Preparation method and application of organic silicon tackifier

Abstract

The invention relates to the technical field of tackifiers, and discloses a preparation method and application of an organic silicon tackifier. Vinyl isophthalic acid and epoxy chloropropane are subjected to an esterification reaction under catalysis of tetraethylammonium bromide to obtain vinyl epoxypropyl isophthalate; and carrying out polymerization reaction on the modified rosin, allyl propionate modified rosin and alkenyl silicone oil under the initiation of azodiisobutyronitrile to obtain the organic silicon tackifier. And adding the organic silicon tackifier into the base material, and uniformly mixing to obtain the silicone rubber adhesive. The organic silicon tackifier prepared by the invention contains ester groups, carboxyl groups and epoxy groups with relatively strong polarity, and is easy to chemically react with a base material or form secondary valence bonds, so that the adhesion of a silicon rubber adhesive is enhanced, and the organic silicon tackifier is easy to tangle with each other after being added into silicon rubber to form a network structure, so that the mechanical property of the silicon rubber is enhanced. The tackifier prepared by the invention has excellent mechanical property and adhesive property when being applied to silicone rubber.

Description

Technical Field

[0001] The invention relates to the technical field of tackifiers, and in particular to a preparation method and application of an organosilicon tackifier. Background Art

[0002] Rosin is an oil resin exuded from pine plants of the genus Pinus in the Pinaceae family. Rosin ester is a product obtained by esterification of rosin or modified rosin and alcohols. It has the characteristics of viscosity enhancement, film formation, solubility, and good compatibility, and is widely used in various viscosity enhancement fields. Silicone oil refers to a linear polysiloxane product that remains in a liquid state at room temperature. It has good chemical stability, insulation, viscosity, and compression resistance. It is widely used in construction, electronics and electrical, textiles, chemical and light industry, medicine and medical fields. Silicone rubber adhesive is a special adhesive with excellent high and low temperature resistance, insulation, waterproof and other characteristics. It is widely used in aircraft manufacturing, construction, medical and health fields, but the side chain groups of silicone rubber are mainly low polar groups such as methyl and ethyl, with low surface energy and poor adhesion to other materials, which limits its application range. Therefore, tackifiers are added to silicone rubber to improve the adhesion between silicone rubber and substrates. For example, the patent application publication number CN103468200A discloses an environmentally friendly two-component silicone rubber adhesive and its preparation method. The invention includes the following components: dihydroxy polydimethylsiloxane, silicon dioxide, methyl silicone oil / ethoxy-terminated polydimethylsiloxane, crosslinking agent and other components. The prepared silicone rubber adhesive has the advantages of environmental friendliness, excellent bonding performance, fast curing, excellent aging resistance, etc. However, the bonding effect is not good. Summary of the invention

[0003] The technical problem solved by the present invention is: to provide a preparation method of an organosilicon tackifier and application thereof; the prepared organosilicon tackifier is applied to silicone rubber to enhance the mechanical properties and bonding properties of the silicone rubber adhesive.

[0004] The technical solution of the present invention is:

[0005] A method for preparing an organosilicon tackifier, the preparation method comprising the following steps:

[0006] (1) Add vinyl isophthalic acid and tetraethylammonium bromide catalyst into a flask containing toluene solvent, stir to dissolve, add sodium hydroxide solution, stir to disperse, and finally add epichlorohydrin, reflux at 100-115° C. for 2-4 hours, add deionized water, stand to separate, concentrate the organic phase, wash with n-hexane, and obtain vinyl isophthalic acid glycidyl ester, the reaction formula of which is:

[0007]

[0008] (2) placing the allyl ester modified rosin in a flask filled with ethanol solvent, stirring to dissolve, heating to 70-85° C., adding azobisisobutyronitrile initiator, vinyl isophthalic acid glycidyl ester, and alkenyl silicone oil, and reacting for 4-6 hours to obtain an organosilicon tackifier.

[0009] Preferably, in step (1), the mass ratio of vinyl isophthalic acid, tetraethylammonium bromide and epichlorohydrin is 100:0.2-0.6:160-200.

[0010] Preferably, the mass fraction of the sodium hydroxide solution in step (1) is 30-45%.

[0011] Preferably, in step (2), the mass ratio of allyl ester-modified rosin, azobisisobutyronitrile, vinyl isophthalate glycidyl, and alkenyl silicone oil is 15-35:1-1.8:10-25:100.

