Clothing cleaning agent with efficient decontamination and protection functions and preparation method of clothing cleaning agent
By modifying the combination of butyl dieneate sulfonate and surfactant, the problem of insufficient permeability and anti-stain redeposition properties of traditional clothing cleaning agents is solved, and efficient decontamination and deep cleaning are achieved.
Patent Information
- Application Number
- CN202411235866.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-04
- Publication Date
- 2024-12-13
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
Traditional clothing cleaning agents have insufficient penetration and infiltration performance on clothing, and have poor anti-staining performance, making it difficult to meet the needs of modern families for efficient, environmentally friendly and multifunctional cleaning.
Modify the sulfonate group of butyl dienolate sulfonate by using a combination of modified butyl dienolate sulfonate, anionic surfactant, nonionic surfactant, mixed polymer, biological enzyme and solvent. The group and hydrophobic fluorophobic chains reduce water surface tension, enhance wetting performance, and improve decontamination efficiency through synergistic effects.
It significantly improves the permeability and dispersion of the cleaning agent, enhances the detergent effect, reduces the redeposition of stains, and provides a more thorough cleaning and deep cleaning effect.
Smart Images

Figure BDA0005027708960000031 
Figure BDA0005027708960000041 
Figure BDA0005027708960000061
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of detergent processing, and in particular to a highly efficient decontamination and protective clothing detergent and a preparation method thereof. Background Art
[0002] Clothes detergent is a cleaning product that can effectively remove various stains, oil stains, sweat stains and other impurities on clothes. With the improvement of living standards, consumers' demand for clothing cleaning and maintenance is increasing. Traditional laundry detergents such as washing powder and laundry liquid can no longer meet the modern family's demand for efficient, environmentally friendly and multi-functional cleaning.
[0003] A Chinese invention patent with publication number CN114196483A discloses a laundry detergent with decontamination and anti-staining functions and a preparation method thereof. The laundry detergent comprises fatty alcohol ether carboxylate, tridecanol ether, an anti-staining agent and water. By weight percentage, the content of fatty alcohol ether carboxylate is 3-10%, the content of tridecanol ether is 8-15%, and the content of the anti-staining agent is 2-8%. The laundry detergent of the patent has strong decontamination ability and good cleaning effect. It can effectively prevent the staining and color transfer of fabrics, does not contain difficult-to-degrade components, has mild performance, and is green and environmentally friendly.
[0004] The main ingredients of laundry detergents include surfactants, builders, stabilizers, brighteners, fragrances and enzymes. Surfactants are the core of laundry detergents and are used to reduce the surface tension of water, separate stains from the surface of clothes and form emulsions with the active components in the detergent to be suspended in water, thereby achieving the purpose of stain removal. However, the penetration and wetting performance of traditional laundry detergents on clothes needs to be further improved. The emulsion droplets formed when washing clothes with laundry detergents are easy to agglomerate to form larger emulsified particles, which are easy to attach to clothes again and are not easy to be washed off, forming secondary deposition, resulting in poor anti-stain redeposition performance of the detergent. The overall washing experience of using detergents to wash clothes needs to be further improved.
[0005] In view of the technical defects in this aspect, a solution is now proposed. Summary of the invention
[0006] The object of the present invention is to provide a highly efficient stain removal and protection clothing detergent and a preparation method thereof, so as to solve the technical problems in the prior art that the penetration and wetting performance of clothing by clothing detergents needs to be further improved and the anti-stain redeposition performance is poor.
[0007] The purpose of the present invention can be achieved through the following technical scheme: a highly efficient decontamination and protective clothing detergent, comprising the following components in parts by weight: 20-30 parts of modified dienoic acid butyl ester sulfonate, 20-30 parts of anionic surfactants, 30-35 parts of nonionic surfactants, 3-5 parts of mixed polymers, 2-3 parts of biological enzymes, 1-2 parts of washing aids and 35-45 parts of solvents.
[0008] Furthermore, the anionic surfactant is one or more combinations of sodium dodecylbenzene sulfonate, fatty acids, and sodium lauryl alcohol polyoxyethylene ether sulfate, and the nonionic surfactant is one or two of fatty alcohol polyoxyethylene ether, fatty alcohol alkoxy compounds, and alkyl glycosides.
