High-efficiency softener with lasting fragrance, preparation method and application thereof

Abstract

The invention discloses a high-efficiency softener capable of keeping fragrance for a long time as well as a preparation method and application of the high-efficiency softener capable of keeping fragrance for a long time. Comprising the following components: softened water, microcrystalline cellulose, propylene glycol, cationic imidazoline, an organosilicon emulsion, coconut oil, DMDM hydantoin, hydrogenated castor oil, diisocyanate, peroxide, acrylic acid, essence and essence microcapsules. According to the efficient softener disclosed by the invention, the essence microcapsules prepared by a special process are added, so that the fragrance retention time on clothes can be prolonged, the clothes are good in flexibility, and the stability of the efficient softener is good.

Description

Technical Field

[0001] The invention relates to the technical field of cleaning products, and in particular to a high-efficiency softener with long-lasting fragrance and a preparation method thereof. Background Art

[0002] Fabric softener, also known as fabric softener or clothing care agent, is a type of washing and care product. In the "Fabric Softener Industry Standard", it is defined as a washing and care product that is suitable for use with detergents in the fabric washing and care process to make the fabric soft, fluffy, and eliminate static electricity.

[0003] Consumers' demands for fabric softeners are becoming increasingly diversified and personalized. In addition to the basic softening effect, consumers also pay attention to the product's safety, environmental protection, fragrance, and special functions.

[0004] The effective content of traditional fabric softener is only about 5%, and about 90% is water. This brings unnecessary cost waste in transportation and packaging, and is not conducive to energy conservation and consumption reduction, water conservation and emission reduction; the fragrance of traditional fabric softener on clothes usually only lasts for 2-3 hours.

[0005] In concentrated softener products, in order to make the product have a better fragrance retention effect, the amount of fragrance added is generally more than 1%. Fragrance is a lipophilic substance. The higher the amount added, the more likely the product will have quality problems such as stratification.

[0006] Therefore, it is a technical problem that technicians in this field need to solve urgently to produce a softener that can make clothes soft, lastingly add fragrance, and not easily delaminate. Summary of the invention

[0007] The purpose of the present invention is to provide a high-efficiency softener with long-lasting fragrance, which can leave fragrance on clothes for a long time and the product is not easy to delaminate.

[0008] Furthermore, the present invention provides a method for preparing the above-mentioned high-efficiency softener with long-lasting fragrance.

[0009] Furthermore, the present invention also provides the use of the above-mentioned high-efficiency softener with long-lasting fragrance.

[0010] A long-lasting, highly effective fabric softener containing the following ingredients:

[0011] Softened water

[0012] Microcrystalline Cellulose

[0013] Propylene glycol

[0014] Cationic imidazoline

[0015] Silicone Emulsion

[0016] Coconut Oil

[0017] DMDM Hydantoin

[0018] Hydrogenated castor oil

[0019] Diisocyanates

[0020] peroxide

[0021] acrylic acid

[0022] essence

[0023] Fragrance microcapsules.

[0024] Preferably, the high-efficiency softener with long-lasting fragrance comprises the following components by weight: 250-300 parts of softened water;

[0025] 8-20 parts of microcrystalline cellulose;

[0026] Propylene glycol 20-30 parts;

[0027] Cationic imidazoline 20-30 parts;

[0028] 20-40 parts of silicone emulsion;

[0029] 4-6 parts coconut oil;

[0030] DMDM hydantoin 2-3 parts;

[0031] 10-15 parts of hydrogenated castor oil;

[0032] 20-50 parts of diisocyanate;

[0033] Peroxide 20-50 parts;

[0034] Acrylic acid 18-40 parts;

[0035] 15-20 parts of flavor;

[0036] 10-20 parts of flavor microcapsules.

[0037] More preferably, the high-efficiency softener with long-lasting fragrance comprises the following components in parts by weight:

[0038] 250 parts of softened water;

[0039] 20 parts of microcrystalline cellulose;

[0040] Propylene glycol 20 parts;

[0041] 30 parts of cationic imidazoline;

[0042] 40 parts of silicone emulsion;

[0043] 4 parts coconut oil;

[0044] DMDM hydantoin 2 parts;

[0045] 15 parts of hydrogenated castor oil;

[0046] 30 parts of diisocyanate;

[0047] Peroxide 30 parts;

[0048] Acrylic acid 18 parts;

[0049] 15 parts of flavor;

[0050] 20 portions of flavor microcapsules.

