Silica gel prepared based on environment-friendly efficient dissolved methyl silicone resin

Abstract

The invention discloses silica gel prepared based on environment-friendly efficient dissolved methyl silicone resin, and relates to the technical field of adhesives. Comprising the following steps: step 1, stirring and dissolving acrylate modified vinyl silicone oil and methyl silicone resin to obtain liquid S; 2, mixing the liquid S, acrylate modified vinyl silicone oil and a Karst catalyst to obtain a component A; 3, mixing the liquid S, acrylate modified vinyl silicone oil, hydrogen-rich silicone oil, hydrogen-terminated silicone oil and alkynol to obtain a component B; and step 4, mixing the component A and the component B to obtain the silica gel. The preparation method has the beneficial effects that the silicon resin powder is dissolved in a solvent-free manner, so that the excellent viscosity and flexibility of the silica gel and the easy stripping property of the protective film are realized. The environment-friendly method not only reduces the influence on the environment, but also reduces the energy consumption and improves the efficiency due to short dissolution time.

Description

Technical Field

[0001] The invention relates to the technical field of adhesives, in particular to a silicone gel prepared by dissolving methyl silicone resin in an environmentally friendly and efficient manner. Background Art

[0002] As a unique adhesive, silicone gel has a huge application in medical tapes, foam dressings, hydrogel dressings and wearable products due to its excellent properties such as natural physiological inertness, low allergenicity, and comfortable skin adhesion. Some traditional adhesive manufacturers, silicone manufacturers and dressing manufacturers in China are also actively developing silicone gel.

[0003] At present, some domestic manufacturers can make the viscosity of silicone gel relatively high, which can meet the viscosity requirements of silicone gel as an adhesive, and are basically comparable to foreign giants. When preparing high-viscosity silicone gel, we need to dissolve the required silicone resin in the required silicone oil, and then add various additives to process it into products under certain processing equipment and processing conditions. However, there are currently several methods for dissolving silicone resin powder to prepare silicone gel: (1) Indirect method, using xylene or toluene as solvent to dissolve silicone resin powder in silicone oil, and then volatilizing the solvent. The advantage of this method is that the silicone resin powder is dissolved efficiently and quickly, but the disadvantage is that it is not environmentally friendly, and the subsequent processing of the volatilization solvent link increases energy consumption. For example, US20190112431A1 discloses a method for preparing silicone gel by dissolving silicone resin powder with a solvent; (2) Using vinyl silicone oil to dissolve methyl vinyl silicone resin powder to prepare silicone gel. The advantages of this method are environmental protection, no volatile solvent step in subsequent processing, easy processing, and methyl vinyl silicone resin powder is also relatively easy to dissolve. However, the viscosity-enhancing effect of this resin is poor. For example, CN116640555A discloses a method for dissolving methyl vinyl silicone resin powder with vinyl silicone oil to prepare silicone gel; (3) Using vinyl silicone oil to dissolve methyl silicone resin powder to prepare silicone gel. The advantages of this method are environmental protection, convenient and direct processing, and the prepared silicone gel has better performance. The disadvantage is that it takes a long time to dissolve the silicone resin powder. For example, CN117106410A discloses a method for preparing silicone gel by dissolving methyl silicone resin powder with vinyl silicone oil.

[0004] In order to solve the shortcomings of the above method, the present invention obtains a silicone gel prepared based on environmentally friendly and efficient dissolution of methyl silicone resin. Summary of the invention

[0005] The purpose of the present invention is to provide a silicone gel prepared by dissolving methyl silicone resin in an environmentally friendly and efficient manner to solve the problems raised in the prior art.

[0006] To achieve the above object, the present invention provides the following technical solutions: A silicone gel prepared based on environmentally friendly and efficient dissolution of methyl silicone resin, comprising the following steps: Step 1: Mix acrylate-modified vinyl silicone oil and methyl silicone resin, stir and dissolve at 120-130° C. and 350-380 rpm for 10-15 hours to obtain liquid S; Step 2: Mix liquid S, acrylate-modified vinyl silicone oil and Custer catalyst, and stir at 350-380 rpm for 1-2 hours at room temperature to obtain component A; Step 3: Mix liquid S, acrylate-modified vinyl silicone oil, multi-hydrogen silicone oil, terminal hydrogen silicone oil, and acetylenic alcohol, and stir at room temperature at 350-400 rpm for 1-3 hours to obtain component B; Step 4: Mix component A and component B to obtain silicone gel.

