AES concentrated formula with high-activity components and preparation method of AES concentrated formula

Abstract

The invention discloses an AES concentrated formula with high-activity components and a preparation method of the AES concentrated formula. The invention discloses an AES (acrylonitrile-ethylene-propylene-diene monomer styrene) water-based detergent which comprises the following components in percentage by weight: 25%-35% of AES, 8%-12% of sodium n-alkyl benzene sulfonate, 5%-8% of alkyl glycoside, 4%-6% of cocamidopropyl betaine, 18%-28% of a composite chelating agent, 2%-4% of sodium chloride, 0.3%-0.5% of EDTA (Ethylene Diamine Tetraacetic Acid)-disodium, 0.5%-1% of sodium benzoate, 3%-5% of propylene glycol and the balance of deionized water. AES is used as a main surfactant, and forms a ternary compound system with sodium n-alkyl benzene sulfonate, alkyl glycoside and cocamidopropyl betaine. Through the synergistic effect of the surfactants of different ion types, the critical micelle concentration (CMC) and the micelle aggregation number are remarkably improved, so that the active ingredients can form a stable micelle structure at a lower concentration, and the dirt-removing power and the foaming performance are improved. Sodium tripolyphosphate, sodium pyrophosphate and sodium citrate form a composite chelating agent, the chelating capacity of the composite chelating agent on Ca < 2 + >, Mg < 2 + > and other metal ions is larger than or equal to 300 mgCaCO3 / g, the inhibition effect of hard water on a surfactant can be effectively eliminated, and the stability of the formula under different water quality conditions is enhanced.

Description

Technical Field

[0001] The present invention relates to the technical field of AES concentrated formulations, and specifically provides an AES concentrated formulation with high active ingredients and a preparation method thereof. Background Art

[0002] Sodium alcohol polyoxyethylene ether sulfate (AES) is an anionic surfactant widely used in the fields of detergents, cosmetics, etc., and has good detergency, emulsifying and foaming properties. However, traditional AES concentrated formulations have the following problems: First, the content of active ingredients is insufficient (usually the active matter content ≤ 70%), resulting in limited washing efficiency per unit volume; second, the stability of the formulation system is poor, and layering and turbidity are likely to occur at high temperatures or during long-term storage; third, the synergistic effect with other surfactants is insufficient, making it difficult to meet the requirements of high-end detergents for multifunctionality.

[0003] In the existing patent with the patent number CN101942082A, it specifically discloses a preparation method of powdered AES or AES mixture, which is achieved by physical concentration. However, this method has a significant defect, that is, the physical concentration process easily leads to a sudden increase in the viscosity of the system, thereby affecting the processing performance and challenging the production efficiency and cost control of the product. In addition, the stability of the formulation system and the synergistic effect between AES and other surfactants have not been deeply explored.

[0004] In the existing patent with the patent number CN112646166A, it specifically discloses a method for rapidly improving the dissolution performance of sodium alcohol polyoxyethylene ether sulfate, which is achieved by simple compounding. Although this method is easy to operate, it also has deficiencies. Simple compounding is difficult to achieve synergistic effects among various components, resulting in the comprehensive performance of the product not meeting expectations. In addition, the problem of poor stability of the formulation system has not been effectively solved.

[0005] In summary, the methods for improving the active ingredients of AES in the prior art have many deficiencies. Therefore, it is of great practical significance to develop an AES concentrated formulation with high activity, high stability and strong synergistic effect. Summary of the Invention

[0006] The purpose of the present invention is to provide an AES concentrated formulation with high active ingredients and a preparation method thereof to solve the problems raised in the above background art.

[0007] To achieve the above object, the present invention provides the following technical solution: An AES concentrated formula with high active ingredients, comprising by weight percentage: 25%-35% of AES, 8%-12% of linear alkylbenzene sulfonate, 5%-8% of alkyl polyglycoside, 4%-6% of cocamidopropyl betaine, 18%-28% of composite chelating agent, 2%-4% of sodium chloride, 0.3%-0.5% of disodium EDTA, 0.5%-1% of sodium benzoate, 3%-5% of propylene glycol, and the balance of deionized water.

