Silicone rubber adhesive and preparation method thereof

Abstract

The invention relates to a silicone rubber adhesive and a preparation method thereof, and relates to the technical field of silicone rubber adhesives, the silicone rubber adhesive comprises the following components: 100 parts of hydroxyl-terminated polydimethylsiloxane and nano calcium carbonate, and 40-60 parts of nano calcium carbonate; 2 to 3 parts of methyl trimethoxy silane; 1 to 2 parts of bis (ethyl acetoacetate) diisopropyl titanate; 0.3 to 0.7 part of a tackifier; the tackifier comprises a compound with a structural general formula as shown in a formula I or a formula II. Compared with the existing silicone rubber adhesive, the silicone rubber adhesive provided by the invention contains the tackifier with a specific structure, so that the construction speed can be remarkably increased, the use requirement of rapid construction is met, and the defects of the existing silicone rubber adhesive are overcome.

Description

Technical Field

[0001] The present invention relates to the technical field of silicone rubber adhesives, and in particular to a silicone rubber adhesive and a preparation method thereof. Background Art

[0002] Silicone rubber adhesive is a special adhesive made of high molecular weight linear polysiloxane mixed with fillers and other additives. It is easy to operate, convenient to use, and has high bonding strength. Because silicone rubber adhesive has excellent properties such as high temperature resistance, low temperature resistance, insulation, waterproof, and weather resistance, it is widely used in aircraft manufacturing, electrical and electronic component manufacturing, construction, medical and health care, etc.

[0003] Existing silicone rubber adhesives usually use γ-aminopropyltriethoxysilane (industrial grade KH550) and γ-glycidyloxypropyltrimethoxysilane (industrial grade KH560) as tackifiers, which are not suitable for engineering applications with a short cycle and cannot meet the usage requirements of certain specific scenarios. Summary of the invention

[0004] In order to solve the above problems, the present invention provides a silicone rubber adhesive and a preparation method thereof.

[0005] In a first aspect, the present invention provides a silicone rubber adhesive, which comprises the following components in parts by weight:

[0006] Hydroxyl-terminated polydimethylsiloxane and nano calcium carbonate, 100 parts in total, with 40 to 60 parts of nano calcium carbonate;

[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 a compound with a general structural formula as shown in Formula I or Formula II;

[0011] The formula I and the formula II:

[0012]

[0013] In the formula I and the formula II: R 1 is hydrogen, methyl, ethyl, propyl, n-butyl, cyclohexyl or phenyl; R 2 is methyl, ethyl, propyl, cyclohexyl, phenyl, a group represented by formula III or a group represented by formula IV; R 3 is methyl, ethyl, n-propyl, isopropyl, butyl or isobutyl; R 4 is methyl or ethyl;

[0014] The formula III and the formula IV:

[0015]

[0016] In the formula III and the formula IV: R 5 It is methyl or ethyl.

[0017] Furthermore, the silicone rubber adhesive comprises the following components in parts by weight:

[0018] Hydroxy-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] Thickener, 0.5 parts.

[0023] Furthermore, the R 3 isopropyl, butyl or isobutyl; said R 1 is n-butyl or phenyl; said R 2 It is a group represented by formula III.

[0024] Furthermore, the R 3 isopropyl; said R 4 is methyl; said R 1 is n-butyl; said R 5 It is methyl.

