A silicone rubber adhesive and its preparation method
By preparing a tackifier with a specific structure, the problem of slow construction speed of existing silicone rubber adhesives has been solved, achieving a rapid construction effect.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- DONGGUAN SILICON ART NEW MATERIALS CO LTD
- Filing Date
- 2024-10-21
- Publication Date
- 2026-05-26
AI Technical Summary
Existing silicone rubber adhesives have a slow application speed in certain specific scenarios, which cannot meet the needs of rapid construction.
Tackifiers with specific structures are prepared through amino-epoxy ring-opening addition reaction and hydroxyl-titanium ester transesterification reaction. The tackifiers include compounds 001, 002, and 003, which are used to mix with hydroxyl-terminated polydimethylsiloxane, nano-calcium carbonate, and other components to form silicone rubber adhesives.
It significantly improves the application speed of silicone rubber adhesives, meeting the needs of rapid construction.
Smart Images

Figure QLYQS_1 
Figure BDA0005094436120000021 
Figure BDA0005094436120000022
Abstract
Description
Technical Field
[0001] This invention relates to the field of silicone rubber adhesives, and more particularly to a silicone rubber adhesive and its preparation method. Background Technology
[0002] Silicone rubber adhesives are a type of specialty adhesive composed of high-molecular-weight linear polysiloxanes mixed with fillers and other additives. They are simple to handle, easy to use, and exhibit high bonding strength. Due to their excellent properties such as high-temperature resistance, low-temperature resistance, insulation, water resistance, and weather resistance, silicone rubber adhesives are widely used in aircraft manufacturing, electrical and electronic component manufacturing, construction, and medical and health fields.
[0003] Existing silicone rubber adhesives typically use γ-aminopropyltriethoxysilane (industrial grade KH550) and γ-glycidoxypropyltrimethoxysilane (industrial grade KH560) as tackifiers, which are not suitable for engineering applications with short cycles and cannot meet the usage requirements of certain specific scenarios. Summary of the Invention
[0004] To address the above problems, this invention provides a silicone rubber adhesive and its preparation method.
[0005] In a first aspect, the present invention provides a silicone rubber adhesive, which, by weight parts, comprises the following components:
[0006] Hydroxyl-terminated polydimethylsiloxane and nano-calcium carbonate, totaling 100 parts, with nano-calcium carbonate comprising 40 to 60 parts;
[0007] Methyltrimethoxysilane, 2 to 3 parts;
[0008] Diisopropyl bis(ethyl acetoacetate) titanate, 1 to 2 parts;
[0009] Tackifier, 0.3 to 0.7 parts;
[0010] The tackifier includes compounds with a general structural formula as shown in Formula I or Formula II;
[0011] Equation I and Equation II:
[0012]
[0013] In equations I and II: R 1 It is hydrogen, methyl, ethyl, propyl, n-butyl, cyclohexyl, or phenyl; R 2 It is methyl, ethyl, propyl, cyclohexyl, phenyl, a group represented by Formula III or a group represented by Formula IV; R 3 It is methyl, ethyl, n-propyl, isopropyl, butyl, or isobutyl; R 4 It is methyl or ethyl;
[0014] Formulas III and IV:
[0015]
[0016] In formulas III and IV: R 5 It can be methyl or ethyl.
[0017] Further, by weight, the silicone rubber adhesive comprises the following components:
[0018] Hydroxyl-terminated polydimethylsiloxane, 50 parts;
[0019] Nano-calcium carbonate, 50 parts;
[0020] Methyltrimethoxysilane, 2.5 parts;
[0021] Diisopropyl bis(ethyl acetoacetate) titanate, 1.5 parts;
[0022] Tackifier, 0.5 parts.
[0023] Furthermore, the R 3 It is isopropyl, butyl, or isobutyl; the R 1 It is n-butyl or phenyl; the R 2 It is the group shown in Formula III.
[0024] Furthermore, the R 3 It is isopropyl; the R 4 The R is methyl; 1 It is n-butyl; the R 5 It is a methyl group.
