Non-ionic polymerization emulsion and preparation method thereof

By optimizing the stepwise polymerization process and catalyst, a nonionic emulsion with high internal phase viscosity and small particle size was prepared, which solved the problems of low polymerization efficiency and poor stability, and met the compatibility and stability requirements of high-end applications.

CN121824951AInactive Publication Date: 2026-04-10SICHUAN DOWELL SCI & TECH INC
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
SICHUAN DOWELL SCI & TECH INC
Filing Date
2026-01-19
Publication Date
2026-04-10
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

Existing nonionic emulsion polymerization technology suffers from low polymerization efficiency, difficulty in achieving high internal phase viscosity, and improper catalyst addition can easily lead to side reactions, affecting product stability and performance consistency, thus limiting its use in high-end applications.

Method used

A stepwise polymerization process was adopted, with some catalyst added before phase inversion. Combined with a reasonable ratio of siloxane oligomer and nonionic emulsifier, and by controlling the stirring shear parameters and diluting in stages, the pH value was adjusted with a neutralizing agent to prepare a small particle size emulsion with high internal phase viscosity.

Benefits of technology

It significantly improves polymerization efficiency, produces stable emulsions with high internal phase viscosity to meet the needs of high-end applications, and has strong compatibility, making it suitable for sensitive scenarios and extending product shelf life.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention belongs to the field of auxiliaries, and particularly relates to a nonionic polymerization emulsion and a preparation method thereof. The nonionic polymerization emulsion is prepared from the following raw materials in percentage by weight: 30 to 90 percent of siloxane low polymer, 2 to 30 percent of nonionic emulsifier, 0.05 to 5 percent of catalyst, 0.05 to 5 percent of neutralizer and the balance of water. The preparation method comprises the following steps: mixing an emulsifier, a part of water and a part of a catalyst, adding a siloxane low polymer, stirring and shearing to obtain an ointment-in-water body, diluting, adding the rest of the catalyst to prepare a pre-emulsion, heating, polymerizing, neutralizing and terminating the reaction. The problems of low nonionic polymerization efficiency and insufficient internal phase viscosity are solved, and the product is high in internal phase viscosity, uniform in particle size, good in stability and suitable for the fields of spinning, leather, personal care and the like.
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Description

TECHNICAL FIELD

[0001] The present application belongs to the field of auxiliaries, and particularly relates to a non-ionic polymer emulsion and a preparation method thereof. BACKGROUND

[0002] The application field of silicone emulsion is very wide, and the main application fields are in textile leather and personal care. There are two preparation methods of silicone emulsion at present, one is mechanical emulsification method, and the other is emulsion polymerization method. The former has simple process, but it is difficult to make the emulsion particle size very small when preparing high-viscosity silicone oil emulsion, and the emulsion polymerization method makes up for this shortcoming and can make small-particle-size emulsion with internal phase viscosity of millions of centipoise.

[0003] The emulsion polymerization technology can be divided into ionic (anionic, cationic) and non-ionic according to the type of emulsifier used. In current industrial production, ionic emulsion polymerization method, especially anionic process, occupies a dominant position due to its fast polymerization rate, large internal phase viscosity improvement space and other characteristics. However, ionic emulsion has significant limitations: in sensitive scenarios such as personal care, ionic emulsifiers may cause skin irritation and allergic reactions; in textile fiber finishing, ionic residues can easily lead to decreased fiber hydrophilicity and poor dyeing uniformity; at the same time, the compatibility of ionic emulsion with other systems is poor, which limits its application in composite auxiliaries.

[0004] Non-ionic emulsion has the advantages of low irritation, high compatibility, strong electrolyte stability, etc. due to the absence of ionic groups in the emulsifier, which meets the needs of high-end application scenarios. However, the existing non-ionic emulsion polymerization technology has been facing two major pain points for a long time: first, low polymerization efficiency, the emulsifying ability of non-ionic emulsifiers is weaker than that of ionic ones, leading to insufficient dispersion of the oil phase, low contact efficiency of the catalyst and the monomer, and insufficient monomer conversion; second, it is difficult to achieve high internal phase viscosity, the internal phase viscosity of the non-ionic silicone emulsion prepared by the existing technology is generally low, which cannot meet the performance requirements of high softness in textile and long-lasting lubrication in personal care. In addition, in the existing non-ionic polymerization system, the catalyst is mostly added at one time, which can easily cause local concentration to be too high to trigger side reactions, or the concentration to be too low to cause insufficient polymerization, further exacerbating the problems of product stability and performance consistency.