[0009] Furthermore, the washing aid is one or more of potassium sulfite, triethanolamine, and monoethanolamine; the mixed polymer is composed of sodium polyacrylate, maleic acid-acrylic acid copolymer, and polyethyleneimine in a weight ratio of 2:1:1; the biological enzyme is one or more of protease, lipase, amylase, cellulase, and pectinase; and the solvent is composed of propylene glycol, glycerol, and polyethylene glycol in a weight ratio of 4:2:1.
[0010] Furthermore, the preparation method of modified dienoic acid butyl ester sulfonate is as follows: add modified dienoic acid butyl ester, isopropanol and tert-butyl perbenzoate into a reactor and stir, increase the temperature of the reactor to 50-60°C, add sodium bisulfite solution dropwise into the reactor, keep the reaction warm for 22-24 hours, and post-treat to obtain modified dienoic acid butyl ester sulfonate.
[0011] The synthetic reaction equation of modified dienoic acid butyl ester sulfonate is:
[0012]
[0013] The synthetic reaction mechanism of modified dienoic acid butyl ester sulfonate is:
[0014] Tert-butyl perbenzoate is used as a free radical initiator, which decomposes under heating conditions to generate free radicals to attack double bonds on modified dienoic acid butyl ester molecules, forming active free radicals on the modified dienoic acid butyl ester molecular chain. Sodium bisulfite is used as a sulfonating agent, and ferric chloride is used as a catalyst to promote the reaction of bisulfite ions with active free radicals on the modified dienoic acid butyl ester molecular chain, so that sulfonic acid groups are introduced into the modified dienoic acid butyl ester molecular chain. In the process of adjusting the pH value of the reaction system in post-treatment, the sulfonic acid groups react with sodium hydroxide to form sodium sulfonate on the molecular chain, so as to prepare modified dienoic acid butyl ester sulfonate.
[0015] Mass spectrometry analysis data are: m / z: 253.2042 (100.0%), 254.2075 (16.2%), 255.2109 (1.2%); elemental analysis: C, 71.10; H, 10.74; N, 5.53; O, 12.63.
[0016] Furthermore, the amount ratio of the modified dienoic acid butyl ester, isopropanol, tert-butyl perbenzoate and sodium bisulfite solution is 10g:30mL:0.5g:40g, the sodium bisulfite solution is composed of sodium bisulfite, ferric chloride and purified water in a weight ratio of 25:0.1:60, and the post-treatment comprises: after the reaction is completed, the temperature of the reactor is reduced to room temperature, sodium hydroxide solution is added dropwise to the reactor, the pH of the system is adjusted to 7-8, the reaction solution is washed with petroleum ether 3 times, the isopropanol and water mixture is transferred to a rotary evaporator with a water bath temperature of 70-80°C, the solvent is evaporated under reduced pressure, the water bath temperature is reduced to 55-60°C, anhydrous ethanol is added to the rotary evaporator, and the mixture is dispersed under normal pressure for 20-30min, filtered, and the filtrate is transferred to a rotary evaporator with a temperature of 55-60°C, and the solvent is evaporated under reduced pressure to obtain modified dienoic acid butyl ester sulfonate.
[0017] Furthermore, the preparation method of modified dienoic acid butyl ester is: add 12-aminododec-4,8-dienoic acid butyl ester, 3,3,4,4,5,5,6,6,6-nonafluorohexanoyl chloride, and N,N-dimethylformamide to a nitrogen-protected reactor and stir, add an acid binding agent to the reactor, react at room temperature for 6-8 hours, and post-treat to obtain modified dienoic acid butyl ester.
[0018] The synthetic reaction equation of modified dienoic acid butyl ester is:
[0019]
[0020] The synthetic reaction mechanism of modified dienoic acid butyl ester is:
[0021] Under the promotion of the acid-binding agent, the amino group on the 12-aminododec-4,8-dienoic acid butyl ester molecule undergoes a nucleophilic substitution reaction with the acyl chloride on the 3,3,4,4,5,5,6,6,6-nonafluorohexanoyl chloride molecule to form a modified dienoic acid butyl ester with a fluorine segment modified dodec-4,8-dienoic acid butyl ester.
[0022] Mass spectrometry analysis data are: m / z: 513.1925 (100.0%), 514.1959 (22.7%), 515.1993 (2.5%); elemental analysis: C, 49.12; H, 5.50; F, 33.30; N, 2.73; O, 9.35.
