, fruit essence and the like. These essences can impart unique fragrance to laundry agents and are transmitted to clothes, so that the wearer can feel a pleasant atmosphere. High-end laundry agents also use natural plant-extracted essences, which are safe and harmless and bring natural fragrance. Secondly, essences not only add fragrance, but also have antibacterial and mildew-proof effects, inhibit the breeding of bacteria and mold, and protect the cleanliness of clothes. At the same time, essences can mask chemical odors and improve the use experience.

[0003] The chemical components of essence are mainly composed of alcohol, ether, aldehyde, ketone and ester aromatic compounds. However, since essence itself has the characteristics of being easy to volatilize and sensitive to light and heat, its fragrance persistence cannot be guaranteed when it is directly added to laundry liquid. SUMMARY

[0004] The purpose of the present application is to provide a long-lasting fragrance essence, a laundry composition containing the essence and a preparation method. The present application forms a network structure by modifying the fiber of Hippophae rhamnoides Linn and chitosan, and prepares adsorption particles to adsorb more essence. The adsorption particles form a coating layer structure by copolymerization with methyl acrylate and eugenol, which can well protect the essence. The coating layer decomposes slowly and has long-term stability, so that the laundry composition can last long.

[0005] The purpose of the present application can be achieved by the following technical solutions:

[0006] A preparation method of a long-lasting fragrance essence comprises the following steps:

[0007] 1) After ultrasonic mixing of modified Hippophae rhamnoides Linn fiber and chitosan solution, heating and stirring are carried out, and then cooling to room temperature, freeze-drying is carried out to obtain adsorption particles;

[0008] 2) The adsorption particles are placed in an ethanol aqueous solution, and after stirring treatment with essence, standing is carried out to obtain a pre-prepared solution;

[0009] 3) After mixing methyl acrylate and eugenol are added to the pre-prepared solution, an initiator is slowly added dropwise, heating reaction is carried out after dropwise addition is completed, cooling to room temperature is carried out, and then filtration and drying are carried out to obtain a long-lasting fragrance essence.

[0010] As a preferred technical scheme of the present application, in step 1), the ultrasonic mixing time is 8-10 min; the heating stirring is stirring for 2.5-3.0 h at 28-30℃; the mass ratio of the modified caragana fiber and the chitosan solution is 2-3:900; the chitosan solution is mixed by chitosan, deionized water and acetic acid in a ratio of 2.0-2.2 g:95-100 mL:2 mL.

[0011] As a preferred technical scheme of the present application, the degree of deacetylation of the chitosan is ≥95%; the chitosan is an amorphous polymer, and after the caragana fiber is introduced, it is converted into a crystalline polymer, and the increase of the crystallinity can enhance the stability of the adsorption particles.

[0012] As a preferred technical scheme of the present application, in step 2), the stirring treatment is stirring for 1.5-2.0 h at 500-600 r / min; the standing time is 45-60 min; the mass ratio of the adsorption particles, the ethanol aqueous solution and the essence is 20:50-60:2.5-3.0; the essence is one or more of orange oil essence, lily essence, lavender essence and rose essence.

[0013] As a preferred technical scheme of the present application, in step 3), the heating reaction is heating for 5-6 h at 70-75℃; the mass ratio of the pre-prepared solution, methyl acrylate, eugenol and initiator is 80:4-5:3-3.5:0.12-0.15; the initiator is one or both of benzoyl peroxide and azobis isobutyronitrile.

[0014] As a preferred technical scheme of the present application, the preparation method of the modified caragana fiber comprises the following steps: placing the caragana fiber in anhydrous ethanol, adding a coupling agent for stirring reaction, removing the filtrate, and washing and drying to obtain the modified caragana fiber.

[0015] As a preferred technical scheme of the present application, in the preparation of the modified caragana fiber, the mass ratio of the caragana fiber, the anhydrous ethanol and the coupling agent is 12-15:80-85:6-8; the stirring reaction is stirring for 6-8 h at 60-70℃; the coupling agent is vinyltrimethoxysilane.

[0016] As a preferred technical scheme of the present application, part of the hydroxyl groups on the surface of the caragana fiber are modified by vinyltrimethoxysilane, unsaturated carbon-carbon double bonds are introduced, so that the adsorption particles can participate in the subsequent polymerization reaction, and chemical bond connection is introduced, thereby increasing the binding force in the system.