[0051] Wherein, the essence microcapsule is prepared by the following method:

[0052] Step (1) 10 parts by weight of essence is dissolved in 30 parts by weight of coconut oil, and 5 parts by weight of diisocyanate is added to prepare an oil phase solution;

[0053] Step (2) dissolving 2 parts by weight of acrylic acid in water, adding 0.5 parts by weight of peroxide as an initiator, to prepare an aqueous solution;

[0054] Step (3) mixing the oil phase and the water phase under stirring to form an emulsion, the reaction temperature is controlled at 60° C., and the reaction time is 1 hour;

[0055] Step (4) uses a centrifuge at 5000 rpm for 10 minutes to separate the flavor microcapsules from the reaction system, washes the separated flavor microcapsules with deionized water to remove unreacted monomers and solvent, and freeze-dries them at -40°C for 24 hours to obtain flavor microcapsules with a particle size of 100-200 μm.

[0056] The particle size of the microcrystalline cellulose is between 50 and 500 microns, the average particle size is 100 to 200 microns, and the specific surface area is greater than 1 m 2 / g. Microcrystalline cellulose, the particle size of which is between 50-500 microns, the average particle size is 100-200 microns, and the specific surface area is 1-10m 2 / g, has high crystal purity and good dispersibility, is insoluble in water, and can provide effective thickening and stabilizing effects. The preparation method can be: using wood pulp or other plant fibers as raw materials, obtaining microcrystalline cellulose through acid hydrolysis, post-treatment, neutralization and drying steps, and controlling the particle size between 50-500 microns through screening to ensure its thickening effect and stability in softeners.

[0057] Wherein, the cationic imidazoline is mixed with imidazole, coconut amine and stearic acid in a mass ratio of 1:1.5:0.67. It is generated by heating reaction. The generated cationic imidazoline has antistatic properties, excellent lubrication effect and the characteristics of enhancing fiber affinity. It can be selected from BASF SE, model: Dehyton ML.

[0058] Wherein, the organosilicon emulsion is prepared by the following method:

[0059] 35 wt% of polydimethylsiloxane (PDMS), 3 wt% of a nonionic emulsifier (such as Tween 80), 60 wt% of water, 1 wt% of xanthan gum, and 1 wt% of sodium polyacrylate are uniformly mixed to obtain a PDMS.

[0060] The emulsion has excellent stability, lubricity and softness, and is suitable for water-based softener formulations, and can improve the antistatic properties of softeners and the glossiness of fabrics. It can be selected from Maitu High-Tech Materials Group, model: Y-23179.

[0061] Wherein, the hydrogenated castor oil is prepared by the following method:

[0062] Castor oil and hydrogen are hydrogenated at a temperature of 180-220°C using a nickel catalyst, the degree of hydrogenation is controlled at 70%-95%, and the reaction time is 2-6 hours, and hydrogenated castor oil is finally obtained. Hydrogenated castor oil is made by hydrogenating castor oil (CastorOil) under the action of a nickel catalyst, with a degree of hydrogenation of 70%-95%, a melting point of 40-85°C, and has strong lubricity and thickening effects. It has the appearance of a white solid block or viscous liquid, and can be used to improve the emulsification, stability and lubricity of softener formulas;

[0063] The preparation method of hydrogenated castor oil includes: hydrogenating castor oil with hydrogen at a temperature of 180-220°C using a nickel catalyst, controlling the degree of hydrogenation at 70%-95%, and reacting for 2-6 hours to finally obtain hydrogenated castor oil. Hydrogenated castor oil is used in the formulation of water-based softener to improve the lubricity, antistatic properties and stability of the product.

[0064] Wherein, the peroxide is selected from one or more of hydrogen peroxide (H2O2), benzoyl peroxide, and sodium persulfite. Hydrogen peroxide (H2O2): used as an oxidant and bleaching agent to improve the cleaning effect of the formula. Benzoyl peroxide (Benzoyl Peroxide): used as a polymerization initiator and cross-linking agent, which can improve the stability and heat resistance of the formula. Sodium persulfate (Sodium Persulfate): used as a strong oxidant in the detergent formula to enhance the decontamination and bleaching effects of the product.