[0023] Furthermore, the amount ratio of the 12-aminododecane-4,8-dienoic acid butyl ester, 3,3,4,4,5,5,6,6,6-nonafluorohexanoyl chloride, N,N-dimethylformamide and acid binding agent is 1g:1.2g:7mL:0.4g, the acid binding agent is sodium bicarbonate, and the post-treatment comprises: after the reaction is completed, the temperature of the reactor is increased to 95-100°C, the low boiling point solvent is evaporated under reduced pressure, the temperature of the reactor is reduced to room temperature, anhydrous ethanol is added to the reactor, stirred and dispersed for 30-50min, filtered, and the filtrate is transferred to a rotary evaporator with a water bath temperature of 50-60°C, and ethanol is evaporated under reduced pressure to obtain modified dienoic acid butyl ester.
[0024] Furthermore, the preparation method of 12-aminododec-4,8-dienoic acid butyl ester is as follows: 12-aminododec-4,8-dienoic acid, n-butanol, toluene and a catalyst are added to a nitrogen-protected reactor and stirred, the temperature of the reactor is increased to 90-100° C., the reactor is kept warm for 6-8 hours, and 12-aminododec-4,8-dienoic acid butyl ester is obtained by post-treatment.
[0025] Furthermore, the amount ratio of the 12-aminododec-4,8-dienoic acid, n-butanol, toluene and catalyst is 5g:3g:20mL:0.5g, the catalyst is 80-90wt% sulfuric acid, and the post-treatment includes: after the reaction is completed, the temperature of the reactor is lowered to room temperature, purified water is added to the reactor, stirred for 20-30min, allowed to stand for separation, the organic phase is washed with purified water 3 times, dried with anhydrous sodium sulfate for 40-60min, filtered, and the filtrate is transferred to a rotary evaporator with a water bath temperature of 75-85°C, and the solvent is evaporated under reduced pressure to obtain 12-aminododec-4,8-dienoic acid butyl ester.
[0026] The synthetic reaction equation of 12-amino dodeca-4,8-dienoic acid butyl ester is:
[0027]
[0028] The synthetic reaction mechanism of 12-amino dodeca-4,8-dienoic acid butyl ester is:
[0029] Under the condition of concentrated sulfuric acid as a catalyst, the carboxyl group on 12-aminododec-4,8-dienoic acid and the hydroxyl group on n-butanol undergo esterification reaction under high temperature environment to prepare 12-aminododec-4,8-dienoic acid butyl ester.
[0030] Mass spectrometry analysis data are: m / z: 253.2042 (100.0%), 254.2075 (16.2%), 255.2109 (1.2%); elemental analysis: C, 71.10; H, 10.74; N, 5.53; O, 12.63.
[0031] A method for preparing a highly efficient decontamination and protective clothing detergent comprises the following steps: adding modified dienoic acid butyl ester sulfonate, anionic surfactant, nonionic surfactant, mixed polymer, biological enzyme, detergent aid and solvent into a reaction kettle in a weight proportion, stirring until the system is dissolved, standing to degas, and obtaining the clothing detergent.
[0032] Furthermore, the stirring speed of the reactor is 200-300 r / min, and the temperature of the reactor is 50-60°C.
[0033] The present invention has the following beneficial effects:
[0034] 1. The highly effective decontamination and protective clothing detergent of the present invention comprises a hydrophilic sulfonate group and a hydrophobic fluorinated hydrocarbon chain in the molecular structure of the prepared modified dienoic acid butyl ester sulfonate, which can spontaneously aggregate on the interface in water to form an ordered molecular layer, thereby significantly reducing the surface tension of water, making it easier for the detergent to penetrate into the tiny gaps in clothing fibers and come into close contact with the stains, thus laying a good foundation for the subsequent decontamination process. In addition, the hydrophobic fluorinated hydrocarbon chain part of the modified dienoic acid butyl ester sulfonate can interact with hydrophobic stains such as oil and sebum, and through intermolecular interactions such as van der Waals forces, the hydrophobic fluorinated hydrocarbon chain part of the modified dienoic acid butyl ester sulfonate can interact with hydrophobic stains such as oil and sebum, and can form an orderly molecular layer on the surface of the clothing. Use force to peel off the stains from the surface of the clothes. The sulfonate group is a strong hydrophilic group. Its presence significantly increases the solubility of modified dienoic acid butyl ester sulfonate in water. The hydrophilic sulfonate group allows these peeled stains to be stably dispersed in the aqueous solution to form tiny droplets or suspended particles to prevent them from redepositing on the clothes. This emulsification and dispersion effect greatly improves the decontamination efficiency of the detergent. Modified dienoic acid butyl ester sulfonate is used in combination with other surfactants, washing aids, biological enzymes and other components. The synergistic effect between these components can further enhance the decontamination effect of the detergent.