[0017] The present application discloses a laundry composition containing a long-lasting fragrance, which comprises the following components in parts by weight:

[0018]

[0019] As a preferred technical scheme of the present application, the surfactant is mixed by cocamide propyl betaine, lauryl propyl amine oxide, coconut acid methyl monoethanolamide, isomeric alcohol polyoxyethylene ether in a mass ratio of 2:3-4:4.5-5.0:3.4-3.8.

[0020] As a preferred technical scheme of the present application, the amphoteric surfactant is compounded with the nonionic surfactant, and the content is controlled, so that the laundry composition obtains better softening effect and improves the high and low temperature stability.

[0021] As a preferred technical scheme of the present application, the enzyme agent is one or more of protease, lipase and amylase; the preservative is one or more of kathon, methyl isothiazolinone, 5-chloro-2-methyl-4-isothiazolin-3-one and 2-methyl-4-isothiazolin-3-one; and the antibacterial agent is one or more of silver ion antibacterial agent and plant extract.

[0022] The present application discloses a preparation method of a laundry composition, and the preparation method comprises the following steps:

[0023] S1, after mixing each raw material of the laundry composition, heating and stirring at 55-65 DEG C for 30-45 min, cooling to 40-50 DEG C and continuing to stir for 45-60 min, to obtain a liquid;

[0024] S2, the liquid is added to a laundry bead automatic packaging machine, and is packaged by using polyvinyl alcohol water-soluble film.

[0025] The present application has the following beneficial effects:

[0026] The present application forms a network structure by modifying the caragana fiber and chitosan, and prepares the adsorption particles to adsorb more essence, and the adsorption particles form a coating layer structure by copolymerization with methyl acrylate and eugenol, which can well protect the essence, the coating layer decomposes slowly, has long-term stability, and makes the laundry composition last long. DETAILED DESCRIPTION

[0027] In order to further illustrate the technical means and effects adopted by the present application to achieve the predetermined application purposes, the specific embodiments, structures, features and effects according to the present application are described in detail as follows in combination with examples.

[0028] Example 1

[0029] A long-lasting essence preparation method comprises the following steps:

[0030] 1) mixing the modified caragana fiber and the chitosan solution by ultrasonic mixing, then heating and stirring, cooling to room temperature, and freeze-drying to obtain the adsorption particles;

[0031] In step 1), the ultrasonic mixing time is 8 min; the heating and stirring is at 28℃ for 2.5 h; the mass ratio of the modified caragana fiber to the chitosan solution is 2:900; the chitosan solution is mixed by chitosan, deionized water and acetic acid in a ratio of 2.0 g:95 mL:2 mL;

[0032] 2) placing the adsorption particles in an ethanol aqueous solution, adding essence and stirring, and then standing to obtain a pre-prepared solution;

[0033] In step 2), the stirring is at 500 r / min for 1.5 h; the standing time is 45 min; the mass ratio of the adsorption particles, the ethanol aqueous solution and the essence is 20:50:2.5; the essence is orange oil essence;

[0034] 3) adding methyl acrylate and eugenol to the pre-prepared solution, slowly adding an initiator, and then heating to react, cooling to room temperature, filtering and drying to obtain the long-lasting fragrance essence;

[0035] In step 3), the heating reaction is at 70℃ for 5 h; the mass ratio of the pre-prepared solution, methyl acrylate, eugenol and the initiator is 80:4:3:0.12; the initiator is benzoyl peroxide;

[0036] The preparation method of the modified caragana fiber comprises the following steps: placing caragana fiber in anhydrous ethanol, adding a coupling agent and stirring to react, removing the filtrate, washing and drying to obtain the modified caragana fiber; in the preparation of the modified caragana fiber, the mass ratio of the caragana fiber, the anhydrous ethanol and the coupling agent is 12:80:6; the stirring is at 60℃ for 6 h; and the coupling agent is vinyltrimethoxysilane.

[0037] A laundry composition containing long-lasting fragrance essence comprises the following components by weight fraction:

[0038]

[0039] The surfactant is mixed by cocamide propyl betaine, lauramide propyl amine oxide, methyl monoethanolamide of coconut acid and isomeric alcohol polyoxyethylene ether in a mass ratio of 2:3:4.5:3.4; the enzyme agent is mixed by protease, lipase and amylase in a mass ratio of 1.5:1.2:1; and the antibacterial agent is silver lactate.

[0040] A preparation method of a laundry composition comprises the following steps:

[0041] S1, after mixing each raw material of the laundry composition, heating and stirring at 55℃ for 30 min, cooling to 40℃ and continuing to stir for 45 min, to obtain a liquid;

[0042] S2, adding the liquid into a laundry bead automatic packaging machine, and using polyvinyl alcohol water-soluble film for packaging, to obtain the product.