[0012] Preferably, the preparation method of the alkenyl silicone oil in step (2) is as follows:

[0013] (3) Tripropylene glycol diacrylate and Karstedt platinum catalyst are placed in a flask filled with isopropanol solvent, stirred to dissolve, hydrogenated silicone oil is added thereto, reacted at 50-70° C. for 2-4 hours, cooled to room temperature, activated carbon is added thereto to adsorb the Karstedt platinum catalyst, filtered, and the filtrate is subjected to reduced pressure distillation to obtain vinyl silicone oil, the reaction formula of which is:

[0014]

[0015] Preferably, in step (3), the mass ratio of hydrogenated silicone oil, tripropylene glycol diacrylate and Karstedt platinum catalyst is 100:120-200:0.06-0.12.

[0016] Preferably, vinyl silicone oil, vinyl MQ resin, white carbon black and hexamethyldisilazane are mixed uniformly at high speed, heated to 110-130° C., and vacuumed to remove low-boiling substances to obtain a base material. Hydrogenated silicone oil, 1-ethynylcyclohexanol inhibitor and Karstedt platinum catalyst are sequentially added to the base material and mixed uniformly. Vacuum is removed to remove bubbles. Finally, an organosilicon tackifier is added thereto, mixed uniformly, vacuumed to remove bubbles, and dried to obtain a silicone rubber adhesive.

[0017] Preferably, in the step, the mass ratio of vinyl silicone oil, vinyl MQ resin, white carbon black, hexamethyldisilazane, hydrogenated silicone oil, 1-ethynylcyclohexanol inhibitor, Karstedt platinum catalyst, and silicone tackifier is 100:20-30:15-25:5-12:1-3:0.05-0.1:0.02-0.1:1-5.

[0018] The beneficial technical effects of the present invention are:

[0019] Vinyl isophthalic acid reacts with epichlorohydrin under the catalysis of tetraethylammonium bromide to obtain vinyl isophthalic acid glycidyl ester, and tripropylene glycol diacrylate reacts with hydrogenated silicone oil under the catalysis of Karstedt platinum catalyst to obtain alkenyl silicone oil. Allyl ester-modified rosin, vinyl isophthalic acid glycidyl ester, and alkenyl silicone oil react under the initiation of azobisisobutyronitrile to obtain an organosilicon tackifier. Finally, vinyl silicone oil, vinyl MQ resin, white carbon black, and hexamethyldisilazane are uniformly mixed to prepare a base material, and then hydrogenated silicone oil, 1-ethynylcyclohexanol inhibitor, Karstedt platinum catalyst, and organosilicon tackifier are added to the base material and mixed uniformly to obtain a silicone rubber adhesive.

[0020] The organosilicon tackifier prepared by the present invention has an ester group with strong polarity in the vinyl isophthalic acid glycidyl ester structure and the allyl ester modified rosin structure, which is easy to form secondary bonds such as hydrogen bonds and van der Waals forces with the adhered substrate to enhance the adhesion of the silicone rubber adhesive. In addition, the epoxy group in the vinyl isophthalic acid glycidyl ester has a large ring tension and polarity, and can undergo a ring-opening reaction with the substrate containing active hydrogen, thereby improving the adhesion between the silicone rubber and the adhered substrate. In addition, the carboxyl group contained in the product of ester hydrolysis and the carboxyl polar group in the allyl ester modified rosin structure are easy to react with the group on the surface of the substrate to form a strong chemical bond, further improving the adhesion of the silicone rubber adhesive.

[0021] The alkenyl silicone oil and silicone rubber in the organosilicon tackifier both have siloxane bonds, so the alkenyl silicone oil and silicone rubber have good compatibility, and the double bonds in the organosilicon tackifier that are not involved in the reaction can undergo a silyl hydrogen addition reaction with the silicon hydrogen bonds of the silicone rubber, and the tackifier is connected to the silicone rubber in the form of a chemical bond, thereby enhancing the mechanical properties of the silicone rubber, and the organosilicon adhesive is added to the silicone rubber, wherein the long-chain molecules of the two are entangled with each other to form a three-dimensional network cross-linked structure, the molecular chain is not easy to slip, and the stress of the molecular chain in the stretching or tearing deformation is more easily dispersed in other molecular chains, thereby increasing the mechanical properties of the adhesive, and the organosilicon adhesive has more polar groups in the molecular chain, which can form stronger chemical bonds such as hydrogen bonds to interact with each other, and synergistically assist, thereby further improving the mechanical properties of the silicone rubber adhesive. The tackifier prepared by the present invention has excellent mechanical properties and bonding properties when applied to silicone rubber. DETAILED DESCRIPTION

[0022] The present invention is described in detail below, and the technical solutions in the embodiments of the present invention are clearly and completely described. Obviously, the described embodiments are only 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.