[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 the compound 001, the compound 002, the compound 003, the compound 004, the compound 005, the compound 006, the compound 007, the compound 008, the compound 009, the compound 011 and the compound 013 are as follows:

[0027]

[0028] Furthermore, the preparation method of the tackifier comprises the following steps:

[0029] Mixing a titanate compound represented by formula VI and a glycidoxy compound represented by formula VII or formula VIII to obtain a mixture;

[0030] The amine compound represented by formula V is added dropwise to the mixture, and after the addition is completed, the reaction is carried out so that R is no longer distilled out. 3 -OH compound is the end point of the reaction;

[0031] The formula V, the formula VI, the formula VII and the formula VIII:

[0032]

[0033] In the formula V: R 1 is hydrogen, methyl, ethyl, propyl, n-butyl, cyclohexyl or phenyl; R 2 is methyl, ethyl, propyl, cyclohexyl, phenyl, a group represented by the formula III or a group represented by the formula IV;

[0034] In the formula VI: R 3 is methyl, ethyl, n-propyl, isopropyl, butyl or isobutyl;

[0035] In the formula VII and the formula VIII: R 4 It is 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 glycidoxy 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 glycidoxy compound represented by formula VII or formula VIII is 1:1:1.

[0038] Furthermore, the working condition parameters of the dropping include: the dropping temperature is 80-100° C., and the dropping time is ≤2 hours.

[0039] Furthermore, the temperature for the reaction after the dropwise addition is 90-110°C.

[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] Obtaining the tackifier;

[0042] The tackifier is mixed with the remaining components in the silicone rubber adhesive to obtain the silicone rubber adhesive.

[0043] The above technical solution provided by the present invention has at least the following advantages compared with the prior art:

[0044] The present invention provides a silicone rubber adhesive. Compared with the existing silicone rubber adhesive, the silicone rubber adhesive provided by the present invention contains a tackifier with a specific structure, which can significantly improve the construction speed, meet the use requirements of rapid construction, and make up for the shortcomings of the existing silicone rubber adhesive. DETAILED DESCRIPTION

[0045] In order to make the purpose, technical solution and advantages of the present invention clearer, the technical solution of the present invention will be clearly and completely described in combination with the present invention. Obviously, the described embodiments are 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.

[0046] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present 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 comprises the following components in parts by weight:

[0048] Hydroxyl-terminated polydimethylsiloxane and nano-calcium carbonate, 100 parts in total, with 40 to 60 parts of nano-calcium carbonate;

[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 a compound with a general structural formula as shown in Formula I or Formula II;

[0053] The formula I and the formula II:

[0054]

[0055] In the formula I and the formula II: R 1 is hydrogen, methyl, ethyl, propyl, n-butyl, cyclohexyl or phenyl; R 2 is methyl, ethyl, propyl, cyclohexyl, phenyl, a group represented by formula III or a group represented by formula IV; R 3 is methyl, ethyl, n-propyl, isopropyl, butyl or isobutyl; R 4 is methyl or ethyl;

[0056] The formula III and the formula IV:

[0057]

[0058] In the formula III and the formula IV: R 5 It is methyl or ethyl.

[0059] The present invention provides a silicone rubber adhesive. Compared with the existing silicone rubber adhesive, the silicone rubber adhesive provided by the present invention contains a tackifier with a specific structure, which can significantly improve the construction speed, meet the use requirements of rapid construction, and make up for the shortcomings of the existing silicone rubber adhesive.

[0060] In some specific embodiments, the silicone rubber adhesive comprises the following components in parts by weight:

[0061] Hydroxy-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] Thickener, 0.5 parts.

[0066] In some specific embodiments, the R 3 isopropyl, butyl or isobutyl; said R 1 is n-butyl or phenyl; said R 2 It is a group represented by formula III.

[0067] In some specific embodiments, the R 3 isopropyl; said R 4 is methyl; said R 1 is n-butyl; said R 5 It is methyl.