[0065] A method for preparing the above-mentioned high-efficiency softener with long-lasting fragrance comprises the following steps:

[0066] (1) Preparation of base solution:

[0067] Add 250-300 parts by weight of softened water into a stirring tank and heat to 40-50°C to dissolve the ingredients;

[0068] (2) Add dissolved water-soluble ingredients:

[0069] Add 8-20 parts by weight of microcrystalline cellulose and 20-30 parts by weight of propylene glycol to water. Microcrystalline cellulose helps to improve emulsification stability. Stir until completely dissolved to ensure a uniform solution.

[0070] (3) Add emulsifying ingredients:

[0071] Add 20-30 parts by weight of cationic imidazoline and 20-40 parts by weight of silicone emulsion to the mixture and continue stirring to ensure that the emulsion is evenly dispersed;

[0072] (4) Addition of essence microcapsules and oily ingredients:

[0073] Slowly add 10-20 parts by weight of flavor microcapsules and 4-6 parts by weight of coconut oil into the formula. The flavor microcapsules effectively improve the persistence of the fragrance, and the coconut oil can help improve the encapsulation effect of the microcapsules;

[0074] (5) Cross-linking reaction and stabilization:

[0075] Add 10-15 parts by weight of hydrogenated castor oil, and then add 20-50 parts by weight of diisocyanate and 18-40 parts by weight of acrylic acid to promote the crosslinking reaction and enhance the stability of the formula;

[0076] (6) Addition of peroxide:

[0077] Slowly add 20-50 parts by weight of hydrogen peroxide to promote the cross-linking reaction, enhance the oxidative stability, and ensure the lasting aroma;

[0078] (7) Final stirring and cooling:

[0079] Continue stirring the formula to ensure that all ingredients are evenly dispersed, and cool the mixture to room temperature to ensure that the product is stable and does not separate;

[0080] (8) pH adjustment and packaging:

[0081] Add 15-20 parts by weight of fragrance and 2-3 parts by weight of DMDM ​​hydantoin, check the pH value, and then adjust it to 4.5-5.5 with acrylic acid, and use it together with softener. The final product is packaged in a metering pump container to prevent the fragrance from volatilizing and ensure product stability.

[0082] An application method of the above-mentioned high-efficiency softener with long-lasting fragrance, which is used in conjunction with a metering pump. 8g of liquid is discharged by pressing one pump, and 2kg of clothes can be softened and scented.

[0083] Compared with the prior art, the high-efficiency softener with long-lasting fragrance of the present invention comprises the following ingredients: softened water, microcrystalline cellulose, propylene glycol, cationic imidazoline, silicone emulsion, coconut oil, DMDM ​​hydantoin, hydrogenated castor oil, diisocyanate, peroxide, acrylic acid, essence, and essence microcapsule. The high-efficiency softener of the present invention is added with essence microcapsule prepared by special process, which can increase the fragrance retention time on clothes, improve the softness of clothes, and improve the stability of the high-efficiency softener. DETAILED DESCRIPTION

[0084] In order to enable those skilled in the art to better understand the scheme of the present invention, the present invention is further described in detail below in conjunction with specific implementation methods.

[0085] The sources of materials used in the embodiments of the present invention are as follows:

[0086] Softened water: deionized water, commercially available;

[0087] Microcrystalline cellulose: FMC Corporation (USA), brand name: Particle size: 50-250μm, specific surface area>1m 2 / g.

[0088] Propylene glycol: Dow Chemical Company

[0089] Cationic imidazoline: BASF SE, model: Dehyton ML

[0090] Silicone emulsion: Momentive High-Tech Materials Group, Model: Y-23179

[0091] DMDM Hydantoin: Akzo Nobel, Model: DMDM ​​Hydantoin

[0092] Hydrogenated castor oil: BASF SE, model: CO 40

[0093] Fragrance, Givaudan Fragrances & Fragrances (Shanghai) Co., Ltd., Model: C50691

[0094] Fragrance microcapsules, Firmenich Fragrances (China) Co., Ltd., Model: PMC10C286

[0095] Coconut Oil:

[0096] Diisocyanate: IPDI, Evonik Industries AG, model: VESTANT TMDI;

[0097] Acrylic acid: commercially available; The Dow Chemical Company, USA;

[0098] Peroxide: Manufacturer: Akzo Nobel NV, model: Trigonox V388.

