Color paste for silicone adhesive and preparation method of color paste

Abstract

The invention belongs to the technical field of color paste, and particularly discloses a silicone adhesive color paste which comprises the following components in parts by weight: 0.2-0.5 part of dibutyltin diacetate, 4-8 parts of hydrogen-containing silicone oil, 16-22 parts of modified carbon black, 15-25 parts of epoxy-terminated silicone oil and 50-60 parts of dimethyl silicone oil. The color paste for the silicone adhesive is a silicone oil system (anhydrous), has excellent compatibility with the silicone adhesive, can effectively improve the color stability of the silicone adhesive after being added into the silicone adhesive, has good dispersity in the silicone adhesive system, has various reactive groups, has excellent stability, and can be used for preparing the silicone adhesive. Meanwhile, the aging resistance of the silicone adhesive can be improved, and the silicone adhesive has a wide application prospect in the silicone adhesive.

Description

Technical Field

[0001] The present invention relates to the technical field of color pastes, and in particular to a color paste for silicone adhesive and a preparation method thereof. Background Art

[0002] With the rapid development of industries such as construction, automobiles, and electronics, the demand for sealing and bonding materials is increasing. As a high-performance sealing and bonding material, silicone adhesive is widely used in various fields due to its excellent weather resistance, high and low temperature resistance, chemical corrosion resistance, and good elastic recovery ability. However, in order to meet the requirements of color and aesthetics in different applications, the research and development of color paste for silicone adhesive is particularly important.

[0003] At present, the research and development of silicone adhesives focuses on the design of silicone adhesive formula systems. There are many silicone adhesive color paste products on the market, but they still have some shortcomings in performance. For example, the color paste is prone to fading or discoloration, affecting the overall appearance and durability of the product; some color pastes have problems such as uneven dispersion and coarse particles during the preparation process, resulting in a decrease in the performance of silicone adhesives.

[0004] In view of this, this application is filed. Summary of the invention

[0005] The present invention provides a color paste for silicone adhesive and a preparation method thereof. The color paste has excellent compatibility with silicone adhesive, can effectively improve the storage stability of silicone adhesive, and has broad application prospects in silicone adhesive.

[0006] The present invention solves the technical problem by adopting the following technical solutions: A color paste for silicone adhesive comprises the following components in parts by weight: 0.2-0.5 parts of dibutyltin diacetate, 4-8 parts of hydrogen-containing silicone oil, 16-22 parts of modified carbon black, 15-25 parts of epoxy-terminated silicone oil, and 50-62 parts of dimethyl silicone oil.

[0007] The present invention combines the above-mentioned raw materials to obtain a color paste for silicone glue with excellent performance. The color paste for silicone glue is a silicone oil system (anhydrous) and has excellent compatibility with silicone glue. Adding it to silicone glue can effectively improve the color stability of silicone glue and has good dispersibility in the silicone glue system. At the same time, the color paste of the present invention has multiple reactive groups, which not only has excellent stability and improves storage stability, but also can improve the aging resistance of silicone glue, and has broad application prospects in silicone glue.

[0008] As a preferred embodiment of the present invention, the following components are included in parts by weight: 0.3 parts of dibutyltin diacetate, 5 parts of hydrogen-containing silicone oil, 20 parts of modified carbon black, 20 parts of terminal epoxy silicone oil, and 54.7 parts of dimethyl silicone oil.

[0009] As a preferred embodiment of the present invention, the preparation method of the modified carbon black is: (1) Add carbon black, sodium dodecylbenzene sulfonate and nitric acid solution into sulfuric acid solution and stir evenly to obtain a precursor solution; (2) Add 2-amino-6-methyl-4-pyrimidinol and dibutyltin dilaurate to isophorone diisocyanate, react at 65-80°C for 2-5 hours to obtain a modified solution; (3) Add γ-mercaptopropyltriethoxysilane, modifying liquid and stannous octoate to the precursor solution, adjust the pH to 8.5-9.5, react at 65-80°C for 2-5h, and dry to obtain modified carbon black.

