Tackifier, single-component addition type organic silicon sealant and preparation method of single-component addition type organic silicon sealant
By introducing new tackifiers and other specific materials into the single-component addition silicone sealant, the problem of reverse sticking of sealant after high temperature aging is solved, and the efficient bonding and anti-compression and anti-adhesion characteristics of metal substrates are improved.
Patent Information
- Application Number
- CN202311796157.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-25
- Publication Date
- 2025-06-27
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Figure BDA0004627766820000021 
Figure BDA0004627766820000031 
Figure BDA0004627766820000051
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of sealants, and particularly to a tackifier, a one-component addition-cured silicone sealant and a preparation method thereof. Background Art
[0002] The core components of new energy electric vehicles include power batteries, electric drive systems and high-voltage electric control systems. Whether it is a power battery, an electric drive system or a high-voltage electric control system, it is necessary to seal the outer shell with a sealant / seal ring to isolate external water, dust, oil and other impurities, meeting the requirements of IP67 protection level.
[0003] There are mainly three processes for sealing new energy vehicle systems: the seal ring process, the FIPG process and the CIPG process. The traditional seal ring process is to install a formed prefabricated seal ring on the sealing surface, and the seal is achieved after press-fitting. The advantage of this process is that the molded seal ring has high dimensional accuracy, but the process requires manual operation, cannot achieve automatic dispensing, the accuracy and consistency of manual installation are poor, and various molds need to be made according to different sealing structures, resulting in high mold costs. The FIPG process, also known as the "wet assembly method", is to apply a liquid sealant on the sealing surface, assemble the product in the state where the sealant is not cured, and then it is necessary to place it for a period of time to completely cure the sealant, so that the upper and lower contacting sealing panels are well bonded to achieve the sealing effect. The advantage of this process is that it realizes the automation process of dispensing and has high sealing reliability, but since both sides of the sealing surface are bonded, it is difficult to repair later. The CIPG process, also known as the "dry assembly method", is a process of applying a liquid sealant (usually a heat-cured addition silicone rubber) to the sealing surface and then using mechanical locking (i.e., compression) to achieve seal protection. This process combines the advantages of the traditional seal ring and FIPG. It not only realizes the automatic dispensing process, but also is convenient for later disassembly and repair due to the use of a single-sided bonding method.
[0004] At present, the CIPG process generally uses a heat-cured one-component addition-cured silicone sealant, but this product usually has the problem of reverse adhesion after high-temperature aging, that is, after the cured glue line is compressed, it also shows adhesion or sticking to the reverse material after high-temperature aging, resulting in difficult disassembly and easy damage to the glue line and inability to be used again. Summary of the Invention
[0005] Based on this, the purpose of the present invention is to provide a one-component addition-cured silicone sealant with anti-compression reverse adhesion characteristics.
[0006] In order to achieve the above purpose, the present invention includes the following technical solutions.
[0007] On the one hand, the present invention provides a tackifier which, while achieving effective adhesion to a metal substrate, can improve the reverse adhesion of a silicone sealant to the back cover plate. The tackifier is obtained by reacting tetramethylcyclotetrasiloxane, dimethylmethoxyvinylsilane, and allyl glycidyl ether under the catalysis of a platinum catalyst.
[0008] On the second hand, the present invention provides a preparation method of the tackifier, comprising the following steps:
[0009] Add an organic solvent, tetramethylcyclotetrasiloxane, and a platinum catalyst to a reactor and stir evenly; heat the resulting mixture to 60°C - 80°C under the protection of an inert gas, and dropwise add the allyl glycidyl ether and dimethylmethoxyvinylsilane respectively, and react for 2h - 3h; remove low boilers, the organic solvent, and the platinum catalyst to obtain the tackifier.
[0010] On the third aspect, the present invention provides a one-component addition-curing silicone sealant, and the raw materials for its preparation include the tackifier of the present invention.
