WO2021035909A1 - 一种热固化有机硅胶黏剂的制备方法 - Google Patents

一种热固化有机硅胶黏剂的制备方法 Download PDF

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WO2021035909A1
WO2021035909A1 PCT/CN2019/112261 CN2019112261W WO2021035909A1 WO 2021035909 A1 WO2021035909 A1 WO 2021035909A1 CN 2019112261 W CN2019112261 W CN 2019112261W WO 2021035909 A1 WO2021035909 A1 WO 2021035909A1
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component
preparing
parts
epoxy resin
stirring
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郭浩
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Zhuhai Fudan Innovation Research Institute
Fudan University
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Zhuhai Fudan Innovation Research Institute
Fudan University
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

Definitions

  • the invention relates to the technical field of polymer materials, in particular to a method for preparing a thermally curable organic silica gel adhesive.
  • Patent CN 107674639 A discloses a preparation method of organosilicone adhesive, including the steps of preparing component A, preparing component B, and mixing component A and component B and then curing. After preparing component A and component B, In the step, the raw materials are added to the first material tank and mixed for stirring, which can be carried out directly in the open system without special inert gas protection or stirring under vacuum conditions; in addition, the stirred mixture is removed from the first material The cylinder is filtered through a 300-400 mesh filter to the second cylinder under normal pressure, and high pressure extrusion is not required.
  • the patent has the following shortcomings: the obtained organic silicone adhesive has properties such as refractive index, light transmittance and thermal curing. It is difficult to meet the higher requirements for use.
  • the purpose of the present invention is to provide a method for preparing a thermally curable organic silicone adhesive in order to solve the above-mentioned problems.
  • a preparation method of thermal curing organic silicone adhesive includes the following steps:
  • Component A Weigh in parts by weight: 20-50 parts of vinyl-terminated silicone oil, 10-18 parts of epoxy resin compound and 0.005-0.01 parts of platinum catalyst;
  • component B Weigh in parts by weight: 25-40 parts of phenyl hydrogen-containing silicone oil, 3-6 parts of toughening agent, 1-2 parts of fluorine-containing compound;
  • the stirring speed in the mixing tank is both 80-100 rpm/min.
  • the time for stirring and continuing to stir in the mixing tank is 90 to 120 minutes.
  • the filter screen is a 400 mesh filter screen.
  • the vinyl-terminated silicone oil is a single-terminated vinyl polymethylsiloxane with a viscosity of 200-10000 cps.
  • the epoxy resin compound is selected from the group consisting of glycidyl ether epoxy resin, glycidyl ester epoxy resin, glycidyl amine epoxy resin, linear aliphatic epoxy resin or alicyclic epoxy resin. Oxy resin.
  • the platinum catalyst is chloroplatinic acid tetraethyldiethylenedisilane complex.
  • the phenyl hydrogen-containing silicone oil contains one or more phenyl hydrogen-containing polysiloxanes with a hydrogen content of 0.01 to 0.5%.
  • the toughening agent is selected from the group consisting of dioctyl phthalate, diisodecyl phthalate, dibutyl phthalate, dioctyl azelate, dioctyl sebacate, cyclic One or more of oxygenated soybean oil, tricresyl phosphate, triphenyl phosphate or trioctyl phosphate.
  • the fluorine-containing compound is perfluoromethyl methacrylate.
  • the present invention uses vinyl-terminated silicone oil (single-ended vinyl polymethylsiloxane) to react with epoxy resin compounds and platinum catalyst to form component A.
  • the phenyl hydrogen-containing silicone oil, the toughening agent, and the fluorine-containing compound are reacted to form component B.
  • the component A and component B are mixed and then cured to obtain a thermosetting silicone.
  • the single-end blocked vinyl is added Polymethylsiloxane, single-ended vinyl polymethylsiloxane and epoxy compounds undergo an addition reaction.
  • the epoxy resin structure contains polar groups such as hydroxyl and epoxy groups, which make the molecules and phase
  • the surface of the adjacent object has greater adsorption, which improves the overall adhesion of the adhesive; and the addition of fluorine-containing compounds significantly improves the heat resistance of the silicone adhesive.
  • the prepared silicone adhesive has More excellent refractive index, light transmittance and thermal curing properties.