[0008] Preferably, it comprises by weight percentage: 28.0% of AES, 10.0% of linear alkylbenzene sulfonate, 6.0% of alkyl polyglycoside, 5.0% of cocamidopropyl betaine, 20% of composite chelating agent, 3.0% of sodium chloride, 0.4% of disodium EDTA, 4.0% of propylene glycol, 0.8% of sodium benzoate, and the balance of deionized water.

[0009] Preferably, it comprises by weight percentage: 32.0% of AES, 9.0% of linear alkylbenzene sulfonate, 7.0% of alkyl polyglycoside, 4.5% of cocamidopropyl betaine, 23.5% of composite chelating agent, 2.5% of sodium chloride, 0.35% of disodium EDTA, 5.0% of propylene glycol, 0.6% of sodium benzoate, and the balance of deionized water.

[0010] Preferably, the number of moles of ethylene oxide added in the AES molecule is 3-5.

[0011] Preferably, the composite chelating agent comprises: sodium tripolyphosphate, sodium pyrophosphate and sodium citrate, and the mass ratio of sodium tripolyphosphate, sodium pyrophosphate and sodium citrate is: 10-18:5-8:3-5.

[0012] A preparation method of an AES concentrated formula with high active ingredients, comprising the following steps:

[0013] Step 1, raw material pretreatment: Crush, mix and dry sodium tripolyphosphate, sodium pyrophosphate and sodium citrate, and weigh AES, linear alkylbenzene sulfonate, alkyl polyglycoside and cocamidopropyl betaine for melting to obtain a molten surfactant mixture for standby;

[0014] Step 2, mixing reaction: Add deionized water to the reaction kettle, stir, and sequentially add the pretreated composite chelating agent and molten surfactant mixture; add propylene glycol and disodium EDTA and stir again; adjust the pH of the system with sodium hydroxide solution, add sodium chloride for viscosity adjustment, and finally add sodium benzoate and essence, and stir evenly to obtain a reaction solution;

[0015] Step 3, post-treatment: Age the reaction solution, filter it through a 100-mesh filter cloth to obtain a clear and transparent AES concentrated solution;

[0016] Step 4. Performance test: Test the detergency, foam performance and stability of the obtained clear and transparent AES concentrate.

[0017] Preferably, in step 1, 10%-18% of sodium tripolyphosphate, 5%-8% of sodium pyrophosphate, and 3%-5% of sodium citrate are crushed to 80-100 mesh, mixed evenly and then added to a high-speed dispersion kettle, and dried at 60-70°C for 30 minutes; Weigh AES, linear alkylbenzene sulfonate, alkyl polyglycoside, and cocamidopropyl betaine, heat to 50-55°C to melt, and obtain a molten surfactant mixture for standby.

[0018] Preferably, in step 2, deionized water is added to the reaction kettle, the stirring is started, and the rotation speed is 200-300 r / min. The pretreated composite chelating agent and the molten surfactant mixture are added in sequence, and the reaction is carried out at 45-50°C for 40 minutes; 3%-5% of propylene glycol and 0.3%-0.5% of EDTA disodium are added, the stirring speed is adjusted to 150-200 r / min, and the reaction is carried out under insulation for 20 minutes; The pH of the system is adjusted to 7.0-7.5 with 30% sodium hydroxide solution, sodium chloride is added for viscosity adjustment, and finally 0.5%-1% of sodium benzoate and 0.1-0.3% of essence are added, and stirred evenly to obtain a reaction solution.

[0019] Preferably, in step 3, the reaction solution is aged at 25-30°C for 24 hours and filtered through a 100-mesh filter cloth to obtain a clear and transparent AES concentrate.

[0020] Compared with the prior art, the beneficial effects of the present invention are:

[0021] 1. The multi-surfactant synergistic system AES is used as the main surfactant to form a ternary compound system with linear alkylbenzene sulfonate, alkyl polyglycoside, and cocamidopropyl betaine. Through the synergistic effect of surfactants of different ionic types, the critical micelle concentration (CMC) and micelle aggregation number are significantly increased, so that the active ingredients can form a stable micelle structure at a lower concentration, thereby improving the detergency and foaming performance.