[0023] The preparation method of allyl ester modified rosin is as follows: add 10g of rosin powder into a flask filled with toluene solvent, stir to dissolve, add 13g of thionyl chloride thereto, heat to 60°C to react for 2.5h, distill under reduced pressure, add toluene solvent and pyridine catalyst thereto, add 8g of hydroxyethyl methacrylate thereto at 50°C, react for 0.5h, keep warm to react for 3h, wash with saturated sodium chloride, distill under reduced pressure to obtain allyl ester modified rosin.

[0024] Example 1

[0025] (1) 5 g of vinyl isophthalic acid and 0.01 g of tetraethylammonium bromide catalyst were added to a flask containing toluene solvent, stirred to dissolve, 40% by mass sodium hydroxide solution was added thereto, stirred to disperse, and finally 10 g of epichlorohydrin was added thereto. The mixture was refluxed at 110° C. for 3 h, deionized water was added, the mixture was allowed to stand for stratification, the organic phase was concentrated, and the mixture was washed with n-hexane to obtain vinyl isophthalic acid glycidyl ester.

[0026] (2) 40 g of tripropylene glycol diacrylate and 0.02 g of Karstedt's platinum catalyst are placed in a flask filled with isopropanol solvent and stirred to dissolve. 25 g of hydrogenated silicone oil is added thereto and reacted at 60° C. for 4 h. The mixture is cooled to room temperature and activated carbon is added thereto to adsorb the Karstedt's platinum catalyst. The mixture is filtered and the filtrate is distilled under reduced pressure to obtain vinyl silicone oil.

[0027] (3) 3 g of allyl ester-modified rosin was placed in a flask filled with ethanol solvent, stirred to dissolve, and heated to 80° C., 0.2 g of azobisisobutyronitrile initiator, 3 g of vinyl isophthalic acid glycidyl ester, and 20 g of vinyl silicone oil were added thereto, and the mixture was reacted for 5 h to obtain an organosilicon tackifier.

[0028] (4) 200 g of vinyl silicone oil, 60 g of vinyl MQ resin, 40 g of white carbon black, and 10 g of hexamethyldisilazane were mixed uniformly at high speed, heated to 120° C., and vacuumed to remove low-boiling substances to obtain a base material. 4 g of hydrogenated silicone oil, 0.15 g of 1-ethynylcyclohexanol inhibitor, and 0.1 g of Karstedt platinum catalyst were added to the base material in sequence, mixed uniformly, vacuumed to remove bubbles, and finally 2 g of an organosilicon tackifier was added thereto, mixed uniformly, vacuumed to remove bubbles, and dried to obtain a silicone rubber adhesive.

[0029] Example 2

[0030] (1) Add 5 g of vinyl isophthalic acid and 0.01 g of tetraethylammonium bromide catalyst into a flask containing toluene solvent, stir to dissolve, add 30% by mass sodium hydroxide solution, stir to disperse, and finally add 9 g of epichlorohydrin. Reflux at 110° C. for 4 h, add deionized water, stand to separate, concentrate the organic phase, and wash with n-hexane to obtain vinyl isophthalic acid glycidyl ester.

[0031] (2) 40 g of tripropylene glycol diacrylate and 0.015 g of Karstedt's platinum catalyst are placed in a flask filled with isopropanol solvent and stirred to dissolve. 25 g of hydrogenated silicone oil is added thereto and reacted at 60° C. for 2 h. The mixture is cooled to room temperature and activated carbon is added thereto to adsorb the Karstedt's platinum catalyst. The mixture is filtered and the filtrate is distilled under reduced pressure to obtain vinyl silicone oil.

[0032] (3) 6 g of allyl ester-modified rosin was placed in a flask filled with ethanol solvent, stirred to dissolve, and heated to 80° C., 0.3 g of azobisisobutyronitrile initiator, 2 g of vinyl isophthalic acid glycidyl ester, and 20 g of vinyl silicone oil were added thereto, and the mixture was reacted for 4 h to obtain an organosilicon tackifier.