  • component A weigh 25 parts by weight of 1000cps-terminated vinyl silicone oil, 12 parts of epoxy resin compound glycidyl ether epoxy resin, and 0.008 parts of chloroplatinic acid tetraethyldiethylenedisilane complex; Add the above-mentioned vinyl-terminated silicone oil and epoxy resin compounds weighed into the mixing kettle one by one, start stirring (90rpm/min) to maintain stirring for 90 minutes, then add platinum catalyst, continue stirring at the same speed for 90 minutes; The mixture obtained by stirring flows out from the mixing kettle through a 400 mesh filter at normal pressure, and enters the barrel to obtain component A.
  • Preparation component B Weigh 30 parts of phenyl hydrogen-containing silicone oil with a hydrogen content of 0.15% by weight, 4 parts of toughening agent dioctyl azelate, and 1 part of perfluoromethyl methacrylate; Take the phenyl hydrogen-containing silicone oil and the toughening agent, add them to the mixing kettle in turn, start stirring (90 rpm/min) to maintain stirring for 90 minutes, then add the fluorine-containing compound, and continue stirring at the same speed for 90 minutes; The mixture flows out of the mixing kettle through a 400 mesh filter at normal pressure and flows out into the barrel to obtain component B.
  • component A Preparation of component A: Weigh out 35 parts of 900cps-terminated vinyl silicone oil in parts by weight, 12 parts of epoxy resin compound linear aliphatic epoxy resin, and 0.005 parts of chloroplatinic acid tetraethyldiethylenedisilane complex ; Add the above-mentioned vinyl-terminated silicone oil and epoxy resin compounds weighed in sequence to the mixing kettle, start stirring (90rpm/min) to maintain stirring for 90 minutes, then add platinum catalyst, and continue stirring for 90 minutes at the same speed; The mixture obtained after stirring flows out of the mixing kettle through a 400 mesh filter at normal pressure and flows out into the barrel to obtain component A.
  • component B weigh 35 parts of phenyl hydrogen-containing silicone oil with a hydrogen content of 0.18%, 5 parts of toughening agent dioctyl sebacate, and 1 part of perfluoromethyl methacrylate; Take the phenyl hydrogen-containing silicone oil and the toughening agent, add them to the mixing kettle in turn, start stirring (90 rpm/min) to maintain stirring for 90 minutes, then add the fluorine-containing compound, and continue stirring at the same speed for 90 minutes; The mixture flows out of the mixing kettle through a 400 mesh filter at normal pressure and flows out into the barrel to obtain component B.
  • component A Preparation of component A: Weigh 20 parts of 10000cps-terminated vinyl silicone oil, 12 parts of epoxy resin compound glycidyl ester epoxy resin, and 0.008 parts of chloroplatinic acid tetraethyldiethylenedisilane complex by weight; Add the above-mentioned vinyl-terminated silicone oil and epoxy resin compounds weighed into the mixing kettle in turn, start stirring (120 rpm/min) to maintain stirring for 120 minutes, then add platinum catalyst, and continue stirring at the same speed for 120 minutes; The mixture obtained by stirring flows out from the mixing kettle through a 400-mesh filter at normal pressure, and enters the barrel to obtain component A.
  • component B Preparation of component B: Weigh 30 parts of phenyl hydrogen-containing silicone oil with a hydrogen content of 0.15% by weight, 4 parts of toughening agent triphenyl phosphate, and 1.5 parts of perfluoromethyl methacrylate; The phenyl hydrogen-containing silicone oil and the toughening agent are sequentially added to the mixing kettle, and the stirring is started (120rpm/min) to maintain the stirring for 120 minutes, then the fluorine-containing compound is added, and the stirring is continued at the same speed for 120 minutes; The mixing kettle is filtered out under normal pressure through a 400 mesh filter screen, and then enters the barrel to obtain component B.
  • component A weigh 40 parts of 5000cps-terminated vinyl silicone oil, 12 parts of epoxy resin compound glycidylamine epoxy resin, and 0.008 parts of chloroplatinic acid tetraethyldiethylenedisilane complex by weight; Add the above-mentioned vinyl-terminated silicone oil and epoxy resin compounds weighed into the mixing kettle one by one, start stirring (90rpm/min) to maintain stirring for 90 minutes, then add platinum catalyst, continue stirring at the same speed for 90 minutes; The mixture obtained by stirring flows out from the mixing kettle through a 400 mesh filter at normal pressure, and enters the barrel to obtain component A.
