Deepening silicone oil emulsion and preparation method thereof
By combining amino-modified silicone oil and acrylate-modified polyether silicone oil, the yellowing and tear strength reduction caused by amino-modified silicone oil when deepening the fabric is solved, achieving better dyeing depth and feel.
Patent Information
- Application Number
- CN202411928110.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-25
- Publication Date
- 2025-04-01
- Estimated Expiration
- 2044-12-25
AI Technical Summary
While deepening the fabric, amino silicone oil will reduce the friction between the fibers, affect the tear strength and performance of the fabric, and may cause the fabric to turn yellow.
The combination of amino-modified silicone oil and acrylate modified polyether silicone oil is adopted to introduce acrylate modified polyether silicone oil chain segments to reduce yellowing problems, and through the introduction of hydrophilic groups, the stability and permeability of the emulsion are improved, and the feel and depth-enhancing effect of the fabric are improved.
It effectively reduces the yellowing problem of fabrics, and at the same time improves the dyeing depth and feel of the fabrics, improves the friction between fibers, and reduces the adverse effects of deepening silicone oil on the fracture strength of the fabric.
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Figure BDA0005209705310000081
Abstract
Description
Technical Field
[0001] The invention relates to the field of deepening silicone oil, in particular to a deepening silicone oil emulsion and a preparation method thereof. Background Art
[0002] Darkening finishing is an important fabric finishing process, which is used to solve the technical problem that increasing the dye concentration still makes it difficult to achieve the dyeing depth required for medium and dark fabrics. It can save dye usage, increase the dyeing depth of fabrics, and reduce the discharge of dye-containing wastewater and treatment costs.
[0003] The principle of deepening silicone oil is to cover the surface of the fabric with a layer of low refractive index film to reduce the refractive index of the surface of the fabric fiber, thereby changing the degree of reflection and refraction of light by the fiber and increasing the absorption of incident light by the dye, thereby significantly increasing the dyeing depth of the fabric and playing a deepening role.
[0004] The commonly used deepening silicone oil is amino silicone oil. Amino silicone oil has good chemical reactivity, strong two-phase lubricity and compatibility, so it is widely used in textile finishing and textile dyeing and finishing. Amino silicone oil not only has a good deepening effect, but also can improve the feel of the fabric and make the fabric softer.
[0005] However, amino silicone oil is a large molecular polysiloxane structure, which will reduce the friction between fibers and greatly affect the tear strength and performance of the fabric. At the same time, the use of amino silicone oil will also cause yellowing of the fabric. Summary of the invention In order to enable the darkening silicone oil to play a darkening role while reducing the impact on the tear strength and yellowing problems of the fabric, the present application provides a darkening silicone oil emulsion and a preparation method thereof.
[0007] The present application provides a darkening silicone oil emulsion and a preparation method thereof using the following technical solutions: In a first aspect, the present application provides a darkening silicone oil emulsion, comprising the following raw materials in parts by weight: 55-70 parts of amino modified silicone oil; 30-45 parts of acrylate modified polyether silicone oil; Emulsifier 25-38 parts; 1-4 parts of organic acid; 220-260 parts of water; The acrylate-modified polyether silicone oil comprises the following raw materials in parts by weight: 10-18 parts of hydrogen silicone oil; 6-12 parts of allyl polyoxyethylene polyoxypropylene ether; 2-5 parts of acrylate monomer; Chloroplatinic acid 0.5-1 part; The acrylic acid ester monomer is selected from one or more of hydroxyethyl acrylate, N-hydroxyethyl acrylamide, and 4-hydroxybutyl acrylate.
[0008] By adopting the above technical scheme, amino-modified silicone oil and acrylate-modified polyether silicone oil are selected for compounding, and acrylate-modified polyether silicone oil segments are introduced into the formed copolymer to reduce the yellowing problem of the fabric. At the same time, by introducing hydrophilic groups such as hydroxyl groups, the emulsion of the darkening silicone oil is stabilized and can penetrate into the interior of the fabric, giving the fabric a soft and fluffy feel. The amino-modified silicone oil forms a low-refractive index film on the surface of the fabric, and the introduction and polymerization of the acrylate monomer enables the surface of the fabric to form a rough and uneven surface, changing the reflection and refraction of light, improving the darkening effect, and improving the friction between fibers, reducing the adverse effects of the darkening silicone oil on the breaking strength of the fabric.