[0099] Examples and Comparative Examples

[0100] Preparation of flavor microcapsules:

[0101] Step (1), taking 10 parts by weight of essence, dissolving it in 30 parts by weight of coconut oil, and adding 5 parts by weight of diisocyanate to prepare an oil phase solution;

[0102] Step (2), dissolving 2 parts by weight of acrylic acid in water, adding 0.5 parts by weight of peroxide as an initiator, to prepare an aqueous solution;

[0103] Step (3), mixing the oil phase and the water phase under stirring to form an emulsion, the reaction temperature is controlled at 60° C., and the reaction time is 1 hour;

[0104] Step (4), using a centrifuge to separate the microcapsules to obtain flavor microcapsules with a particle size of 100-200 μm.

[0105] Prepare the materials according to Table 1, and then prepare the softener as follows:

[0106] (1) Preparation of base solution:

[0107] Add softened water to the mixing tank and heat to 40-50°C to facilitate dissolution of the ingredients;

[0108] (2) Add dissolved water-soluble ingredients:

[0109] Add microcrystalline cellulose and propylene glycol to water. Microcrystalline cellulose helps improve emulsion stability and avoid stratification. Stir until completely dissolved to ensure a uniform solution.

[0110] (3) Add emulsifying ingredients:

[0111] Add the cationic imidazoline and silicone emulsion to the mixture and continue stirring to ensure that the emulsion is evenly dispersed;

[0112] (4) Addition of essence microcapsules and oily ingredients:

[0113] Slowly add the flavor microcapsules and coconut oil into the formula. The flavor microcapsules effectively improve the persistence of the fragrance, and coconut oil can help improve the encapsulation effect of the microcapsules.

[0114] (5) Cross-linking reaction and stabilization:

[0115] Add hydrogenated castor oil, which helps stabilize the formula and prevent the fragrance from volatilizing;

[0116] Adding diisocyanate (such as IPDI) and acrylic acid to the formula promotes cross-linking reaction and enhances the stability of the formula;

[0117] (6) Addition of peroxide:

[0118] Slowly add hydrogen peroxide to promote cross-linking reaction, enhance oxidative stability and ensure long-lasting aroma;

[0119] (7) Final stirring and cooling:

[0120] Continue stirring the formula to ensure that all ingredients are evenly dispersed, and cool the mixture to room temperature to ensure that the formula is stable and does not separate;

[0121] (8) pH adjustment and packaging:

[0122] Add fragrance and DMDM ​​hydantoin, check the pH value, and then use acrylic acid to adjust to 4.5-5.5, which is suitable for softener use. The final product is packaged in a metered pump container to prevent the fragrance from volatilizing and ensure product stability.

[0123] Table 1 Softener raw materials and proportions

[0124] Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Softened water 250 280 300 700 680 400 450 400 500 Microcrystalline Cellulose 20 12 8 / / 10 / 12 8 Propylene glycol 20 30 25 / 30 20 30 30 25 Cationic imidazoline 30 25 20 20 25 30 25 25 20 Silicone Emulsion 40 30 20 30 30 40 30 30 20 Coconut Oil 4 6 5 4 6 7 6 6 5 DMDM Hydantoin 2 3 2.5 2 3 2 3 3 2.5 Hydrogenated castor oil 15 10 10 10 10 15 10 10 10 Diisocyanates 30 20 50 20 30 / 20 30 50 Hydrogen Peroxide 30 20 50 20 30 20 20 / 50 acrylic acid 18 25 40 18 25 40 18 25 40 essence 15 18 20 10 15 15 0 18 20 Fragrance microcapsules 20 18 10 0 0 10 0 18 10

[0125] The softeners prepared in the examples and comparative examples were subjected to performance tests.

