CN104817699A - Vinyl silicone oil and preparation method thereof - Google Patents

Vinyl silicone oil and preparation method thereof Download PDF

Info

Publication number
CN104817699A
CN104817699A CN 201510199209 CN201510199209A CN104817699A CN 104817699 A CN104817699 A CN 104817699A CN 201510199209 CN201510199209 CN 201510199209 CN 201510199209 A CN201510199209 A CN 201510199209A CN 104817699 A CN104817699 A CN 104817699A
Authority
CN
Grant status
Application
Patent type
Prior art keywords
silicone
oil
method
vinyl
preparation
Prior art date
Application number
CN 201510199209
Other languages
Chinese (zh)
Inventor
张静
李童成
应静桦
王彩凤
张喆
Original Assignee
浙江润禾有机硅新材料有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date

Links

Abstract

The invention relates to a preparation method of a modified silicone oil, i.e., a vinyl silicone oil containing an alkylene structure; and specifically, the invention relates to preparation steps and a preparation method of the vinyl silicone oil containing the alkylene structure. The method comprises the following steps: preparing carbon-carbon bond and silicon-oxygen bond into cyclic prepolymer polysiloxane A1 and A2 through silicon-hydrogen addition reaction; then concurrently balancing with polydimethylsiloxane cyclic mixture, hexamethyldisiloxane, divinyl-tetramethyl-disiloxane, tetramethyl tetravinyl cyclotetrasiloxane, or the like; and then neutralizing, filtering, and extracting low-boiling-point substances, thereby obtaining a colorless transparent liquid. The vinyl silicone oil is especially applicable to the requirements of low moisture permeation and low oxygen permeation in the LED packaging industry, and is of a certain acceleration effect to splicing packaging brackets.

Description

一种乙烯基硅油及其制备方法 One vinyl silicone oils and its preparation method

技术领域 FIELD

[0001] 本发明涉及一种改性硅油即含亚烷基结构的乙烯基硅油的制备方法,具体而言, 本发明涉及含亚烷基结构的乙烯基硅油的制备步骤及方法。 [0001] The present invention relates to a method of preparing modified silicone oil-containing vinyl silicone oil that is an alkylene group of the structure, specifically, the present invention relates to a method and a vinyl-containing silicone steps alkylene structure.

背景技术 Background technique

[0002] 硅油是有机硅化合物中重要的种类,通常是指室温下保持液体状态的线性聚硅烷产品,结构式如下: [0002] The organic silicon compound is a silicone oil important species, generally refers to remain liquid at room temperature and a linear polysilane of the product, the following structural formula:

Figure CN104817699AD00041

式中,R为烷基,芳基;R'为烷基,芳基,氣碳官能基及聚酿链等;X为烷基、芳基、链條基、氣、羟基、烷氧基、乙醜氧基、氣、碳官能基及聚醚链等;n、m=0、l、2、3...... 由于硅和碳同属元素周期表第IVA族元素,故具有某些相似的化学性质。 Wherein, R is alkyl, aryl; R 'is an alkyl group, an aryl group, a functional group and carbon gas poly stuffed chain; X is an alkyl group, an aryl group, a chain group, air, hydroxy, alkoxy, Chou group, air, carbon chain and a polyether functional group; n, m = 0, l, 2,3 ...... since the silicon and carbon elements belong to group IVA of the periodic table, it has some similar chemical properties. 如硅和碳均有4个未成对的S电子及P电子,它们可与电负性较高的元素(如Fe、0、Cl等)及电负性较低的基团(如H-、CH3-、C6H5-等)结合,达到共价饱和。 The silicon and carbon are four unpaired electrons of S and P electronics, they may be higher electronegative elements (such as Fe, 0, Cl, etc.) and the electrically negative low group (such as H-, CH3-, C6H5-, etc.) in combination, to achieve covalent saturation. 硅原子可以同碳原子形成共价键, 也可以同有机基团结合,生成许多有机硅化合物。 Silicon atoms may form a covalent bond with the carbon atom may be combined with an organic group, the organic silicon compound generating a number. 但两者所处的周期不停,因而存在不少差异。 However, both the period in which the stop, and thus there are many differences. 如碳与氧优先生成双键,而硅主要形成单键。 The carbon to oxygen double bond is preferentially formed, mainly silicon and form a single bond. 在形成聚合物时碳是以CCC为主链。 When forming the polymer main chain carbon is CCC. 而硅则主要以Si-0-Si为主链。 And silicon is mainly Si-0-Si as a main chain. 该链是构成聚硅氧烷的基本链型。 The chain is substantially composed of polysiloxane chain.

