Organic silicon rubber pressure-sensitive adhesive color paste and preparation method thereof

By combining methyl MQ silicone resin, silicone rubber, modified tackifying resin, modified toner and other components, combined with 2,6-di-tert-butyl p-cresol modified p-tert-octyl p-phenol formaldehyde resin and Modified nano-color powder solves the problem of discoloration of silicone rubber color paste, and realizes high stability and environmentally friendly silicone rubber pressure-sensitive glue color paste, suitable for applications under high temperature and high humidity conditions.

CN119264736APending Publication Date: 2025-01-07明光科迪纳微新材料股份有限公司 +1

Patent Information

Application Number
CN202411278999.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-09-12
Publication Date
2025-01-07

AI Technical Summary

Technical Problem

The existing silicone rubber pressure-sensitive glue color paste is prone to discoloration when used outdoors, and the addition of too much antioxidant causes other components of the system to be dispersed, which affects the use effect of the color paste. The preparation steps are cumbersome and do not meet the requirements of green and environmental protection.

Method used

20-22 parts of methyl MQ silicone resin, 20-23 parts of silicone rubber, 20-25 parts of modified tackifying resin, 20-25 parts of solvent, 37-38 parts of modified toner, 3-5 parts of anti-resistance The combination of oxidant, 2-3 parts of dispersant, 1-2 parts of ultraviolet absorber is improved by using the use of 2,6-di-tert-butyl p-cresol modified p-tert-octylphenol formaldehyde resin and modified nano-color powder. The antioxidant and dispersibility of the color paste can prepare stable and environmentally friendly silicone rubber pressure-sensitive glue color paste.

Benefits of technology

It realizes the high stability and environmental protection performance of the pressure-sensitive adhesive color paste of silicone rubber, improves the oxidation resistance and dispersion of the color paste, ensures the use effect under high temperature and high humidity conditions, and meets the requirements of green and environmental protection.

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Abstract

The invention relates to an organic silicon rubber pressure-sensitive adhesive color paste technology and a preparation method thereof, and the organic silicon rubber pressure-sensitive adhesive color paste is prepared from the following raw materials in parts by mass: 20-22 parts of methyl MQ organic silicon resin, 20-23 parts of organic silicon rubber, 20-25 parts of modified tackifying resin, 1-2 parts of a curing agent, 1-2 parts of a defoaming agent, 1-2 parts of a defoaming agent, and 1-2 parts of a defoaming agent. 20-25 parts of a solvent, 37-38 parts of modified toner, 3-5 parts of an antioxidant, 2-3 parts of a dispersing agent and 1-2 parts of an ultraviolet absorbent. According to the technical scheme, the anti-yellowing capacity of the color paste is improved by using 2, 6-butylated hydroxytoluene modified p-tert-octylphenol formaldehyde resin, and the stability of the color paste is improved by selecting specific modified tackifying resin and modified toner and adding the modified color paste.
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Description

Technical Field

[0001] The invention relates to the technical field of silicone rubber pressure-sensitive adhesive color paste, and in particular to an organosilicon rubber pressure-sensitive adhesive color paste and a preparation method thereof. Background Art

[0002] As people's demand for environmentally friendly, high-performance coatings and inks increases, silicone rubber pressure-sensitive adhesive color pastes are favored by the market due to their excellent weather resistance, chemical resistance, temperature resistance and environmental protection performance. Therefore, it is expected that the silicone rubber pressure-sensitive adhesive color paste market will continue to maintain a growth trend in the next few years.