[0126] 1. Fragrance test

[0127] Test samples: Examples and comparative examples and commercially available concentrated fragrance softeners

[0128] Test method: Fill the test sample into a press-type quantitative liquid dispensing fabric cleaning container, take 30*30cm2 identical towels and divide them into several groups, each group has 50 towels (total weight is about 2.1kg). Put the towels in the washing machine, take a pump of softener and put it into the washing machine tank to soften the clothes.

[0129] Fragrance test:

[0130] Subjects: 35 women aged 18 to 45, with no cold or other discomfort, unobstructed nasal cavity, no smoking, and no body odor.

[0131] Test method: The subjects are required to evaluate the fragrance of the clothes after being placed. If more than 50% of the subjects in each group evaluate that they can smell it, the test result is "smellable", otherwise it is "unsmellable".

[0132] 2. Softening effect (softness of fabric)

[0133] Test samples: Examples and comparative examples and commercially available concentrated fragrance softeners

[0134] Test method: (simulated hand washing)

[0135] (1) Amount of test substance: Add 2000 mL of clean water to a wash basin and pour 8 g of the test substance into the wash basin.

[0136] (2) Wear disposable gloves and stir thoroughly to ensure complete dissolution;

[0137] (3) After the test substance is fully dissolved, place three 100% cotton towels to be tested into the solution and soak them completely for 5 minutes; after 5 minutes, rub the fabric to be tested 10 times (5 times on the front and 5 times on the back).

[0138] (4) Take the towel to be tested out of the soaking solution, wring it out, and let it air dry at room temperature. Then put it in a storage box and label it.

[0139] (5) Fold the three dried towels in half twice and stack them up, then measure their height.

[0140] (6) Repeat the test twice using the same method and take the average height for calculation.

[0141] Results test:

[0142] Compare the height of towels after washing with the examples and commercially available concentrated fragrance-retaining softeners.

[0143] Test method: The measurement personnel confirm the test result by measuring the height. The test result is the higher range value.

[0144] 3. Emulsion stability test

[0145] The examples, comparative examples and commercial concentrated softener samples were placed in an oven at 50° C. for 30 days to observe the appearance of the samples and the time it takes for them to remain free of delamination.

[0146]

[0147]

[0148] It can be seen from the above data that the softener of the embodiment of the present invention has a fragrance retention time, softness of clothes after washing and stability that are significantly better than those of the comparative example and the commercially available concentrated fragrance-retaining softener.

[0149] The above description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but will conform to the widest scope consistent with the principles disclosed herein.

Claims

1. A long-lasting and highly effective softener, characterized in that Includes the following ingredients: Softened water Microcrystalline Cellulose Propylene glycol Cationic imidazoline Silicone Emulsion Coconut Oil DMDM Hydantoin Hydrogenated castor oil Diisocyanates peroxide acrylic acid essence Fragrance microcapsules.

2. The long-lasting and fragrant high-efficiency softener according to claim 1, characterized in that The composition comprises the following components by weight: 250-300 parts of softened water; 8-20 parts of microcrystalline cellulose; Propylene glycol 20-30 parts; Cationic imidazoline 20-30 parts; 20-40 parts of silicone emulsion; 4-6 parts coconut oil; DMDM hydantoin 2-3 parts; 10-15 parts of hydrogenated castor oil; 20-50 parts of diisocyanate; Peroxide 20-50 parts; Acrylic acid 18-40 parts; 15-20 parts of flavor; 10-20 parts of flavor microcapsules.

3. The high-efficiency softener with long-lasting fragrance as claimed in claim 2, characterized in that The composition comprises the following components by weight: 250 parts of softened water; 20 parts of microcrystalline cellulose; Propylene glycol 20 parts; Cationic imidazoline 30 parts; 40 parts of silicone emulsion; 4 parts coconut oil; DMDM hydantoin 2 parts; 15 parts of hydrogenated castor oil; 30 parts of diisocyanate; Peroxide 30 parts; Acrylic acid 18 parts; 15 parts of flavor; 20 portions of flavor microcapsules.