[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 the compound 001, the compound 002, the compound 003, the compound 004, the compound 005, the compound 006, the compound 007, the compound 008, the compound 009, the compound 011 and the compound 013 are as follows:

[0070]

[0071] In some specific embodiments, the preparation method of the tackifier comprises the following steps:

[0072] Mixing a titanate compound represented by formula VI and a glycidoxy compound represented by formula VII or formula VIII to obtain a mixture;

[0073] The amine compound represented by formula V is added dropwise to the mixture, and after the addition is completed, the reaction is carried out so that R is no longer distilled out. 3 -OH compound is the end point of the reaction;

[0074] The formula V, the formula VI, the formula VII and the formula VIII:

[0075]

[0076] In the formula V: R 1 is hydrogen, methyl, ethyl, propyl, n-butyl, cyclohexyl or phenyl; R 2 is methyl, ethyl, propyl, cyclohexyl, phenyl, a group represented by the formula III or a group represented by the formula IV;

[0077] In the formula VI: R 3 is methyl, ethyl, n-propyl, isopropyl, butyl or isobutyl;

[0078] In the formula VII and the formula VIII: R 4 It is methyl or ethyl.

[0079] The preparation method of the tackifier provided by the present invention is to carry out a ring-opening addition reaction (referred to as the amino-epoxy ring-opening addition reaction) of the amino group in the amine compound shown in formula V and the epoxy group in the glycidoxy compound shown in formula VII or formula VIII to obtain a hydroxyl-containing intermediate, and the hydroxyl-containing intermediate is further subjected to an ester exchange reaction (referred to as the hydroxyl-titanate compound ester exchange reaction) with the titanate compound shown in formula VI. After the reaction is completed, no additional separation and purification steps are required, and the obtained reaction system mixture is the target product-tackifier. The operation of the entire reaction process is simple, no additional specific equipment is required, and it is suitable for industrial 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 glycidoxy 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 glycidoxy compound represented by formula VII or formula VIII is 1:1:1.

[0082] In some specific embodiments, the working condition parameters of the dropwise addition include: the dropwise addition temperature is 80-100° C., and the dropwise addition time is ≤2 hours.

[0083] In some specific embodiments, the temperature for the reaction after the dropwise addition is 90-110°C.

[0084] In some specific embodiments, taking N-[3-(trimethoxysilyl)propyl]n-butylamine, tetraisopropyl titanate and 3-[(2,3)-epoxypropoxy]propyltrimethoxysilane as reaction raw materials as an example, the preparation method of the above-mentioned tackifier includes the following process:

[0085] Prepare N-[3-(trimethoxysilyl)propyl]n-butylamine, tetraisopropyl titanate and 3-[(2,3)-epoxypropyloxy]propyltrimethoxysilane in a molar ratio of 1:1:1;

[0086] Mix 3-[(2,3)-epoxypropoxy]propyltrimethoxysilane and tetraisopropyl titanate, and control the temperature of the mixture to 90° C.;

[0087] At a temperature of 80-100° C., N-[3-(trimethoxysilyl)propyl]-n-butylamine is added dropwise to the mixture within 2 hours; and

[0088] The reaction is continued at a temperature of 90-110°C for a suitable period of time until no more isopropanol is distilled off.

[0089] In a second aspect, 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] Obtaining the tackifier;

[0091] The tackifier is mixed with the remaining components in the silicone rubber adhesive to obtain the silicone rubber adhesive.

[0092] It should be noted that the raw materials involved in the silicone rubber adhesive and the preparation method thereof provided by the present invention, unless otherwise specified or explained, can be directly selected from commercially available products; at the same time, the operating steps involved, unless otherwise specified or explained, can be carried out according to the amino-epoxy ring-opening addition reaction condition parameters and the ester exchange reaction condition parameters of hydroxyl-titanate compounds disclosed in the existing preparation process in the art or using existing equipment, and will not be described one by one here.

[0093] The present invention will be further described below in conjunction with specific examples. It should be understood that these examples are intended only to illustrate the present invention and are not intended to limit the scope of the present invention. The experimental methods in the following examples that do not specify specific conditions are usually measured according to national standards. If there is no corresponding national standard, then the conditions recommended by the manufacturer are followed.

[0094] In the following embodiments: materials and reagents, unless otherwise specified, are of analytical grade; necessary raw material impurity removal and purification, reaction vessel selection, stirring and homogenization, temperature control, waterproofing, oxygen isolation, ventilation, distillation separation and silica gel column separation and other conventional operations are needless to be elaborated; the reaction temperature is selected as needed within the range of room temperature to 150°C.