[0025] Further, the tackifier is compound 001, compound 002, compound 003, compound 004, compound 005, compound 006, compound 007, compound 008, compound 009, compound 011 or compound 013;
[0026] The chemical structural formulas of compounds 001, 002, 003, 004, 005, 006, 007, 008, 009, 011, and 013 are shown below:
[0027]
[0028] Furthermore, the method for preparing the thickener includes the following steps:
[0029] A mixture is obtained by mixing the titanate compound shown in Formula VI with the epoxy propylene oxide compound shown in Formula VII or Formula VIII;
[0030] An amine compound of formula V is added dropwise to the mixture, and the reaction is carried out after the addition is complete so that R is no longer distilled off. 3 The -OH compound is the endpoint of the reaction;
[0031] Formulas V, VI, VII, and VIII:
[0032]
[0033] In equation V: R 1 It is hydrogen, methyl, ethyl, propyl, n-butyl, cyclohexyl, or phenyl; R 2 It can be methyl, ethyl, propyl, cyclohexyl, phenyl, or a group represented by formula III or formula IV;
[0034] In equation VI: R 3 It can be methyl, ethyl, n-propyl, isopropyl, butyl, or isobutyl;
[0035] In equations VII and VIII: R 4 It can be methyl or ethyl.
[0036] Furthermore, the molar ratio of the amine compound represented by Formula V, the titanate compound represented by Formula VI, and the epoxypropoxy compound represented by Formula VII or Formula VIII is 1:(1-4):1.
[0037] Furthermore, the molar ratio of the amine compound represented by Formula V, the titanate compound represented by Formula VI, and the epoxypropoxy compound represented by Formula VII or Formula VIII is 1:1:1.
[0038] Furthermore, the operating conditions for the dripping process include: a dripping temperature of 80-100℃ and a dripping time of ≤2 hours.
[0039] Furthermore, the reaction temperature is 90-110℃ after the addition is complete.
[0040] In a second aspect, the present invention provides a method for preparing the silicone rubber adhesive according to any one of the first aspects, the preparation method comprising the following steps:
[0041] The thickener is obtained;
[0042] The tackifier and the remaining components of the silicone rubber adhesive are mixed to obtain the silicone rubber adhesive.
[0043] The technical solution provided by this invention has at least the following advantages compared with the prior art:
[0044] This invention provides a silicone rubber adhesive. Compared with existing silicone rubber adhesives, the silicone rubber adhesive provided by this invention contains a tackifier with a specific structure, which can significantly improve the construction speed, meet the needs of rapid construction, and make up for the shortcomings of existing silicone rubber adhesives. Detailed Implementation
[0045] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions of this invention will be clearly and completely described below in conjunction with this invention. Obviously, the described embodiments are only some embodiments of this invention, not all embodiments. Based on the embodiments of this invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this invention.
[0046] Unless otherwise specified, all raw materials, reagents, instruments and equipment used in this invention can be purchased from the market or prepared by existing methods.
[0047] In a first aspect, the present invention provides a silicone rubber adhesive, which, by weight parts, comprises the following components:
[0048] Hydroxyl-terminated polydimethylsiloxane and nano-calcium carbonate, totaling 100 parts, with nano-calcium carbonate comprising 40 to 60 parts;
[0049] Methyltrimethoxysilane, 2 to 3 parts;
[0050] Diisopropyl bis(ethyl acetoacetate) titanate, 1 to 2 parts;
[0051] Tackifier, 0.3 to 0.7 parts;
[0052] The tackifier includes compounds with a general structural formula as shown in Formula I or Formula II;
[0053] Equation I and Equation II:
[0054]
[0055] In equations I and II: R 1 It is hydrogen, methyl, ethyl, propyl, n-butyl, cyclohexyl, or phenyl; R 2 It is methyl, ethyl, propyl, cyclohexyl, phenyl, a group represented by Formula III or a group represented by Formula IV; R 3 It is methyl, ethyl, n-propyl, isopropyl, butyl, or isobutyl; R 4 It is methyl or ethyl;
[0056] Formulas III and IV:
[0057]
[0058] In formulas III and IV: R 5 It can be methyl or ethyl.
[0059] This invention provides a silicone rubber adhesive. Compared with existing silicone rubber adhesives, the silicone rubber adhesive provided by this invention contains a tackifier with a specific structure, which can significantly improve the construction speed, meet the needs of rapid construction, and make up for the shortcomings of existing silicone rubber adhesives.