[0003] 硅油是一类品种,系列较多,应用范围较广的有机硅产品。 [0003] is a silicone oil varieties, more series, a wide range of applications of silicone products. 具有优异的离型性、透气透湿性。 It has excellent releasability, breathable properties. 但用于LED封装材料,则需要增加与基材的粘接性,降低它的透气透湿性能。 However, a LED encapsulating material, it is necessary to increase adhesion to the substrate, reduce its breathable properties. 在硅油的硅氧烷主链节上嵌进碳碳链的亚烷基结构,既能保持硅油的其它优良的性能,同时也能很好改善粘接性和透气透湿性。 Embedded in a carbon-carbon chain of the siloxane backbone of the alkylene silicone section, both maintaining other excellent properties of silicone, but also can improve adhesion and very good water vapor permeability resistance.

[0004] 在LED行业,封装材料对LED的影响至关重要。 [0004] In the LED industry, the impact of LED encapsulating material is essential. LED封装材料已经由原先的环氧类材料逐步转变成为有机娃材料。 LED encapsulating material has an epoxy-based material from the original gradually transformed into baby organic material. 为了达到封装材料耐紫外、耐热老化以及低应力等要求,根据不同用途,封装材料大致分为低折硅胶跟高折硅胶两大类。 In order to meet the requirements of the encapsulation material UV resistance, heat aging, and low stress, according to different uses, packaging materials are roughly classified into low refractive silica with a high refractive silicone into two categories. 低折硅胶有很好的透明度及机械性能,耐黄变比高折封装胶有优势,但也存在一定的缺陷,由于其结构问题,使得透气透湿性比高折封装胶差。 Low refractive silica gel has good mechanical properties and transparency, yellowing resistance ratio packaging plastic off has advantages, but there are some defects, due to structural problems, so that the water vapor permeability of the packaging plastic off ratio difference. 本发明针对此问题,对线性乙烯基硅油结构进行调整,引进亚烷基结构,以提高其耐透气透湿性能。 The present invention is directed to this problem, the linear vinyl silicone oil to adjust the structure, the introduction of the alkylene, to increase its resistance to moisture permeability properties.

发明内容 SUMMARY

[0005] 针对现有低折硅胶跟高折硅胶之间的差异,本发明的第一个目的是公开了一种新型的改性乙烯基硅油,即为含亚烷基的乙烯基硅油。 [0005] for the differences between the conventional low refractive silica with a high refractive silicone, a first object of the present invention is to disclose a novel vinyl-modified silicone oil, that is an alkylene group containing vinyl silicone oil. 本发明第二个目的是指在常规有机硅硅油的硅氧链接中加入碳碳键制成含亚烷基改性硅油的一种合成方法。 A second object of the present invention refers to the addition of a carbon-carbon bond linking silicone silicone silicone oil in a conventional method of synthesis of alkyl-modified silicone-containing alkylene made. 所得硅油能满足低折硅胶的透气透湿性,也能满足高折硅胶的应力影响问题,是LED封装胶行业比较好的材料选择。 The resulting silicone oil to meet the water vapor permeability of the low refractive silica, but also to meet the stress of the impact of high refractive silicone, the LED packaging adhesive SECTOR good material choice.