[0007] More optimally: the liquid S comprises the following components: by weight, 50-100 parts of acrylate-modified vinyl silicone oil and 60-120 parts of methyl silicone resin; The component A comprises the following components: by weight, 10-30 parts of liquid S, 10-30 parts of acrylate-modified vinyl silicone oil, and 0.1-1 parts of Custer catalyst; The component B comprises the following components: by weight, 10-30 parts of liquid S, 1-20 parts of acrylate-modified vinyl silicone oil, 10-30 parts of multi-hydrogen-containing silicone oil, 0.1-10 parts of terminal hydrogen-containing silicone oil, and 0.001-1 part of acetylenic alcohol.

[0008] More optimally, the acrylic acid content in the acrylate-modified vinyl silicone oil is 0.1-10 mmol / g, the vinyl content is 0.001-10 mmol / g, and the viscosity is 100-10000 Pa.s.

[0009] In a further embodiment, the acrylate-modified vinyl silicone oil includes one of SK-Privi027 and SK-Privi028, and has an acrylic acid content of 0.2-1 mmol / g, a vinyl content of 0.085-1.619 mmol / g, and a viscosity of 1000-1250 pa.s.

[0010] More optimally, the average molecular weight of the methyl silicone resin is between 1000 and 5000.

[0011] More optimally, the metal platinum content of the Castel catalyst is 1000-10000ppm.

[0012] More optimally, the hydrogen content of the multi-hydrogenated silicone oil is 1-20 mmol / g.

[0013] More optimally, the hydrogen content of the terminal hydrogenated silicone oil is 0.1-10 mmol / g.

[0014] More optimally: the alkynol is ethynyl cyclohexanol.

[0015] Compared with the prior art, the beneficial effects of the present application are as follows: the present invention dissolves silicone resin powder without solvent, thereby achieving excellent viscosity and softness of silicone gel and easy peelability of protective film. This environmentally friendly method not only reduces the impact on the environment, but also reduces energy consumption and improves efficiency due to the short dissolution time. In addition, compared with conventional vinyl silicone oil, acrylate-modified vinyl silicone oil has stronger polarity and dissolves silicone resin more quickly and efficiently; at the same time, it has greater surface energy and has better wettability to more material surfaces. DETAILED DESCRIPTION

[0016] Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in the field without making any creative work shall fall within the scope of protection of the present invention.

[0017] It should be noted that the purchase manufacturers of all raw materials involved in the present invention are not subject to any special restrictions and exemplarily include: in the following embodiments, the models of acrylate-modified vinyl silicone oil are SK-Privi027 (acrylic acid content is 1 mmol / g, vinyl content is 0.085 mmol / g, and viscosity is 1250 pa.s), SK-Privi028 (acrylic acid content is 0.2 mmol / g, vinyl content is 1.619 mmol / g, and viscosity is 1000 pa.s); methyl silicone resin (MQ101), Custer catalyst (ACS-Pt-30), multi-hydrogenated silicone oil (484), terminal hydrogenated silicone oil (MDH180), and ethynyl cyclohexanol (ACS-MA-8900).

[0018] Embodiment 1: A silicone gel prepared based on environmentally friendly and efficient dissolution of methyl silicone resin, comprising the following steps: Step 1: Place a beaker in a self-controlled oil bath, equipped with a stirrer, add 140 g of acrylate-modified vinyl silicone oil (SK-Privi027) and 140 g of methyl silicone resin powder into the beaker, stir at 120°C for 12 hours, and the resin is completely dissolved to obtain liquid S1; Step 2: Weigh 17.3 g of liquid S1, 17.6 g of acrylate-modified vinyl silicone oil, and 0.17 g of Custer catalyst in a beaker, and stir at room temperature for 1 h to obtain component A; Step 3: In a beaker, weigh 17.3 g of liquid S1, 8.0 g of acrylate-modified vinyl silicone oil, 9.2 g of terminal hydrogen-containing silicone oil, 0.46 g of multi-hydrogen-containing silicone oil, and 0.01 g of ethynyl cyclohexanol, and stir at room temperature for 1 h to obtain component B; Step 4: Prepare silicone gel by mixing component A and component B in a ratio of 1:1.