[0043] Example 2

[0044] A method for preparing a long-lasting fragrance includes the following steps:

[0045] 1) After ultrasonic mixing of the modified caragana fiber and chitosan solution, heating and stirring, cooling to room temperature, and freeze-drying, adsorbed particles are obtained;

[0046] In step 1), the ultrasonic mixing time is 9 min; the heating and stirring is at 29℃ for 2.8 h; the mass ratio of the modified caragana fiber and chitosan solution is 2.5:900; the chitosan solution is mixed by chitosan, deionized water and acetic acid in a ratio of 2.1g:98mL:2mL;

[0047] 2) After stirring treatment of the adsorbed particles in an ethanol aqueous solution and adding a fragrance, standing is performed to obtain a pre-prepared solution;

[0048] In step 2), the stirring treatment is at 550r / min for 1.8 h; the standing time is 52 min; the mass ratio of the adsorbed particles, the ethanol aqueous solution and the fragrance is 20:55:2.8; the fragrance is orange oil fragrance;

[0049] 3) After adding methyl acrylate and eugenol to the pre-prepared solution, slowly adding an initiator, heating reaction after the addition is completed, cooling to room temperature, filtering, and drying, a long-lasting fragrance is obtained;

[0050] In step 3), the heating reaction is at 72℃ for 5.5 h; the mass ratio of the pre-prepared solution, methyl acrylate, eugenol and initiator is 80:4.5:3.2:0.14; the initiator is benzoyl peroxide;

[0051] The preparation method of the modified caragana fiber includes the following steps: placing caragana fiber in anhydrous ethanol, stirring and reacting after adding a coupling agent, removing the filtrate, washing and drying, to obtain the product; in the preparation of the modified caragana fiber, the mass ratio of the caragana fiber, anhydrous ethanol and coupling agent is 14:82:7; the stirring and reacting is at 65℃ for 7 h; the coupling agent is vinyltrimethoxysilane.

[0052] A laundry composition containing a long-lasting fragrance includes the following components by weight fraction:

[0053]

[0054] The surfactant is mixed by cocamide propyl betaine, lauryl propyl amine oxide, coconut acid methyl monoethanolamide, isomeric alcohol polyoxyethylene ether in a mass ratio of 2:3.5:4.8:3.6; the enzyme agent is mixed by protease, lipase and amylase in a mass ratio of 1.5:1.2:1; the preservative is mixed by casson and methyl isothiazolinone in a mass ratio of 3:1; the antibacterial agent is silver lactate.

[0055] A preparation method of a laundry composition comprises the following steps:

[0056] S1, after mixing each raw material of the laundry composition, heating and stirring at 60 DEG C for 38 min, cooling to 45 DEG C and continuing to stir for 52 min, to obtain a liquid;

[0057] S2, the liquid is added to a laundry bead automatic packaging machine, and polyvinyl alcohol water-soluble film is used for packaging, to obtain the product.

[0058] Example 3

[0059] A preparation method of a long-lasting fragrance comprises the following steps:

[0060] 1) after ultrasonic mixing of the modified caragana fiber and chitosan solution, heating and stirring, cooling to room temperature, freeze-drying, to obtain adsorption particles;

[0061] In step 1), the ultrasonic mixing time is 10 min; the heating and stirring is at 30 DEG C for 3.0 h; the mass ratio of the modified caragana fiber and chitosan solution is 3:900; the chitosan solution is mixed by chitosan, deionized water and acetic acid in a ratio of 2.2g:100mL:2mL;

[0062] 2) the adsorption particles are placed in an ethanol aqueous solution, and after stirring treatment of the fragrance, standing, to obtain a pre-prepared solution;

[0063] In step 2), the stirring treatment is at 600r / min for 2.0h; the standing time is 60 min; the mass ratio of the adsorption particles, ethanol aqueous solution and fragrance is 20:60:3.0; the fragrance is orange oil fragrance;

[0064] 3) after adding methyl acrylate and eugenol to the pre-prepared solution, slowly adding initiator, after the completion of the dropwise addition, heating reaction, cooling to room temperature, filtering, drying, to obtain long-lasting fragrance;

[0065] In step 3), the heating reaction is heating at 75℃ for 6h; the mass ratio of the pre-prepared solution, methyl acrylate, eugenol and initiator is 80:5:3.5:0.15; the initiator is benzoyl peroxide;

[0066] The preparation method of the modified caragana fiber comprises the following steps: placing caragana fiber in anhydrous ethanol, adding a coupling agent for stirring reaction, removing the filtrate, and washing and drying to obtain the modified caragana fiber; in the preparation of the modified caragana fiber, the mass ratio of the caragana fiber, anhydrous ethanol and the coupling agent is 15:85:8; the stirring reaction is stirring at 70℃ for 8h; and the coupling agent is vinyltrimethoxysilane.