[0033] (4) 200 g of vinyl silicone oil, 50 g of vinyl MQ resin, 40 g of white carbon black, and 20 g of hexamethyldisilazane were mixed uniformly at high speed, heated to 130° C., and vacuumed to remove low-boiling substances to obtain a base material. 5 g of hydrogenated silicone oil, 0.1 g of 1-ethynylcyclohexanol inhibitor, and 0.2 g of Karstedt platinum catalyst were added to the base material in sequence and mixed uniformly. The mixture was vacuumed to remove bubbles. Finally, 4 g of an organosilicon tackifier was added thereto, mixed uniformly, vacuumed to remove bubbles, and dried to obtain a silicone rubber adhesive.

[0034] Example 3

[0035] (1) Add 5 g of vinyl isophthalic acid and 0.01 g of tetraethylammonium bromide catalyst into a flask containing toluene solvent, stir to dissolve, add 45% by mass sodium hydroxide solution, stir to disperse, and finally add 9 g of epichlorohydrin. Reflux at 115° C. for 3 h, add deionized water, stand to separate, concentrate the organic phase, and wash with n-hexane to obtain vinyl isophthalic acid glycidyl ester.

[0036] (2) 40 g of tripropylene glycol diacrylate and 0.02 g of Karstedt's platinum catalyst are placed in a flask filled with isopropanol solvent and stirred to dissolve. 25 g of hydrogenated silicone oil is added thereto and reacted at 60° C. for 2 h. The mixture is cooled to room temperature and activated carbon is added thereto to adsorb the Karstedt's platinum catalyst. The mixture is filtered and the filtrate is distilled under reduced pressure to obtain vinyl silicone oil.

[0037] (3) 4 g of allyl ester-modified rosin was placed in a flask filled with ethanol solvent, stirred to dissolve, and heated to 80° C., 0.3 g of azobisisobutyronitrile initiator, 3 g of vinyl isophthalic acid glycidyl ester, and 20 g of vinyl silicone oil were added thereto, and the mixture was reacted for 6 h to obtain an organosilicon tackifier.

[0038] (4) 200 g of vinyl silicone oil, 50 g of vinyl MQ resin, 40 g of white carbon black, and 20 g of hexamethyldisilazane were mixed uniformly at high speed, heated to 120° C., and vacuumed to remove low-boiling substances to obtain a base material. 4 g of hydrogenated silicone oil, 0.15 g of 1-ethynylcyclohexanol inhibitor, and 0.1 g of Karstedt platinum catalyst were added to the base material in sequence, mixed uniformly, vacuumed to remove bubbles, and finally 6 g of an organosilicon tackifier was added thereto, mixed uniformly, vacuumed to remove bubbles, and dried to obtain a silicone rubber adhesive.

[0039] Example 4

[0040] (1) Add 5 g of vinyl isophthalic acid and 0.01 g of tetraethylammonium bromide catalyst into a flask containing toluene solvent, stir to dissolve, add 45% by mass sodium hydroxide solution, stir to disperse, and finally add 9 g of epichlorohydrin. Reflux at 100° C. for 3 h, add deionized water, stand to separate, concentrate the organic phase, and wash with n-hexane to obtain vinyl isophthalic acid glycidyl ester.

[0041] (2) 30 g of tripropylene glycol diacrylate and 0.03 g of Karstedt's platinum catalyst are placed in a flask filled with isopropanol solvent and stirred to dissolve. 25 g of hydrogenated silicone oil is added thereto and reacted at 60° C. for 3 h. The mixture is cooled to room temperature and activated carbon is added thereto to adsorb the Karstedt's platinum catalyst. The mixture is filtered and the filtrate is distilled under reduced pressure to obtain vinyl silicone oil.

[0042] (3) 5 g of allyl ester-modified rosin was placed in a flask filled with ethanol solvent, stirred to dissolve, and heated to 80° C., and 0.36 g of azobisisobutyronitrile initiator, 5 g of vinyl isophthalic acid glycidyl ester, and 20 g of vinyl silicone oil were added thereto, and the mixture was reacted for 5 h to obtain an organosilicon tackifier.