[0010] The present invention creatively pre-treats carbon black with sodium dodecylbenzene sulfonate, nitric acid solution and sulfuric acid solution to effectively improve its activity and the content of its surface functional groups, reacts 2-amino-6-methyl-4-pyrimidinol with isophorone diisocyanate, wherein the 2-amino-6-methyl-4-pyrimidinol has an amino group and an imino group, and the isophorone diisocyanate has two NCO groups. One NCO group of the isophorone diisocyanate reacts with the amino group to obtain a modified liquid, and γ-mercaptopropyl triethoxysilane, the modified liquid and stannous octoate are added to the precursor liquid. Under alkaline conditions, the γ-mercaptopropyl triethoxysilane is adsorbed and grafted on the surface of carbon black, hydrolyzed to form silanol groups, and the silanol groups undergo a deprotonation reaction to generate silicon oxide anions (SiO - ) and hydrogen ions (H + ), the imino group acts as a nucleophilic reagent to carry out nucleophilic attack on the silicon oxygen anion to form a silicon nitrogen compound, and the reaction product of 2-amino-6-methyl-4-pyrimidinol and isophorone diisocyanate is grafted on the surface of carbon black. The other NCO group of the isophorone diisocyanate can react with the terminal epoxy silicone oil in the system. Through ingenious design, the performance of carbon black is effectively improved, its stability and compatibility are improved, its dispersibility and stability in silicone glue are improved, and the aging resistance of silicone glue can be effectively improved.

[0011] Wherein, the molar concentration of the nitric acid solution is 1-5 mol / L.

[0012] Wherein, the molar concentration of the sulfuric acid solution is 1-5 mol / L.

[0013] As a preferred embodiment of the present invention, the mass ratio of the carbon black, sodium dodecylbenzene sulfonate, nitric acid solution and sulfuric acid solution is 1: (0.1-0.3): (0.2-0.4): (2-6).

[0014] As a preferred embodiment of the present invention, the mass ratio of 2-amino-6-methyl-4-pyrimidinol, dibutyltin dilaurate and isophorone diisocyanate is 1:(3-6):(0.02-0.05).

[0015] As a preferred embodiment of the present invention, the mass ratio of the γ-mercaptopropyltriethoxysilane, the modifying liquid, stannous octoate, and the precursor liquid is (0.1-0.3):(0.2-0.5):(0.01-0.03):1.

[0016] As a preferred embodiment of the present invention, the viscosity of the epoxy-terminated silicone oil at 25° C. is 140-300 mPa·s, and the epoxy value is 0.018-0.028 mol / 100 g.

[0017] As a preferred embodiment of the present invention, the dimethyl silicone oil has a viscosity of 350-500 mPa·s at 25° C. and a molecular weight of 13650-17250.

[0018] As a preferred embodiment of the present invention, the hydrogen-containing silicone oil has a viscosity of 15-30 mPa·s at 25° C. and a hydrogen content of 1.58-1.62 wt %.

[0019] The present invention also provides a method for preparing a color paste for silicone adhesive, comprising the following steps: Add dibutyltin diacetate, hydrogen-containing silicone oil, modified carbon black, and terminal epoxy silicone oil to dimethyl silicone oil, react at 55-70°C for 2-6 hours, grind the mixture with a sand mill to a particle size of less than 0.25 μm, and obtain a color paste for silicone glue.

[0020] Beneficial effects of the present invention: the color paste for silicone adhesive of the present invention is a silicone oil system (anhydrous), which has excellent compatibility with silicone adhesive. Adding it to silicone adhesive can effectively improve the color stability of silicone adhesive and has good dispersibility in the silicone adhesive system. At the same time, the color paste of the present invention has multiple reactive groups, which not only has excellent stability and improves storage stability, but also can improve the aging resistance of silicone adhesive, and has broad application prospects in silicone adhesive. DETAILED DESCRIPTION

[0021] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the present invention, not 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.

[0022] In the present invention, the technical features described in an open manner include closed technical solutions composed of the listed features, and also include open technical solutions containing the listed features.

[0023] In the present invention, when it comes to numerical ranges, unless otherwise specified, the above numerical ranges are deemed to be continuous and include the minimum and maximum values ​​of the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values ​​of the range is included. In addition, when multiple ranges are provided to describe features or characteristics, the ranges can be merged. In other words, unless otherwise specified, all ranges disclosed herein should be understood to include any and all subranges included therein.

[0024] In the present invention, there is no particular limitation on the specific dispersion and stirring treatment methods.

[0025] The reagents or instruments used in the present invention without indicating the manufacturer are all conventional products that can be obtained commercially. The raw materials used in the comparative examples and the raw materials used in the parallel experiments of the embodiments are the same commercially available products unless otherwise specified.