[0006] 为了实现上述的第一个目的,本发明采用了以下的技术方案: 一种含亚烷基结构乙烯基硅油,其特征在于,所述的硅油结构为以下结构式中的一种或两种的混合: [0006] To achieve the above first object, the present invention adopts the following technical solutions: A structure containing an alkylene vinyl silicone oil, wherein the silicone structure is one of the following two formulas or species mixed:

Figure CN104817699AD00051

上述的nl、n2、n3分别为大于等于0的正整数且不能够全部为0,上述的ml、m2分别为大于等于〇的正整数且不能够全部为〇,q为大于等于1的正整数。 Above nl, n2, n3 are positive integers greater than 0 and not all can be 0, the above-described ml, m2 are positive integers greater than or equal square and not all can be square, q is a positive integer greater than or equal to 1 .

[0007] 作为优选,所述的111、112、113为1~100的正整数,1111、1112分别为1~100的正整数,9 为1~100的正整数。 [0007] Advantageously, according to a positive integer from 1 to 111, 112, 100, 1111 and 1112 respectively a positive integer of 1 to 100, 9 is a positive integer of 1 to 100.

[0008] 作为优选,所述的nl、n2、n3为2~50的正整数,ml、m2分别为2~50的正整数,q为2~50的正整数。 [0008] Advantageously, said nl, n2, n3 is a positive integer of 2 to 50, ml, m2 are each a positive integer of 2 to 50, q is a positive integer of 2 to 50.

[0009] 为了实现上述的第二个目的,本发明采用了以下的技术方案: 一种制备上述的含亚烷基结构乙烯基硅油的制备方法,该方法包括以下的步骤: 1) 聚硅氧烷A的制备: 将氢硅氧烷与含烯基的硅烷或硅氧烷,在铂催化剂作用下,加成反应得下列结构式产 [0009] To achieve the above second object, the present invention adopts the following technical solutions: A alkylene group containing the above-described method for preparing the preparation of vinyl silicone oil structure, the method comprising the steps of: 1) silicone a preparation of alkoxy: hydrogen siloxane and the alkenyl group-containing silane or siloxane, platinum catalyst in the addition reaction to give the following structural formula yield

Figure CN104817699AD00052

上述的n为大于等于1的正整数; 2) 由上述步骤1)产物,再与八甲基环四硅氧烷及1,1,3,3 -四甲基_1,3 -二乙烯基二硅氧烷,在酸催化下,平衡聚合;除去低挥发份组份,得以下结构式(1)和(2)的产物: The above n is a positive integer greater than or equal to 1; 2) the above Step 1) product, and the octamethyl cyclotetrasiloxane and 1,1,3,3 - tetramethyl _1,3 - divinyl disiloxane, under acid catalysis, the polymerization balance; removing low-volatile ingredients, have the following structural formula (1) (2) and the product of:

Figure CN104817699AD00061

3)由上述结构式(1)和/或(2)的产物,与八甲基环四硅氧烷,四甲基四乙烯基环四硅氧烷,六甲基二硅氧烷,在酸催化下,平衡聚合;得含亚烷基结构的乙烯基硅油,除去低挥发份组份,得结构式(5)和/或(6)所示的含亚烷基结构的乙烯基硅油产物。 3) the product of the above formula (1) and / or (2), and the octamethyl cyclotetrasiloxane, tetramethyl tetravinyl cyclotetrasiloxane, hexamethyldisiloxane, in acid catalysis under equilibrium polymerization; vinyl-containing silicone oil have an alkylene structure, removing low volatile ingredients to give structural formulas (5) and / or vinyl silicone oil product containing alkylene group represented by structure (6).