  • component B Preparation of component B: Weigh 30 parts of phenyl hydrogen-containing silicone oil with a hydrogen content of 0.12%, 4 parts of toughening agent tricresyl phosphate, and 1.3 parts of perfluoromethyl methacrylate in parts by weight; The phenyl hydrogen-containing silicone oil and the toughening agent are added to the mixing kettle in sequence, and the stirring is started (90rpm/min) to maintain the stirring for 90 minutes, and then the fluorine-containing compound is added, and the stirring is continued for 90 minutes at the same speed; The mixing kettle is filtered out under normal pressure through a 400 mesh filter screen, and then enters the barrel to obtain component B.
  • component A Preparation of component A: Weigh 20 parts of 4000cps-terminated vinyl silicone oil, 10 parts of epoxy resin compound alicyclic epoxy resin, and 0.008 parts of chloroplatinic acid tetraethyldiethylenedisilane complex by weight; Add the above-mentioned vinyl-terminated silicone oil and epoxy resin compounds weighed into the mixing kettle one by one, start stirring (90rpm/min) to maintain stirring for 90 minutes, then add platinum catalyst, continue stirring at the same speed for 90 minutes; The mixture obtained by stirring flows out from the mixing kettle through a 400 mesh filter at normal pressure, and enters the barrel to obtain component A.
  • component B Preparation of component B: Weigh 30 parts of phenyl hydrogen-containing silicone oil with 0.5% hydrogen content, 4 parts of toughening agent epoxy soybean oil, and 1.5 parts of perfluoromethyl methacrylate in parts by weight; The phenyl hydrogen-containing silicone oil and the toughening agent are added to the mixing kettle in sequence, and the stirring is started (90rpm/min) to maintain the stirring for 90 minutes, and then the fluorine-containing compound is added, and the stirring is continued for 90 minutes at the same speed; The mixing kettle is filtered out under normal pressure through a 400 mesh filter screen, and then enters the barrel to obtain component B.
  • component A weigh out 25 parts of 600cps-terminated vinyl silicone oil, 15 parts of epoxy resin compound alicyclic epoxy resin, and 0.008 parts of chloroplatinic acid tetraethyldiethylenedisilane complex by weight; Add the above-mentioned vinyl-terminated silicone oil and epoxy resin compounds weighed into the mixing kettle one by one, start stirring (90rpm/min) to maintain stirring for 90 minutes, then add platinum catalyst, continue stirring at the same speed for 90 minutes; The mixture obtained by stirring flows out from the mixing kettle through a 400 mesh filter at normal pressure, and enters the barrel to obtain component A.
  • component B Preparation of component B: Weigh 30 parts of phenyl hydrogen-containing silicone oil with a hydrogen content of 0.15% by weight, 5 parts of diisodecyl phthalate as a toughening agent, and 1.6 parts of perfluoromethyl methacrylate; Add the weighed phenyl hydrogen-containing silicone oil and the toughening agent to the mixing kettle one by one, start stirring (90rpm/min) and maintain the stirring for 90 minutes, then add the fluorine-containing compound, and continue stirring for 90 minutes at the same speed; The obtained mixture flows out of the mixing kettle through a 400-mesh filter under normal pressure, and enters the barrel to obtain component B.
  • component A weigh 25 parts by weight of 1000cps-terminated vinyl silicone oil, 16 parts of epoxy resin compound glycidyl ether epoxy resin, and 0.008 parts of chloroplatinic acid tetraethyldiethylenedisilane complex; Add the above-mentioned vinyl-terminated silicone oil and epoxy resin compounds weighed into the mixing kettle one by one, start stirring (90rpm/min) to maintain stirring for 90 minutes, then add platinum catalyst, continue stirring at the same speed for 90 minutes; The mixture obtained by stirring flows out from the mixing kettle through a 400 mesh filter at normal pressure, and enters the barrel to obtain component A.
  • component B Preparation of component B: Weigh 30 parts of phenyl hydrogen-containing silicone oil with a hydrogen content of 0.15% by weight, 4 parts of toughening agent dioctyl phthalate, and 2 parts of perfluoromethyl methacrylate; Weigh the phenyl hydrogen-containing silicone oil and the toughening agent, add them to the mixing kettle one by one, start stirring (90rpm/min) to maintain stirring for 90 minutes, then add the fluorine-containing compound, and continue stirring for 90 minutes at the same speed; the result will be obtained after stirring.
  • the mixture from the mixing kettle is filtered through a 400 mesh filter at atmospheric pressure and flows out into the barrel to obtain component B.