[0026] The sources of the raw materials of the embodiments and comparative examples are as follows: Hydrogen-containing silicone oil: The viscosity at 25°C is 15~30mPa·s, the hydrogen content is 1.58~1.62wt%, Jiangxi Xinjiayi New Materials, model: XJY-701.

[0027] Epoxy-terminated silicone oil-1: The viscosity at 25°C is 140~190mPa·s, the epoxy value is 0.025~0.028mol / 100g, Shanghai Yandi New Materials, model: 276-8K.

[0028] Epoxy-terminated silicone oil-2: The viscosity at 25°C is 220~300mPa·s, the epoxy value is 0.018~0.021mol / 100g, Shanghai Yandi New Materials, model: 276-10K.

[0029] Dimethyl silicone oil-1: The viscosity at 25°C is 350 mPa·s, the molecular weight is 13650, Jiangxi Ke Rui New Materials, model: 201-350.

[0030] Dimethyl silicone oil-2: The viscosity at 25°C is 500mPa·s, the molecular weight is 17250, Jiangxi Kerui New Materials, model: 201-500.

[0031] Dimethyl silicone oil-3: The viscosity at 25°C is 1000mPa·s, the molecular weight is 28000, Jiangxi Kerui New Materials, model: 201-1000.

[0032] Dimethyl silicone oil-4: viscosity at 25°C is 100mPa·s, molecular weight is 5970, Jiangxi Ke Rui New Materials, model: 201-100.

[0033] Carbon black: Tianjin Jindadi Chemical, model: S666.

[0034] Example 1 A color paste for silicone adhesive comprises the following components in parts by weight: 0.3 parts of dibutyltin diacetate, 5 parts of hydrogen-containing silicone oil, 20 parts of modified carbon black, 20 parts of terminal epoxy silicone oil-1, and 54.7 parts of dimethyl silicone oil-1.

[0035] The preparation method of the modified carbon black is: (1) Add carbon black, sodium dodecylbenzene sulfonate, and 2 mol / L nitric acid solution to 4 mol / L sulfuric acid solution, and stir evenly at 300 rpm to obtain a precursor solution; the mass ratio of the carbon black, sodium dodecylbenzene sulfonate, nitric acid solution, and sulfuric acid solution is 1:0.2:0.3:5.

[0036] (2) adding 2-amino-6-methyl-4-pyrimidinol and dibutyltin dilaurate to isophorone diisocyanate, reacting at 75° C. for 4 hours to obtain a modified liquid; the mass ratio of the 2-amino-6-methyl-4-pyrimidinol, dibutyltin dilaurate and isophorone diisocyanate is 1:5:0.04; (3) Add γ-mercaptopropyl triethoxysilane, modifying liquid, and stannous octoate to the precursor solution, adjust the pH to 9 with 1 mol / L sodium hydroxide solution, react at 75°C for 4 hours, and dry to obtain modified carbon black. The mass ratio of γ-mercaptopropyl triethoxysilane, modifying liquid, stannous octoate, and precursor solution is 0.2:0.4:0.02:1.

[0037] The method for preparing the color paste for silicone adhesive comprises the following steps: Add dibutyltin diacetate, hydrogen-containing silicone oil, modified carbon black, and terminal epoxy silicone oil-1 to dimethyl silicone oil-1, react at 65° C. for 4 hours, grind the mixture with a sand mill to a particle size of less than 0.25 μm, and obtain a color paste for silicone glue.

[0038] Example 2 A color paste for silicone adhesive comprises the following components in parts by weight: 0.2 parts of dibutyltin diacetate, 8 parts of hydrogen-containing silicone oil, 16 parts of modified carbon black, 15 parts of epoxy-terminated silicone oil, and 60.8 parts of dimethyl silicone oil-1.

[0039] The preparation method of the modified carbon black is: (1) Add carbon black, sodium dodecylbenzene sulfonate, and 2 mol / L nitric acid solution to 4 mol / L sulfuric acid solution, and stir evenly at 300 rpm to obtain a precursor solution; the mass ratio of the carbon black, sodium dodecylbenzene sulfonate, nitric acid solution, and sulfuric acid solution is 1:0.2:0.3:5.