[0022] 2. The chelating co-builder system is composed of sodium tripolyphosphate, sodium pyrophosphate and sodium citrate to form a composite chelating agent, and the chelating ability for metal ions such as Ca 2+ and Mg 2 + is ≥ 300 mgCaCO3 / g, which can effectively eliminate the inhibitory effect of hard water on surfactants and enhance the stability of the formulation under different water quality conditions.

[0023] 3. The rheology control technology adjusts the system viscosity through sodium chloride (the viscosity is controlled at 1000 - 1500 mPa·s at 25°C), propylene glycol is used as a solvent to reduce the crystallization tendency of AES, and disodium EDTA inhibits the oxidative degradation caused by metal ions, jointly ensuring the processing performance and storage stability of the formulation. Description of the Drawings

[0024] Figure 1 is the flowchart of the preparation method of the present invention. Detailed Embodiments

[0025] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without making creative efforts shall fall within the protection scope of the present invention.

[0026] Please refer to Figure 1 , the present invention provides an AES concentrated formulation with high active ingredients, including by weight percentage: 25% - 35% of AES, 8% - 12% of linear alkylbenzene sulfonate, 5% - 8% of alkyl polyglycoside, 4% - 6% of cocamidopropyl betaine, 18% - 28% of composite chelating agent, 2% - 4% of sodium chloride, 0.3% - 0.5% of disodium EDTA, 0.5% - 1% of sodium benzoate, 3% - 5% of propylene glycol, and the balance of deionized water.

[0027] Preferably, the number of moles of ethylene oxide added in the AES molecule is 3 - 5.

[0028] Preferably, the composite chelating agent includes: sodium tripolyphosphate, sodium pyrophosphate, and sodium citrate, and the mass ratio of sodium tripolyphosphate, sodium pyrophosphate, and sodium citrate is: 10 - 18:5 - 8:3 - 5.

[0029] A preparation method of an AES concentrated formulation with high active ingredients includes the following steps:

[0030] Step 1. Raw material pretreatment: Crush 10% - 18% of sodium tripolyphosphate, 5% - 8% of sodium pyrophosphate, and 3% - 5% of sodium citrate to 80 - 100 mesh, mix them evenly and add them to a high-speed dispersion kettle, and dry for 30 minutes at 60 - 70°C; weigh AES, linear alkylbenzene sulfonate, alkyl polyglycoside, and cocamidopropyl betaine, heat them to 50 - 55°C to melt, and obtain a molten surfactant mixture for standby;

[0031] Step 2. Mixing reaction: Add deionized water into the reactor, start stirring at a speed of 200 - 300 r / min, and successively add the pretreated composite chelating agent and the molten surfactant mixture. Keep the temperature at 45 - 50 °C and react for 40 minutes; add 5% propylene glycol and 0.35% disodium EDTA, adjust the stirring speed to 150 - 200 r / min, and keep the temperature for reaction for 20 minutes; adjust the pH of the system to 7.0 - 7.5 with 30% sodium hydroxide solution, add sodium chloride for viscosity adjustment, and finally add 0.6% sodium benzoate and 0.1 - 0.3% essence, stir evenly to obtain the reaction solution;

[0032] Step 3. Post-treatment: Age the reaction solution at 25 - 30 °C for 24 hours, and filter it through a 100-mesh filter cloth to obtain a clear and transparent AES concentrate;

[0033] Step 4. Performance test: Test the detergency, foam performance and stability of the obtained clear and transparent AES concentrate.