[0011] Preferably, the raw materials for the preparation of the one-component addition-curing silicone sealant include a platinum catalyst and the following components in parts by weight:
[0012]
[0013]
[0014] The dosage of the platinum catalyst is 0.5 ppm - 10 ppm based on the mass of platinum;
[0015] The release regulator is a fluorosilane.
[0016] Preferably, the release regulator is selected from one or a combination of 3,3,3-trifluoropropyl dimethylmethoxysilane (dimethylmethoxy(3,3,3-fluoropropyl)silane), 3,3,3-trifluoropropyl dimethylethoxysilane, 3,3,3-trifluoropropyl methyldimethoxysilane, and 3,3,3-trifluoropropyl methyldiethoxysilane.
[0017] On the fourth aspect, the present invention further provides a preparation method of the one-component addition-curing silicone sealant, comprising the following steps:
[0018] (1) Put the terminal vinyl silicone oil into a kneader, then batchwise add fumed silica, knead for 1h - 2h, then heat up to 120°C - 150°C and evacuate, and knead for 2h - 4h to obtain a base material;
[0019] (2) Put the base material, a hydrogen-containing crosslinking agent, and fumed titanium dioxide into a planetary mixer, and stir for 30min - 60min after adding to mix evenly;
[0020] (3) Put the tackifier, inhibitor, and release regulator into a planetary mixer and stir for 30 min to 60 min until evenly mixed;
[0021] (4) Put the platinum catalyst into a planetary mixer, stir and mix under vacuum for 20 min to 40 min to obtain the one-component addition-curing silicone sealant.
[0022] The present invention uses tetramethylcyclotetrasiloxane, dimethylmethoxyvinylsilane, and allyl glycidyl ether as raw materials, and under the catalysis of a platinum catalyst, a novel tackifier is obtained through reaction. Using this tackifier in the preparation of addition-curing silicone sealants can achieve effective adhesion to metal substrates while improving the anti-sticking phenomenon of the silicone sealant to the reverse cover plate.
[0023] Furthermore, using the novel tackifier prepared by the present invention, vinyl-terminated silicone oil, fumed silica, hydrogen-containing crosslinking agent, fumed titanium dioxide, release regulator, etc. as raw materials, a one-component addition-curing silicone sealant with excellent anti-compression anti-sticking properties is prepared. Among them, the self-made tackifier achieves high adhesiveness to metal substrates and, to a certain extent, improves the anti-sticking phenomenon of the silicone sealant to the reverse cover plate; the post-curing of the sealant is effectively controlled by fumed titanium dioxide, and the hydroxyl groups on the fumed titanium dioxide have a hydrogen bond anchoring effect on the active groups of the residual tackifier in the cured colloid, which can slow down the migration of the residual tackifier to the reverse substrate; using fluorosilane as the release regulator, it migrates to the colloid interface (solid-gas interface) to form a release layer, thereby avoiding further reaction between the residual tackifier and the reverse substrate and effectively reducing the risk of anti-sticking. Through the synergistic cooperation of each component, the prepared one-component addition-curing silicone sealant not only has excellent adhesion performance to metal substrates, but also will not cause adhesion and sticking to the reverse contact substrate after being compressed and baked at high temperature for a long time, and has excellent anti-compression anti-sticking properties. Specific Embodiments
[0024] The technical solutions of the present invention will be further described below through specific examples. Those skilled in the art should understand that the examples are only for helping to understand the present invention and should not be regarded as specific limitations to the present invention.
[0025] Unless otherwise defined, all technical and scientific terms used in the present invention have the same meaning as commonly understood by those skilled in the technical field to which the present invention belongs. The terms used in the specification of the present invention are only for the purpose of describing specific embodiments and are not used to limit the present invention.
[0026] The terms "comprise" and "have" and any variations thereof in the present invention are intended to cover non-exclusive inclusion. For example, a process, method, device, product or equipment that includes a series of steps is not limited to the listed steps or modules, but optionally further includes steps not listed, or optionally further includes other steps inherent to these processes, methods, products or equipment.