[0035] 2. The highly efficient decontamination and protective clothing detergent of the present invention, the anionic surfactant and the nonionic surfactant can reduce the surface tension of water, so that the clothing detergent can penetrate into the tiny gaps of clothing fibers. The modified dienoic acid butyl ester sulfonate is another anionic surfactant, and the sulfonate group in its molecular structure also enhances its wetting performance. When these anionic surfactants, nonionic surfactants and modified dienoic acid butyl ester sulfonate act together, the wetting effect of the detergent is further improved. The anionic surfactant and the nonionic surfactant can combine with the grease and protein in the stains through their hydrophobic groups, while the hydrophilic groups face the water phase to form a molecular film that wraps the stains, and the originally water-insoluble stains are dispersed into tiny droplets, which can be easily washed away by water. In addition, the anionic surfactant can also combine with ionic substances (such as calcium, magnesium ions, etc.) in the stains to form insoluble precipitates to prevent them from being redeposited on clothing. The enhancement of such permeability and dispersibility enables the detergent to remove stains more thoroughly and improve the cleaning effect.
[0036] 3. The high-efficiency stain removal and protective clothing detergent of the present invention, the long-chain structure in the polymer molecules of the mixed polymer can form a network or chain structure in the water, disperse the stain particles that may have originally gathered together, and prevent them from combining with each other to form larger particles. This dispersion effect helps the stain particles to be more evenly distributed in the washing liquid, thereby being easier to wash away. In addition, during the washing process, the dispersed stain particles may settle to the bottom of the washing container due to gravity. However, the presence of the mixed polymer can form a stable suspension layer to suspend the stain particles in the washing liquid, preventing the stains from being redeposited on the clothes during the washing process, thereby improving the anti-redeposition performance of the detergent. The biological enzyme can decompose stains such as grease and starch. The addition of the biological enzyme can further promote the decomposition of the stains and form a Into smaller emulsified particles, the main function of detergents such as potassium sulfite, triethanolamine, monoethanolamine, etc. in detergents is to adjust the pH value, so that the components in the laundry detergent are in the best working state and improve the decontamination efficiency. In addition, detergents can also combine with hard water components such as calcium and magnesium ions in the water to form soluble chelates, which prevent hard water ions from combining with surfactants to form precipitates, thereby maintaining the activity of the surfactant and ensuring that the cleaning effect is not affected by hard water. By optimizing the composition of the solvent, the fluidity and permeability of the detergent are improved. Detergents with good fluidity are more likely to spread on the surface of clothes and fully contact with stains, while detergents with strong permeability can more easily penetrate into the fibers of clothes to achieve a deep cleaning effect. The various substances in the laundry detergent work together to make the detergent perform well in removing stains. DETAILED DESCRIPTION
[0037] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0038] The sodium polyacrylate in this application is selected from Shandong Huantai County Jinlong Chemical Co., Ltd., with a molecular weight of 2000-5000; the maleic acid-acrylic acid copolymer is selected from Wuhan Huaxiang Kejie Biotechnology Co., Ltd.; the polyethyleneimine is selected from Shanghai Youen Chemical Co., Ltd., with a molecular weight of 1200, and the polyethylene glycol is selected from Zhengzhou Huixi Chemical Products Co., Ltd., with a molecular weight of 2000.
[0039] Example 1
[0040] This embodiment provides a method for preparing a highly efficient decontamination and protective clothing detergent, comprising the following steps:
[0041] S1. Preparation of modified dienoic acid butyl ester
[0042] Weigh: 50 g of 12-aminododec-4,8-dienoic acid, 30 g of n-butanol, 200 mL of toluene and 5 g of 80 wt% sulfuric acid, add them to a nitrogen-protected reactor and stir, raise the reactor temperature to 90 ° C, keep the reactor warm for 6-8 hours, lower the reactor temperature to room temperature, add 100 mL of purified water to the reactor, stir for 20 minutes, stand and separate the liquids, wash the organic phase with purified water 3 times, dry it with anhydrous sodium sulfate for 40 minutes, filter it, transfer the filtrate to a rotary evaporator with a water bath temperature of 75 ° C, and evaporate the solvent under reduced pressure to obtain 12-aminododec-4,8-dienoic acid butyl ester.