[0003] With the revolutionary breakthrough of artificial intelligence and the rapid development of technologies such as sensors, chips, and wireless communications, wearable device technology is becoming more mature and its application scenarios are becoming more extensive. At a time when medical reforms and people's health awareness and entertainment needs are growing, the wearable device industry is experiencing a blowout growth. In the field of wireless charging, pressure-sensitive tape helps to bond, fix and protect the modules of the receiving and transmitting ends, so that they can play an energy-efficient role. In the display field, optical pressure-sensitive adhesives are used inside the screen to bond various optical materials, so that they can still maintain optical transparency under high temperature and high humidity conditions and ensure the clarity of imaging. Pressure-sensitive adhesives mainly include polyacrylates, polyurethanes, polyvinyl chlorides, polyvinyl ethers, silicone resins, etc. Silicone-type pressure-sensitive adhesives are increasingly used in daily life because of their excellent high temperature resistance and aging resistance. According to different application scenarios in reality, we often need to change the color of silicone rubber pressure-sensitive adhesives, which makes the application scenarios of silicone rubber pressure-sensitive adhesive color pastes more and more. However, since silicone rubber pressure-sensitive adhesives are often used outdoors, they are prone to discoloration as time goes by. If too much antioxidant is added, it will cause other components of the system to be difficult to disperse, affecting the use effect of the color paste. In CN202211251766, the active groups of the active dye are reacted with the amino coupling agent to improve the stability of the dye state. However, due to the complicated preparation steps and the difficulty in obtaining the chemical raw materials used, it does not meet the current national green environmental protection requirements.

[0004] Therefore, it is particularly necessary to develop a stable and environmentally friendly silicone rubber pressure-sensitive adhesive color paste. Summary of the invention

[0005] The purpose of the present invention is to provide a highly stable organic silicone rubber pressure-sensitive adhesive color paste and a preparation method thereof.

[0006] In order to achieve the above-mentioned purpose, the present invention provides the following technical scheme: a silicone rubber pressure-sensitive adhesive color paste, comprising at least the following components in parts by mass: 20-22 parts of methyl MQ silicone resin, 20-23 parts of silicone rubber, 20-25 parts of modified tackifying resin, 20-25 parts of solvent, 37-38 parts of modified color powder, 3-5 parts of antioxidant, 2-3 parts of dispersant, and 1-2 parts of ultraviolet absorber.

[0007] As a preferred technical solution, the modified tackifying resin is 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin.

[0008] As a preferred technical solution, the preparation method of 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin comprises at least the following steps: a) Add tert-octylphenol formaldehyde resin to toluene at 20-25°C and stir for 2 hours to mix evenly to obtain solution A; b) 20-25°C, slowly add 2,6-di-tert-butyl-p-cresol to toluene and stir for 2 hours using a stirrer to obtain a solution B; c) After adding macroporous strongly acidic cation exchange resin to solution B, the temperature was raised to 50°C, dispersion A was added dropwise to solution B, and solution C was obtained after stirring for 2 hours; d) Solution C was filtered to obtain solution D; e) Solution D is distilled at 60-65° C. and a vacuum degree of 20000 Pa to obtain 2,6-di-tert-butyl-p-cresol-modified p-tert-octylphenol formaldehyde resin.

[0009] As a preferred technical solution, the mass ratio of the 2,6-di-tert-butyl-p-cresol (melting point ≥71°C), p-tert-octylphenol formaldehyde resin (softening point of 90-100°C, hydroxymethyl content of 9-12wt%), macroporous strongly acidic cation exchange resin (particle size of 0.45-1.25mm), and toluene is 5-8:40-45:1-2:300-350.

[0010] As a preferred technical solution, the methyl MQ silicone resin is selected from a M:Q ratio of 0.7:1-1:1.

[0011] As a preferred technical solution, the solvent is selected from at least one of benzene, toluene and xylene.

[0012] As a preferred technical solution, the modified color powder is a modified nano color powder, and the color powder can be selected from at least one of: amaranth, carmine, erythrosine, new red, lemon yellow, sunset yellow, indigo yellow, brilliant blue, titanium dioxide, zinc oxide, and lithopone.

[0013] As a preferred technical solution, the method for preparing the modified nano-color powder comprises at least the following steps: a) Add 0.3-0.5 mm zirconium oxide beads to the ball mill and mill at 400-500 r / min for 1-2 hours; b) Initial filtration test: Filter the ground toner and test the fineness to ensure that the fineness of the toner is between 0.05μm and 0.50μm. If the fineness of the color paste is greater than 0.50μm, repeat the grinding.