[0019] Example 2: A silicone gel prepared based on environmentally friendly and efficient dissolution of methyl silicone resin, comprising the following steps: Step 1: Place a beaker in a self-controlled oil bath, equipped with a stirrer, add 140 g of acrylate-modified vinyl silicone oil (SK-Privi027) and 140 g of methyl silicone resin powder into the beaker, stir at 120°C for 12 hours, and the resin is completely dissolved to obtain liquid S1; Step 2: In a beaker, weigh 19.4 g of liquid S1, 15.4 g of acrylate-modified vinyl silicone oil, and 0.17 g of Custer catalyst, and stir at room temperature for 1 h to obtain component A; Step 3: In a beaker, weigh 19.4 g of liquid S1, 5.7 g of acrylate-modified vinyl silicone oil, 9.5 g of terminal hydrogen-containing silicone oil, 0.46 g of multi-hydrogen-containing silicone oil, and 0.01 g of ethynyl cyclohexanol, and stir at room temperature for 1 hour to obtain component B; Step 4: Prepare silicone gel by mixing component A and component B in a ratio of 1:1.

[0020] Embodiment 3: A silicone gel prepared based on environmentally friendly and efficient dissolution of methyl silicone resin, comprising the following steps: Step 1: Place a beaker in a self-controlled oil bath, equipped with a stirrer, add 140 g of acrylate-modified vinyl silicone oil (SK-Privi028) and 140 g of methyl silicone resin powder into the beaker, stir at 120°C for 12 hours, and the resin is completely dissolved to obtain liquid S1; Step 2: Weigh 21.6 g of liquid S1, 13.3 g of acrylate-modified vinyl silicone oil, and 0.17 g of Custer catalyst in a beaker, and stir at room temperature for 1 h to obtain component A; Step 3: In a beaker, weigh 21.6 g of liquid S1, 3.3 g of acrylate-modified vinyl silicone oil, 9.7 g of terminal hydrogen-containing silicone oil, 0.46 g of multi-hydrogen-containing silicone oil, and 0.01 g of ethynyl cyclohexanol, and stir at room temperature for 1 hour to obtain component B; Step 4: Prepare silicone gel by mixing component A and component B in a ratio of 1:1.

[0021] Example 4: A silicone gel prepared based on environmentally friendly and efficient dissolution of methyl silicone resin, comprising the following steps: Step 1: Place a beaker in a self-controlled oil bath, equipped with a stirrer, add 140 g of acrylate-modified vinyl silicone oil (SK-Privi028) and 140 g of methyl silicone resin powder into the beaker, stir at 120°C for 12 hours, and the resin is completely dissolved to obtain liquid S1; Step 2: Weigh 23.6 g of liquid S1, 11.2 g of acrylate-modified vinyl silicone oil, and 0.17 g of Custer catalyst in a beaker, and stir at room temperature for 1 h to obtain component A; Step 3: In a beaker, weigh 23.6 g of liquid S1, 0.9 g of acrylate-modified vinyl silicone oil, 10.0 g of terminal hydrogen-containing silicone oil, 0.46 g of multi-hydrogen-containing silicone oil, and 0.01 g of ethynyl cyclohexanol, and stir at room temperature for 1 hour to obtain component B; Step 4: Prepare silicone gel by mixing component A and component B in a ratio of 1:1.

[0022] Comparative Example 1: A silicone gel prepared based on environmentally friendly and efficient dissolution of methyl silicone resin, comprising the following steps: Step 1: Place a beaker in a self-controlled oil bath, equipped with a stirrer, add 140 g of hydroxyl-modified vinyl silicone oil and 140 g of methyl silicone resin powder into the beaker, stir at 120° C. for 48 h, and the resin is completely dissolved to obtain liquid S2; Step 2: Weigh 11.4 g of liquid S2, 23.4 g of hydroxyl-modified vinyl silicone oil, and 0.17 g of Custer catalyst in a beaker, and stir at room temperature for 1 hour to obtain component A; Step 3: In a beaker, weigh 11.4 g of liquid S2, 12.4 g of hydroxyl-modified vinyl silicone oil, 10.7 g of terminal hydrogen-containing silicone oil, 0.45 g of polyhydrogen-containing silicone oil, and 0.01 g of ethynyl cyclohexanol, and stir at room temperature for 1 hour to obtain component B; Step 4: Prepare silicone gel by mixing component A and component B in a ratio of 1:1.