[0027] As used in the present invention, "a plurality of" means two or more. "And / or" describes the association relationship of associated objects and indicates that there can be three relationships. For example, A and / or B can represent three situations: A exists alone, A and B exist simultaneously, and B exists alone. The character " / " generally represents an "or" relationship between the associated objects before and after.
[0028] In one embodiment of the present invention, the present invention provides a tackifier, which is obtained by reacting tetramethylcyclotetrasiloxane, dimethylmethoxyvinylsilane and allyl glycidyl ether under the catalysis of a platinum catalyst. While achieving effective adhesion to the metal substrate, this tackifier can improve the reverse adhesion phenomenon of the silicone sealant to the back cover plate.
[0029] In some of these embodiments, the mass ratio of the tetramethylcyclotetrasiloxane, dimethylmethoxyvinylsilane and allyl glycidyl ether is 50:20 - 30:15 - 25.
[0030] In some of these embodiments, the mass ratio of the tetramethylcyclotetrasiloxane, dimethylmethoxyvinylsilane and allyl glycidyl ether is 50:25:20.
[0031] In some of these embodiments, the platinum catalyst is one or a combination of chloroplatinic acid, chloroplatinic acid - isopropanol complex, and Karstedt's catalyst.
[0032] In another embodiment of the present invention, the present invention provides a method for preparing the tackifier, which includes the following steps:
[0033] Add an organic solvent, tetramethylcyclotetrasiloxane and a platinum catalyst to a reactor and stir evenly; heat the resulting mixture to 60°C - 80°C under the protection of an inert gas, and dropwise add the allyl glycidyl ether and dimethylmethoxyvinylsilane respectively, and react for 2h - 3h; remove low boilers, the organic solvent and the platinum catalyst to obtain the tackifier.
[0034] In some of these embodiments, the organic solvent is toluene.
[0035] In some of these embodiments, the addition amount of the organic solvent is 0.8 - 1.2 times the weight of the tetramethylcyclotetrasiloxane.
[0036] In some of these embodiments, the addition amount of the platinum catalyst is 0.5 ppm to 5 ppm based on the mass of platinum.
[0037] In another embodiment of the present invention, the present invention also provides a one-component addition-curing silicone sealant, and the raw materials for its preparation include the tackifier described in the present invention.
[0038] In some of these embodiments, the raw materials for the preparation of the one-component addition-curing silicone sealant include a platinum catalyst and the following components in parts by weight:
[0039]
[0040]
[0041] The amount of the platinum catalyst used is 0.5 ppm to 10 ppm based on the mass of platinum;
[0042] The release regulator is a fluorosilane.
[0043] In some of these embodiments, the raw materials for the preparation of the one-component addition-curing silicone sealant include a platinum catalyst and the following components in parts by weight:
[0044]
[0045] In some of these embodiments, the release regulator is selected from one or a combination of trifluoropropyl dimethyl methoxysilane (dimethyl methoxy(3,3,3-fluoropropyl)silane), trifluoropropyl dimethyl ethoxysilane, trifluoropropyl methyl dimethoxysilane, and trifluoropropyl methyl diethoxysilane.
[0046] In some of these embodiments, the amount of the platinum catalyst in the one-component addition-curing silicone sealant is 3 ppm to 8 ppm based on the mass of platinum.
[0047] In some of these embodiments, the viscosity of the terminal vinyl silicone oil at 25 °C is 1000 mPa·s to 100000 mPa·s, preferably 5000 mPa·s to 20000 mPa·s; more preferably 8000 mPa·s to 12000 mPa·s.
[0048] In some of these embodiments, the specific surface area of the fumed silica is 100 m 2 / g to 400 m 2 / g, preferably 150 m 2 / g to 250 m 2 / g.
[0049] In some of these embodiments, the hydrogen-containing crosslinking agent is side hydrogen-containing silicone oil and / or terminal side hydrogen-containing silicone oil.