[0034] Example 1:

[0035] A preparation method of an AES concentrate formula with high active ingredients, comprising the following steps:

[0036] Step 1. Raw material pretreatment: Crush 12% sodium tripolyphosphate, 6% sodium pyrophosphate and 4% sodium citrate to 80 - 100 mesh, mix evenly and add them to a high-speed dispersion kettle, and dry at 65 °C for 30 minutes; weigh 28% AES, 10% linear alkylbenzene sulfonate, 6% alkyl polyglycoside and 5% cocamidopropyl betaine, heat to 50 - 55 °C to melt to obtain a molten surfactant mixture for standby;

[0037] Step 2. Mixing reaction: Add deionized water into the reactor, start stirring at a speed of 200 - 300 r / min, and successively add the pretreated composite chelating agent and the molten surfactant mixture. Keep the temperature at 45 °C and react for 40 minutes; add 4% propylene glycol and 0.4% disodium EDTA, adjust the stirring speed to 150 - 200 r / min, and keep the temperature for reaction for 20 minutes; adjust the pH of the system to 7.2 with 30% sodium hydroxide solution, add sodium chloride for viscosity adjustment, and finally add 0.8 sodium benzoate and 0.1 - 0.3% essence, stir evenly to obtain the reaction solution;

[0038] Step 3. Post-treatment: Age the reaction solution at 25 - 30 °C for 24 hours, and filter it through a 100-mesh filter cloth to obtain a clear and transparent AES concentrate with an active matter content of 38.5%, a viscosity of 1200 mPa·s at 25 °C, and no delamination phenomenon after 3 months of accelerated aging test at 50 °C.

[0039] Example 2:

[0040] A preparation method of an AES concentrated formula with high active ingredients, comprising the following steps:

[0041] Step 1, raw material pretreatment: Crush 13% of sodium tripolyphosphate, 7% of sodium pyrophosphate, and 3.5% of sodium citrate to 80-100 mesh, mix evenly and add to a high-speed dispersion kettle, and dry at 65°C for 30 minutes; Weigh 32% of AES, 9% of linear alkylbenzene sulfonate, 7% of alkyl polyglycoside, and 4.5% of cocamidopropyl betaine, heat to 50-55°C to melt, and obtain a molten surfactant mixture for standby;

[0042] Step 2, mixing reaction: Add deionized water to the reaction kettle, start stirring at a speed of 200-300 r / min, and sequentially add the pretreated composite chelating agent and molten surfactant mixture, and keep the temperature at 45°C for reaction for 40 minutes; Add 5% of propylene glycol and 0.35% of EDTA disodium, adjust the stirring speed to 150-200 r / min, and keep the temperature for reaction for 20 minutes; Adjust the pH of the system to 7.2 with 30% sodium hydroxide solution, add sodium chloride for viscosity adjustment, and finally add 0.6% of sodium benzoate and 0.1-0.3% of essence, stir evenly to obtain a reaction solution;

[0043] Step 3, post-treatment: Age the reaction solution at 25-30°C for 24 hours, filter through a 100-mesh filter cloth to obtain a clear and transparent AES concentrated solution with an active ingredient content of 40.0%, a viscosity of 1250 mPa·s at 25°C, and no delamination phenomenon after 3 months of accelerated aging test at 50°C.

[0044] Example 3:

[0045] A preparation method of an AES concentrated formula with high active ingredients, comprising the following steps:

[0046] Step 1, raw material pretreatment: Crush 10% of sodium tripolyphosphate, 8% of sodium pyrophosphate, and 3% of sodium citrate to 80-100 mesh, mix evenly and add to a high-speed dispersion kettle, and dry at 65°C for 30 minutes; Weigh 35% of AES, 10% of linear alkylbenzene sulfonate, 6% of alkyl polyglycoside, and 5% of cocamidopropyl betaine, heat to 50-55°C to melt, and obtain a molten surfactant mixture for standby;

[0047] Step 2. Mixing reaction: Add deionized water into the reaction kettle, start stirring at a speed of 200 - 300 r / min, and successively add the pretreated composite chelating agent and the molten surfactant mixture. Keep the temperature at 45°C and react for 40 minutes; add 4% propylene glycol and 0.5% EDTA disodium, adjust the stirring speed to 150 - 200 r / min, and keep the temperature for reaction for 20 minutes; adjust the pH of the system to 7.2 with 30% sodium hydroxide solution, add sodium chloride for viscosity adjustment, and finally add 0.5% sodium benzoate and 0.1 - 0.3% essence, and stir evenly to obtain the reaction solution;

[0048] Step 3. Post-treatment: Age the reaction solution at 25 - 30°C for 24 hours, filter it through a 100-mesh filter cloth to obtain a clear and transparent AES concentrate with an active matter content of 35.0%, a viscosity of 1180 mPa·s at 25°C, and no delamination phenomenon after 3 months of accelerated aging test at 50°C.