  • component A weigh 35 parts by weight of 8000cps-terminated vinyl silicone oil, 11 parts of epoxy resin compound glycidylamine epoxy resin, and 0.008 parts of chloroplatinic acid tetraethyldiethylenedisilane complex; Add the above-mentioned vinyl-terminated silicone oil and epoxy resin compounds weighed into the mixing kettle one by one, start stirring (100rpm/min) to maintain stirring for 90 minutes, then add platinum catalyst, continue stirring at the same speed for 90 minutes; The mixture obtained by stirring flows out from the mixing kettle through a 400 mesh filter at normal pressure, and enters the barrel to obtain component A.
  • component B Preparation of component B: Weigh 30 parts of phenyl hydrogen-containing silicone oil with a hydrogen content of 0.4%, 4 parts of toughening agent dibutyl phthalate, and 1 part of perfluoromethyl methacrylate; Weigh the phenyl hydrogen-containing silicone oil and the toughening agent, add them to the mixing kettle one by one, start stirring (100rpm/min) to maintain stirring for 90 minutes, then add the fluorine-containing compound, and continue stirring for 90 minutes at the same speed; the result will be obtained after stirring
  • the mixture from the mixing kettle is filtered through a 400 mesh filter at atmospheric pressure and flows out into the barrel to obtain component B.
  • the instrument used is the DRTG-81 split light transmittance tester; the component A and component B obtained in the above implementation examples are mixed to obtain a colorless and transparent liquid, and the pressure is removed Then take a small amount and apply a small amount on a glass plate of 10cm in length, 5cm in width and 2mm in thickness.
  • the thickness of the coated silicone adhesive is 0.5mm, then heat to 60°C, take it out after 20 minutes, and cool to room temperature to solidify .
  • the instrument used is the DR-M4 multi-wavelength Abbe refractometer (wavelength 589nm). The test results are shown in Table 1 below:
  • Example 1 no Colorless and transparent >99.5 1.4941
  • Example 2 no Colorless and transparent >99.6 1.5138