[0095] Example 1

[0096] One embodiment of the present application discloses a viscosity-enhancing compound - Compound 001.

[0097] The preparation method of the tackifier compound-compound 001 and tackifier M01 comprises 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, add a 250ml constant pressure dropping funnel, a condenser and a thermometer to the four-necked flask, and connect the condenser to the receiving flask;

[0100] S20. Mixing the titanate of the general formula VI and the silane of the general formula VII, controlling the temperature of the mixture to 90 ° C;

[0101] S30 At a temperature of 90° C., within 2 hours, using a 250 ml constant pressure dropping funnel, the amine of the general formula V is added dropwise to the mixture;

[0102] S40. At a temperature of 90-110 ° C, the reaction is continued for an appropriate time until the reaction system no longer distills isopropanol;

[0103] S50. Receive the liquid in the bottle, weighing the mass to be 57g;

[0104] S60. After the reaction is completed, the mixture obtained is thickener M01, which is separated by a silica gel column to obtain thickening compound 001.

[0105] In this example, the distillate in the receiving bottle has a distinct characteristic irritating odor, which is identified as isopropanol by gas chromatography and infrared absorption spectroscopy. The viscosity-enhancing compound - Compound 001, according to molecular structure identification, conforms to the general formula I, R 3 is isopropyl, R 4 is methyl, R 1 is n-butyl, R 2 Conforms to the general formula III, R 5 It is methyl.

[0106] In this example, the above-mentioned tackifier M01 is also used to prepare a silicone rubber adhesive, specifically a silicone rubber adhesive A01 containing the tackifier M01:

[0107] Silicone rubber adhesive A01, with silicone rubber as the matrix and tackifier M01 as the tackifying component, includes the following components in parts by mass:

[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 Nanomaterial Co., Ltd., model NPCC-201, average particle size 50 nm;

[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] Thickener M01, 0.5 parts.

[0113] The preparation process of silicone rubber adhesive A01 is mainly as follows: adding nano calcium carbonate filler to 107 glue and homogenizing for 40 minutes; adding methyltrimethoxysilane and diisopropyl bis(ethyl acetoacetate) titanate in sequence and mixing for 15 minutes; adding tackifier M01 and mixing for 6 minutes; and sealing the product in a dispensing tube.

[0114] Example 2

[0115] Another embodiment of the present application discloses a viscosity-enhancing compound - Compound 003.

[0116] The preparation method of the viscosity-increasing compound-Compound 003 is basically the same as that of the viscosity-increasing compound-Compound 001, but there are the following differences:

[0117] The reaction raw materials are: 1 mol of diphenylamine, 1.5 mol of 3-[(2,3)-epoxypropoxy]propyltriethoxysilane, and 1 mol of tetraisopropyl titanate;

[0118] It is recorded as viscosity enhancer M03;

[0119] The viscosity-enhancing compound - Compound 003 was identified through molecular structure and was found to conform to Formula I.

[0120] This embodiment also discloses a silicone rubber adhesive A03 containing a tackifier M03.

[0121] The composition and preparation method of silicone rubber adhesive A03 are basically the same as those of silicone rubber adhesive A01, but 0.7 parts of tackifier M03 replaces tackifier M01.

[0122] Example 3

[0123] Another embodiment of the present application discloses a viscosity-enhancing compound - Compound 005.

[0124] The preparation method of the viscosity-increasing compound-Compound 005 is basically the same as that of the viscosity-increasing compound-Compound 001, but there are the following differences:

[0125] The reaction raw materials are: 1 mol of dimethylamine, 2.5 mol of 3-[(2,3)-epoxypropoxy]propyltriethoxysilane, and 1 mol of tetraisopropyl titanate;

[0126] It is recorded as viscosity enhancer M05;

[0127] The viscosity-enhancing compound, Compound 005, was identified through molecular structure and was found to conform to Formula I.