[0049] Perform performance tests on the clear and transparent AES concentrates obtained in the above Example 1, Example 2, and Example 3,

[0050] 1. Detergency test: Refer to GB / T 13174-2021, the decontamination value for sebum-stained cloth is 22% higher than that of the commercially available 70% AES concentrate;

[0051] 2. Foam performance: Measured by a Ross-Miles foam meter, the initial foam height is 180 mm, and the foam height after 5 minutes is 150 mm (better than the standard requirements);

[0052] 3. Stability: No crystallization after freezing at -10°C for 24 hours, and the transparency retention rate ≥ 95% after storage at 45°C for 6 months.

[0053] During specific use, users can adjust the proportions of each component according to actual needs to obtain the best washing effect and stability. For example, in hard water areas, the dosage of the composite chelating agent can be appropriately increased to improve the chelating ability for metal ions and prevent the inhibitory effect of hard water on the activity of surfactants. At the same time, by adjusting the dosage of sodium chloride, the viscosity of the system can be controlled to meet the requirements of different application scenarios.

[0054] In addition, the AES concentrate formula of the present invention also has good environmental performance. The raw materials used are all environmentally friendly surfactants and additives, with good biodegradability and no pollution to the environment. During the preparation process, by precisely controlling the conditions of each step, the emissions of waste water and waste gas are reduced, which is in line with the development trend of green chemistry.

[0055] In practical applications, the AES concentrated formula of the present invention can be used to prepare various detergent products, such as washing powder, laundry detergent, dishwashing liquid, etc. Its excellent detergency, foaming performance and stability can provide users with a better washing experience. At the same time, due to the synergistic effect of each component in the formula, the comprehensive performance of the product is superior to that of traditional AES concentrates, and it has broad market application prospects.

[0056] In summary, the present invention provides an AES concentrated formula with high active ingredients and a preparation method. By optimizing the formula composition and preparation process, the detergency, foaming performance and stability of the product are significantly improved. At the same time, it has good environmental performance and broad application prospects.

[0057] The preparation method has a simple process, convenient operation and is easy to realize industrial production. The parameter selection in each step has been carefully designed and optimized to ensure the quality and performance of the final product. For example, the crushing and drying operations in the raw material pretreatment step help to improve the dispersibility and reaction activity of the raw materials; the control of temperature, stirring speed and reaction time in the mixing reaction step ensures the full reaction and uniform mixing between components; the aging and filtration operations in the post-treatment step further improve the clarity and stability of the product.

[0058] In addition, the AES concentrated formula of the present invention also has good economic benefits. By optimizing the formula composition and preparation process, the production cost is reduced and the cost performance of the product is improved. At the same time, due to the comprehensive performance of the product being superior to that of traditional AES concentrates, it has stronger competitiveness in the market.

[0059] In summary, the present invention provides an AES concentrated formula with high active ingredients and a preparation method. The formula composition is reasonable, the preparation process is simple and feasible, the product performance is excellent, environmentally friendly and economical, and it has broad market application prospects.

[0060] Although the present invention has been described in detail with reference to the foregoing embodiments, for those skilled in the art, they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements for some of the technical features. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. An AES concentrated formula with high active ingredients, characterized in that: Comprising by weight percentage: 25%-35% of AES, 8%-12% of linear alkylbenzene sulfonate, 5%-8% of alkyl polyglycoside, 4%-6% of cocoamidopropyl betaine, 18%-28% of compound chelating agent, 2%-4% of sodium chloride, 0.3%-0.5% of disodium EDTA, 0.5%-1% of sodium benzoate, 3%-5% of propylene glycol and the balance of deionized water.