[0043] S2. Preparation of modified butyl diene acid
[0044] Weigh: 50 g of 12-aminododec-4,8-dienoic acid butyl ester, 60 g of 3,3,4,4,5,5,6,6,6-nonafluorohexanoyl chloride, and 350 mL of N,N-dimethylformamide, add them to a nitrogen-protected reactor and stir, add 20 g of sodium bicarbonate to the reactor, react at room temperature for 6 hours, raise the temperature of the reactor to 95°C, evaporate the low boiling point solvent under reduced pressure, lower the temperature of the reactor to room temperature, add 350 mL of anhydrous ethanol to the reactor, stir and disperse for 30 minutes, filter, transfer the filtrate to a rotary evaporator with a water bath temperature of 50°C, and evaporate ethanol under reduced pressure to obtain modified dienoic acid butyl ester.
[0045] S3, preparation of modified dienoic acid butyl ester sulfonate
[0046] Mix sodium bisulfite, ferric chloride and purified water in a weight ratio of 25:0.1:60 to obtain a sodium bisulfite solution for later use;
[0047] Weigh: 50 g of modified dienoic acid butyl ester, 150 mL of isopropanol and 2.5 g of tert-butyl perbenzoate are added to the reactor and stirred. The temperature of the reactor is raised to 50 ° C. 200 g of sodium bisulfite solution is added dropwise to the reactor. The reaction is kept warm for 22 hours. The temperature of the reactor is lowered to room temperature. Sodium hydroxide solution is added dropwise to the reactor to adjust the pH of the system to 7. After the reaction solution is washed 3 times with petroleum ether, the isopropanol and water mixture is transferred to a rotary evaporator with a water bath temperature of 70 ° C. The solvent is evaporated under reduced pressure, the water bath temperature is lowered to 55 ° C. 500 mL of anhydrous ethanol is added to the rotary evaporator, and the mixture is dispersed under normal pressure for 20 minutes. Filter, transfer the filtrate to a rotary evaporator at a temperature of 55 ° C., and evaporate the solvent under reduced pressure to obtain modified dienoic acid butyl ester sulfonate.
[0048] S4. Preparation of laundry detergent
[0049] Mixing sodium polyacrylate, maleic acid-acrylic acid copolymer and polyethyleneimine in a weight ratio of 2:1:1 to obtain a mixed polymer;
[0050] Propylene glycol, glycerol and polyethylene glycol are mixed uniformly in a weight ratio of 4:2:1 to obtain a solvent;
[0051] Weigh by weight: 20 parts of modified dienoic acid butyl ester sulfonate, 20 parts of sodium dodecylbenzene sulfonate, 30 parts of fatty alcohol polyoxyethylene ether, 3 parts of mixed polymer, 1 part of protease, 1 part of pectinase bioenzyme, 1 part of potassium sulfite and 35 parts of solvent, add into the reactor, raise the temperature of the reactor to 50°C, set the stirring speed to 200 r / min, stir until the system is dissolved, let stand to degas, and obtain a clothing detergent.
[0052] Example 2
[0053] This embodiment provides a method for preparing a highly efficient decontamination and protective clothing detergent, comprising the following steps:
[0054] S1. Preparation of modified dienoic acid butyl ester
[0055] Weigh: 50 g of 12-aminododec-4,8-dienoic acid, 30 g of n-butanol, 200 mL of toluene and 5 g of 85 wt% sulfuric acid, add them to a nitrogen-protected reactor and stir, raise the reactor temperature to 95 ° C, keep the reactor warm for 7 hours, lower the reactor temperature to room temperature, add 100 mL of purified water to the reactor, stir for 25 minutes, stand and separate the liquids, wash the organic phase with purified water 3 times, dry it with anhydrous sodium sulfate for 50 minutes, filter it, transfer the filtrate to a rotary evaporator with a water bath temperature of 80 ° C, and evaporate the solvent under reduced pressure to obtain 12-aminododec-4,8-dienoic acid butyl ester.