[0128] This embodiment also discloses a silicone rubber adhesive A05 containing a tackifier M05.

[0129] The composition and preparation method of silicone rubber adhesive A05 are basically the same as those of silicone rubber adhesive A01, but 0.4 parts of tackifier M05 replaces tackifier M01.

[0130] Example 4

[0131] Another embodiment of the present application discloses a viscosity-enhancing compound - Compound 007.

[0132] The preparation method of the viscosity-increasing compound-Compound 007 is basically the same as that of the viscosity-increasing compound-Compound 001, but there are the following differences:

[0133] The reaction raw materials are: 1 mol of methylethylamine, 3 mol of 3-[(2,3)-epoxypropoxy]propyltriethoxysilane, and 1 mol of tetrabutyl titanate;

[0134] It is recorded as viscosity enhancer M07;

[0135] The viscosity-enhancing compound, Compound 007, was identified through molecular structure and was found to conform to Formula I.

[0136] This embodiment also discloses a silicone rubber adhesive A07 containing a tackifier M07.

[0137] The composition and preparation method of silicone rubber adhesive A07 are basically the same as those of silicone rubber adhesive A01, but 0.5 parts of tackifier M07 replaces tackifier M01.

[0138] Example 5

[0139] Another embodiment of the present application discloses a viscosity-enhancing compound - Compound 009.

[0140] The preparation method of the viscosity-increasing compound-Compound 009 is basically the same as that of the viscosity-increasing compound-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] It is recorded as viscosity enhancer M09;

[0143] The viscosity-enhancing compound, Compound 009, was identified through molecular structure and was found to conform to Formula I.

[0144] This embodiment also discloses a silicone rubber adhesive A09 containing a tackifier M09.

[0145] The composition and preparation method of silicone rubber adhesive A09 are basically the same as those of silicone rubber adhesive A01, but 0.3 parts of tackifier M09 replaces tackifier M01.

[0146] Example 6

[0147] Another embodiment of the present application discloses a viscosity-enhancing compound - Compound 011.

[0148] The preparation method of the viscosity-increasing compound-Compound 011 is basically the same as that of the viscosity-increasing compound-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] It is recorded as tackifier M11;

[0151] The viscosity-enhancing compound - Compound 011 was identified through molecular structure and was found to conform to the general formula I.

[0152] This embodiment also discloses a silicone rubber adhesive A11 containing a tackifier M11.

[0153] The composition and preparation method of silicone rubber adhesive A11 are basically the same as those of silicone rubber adhesive A01, but 0.4 parts of tackifier M11 replaces tackifier M01.

[0154] Example 7

[0155] Another embodiment of the present application discloses a viscosity-increasing compound - Compound 013.

[0156] The preparation method of the viscosity-increasing compound-Compound 013 is basically the same as that of the viscosity-increasing compound-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)-epoxypropyloxy]propyltriethoxysilane, and 1 mol of tetraisopropyl titanate;

[0158] It is recorded as tackifier M11;

[0159] The viscosity-enhancing compound - Compound 003 was identified through molecular structure and was found to conform to Formula I.

[0160] This embodiment also discloses a silicone rubber adhesive A03 containing a tackifier M03.

[0161] The composition and preparation method of silicone rubber adhesive A03 are basically the same as those of silicone rubber adhesive A01, but 0.7 parts of tackifier M03 replaces tackifier M01.

[0162] Example 8

[0163] Another embodiment of the present application discloses a viscosity-enhancing compound - Compound 002.

[0164] The preparation method of the viscosity-increasing compound-Compound 003 is basically the same as that of the viscosity-increasing compound-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)-epoxypropyloxy]propyldimethoxymethylsilane, and 1 mol of tetraisopropyl titanate;

[0166] It is recorded as viscosity enhancer M02;

[0167] The viscosity-enhancing compound, compound 000, was identified through molecular structure and was found to conform to general formula II.