4. The high-efficiency softener with long-lasting fragrance as claimed in any one of claims 1 to 3, characterized in that The essence microcapsules are prepared by the following method: Step (1) 10 parts by weight of essence is dissolved in 30 parts by weight of coconut oil, and 5 parts by weight of diisocyanate is added to prepare an oil phase solution; Step (2) dissolving 2 parts by weight of acrylic acid in water, adding 0.5 parts by weight of peroxide as an initiator, to prepare an aqueous solution; Step (3) mixing the oil phase and the water phase under stirring to form an emulsion, the reaction temperature is controlled at 60° C., and the reaction time is 1 hour; Step (4) uses a centrifuge at 5000 rpm for 10 minutes to separate the flavor microcapsules from the reaction system, washes the separated flavor microcapsules with deionized water to remove unreacted monomers and solvent, and freeze-dries them at -40°C for 24 hours to obtain flavor microcapsules with a particle size of 100-200 μm.

5. The high-efficiency softener with long-lasting fragrance as claimed in any one of claims 1 to 3, characterized in that: The particle size of the microcrystalline cellulose is between 50 and 500 microns, the average particle size is 100 to 200 microns, and the specific surface area is greater than 1 m 2 / g.

6. The high-efficiency softener with long-lasting fragrance as claimed in any one of claims 1 to 3, characterized in that: The cationic imidazoline is prepared by mixing imidazole, coconut amine and stearic acid in a mass ratio of 1:1.5:0.

67.

7. The high-efficiency softener with long-lasting fragrance as claimed in any one of claims 1 to 3, characterized in that: The organosilicon emulsion is prepared by the following method: 35 wt% of polydimethylsiloxane, 3 wt% of nonionic emulsifier, 60 wt% of water, 1 wt% of xanthan gum and 1 wt% of sodium polyacrylate are uniformly mixed to obtain a product; The hydrogenated castor oil is prepared by the following method: Castor oil and hydrogen are subjected to hydrogenation reaction at a temperature of 180-220° C. using a nickel catalyst, the degree of hydrogenation is controlled at 70%-95%, and the reaction time is 2-6 hours, to finally obtain hydrogenated castor oil.

8. The high-efficiency softener with long-lasting fragrance as claimed in any one of claims 3, characterized in that: The peroxide is selected from one or more of hydrogen peroxide, benzoyl peroxide and sodium persulfite.

9. A method for preparing a high-efficiency softener with a long-lasting fragrance as claimed in any one of claims 1 to 8, characterized in that The following steps are involved: (1) Preparation of base solution: Add 250-300 parts by weight of softened water into a stirring tank and heat to 40-50°C to dissolve the ingredients; (2) Add dissolved water-soluble ingredients: Add 8-20 parts by weight of microcrystalline cellulose and 20-30 parts by weight of propylene glycol to water and stir until completely dissolved to ensure a uniform solution; (3) Add emulsifying ingredients: Add 20-30 parts by weight of cationic imidazoline and 20-40 parts by weight of silicone emulsion to the mixture and continue stirring to ensure that the emulsion is evenly dispersed; (4) Addition of essence microcapsules and oily ingredients: Slowly add 10-20 parts by weight of essence microcapsules and 4-6 parts by weight of coconut oil into the formula; (5) Cross-linking reaction and stabilization: Add 10-15 parts by weight of hydrogenated castor oil, and then add 20-50 parts by weight of diisocyanate and 18-40 parts by weight of acrylic acid to promote the crosslinking reaction and enhance the stability of the formula; (6) Addition of peroxide: Slowly add 20-50 parts by weight of hydrogen peroxide to promote the cross-linking reaction, enhance the oxidative stability, and ensure the lasting aroma; (7) Final stirring and cooling: Continue stirring the formula to ensure that all ingredients are evenly dispersed, and cool the mixture to room temperature to ensure that the product is stable and does not separate; (8) pH adjustment and packaging: Add 15-20 parts by weight of flavor and 2-3 parts by weight of DMDM ​​hydantoin, check the pH value, and then adjust it to 4.5-5.5 with acrylic acid. Package the final product in a metering pump container to prevent the flavor from volatilizing and ensure product stability.

10. A method for using the high-efficiency softener with long-lasting fragrance as claimed in any one of claims 1 to 8, characterized in that: Use with a metering pump, one pump will deliver 8g of liquid, which can soften and scent 2kg of clothes.

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