[0005] Therefore, the present application is proposed based on the above. SUMMARY

[0006] In order to solve the problems existing in the prior art, the present application provides a non-ionic polymer emulsion, which comprises the following preparation raw materials in weight percentage: siloxane oligomer 30-90%, non-ionic emulsifier 2-30%, catalyst 0.05-5%, neutralizing agent 0.05-5%, and the balance of water; wherein: The siloxane oligomer comprises one or both of cyclic siloxane and short-chain hydroxyl-terminated siloxane; The non-ionic emulsifier comprises one or more than two combinations of polyoxyalkylene alkyl ether, polyoxyalkylene alkyl phenyl ether, polyoxyalkylene lauryl ether, and polyoxyalkylene sorbitol ester; The catalyst comprises an acid catalyst or a base catalyst; the acid catalyst comprises one or more than two combinations of sulfuric acid, hydrochloric acid, phosphoric acid, formic acid, and acetic acid; the base catalyst comprises one or more than two combinations of lithium hydroxide, potassium hydroxide, sodium hydroxide, ammonium hydroxide, triethanolamine, and ethanolamine; The neutralizing agent is a neutralizing agent for neutralizing the catalyst. Alkalis such as lithium hydroxide, potassium hydroxide, sodium hydroxide, ammonium hydroxide, triethanolamine, and ethanolamine, or acids such as sulfuric acid, hydrochloric acid, phosphoric acid, formic acid, and acetic acid can be selected.

[0007] The water can be deionized water, well water, mineral water, tap water, or the like.

[0008] Preferably, the non-ionic polymeric emulsion comprises the following weight percentages of raw materials: 70% of siloxane oligomer, 14.57% of non-ionic emulsifier, 2% of catalyst, 2.05% of neutralizing agent, and the balance of water.

[0009] Preferably, the cyclic siloxane comprises one or more than two combinations of hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, and dodecamethylcyclohexasiloxane.

[0010] Preferably, the short-chain hydroxyl-terminated siloxane is shown in Formula I: Formula I wherein R1 and R2 are alkyl groups or phenyl groups containing 1-6 carbon atoms; and n is an integer representing the degree of polymerization, which is not specifically limited, but the viscosity of the short-chain hydroxyl-terminated siloxane is required to be 10-2000 mPa·s.

[0011] Preferably, R1 and R2 are methyl, ethyl, propyl, phenyl, or allyl.

[0012] Based on the same technical concept, still another aspect of the present application provides a preparation method of a non-ionic polymeric emulsion, which comprises the following steps: (1) mixing a non-ionic emulsifier, part of water, and part of a catalyst uniformly, adding a siloxane oligomer to perform stirring and shearing, and obtaining an oil-in-water paste; (2) adding the remaining water to the oil-in-water paste to dilute, then adding the remaining catalyst, stirring uniformly, and obtaining a pre-emulsion; (3) heating the pre-emulsion to perform polymerization, and obtaining a polymerization liquid; (4) Add a neutralizing agent to the polymerization liquid to terminate the polymerization, thereby obtaining the nonionic polymer emulsion.

[0013] Preferably, in step (1), the stirring and shearing speed is 300-8000 r / min, and the stirring and shearing time is 10-60 min.

[0014] Preferably, in step (2), the stirring speed is 100-2000 r / min and the stirring time is 10-60 min.

[0015] Preferably, in step (3), the heating polymerization temperature is 10-95℃ and the time is 2-72h.

[0016] It should be noted that, in order to improve the applicability of nonionic emulsions, relevant additives, such as fragrances, colorants, thickeners, and preservatives, can be added as needed to improve performance.