[0040] (2) adding 2-amino-6-methyl-4-pyrimidinol and dibutyltin dilaurate to isophorone diisocyanate, reacting at 75° C. for 4 hours to obtain a modified liquid; the mass ratio of the 2-amino-6-methyl-4-pyrimidinol, dibutyltin dilaurate and isophorone diisocyanate is 1:5:0.04; (3) Add γ-mercaptopropyl triethoxysilane, modifying liquid, and stannous octoate to the precursor solution, adjust the pH to 9 with 1 mol / L sodium hydroxide solution, react at 75°C for 4 hours, and dry to obtain modified carbon black. The mass ratio of γ-mercaptopropyl triethoxysilane, modifying liquid, stannous octoate, and precursor solution is 0.2:0.4:0.02:1.

[0041] The method for preparing the color paste for silicone adhesive comprises the following steps: Add dibutyltin diacetate, hydrogen-containing silicone oil, modified carbon black, and terminal epoxy silicone oil-1 to dimethyl silicone oil-1, react at 65° C. for 4 hours, grind the mixture with a sand mill to a particle size of less than 0.25 μm, and obtain a color paste for silicone glue.

[0042] Example 3 A color paste for silicone adhesive comprises the following components in parts by weight: 0.5 parts of dibutyltin diacetate, 4 parts of hydrogen-containing silicone oil, 22 parts of modified carbon black, 25 parts of epoxy-terminated silicone oil, and 48.5 parts of dimethyl silicone oil-1.

[0043] The preparation method of the modified carbon black is: (1) Add carbon black, sodium dodecylbenzene sulfonate, and 2 mol / L nitric acid solution to 4 mol / L sulfuric acid solution, and stir evenly at 300 rpm to obtain a precursor solution; the mass ratio of the carbon black, sodium dodecylbenzene sulfonate, nitric acid solution, and sulfuric acid solution is 1:0.2:0.3:5.

[0044] (2) adding 2-amino-6-methyl-4-pyrimidinol and dibutyltin dilaurate to isophorone diisocyanate, reacting at 75° C. for 4 hours to obtain a modified liquid; the mass ratio of the 2-amino-6-methyl-4-pyrimidinol, dibutyltin dilaurate and isophorone diisocyanate is 1:5:0.04; (3) Add γ-mercaptopropyl triethoxysilane, modifying liquid, and stannous octoate to the precursor solution, adjust the pH to 9 with 1 mol / L sodium hydroxide solution, react at 75°C for 4 hours, and dry to obtain modified carbon black. The mass ratio of γ-mercaptopropyl triethoxysilane, modifying liquid, stannous octoate, and precursor solution is 0.2:0.4:0.02:1.

[0045] The method for preparing the color paste for silicone adhesive comprises the following steps: Add dibutyltin diacetate, hydrogen-containing silicone oil, modified carbon black, and terminal epoxy silicone oil-1 to dimethyl silicone oil-1, react at 65° C. for 4 hours, grind the mixture with a sand mill to a particle size of less than 0.25 μm, and obtain a color paste for silicone glue.

[0046] Example 4 A color paste for silicone adhesive comprises the following components in parts by weight: 0.3 parts of dibutyltin diacetate, 5 parts of hydrogen-containing silicone oil, 20 parts of modified carbon black, 20 parts of terminal epoxy silicone oil-2, and 54.7 parts of dimethyl silicone oil-1.

[0047] The preparation method of the modified carbon black is: (1) Add carbon black, sodium dodecylbenzene sulfonate, and 2 mol / L nitric acid solution to 4 mol / L sulfuric acid solution, and stir evenly at 300 rpm to obtain a precursor solution; the mass ratio of the carbon black, sodium dodecylbenzene sulfonate, nitric acid solution, and sulfuric acid solution is 1:0.2:0.3:5.

[0048] (2) adding 2-amino-6-methyl-4-pyrimidinol and dibutyltin dilaurate to isophorone diisocyanate, reacting at 75° C. for 4 hours to obtain a modified liquid; the mass ratio of the 2-amino-6-methyl-4-pyrimidinol, dibutyltin dilaurate and isophorone diisocyanate is 1:5:0.04; (3) Add γ-mercaptopropyl triethoxysilane, modifying liquid, and stannous octoate to the precursor solution, adjust the pH to 9 with 1 mol / L sodium hydroxide solution, react at 75°C for 4 hours, and dry to obtain modified carbon black. The mass ratio of γ-mercaptopropyl triethoxysilane, modifying liquid, stannous octoate, and precursor solution is 0.2:0.4:0.02:1.