[0060] In some specific embodiments, the silicone rubber adhesive comprises the following components, by weight:
[0061] Hydroxyl-terminated polydimethylsiloxane, 50 parts;
[0062] Nano-calcium carbonate, 50 parts;
[0063] Methyltrimethoxysilane, 2.5 parts;
[0064] Diisopropyl bis(ethyl acetoacetate) titanate, 1.5 parts;
[0065] Tackifier, 0.5 parts.
[0066] In some specific embodiments, the R 3 It is isopropyl, butyl, or isobutyl; the R 1 It is n-butyl or phenyl; the R 2 It is the group shown in Formula III.
[0067] In some specific embodiments, the R 3 It is isopropyl; the R 4 The R is methyl; 1 It is n-butyl; the R 5 It is a methyl group.
[0068] In some specific embodiments, the tackifier is compound 001, compound 002, compound 003, compound 004, compound 005, compound 006, compound 007, compound 008, compound 009, compound 011 or compound 013;
[0069] The chemical structural formulas of compounds 001, 002, 003, 004, 005, 006, 007, 008, 009, 011, and 013 are shown below:
[0070]
[0071] In some specific embodiments, the method for preparing the tackifier includes the following steps:
[0072] A mixture is obtained by mixing the titanate compound shown in Formula VI with the epoxy propylene oxide compound shown in Formula VII or Formula VIII;
[0073] An amine compound of formula V is added dropwise to the mixture, and the reaction is carried out after the addition is complete so that R is no longer distilled off. 3 The -OH compound is the endpoint of the reaction;
[0074] Formulas V, VI, VII, and VIII:
[0075]
[0076] In equation V: R 1 It is hydrogen, methyl, ethyl, propyl, n-butyl, cyclohexyl, or phenyl; R 2 It can be methyl, ethyl, propyl, cyclohexyl, phenyl, or a group represented by formula III or formula IV;
[0077] In equation VI: R 3 It can be methyl, ethyl, n-propyl, isopropyl, butyl, or isobutyl;
[0078] In equations VII and VIII: R 4 It can be methyl or ethyl.
[0079] The method for preparing the tackifier provided by this invention involves a ring-opening addition reaction (referred to as amino-epoxy ring-opening addition reaction) between the amino group in an amine compound of formula V and the epoxy group in an epoxypropoxy compound of formula VII or VIII to obtain a hydroxyl-containing intermediate. This hydroxyl-containing intermediate is further subjected to a transesterification reaction (referred to as hydroxyl-titanium ester transesterification reaction) with a titanate compound of formula VI. After the reaction, no additional separation or purification steps are required, and the resulting reaction mixture is the target product – the tackifier. The entire reaction process is simple to operate, requires no additional specific equipment, and is suitable for industrial-scale mass production.
[0080] In some specific embodiments, the molar ratio of the amine compound represented by Formula V, the titanate compound represented by Formula VI, and the epoxypropoxy compound represented by Formula VII or Formula VIII is 1:(1-4):1.
[0081] In some specific embodiments, the molar ratio of the amine compound represented by Formula V, the titanate compound represented by Formula VI, and the epoxypropoxy compound represented by Formula VII or Formula VIII is 1:1:1.
[0082] In some specific embodiments, the operating conditions for the dripping include: a dripping temperature of 80-100℃ and a dripping time of ≤2 hours.
[0083] In some specific embodiments, the reaction temperature is 90-110°C after the addition is completed.
[0084] In some specific embodiments, taking N-[3-(trimethoxysilyl)propyl]n-butylamine, tetraisopropyl titanate, and 3-[(2,3)-epoxypropoxy]propyltrimethoxysilane as reactants, the preparation method of the above-mentioned thickener includes the following process:
[0085] Prepare N-[3-(trimethoxysilyl)propyl]n-butylamine, tetraisopropyl titanate and 3-[(2,3)-epoxypropoxy]propyltrimethoxysilane, with a molar ratio of 1:1:1;
[0086] Mix 3-[(2,3)-epoxypropoxy]propyltrimethoxysilane and tetraisopropyl titanate, and control the temperature of the mixture at 90℃;
[0087] N-[3-(trimethoxysilyl)propyl]n-butylamine was added dropwise to the mixture over 2 hours at a temperature of 80-100°C; and
[0088] Continue the reaction at a temperature of 90-110℃ for an appropriate time until isopropanol no longer distills off.