[0067] A laundry composition containing a long-lasting fragrance comprises the following components by weight fraction:

[0068]

[0069] The surfactant is mixed by cocamidopropyl betaine, lauramidopropylamine oxide, cocamide methyl monoethanolamide and isomeric alcohol polyoxyethylene ether according to the mass ratio 2:4:5.0:3.8; the enzyme agent is mixed by protease, lipase and amylase according to the mass ratio 1.5:1.2:1; the preservative is mixed by kathon and methyl isothiazolinone according to the mass ratio 3:1; and the antibacterial agent is silver lactate.

[0070] A preparation method of a laundry composition comprises the following steps:

[0071] S1, after mixing each raw material of the laundry composition, heating and stirring at 65℃ for 45min, cooling to 50℃ and continuing to stir for 60min to obtain a liquid;

[0072] S2, adding the liquid into a washing bead automatic packaging machine, and using polyvinyl alcohol water-soluble film for packaging to obtain the laundry composition.

[0073] Comparative Example 1

[0074] Comparative Example 1 is different from Example 2 in that caragana fiber is used instead of modified caragana fiber, and the rest of the components, preparation steps and parameters are consistent.

[0075] Comparative Example 2

[0076] Comparative Example 2 is different from Example 2 in that no modified caragana fiber is used, and the rest of the components, preparation steps and parameters are consistent.

[0077] Comparative Example 3

[0078] Comparative Example 3 is different from Example 2 in that allyl benzene is used instead of eugenol, and the rest of the components, preparation steps and parameters are consistent.

[0079] Comparative Example 4

[0080] Comparative Example 4 is different from Example 2 in that methyl acrylate is used instead of eugenol, and the rest of the components, preparation steps and parameters are consistent.

[0081] Fragrance retention test

[0082] 1. Test material: laundry compositions prepared in Examples 1-3 and Comparative Examples 1-4.

[0083] 2. Test method:

[0084] 100% pure cotton towels were selected, and the washed towels were naturally air-dried and placed for one month, and then the fragrance retention degree of the towels was evaluated, and the towels were kneaded during testing; the results are shown in Table 1.

[0085] Table 1

[0086]

[0087]

[0088] Among them, “+++” represents strong fragrance; “++” represents moderate fragrance; and “+” represents fragrance.

[0089] From the test results in Table 1, it can be seen that the fragrance retention effect of the laundry compositions prepared in Examples 1-3 is significantly better than that of Comparative Examples 1-4. This is because the network structure is formed by the hydrogen bond action of the modified caragana fiber and chitosan, which increases the stability of chitosan, and the surface of the prepared adsorption particles has abundant hydroxyl, carboxyl and amino groups to provide adsorption sites, which significantly improves the adsorption performance of the perfume. The adsorption particles have an unsaturated carbon-carbon double bond introduced by copolymerization with methyl acrylate and eugenol to form a coating layer structure, which can well protect the perfume, and the coating layer decomposes slowly and has long-term stability, so that the laundry composition has a long-lasting fragrance. The eugenol contains a hydroxyl group, which can form a hydrogen bond with the adsorption particles to improve the coating rate, and the eugenol also contains a stable phenyl group, which further improves the stability of the perfume microcapsule, thereby obtaining a laundry composition with fresh fragrance, high stability and long shelf life.

[0090] Stain removal test

[0091] According to the national standard GB / T13174-2008; the results are shown in Table 2.

[0092] Table 2

[0093] Carbon black stained cloth Egg protein stained cloth Sebum stained cloth Example 1 1.15 3.64 1.29 Example 2 1.17 3.62 1.30 Example 3 1.16 3.68 1.37

[0094] From the test results in Table 2, it can be seen that the laundry compositions prepared in Examples 1-3 have good detergency.