2. The AES concentrated formulation with high active ingredients according to claim 1, characterized in that: Comprising by weight percentage: 28.0% of AES, 10.0% of linear alkylbenzene sulfonate, 6.0% of alkyl polyglycoside, 5.0% of cocoamidopropyl betaine, 20% of compound chelating agent, 3.0% of sodium chloride, 0.4% of disodium EDTA, 4.0% of propylene glycol, 0.8% of sodium benzoate, and the balance is deionized water.

3. The AES concentrated formulation with high active ingredients according to claim 1, characterized in that: Comprising by weight percentage: 32.0% of AES, 9.0% of linear alkylbenzene sulfonate, 7.0% of alkyl polyglycoside, 4.5% of cocoamidopropyl betaine, 23.5% of compound chelating agent, 2.5% of sodium chloride, 0.35% of disodium EDTA, 5.0% of propylene glycol, 0.6% of sodium benzoate, and the balance is deionized water.

4. An AES concentrated formulation with high active ingredients according to claim 1, characterized in that: The molar number of ethylene oxide addition in the AES molecule is 3-5.

5. An AES concentrated formulation with high active ingredients according to any one of claims 1 - 4, characterized in that: The compound chelating agent includes: sodium tripolyphosphate, sodium pyrophosphate and sodium citrate, and the mass ratio of sodium tripolyphosphate, sodium pyrophosphate and sodium citrate is: 10-18:5-8:3-5.

6. The preparation method of an AES concentrated formula with high active ingredients according to any one of claims 1-5, characterized in that: Including the following steps: Step 1, raw material pretreatment: Crush, mix and dry sodium tripolyphosphate, sodium pyrophosphate and sodium citrate, weigh AES, linear alkylbenzene sulfonate, alkyl polyglycoside, cocoamidopropyl betaine and melt them to obtain a molten surfactant mixture for standby; Step 2, mixing reaction: Add deionized water to the reaction kettle, stir, and sequentially add the pretreated compound chelating agent and molten surfactant mixture; add propylene glycol and disodium EDTA and stir again; adjust the pH of the system with sodium hydroxide solution, add sodium chloride for viscosity adjustment, and finally add sodium benzoate and essence, and stir evenly to obtain a reaction solution; Step 3, post-treatment: Age the reaction solution, filter it through a 100-mesh filter cloth to obtain a clear and transparent AES concentrate; Step 4, performance test: Test the detergency, foam performance and stability of the obtained clear and transparent AES concentrate.

7. The preparation method of an AES concentrated formula with high active ingredients according to claim 6, characterized in that: Specifically, in Step 1, 10%-18% of sodium tripolyphosphate, 5%-8% of sodium pyrophosphate, 3%-5% of sodium citrate are crushed to 80-100 meshes, mixed evenly and then added to a high-speed dispersion kettle, and dried at 60-70 °C for 30 minutes; weigh AES, linear alkylbenzene sulfonate, alkyl polyglycoside, cocoamidopropyl betaine, heat to 50-55 °C and melt to obtain a molten surfactant mixture for standby.

8. The preparation method of an AES concentrated formula with high active ingredients according to claim 6, characterized in that: Specifically, in the second step, deionized water is added to the reactor, stirring is started at a speed of 200 - 300 r / min, and the pretreated composite chelating agent and the molten surfactant mixture are added in sequence, and the reaction is carried out at a temperature of 45 - 50 °C for 40 minutes; 3% - 5% of propylene glycol and 0.3% - 0.5% of EDTA disodium are added, the stirring speed is adjusted to 150 - 200 r / min, and the reaction is carried out under insulation for 20 minutes; The pH of the system is adjusted to 7.0 - 7.5 with 30% sodium hydroxide solution, sodium chloride is added for viscosity adjustment, and finally 0.5% - 1% of sodium benzoate and 0.1 - 0.3% of essence are added, and stirred evenly to obtain the reaction solution.

9. The preparation method of an AES concentrated formula with high active ingredients according to claim 6, characterized in that: Specifically, in the third step, the reaction solution is aged at 25 - 30 °C for 24 hours and filtered through a 100 - mesh filter cloth to obtain a clear and transparent AES concentrate.

Images