[0089] Secondly, based on the same inventive concept, the present invention provides a method for preparing the silicone rubber adhesive according to any one of the first aspects, the preparation method comprising the following steps:
[0090] The thickener is obtained;
[0091] The tackifier and the remaining components of the silicone rubber adhesive are mixed to obtain the silicone rubber adhesive.
[0092] It should be noted that, unless otherwise specified or indicated, the raw materials involved in the silicone rubber adhesive and its preparation method provided by this invention can be directly selected from commercially available products; at the same time, unless otherwise specified or indicated, the operation steps involved can be carried out according to the ring-opening addition reaction conditions of amino-epoxy groups and the transesterification reaction conditions of hydroxyl-titanium ester compounds disclosed in the existing preparation processes in the art, or using existing equipment, and will not be described in detail here.
[0093] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Experimental methods in the following embodiments, unless otherwise specified, are generally performed according to national standards. If no corresponding national standard exists, then generally accepted international standards, conventional conditions, or conditions recommended by the manufacturer are followed.
[0094] In the following examples: Unless otherwise specified, the materials and reagents are of analytical grade; the necessary raw material purification, reaction vessel selection, stirring and homogenization, temperature control, waterproofing, oxygen isolation, ventilation, distillation and silica gel column separation and other routine operations are not described in detail; the reaction temperature is selected as needed within the range of room temperature to 150°C.
[0095] Example 1
[0096] One embodiment of this application discloses a tackifying compound - compound 001.
[0097] The preparation method of tackifying compound 001 and tackifier M01 includes the following steps:
[0098] S10. Weigh: 1 mol of N-(n-butyl)-γ-aminopropyltrimethoxysilane {also known as N-[3-(trimethoxysilyl)propyl]n-butylamine, conforming to the general formula V}, 1 mol of 3-[(2,3)-epoxypropoxy]propyltrimethoxysilane (conforming to the general formula VII), and 1 mol of tetraisopropyl titanate (conforming to the general formula VI);
[0099] S11. Prepare a 1000ml four-necked flask as a reaction vessel. Attach a 250ml constant pressure dropping funnel, a condenser, and a thermometer to the four-necked flask. Connect the condenser to the receiving bottle.
[0100] S20. Mix the titanate of general formula VI and the silane of general formula VII, and control the temperature of the mixture to 90°C;
[0101] S30, at a temperature of 90°C, adds the amine of general formula V to the mixture dropwise using a 250ml constant pressure dropping funnel over 2 hours;
[0102] S40. Continue the reaction at a temperature of 90-110℃ for an appropriate time, until the reaction system no longer distills out isopropanol;
[0103] S50. Accept the liquid in the bottle and weigh it to be 57g;
[0104] S60. The mixture obtained after the reaction is the thickener M01, which is separated by silica gel column chromatography to obtain the thickening compound 001.
[0105] In this example, the distillate from the receiving flask had a distinctly pungent odor and was identified as isopropanol by gas chromatography and infrared absorption spectroscopy. The thickening compound, compound 001, conformed to general formula I, R... 3 It is isopropyl, R 4 It is methyl, R 1 It is n-butyl, R 2 Conforms to the general formula III shown, R 5 It is a methyl group.
[0106] This example also applies the aforementioned tackifier M01 to the preparation of silicone rubber adhesives, specifically a silicone rubber adhesive A01 containing tackifier M01:
[0107] Silicone rubber adhesive A01, with silicone rubber as the base and tackifier M01 as the tackifying component, comprises the following components in parts by weight:
[0108] Hydroxyl-terminated polydimethylsiloxane, 50 parts, commonly known as 107 glue, viscosity 18,000 to 22,000 cSt;
[0109] Nano calcium carbonate, 50 parts, purchased from Shanxi Ruicheng Xintai Nanomaterials Co., Ltd., model NPCC-201, average particle size 50nm;
[0110] Methyltrimethoxysilane, 2.5 parts, chemically pure, purchased from Guangzhou Shanghe Chemical Technology Co., Ltd.;
[0111] Diisopropyl bis(ethyl acetoacetate) titanate, 1.5 parts, chemically pure, purchased from Guangdong Wengjiang Chemical Reagent Co., Ltd.