[0014] As a preferred technical solution, the antioxidants are antioxidant 168 and antioxidant 1010, wherein the mass ratio of antioxidant 168 to antioxidant 1010 is 1:2.

[0015] As a preferred technical solution, the dispersant is a polyacrylate ammonium salt dispersant.

[0016] As a preferred solution, the ultraviolet absorber is selected from at least one of the ultraviolet absorber 234 and the ultraviolet absorber 622 .

[0017] As a preferred solution, the organic silicone rubber is organic silicone 107 rubber.

[0018] The steps for preparing silicone rubber pressure-sensitive adhesive color paste are as follows: Step S1: Weigh the solvent, methyl MQ silicone resin, silicone rubber, antioxidant, dispersant, UV absorber, modified color powder, and modified tackifying resin respectively, put them into a mixing container and stir them evenly; obtain mixture 1, Step S2: Transfer the mixture 1 to a high-speed disperser and mix it again, then put it into a centrifugal sand mill for grinding. Grind continuously for 7 hours, control the grinding temperature not higher than 45°C, and obtain a color paste particle size D50 less than 90nm to obtain a uniform mixture.

[0019] M: monofunctional siloxane unit; Q: tetrafunctional siloxane unit.

[0020] Beneficial Effects The present invention provides a silicone rubber pressure-sensitive adhesive color paste and a preparation method thereof. The present invention compounds multiple components to synergistically enhance the synergy. The antioxidant property of the color paste is improved by using 2,6-di-tert-butyl-p-cresol to modify p-tert-octylphenol formaldehyde resin, and the dispersibility of the color powder is improved by using modified nano-color powder, thereby improving the stability of the color paste. DETAILED DESCRIPTION

[0021] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. 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] Example 1 The method for preparing the silicone rubber pressure-sensitive adhesive color paste in this embodiment is as follows: 1. First, prepare modified 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin: a) At 23°C, add 40 parts of tert-octylphenol formaldehyde resin to 300 parts of toluene, and stir for 2 hours using a stirrer to mix evenly to obtain solution A; b) 22 ° C, 5 parts of 2,6-di-tert-butyl-p-cresol was slowly added to 50 parts of toluene, and stirred for 2 hours using a stirrer to obtain a solution B; c) After adding 1 part of macroporous strong acidic cation exchange resin to solution B, the temperature was raised to 50°C, and dispersion A was added dropwise to solution B, and stirred for 2 hours to obtain solution C; d) Solution C was filtered to obtain solution D; e) Toluene is removed by distillation at 63° C. and a vacuum degree of 20,000 Pa to obtain 2,6-di-tert-butyl-p-cresol-modified p-tert-octylphenol formaldehyde resin.

[0023] The 2,6-di-tert-butyl-p-cresol (melting point ≥ 71°C) was purchased from LANXESS, Germany, with the brand name Antioxidant 264; 4-tert-octylphenol formaldehyde resin (softening point of 90-100°C, hydroxymethyl content of 9-12%) was purchased from Wuhan Haishan, with the brand name WL-2203; macroporous strong acid cation exchange resin (effective particle size of 0.45-1.25 mm) was purchased from Anhui Wanshu Chemical Sales Co., Ltd., with the brand name: D001H.

[0024] 2. The method for preparing modified zinc oxide nano-color powder is as follows; a) Take 10 parts of zinc oxide and add it into a ball mill, then add 0.4 mm zirconium oxide beads as a grinding aid, and ball mill at 400 r / min for 1.5 hours; b) Filtration test shows that the fineness of the toner is 0.2μm, which meets the fineness requirements.

[0025] The zinc oxide was purchased from Hebei Zhiyi Co., Ltd., with the brand name Type 1.