[0056] S2. Preparation of modified butyl diene acid
[0057] Weigh: 50 g of 12-aminododec-4,8-dienoic acid butyl ester, 60 g of 3,3,4,4,5,5,6,6,6-nonafluorohexanoyl chloride, and 350 mL of N,N-dimethylformamide, add them to a nitrogen-protected reactor and stir, add 20 g of sodium bicarbonate to the reactor, react at room temperature for 6-8 hours, raise the temperature of the reactor to 97°C, evaporate the low boiling point solvent under reduced pressure, lower the temperature of the reactor to room temperature, add 350 mL of anhydrous ethanol to the reactor, stir and disperse for 40 minutes, filter, transfer the filtrate to a rotary evaporator with a water bath temperature of 55°C, and evaporate ethanol under reduced pressure to obtain modified dienoic acid butyl ester.
[0058] S3, preparation of modified dienoic acid butyl ester sulfonate
[0059] Mix sodium bisulfite, ferric chloride and purified water in a weight ratio of 25:0.1:60 to obtain a sodium bisulfite solution for later use;
[0060] Weigh: 50 g of modified dienoic acid butyl ester, 150 mL of isopropanol and 2.5 g of tert-butyl perbenzoate are added to the reactor and stirred. The temperature of the reactor is raised to 55 ° C. 200 g of sodium bisulfite solution is added dropwise to the reactor. The reaction is kept warm for 23 hours. The temperature of the reactor is lowered to room temperature. Sodium hydroxide solution is added dropwise to the reactor to adjust the pH of the system to 7.5. After the reaction solution is washed 3 times with petroleum ether, the isopropanol and water mixture is transferred to a rotary evaporator with a water bath temperature of 75 ° C. The solvent is evaporated under reduced pressure, the water bath temperature is lowered to 57 ° C. 500 mL of anhydrous ethanol is added to the rotary evaporator, and the mixture is dispersed under normal pressure for 25 minutes. Filter, transfer the filtrate to a rotary evaporator at a temperature of 57 ° C., and evaporate the solvent under reduced pressure to obtain modified dienoic acid butyl ester sulfonate.
[0061] S4. Preparation of laundry detergent
[0062] Mixing sodium polyacrylate, maleic acid-acrylic acid copolymer and polyethyleneimine in a weight ratio of 2:1:1 to obtain a mixed polymer;
[0063] Propylene glycol, glycerol and polyethylene glycol are mixed uniformly in a weight ratio of 4:2:1 to obtain a solvent;
[0064] Weigh by weight: 25 parts of modified dienoic acid butyl ester sulfonate, 25 parts of fatty acids, 33 parts of fatty alcohol alkoxy compounds, 4 parts of mixed polymers, 1 part of lipase, 1 part of amylase, 0.5 parts of pectinase, 1.5 parts of triethanolamine and 40 parts of solvent, add into the reactor, raise the temperature of the reactor to 55°C, set the stirring speed to 250 r / min, stir until the system is dissolved, let stand to degas, and obtain a clothing detergent.
[0065] Example 3
[0066] This embodiment provides a method for preparing a highly efficient decontamination and protective clothing detergent, comprising the following steps:
[0067] S1. Preparation of modified dienoic acid butyl ester
[0068] Weigh: 50 g of 12-aminododec-4,8-dienoic acid, 30 g of n-butanol, 200 mL of toluene and 5 g of 90 wt% sulfuric acid, add them to a nitrogen-protected reactor and stir, raise the reactor temperature to 100 ° C, keep the reactor warm for 8 hours, lower the reactor temperature to room temperature, add 100 mL of purified water to the reactor, stir for 30 minutes, stand for separation, wash the organic phase with purified water 3 times, dry it with anhydrous sodium sulfate for 60 minutes, filter it, transfer the filtrate to a rotary evaporator with a water bath temperature of 85 ° C, and evaporate the solvent under reduced pressure to obtain 12-aminododec-4,8-dienoic acid butyl ester.
[0069] S2. Preparation of modified butyl diene acid
[0070] Weigh: 50 g of 12-aminododec-4,8-dienoic acid butyl ester, 60 g of 3,3,4,4,5,5,6,6,6-nonafluorohexanoyl chloride, and 350 mL of N,N-dimethylformamide, add them to a nitrogen-protected reactor and stir, add 20 g of sodium bicarbonate to the reactor, react at room temperature for 8 hours, raise the temperature of the reactor to 100°C, evaporate the low boiling point solvent under reduced pressure, lower the temperature of the reactor to room temperature, add 350 mL of anhydrous ethanol to the reactor, stir and disperse for 50 minutes, filter, transfer the filtrate to a rotary evaporator with a water bath temperature of 60°C, and evaporate ethanol under reduced pressure to obtain modified dienoic acid butyl ester.