[0112] Tackifier M01, 0.5 parts.
[0113] The preparation process of silicone rubber adhesive A01 is mainly as follows: add nano calcium carbonate filler to 107 glue and homogenize for 40 min; add methyltrimethoxysilane and diisopropyl bis(ethyl acetoacetate) titanate in sequence and mix for 15 min; add tackifier M01 and mix for 6 min; seal the product in a dispensing tube.
[0114] Example 2
[0115] Another embodiment of this application discloses a tackifying compound - compound 003.
[0116] The preparation method of thickening compound 003 is basically the same as that of thickening compound 001, but there are the following differences:
[0117] The reaction raw materials are: 1 mol diphenylamine, 1.5 mol 3-[(2,3)-epoxypropoxy]propyltriethoxysilane, and 1 mol tetraisopropyl titanate;
[0118] This is designated as tackifier M03;
[0119] The tackifying compound, compound 003, was identified by molecular structure and conforms to general formula I.
[0120] This embodiment also discloses a silicone rubber adhesive A03 containing tackifier M03.
[0121] Silicone rubber adhesive A03 has the same composition and preparation method as silicone rubber adhesive A01, but 0.7 parts of tackifier M03 are used instead of tackifier M01.
[0122] Example 3
[0123] Another embodiment of this application discloses a tackifying compound - compound 005.
[0124] The preparation method of thickening compound 005 is basically the same as that of thickening compound 001, but there are the following differences:
[0125] The reaction raw materials are: 1 mol dimethylamine, 2.5 mol 3-[(2,3)-epoxypropoxy]propyltriethoxysilane, and 1 mol tetraisopropyl titanate;
[0126] This is designated as tackifier M05;
[0127] The tackifying compound, compound 005, was identified by molecular structure and conforms to general formula I.
[0128] This embodiment also discloses a silicone rubber adhesive A05 containing tackifier M05.
[0129] Silicone rubber adhesive A05 has the same composition and preparation method as silicone rubber adhesive A01, but 0.4 parts of tackifier M05 are used instead of tackifier M01.
[0130] Example 4
[0131] Another embodiment of this application discloses a thickening compound - compound 007.
[0132] The preparation method of thickening compound 007 is basically the same as that of thickening compound 001, but there are the following differences:
[0133] The reaction raw materials are: 1 mol methyl ethylamine, 3 mol 3-[(2,3)-epoxypropoxy]propyltriethoxysilane, and 1 mol tetrabutyl titanate;
[0134] Designated as tackifier M07;
[0135] The tackifying compound, compound 007, was identified by molecular structure and conforms to general formula I.
[0136] This embodiment also discloses a silicone rubber adhesive A07 containing tackifier M07.
[0137] Silicone rubber adhesive A07 has the same composition and preparation method as silicone rubber adhesive A01, but 0.5 parts of tackifier M07 replace tackifier M01.
[0138] Example 5
[0139] Another embodiment of this application discloses a tackifying compound - compound 009.
[0140] The preparation method of thickening compound 009 is basically the same as that of thickening compound 001, but there are the following differences:
[0141] The reaction raw materials are: 1 mol of γ-aminopropyltrimethoxysilane, 1 mol of 3-[(2,3)-epoxypropoxy]propyltrimethoxysilane, and 1 mol of tetraisopropyl titanate.
[0142] This is designated as tackifier M09;
[0143] The tackifying compound, compound 009, was identified by molecular structure and conforms to general formula I.
[0144] This embodiment also discloses a silicone rubber adhesive A09 containing tackifier M09.
[0145] Silicone rubber adhesive A09 has the same composition and preparation method as silicone rubber adhesive A01, but 0.3 parts of tackifier M09 are used instead of tackifier M01.
[0146] Example 6
[0147] Another embodiment of this application discloses a tackifying compound - compound 011.
[0148] The preparation method of thickening compound 011 is basically the same as that of thickening compound 001, but there are the following differences:
[0149] The reaction raw materials are: 1 mol of N-(phenyl)-γ-aminopropyltrimethoxysilane, 4 mol of 3-[(2,3)-epoxypropoxy]propyltrimethoxysilane, and 1 mol of tetraisopropyl titanate.