[0050] In some of these embodiments, the hydrogen content of the hydrogen-containing crosslinking agent is 0.2 wt% to 2 wt%, and the viscosity is 10 mPa·s to 200 mPa·s.
[0051] In some of these embodiments, the hydrogen content of the hydrogen-containing crosslinking agent is 0.5 wt% to 1.2 wt%, and the viscosity is 20 mPa·s to 120 mPa·s.
[0052] In some of these embodiments, the inhibitor is selected from one or a combination of 1-ethynyl-1-cyclohexanol, tetramethyltetravinylcyclotetrasiloxane, 2-methyl-3-butyn-2-ol, 3-methyl-1-hexyn-3-ol, 3,5-dimethyl-1-hexyn-3-ol, and 3-methyl-1-dodecyn-3-ol.
[0053] In some of these embodiments, the specific surface area of the fumed titanium dioxide is 30 m 2 / g to 100 m 2 / g, preferably 40 m 2 / g to 60 m 2 / g.
[0054] In some of these embodiments, the platinum catalyst is selected from one or a combination of chloroplatinic acid, chloroplatinic acid-isopropanol complex, and Karstedt's catalyst.
[0055] In another embodiment of the present invention, the present invention also provides a method for preparing the one-component addition-curable silicone sealant, comprising the following steps:
[0056] (1) Put the terminal vinyl silicone oil into a kneader, then batchwise add fumed silica, knead for 1 h to 2 h, then raise the temperature to 120 °C to 150 °C and evacuate to vacuum, and knead for 2 h to 4 h to obtain a base material;
[0057] (2) Put the base material, hydrogen-containing crosslinking agent, and fumed titanium dioxide into a planetary mixer, and stir for 30 min to 60 min after adding until evenly mixed;
[0058] (3) Put the tackifier, inhibitor, and release regulator into a planetary mixer, and stir for 30 min to 60 min until evenly mixed;
[0059] (4) Put the platinum catalyst into a planetary mixer, stir and evacuate to vacuum and mix for 20 min to 40 min to obtain the one-component addition-curable silicone sealant.
[0060] The viscosity mentioned in the present invention refers to the viscosity under the test condition of 25 °C.
[0061] The "terminal vinyl silicone oil" described in the present invention refers to polydimethylsiloxane with Si-Vi groups at both ends of each molecule, where Vi refers to vinyl.
[0062] The "side hydrogen-containing silicone oil" described in the present invention refers to polydimethylsiloxane containing Si-H groups, and the Si-H groups are present in the side chains of the molecules rather than at the ends.
[0063] The "terminal and side hydrogen-containing silicone oil" described in the present invention refers to polydimethylsiloxane with Si-H groups at both ends of each molecule and also containing Si-H groups in the side chains.
[0064] In the following examples, the content of the Karstedt catalyst is based on the mass of platinum.
[0065] The following are specific examples.
[0066] The preparation method of the self-made tackifier used in the following examples is as follows:
[0067] (1) Add 45 parts by weight of toluene, 50 parts by weight of tetramethylcyclotetrasiloxane and 2 ppm of Karstedt catalyst into a reaction kettle, and stir evenly at room temperature;
[0068] (2) Under the protection of nitrogen, heat up to 70 °C, and dropwise add 20 parts by weight of allyl glycidyl ether and 25 parts by weight of dimethylmethoxyvinylsilane respectively, react for 2.5 h, and turn off the nitrogen;
[0069] (3) After the reaction, remove the low-boiling substances and toluene under reduced pressure, and adsorb and remove the Karstedt catalyst with activated carbon to obtain the self-made tackifier.
[0070] Example 1
[0071] A one-component addition-curing silicone sealant, and its raw material composition is as follows:
[0072]
[0073] The specific preparation method includes the following steps:
[0074] (1) Put the terminal vinyl silicone oil into a kneader, then add the fumed silica in batches, knead at room temperature for 1 h, then heat up to 120 °C and evacuate to -0.09 MPa, and knead for 3 h to obtain the base material;
[0075] (2) Put the base material, the hydrogen-containing crosslinking agent and the fumed titanium dioxide into a planetary mixer, and stir for 45 min until evenly mixed after adding;
[0076] (3) Put the self-made tackifier, the inhibitor and the release regulator into a planetary mixer, and stir for 50 min until evenly mixed;
[0077] (4) Put the catalyst into a planetary mixer, stir and evacuate to -0.09 MPa for 30 min to obtain the one-component addition-curing silicone sealant.