[0043] (4) 200 g of vinyl silicone oil, 60 g of vinyl MQ resin, 40 g of white carbon black, and 20 g of hexamethyldisilazane were mixed uniformly at high speed, heated to 120° C., and decompressed and evacuated to remove low-boiling substances to obtain a base material. 6 g of hydrogenated silicone oil, 0.1 g of 1-ethynylcyclohexanol inhibitor, and 0.15 g of Karstedt platinum catalyst were added to the base material in sequence and mixed uniformly. The mixture was evacuated to remove bubbles. Finally, 8 g of an organosilicon tackifier was added thereto, mixed uniformly, and the mixture was vacuumed to remove bubbles. The mixture was dried to obtain a silicone rubber adhesive.

[0044] Example 5

[0045] (1) Add 5 g of vinyl isophthalic acid and 0.02 g of tetraethylammonium bromide catalyst into a flask containing toluene solvent, stir to dissolve, add 35% by mass sodium hydroxide solution, stir to disperse, and finally add 9 g of epichlorohydrin. Reflux at 110° C. for 4 h, add deionized water, stand to separate, concentrate the organic phase, and wash with n-hexane to obtain vinyl isophthalic acid glycidyl ester.

[0046] (2) 40 g of tripropylene glycol diacrylate and 0.015 g of Karstedt's platinum catalyst are placed in a flask filled with isopropanol solvent and stirred to dissolve. 25 g of hydrogenated silicone oil is added thereto and reacted at 60° C. for 4 h. The mixture is cooled to room temperature and activated carbon is added thereto to adsorb the Karstedt's platinum catalyst. The mixture is filtered and the filtrate is distilled under reduced pressure to obtain vinyl silicone oil.

[0047] (3) 5 g of allyl ester-modified rosin was placed in a flask filled with ethanol solvent, stirred to dissolve, and heated to 80° C., and 0.3 g of azobisisobutyronitrile initiator, 3 g of vinyl isophthalic acid glycidyl ester, and 20 g of vinyl silicone oil were added thereto, and the reaction was carried out for 6 h to obtain an organosilicon tackifier.

[0048] (4) 200 g of vinyl silicone oil, 50 g of vinyl MQ resin, 40 g of white carbon black, and 20 g of hexamethyldisilazane were mixed uniformly at high speed, heated to 120° C., and vacuumed to remove low-boiling substances to obtain a base material. 6 g of hydrogenated silicone oil, 0.1 g of 1-ethynylcyclohexanol inhibitor, and 0.1 g of Karstedt platinum catalyst were added to the base material in sequence and mixed uniformly. The air bubbles were removed by vacuuming. Finally, 10 g of an organosilicon tackifier was added thereto, mixed uniformly, vacuumed to remove air bubbles, and dried to obtain a silicone rubber adhesive.

[0049] Comparative Example 1

[0050] (1) 40 g of tripropylene glycol diacrylate and 0.02 g of Karstedt's platinum catalyst are placed in a flask filled with isopropanol solvent and stirred to dissolve. 25 g of hydrogenated silicone oil is added thereto and reacted at 60° C. for 4 h. The mixture is cooled to room temperature and activated carbon is added thereto to adsorb the Karstedt's platinum catalyst. The mixture is filtered and the filtrate is subjected to reduced pressure distillation to obtain vinyl silicone oil.

[0051] (2) 200 g of vinyl silicone oil, 60 g of vinyl MQ resin, 40 g of white carbon black, and 10 g of hexamethyldisilazane were mixed uniformly at high speed, heated to 120° C., and vacuumed to remove low-boiling substances to obtain a base material. 4 g of hydrogenated silicone oil, 0.15 g of 1-ethynylcyclohexanol inhibitor, and 0.1 g of Karstedt platinum catalyst were added to the base material in sequence, mixed uniformly, vacuumed to remove bubbles, and finally 2 g of alkenyl silicone oil was added thereto, mixed uniformly, vacuumed to remove bubbles, and dried to obtain a silicone rubber adhesive.

[0052] Comparative Example 2

[0053] (1) 5 g of vinyl isophthalic acid and 0.01 g of tetraethylammonium bromide catalyst were added to a flask containing toluene solvent, stirred to dissolve, 40% by mass sodium hydroxide solution was added thereto, stirred to disperse, and finally 10 g of epichlorohydrin was added thereto. The mixture was refluxed at 110° C. for 3 h, deionized water was added, the mixture was allowed to stand for stratification, the organic phase was concentrated, and the mixture was washed with n-hexane to obtain vinyl isophthalic acid glycidyl ester.