[0150] This is designated as tackifier M11;
[0151] The tackifying compound, compound 011, was identified by molecular structure and conforms to general formula I.
[0152] This embodiment also discloses a silicone rubber adhesive A11 containing tackifier M11.
[0153] Silicone rubber adhesive A11 has the same composition and preparation method as silicone rubber adhesive A01, but 0.4 parts of tackifier M11 replace tackifier M01.
[0154] Example 7
[0155] Another embodiment of this application discloses a thickening compound - compound 013.
[0156] The preparation method of thickening compound 013 is basically the same as that of thickening compound 001, but there are the following differences:
[0157] The reaction raw materials are: 1 mol of N-(n-butyl)-γ-aminopropyldimethoxymethylsilane, 2 mol of 3-[(2,3)-epoxypropoxy]propyltriethoxysilane, and 1 mol of tetraisopropyl titanate.
[0158] This is designated as tackifier M11;
[0159] The tackifying compound, compound 003, was identified by molecular structure and conforms to general formula I.
[0160] This embodiment also discloses a silicone rubber adhesive A03 containing tackifier M03.
[0161] Silicone rubber adhesive A03 has the same composition and preparation method as silicone rubber adhesive A01, but 0.7 parts of tackifier M03 are used instead of tackifier M01.
[0162] Example 8
[0163] Another embodiment of this application discloses a tackifying compound - compound 002.
[0164] The preparation method of thickening compound 003 is basically the same as that of thickening compound 001, but there are the following differences:
[0165] The reaction raw materials are: 1 mol of N-(n-butyl)-γ-aminopropyltrimethoxysilane, 2 mol of 3-[(2,3)-epoxypropoxy]propyldimethoxymethylsilane, and 1 mol of tetraisopropyl titanate;
[0166] This is designated as tackifier M02;
[0167] The tackifying compound, compound 000, was identified by molecular structure and conforms to general formula II.
[0168] This embodiment also discloses a silicone rubber adhesive A02 containing tackifier M00.
[0169] Silicone rubber adhesive A02 has the same composition and preparation method as silicone rubber adhesive A01, but 0.5 parts of tackifier M00 are used instead of tackifier M01.
[0170] Example 9
[0171] Another embodiment of this application discloses a tackifying compound - compound 004.
[0172] The preparation method of thickening compound 003 is basically the same as that of thickening compound 001, but there are the following differences:
[0173] The reaction raw materials are: 1 mol of dicyclohexylamine, 3 mol of 3-[(2,3)-epoxypropoxy]propyldiethoxymethylsilane, and 1 mol of tetraisopropyl titanate;
[0174] This is designated as tackifier M04;
[0175] The tackifying compound, compound 004, was identified by molecular structure and conforms to general formula II.
[0176] This embodiment also discloses a silicone rubber adhesive A04 containing tackifier M04.
[0177] Silicone rubber adhesive A04 has the same composition and preparation method as silicone rubber adhesive A01, but 0.7 parts of tackifier M04 are used instead of tackifier M01.
[0178] Example 10
[0179] Another embodiment of this application discloses a thickening compound - compound 006.
[0180] The preparation method of thickening compound 006 is basically the same as that of thickening compound 001, but there are the following differences:
[0181] The reaction raw materials are: 1 mol of N-(methyl)-aniline, 1 mol of 3-[(2,3)-epoxypropoxy]propyl dimethoxymethylsilane, and 1 mol of tetramethyl titanate;
[0182] This is designated as tackifier M06;
[0183] The tackifying compound, compound 006, was identified by molecular structure and conforms to general formula II.
[0184] This embodiment also discloses a silicone rubber adhesive A06 containing tackifier M06.
[0185] Silicone rubber adhesive A06 has the same composition and preparation method as silicone rubber adhesive A01, but 0.6 parts of tackifier M06 replace tackifier M01.
[0186] Example 11
[0187] Another embodiment of this application discloses a tackifying compound - compound 008.
[0188] The preparation method of thickening compound 008 is basically the same as that of thickening compound 001, but there are the following differences:
[0189] The reaction raw materials are: 1 mol of N-(methyl)-γ-aminopropyltriethoxysilane, 1 mol of 3-[(2,3)-epoxypropoxy]propyldiethoxymethylsilane, and 1 mol of tetrabutyl titanate;
[0190] This is designated as tackifier M08;
[0191] The tackifying compound, compound 008, was identified by molecular structure and conforms to general formula II.