[0026] Take 20 parts of methyl MQ silicone resin with an MQ ratio of 1:1, 21 parts of 107 silicone rubber, 23 parts of modified tackifying resin, 22 parts of toluene, 7 parts of modified zinc oxide color powder, 1 part of antioxidant 168, 2 parts of antioxidant 1010, 2 parts of polyacrylate ammonium salt dispersant, and 1 part of ultraviolet absorber 234; the modified tackifying resin is 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin, and the modified color powder is modified nano color powder. Add the above components into a mixing container and stir evenly to obtain a mixture 1; then transfer the mixture 1 to a high-speed disperser and mix it again evenly, then put it into a centrifugal separation sand mill for grinding, grind continuously for 7 hours, control the grinding temperature at 40°C, and obtain a uniform mixture.

[0027] Comparative Example 1 1. First, prepare modified 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin, the steps are as follows: a) At 23°C, add 40 parts of tert-octylphenol formaldehyde resin to 300 parts of toluene, and stir for 2 hours using a stirrer to mix evenly to obtain solution A; b) 22 ° C, 5 parts of 2,6-di-tert-butyl-p-cresol was slowly added to 50 parts of toluene, and stirred for 2 hours using a stirrer to obtain a solution B; c) After adding 1 part of macroporous strong acidic cation exchange resin to solution B, the temperature was raised to 50°C, and dispersion A was added dropwise to solution B, and stirred for 2 hours to obtain solution C; d) Solution C was filtered to obtain solution D; e) Toluene was removed by distillation at 63° C. and a vacuum degree of 20,000 Pa to obtain 44 parts of 2,6-di-tert-butyl-p-cresol-modified p-tert-octylphenol formaldehyde resin.

[0028] The 2,6-di-tert-butyl-p-cresol (melting point ≥ 71°C) was purchased from LANXESS, Germany, with the brand name Antioxidant 264; 4-tert-octylphenol formaldehyde resin (softening point of 90-100°C, hydroxymethyl content of 9-12%) was purchased from Wuhan Haishan, with the brand name WL-2203; macroporous strong acid cation exchange resin (effective particle size of 0.45-1.25 mm) was purchased from Anhui Wanshu Chemical Sales Co., Ltd., with the brand name: D001H.

[0029] 2. The method for preparing modified zinc oxide nano-color powder is as follows; Step 1: Take 10 parts of zinc oxide and add it to the ball mill, then add 0.4mm zirconium oxide. Step 2: The beads are used as grinding aids and ball milled at 400r / min for 1.5 hours; Filtration test shows that the fineness of the toner is 0.2μm, which meets the fineness requirements.

[0030] The zinc oxide was purchased from Hebei Zhiyi Co., Ltd., with the brand name Type 1.

[0031] Take 20 parts of methyl MQ silicone resin with an MQ ratio of 1:1, 21 parts of 107 silicone rubber, 23 parts of modified tackifying resin, 22 parts of toluene, 10 parts of modified zinc oxide color powder, 1 part of antioxidant 168, 2 parts of antioxidant 1010, and 1 part of ultraviolet absorber 234; the modified tackifying resin is 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin, and the modified color powder is modified nano color powder. Add the above components into a mixing container and stir evenly to obtain a mixture 1; then transfer the mixture 1 to a high-speed disperser and mix it evenly again, then put it into a centrifugal sand mill for grinding, grind continuously for 7 hours, control the grinding temperature at 40°C, and obtain a uniform mixture.

[0032] Comparative Example 2 1. First, prepare modified 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin, the steps are as follows: a) At 23°C, add 40 parts of tert-octylphenol formaldehyde resin to 300 parts of toluene, and stir for 2 hours using a stirrer to mix evenly to obtain solution A; b) 22 ° C, 5 parts of 2,6-di-tert-butyl-p-cresol was slowly added to 50 parts of toluene, and stirred for 2 hours using a stirrer to obtain a solution B; c) After adding 1 part of macroporous strong acidic cation exchange resin to solution B, the temperature was raised to 50°C, and dispersion A was added dropwise to solution B, and stirred for 2 hours to obtain solution C; d) Solution C was filtered to obtain solution D; e) Toluene was removed by distillation at 63° C. and a vacuum degree of 20,000 Pa to obtain 44 parts of 2,6-di-tert-butyl-p-cresol-modified p-tert-octylphenol formaldehyde resin.