[0017] The beneficial effects of this invention are as follows: 1. Significantly improves polymerization efficiency: This invention significantly improves the polymerization efficiency of emulsions by optimizing the catalyst addition method (adding part of the catalyst before phase inversion and supplementing the remaining catalyst after phase inversion dilution), thus solving the problem of insufficient polymerization reaction in existing non-ionic systems.

[0018] 2. Achieving a breakthrough in high internal phase viscosity: This invention, through the rational ratio of siloxane oligomers and nonionic emulsifiers, combined with a stepwise polymerization process, prepares emulsions with internal phase viscosities that can reach hundreds of thousands of mPa·s. This overcomes the technical shortcoming of nonionic polymerization in achieving high internal phase viscosity and meets the stringent requirements of high-end application scenarios for emulsion viscosity.

[0019] 3. Optimization of emulsion particle size and stability: By controlling the stirring and shearing parameters and the step-dilution process, the nonionic polymeric emulsion prepared by this invention has a uniform and small particle size. Combined with the pH adjustment effect of the neutralizing agent, the emulsion does not separate or exhibit oil floating phenomenon after being stored at 50°C for 1 month, which solves the problem of poor stability of existing high-viscosity emulsions and extends the product shelf life.

[0020] 4. Strong compatibility and low irritation: This invention uses a nonionic emulsifier system, and the product does not contain ionic residues. It has good compatibility with cationic, anionic, and nonionic auxiliaries, and can be widely compounded. It also has extremely low irritation and is suitable for sensitive scenarios such as personal care and infant textiles, breaking through the application limitations of ionic emulsions. Detailed Implementation

[0021] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be described in detail below. Obviously, the described embodiments are merely some embodiments of this invention, and not all embodiments. Based on the embodiments of this invention, all other implementation methods obtained by those skilled in the art without creative effort are within the scope of protection of this invention.

[0022] Example 1 This embodiment provides a method for preparing a nonionic polymeric emulsion, the method comprising the following steps (detailed): (a) Raw material preparation: Siloxane oligomer: short-chain hydroxyl-terminated siloxane, viscosity 67.2 mPa·s, grade XIAMETER PMX-0156 silanol silicone oil, purchased from Dow (Zhangjiagang) Investment Co., Ltd.

[0023] Nonionic emulsifiers: secondary alcohol polyoxyethylene ether, brand name TERGITO 15-S-40 (70% Aqueous) surfactant, purchased from Dow Chemical (Shanghai) Co., Ltd.; and secondary alcohol polyoxyethylene ether, brand name TERGITO 15-S-9 surfactant, purchased from Dow Chemical (Shanghai) Co., Ltd.

[0024] Catalyst: Potassium hydroxide, purchased from Sinopharm Chemical Reagent Co., Ltd.

[0025] Neutralizing agent: acetic acid, purchased from Sinopharm Chemical Reagent Co., Ltd.

[0026] Water: Deionized water, homemade.

[0027] (II) Preparation process: (1) In a 500mL three-necked flask, add 18g of TERGITO 15-S-9, 25.71g of TERGITO 15-S-40 and 10.29g of deionized water in sequence; start the top-mounted stirrer and stir at 150r / min for 15min (the purpose of this operation is to fully dissolve and mix the two emulsifiers to form a uniform aqueous phase base, which lays the foundation for subsequent oil phase dispersion), until the system is free of obvious particles and is transparent and uniform.

[0028] (2) Slowly add 3g of 50% KOH aqueous solution to the above aqueous system and continue stirring at 150r / min for 5min (to allow the catalyst to fully integrate with the aqueous phase, initially activate the catalytic activity, and create conditions for the polymerization reaction of siloxane oligomers). The dropping speed is controlled at 1 drop / second to avoid excessive local alkalinity that could lead to emulsifier decomposition.

[0029] (3) While stirring, slowly add 210g of XIAMETER PMX-0156 silicone oil (to avoid oil phase agglomeration and ensure that the oil phase is evenly dispersed in the water phase); increase the speed of the mixer to 1000r / min and continue stirring and shearing for 10min (by mechanical shearing force to break the oil phase particles, the oil phase is encapsulated by the water phase to form a stable oil-in-water paste, and the shearing parameter control can ensure that the initial particle size of the oil phase meets the requirements), and finally obtain the oil-in-water paste.