[0049] The method for preparing the color paste for silicone adhesive comprises the following steps: Add dibutyltin diacetate, hydrogenated silicone oil, modified carbon black, and epoxy-terminated silicone oil-2 to dimethyl silicone oil-1, react at 65° C. for 4 hours, grind the mixture with a sand mill to a particle size of less than 0.25 μm, and obtain a color paste for silicone glue.

[0050] Example 5 A color paste for silicone adhesive comprises the following components in parts by weight: 0.3 parts of dibutyltin diacetate, 5 parts of hydrogen-containing silicone oil, 20 parts of modified carbon black, 20 parts of terminal epoxy silicone oil-1, and 54.7 parts of dimethyl silicone oil-2.

[0051] The preparation method of the modified carbon black is: (1) Add carbon black, sodium dodecylbenzene sulfonate, and 2 mol / L nitric acid solution to 4 mol / L sulfuric acid solution, and stir evenly at 300 rpm to obtain a precursor solution; the mass ratio of the carbon black, sodium dodecylbenzene sulfonate, nitric acid solution, and sulfuric acid solution is 1:0.2:0.3:5.

[0052] (2) adding 2-amino-6-methyl-4-pyrimidinol and dibutyltin dilaurate to isophorone diisocyanate, reacting at 75° C. for 4 hours to obtain a modified liquid; the mass ratio of the 2-amino-6-methyl-4-pyrimidinol, dibutyltin dilaurate and isophorone diisocyanate is 1:5:0.04; (3) Add γ-mercaptopropyl triethoxysilane, modifying liquid, and stannous octoate to the precursor solution, adjust the pH to 9 with 1 mol / L sodium hydroxide solution, react at 75°C for 4 hours, and dry to obtain modified carbon black. The mass ratio of γ-mercaptopropyl triethoxysilane, modifying liquid, stannous octoate, and precursor solution is 0.2:0.4:0.02:1.

[0053] The method for preparing the color paste for silicone adhesive comprises the following steps: Add dibutyltin diacetate, hydrogen-containing silicone oil, modified carbon black, and terminal epoxy silicone oil-1 to dimethyl silicone oil-2, react at 65° C. for 4 hours, grind the mixture with a sand mill to a particle size of less than 0.25 μm, and obtain a color paste for silicone glue.

[0054] Example 6 A color paste for silicone adhesive comprises the following components in parts by weight: 0.3 parts of dibutyltin diacetate, 5 parts of hydrogen-containing silicone oil, 20 parts of modified carbon black, 20 parts of terminal epoxy silicone oil-1, and 54.7 parts of dimethyl silicone oil-3.

[0055] The preparation method of the modified carbon black is: (1) Add carbon black, sodium dodecylbenzene sulfonate, and 2 mol / L nitric acid solution to 4 mol / L sulfuric acid solution, and stir evenly at 300 rpm to obtain a precursor solution; the mass ratio of the carbon black, sodium dodecylbenzene sulfonate, nitric acid solution, and sulfuric acid solution is 1:0.2:0.3:5.

[0056] (2) adding 2-amino-6-methyl-4-pyrimidinol and dibutyltin dilaurate to isophorone diisocyanate, reacting at 75° C. for 4 hours to obtain a modified liquid; the mass ratio of the 2-amino-6-methyl-4-pyrimidinol, dibutyltin dilaurate and isophorone diisocyanate is 1:5:0.04; (3) Add γ-mercaptopropyl triethoxysilane, modifying liquid, and stannous octoate to the precursor solution, adjust the pH to 9 with 1 mol / L sodium hydroxide solution, react at 75°C for 4 hours, and dry to obtain modified carbon black. The mass ratio of γ-mercaptopropyl triethoxysilane, modifying liquid, stannous octoate, and precursor solution is 0.2:0.4:0.02:1.

[0057] The method for preparing the color paste for silicone adhesive comprises the following steps: Add dibutyltin diacetate, hydrogen-containing silicone oil, modified carbon black, and terminal epoxy silicone oil-1 to dimethyl silicone oil-3, react at 65°C for 4 hours, grind the mixture with a sand mill to a particle size of less than 0.25 μm, and obtain a color paste for silicone glue.