[0009] Optionally, the amino-modified silicone oil comprises the following raw materials in parts by weight: 60-75 parts of silicone linear body; 2-4 parts of aminosilane coupling agent; 7-12 parts of capping agent; Catalyst 0.1-0.4 parts; Hexafluorobutyl acrylate 13-18 parts.
[0010] By adopting the above technical scheme, organic silicon linear body is selected to replace the commonly used octamethylcyclotetrasiloxane. After reacting with the aminosilane coupling agent, the grafting distribution of the amino group is more uniform, and it has better softness and smoothness. Hexafluorobutyl acrylate is selected for modification, and organic fluorine with a low refractive index is introduced to achieve better deepening effect. At the same time, the introduction of organic fluorine has an inhibitory effect on the yellowing of amino-modified silicone oil.
[0011] Optionally, the aminosilane coupling agent is one or more of coupling agent HD-121, coupling agent HD-110, and coupling agent KH-608.
[0012] By adopting the above technical scheme, an aminosilane coupling agent with secondary / tertiary amino groups is selected, and the reaction activity of hydrogen in the amino group is weak, thereby reducing the probability of yellowing of the fabric caused by amino oxidation.
[0013] Optionally, the organic silicon linear body is selected from one or more of terminal hydroxyl polydimethylsiloxane and trimethylsilane-terminated polydimethylsiloxane.
[0014] By adopting the above technical solution, the selection of organic silicone linear bodies allows the amino groups to be evenly grafted into the molecular chains of siloxane, thereby improving the compatibility of the amino silicone oil system.
[0015] Optionally, the aminosilane coupling agent is coupling agent HD-110, and the organic silicon linear body is hydroxy-terminated polydimethylsiloxane.
[0016] By adopting the above technical scheme, when the above combination is selected, the amino grafting of the amino silicone oil formed is evenly distributed, and the group steric hindrance of the molecular chain is large and not easy to move, so that the amino-modified silicone oil is not easy to yellow, and has good darkening effect and softness.
[0017] Optionally, the catalyst is one or more of potassium hydroxide, sodium hydroxide, and tetramethylammonium hydroxide.
[0018] Optionally, the emulsifier is selected from one or more of isomeric tridecanol polyoxyethylene ether, lauryl alcohol polyoxyethylene ether, and isomeric decanol polyoxyethylene ether.
[0019] By adopting the above technical solution, the selection of emulsifier determines the stability and compatibility of the darkening silicone oil emulsion. Through compound selection, the darkening silicone oil emulsion can be stored stably without demulsification and stratification.
[0020] Optionally, the organic acid is one or more of acetic acid, glacial acetic acid, and formic acid.
[0021] In a second aspect, the present application provides a method for preparing a darkening silicone oil emulsion, comprising the following steps: Add hydrogenated silicone oil and a certain amount of toluene into a flask, heat and stir, add chloroplatinic acid at 50-55°C, add a mixed solution of allyl polyoxyethylene polyoxypropylene ether and acrylate monomer dropwise into the flask at 87-90°C, continue the reaction for 5-6 hours, remove the solvent by distillation under reduced pressure, and obtain acrylate-modified polyether silicone oil; After mixing the acrylate-modified polyether silicone oil, amino-modified silicone oil and emulsifier, stir and emulsify for 20-30 minutes, add organic acid and water, and continue stirring for 2-2.5 hours to obtain a darkening silicone oil emulsion.
[0022] By adopting the technical scheme, a darkening silicone oil emulsion with excellent darkening effect and excellent hand feel is prepared.
[0023] Optionally, the amino-modified silicone oil is prepared by the following steps: Add organic silicon linear body and aminosilane coupling agent into the reaction bottle, stir and heat to 80-85°C, add end-capping agent and catalyst, stir at constant temperature for 2-3h, heat and vacuum, then cool to room temperature, add glacial acetic acid to neutralize to pH 6.5-7, and obtain aminosilicone oil; Amino silicone oil and a certain amount of toluene are placed in another reaction bottle, heated to 60-62°C under nitrogen protection, stirred and refluxed for 5-5.5 hours, hexafluorobutyl acrylate is added dropwise, reacted for 5-5.5 hours, and the solvent is removed by reduced pressure distillation to obtain amino-modified silicone oil.
[0024] By adopting the above technical scheme, after the amino silicone oil is generated, hexafluorobutyl acrylate and the amino group in the amino silicone oil are used to undergo an addition reaction to introduce a fluoroalkyl acrylate chain segment, thereby improving the darkening effect and reducing yellowing.