[0168] This embodiment also discloses a silicone rubber adhesive A02 containing a tackifier M00.

[0169] The composition and preparation method of silicone rubber adhesive A02 are basically the same as those of silicone rubber adhesive A01, but 0.5 parts of tackifier M00 replaces tackifier M01.

[0170] Example 9

[0171] Another embodiment of the present application discloses a viscosity-enhancing compound - Compound 004.

[0172] The preparation method of the viscosity-increasing compound-Compound 003 is basically the same as that of the viscosity-increasing compound-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] It is recorded as viscosity enhancer M04;

[0175] The molecular structure of the viscosity-enhancing compound, compound 004, was identified to be consistent with general formula II.

[0176] This embodiment also discloses a silicone rubber adhesive A04 containing a tackifier M04.

[0177] The composition and preparation method of silicone rubber adhesive A04 are basically the same as those of silicone rubber adhesive A01, but 0.7 parts of tackifier M04 replaces tackifier M01.

[0178] Example 10

[0179] Another embodiment of the present application discloses a viscosity-enhancing compound - Compound 006.

[0180] The preparation method of the viscosity-increasing compound-Compound 006 is basically the same as that of the viscosity-increasing compound-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]propyldimethoxymethylsilane, and 1 mol of tetramethyl titanate;

[0182] It is recorded as viscosity enhancer M06;

[0183] The viscosity-enhancing compound, Compound 006, was identified through molecular structure and was found to conform to Formula II.

[0184] This embodiment also discloses a silicone rubber adhesive A06 containing a tackifier M06.

[0185] The composition and preparation method of silicone rubber adhesive A06 are basically the same as those of silicone rubber adhesive A01, but 0.6 parts of tackifier M06 replaces tackifier M01.

[0186] Embodiment 11

[0187] Another embodiment of the present application discloses a viscosity-enhancing compound - Compound 008.

[0188] The preparation method of the viscosity-increasing compound-Compound 008 is basically the same as that of the viscosity-increasing compound-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)-epoxypropyloxy]propyldiethoxymethylsilane, and 1 mol of tetrabutyl titanate;

[0190] It is recorded as tackifier M08;

[0191] The viscosity-enhancing compound, Compound 008, was identified through molecular structure and was found to conform to Formula II.

[0192] This embodiment also discloses a silicone rubber adhesive A08 containing a tackifier M08.

[0193] The composition and preparation method of silicone rubber adhesive A08 are basically the same as those of silicone rubber adhesive A01, but 0.5 parts of tackifier M08 replaces tackifier M01.

[0194] Comparative Example 1

[0195] A silicone rubber adhesive was prepared, whose composition and preparation method were basically the same as those of silicone rubber adhesive A01, but 0.5 parts of KH550 was used to replace the tackifier M01.

[0196] Comparative Example 2

[0197] A silicone rubber adhesive was prepared, whose composition and preparation method were basically the same as those of silicone rubber adhesive A01, but 0.25 parts of KH550 and 0.25 parts of KH560 were used to replace the tackifier M01.

[0198] Test Case

[0199] The silicone rubber adhesives of Comparative Example 1 and Comparative Example 2, as well as the above-mentioned silicone rubber adhesives A01, A03, A05, A07, A09, A11, A13, A02, A04, A06 and A08, their unaged samples and aged samples were tested for surface drying time and tack-free time at 23±2°C and RH50±5% with reference to GB / T13477.17-2017 to evaluate the curing state.

[0200] The results are shown in Tables 1 and 2 below.

[0201] Table 1

[0202]

[0203]

[0204] Table 2

[0205]

[0206] It can be seen from Tables 1 and 2 that the test results of silicone rubber adhesives A01, A03, A05, A07, A09, A11, A13, A02, A04, A06 and A08 are better than those of the two comparative examples.