[0030] (4) Adjust the speed of the mixer to 100 r / min, slowly add 16.32 g of deionized water to the oil-in-water paste (to adjust the solid content of the system, reduce the viscosity of the paste, and provide sufficient space for the subsequent catalyst dispersion and polymerization reaction), and stir for 10 min until the paste gradually flows, the system is uniform, and there is no local clumping.

[0031] (5) Add 9g of 50% KOH aqueous solution to the diluted system and stir at 100r / min for 10min (to supplement the amount of catalyst and ensure that the polymerization reaction continues to proceed fully. Adding in batches can improve the utilization rate of the catalyst and avoid the problem of local concentration being too high or too low due to one-time addition) to form a uniform and stable pre-emulsion.

[0032] (6) After sealing the three-necked flask containing the pre-emulsion, place it in a 50°C constant temperature oven and let it stand for 24 hours to polymerize. (At a suitable temperature, the siloxane oligomer reacts and gradually increases the viscosity of the internal phase. Standing at a constant temperature can avoid emulsion breakage caused by stirring and ensure that the polymerization reaction proceeds uniformly.)

[0033] (7) Take out the polymerized system and cool it to 25°C. While stirring at 100 r / min, slowly add 7.68 g of 80% acetic acid aqueous solution (to neutralize the remaining KOH in the system, terminate the polymerization reaction, avoid residual catalyst causing the emulsion to deteriorate in the later stage, and improve the storage stability of the emulsion). After the addition is completed, continue stirring for 10 min to ensure that the pH of the system is uniform.

[0034] (8) Filter the neutralized emulsion through a stainless steel filter screen (to remove small amounts of coagulated material or impurities that may be generated during the polymerization process and improve product purity). Collect the filtered emulsion, which is the final nonionic polymerized emulsion product.

[0035] Example 2 This embodiment provides a method for preparing a nonionic polymeric emulsion, the method comprising the following steps (briefly described): Add 10.29g of deionized water to 18g of 15-S-9 and 25.71g of 15-S-40, and mix well. Then add 3g of KOH (50%) and mix well. Next, add 210g of hydroxyl silicone oil PMX-0156 and stir at 1000 rpm for 10 minutes using a top-mounted mixer to induce phase inversion into an oil-in-water paste. Adjust the speed to 100 rpm and slowly add 16.32g of deionized water to the paste, stirring for 10 minutes. Then add 9g of KOH (50%) and stir for 10 minutes. Place the resulting sample in an 80℃ oven and let it stand for 24 hours. After that, remove it and add 7.68g of acetic acid (80%), stirring at 100 rpm for 10 minutes using a top-mounted mixer to obtain the final nonionic polymer emulsion product.

[0036] Example 3 This embodiment provides a method for preparing a nonionic polymeric emulsion, the method comprising the following steps (briefly described): Add 6.18g of deionized water to 10.8g of 15-S-9 and 15.42g of 15-S-40, and mix well. Then add 3g of KOH (50%) and mix well. Next, add 210g of hydroxyl silicone oil PMX-0156 and stir at 1000 rpm for 10 minutes using a top-mounted mixer to induce phase inversion into an oil-in-water emulsion. Adjust the speed to 100 rpm and slowly add 47.76g of deionized water to the emulsion, stirring for 10 minutes. Then add 3g of KOH (50%) and stir for 10 minutes. Place the resulting sample in a 50℃ oven and let it stand for 24 hours. Afterward, remove the sample and add 3.84g of acetic acid (80%), stirring at 100 rpm for 10 minutes using a top-mounted mixer to obtain the final nonionic polymer emulsion product.