[0078] Example 2
[0079] A one-component addition-curing silicone sealant, and its raw material composition is as follows:
[0080]
[0081] The specific preparation method includes the following steps:
[0082] (1) Put the vinyl-terminated silicone oil into a kneader, then add the fumed silica in batches, knead at room temperature for 1 h, then heat up to 120 °C and evacuate to -0.09 MPa, and knead for 3 h to obtain the base material;
[0083] (2) Put the base material, hydrogen-containing crosslinking agent and fumed titanium dioxide into a planetary mixer, and stir for 45 min until evenly mixed after adding;
[0084] (3) Put the self-made tackifier, inhibitor and release regulator into a planetary mixer, and stir for 50 min until evenly mixed;
[0085] (4) Put the catalyst into a planetary mixer, stir and evacuate to -0.09 MPa for 30 min to obtain the one-component addition-curing silicone sealant.
[0086] Example 3
[0087] A one-component addition-curing silicone sealant, and its raw material composition is as follows:
[0088]
[0089] The specific preparation method includes the following steps:
[0090] (1) Put the vinyl-terminated silicone oil into a kneader, then add the fumed silica in batches, knead at room temperature for 1 h, then heat up to 120 °C and evacuate to -0.09 MPa, and knead for 3 h to obtain the base material;
[0091] (2) Put the base material, hydrogen-containing crosslinking agent and fumed titanium dioxide into a planetary mixer, and stir for 45 min until evenly mixed after adding;
[0092] (3) Put the self-made tackifier, inhibitor and release regulator into a planetary mixer, and stir for 50 min until evenly mixed;
[0093] (4) Put the catalyst into a planetary mixer, stir and evacuate to -0.09 MPa for 30 min to obtain the single-component addition-curing silicone sealant.
[0094] Example 4
[0095] A single-component addition-curing silicone sealant, whose raw material composition is as follows:
[0096]
[0097] The specific preparation method includes the following steps:
[0098] (1) Put the vinyl-terminated silicone oil into a kneader, then add the fumed silica in batches, knead at room temperature for 1 h, then raise the temperature to 120 °C and evacuate to -0.09 MPa, and knead for 3 h to obtain the base material;
[0099] (2) Put the base material, hydrogen-containing crosslinking agent and fumed titanium dioxide into a planetary mixer, and stir for 45 min after adding until evenly mixed;
[0100] (3) Put the self-made tackifier, inhibitor and release regulator into a planetary mixer, and stir for 50 min until evenly mixed;
[0101] (4) Put the catalyst into a planetary mixer, stir and evacuate to -0.09 MPa for 30 min to obtain the single-component addition-curing silicone sealant.
[0102] Example 5
[0103] A single-component addition-curing silicone sealant, whose raw material composition is as follows:
[0104]
[0105] The specific preparation method includes the following steps:
[0106] (1) Put the vinyl-terminated silicone oil into a kneader, then add the fumed silica in batches, knead at room temperature for 1 h, then raise the temperature to 120 °C and evacuate to -0.09 MPa, and knead for 3 h to obtain the base material;
[0107] (2) Put the base material, hydrogen-containing crosslinking agent and fumed titanium dioxide into a planetary mixer, and stir for 45 min after adding until evenly mixed;
[0108] (3) Put the self-made tackifier, inhibitor and release regulator into a planetary mixer, and stir for 50 min until evenly mixed;
[0109] (4) Put the catalyst into a planetary mixer, stir and evacuate to -0.09 MPa for 30 min to obtain the one-component addition-curing silicone sealant.