[0033] The 2,6-di-tert-butyl-p-cresol (melting point ≥ 71°C) was purchased from LANXESS, Germany, with the brand name Antioxidant 264; 4-tert-octylphenol formaldehyde resin (softening point of 90-100°C, hydroxymethyl content of 9-12%) was purchased from Wuhan Haishan, with the brand name WL-2203; macroporous strong acid cation exchange resin (effective particle size of 0.45-1.25 mm) was purchased from Anhui Wanshu Chemical Sales Co., Ltd., with the brand name: D001H.

[0034] Take 20 parts of methyl MQ silicone resin with an MQ ratio of 1:1, 21 parts of 107 silicone rubber, 23 parts of modified tackifying resin, 22 parts of toluene, 10 parts of ordinary zinc oxide color powder, 1 part of antioxidant 168, 2 parts of antioxidant 1010, 2 parts of polyacrylate ammonium salt dispersant, and 1 part of ultraviolet absorber 234; the modified tackifying resin is 2,6-di-tert-butyl-p-cresol modified 4-tert-octylphenol formaldehyde resin, and the zinc oxide color powder is purchased from Hebei Zhiyi Co., Ltd., brand Type 1; add the above components into a mixing container and stir evenly to obtain a mixture 1; then transfer the mixture 1 to a high-speed disperser and mix it again, and then put it into a centrifugal sand mill for grinding, and grind it continuously for 7 hours, control the grinding temperature at 40°C, and obtain a uniform mixture.

[0035] Comparative Example 3 1. First, prepare modified 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin, the steps are as follows: a) At 23°C, add 40 parts of tert-octylphenol formaldehyde resin to 300 parts of toluene, and stir for 2 hours using a stirrer to mix evenly to obtain solution A; b) 22 ° C, 5 parts of 2,6-di-tert-butyl-p-cresol was slowly added to 50 parts of toluene, and stirred for 2 hours using a stirrer to obtain a solution B; c) After adding 1 part of macroporous strong acidic cation exchange resin to solution B, the temperature was raised to 50°C, and dispersion A was added dropwise to solution B, and stirred for 2 hours to obtain solution C; d) Solution C was filtered to obtain solution D; e) Toluene was removed by distillation at 63° C. and a vacuum degree of 20,000 Pa to obtain 44 parts of 2,6-di-tert-butyl-p-cresol-modified p-tert-octylphenol formaldehyde resin.

[0036] The 2,6-di-tert-butyl-p-cresol (melting point ≥ 71°C) was purchased from LANXESS, Germany, with the brand name Antioxidant 264; 4-tert-octylphenol formaldehyde resin (softening point of 90-100°C, hydroxymethyl content of 9-12%) was purchased from Wuhan Haishan, with the brand name WL-2203; macroporous strong acid cation exchange resin (effective particle size of 0.45-1.25 mm) was purchased from Anhui Wanshu Chemical Sales Co., Ltd., with the brand name: D001H.

[0037] 2. The method for preparing modified zinc oxide nano-color powder is as follows; a) Step 1: Take 10 parts of zinc oxide and add it into a ball mill, then add 0.4 mm zirconium oxide beads as a grinding aid, and ball mill at 400 r / min for 1.5 hours; b) Step 2: Filtration test: the fineness of the toner is 0.2μm, which meets the fineness requirements.

[0038] The zinc oxide was purchased from Hebei Zhiyi Co., Ltd., with the brand name Type 1.