  • Example 3 no Colorless and transparent >99.2 1.5237
  • Example 4 no Colorless and transparent >99.9 1.6739
  • Example 5 no Colorless and transparent >99.1 1.5141
  • Example 6 no Colorless and transparent >99.2 1.4940
  • Example 7 no Colorless and transparent >99.6 1.5145
  • Example 8 no Colorless and transparent >99.3 1.5139

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

本发明涉及一种热固化有机硅胶黏剂的制备方法，步骤为：将端乙烯基硅油和环氧树脂类化合物依次加入混合釜中搅拌，然后加入铂催化剂搅拌，得到组分A；将苯基含氢硅油、增韧剂依次加入混合釜中搅拌，然后加入含氟化合物搅拌，得到组分B；将组分A和组分B混合后固化，即制得热固化有机硅胶黏剂。与传统的有机硅胶粘剂制备工艺相比，本发明所提供的热固化有机硅胶黏剂的制备方法既简化了生产条件，同时也节约了生产时间，并且按照本发明的方法所制得的有机硅胶黏剂具有很高的折射率、透光率以及热固化等性能。

Description

一种热固化有机硅胶黏剂的制备方法 技术领域
本发明涉及高分子材料技术领域，尤其是涉及一种热固化有机硅胶黏剂的制备方法。
背景技术
迄今为止，胶黏剂的传统生产工艺大多数是在真空搅拌机中通过高速分散、高压挤出、真空消泡和挤出灌装等几个阶段来完成的。在这些生产工艺中，普遍存在一些技术缺陷，如：生产条件苛刻、生产过程复杂、生产时间长、生产效率低等。
随着有机硅胶粘剂在各个工业技术领域的广泛应用，其制备工艺也受到了重视和研究。如何开发出一种便捷、高效、适合于大规模工厂化生产的有机硅胶粘剂制备工艺是亟待解决的问题。
专利CN 107674639 A公开了一种有机硅胶黏剂的制备方法，包括制备组分A、制备组分B以及将组分A和组分B混合后固化的步骤，在制备组分A和组分B的步骤中，将原料加入第一料缸混合进行搅拌，可直接在敞开体系中进行，不需要特定的惰性气体保护或者在真空的条件下进行搅拌；此外，将搅拌好的混合物从第一料缸经过300～400目的滤网常压过滤到第二料缸，不需要高压挤出，但该专利存在以下不足：所制得的有机硅胶黏剂的折射率、透光率以及热固化等性能难以满足较高要求的场合使用。
发明内容
本发明的目的就是为了解决上述问题而提供一种热固化有机硅胶黏剂的制备方法。
本发明的目的通过以下技术方案实现：
一种热固化有机硅胶黏剂的制备方法，包括如下步骤：
(1)制备组分A：以重量份计称取：端乙烯基硅油20～50份、 环氧树脂类化合物10～18份和铂催化剂0.005～0.01份；
将端乙烯基硅油和环氧树脂类化合物依次加入混合釜中搅拌，然后加入铂催化剂，继续搅拌，将得到的混合物从混合釜经滤网常压过滤，得到组分A；
(2)制备组分B：以重量份计称取：苯基含氢硅油25～40份、增韧剂3～6份、含氟化合物1-2份；
将苯基含氢硅油、增韧剂依次加入混合釜中搅拌，然后加入含氟化合物，继续搅拌，将得到的混合物经滤网常压过滤，得到组分B；
(3)将所述组分A和所述组分B混合后固化，即制得热固化有机硅胶黏剂。
优选地，制备组分A和制备组分B的步骤中，在混合釜中的搅拌速度均为80～100rpm/min。
优选地，制备组分A和制备组分B的步骤中，在混合釜中搅拌和继续搅拌的时间为90～120分钟。
优选地，制备组分A和制备组分B的步骤中，所述滤网为400目滤网。
优选地，所述端乙烯基硅油为单端封乙烯基聚甲基硅氧烷，粘度为200-10000cps。
优选地，所述环氧树脂类化合物选自缩水甘油醚类环氧树脂、缩水甘油酯类环氧树脂、缩水甘油胺类环氧树脂、线型脂肪族类环氧树脂或脂环族类环氧树脂。
优选地，所述铂催化剂为氯铂酸四乙基二乙烯二硅烷络合物。
优选地，所述苯基含氢硅油包含一种或者几种含氢量在0.01～0.5％的苯基含氢聚硅氧烷。
优选地，所述增韧剂选自邻苯二甲酸二辛酯、邻苯二甲酸二异癸酯、邻苯二甲酸二丁酯、壬二酸二辛酯、癸二酸二辛酯、环氧大豆油、磷酸三甲苯酯、磷酸三苯酯或磷酸三辛酯中的一种或几种。
优选地，所述含氟化合物为甲基丙烯酸全氟甲酯。
与专利CN 107674639 A公开的有机硅胶黏剂相比，本发明采用端乙烯基硅油(单端封乙烯基聚甲基硅氧烷)、与环氧树脂类化合物及铂催化剂先反应生成组分A，将苯基含氢硅油、增韧剂、含氟化合物反应生成组分B，组分A和组分B混合后固化，制得热固化有机硅，本发明中由于添加了单端封乙烯基聚甲基硅氧烷，单端封乙烯基聚甲基硅氧烷与环氧树脂类化合物发生加成反应，环氧树脂结构中含有羟基和环氧基等极性基团，使分子与相邻物体表面产生了较大的吸附性，提高了胶黏剂整体的粘附性；而含氟化合物的加入，显著提升了有机硅胶黏剂的耐热性，所制得的有机硅胶黏剂具有更优异的折射率、透光率以及热固化等性能。