[0110] Comparative Example 1
[0111] A one-component addition-curing silicone sealant, and its raw material composition is as follows:
[0112]
[0113]
[0114] The specific preparation method includes the following steps:
[0115] (1) Put the vinyl-terminated silicone oil into a kneader, then add the fumed silica in batches, knead at room temperature for 1 h, then heat up to 120 °C and evacuate to -0.09 MPa, and knead for 3 h to obtain the base material;
[0116] (2) Put the base material, hydrogen-containing crosslinking agent and fumed titanium dioxide into a planetary mixer, and stir for 45 min until evenly mixed after adding;
[0117] (3) Put the self-made tackifier and inhibitor into a planetary mixer, and stir for 50 min until evenly mixed;
[0118] (4) Put the catalyst into a planetary mixer, stir and evacuate to -0.09 MPa for 30 min to obtain the one-component addition-curing silicone sealant.
[0119] Comparative Example 2
[0120] A one-component addition-curing silicone sealant, and its raw material composition is as follows:
[0121]
[0122]
[0123] The specific preparation method includes the following steps:
[0124] (1) Put the vinyl-terminated silicone oil into a kneader, then add the fumed silica in batches, knead at room temperature for 1 h, then heat up to 120 °C and evacuate to -0.09 MPa, and knead for 3 h to obtain the base material;
[0125] (2) Put the base material and hydrogen-containing crosslinking agent into a planetary mixer, and stir for 45 min until evenly mixed after adding;
[0126] (3) Put the self-made tackifier, inhibitor and release regulator into a planetary mixer, and stir for 50 min until evenly mixed;
[0127] (4) Put the catalyst into a planetary mixer, stir and evacuate to -0.09 MPa and mix for 30 min to obtain the single-component addition-curing silicone sealant.
[0128] Comparative Example 3
[0129] A single-component addition-curing silicone sealant, the raw material composition thereof is as follows:
[0130]
[0131]
[0132] The specific preparation method comprises the following steps:
[0133] (1) Put the vinyl-terminated silicone oil into a kneader, then batchwise add the fumed silica, knead at room temperature for 1 h, then raise the temperature to 120 °C and evacuate to -0.09 MPa, and knead for 3 h to obtain the base material;
[0134] (2) Put the base material, the hydrogen-containing crosslinking agent and the fumed titanium dioxide into a planetary mixer, and stir for 45 min until evenly mixed after adding;
[0135] (3) Put the commercially available tackifier, inhibitor and release regulator into a planetary mixer, and stir for 50 min until evenly mixed;
[0136] (4) Put the catalyst into a planetary mixer, stir and evacuate to -0.09 MPa and mix for 30 min to obtain the single-component addition-curing silicone sealant.
[0137] Comparative Example 4
[0138] A single-component addition-curing silicone sealant, the raw material composition thereof is as follows:
[0139]
[0140] The specific preparation method comprises the following steps:
[0141] (1) Put the vinyl-terminated silicone oil into a kneader, then batchwise add the fumed silica, knead at room temperature for 1 h, then raise the temperature to 120 °C and evacuate to -0.09 MPa, and knead for 3 h to obtain the base material;
[0142] (2) Put the base material and the hydrogen-containing crosslinking agent into a planetary mixer, and stir for 45 min until evenly mixed after adding;
[0143] (3) Put the commercially available tackifier and inhibitor into a planetary mixer, and stir for 50 min until evenly mixed;
[0144] (4) Put the catalyst into a planetary mixer, stir and evacuate to -0.09 MPa for 30 min to obtain the single-component addition-curing silicone sealant.