[0039] Take 20 parts of methyl MQ silicone resin with an MQ ratio of 1:1, 21 parts of 107 silicone rubber, 23 parts of modified tackifying resin, 22 parts of toluene, 10 parts of modified zinc oxide color powder, and 2 parts of polyacrylate ammonium salt dispersant; the modified tackifying resin is 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin, and the modified color powder is modified nano color powder. Add the above components into a mixing container and stir evenly to obtain a mixture 1; then transfer the mixture 1 to a high-speed disperser and mix it evenly again, then put it into a centrifugal sand mill for grinding, grind continuously for 7 hours, control the grinding temperature at 40°C, and obtain a uniform mixture.

[0040] Comparative Example 4 1. The method for preparing modified zinc oxide nano-color powder is as follows; Step 1: Take 10 parts of zinc oxide and add it into a ball mill, then add 0.4 mm zirconium oxide beads as a grinding aid, and ball mill at 400 r / min for 1.5 hours; Step 2: Filtration test: the fineness of the toner is 0.2μm, which meets the fineness requirements.

[0041] The zinc oxide was purchased from Hebei Zhiyi Co., Ltd., with the brand name Type 1.

[0042] Take 20 parts of methyl MQ silicone resin with an MQ ratio of 1:1, 21 parts of 107 silicone rubber, 23 parts of tackifying resin, 22 parts of toluene, 10 parts of modified zinc oxide color powder, 1 part of antioxidant 168, 2 parts of antioxidant 1010, 2 parts of polyacrylate ammonium salt dispersant, and 1 part of ultraviolet absorber 234; the tackifying resin is tert-octylphenol formaldehyde resin, tert-octylphenol formaldehyde resin (softening point is 90-100℃, hydroxymethyl content is 9-12%) purchased from Wuhan Haishan, brand WL-2203; the modified color powder is modified nano color powder. Add the above components into a mixing container and stir evenly to obtain a mixture 1; then transfer the mixture 1 to a high-speed disperser and mix it again, then put it into a centrifugal separation sand mill for grinding, grind continuously for 7 hours, control the grinding temperature at 40℃, and obtain a uniform mixture.

[0043] Comparative Example 5 1. First, prepare modified 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin, the steps are as follows: a) At 23°C, add 40 parts of tert-octylphenol formaldehyde resin to 300 parts of toluene, and stir for 2 hours using a stirrer to mix evenly to obtain solution A; b) 22 ° C, 5 parts of 2,6-di-tert-butyl-p-cresol was slowly added to 50 parts of toluene, and stirred for 2 hours using a stirrer to obtain a solution B; c) After adding 1 part of macroporous strong acidic cation exchange resin to solution B, the temperature was raised to 50°C, and dispersion A was added dropwise to solution B, and stirred for 2 hours to obtain solution C; d) Solution C was filtered to obtain solution D; e) Toluene was removed by distillation at 63° C. and a vacuum degree of 20,000 Pa to obtain 44 parts of 2,6-di-tert-butyl-p-cresol-modified p-tert-octylphenol formaldehyde resin.

[0044] The 2,6-di-tert-butyl-p-cresol (melting point ≥ 71°C) was purchased from LANXESS, Germany, with the brand name Antioxidant 264; 4-tert-octylphenol formaldehyde resin (softening point of 90-100°C, hydroxymethyl content of 9-12%) was purchased from Wuhan Haishan, with the brand name WL-2203; macroporous strong acid cation exchange resin (effective particle size of 0.45-1.25 mm) was purchased from Anhui Wanshu Chemical Sales Co., Ltd., with the brand name: D001H.

[0045] 2. The method for preparing modified zinc oxide nano-color powder is as follows; Step 1: Take 10 parts of zinc oxide and add it into a ball mill, then add 0.4 mm zirconium oxide beads as a grinding aid, and ball mill at 400 r / min for 1.5 hours; Step 2: Filtration test: the fineness of the toner is 0.2μm, which meets the fineness requirements.

[0046] The zinc oxide was purchased from Hebei Zhiyi Co., Ltd., with the brand name Type 1.