[0071] S3, preparation of modified dienoic acid butyl ester sulfonate
[0072] Mix sodium bisulfite, ferric chloride and purified water in a weight ratio of 25:0.1:60 to obtain a sodium bisulfite solution for later use;
[0073] Weigh: 50 g of modified dienoic acid butyl ester, 150 mL of isopropanol and 2.5 g of tert-butyl perbenzoate are added to the reactor and stirred. The temperature of the reactor is raised to 60 ° C. 200 g of sodium bisulfite solution is added dropwise to the reactor. The reaction is kept warm for 24 hours. The temperature of the reactor is lowered to room temperature. Sodium hydroxide solution is added dropwise to the reactor to adjust the pH of the system to 8. After the reaction solution is washed 3 times with petroleum ether, the isopropanol and water mixture is transferred to a rotary evaporator with a water bath temperature of 80 ° C. The solvent is evaporated under reduced pressure, the water bath temperature is lowered to 60 ° C. 500 mL of anhydrous ethanol is added to the rotary evaporator, and the mixture is dispersed under normal pressure for 30 minutes. Filter, transfer the filtrate to a rotary evaporator at a temperature of 60 ° C., and evaporate the solvent under reduced pressure to obtain modified dienoic acid butyl ester sulfonate.
[0074] S4. Preparation of laundry detergent
[0075] Mixing sodium polyacrylate, maleic acid-acrylic acid copolymer and polyethyleneimine in a weight ratio of 2:1:1 to obtain a mixed polymer;
[0076] Propylene glycol, glycerol and polyethylene glycol are mixed uniformly in a weight ratio of 4:2:1 to obtain a solvent;
[0077] Weigh by weight: 30 parts of modified dienoic acid butyl ester sulfonate, 30 parts of sodium lauryl polyoxyethylene ether sulfate, 35 parts of fatty alcohol alkoxy compounds, 5 parts of mixed polymers, 1 part of protease, 1 part of cellulase, 1 part of pectinase bioenzyme, 2 parts of monoethanolamine and 45 parts of solvent, add into the reactor, raise the temperature of the reactor to 60°C, set the stirring speed to 300 r / min, stir until the system is dissolved, let stand to degas, and obtain a clothing detergent.
[0078] Comparative Example 1
[0079] The difference between this comparative example and Example 3 is that steps S1 to S3 are omitted and modified butyl diene sulfonate is not added in step S4.
[0080] Comparative Example 2
[0081] The difference between this comparative example and Example 3 is that no mixed polymer is added in step S4.
[0082] Comparative Example 3
[0083] The difference between this comparative example and Example 3 is that no anionic surfactant is added in step S4.
[0084] Performance Test:
[0085] With reference to the standard GB / T 13174-2021 "Determination of the detergency and cyclic washing performance of detergents for clothing", the cleaning agents prepared in Examples 1-3 and Comparative Examples 1-3 were tested for their decontamination values on carbon black oily cloth and sebum-stained cloth, their decontamination ratios relative to standard detergents, and their whiteness retention values after 20 cycles of washing. The specific test results are shown in Table 1 below.
[0086] Table 1-Performance test data of the sample
[0087]
[0088] Data analysis;
[0089] A comparative analysis of the data in Table 1 above shows that the clothes detergent prepared by the present invention has a decontamination value of 13.8, a decontamination ratio of 1.72, and a whiteness retention value of 98.2% for carbon black oily cloth, a decontamination value of 14.3, a decontamination ratio of 1.33, and a whiteness retention value of 98.7% for sebum-stained cloth, and all performance parameters are better than those of the comparative example, indicating that the present invention combines the prepared modified dienoic acid butyl ester sulfonate with anionic surfactants, nonionic surfactants, mixed polymers, biological enzymes, detergent aids, and solvents, and optimizes the dosage ratio of each component, which can not only effectively decontaminate carbon black oily cloth and sebum-stained cloth, but also improve the anti-stain redeposition performance of the detergent.
[0090] The above contents are merely examples and explanations of the structure of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the structure of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.
[0091] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0092] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to specific implementation methods. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.