[0192] This embodiment also discloses a silicone rubber adhesive A08 containing tackifier M08.
[0193] Silicone rubber adhesive A08 has the same composition and preparation method as silicone rubber adhesive A01, but 0.5 parts of tackifier M08 are used instead of tackifier M01.
[0194] Comparative Example 1
[0195] The preparation method of the silicone rubber adhesive is basically the same as that of silicone rubber adhesive A01, but 0.5 parts of KH550 are used to replace the tackifier M01.
[0196] Comparative Example 2
[0197] The silicone rubber adhesive is prepared in a manner that is basically the same as that of silicone rubber adhesive A01, but with 0.25 parts of KH550 and 0.25 parts of KH560 replacing the tackifier M01.
[0198] Test case
[0199] The silicone rubber adhesives of Comparative Examples 1 and 2, as well as the aforementioned silicone rubber adhesives A01, A03, A05, A07, A09, A11, A13, A02, A04, A06, and A08, were tested for surface drying time and detack time under the conditions of 23±2℃ and RH50±5% in accordance with GB / T13477.17-2017, and the curing state was evaluated.
[0200] The results are shown in Tables 1 and 2 below.
[0201] Table 1
[0202]
[0203]
[0204] Table 2
[0205]
[0206] As shown in Tables 1 and 2, the test results of silicone rubber adhesives A01, A03, A05, A07, A09, A11, A13, A02, A04, A06 and A08 are all better than those of the two comparative examples.
[0207] The above description is merely a specific embodiment of the present invention, enabling those skilled in the art to understand or implement the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Therefore, the present invention is not to be limited to the embodiments shown herein, but is to be accorded the widest scope consistent with the principles and novel features claimed herein.
Claims
1. A silicone rubber adhesive, characterized in that, The silicone rubber adhesive comprises the following components in parts by weight: Hydroxyl-terminated polydimethylsiloxane and nano-calcium carbonate, totaling 100 parts, with nano-calcium carbonate comprising 40 to 60 parts; Methyltrimethoxysilane, 2 to 3 parts; Diisopropyl bis(ethyl acetoacetate) titanate, 1 to 2 parts; Tackifier, 0.3 to 0.7 parts; The preparation method of the thickener includes the following steps: A mixture is obtained by mixing the titanate compound shown in Formula VI with the epoxy propylene oxide compound shown in Formula VII or Formula VIII; Add the amine compound of formula V dropwise to the mixture, and after the addition is complete, carry out the reaction until no more R3-OH compound is distilled off; Formulas V, VI, VII, and VIII: ; In Formula V: R1 is hydrogen, methyl, ethyl, propyl, n-butyl, cyclohexyl, or phenyl; R2 is methyl, ethyl, propyl, cyclohexyl, phenyl, the group shown in Formula III, or the group shown in Formula IV; In formula VI: R3 is methyl, ethyl, n-propyl, isopropyl, butyl, or isobutyl; In formulas VII and VIII: R4 is methyl or ethyl; The molar ratio of the amine compound represented by Formula V, the titanate compound represented by Formula VI, and the epoxypropoxy compound represented by Formula VII or Formula VIII is 1:(1~4):
1.
2. The silicone rubber adhesive according to claim 1, characterized in that, The silicone rubber adhesive comprises the following components in parts by weight: Hydroxyl-terminated polydimethylsiloxane, 50 parts; Nano-calcium carbonate, 50 parts; Methyltrimethoxysilane, 2.5 parts; Diisopropyl bis(ethyl acetoacetate) titanate, 1.5 parts; Tackifier, 0.5 parts.
3. The silicone rubber adhesive according to claim 1, characterized in that, The operating conditions for the dripping process include: dripping temperature of 80-100℃ and dripping time of ≤2 hours.
4. The silicone rubber adhesive according to claim 1, characterized in that, The reaction temperature is 90-110℃ after the addition is complete.
5. A method for preparing the silicone rubber adhesive according to any one of claims 1 to 4, characterized in that, The preparation method includes the following steps: The thickener is obtained; The tackifier and the remaining components of the silicone rubber adhesive are mixed to obtain the silicone rubber adhesive.