[0054] (2) 40 g of tripropylene glycol diacrylate and 0.02 g of Karstedt's platinum catalyst are placed in a flask filled with isopropanol solvent and stirred to dissolve. 25 g of hydrogenated silicone oil is added thereto and reacted at 60° C. for 4 h. The mixture is cooled to room temperature and activated carbon is added thereto to adsorb the Karstedt's platinum catalyst. The mixture is filtered and the filtrate is distilled under reduced pressure to obtain vinyl silicone oil.

[0055] (3) 0.2 g of azobisisobutyronitrile initiator, 3 g of vinyl isophthalic acid glycidyl ester, and 20 g of vinyl silicone oil were placed in a flask filled with ethanol solvent, stirred to dissolve, and heated to 80° C. for reaction for 5 h to obtain an organosilicon tackifier.

[0056] (4) 200 g of vinyl silicone oil, 60 g of vinyl MQ resin, 40 g of white carbon black, and 10 g of hexamethyldisilazane were mixed uniformly at high speed, heated to 120° C., and vacuumed to remove low-boiling substances to obtain a base material. 4 g of hydrogenated silicone oil, 0.15 g of 1-ethynylcyclohexanol inhibitor, and 0.1 g of Karstedt platinum catalyst were added to the base material in sequence, mixed uniformly, vacuumed to remove bubbles, and finally 2 g of an organosilicon tackifier was added thereto, mixed uniformly, vacuumed to remove bubbles, and dried to obtain a silicone rubber adhesive.

[0057] Comparative Example 3

[0058] (1) 40 g of tripropylene glycol diacrylate and 0.02 g of Karstedt's platinum catalyst are placed in a flask filled with isopropanol solvent and stirred to dissolve. 25 g of hydrogenated silicone oil is added thereto and reacted at 60° C. for 4 h. The mixture is cooled to room temperature and activated carbon is added thereto to adsorb the Karstedt's platinum catalyst. The mixture is filtered and the filtrate is subjected to reduced pressure distillation to obtain vinyl silicone oil.

[0059] (2) 3 g of allyl ester-modified rosin was placed in a flask filled with ethanol solvent, stirred to dissolve, and heated to 80° C., 0.2 g of azobisisobutyronitrile initiator and 20 g of vinyl silicone oil were added thereto, and the reaction was carried out for 5 h to obtain an organosilicon tackifier.

[0060] (3) 200 g of vinyl silicone oil, 60 g of vinyl MQ resin, 40 g of white carbon black, and 10 g of hexamethyldisilazane were mixed uniformly at high speed, heated to 120° C., and vacuumed to remove low-boiling substances to obtain a base material. 4 g of hydrogenated silicone oil, 0.15 g of 1-ethynylcyclohexanol inhibitor, and 0.1 g of Karstedt platinum catalyst were added to the base material in sequence, mixed uniformly, vacuumed to remove bubbles, and finally 2 g of an organosilicon tackifier was added thereto, mixed uniformly, vacuumed to remove bubbles, and dried to obtain a silicone rubber adhesive.

[0061] Use a universal tensile testing machine to test the tensile properties of silicone rubber adhesive.

[0062] Use a Shore A durometer to test the Shore A hardness of silicone rubber.

[0063] Shore A Hardness Tensile strength / MPa Elongation at break / % Example 1 19 5.1 795 Example 2 21 5.4 835 Example 3 22 5.8 880 Example 4 24 6.4 945 Example 5 21 6.0 900 Comparative Example 1 17 4.2 740 Comparative Example 3 18 4.5 775 Comparative Example 3 18 4.3 731

[0064] The mechanical properties of Examples 1-5 are better than those of Comparative Examples 1-3, because silicone tackifiers are added to Examples 1-5. The performance of Example 4 is the best, because the more silicone tackifiers are added, the stronger the interaction is, but the mechanical properties of Example 5 are worse than those of Example 4, because when more silicone tackifiers are added, the crosslinking density is higher, which makes the silicone rubber brittle, causing stress concentration, thereby reducing the mechanical properties. Comparative Examples 1-3 sequentially add alkenyl silicone oil, alkenyl silicone oil and vinyl isophthalic acid glycidyl, alkenyl silicone oil and allyl ester modified rosin, which have a certain degree of crosslinking and secondary bonds such as hydrogen bonds, but their mechanical properties are still not as good as the composite effect of the three, so their mechanical properties are poor.