[0207] The foregoing is merely a specific embodiment of the present invention, which enables those skilled in the art to understand or implement the present invention. Various modifications to these embodiments will be 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 present invention. Therefore, the present invention will not be limited to the embodiments shown herein, but rather to 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, 100 parts in total, with 40 to 60 parts of nano-calcium carbonate; Methyltrimethoxysilane, 2 to 3 parts; Diisopropyl bis(ethyl acetoacetate) titanate, 1 to 2 parts; Tackifier, 0.3 to 0.7 parts; The tackifier includes a compound with a general structural formula as shown in Formula I or Formula II; The formula I and the formula II: In the formula I and the formula II: R 1 is hydrogen, methyl, ethyl, propyl, n-butyl, cyclohexyl or phenyl; R 2 is methyl, ethyl, propyl, cyclohexyl, phenyl, a group represented by formula III or a group represented by formula IV; R 3 is methyl, ethyl, n-propyl, isopropyl, butyl or isobutyl; R 4 is methyl or ethyl; The formula III and the formula IV: In the formula III and the formula IV: R 5 It is methyl or ethyl.

2. The silicone rubber adhesive according to claim 1, characterized in that: The silicone rubber adhesive comprises the following components in parts by weight: Hydroxy-terminated polydimethylsiloxane, 50 parts; Nano calcium carbonate, 50 parts; Methyltrimethoxysilane, 2.5 parts; Diisopropyl bis(ethyl acetoacetate) titanate, 1.5 parts; Thickener, 0.5 parts.

3. The silicone rubber adhesive according to claim 1, characterized in that: The R 3 isopropyl, butyl or isobutyl; said R 1 is n-butyl or phenyl; said R 2 It is a group represented by formula III.

4. The silicone rubber adhesive according to claim 1, characterized in that: The R 3 isopropyl; said R 4 is methyl; said R 1 is n-butyl; said R 5 It is methyl.

5. The silicone rubber adhesive according to claim 1, characterized in that: 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; The chemical structural formulas of the compound 001, the compound 002, the compound 003, the compound 004, the compound 005, the compound 006, the compound 007, the compound 008, the compound 009, the compound 011 and the compound 013 are as follows:

6. The silicone rubber adhesive according to claim 1, wherein the preparation method of the tackifier comprises the following steps: Mixing a titanate compound represented by formula VI and a glycidoxy compound represented by formula VII or formula VIII to obtain a mixture; The amine compound represented by formula V is added dropwise to the mixture, and after the addition is completed, the reaction is carried out so that R is no longer distilled out. 3 -OH compound is the end point of the reaction; The formula V, the formula VI, the formula VII and the formula VIII: In the formula V: R 1 is hydrogen, methyl, ethyl, propyl, n-butyl, cyclohexyl or phenyl; R 2 is methyl, ethyl, propyl, cyclohexyl, phenyl, a group represented by the formula III or a group represented by the formula IV; In the formula VI: R 3 is methyl, ethyl, n-propyl, isopropyl, butyl or isobutyl; In the formula VII and the formula VIII: R 4 It is methyl or ethyl.

7. The silicone rubber adhesive according to claim 6, characterized in that: The molar ratio of the amine compound represented by formula V, the titanate compound represented by formula VI, and the glycidoxy compound represented by formula VII or formula VIII is 1:(1-4):

1.

8. The silicone rubber adhesive according to claim 6, characterized in that: The working condition parameters of the dropping include: the dropping temperature is 80-100° C., and the dropping time is ≤2 hours.

9. The silicone rubber adhesive according to claim 6, characterized in that: After the addition is complete, the reaction temperature is 90-110°C.

10. A method for preparing the silicone rubber adhesive according to any one of claims 1 to 9, characterized in that: The preparation method comprises the following steps: Obtaining the tackifier; The tackifier is mixed with the remaining components in the silicone rubber adhesive to obtain the silicone rubber adhesive.

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