[0037] Example 4 This embodiment provides a method for preparing a nonionic polymeric emulsion into an ointment. The rotation speed is adjusted to 100 r / min, and 47.76 g of deionized water is slowly added to the ointment, followed by stirring. The preparation method includes the following steps (briefly described): Add 6.18g of deionized water to 10.8g of 15-S-9 and 15.42g of 15-S-40, and mix well. Then add 3g of KOH (50%) and mix well. Next, add 210g of hydroxyl silicone oil PMX-0156 and stir at 1000 rpm for 10 minutes using a top-mounted stirrer until the phase inversion to water-in-oil phase is achieved (0 minutes). Then add 3g of KOH (50%) and stir for 10 minutes. Place the resulting sample in an 80℃ oven and let it stand for 24 hours. After that, remove the sample and add 3.84g of acetic acid (80%), and stir at 100 rpm for 10 minutes using a top-mounted stirrer to obtain the final nonionic polymer emulsion product.

[0038] Example 5 This embodiment provides a method for preparing a nonionic polymeric emulsion, the method comprising the following steps (briefly described): Add 14.88g of deionized water to 10.8g of 15-S-9 and 15.42g of 15-S-40, and mix well. Then add 3g of KOH (50%) and mix well. Next, add 210g of hydroxyl silicone oil PMX-0156 and stir for 10 minutes using a top-mounted mixer at 1000 rpm to induce phase inversion into an oil-in-water emulsion. Adjust the speed to 100 rpm and slowly add 29.22g of deionized water to the emulsion, stirring for 10 minutes. Then add 9g of KOH (50%) and stir for 10 minutes. Place the resulting sample in an 80℃ oven and let it stand for 24 hours. Afterward, remove the sample and add 7.68g of acetic acid (80%), stirring for 10 minutes using a top-mounted mixer at 100 rpm to obtain the final nonionic polymer emulsion product.

[0039] Example 6 This embodiment provides a method for preparing a nonionic polymeric emulsion, the method comprising the following steps (briefly described): Add 2.58g of deionized water to 51.42g of 15-S-40 and mix well. Then add 3g of KOH (50%) and mix well. Next, add 210g of hydroxyl silicone oil PMX-0156 and stir for 10 minutes using a top-mounted mixer at 1000 rpm to form an oil-in-water emulsion. Adjust the speed to 100 rpm and slowly add 16.32g of deionized water to the emulsion, stirring for 10 minutes. Then add 9g of KOH (50%) and stir for 10 minutes. Place the resulting sample in a 50℃ oven and let it stand for 24 hours. After that, remove it and add 7.68g of acetic acid (80%), stirring for 10 minutes using a top-mounted mixer at 100 rpm to obtain the final nonionic polymer emulsion product.

[0040] Example 7 Add 2.58g of deionized water to 51.42g of 15-S-40 and mix well; then add 3g of KOH (50%) and mix well; then add 210g of hydroxyl silicone oil PMX-0156 and stir at 1000rpm for 10min using a top-mounted mixer to induce phase inversion into an oil-in-water emulsion. Adjust the speed to 100rpm and slowly add 16.32g of deionized water to the emulsion, stirring for 10min, then add 9g of KOH (50%) and stir for 10min. Place the resulting sample in a 50℃ oven and let it stand for 28h. Afterward, remove the sample and add 7.68g of acetic acid (80%), stirring at 100rpm for 10min using a top-mounted mixer to obtain the final emulsion product.

[0041] Comparative Example 1 Add 10.29g of deionized water to 18g of 15-S-9 and 25.71g of 15-S-40, and mix thoroughly. Then add 210g of hydroxyl silicone oil PMX-0156 and stir at 1000 rpm for 10 minutes using a top-mounted mixer to induce phase inversion into an oil-in-water emulsion. Adjust the speed to 100 rpm and slowly add 16.32g of deionized water to the emulsion, stirring for 10 minutes. Then add 12g of KOH (50%) and stir for 10 minutes. Place the resulting sample in a 50℃ oven and let it stand for 24 hours. Afterward, remove the sample and add 7.68g of acetic acid (80%), stirring at 100 rpm for 10 minutes using a top-mounted mixer to obtain the final emulsion product.

[0042] The difference between Comparative Example 1 and Example 1 is that no KOH was added before the hydroxyl silicone oil was inverted; it was added entirely after the dilution following the inversion.