具体实施方式
下面结合具体实施例对本发明进行详细说明，但绝不是对本发明的限制(以下各实施例中，各种原料每质量份均为1克)。
实施例1
制备组分A：以重量份计称取1000cps端乙烯基硅油25份，环氧树脂类化合物缩水甘油醚类环氧树脂12份，氯铂酸四乙基二乙烯二硅烷络合物0.008份；将称取好的上述端乙烯基硅油和环氧树脂类化合物，依次加入混合釜中，开动搅拌(90rpm/min)维持搅拌90分钟，之后加入铂催化剂，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入桶，得到组分A。
制备组分B：以重量份计称取含氢量为0.15％的苯基含氢硅油30份，增韧剂壬二酸二辛酯4份，甲基丙烯酸全氟甲酯1份；将称取好的苯基含氢硅油，增韧剂，依次加入混合釜中，开动搅拌(90rpm/min)维持搅拌90分钟，之后加入含氟化合物，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入到桶，得到组分B。
使用时，将A组分和B组分加入到反应瓶当中混合，搅拌3分钟，减压条件下抽气3分钟，脱除反应体系中的气泡，然后加热至60℃，30分钟后取出，冷却至室温，即可得到具有热固化特性的有机硅胶黏剂。
实施例2
制备组分A：以重量份计称取900cps端乙烯基硅油35份，环氧树脂类化合物线型脂肪族类环氧树脂12份，氯铂酸四乙基二乙烯二硅烷络合物0.005份；将称取好的上述端乙烯基硅油和环氧树脂类化合物，依次加入混合釜中，开动搅拌(90rpm/min)维持搅拌90分钟，之后加入铂催化剂，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入桶，得到组分A。
制备组分B：以重量份计称取含氢量为0.18％的苯基含氢硅油35份，增韧剂癸二酸二辛酯5份，甲基丙烯酸全氟甲酯1份；将称取好的苯基含氢硅油，增韧剂，依次加入混合釜中，开动搅拌(90rpm/min)维持搅拌90分钟，之后加入含氟化合物，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入到桶，得到组分B。
使用时，将A组分和B组分加入到反应瓶当中混合，搅拌3分钟，减压条件下抽气3分钟，脱除反应体系中的气泡，然后加热至60℃，30分钟后取出，冷却至室温，即可得到具有热固化特性的有机硅胶黏剂。
实施例3
制备组分A：以重量份计称取10000cps端乙烯基硅油20份，环氧树脂类化合物缩水甘油酯类环氧树脂12份，氯铂酸四乙基二乙烯二硅烷络合物0.008份；将称取好的上述端乙烯基硅油和环氧树脂类化合物，依次加入混合釜中，开动搅拌(120rpm/min)维持搅拌120分钟，之后加入铂催化剂，相同转速下继续搅拌120分钟；将经过搅 拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入桶，得到组分A。
制备组分B：以重量份计称取含氢量为0.15％的苯基含氢硅油30份，增韧剂磷酸三苯酯4份，甲基丙烯酸全氟甲酯1.5份；将称取好的苯基含氢硅油，增韧剂，依次加入混合釜中，开动搅拌(120rpm/min)维持搅拌120分钟，之后加入含氟化合物，相同转速下继续搅拌120分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入到桶，得到组分B。
使用时，将A组分和B组分加入到反应瓶当中混合，搅拌3分钟，减压条件下抽气3分钟，脱除反应体系中的气泡，然后加热至60℃，30分钟后取出，冷却至室温，即可得到具有热固化特性的有机硅胶黏剂。
实施例4
制备组分A：以重量份计称取5000cps端乙烯基硅油40份，环氧树脂类化合物缩水甘油胺类环氧树脂12份，氯铂酸四乙基二乙烯二硅烷络合物0.008份；将称取好的上述端乙烯基硅油和环氧树脂类化合物，依次加入混合釜中，开动搅拌(90rpm/min)维持搅拌90分钟，之后加入铂催化剂，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入桶，得到组分A。
制备组分B：以重量份计称取含氢量为0.12％的苯基含氢硅油30份，增韧剂磷酸三甲苯酯4份，甲基丙烯酸全氟甲酯1.3份；将称取好的苯基含氢硅油，增韧剂，依次加入混合釜中，开动搅拌(90rpm/min)维持搅拌90分钟，之后加入含氟化合物，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入到桶，得到组分B。