[0145] Comparative Example 5
[0146] A single-component addition-curing silicone sealant, whose raw material composition is as follows:
[0147]
[0148] The specific preparation method includes the following steps:
[0149] (1) Put the vinyl-terminated silicone oil into a kneader, then add the fumed silica in batches, knead at room temperature for 1 h, then heat up to 120 °C and evacuate to -0.09 MPa, and knead for 3 h to obtain the base material;
[0150] (2) Put the base material and the hydrogen-containing crosslinking agent into a planetary mixer, and stir for 45 min after adding until evenly mixed;
[0151] (3) Put the self-made tackifier and inhibitor into a planetary mixer, and stir for 50 min until evenly mixed;
[0152] (4) Put the catalyst into a planetary mixer, stir and evacuate to -0.09 MPa for 30 min to obtain the single-component addition-curing silicone sealant.
[0153] Perform the following performance tests on the single-component addition-curing silicone sealants of the above examples and comparative examples respectively:
[0154] 1. Tensile shear strength: It is measured according to "GB / T 7124-2008 Determination of Tensile Shear Strength of Adhesives (Rigid Material to Rigid Material)";
[0155] 2. Compression adhesion: Perform high-temperature compression aging according to "GB / T 7759.1-2015 Determination of Compression Set of Vulcanized Rubber or Thermoplastic Rubber - Part 1: At Normal and High Temperatures", without applying a lubricant coating to the contact surface, the test conditions are 150 °C / 168 h, the compression amount is 25%, and determine the percentage of the residual glue area sticking to the contact surface after the specimen is damaged in the entire contact surface.
[0156] The test results are shown in the following table:
[0157]
[0158] As can be seen from the above table, the tensile shear strength of the one-component addition-curing silicone sealant prepared in Examples 1-5 all reached above 3.5 MPa, and no compression anti-sticking occurred; the difference between Comparative Example 1 and Example 5 was that no release regulator was used, resulting in compression anti-sticking in the one-component addition-curing silicone sealant prepared by it, and the anti-sticking area reached 32%; the difference between Comparative Example 2 and Example 5 was that fumed titanium dioxide was not used, resulting in compression anti-sticking in the one-component addition-curing silicone sealant prepared by it, and the anti-sticking area reached 21%; the difference between Comparative Example 3 and Example 5 was that a commercially available tackifier was used, and its tensile shear strength decreased to 2.6 MPa, and the anti-sticking area also reached 28%; the difference between Comparative Example 4 and Example 5 was that a commercially available tackifier was used, and fumed titanium dioxide and release regulator were not used, resulting in a significant decrease in the tensile shear strength of the one-component addition-curing silicone sealant prepared by it, and more serious compression anti-sticking, and the anti-sticking area reached 72%; the difference between Comparative Example 5 and Example 5 was that fumed titanium dioxide and release regulator were not used, resulting in relatively serious compression anti-sticking in the one-component addition-curing silicone sealant prepared by it, and the anti-sticking area reached 43%.
[0159] The technical features of the above-described embodiments can be combined arbitrarily. For the sake of brevity of description, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, it should be considered as the scope recorded in this specification.
[0160] The above-described embodiments only represent several implementation manners of the present invention, and the description is relatively specific and detailed, but it should not be construed as a limitation on the scope of the invention patent. It should be noted that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can still be made, and these all belong to the protection scope of the present invention. Therefore, the protection scope of the invention patent should be subject to the appended claims.
Claims
1. A tackifier, characterized in that, The tackifier is obtained by reacting tetramethylcyclotetrasiloxane, dimethylmethoxyvinylsilane and allyl glycidyl ether under the catalysis of a platinum catalyst.
2. The tackifier according to claim 1, wherein The platinum catalyst is one or a combination of chloroplatinic acid, chloroplatinic acid-isopropanol complex, and Karstedt's catalyst; and / or, The mass ratio of the tetramethylcyclotetrasiloxane, dimethylmethoxyvinylsilane and allyl glycidyl ether is 50:20-30:15-25; preferably 50:25:
20.
3. A method for preparing the tackifier according to any one of claims 1-2, characterized in that, It includes the following steps: Add an organic solvent, tetramethylcyclotetrasiloxane and a platinum catalyst to a reactor, and stir evenly; heat the obtained mixture to 60°C-80°C under the protection of an inert gas, and dropwise add the allyl glycidyl ether and dimethylmethoxyvinylsilane respectively, and react for 2h-3h; remove low boilers, organic solvents and platinum catalyst to obtain the tackifier.