[0065] According to GB / T7124-2008, the bonding performance of the adhesive was measured using aluminum plate as the test substrate.

[0066] Adhesive strength / MPa Example 1 0.28 Example 2 0.31 Example 3 0.38 Example 4 0.49 Example 5 0.45 Comparative Example 1 0.15 Comparative Example 2 0.22 Comparative Example 3 0.19

[0067] The bonding effect of Examples 1-5 is better than that of Comparative Examples 1-3. The silicone tackifiers added in Examples 1-5 contain carboxyl, ester, epoxy and other groups that can react chemically with the active groups on the surface of the substrate to establish chemical bonds and have strong adhesion. The main tackifying components of the silicone tackifier added in Comparative Example 2 are epoxy groups and ester groups, and the main tackifying components of Comparative Example 3 are carboxyl groups and ester groups. Therefore, its tackifying effect is better than that of Comparative Example 1, but not as good as that of Examples 1-5. Therefore, the tackifying effect of the silicone tackifiers in Examples 1-5 is good.

[0068] Finally, it should be noted that the above 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, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing an organosilicon tackifier, characterized in that: The preparation method comprises the following steps: (1) Add vinyl isophthalic acid and tetraethylammonium bromide catalyst into a flask containing toluene solvent, stir to dissolve, add sodium hydroxide solution thereto, stir to disperse, finally add epichlorohydrin thereto, reflux at 100-115° C. for 2-4 hours, add deionized water, stand to separate, concentrate the organic phase, wash with n-hexane, and obtain vinyl isophthalic acid glycidyl ester; (2) placing the allyl ester modified rosin in a flask filled with ethanol solvent, stirring to dissolve, heating to 70-85° C., adding azobisisobutyronitrile initiator, vinyl isophthalic acid glycidyl ester, and alkenyl silicone oil, and reacting for 4-6 hours to obtain an organosilicon tackifier.

2. The method for preparing the organosilicon tackifier according to claim 1, characterized in that: In the step (1), the mass ratio of vinyl isophthalic acid, tetraethylammonium bromide and epichlorohydrin is 100:0.2-0.6:160-200.

3. The method for preparing the organosilicon tackifier according to claim 1, characterized in that: The mass fraction of the sodium hydroxide solution in step (1) is 30-45%.

4. The method for preparing the organosilicon tackifier according to claim 1, characterized in that: In the step (2), the mass ratio of allyl ester modified rosin, azobisisobutyronitrile, vinyl isophthalate glycidyl ester and alkenyl silicone oil is 15-35:1-1.8:10-25:

100.

5. The method for preparing the organosilicon tackifier according to claim 1, characterized in that: The preparation method of alkenyl silicone oil in step (2) is as follows: (3) tripropylene glycol diacrylate and Karstedt platinum catalyst are placed in a flask filled with isopropanol solvent, stirred to dissolve, hydrogenated silicone oil is added thereto, reacted at 50-70° C. for 2-4 hours, cooled to room temperature, activated carbon is added thereto to adsorb the Karstedt platinum catalyst, filtered, and the filtrate is subjected to reduced pressure distillation to obtain vinyl silicone oil.

6. The method for preparing the organosilicon tackifier according to claim 5, characterized in that: In the step (3), the mass ratio of hydrogenated silicone oil, tripropylene glycol diacrylate and Karstedt platinum catalyst is 100:120-200:0.06-0.

12.

7. Use of the organosilicon tackifier obtained by the preparation method according to claim 1 in silicone rubber adhesive, characterized in that: 100 parts by weight of vinyl silicone oil, 20-30 parts of vinyl MQ resin, 15-25 parts of white carbon black and 5-12 parts of hexamethyldisilazane are uniformly mixed at high speed, heated to 110-130° C., and vacuumed to remove low-boiling substances to obtain a base material. 1-3 parts of hydrogenated silicone oil, 0.05-0.1 parts of 1-ethynylcyclohexanol inhibitor and 0.02-0.1 parts of Karstedt platinum catalyst are sequentially added to the base material and mixed evenly. Vacuum is used to remove bubbles. Finally, 1-5 parts of an organosilicon tackifier are added thereto, mixed evenly, vacuumed to remove bubbles, and dried to obtain a silicone rubber adhesive.

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