[0047] Take 20 parts of methyl MQ silicone resin with an MQ ratio of 1:1, 21 parts of 107 silicone rubber, 23 parts of modified tackifying resin, 22 parts of toluene, 10 parts of modified zinc oxide color powder, and 2 parts of polyacrylate ammonium salt dispersant; the modified tackifying resin is 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin, and the modified color powder is modified nano color powder. Add the above components into a mixing container and stir evenly to obtain a mixture 1; then transfer the mixture 1 to a high-speed disperser and mix it evenly again, then put it into a centrifugal sand mill for grinding, grind continuously for 7 hours, control the grinding temperature at 40°C, and obtain a uniform mixture.

[0048] Comparative Example 6 1. First, prepare modified 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin, the steps are as follows: a) At 23°C, add 40 parts of tert-octylphenol formaldehyde resin to 300 parts of toluene, and stir for 2 hours using a stirrer to mix evenly to obtain solution A; b) 22 ° C, 5 parts of 2,6-di-tert-butyl-p-cresol was slowly added to 50 parts of toluene, and stirred for 2 hours using a stirrer to obtain a solution B; a) After adding 1 part of macroporous strong acidic cation exchange resin to solution B, the temperature was raised to 50°C, and dispersion A was added dropwise to solution B, and stirred for 2 hours to obtain solution C; b) Solution C was filtered to obtain solution D; c) Toluene was removed by distillation at 63° C. and a vacuum degree of 20,000 Pa to obtain 44 parts of 2,6-di-tert-butyl-p-cresol-modified p-tert-octylphenol formaldehyde resin.

[0049] The 2,6-di-tert-butyl-p-cresol (melting point ≥ 71°C) was purchased from LANXESS, Germany, with the brand name Antioxidant 264; 4-tert-octylphenol formaldehyde resin (softening point of 90-100°C, hydroxymethyl content of 9-12%) was purchased from Wuhan Haishan, with the brand name WL-2203; macroporous strong acid cation exchange resin (effective particle size of 0.45-1.25 mm) was purchased from Anhui Wanshu Chemical Sales Co., Ltd., with the brand name: D001H.

[0050] 2. The method for preparing modified zinc oxide nano-color powder is as follows; Step 1: Take 10 parts of zinc oxide and add it into a ball mill, then add 0.4 mm zirconium oxide beads as a grinding aid, and ball mill at 400 r / min for 1.5 hours; Step 2: Filtration test: the fineness of the toner is 0.2μm, which meets the fineness requirements.

[0051] The zinc oxide was purchased from Hebei Zhiyi Co., Ltd., with the brand name Type 1.

[0052] Take 20 parts of methyl MQ silicone resin with an MQ ratio of 1:1, 21 parts of 107 silicone rubber, 23 parts of modified tackifying resin, 30 parts of toluene, 10 parts of modified zinc oxide color powder, 1 part of antioxidant 168, 2 parts of antioxidant 1010, 2 parts of polyacrylate ammonium salt dispersant, and 1 part of ultraviolet absorber 234; the modified tackifying resin is 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin, and the modified color powder is modified nano color powder. Add the above components into a mixing container and stir evenly to obtain a mixture 1; then transfer the mixture 1 to a high-speed disperser and mix it evenly again, then put it into a centrifugal sand mill for grinding, grind continuously for 7 hours, control the grinding temperature at 40°C, and obtain a uniform mixture.

[0053] Performance Testing The color pastes prepared in Example 1 and Comparative Examples 1-6 were tested according to the H / T 4786-2014 standard; the yellowing resistance of the color pastes was tested using an ultraviolet accelerated aging test device, model: HE-NK-150;

[0054] As can be seen from the above table, the modified tackifying resin and the modified color powder used in Example 1 have relatively good coloring performance and good yellowing resistance.