[0095] The above descriptions are only the preferred embodiments of the present application, and are not intended to limit the present application in any form. Although the present application has been disclosed as above with the preferred embodiments, it is not intended to limit the present application. Any person skilled in the art can make some changes or modifications to the above disclosed technical contents to make equivalent embodiments with equivalent changes, without departing from the technical solution of the present application. Any modification, change, equivalent change and modification of the above embodiments, which are made according to the technical essence of the present application, without departing from the technical solution of the present application, still belong to the scope of the technical solution of the present application.

Claims

1. A long-lasting fragrance, characterized in that, The preparation method of the long-lasting fragrance is as follows: 1) Modified Caragana korshinskii fiber and chitosan solution were ultrasonically mixed, heated and stirred, cooled to room temperature, and freeze-dried to obtain adsorbent particles; 2) The adsorbent particles were placed in an ethanol-water solution, and after adding fragrance and stirring, the solution was allowed to stand to obtain a pre-prepared solution. 3) After adding methyl acrylate and eugenol to the pre-prepared solution, the initiator is slowly added dropwise. After the addition is complete, the reaction is heated, cooled to room temperature, filtered, and dried to obtain a long-lasting fragrance. The modified Caragana korshinskii fiber is prepared by the following steps: Caragana korshinskii fiber is placed in anhydrous ethanol, a coupling agent is added and stirred to react, the filtrate is removed, and the fiber is washed and dried to obtain the modified Caragana korshinskii fiber. The chitosan solution is prepared by mixing chitosan, deionized water, and acetic acid in a ratio of 2.0-2.2g: 95-100mL: 2mL. The initiator is one or both of benzoyl peroxide and azobisisobutyronitrile; The coupling agent is vinyltrimethoxysilane.

2. The long-lasting fragrance according to claim 1, characterized in that: In step 1), the ultrasonic mixing time is 8-10 min; the heating and stirring is carried out at 28-30℃ for 2.5-3.0 h; and the mass ratio of the modified Caragana korshinskii fiber to the chitosan solution is 2-3:

900.

3. The long-lasting fragrance according to claim 1, characterized in that: In step 2), the stirring treatment is carried out at 500-600 r / min for 1.5-2.0 h; the settling time is 45-60 min; the mass ratio of the adsorbent particles, ethanol aqueous solution and fragrance is 20:50-60:2.5-3.0; the fragrance is one or more of orange oil fragrance, lily fragrance, lavender fragrance and rose fragrance.

4. The long-lasting fragrance according to claim 1, characterized in that: In step 3), the heating reaction is carried out at 70-75°C for 5-6 hours; the mass ratio of the pre-prepared solution, methyl acrylate, eugenol and initiator is 80:4-5:3-3.5:0.12-0.

15.

5. The long-lasting fragrance according to claim 1, characterized in that: In the preparation of the modified Caragana korshinskii fiber, the mass ratio of the Caragana korshinskii fiber, anhydrous ethanol and coupling agent is 12-15:80-85:6-8; the temperature of the stirring reaction is 60-70℃, and the stirring time is 6-8h.

6. A laundry composition comprising the long-lasting fragrance according to any one of claims 1 to 5, characterized in that, The following components are composed of parts by weight. composition: 60-70 parts of surfactant 12-16 parts of propylene glycol 6-8 parts glycerin 7-10 parts of triethanolamine Disodium ethylenediaminetetraacetate 0.5-0.8 parts Citric acid 0-1 part Antibacterial agent 0.6-1 part Preservative 0-0.1 parts Enzyme preparation 0.8-1.5 parts Long-lasting fragrance, 8-10 parts.

7. A laundry composition according to claim 6, characterized in that: The surfactant is composed of cocamidopropyl betaine, lauramide propylamine oxide, cocoyl methyl monoethanolamide, and isomeric alcohol polyoxyethylene ether in a mass ratio of 2:3-4:4.5-5.0:3.4-3.

8.

8. A laundry composition according to claim 6, characterized in that: The enzyme preparation is one or more of protease, lipase and amylase; the preservative is one or more of Kathon, methylisothiazolinone, 5-chloro-2-methyl-4-isothiazolin-3-one and 2-methyl-4-isothiazolin-3-one; the antibacterial agent is one or more of silver ion antibacterial agent and plant extract.

9. A method for preparing the laundry composition of claim 6, characterized in that, The method for preparing the laundry composition includes the following steps: S1. After mixing the components of the laundry composition, heat and stir at 55-65℃ for 30-45 minutes, then cool to 40-50℃ and continue stirring for 45-60 minutes to obtain the liquid. S2. Add the liquid to the automatic packaging machine for laundry detergent pods and seal it with a polyvinyl alcohol water-soluble film to obtain the product.

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