使用时，将A组分和B组分加入到反应瓶当中混合，搅拌3分钟，减压条件下抽气3分钟，脱除反应体系中的气泡，然后加热至 80℃，30分钟后取出，冷却至室温，即可得到具有热固化特性的有机硅胶黏剂。
实施例5
制备组分A：以重量份计称取4000cps端乙烯基硅油20份，环氧树脂类化合物脂环族类环氧树脂10份，氯铂酸四乙基二乙烯二硅烷络合物0.008份；将称取好的上述端乙烯基硅油和环氧树脂类化合物，依次加入混合釜中，开动搅拌(90rpm/min)维持搅拌90分钟，之后加入铂催化剂，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入桶，得到组分A。
制备组分B：以重量份计称取含氢量为0.5％的苯基含氢硅油30份，增韧剂环氧大豆油4份，甲基丙烯酸全氟甲酯1.5份；将称取好的苯基含氢硅油，增韧剂，依次加入混合釜中，开动搅拌(90rpm/min)维持搅拌90分钟，之后加入含氟化合物，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入到桶，得到组分B。
使用时，将A组分和B组分加入到反应瓶当中混合，搅拌3分钟，减压条件下抽气3分钟，脱除反应体系中的气泡，然后加热至60℃，30分钟后取出，冷却至室温，即可得到具有热固化特性的有机硅胶黏剂。
实施例6
制备组分A：以重量份计称取600cps端乙烯基硅油25份，环氧树脂类化合物脂环族类环氧树脂15份，氯铂酸四乙基二乙烯二硅烷络合物0.008份；将称取好的上述端乙烯基硅油和环氧树脂类化合物，依次加入混合釜中，开动搅拌(90rpm/min)维持搅拌90分钟，之后加入铂催化剂，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入桶，得到组分A。
制备组分B：以重量份计称取含氢量为0.15％的苯基含氢硅油30份，增韧剂邻苯二甲酸二异癸酯5份，甲基丙烯酸全氟甲酯1.6份；将称取好的苯基含氢硅油，增韧剂，依次加入混合釜中，开动搅拌(90rpm/min)维持搅拌90分钟，之后加入含氟化合物，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入到桶，得到组分B。
使用时，将A组分和B组分加入到反应瓶当中混合，搅拌3分钟，减压条件下抽气3分钟，脱除反应体系中的气泡，然后加热至60℃，30分钟后取出，冷却至室温，即可得到具有热固化特性的有机硅胶黏剂。
实施例7
制备组分A：以重量份计称取1000cps端乙烯基硅油25份，环氧树脂类化合物缩水甘油醚类环氧树脂16份，氯铂酸四乙基二乙烯二硅烷络合物0.008份；将称取好的上述端乙烯基硅油和环氧树脂类化合物，依次加入混合釜中，开动搅拌(90rpm/min)维持搅拌90分钟，之后加入铂催化剂，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入桶，得到组分A。
制备组分B：以重量份计称取含氢量为0.15％的苯基含氢硅油30份，增韧剂邻苯二甲酸二辛酯4份，甲基丙烯酸全氟甲酯2份；将称取好的苯基含氢硅油，增韧剂，依次加入混合釜中，开动搅拌(90rpm/min)维持搅拌90分钟，之后加入含氟化合物，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入到桶，得到组分B。
使用时，将A组分和B组分加入到反应瓶当中混合，搅拌3分钟，减压条件下抽气3分钟，脱除反应体系中的气泡，然后加热至60℃，30分钟后取出，冷却至室温，即可得到具有热固化特性的有机硅胶黏剂。
实施例8
制备组分A：以重量份计称取8000cps端乙烯基硅油35份，环氧树脂类化合物缩水甘油胺类环氧树脂11份，氯铂酸四乙基二乙烯二硅烷络合物0.008份；将称取好的上述端乙烯基硅油和环氧树脂类化合物，依次加入混合釜中，开动搅拌(100rpm/min)维持搅拌90分钟，之后加入铂催化剂，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入桶，得到组分A。
制备组分B：以重量份计称取含氢量为0.4％的苯基含氢硅油30份，增韧剂邻苯二甲酸二丁酯4份，甲基丙烯酸全氟甲酯1份；将称取好的苯基含氢硅油，增韧剂，依次加入混合釜中，开动搅拌(100rpm/min)维持搅拌90分钟，之后加入含氟化合物，相同转速下继续搅拌90分钟；将经过搅拌得到的混合物从混合釜中经过400目的滤网常压过滤流出，进入到桶，得到组分B。
使用时，将A组分和B组分加入到反应瓶当中混合，搅拌3分钟，减压条件下抽气3分钟，脱除反应体系中的气泡，然后加热至60℃，30分钟后取出，冷却至室温，即可得到具有热固化特性的有机硅胶黏剂。
固化后的有机硅胶黏剂性能测试：
透光率、折光率测定