[0058] Example 7 A color paste for silicone adhesive comprises the following components in parts by weight: 0.3 parts of dibutyltin diacetate, 5 parts of hydrogen-containing silicone oil, 20 parts of modified carbon black, 20 parts of terminal epoxy silicone oil-1, and 54.7 parts of dimethyl silicone oil-4.

[0059] The preparation method of the modified carbon black is: (1) Add carbon black, sodium dodecylbenzene sulfonate, and 2 mol / L nitric acid solution to 4 mol / L sulfuric acid solution, and stir evenly at 300 rpm to obtain a precursor solution; the mass ratio of the carbon black, sodium dodecylbenzene sulfonate, nitric acid solution, and sulfuric acid solution is 1:0.2:0.3:5.

[0060] (2) adding 2-amino-6-methyl-4-pyrimidinol and dibutyltin dilaurate to isophorone diisocyanate, reacting at 75° C. for 4 hours to obtain a modified liquid; the mass ratio of the 2-amino-6-methyl-4-pyrimidinol, dibutyltin dilaurate and isophorone diisocyanate is 1:5:0.04; (3) Add γ-mercaptopropyl triethoxysilane, modifying liquid, and stannous octoate to the precursor solution, adjust the pH to 9 with 1 mol / L sodium hydroxide solution, react at 75°C for 4 hours, and dry to obtain modified carbon black. The mass ratio of γ-mercaptopropyl triethoxysilane, modifying liquid, stannous octoate, and precursor solution is 0.2:0.4:0.02:1.

[0061] The method for preparing the color paste for silicone adhesive comprises the following steps: Add dibutyltin diacetate, hydrogen-containing silicone oil, modified carbon black, and terminal epoxy silicone oil-1 to dimethyl silicone oil-4, react at 65° C. for 4 hours, grind the mixture with a sand mill to a particle size of less than 0.25 μm, and obtain a color paste for silicone glue.

[0062] Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that Comparative Example 1 uses an equal amount of carbon black to replace the modified carbon black.

[0063] A color paste for silicone adhesive comprises the following components in parts by weight: 0.3 parts of dibutyltin diacetate, 5 parts of hydrogen-containing silicone oil, 20 parts of carbon black, 20 parts of terminal epoxy silicone oil-1, and 54.7 parts of dimethyl silicone oil-1.

[0064] Comparative Example 2 The difference between Comparative Example 2 and Example 1 is that the preparation method of the modified carbon black in Comparative Example 2 is different from that in Example 1, and the others are the same.

[0065] The preparation method of the modified carbon black is: (1) Add carbon black, sodium dodecylbenzene sulfonate, and 2 mol / L nitric acid solution to 4 mol / L sulfuric acid solution, stir evenly at 300 rpm to obtain a precursor solution, and dry to obtain modified carbon black; the mass ratio of the carbon black, sodium dodecylbenzene sulfonate, nitric acid solution, and sulfuric acid solution is 1:0.2:0.3:5.

[0066] Comparative Example 3 The difference between Comparative Example 3 and Example 1 is that the preparation method of the modified carbon black in Comparative Example 3 is different from that in Example 1, and the others are the same.

[0067] The preparation method of the modified carbon black is: (1) Add carbon black, sodium dodecylbenzene sulfonate, and 2 mol / L nitric acid solution to 4 mol / L sulfuric acid solution, and stir evenly at 300 rpm to obtain a precursor solution; the mass ratio of the carbon black, sodium dodecylbenzene sulfonate, nitric acid solution, and sulfuric acid solution is 1:0.2:0.3:5.

[0068] (2) Add γ-mercaptopropyl triethoxysilane and stannous octoate to the precursor solution, adjust the pH to 9 with 1 mol / L sodium hydroxide solution, react at 75°C for 4 hours, and dry to obtain modified carbon black. The mass ratio of γ-mercaptopropyl triethoxysilane, stannous octoate and the precursor solution is 0.2:0.02:1.

[0069] Comparative Example 4 The difference between Comparative Example 4 and Example 1 is that Comparative Example 4 uses an equal amount of dimethyl silicone oil to replace the terminal epoxy silicone oil.

[0070] A color paste for silicone adhesive comprises the following components in parts by weight: 0.3 parts of dibutyltin diacetate, 5 parts of hydrogen-containing silicone oil, 20 parts of carbon black, and 74.7 parts of dimethyl silicone oil-1.