[0043] Comparative Example 2 Add 10.29g of deionized water to 18g of 15-S-9 and 25.71g of 15-S-40, and mix thoroughly. Then add 210g of hydroxyl silicone oil PMX-0156 and stir at 1000 rpm for 10 minutes using a top-mounted mixer to induce phase inversion into an oil-in-water emulsion. Adjust the speed to 100 rpm and slowly add 16.32g of deionized water to the emulsion, stirring for 10 minutes. Then add 12g of KOH (50%) and stir for 10 minutes. Place the resulting sample in an 80℃ oven and let it stand for 24 hours. Afterward, remove the sample and add 7.68g of acetic acid (80%), stirring at 100 rpm for 10 minutes using a top-mounted mixer to obtain the final emulsion product.

[0044] The difference between Comparative Example 2 and Example 2 is that no KOH was added before the hydroxyl silicone oil was inverted; it was added entirely after the dilution following the inversion.

[0045] Comparative Example 3 Add 6.18g of deionized water to 10.8g of 15-S-9 and 15.42g of 15-S-40, and mix thoroughly. Then add 210g of hydroxyl silicone oil PMX-0156 and stir for 10 minutes using a top-mounted mixer at 1000 rpm to form an oil-in-water emulsion. Adjust the speed to 100 rpm and slowly add 47.76g of deionized water to the emulsion, stirring for 10 minutes. Then add 6g of KOH (50%) and stir for 10 minutes. Place the resulting sample in a 50℃ oven and let it stand for 24 hours. After that, remove it and add 3.84g of acetic acid (80%), stirring for 10 minutes using a top-mounted mixer at 100 rpm to obtain the final emulsion product.

[0046] The difference between Comparative Example 3 and Example 3 is that no KOH was added before the hydroxyl silicone oil was inverted; it was added entirely after the dilution following the inversion.

[0047] Comparative Example 4 Add 6.18g of deionized water to 10.8g of 15-S-9 and 15.42g of 15-S-40, and mix thoroughly. Then add 210g of hydroxyl silicone oil PMX-0156 and stir for 10 minutes using a top-mounted mixer at 1000 rpm to form an oil-in-water emulsion. Adjust the speed to 100 rpm and slowly add 47.76g of deionized water to the emulsion, stirring for 10 minutes. Then add 6g of KOH (50%) and stir for 10 minutes. Place the resulting sample in an 80℃ oven and let it stand for 24 hours. After that, remove it and add 3.84g of acetic acid (80%), stirring for 10 minutes using a top-mounted mixer at 100 rpm to obtain the final emulsion product.

[0048] The difference between Comparative Example 4 and Example 4 is that no KOH was added before the hydroxyl silicone oil was inverted; it was added entirely after the dilution following the inversion.

[0049] Comparative Example 5 Add 2.58g of deionized water to 51.42g of 15-S-40 and mix well. Then add 210g of hydroxyl silicone oil PMX-0156 and stir for 10 minutes using a top-mounted mixer at 1000 rpm to form an oil-in-water emulsion. Adjust the speed to 100 rpm and slowly add 16.32g of deionized water to the emulsion, stirring for 10 minutes. Then add 12g of KOH (50%) and stir for 10 minutes. Place the resulting sample in a 50℃ oven and let it stand for 24 hours. After that, remove it and add 7.68g of acetic acid (80%), stirring for 10 minutes using a top-mounted mixer at 100 rpm to obtain the final emulsion product.

[0050] The difference between Comparative Example 5 and Example 6 is that no KOH was added before the hydroxyl silicone oil was inverted; it was added entirely after the dilution following the inversion.

[0051] Test case (a) Determination of the viscosity of the internal phase of the emulsion (i.e., the viscosity of the silicone oil in the emulsion). Add 2g of the emulsion to 10mL of isopropanol (IPA), mix thoroughly, and centrifuge at 3000r / min for 10min to separate the lower polymer layer. Repeat the above steps with IPA at least three times to thoroughly remove emulsifiers and water from the polymer. Place the extracted polymer in a petri dish and dry in a vacuum drying oven at 60℃ for 2h. After cooling to room temperature, use a rheological test to determine its viscosity.