[0025] In summary, the present application has at least one of the following beneficial effects: 1. Select amino-modified silicone oil and acrylate-modified polyether silicone oil for compounding, introduce acrylate-modified polyether silicone oil segments into the formed copolymer to reduce the yellowing problem of the fabric, and at the same time, through the introduction of hydrophilic groups such as hydroxyl groups, the emulsion of the deepening silicone oil is stable and can penetrate into the interior of the fabric, giving the fabric a soft and fluffy feel. The amino-modified silicone oil forms a low-refractive index film on the surface of the fabric, and the introduction and polymerization of acrylate monomers enables the surface of the fabric to form a rough and uneven surface, changing the reflection and refraction of light, improving the deepening effect, and improving the friction between fibers, reducing the adverse effects of the deepening silicone oil on the breaking strength of the fabric.
[0026] 2. Organic silicone linear body is used to replace the commonly used octamethylcyclotetrasiloxane. After reacting with aminosilane coupling agent, the grafting distribution of amino group is more uniform, with better softness and smoothness. Hexafluorobutyl acrylate is used for modification, and organic fluorine with low refractive index is introduced to make the deepening effect better. At the same time, the introduction of organic fluorine can inhibit the yellowing of amino-modified silicone oil. DETAILED DESCRIPTION
[0027] The present application is further described in detail below in conjunction with Examples 1-5 and Comparative Example 1.
[0028] In the following examples and comparative examples, the raw materials used are as follows: Hydroxyl-terminated polydimethylsiloxane: purchased from Wuhan Lanabai Pharmaceutical Chemical Co., Ltd., with a relative molecular weight of 1000 and a CAS number of 70131-67-8; Trimethylsilyl-terminated polydimethylsiloxane: purchased from Dow Corning, USA, brand DC200, molecular weight 1000; Coupling agent HD-121: purchased from Hangzhou Dadi Chemical Co., Ltd.; Coupling agent HD-110: purchased from Hubei Rishengchang New Material Technology Co., Ltd.; Coupling agent KH-608: purchased from Hangzhou Jessica Chemical Co., Ltd.; Hydrogenated silicone oil: purchased from Jinan Shengfeng Industry and Trade Co., Ltd.
[0029] Preparation Example Preparation Example 1 Preparation of amino-modified silicone oil The amino-modified silicone oil comprises the following raw materials in parts by weight: 60 g of organic silicone linear body, specifically hydroxy-terminated polydimethylsiloxane; 2g of aminosilane coupling agent, specifically coupling agent HD-121; 7g of end-capping agent, hexamethyldisiloxane; Catalyst 0.1g, potassium hydroxide is selected; Hexafluorobutyl acrylate 13g.
[0030] Amino-modified silicone oil is prepared by the following steps: Add organic silicon linear body and aminosilane coupling agent into the reaction bottle, stir and heat to 80°C, add end-capping agent and catalyst, stir at constant temperature for 2h, heat to 125°C, start the vacuum pump, control the vacuum degree between -0.095-0.1Mpa, evacuate for 1h, then remove the vacuum, cool down, add glacial acetic acid to neutralize to pH 6.5, and obtain amino silicone oil; Amino silicone oil and 180 g of toluene were placed in another reaction bottle, heated to 60° C. under nitrogen protection, stirred and refluxed for 5 h, hexafluorobutyl acrylate was added dropwise, reacted for 5 h, and the solvent was removed by reduced pressure distillation to obtain amino-modified silicone oil.
[0031] Preparation Example 2 Preparation of amino-modified silicone oil The amino-modified silicone oil comprises the following raw materials in parts by weight: 75 g of organic silicone linear body, specifically trimethylsilane-terminated polydimethylsiloxane; 4g of aminosilane coupling agent, specifically coupling agent KH-608; 12g of end-capping agent, hexamethyldisiloxane; Catalyst 0.4g, tetramethylammonium hydroxide; Hexafluorobutyl acrylate 18g.
[0032] Amino-modified silicone oil is prepared by the following steps: Add organic silicon linear body and aminosilane coupling agent into the reaction bottle, stir and heat to 85°C, add end-capping agent and catalyst, stir at constant temperature for 3h, heat to 130°C, start the vacuum pump, control the vacuum degree between -0.095-0.1Mpa, evacuate for 1h, then remove the vacuum, cool down, add glacial acetic acid to neutralize to pH 7, and obtain aminosilicone oil; Amino silicone oil and 230 g of toluene were placed in another reaction bottle, heated to 62° C. under nitrogen protection, stirred and refluxed for 5.5 h, hexafluorobutyl acrylate was added dropwise, reacted for 5.5 h, and the solvent was removed by reduced pressure distillation to obtain amino-modified silicone oil.