[0023] Comparative Example 2: A silicone gel prepared based on environmentally friendly and efficient dissolution of methyl silicone resin, comprising the following steps: Step 1: Place a beaker in a self-controlled oil bath, equipped with a stirrer, add 140 g of hydroxyl-modified vinyl silicone oil and 140 g of methyl silicone resin powder into the beaker, stir at 120° C. for 48 h, and the resin is completely dissolved to obtain liquid S2; Step 2: Weigh 16.6 g of liquid S2, 18.2 g of hydroxyl-modified vinyl silicone oil, and 0.17 g of Custer catalyst in a beaker, and stir at room temperature for 1 hour to obtain component A; Step 3: In a beaker, weigh 16.6 g of S2, 6.5 g of hydroxyl-modified vinyl silicone oil, 11.5 g of terminal hydrogen-containing silicone oil, 0.45 g of multi-hydrogen-containing silicone oil, and 0.01 g of ethynyl cyclohexanol, and stir at room temperature for 1 hour to obtain component B; Step 4: Prepare silicone gel by mixing component A and component B in a ratio of 1:1.

[0024] Testing experiment: The samples obtained from Examples 1-4 and Comparative Examples 1-2 were subjected to cone penetration and 180° peeling force tests. Cone penetration test: Pour the silicone gel into a sample cup and bake it at 140°C for 1 hour. After cooling it at room temperature for 24 hours, use a 1 / 2 cone to perform a cone penetration test, and then convert it into a full-size cone penetration; for the 180° peeling force test, apply 120g / ㎡ of silicone gel on the TPU film, bake it at 140°C for 6 minutes, and place it at room temperature for 24 hours to perform a 180° steel plate peeling force test; the results are shown in the following table:

[0025] Table 1 Conclusion: Examples 1-4 achieve excellent adhesion and softness of silicone gel and easy peelability of protective film by dissolving silicone resin powder without solvent. At the same time, its dissolution time is also shortened, energy consumption is reduced, and efficiency is improved; it is in line with practical applications.

[0026] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A silicone gel prepared by dissolving methyl silicone resin in an environmentally friendly and efficient manner, characterized in that: The following steps are involved: Step 1: Mix acrylate-modified vinyl silicone oil and methyl silicone resin, stir and dissolve at 120-130° C. and 350-380 rpm for 10-15 hours to obtain liquid S; Step 2: Mix liquid S, acrylate-modified vinyl silicone oil and Custer catalyst, and stir at 350-380 rpm for 1-2 hours at room temperature to obtain component A; Step 3: Mix liquid S, acrylate-modified vinyl silicone oil, multi-hydrogen silicone oil, terminal hydrogen silicone oil, and acetylenic alcohol, and stir at 350-400 rpm for 1-3 hours at room temperature to obtain component B; Step 4: Mix component A and component B to obtain silicone gel.

2. The silicone gel prepared by dissolving methyl silicone resin based on environmental protection and high efficiency according to claim 1, characterized in that: The liquid S comprises the following components: 50-100 parts by weight of acrylate-modified vinyl silicone oil and 60-120 parts of methyl silicone resin; The component A comprises the following components: by weight, 10-30 parts of liquid S, 10-30 parts of acrylate-modified vinyl silicone oil, and 0.1-1 parts of Custer catalyst; The component B comprises the following components: by weight, 10-30 parts of liquid S, 1-20 parts of acrylate-modified vinyl silicone oil, 10-30 parts of multi-hydrogen-containing silicone oil, 0.1-10 parts of terminal hydrogen-containing silicone oil, and 0.001-1 part of acetylenic alcohol.

3. The silicone gel prepared by dissolving methyl silicone resin based on environmental protection and high efficiency according to claim 1, characterized in that: The acrylic acid content of the acrylate-modified vinyl silicone oil is 0.1-10 mmol / g, the vinyl content is 0.001-10 mmol / g, and the viscosity is 100-10000 Pa.s.

4. The silicone gel prepared by dissolving methyl silicone resin based on environmental protection and high efficiency according to claim 1, characterized in that: The average molecular weight of the methyl silicone resin is 1000-5000.

5. The silicone gel prepared by dissolving methyl silicone resin based on environmental protection and high efficiency according to claim 1, characterized in that: The metal platinum content of the Castel catalyst is 1000-10000 ppm.

6. The silicone gel prepared by dissolving methyl silicone resin based on environmental protection and high efficiency according to claim 1, characterized in that: The hydrogen content of the multi-hydrogenated silicone oil is 1-20 mmol / g.

7. The silicone gel prepared by dissolving methyl silicone resin based on environmental protection and high efficiency according to claim 1, characterized in that: The hydrogen content of the terminal hydrogen-containing silicone oil is 0.1-10 mmol / g.

8. The silicone gel prepared by dissolving methyl silicone resin based on environmental protection and high efficiency according to claim 1, characterized in that: The acetylenic alcohols include ethynyl cyclohexanol.

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