4. The preparation method of the tackifier according to claim 3, wherein, The organic solvent is toluene; and / or, The addition amount of the organic solvent is 0.8-1.2 times the weight of the tetramethylcyclotetrasiloxane; Based on the mass of platinum, the addition amount of the platinum catalyst is 0.5ppm-5ppm.
5. A one-component addition-curing silicone sealant, characterized in that, The raw materials for its preparation include the tackifier described in any one of claims 1-2.
6. The one-component addition-curing silicone sealant according to claim 5, wherein The raw materials for its preparation include a platinum catalyst and the following components in parts by weight: The dosage of the platinum catalyst is 0.5ppm-10ppm based on the mass of platinum; The release regulator is a fluorosilane.
7. The one-component addition-curing silicone sealant according to claim 6, wherein, The raw materials for its preparation include a platinum catalyst and the following components in parts by weight:
8. The one-component addition-curing silicone sealant according to claim 6 or 7, characterized in that, In the one-component addition-curing silicone sealant, the dosage of the platinum catalyst is 3ppm-8ppm based on the mass of platinum; and / or, The viscosity of the terminal vinyl silicone oil at 25°C is 1000mPa·s-100000mPa·s; and / or, The specific surface area of the fumed silica is 100 m 2 / g to 400 m 2 / g; and / or, The hydrogen-containing crosslinking agent is side hydrogen-containing silicone oil and / or terminal-side hydrogen-containing silicone oil, its hydrogen content is 0.2wt%-2wt%, and the viscosity is 10mPa·s-200mPa·s; and / or, The release regulator is selected from one or a combination of dimethylmethoxy(3,3,3-fluoropropyl)silane, trifluoropropyl dimethyl ethoxysilane, trifluoropropyl methyl dimethoxysilane and trifluoropropyl methyl diethoxysilane; and / or, The inhibitor is selected from one or a combination of 1-ethynyl-1-cyclohexanol, tetramethyltetravinylcyclotetrasiloxane, 2-methyl-3-butyn-2-ol, 3-methyl-1-hexyn-3-ol, 3,5-dimethyl-1-hexyn-3-ol and 3-methyl-1-dodecyn-3-ol; and / or, The specific surface area of the fumed titanium dioxide is 30 m 2 / g to 100 m 2 / g; and / or, The platinum catalyst is selected from one or a combination of chloroplatinic acid, chloroplatinic acid-isopropanol complex, and Karstedt's catalyst.
9. The one-component addition-curing silicone sealant according to claim 8, wherein The viscosity of the terminal vinyl silicone oil at 25°C is 5000mPa·s-20000mPa·s; and / or, The specific surface area of the fumed silica is 150 m 2 / g to 250 m 2 / g; and / or, The hydrogen content of the hydrogen-containing crosslinking agent is 0.5wt%-1.2wt%, and the viscosity is 20mPa·s-120mPa·s; and / or, The specific surface area of the aerosil titanium dioxide is 40 m 2 / g to 60 m 2 / g.
10. A method for preparing a one-component addition-curing silicone sealant according to any one of claims 6-9, characterized in that, It includes the following steps: (1) Put the terminal vinyl silicone oil into a kneader, then add fumed silica in batches, knead for 1 h to 2 h, then heat up to 120 °C to 150 °C and evacuate, and knead for 2 h to 4 h to obtain the base material; (2) Put the base material, hydrogen-containing crosslinking agent and fumed titanium dioxide into a planetary mixer, and stir for 30 min to 60 min after adding until evenly mixed; (3) Put the tackifier, inhibitor and release regulator into a planetary mixer, and stir for 30 min - 60 min until evenly mixed; (4) Put the platinum catalyst into a planetary mixer, stir and evacuate to mix for 20 min to 40 min to obtain the one-component addition-curing silicone sealant.