[0033] Preparation Example 3 Preparation of amino-modified silicone oil The amino-modified silicone oil comprises the following raw materials in parts by weight: 68g of organic silicone linear body, specifically hydroxy-terminated polydimethylsiloxane; 3g of aminosilane coupling agent, specifically coupling agent HD-110; 9g of end-capping agent, hexamethyldisiloxane; Catalyst 0.3g, sodium hydroxide is selected; Hexafluorobutyl acrylate 15g.
[0034] Amino-modified silicone oil is prepared by the following steps: Add organic silicon linear body and aminosilane coupling agent into the reaction bottle, stir and heat to 82°C, add end-capping agent and catalyst, stir at constant temperature for 2.5h, heat to 127°C, start the vacuum pump, control the vacuum degree between -0.095-0.1Mpa, evacuate for 1h, then remove the vacuum, cool down, add glacial acetic acid to neutralize to pH 7, and obtain amino silicone oil; Amino silicone oil and 200 g of toluene were placed in another reaction bottle, heated to 61° C. under nitrogen protection, stirred and refluxed for 5 h, hexafluorobutyl acrylate was added dropwise, reacted for 5.5 h, and the solvent was removed by reduced pressure distillation to obtain amino-modified silicone oil. Example
[0035] Example 1 A silicone oil emulsion comprising the following raw materials: 55 g of amino-modified silicone oil, the amino-modified silicone oil prepared in Preparation Example 1 is selected; Acrylate modified polyether silicone oil 30g; Emulsifier 25g, selected from 20g isomeric tridecanol polyoxyethylene ether and 5g lauryl alcohol polyoxyethylene ether; 1g organic acid, glacial acetic acid; 220g water; Acrylate modified polyether silicone oil includes the following raw materials in parts by weight: 10g hydrogen silicone oil; Allyl polyoxyethylene polyoxypropylene ether 6g; 2g of acrylate monomer, hydroxyethyl acrylate; Chloroplatinic acid 0.5g.
[0036] A silicone oil emulsion is prepared by the following steps: Add hydrogenated silicone oil and 35g toluene into a flask, heat and stir, add chloroplatinic acid at 50°C, and dropwise add a mixed solution of allyl polyoxyethylene polyoxypropylene ether and acrylate monomer into the flask at 87°C. Complete the dropwise addition within 1 hour, continue the reaction for 5 hours, and remove the solvent by distillation under reduced pressure to obtain acrylate-modified polyether silicone oil; After mixing the acrylate-modified polyether silicone oil, amino-modified silicone oil and emulsifier, stir and emulsify for 20 minutes, add organic acid and water, and continue stirring for 2 hours to obtain a darkening silicone oil emulsion.
[0037] Example 2 A silicone oil emulsion comprising the following raw materials: 70 g of amino-modified silicone oil, the amino-modified silicone oil prepared in Preparation Example 2 is selected; Acrylate modified polyether silicone oil 45g; 38g of emulsifier, 25g of isomeric decanol polyoxyethylene ether and 13g of lauryl alcohol polyoxyethylene ether; 4g organic acid, acetic acid is selected; 260g water; Acrylate modified polyether silicone oil includes the following raw materials in parts by weight: Hydrogenated silicone oil 18g; Allyl polyoxyethylene polyoxypropylene ether 12g; 5g of acrylate monomer, 4-hydroxybutyl acrylate; Chloroplatinic acid 1g.
[0038] A silicone oil emulsion is prepared by the following steps: Add hydrogenated silicone oil and 50g toluene into a flask, heat up and stir, add chloroplatinic acid at 55°C, and dropwise add a mixed solution of allyl polyoxyethylene polyoxypropylene ether and acrylate monomer into the flask at 90°C. Complete the dropwise addition within 1 hour, continue the reaction for 6 hours, and remove the solvent by distillation under reduced pressure to obtain acrylate-modified polyether silicone oil; After mixing the acrylate-modified polyether silicone oil, amino-modified silicone oil and emulsifier, stir and emulsify for 30 minutes, add organic acid and water, and continue stirring for 2.5 hours to obtain a darkening silicone oil emulsion.