将上述实施示例中所得到组分A和组分B混合得到的无色透明液体，减压脱除气泡，然后取少量分别加入到石英皿中，然后加热至60℃，20分钟后取出，冷却至室温固化，进行透光率的测试，所采用仪器为DRTG-81分体式透光率测试仪器；将上述实施示例中所得到组分A和组分B混合得到无色透明液体，压脱除气泡，然后取少量分别涂覆于长10cm、宽5cm、厚2mm的玻璃板上，涂覆的有机硅胶黏剂的厚度为0.5mm,然后加热至60℃，20分钟后取出，冷却至室温固化，进行折光率的测试，所采用的仪器为DR-M4多波长阿贝折 射仪(波长589nm)。测试结果如下表1所示：
表1固化后的有机硅胶黏剂透光率、折光率测定
样品 有无气泡 颜色 透光率(％) 折光率
实施例1 无 无色透明 >99.5 1.4941
实施例2 无 无色透明 >99.6 1.5138
实施例3 无 无色透明 >99.2 1.5237
实施例4 无 无色透明 >99.9 1.6739
实施例5 无 无色透明 >99.1 1.5141
实施例6 无 无色透明 >99.2 1.4940
实施例7 无 无色透明 >99.6 1.5145
实施例8 无 无色透明 >99.3 1.5139
热固化性能测定：
将上述实施示例中组分A和组分B混合所得到的无色透明液体，减压脱除气泡，然后加热至60℃，20分钟后取出，冷却至室温固化，然后在300～900℃范围内进行该有机硅胶黏剂的热固化测定，结果如下表2所示：
表2固化后的有机硅胶黏剂热固化性能测试
Figure PCTCN2019112261-appb-000001
Figure PCTCN2019112261-appb-000002
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和使用发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此，本发明不限于上述实施例，本领域技术人员根据本发明的揭示，不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。

Claims (10)

  1. 一种热固化有机硅胶黏剂的制备方法，其特征在于，包括如下步骤：
    (1)制备组分A：以重量份计称取：端乙烯基硅油20～50份、环氧树脂类化合物10～18份和铂催化剂0.005～0.01份；
    将端乙烯基硅油和环氧树脂类化合物依次加入混合釜中搅拌，然后加入铂催化剂，继续搅拌，将得到的混合物从混合釜经滤网常压过滤，得到组分A；
    (2)制备组分B：以重量份计称取：苯基含氢硅油25～40份、增韧剂3～6份、含氟化合物1-2份；
    将苯基含氢硅油、增韧剂依次加入混合釜中搅拌，然后加入含氟化合物，继续搅拌，将得到的混合物经滤网常压过滤，得到组分B；
    (3)将所述组分A和所述组分B混合后固化，即制得热固化有机硅胶黏剂。
  2. 根据权利要求1所述的一种热固化有机硅胶黏剂的制备方法，其特征在于，制备组分A和制备组分B的步骤中，在混合釜中的搅拌速度均为80～100rpm/min。
  3. 根据权利要求1所述的一种热固化有机硅胶黏剂的制备方法，其特征在于，制备组分A和制备组分B的步骤中，在混合釜中搅拌和继续搅拌的时间为90～120分钟。
  4. 根据权利要求1所述的一种热固化有机硅胶黏剂的制备方法，其特征在于，制备组分A和制备组分B的步骤中，所述滤网为400目滤网。
  5. 根据权利要求1所述的一种热固化有机硅胶黏剂的制备方法，其特征在于，所述端乙烯基硅油为单端封乙烯基聚甲基硅氧烷，粘度为200-10000cps。
  6. 根据权利要求1所述的一种热固化有机硅胶黏剂的制备方法，其特征在于，所述环氧树脂类化合物选自缩水甘油醚类环氧树脂、缩水甘油酯类环氧树脂、缩水甘油胺类环氧树脂、线型脂肪族类环氧树脂或脂环族类环氧树脂。
  7. 根据权利要求1所述的一种热固化有机硅胶黏剂的制备方法，其特征在于，所述铂催化剂为氯铂酸四乙基二乙烯二硅烷络合物。
  8. 根据权利要求1所述的一种热固化有机硅胶黏剂的制备方法，其特征在于，所述苯基含氢硅油包含一种或者几种含氢量在0.01～0.5％的苯基含氢聚硅氧烷。
  9. 根据权利要求1所述的一种热固化有机硅胶黏剂的制备方法，其特征在于，所述增韧剂选自邻苯二甲酸二辛酯、邻苯二甲酸二异癸酯、邻苯二甲酸二丁酯、壬二酸二辛酯、癸二酸二辛酯、环氧大豆油、磷酸三甲苯酯、磷酸三苯酯或磷酸三辛酯中的一种或几种。
  10. 根据权利要求1所述的一种热固化有机硅胶黏剂的制备方法，其特征在于，所述含氟化合物为甲基丙烯酸全氟甲酯。
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CN117487482B (zh) * 2024-01-03 2024-03-12 江苏斯瑞达材料技术股份有限公司 一种用于低表面能基材的胶黏剂及其制备方法

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