[0071] Test Case 1. Stability test: The color pastes prepared in the examples and comparative examples were placed at 25° C. for 180 days, and the stability of the pigment color pastes was determined by visually observing whether there was obvious precipitation, flocculation, stratification, or agglomeration of pigment particles.

[0072] 2. The relative tinting strength changes of the color pastes prepared in the examples and comparative examples were tested according to method B (instrumental method) described in Appendix B of HG / T 3951-2007, one day after preparation and after storage at 25°C for 180 days. The color paste prepared in each example and comparative example one day after preparation was used as the standard color paste, and its tinting strength was 100%. The relative tinting strength of the corresponding color paste after storage at room temperature for 180 days was tested.

[0073] Table 1

[0074] It can be seen from Table 1 that the color paste for silicone adhesive of the present invention has excellent stability and color retention.

[0075] Finally, it should be noted that the above embodiments are intended to illustrate the technical solution of the present invention rather than to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solution of the present invention may be modified or replaced by equivalents without departing from the essence and scope of the technical solution of the present invention.

Claims

1. A color paste for silicone adhesive, It is characterized in that The invention comprises the following components in parts by weight: 0.2-0.5 parts of dibutyltin diacetate, 4-8 parts of hydrogen-containing silicone oil, 16-22 parts of modified carbon black, 15-25 parts of epoxy-terminated silicone oil and 50-62 parts of dimethyl silicone oil.

2. The color paste for silicone adhesive according to claim 1, It is characterized in that The invention comprises the following components in parts by weight: 0.3 parts of dibutyltin diacetate, 5 parts of hydrogen-containing silicone oil, 20 parts of modified carbon black, 20 parts of epoxy-terminated silicone oil and 54.7 parts of dimethyl silicone oil.

3. The color paste for silicone adhesive according to claim 1, It is characterized in that The preparation method of the modified carbon black is: (1) Add carbon black, sodium dodecylbenzene sulfonate and nitric acid solution into sulfuric acid solution and stir evenly to obtain a precursor solution; (2) Add 2-amino-6-methyl-4-pyrimidinol and dibutyltin dilaurate to isophorone diisocyanate, react at 65-80°C for 2-5 hours to obtain a modified solution; (3) Add γ-mercaptopropyltriethoxysilane, modifying liquid and stannous octoate to the precursor solution, adjust the pH to 8.5-9.5, react at 65-80°C for 2-5h, and dry to obtain modified carbon black.

4. The color paste for silicone adhesive according to claim 3, It is characterized in that The mass ratio of the carbon black, sodium dodecylbenzene sulfonate, nitric acid solution and sulfuric acid solution is 1: (0.1-0.3): (0.2-0.4): (2-6).

5. The color paste for silicone adhesive according to claim 3, It is characterized in that The mass ratio of the 2-amino-6-methyl-4-pyrimidinol, dibutyltin dilaurate and isophorone diisocyanate is 1:(3-6):(0.02-0.05).

6. The color paste for silicone adhesive according to claim 3, It is characterized in that The mass ratio of the γ-mercaptopropyltriethoxysilane, the modifying liquid, stannous octoate and the precursor liquid is (0.1-0.3):(0.2-0.5):(0.01-0.03):

1.

7. The color paste for silicone adhesive according to claim 1, It is characterized in that The epoxy-terminated silicone oil has a viscosity of 140-300 mPa·s at 25° C. and an epoxy value of 0.018-0.028 mol / 100 g.

8. The color paste for silicone adhesive according to claim 1, It is characterized in that The dimethyl silicone oil has a viscosity of 350-500 mPa·s at 25° C. and a molecular weight of 13650-17250.

9. The color paste for silicone adhesive according to claim 1, It is characterized in that The hydrogen-containing silicone oil has a viscosity of 15-30 mPa·s at 25° C. and a hydrogen content of 1.58-1.62 wt %.

10. The method for preparing the color paste for silicone adhesive according to any one of claims 1 to 9, It is characterized in that The following steps are involved: Add dibutyltin diacetate, hydrogen-containing silicone oil, modified carbon black, and terminal epoxy silicone oil to dimethyl silicone oil, react at 55-70°C for 2-6 hours, grind the mixture with a sand mill to a particle size of less than 0.25 μm, and obtain a color paste for silicone glue.

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