[0039] Example 3 A silicone oil emulsion comprising the following raw materials: 63 g of amino-modified silicone oil, the amino-modified silicone oil prepared in Preparation Example 1 is selected; Acrylate modified polyether silicone oil 38g; 33g of emulsifier, selected from 20g of isomeric tridecanol polyoxyethylene ether and 13g of isomeric decanol polyoxyethylene ether; 2g organic acid, formic acid is used; 245g water; Acrylate modified polyether silicone oil includes the following raw materials in parts by weight: 15g hydrogen silicone oil; Allyl polyoxyethylene polyoxypropylene ether 10g; 3g of acrylate monomer, N-hydroxyethyl acrylamide; Chloroplatinic acid 0.8g.
[0040] A silicone oil emulsion is prepared by the following steps: Add hydrogenated silicone oil and 45g toluene into a flask, heat and stir, add chloroplatinic acid at 52°C, and dropwise add a mixed solution of allyl polyoxyethylene polyoxypropylene ether and acrylate monomer into the flask at 89°C. The dropwise addition is completed within 1 hour, and the reaction is continued for 5.5 hours. The solvent is removed by distillation under reduced pressure to obtain acrylate-modified polyether silicone oil; After mixing the acrylate-modified polyether silicone oil, amino-modified silicone oil and emulsifier, stir and emulsify for 25 minutes, add organic acid and water, and continue stirring for 2.5 hours to obtain a darkening silicone oil emulsion.
[0041] Example 4 The difference between this embodiment and embodiment 1 is that the amino-modified silicone oil in this embodiment is commercially available amino silicone oil purchased from Shandong Yunxin New Material Technology Co., Ltd.
[0042] Example 5 The difference between this embodiment and embodiment 1 is that the amino-modified silicone oil in this embodiment is the amino-modified silicone oil prepared in preparation example 3.
[0043] Comparative Example Comparative Example 1 The difference between this comparative example and Example 1 is that in this comparative example, an equal amount of amino-modified silicone oil is used instead of acrylate-modified polyether silicone oil.
[0044] Performance testing application: The darkening silicone oil prepared in Examples 1-5 and Comparative Example 1 was used to finish black polyester fabric to obtain the finished fabric.
[0045] Finishing process: impregnation of polyester fabric (40 min) - one dip and one roll (bath ratio is 1:20, roll-off rate is 90%) - pre-baking (baking at 80°C for 3 min) - baking (baking at 150°C for 2 min).
[0046] The finished fabrics are tested for performance, including darkening rate, whiteness index, tear strength, and hand feel.
[0047] Darkening rate: Use a computer colorimeter to measure the K / S value of the fabric before and after darkening finishing, take the average value, and calculate the darkening rate. Darkening rate = (K / S 后 -K / S 前 ) / K / S 前 ×100%.
[0048] Whiteness index: The whiteness of the finished fabric is tested with a whiteness meter. Compared with the blank fabric, the whiteness index of the blank fabric is 77.01. The greater the whiteness of the finished fabric, the smaller the difference in whiteness with the blank fabric, which means that the degree of yellowing of the fabric is smaller.
[0049] Tear strength loss rate: According to GB / T 3923.1-2013 "Tensile properties of textile fabrics Part 1: Determination of breaking strength and elongation at break" standard, the tear strength of the fabric before and after finishing is tested, and the tear strength loss rate is calculated.
[0050] Feel: The fabric is evaluated by touching it with hands to feel the fluffiness, softness, resilience, smoothness and coolness after treatment. The feel is divided into 5 levels, the higher the level, the better, with 5 being the best and 1 being the lowest.
[0051] Table 1 Data Analysis: According to Table 1, the darkening silicone oil emulsion prepared in the present application has a high darkening rate for black polyester fabric, and the finished fabric has a good feel. Because acrylate-modified polyether silicone oil copolymer and amino silicone oil modified with hexafluorobutyl acrylate are added to the raw materials, the whiteness index of the fabric changes little, the fabric is less prone to yellowing, and the breaking strength loss rate of the fabric is small.
[0052] According to Example 4 and the examples, when the amino-modified silicone oil prepared in the present application is selected, due to the use of hexafluorobutyl acrylate for modification and the selection of the types of aminosilane coupling agent and silicone linear body in the raw materials, the darkening effect of the darkening silicone oil emulsion prepared by the amino-modified silicone oil in the present application is better, and the yellowing is better inhibited.