Claims
1. A highly efficient decontamination and protective clothing detergent, characterized in that: The invention comprises the following components in parts by weight: 20-30 parts of modified dienoic acid butyl ester sulfonate, 20-30 parts of anionic surfactant, 30-35 parts of nonionic surfactant, 3-5 parts of mixed polymer, 2-3 parts of biological enzyme, 1-2 parts of washing aid and 35-45 parts of solvent.
2. The highly efficient decontamination and protective clothing detergent according to claim 1, characterized in that: The anionic surfactant is one or more combinations of sodium dodecylbenzene sulfonate, fatty acid, and sodium lauryl alcohol polyoxyethylene ether sulfate, and the nonionic surfactant is one or two of fatty alcohol polyoxyethylene ether, fatty alcohol alkoxy compounds, and alkyl glycosides.
3. The highly efficient decontamination and protective clothing detergent according to claim 1, characterized in that: The detergent aid is one or more of potassium sulfite, triethanolamine, and monoethanolamine; the mixed polymer is composed of sodium polyacrylate, maleic acid-acrylic acid copolymer, and polyethylene imine in a weight ratio of 2:1:1; the biological enzyme is one or more of protease, lipase, amylase, cellulase, and pectinase; and the solvent is composed of propylene glycol, glycerol, and polyethylene glycol in a weight ratio of 4:2:
1.
4. The highly efficient decontamination and protective clothing detergent according to claim 1, characterized in that: The preparation method of modified dienoic acid butyl ester sulfonate is as follows: modified dienoic acid butyl ester, isopropanol and tert-butyl perbenzoate are added into a reaction kettle and stirred, the temperature of the reaction kettle is increased to 50-60° C., sodium bisulfite solution is added dropwise into the reaction kettle, the reaction is carried out by heat preservation for 22-24 hours, and modified dienoic acid butyl ester sulfonate is obtained by post-treatment.
5. The highly efficient decontamination and protective clothing detergent according to claim 4, characterized in that: The usage ratio of the modified dienoic acid butyl ester, isopropanol, tert-butyl perbenzoate and sodium bisulfite solution is 10g:30mL:0.5g:40g, and the sodium bisulfite solution is composed of sodium bisulfite, ferric chloride and purified water in a weight ratio of 25:0.1:
60.
6. The highly efficient decontamination and protective clothing detergent according to claim 4, characterized in that: The preparation method of modified dienoic acid butyl ester is as follows: 12-aminododecyl-4,8-dienoic acid butyl ester, 3,3,4,4,5,5,6,6,6-nonafluorohexanoyl chloride and N,N-dimethylformamide are added into a nitrogen-protected reactor and stirred, an acid binding agent is added into the reactor, the reaction is carried out at room temperature for 6-8 hours, and the modified dienoic acid butyl ester is obtained by post-treatment.
7. The highly efficient decontamination and protective clothing detergent according to claim 6, characterized in that: The dosage ratio of the 12-aminododec-4,8-dienoic acid butyl ester, 3,3,4,4,5,5,6,6,6-nonafluorohexanoyl chloride, N,N-dimethylformamide and the acid binding agent is 1g:1.2g:7mL:0.4g, and the acid binding agent is sodium bicarbonate.
8. The highly efficient decontamination and protective clothing detergent according to claim 6, characterized in that: The preparation method of 12-aminododec-4,8-dienoic acid butyl ester is as follows: 12-aminododec-4,8-dienoic acid, n-butanol, toluene and a catalyst are added into a nitrogen-protected reactor and stirred, the temperature of the reactor is increased to 90-100° C., the reactor is kept warm for 6-8 hours, and 12-aminododec-4,8-dienoic acid butyl ester is obtained by post-treatment.
9. The highly efficient decontamination and protective clothing detergent according to claim 8, characterized in that: The usage ratio of the 12-aminododec-4,8-dienoic acid, n-butanol, toluene and catalyst is 5g:3g:20mL:0.5g, and the catalyst is 80-90wt% sulfuric acid.
10. A method for preparing a highly efficient decontamination and protective clothing detergent according to any one of claims 1 to 9, characterized in that: The preparation method of the highly efficient decontamination and protective clothing detergent comprises: adding modified dienoic acid butyl ester sulfonate, anionic surfactant, nonionic surfactant, mixed polymer, biological enzyme, washing aid and solvent into a reaction kettle according to weight proportion, stirring until the system is dissolved, standing to degas, and obtaining the clothing detergent.
Citation Information
Patent Citations
Laundry condensate bead containing alcohol ether solvent, and preparation method thereof
CN111088121A