[0052] (ii) Determination of emulsion particle size The particle size of the emulsion was determined using a Malvern 2000.

[0053] (III) Evaluation of emulsion stability Storage stability of the emulsion at 50℃: The emulsion was placed in a 100mL wide-mouth transparent plastic bottle and left to stand in a 50℃ oven. Observation was conducted weekly for one month. Specific observation method: Visually inspect the appearance and overall changes of the emulsion. If it is homogeneous and shows no signs of oil floating or layering, the emulsion has good stability; otherwise, its stability is poor.

[0054] The detection results of the examples and comparative examples are shown in Table 1.

[0055] Table 1

[0056] The above results clearly demonstrate that the present invention discovers that in nonionic systems, adding a portion of a catalyst to the siloxane oligomer before phase inversion into an oil-in-water emulsion can significantly improve the polymerization efficiency of the emulsion, enabling the preparation of stable polymeric emulsions with high internal phase viscosity and small particle size. The products prepared by this invention can be applied in industries such as textiles, leather, and personal care. The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A nonionic polymeric emulsion, characterized in that, The preparation raw materials include the following weight percentages: 30-90% siloxane oligomer, 2-30% nonionic emulsifier, 0.05-5% catalyst, 0.05-5% neutralizer, and the balance being water; wherein: The siloxane oligomer includes one or two of cyclosiloxanes and short-chain hydroxyl-terminated siloxanes. The nonionic emulsifier includes one or more of polyoxyethylene alkyl ethers, polyoxyethylene alkylphenyl ethers, polyoxyethylene lauryl ethers, and polyoxyethylene sorbitol esters. The catalyst includes an acid catalyst or a base catalyst; the acid catalyst includes one or more of sulfuric acid, hydrochloric acid, phosphoric acid, formic acid, and acetic acid; the base catalyst includes one or more of lithium hydroxide, potassium hydroxide, sodium hydroxide, ammonium hydroxide, triethanolamine, and ethanolamine. The neutralizing agent is used to neutralize the catalyst.

2. The nonionic polymeric emulsion according to claim 1, characterized in that, The raw materials include the following weight percentages: 70% siloxane oligomer, 14.57% nonionic emulsifier, 2% catalyst, 2.05% neutralizer, and the balance water.

3. The nonionic polymeric emulsion according to claim 1, characterized in that, The cyclosiloxanes include one or more combinations of hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, and dodecylcyclohexasiloxane.

4. The nonionic polymeric emulsion according to claim 1, characterized in that, The short-chain hydroxyl-terminated siloxane is shown in Formula I: Formula I Wherein: R1 and R2 are alkyl or phenyl groups containing 1-6 carbon atoms, and the viscosity of the short-chain hydroxyl-terminated siloxane is 10-2000 mPa·s.

5. The nonionic polymeric emulsion according to claim 4, characterized in that, R1 and R2 are methyl, ethyl, propyl, phenyl, or allyl.

6. A method for preparing the nonionic polymeric emulsion according to any one of claims 1-5, characterized in that, The preparation method includes the following steps: (1) Mix nonionic emulsifier, part water and part catalyst evenly, add siloxane oligomer and stir and shear to obtain oil-in-water paste; (2) Add the remaining water to the oil-in-water paste to dilute it, and then add the remaining catalyst. Stir well to obtain a pre-emulsion. (3) The preemulsion is heated and polymerized to obtain a polymer solution; (4) Add a neutralizing agent to the polymerization liquid to terminate the polymerization, thereby obtaining the nonionic polymer emulsion.

7. The method for preparing the nonionic polymeric emulsion according to claim 6, characterized in that, In step (1), the stirring and shearing speed is 300-8000 r / min, and the stirring and shearing time is 10-60 min.

8. The method for preparing the nonionic polymeric emulsion according to claim 6, characterized in that, In step (2), the stirring speed is 100-2000 r / min and the stirring time is 10-60 min.

9. The method for preparing the nonionic polymeric emulsion according to claim 6, characterized in that, In step (3), the heating polymerization temperature is 10-95℃ and the time is 2-72h.