[0053] In Example 5, a specific combination of coupling agent HD-110 and terminal hydroxyl polydimethylsiloxane was selected for the raw materials of amino-modified silicone oil, and the performance of the prepared darkening silicone oil emulsion was the best.
[0054] This specific implementation manner is merely an explanation of the present application and is not a limitation of the present application. After reading this specification, those skilled in the art may make non-creative modifications to the specific implementation manner as needed, but such modifications are protected by the patent law as long as they are within the scope of the claims of the present application.
Claims
1. A silicone oil emulsion for darkening, characterized in that: The invention comprises the following raw materials in parts by weight: 55-70 parts of amino modified silicone oil; 30-45 parts of acrylate modified polyether silicone oil; Emulsifier 25-38 parts; 1-4 parts of organic acid; 220-260 parts of water; The acrylate-modified polyether silicone oil comprises the following raw materials in parts by weight: 10-18 parts of hydrogen silicone oil; 6-12 parts of allyl polyoxyethylene polyoxypropylene ether; 2-5 parts of acrylate monomer; Chloroplatinic acid 0.5-1 part; The acrylic acid ester monomer is selected from one or more of hydroxyethyl acrylate, N-hydroxyethyl acrylamide, and 4-hydroxybutyl acrylate.
2. A silicone oil emulsion according to claim 1, characterized in that: The amino-modified silicone oil comprises the following raw materials in parts by weight: 60-75 parts of silicone linear body; 2-4 parts of aminosilane coupling agent; 7-12 parts of capping agent; Catalyst 0.1-0.4 parts; Hexafluorobutyl acrylate 13-18 parts.
3. A silicone oil emulsion according to claim 2, characterized in that: The aminosilane coupling agent is selected from one or more of coupling agent HD-121, coupling agent HD-110, coupling agent KH-608.
4. A silicone oil emulsion according to claim 2, characterized in that: The organic silicon linear body is selected from one or more of terminal hydroxyl polydimethylsiloxane and trimethylsilane-terminated polydimethylsiloxane.
5. A silicone oil emulsion for darkening according to claim 2, characterized in that: The aminosilane coupling agent is coupling agent HD-110, and the organic silicon linear body is terminal hydroxyl polydimethylsiloxane.
6. A silicone oil emulsion for darkening according to claim 2, characterized in that: The catalyst is selected from one or more of potassium hydroxide, sodium hydroxide, and tetramethylammonium hydroxide.
7. A darkening silicone oil emulsion according to claim 1, characterized in that: The emulsifier is selected from one or more of isomeric tridecanol polyoxyethylene ether, lauryl alcohol polyoxyethylene ether, and isomeric decanol polyoxyethylene ether.
8. The darkening silicone oil emulsion according to claim 1, characterized in that: The organic acid is selected from one or more of acetic acid, glacial acetic acid and formic acid.
9. A method for preparing a darkening silicone oil emulsion according to any one of claims 1 to 8, characterized in that: The steps include: Add hydrogenated silicone oil and a certain amount of toluene into a flask, heat and stir, add chloroplatinic acid at 50-55°C, add a mixed solution of allyl polyoxyethylene polyoxypropylene ether and acrylate monomer dropwise into the flask at 87-90°C, continue the reaction for 5-6 hours, remove the solvent by distillation under reduced pressure, and obtain acrylate-modified polyether silicone oil; After mixing the acrylate-modified polyether silicone oil, amino-modified silicone oil and emulsifier, stir and emulsify for 20-30 minutes, add organic acid and water, and continue stirring for 2-2.5 hours to obtain a darkening silicone oil emulsion.
10. The method for preparing a darkening silicone oil emulsion according to claim 9, characterized in that: The amino-modified silicone oil is prepared by the following steps: Add organic silicon linear body and aminosilane coupling agent into the reaction bottle, stir and heat to 80-85°C, add end-capping agent and catalyst, stir at constant temperature for 2-3h, heat and vacuum, then cool to room temperature, add glacial acetic acid to neutralize to pH 6.5-7, and obtain aminosilicone oil; Amino silicone oil and a certain amount of toluene are placed in another reaction bottle, heated to 60-62°C under nitrogen protection, stirred and refluxed for 5-5.5 hours, hexafluorobutyl acrylate is added dropwise, reacted for 5-5.5 hours, and the solvent is removed by reduced pressure distillation to obtain amino-modified silicone oil.
Citation Information
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