[0055] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A silicone rubber pressure-sensitive adhesive color paste, characterized in that: The invention comprises at least the following components in parts by weight: 20-22 parts of methyl MQ organic silicon resin, 20-23 parts of organic silicon rubber, 20-25 parts of modified tackifying resin, 20-25 parts of solvent, 37-38 parts of modified color powder, 3-5 parts of antioxidant, 2-3 parts of dispersant and 1-2 parts of ultraviolet absorber.

2. The organic silicone rubber pressure-sensitive adhesive paste according to claim 1, characterized in that: The modified tackifying resin is 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin.

3. The organic silicone rubber pressure-sensitive adhesive paste according to claim 2, characterized in that: The preparation method of the 2,6-di-tert-butyl-p-cresol modified p-tert-octylphenol formaldehyde resin comprises at least the following steps: a) Add tert-octylphenol formaldehyde resin to toluene at 20-25°C and stir for 2 hours to mix evenly to obtain solution A; b) 20-25°C, slowly add 2,6-di-tert-butyl-p-cresol to toluene and stir for 2 hours using a stirrer to obtain a solution B; c) After adding macroporous strongly acidic cation exchange resin to solution B, the temperature was raised to 50°C, dispersion A was added dropwise to solution B, and solution C was obtained after stirring for 2 hours; d) Solution C is filtered to obtain solution D; e) Solution D is distilled at 60-65° C. and a vacuum degree of 20000 Pa to obtain 2,6-di-tert-butyl-p-cresol-modified p-tert-octylphenol formaldehyde resin.

4. The organic silicone rubber pressure-sensitive adhesive paste according to claim 2, characterized in that: The mass ratio of the 2,6-di-tert-butyl-p-cresol, the p-tert-octylphenol formaldehyde resin, the macroporous strong acid cation exchange resin and the toluene is 5-8:40-45:1-2:300-350.

5. The organic silicone rubber pressure-sensitive adhesive paste according to claim 1, characterized in that: The M:Q ratio of the methyl MQ silicone resin is 0.7:1-1:

1.

6. The organic silicone rubber pressure-sensitive adhesive paste according to claim 1, characterized in that: The solvent is selected from at least one of benzene, toluene and xylene.

7. The organic silicone rubber pressure-sensitive adhesive paste according to claim 1, characterized in that: The modified color powder is a modified nano color powder, and the color powder can be selected from at least one of amaranth, carmine, erythrosine, new red, lemon yellow, sunset yellow, indigo yellow, brilliant blue, titanium dioxide, zinc oxide, and lithopone.

8. The organic silicone rubber pressure-sensitive adhesive color paste according to claim 7, wherein the method for preparing the modified nano-color powder comprises at least the following steps: a) Add 0.3-0.5 mm zirconium oxide beads to the ball mill and mill at 400-500 r / min for 1-2 hours; b) Initial filtration test: Filter the ground toner and test the fineness to ensure that the fineness of the toner is between 0.05μm and 0.50μm. If the fineness of the color paste is greater than 0.50μm, repeat the grinding.

9. The organic silicone rubber pressure-sensitive adhesive paste according to claim 1, characterized in that: The antioxidants are antioxidant 168 and antioxidant 1010, wherein the mass ratio of antioxidant 168 to antioxidant 1010 is 1:

2.

10. A method for preparing the silicone rubber pressure-sensitive adhesive color paste according to any one of claims 1 to 9, characterized in that: At least the following steps are included: Step S1: Weigh the solvent, methyl MQ silicone resin, silicone rubber, antioxidant, dispersant, UV absorber, modified color powder, and modified tackifying resin respectively, put them into a mixing container and stir them evenly to obtain a mixture 1; Step S2: Transfer the mixture 1 to a high-speed disperser and mix it again, then put it into a centrifugal sand mill for grinding. Grind continuously for 7 hours, control the grinding temperature not higher than 45°C, and obtain a color paste particle size D50 less than 90nm to obtain a uniform mixture.

Citation Information

Patent Citations

  • Preparation method of organic silicon color paste

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