[0010] 作为优选,所述的结构产物A1、A2的原料为1,1,3, 3-四甲基-1,3-二氢基二硅氧烷,二乙烯基硅烷,1,1,3, 3-四甲基-1,3-二乙烯基二硅氧烷,在铂催化剂作用下,进行加成反应制得。 [0010] Advantageously, the structure of the product A1, A2 starting material is 1,1,3,3-tetramethyl-1,3-dihydro-disiloxane, divinyl silane, 1,1, 3, 3-tetramethyl-1,3-divinyldisiloxane, the platinum catalyst, an addition reaction.

[0011] 作为优选,所述的结构产物Al、A2合成采用的催化剂为铂催化剂,作为优选,铂催化剂选用铂-乙烯基硅氧烷配合物或铂-醇溶液。 [0011] Advantageously, the product structures Al, A2 synthesis catalyst employed is a platinum catalyst, preferably a platinum catalyst selected a platinum - vinylsiloxane complex or a platinum - alcoholic solution.

[0012] 作为优选,所述的结构产物A1、A2合成采用的所述反应温度:40~120°C,所述反应时间:5~24小时。 [0012] Advantageously, the structure of the product A1, A2 synthesized by the reaction temperature of: 40 ~ 120 ° C, the reaction time: 5 to 24 hours.

[0013] 作为优选,所述的结构产物Al、A2合成反应结束,除去催化剂,除去铂催化剂的方法,选择金属吸附剂或吸附炭黑。 [0013] Advantageously, the product structures Al, A2 synthesis reaction was completed, the catalyst was removed, the method of removing the platinum catalyst, adsorbent or adsorbent carbon black selected metal.

[0014] 作为优选,所述的结构式(3)和/或(4)合成所述酸催化剂选用三氟甲烷磺酸,浓硫酸或盐酸;所述反应温度30~100°C;所述反应时间4~48小时;反应结束,除去催化剂。 [0014] Advantageously, (3) and / or (4) Synthesis of the acid catalyst of the formula selected trifluoromethanesulfonic acid, concentrated sulfuric acid or hydrochloric acid; the reaction temperature is 30 ~ 100 ° C; the reaction time 4 to 48 hours; the reaction was complete, the catalyst was removed.

[0015] 作为优选,所述的除催化剂方法,选用中和过滤,中和剂选用碳酸钠,碳酸氢钠或六甲基二硅氮烷。 [0015] Advantageously, the method of catalyst addition, and the choice of filter, the choice of neutralizing agent sodium carbonate, sodium bicarbonate or hexamethyl disilazane.

[0016] 本方法是通过硅氢加成反应将碳碳键与硅氧键制成环状预聚物聚硅氧烷Al、A2, 再在一定条件下,与聚二甲基硅氧烷混合环体,六甲基二硅氧烷,二乙烯基四甲基二硅氧烧,四甲基四乙烯基环四硅氧烷等共同平衡,再经中和,过滤,拔出低沸物,得到无色透明液体。 [0016] In this method, by the hydrosilylation reaction with the carbon-carbon bond formed by siloxane bonds, a cyclic polysiloxane prepolymer Al, A2, and then, under certain conditions, mixed with polydimethylsiloxane ring, hexamethyl disiloxane, divinyl tetramethyl disiloxane burning, tetramethyl tetravinyl cyclotetrasiloxane other common balance, and then it was filtered, pulled low boilers, to give a colorless transparent liquid. 本发明产品特别适用于LED灌封行业,对于低透湿透氧的要求,并且对灌封支架的粘接有一定的促进作用。 The present invention is particularly suitable for encapsulating LED industry, the oxygen required for low moisture permeability, and have some role in promoting adhesion potting stent.

具体实施方式 detailed description

[0017] 下面对本发明的事实作具体说明,但实施例不是对本发明保护范围的限制。 [0017] Next, the fact that the present invention will be specifically described, but the examples are not to limit the scope of the present invention.

[0018] 实施例1 : 向500ml干燥的三口瓶中加入二乙烯基硅烷112g,开始加热,在40度下加入催化剂1. 5ppm,搅拌5min后滴加四甲基二氢基二硅氧烷134g,滴加1小时,控制反应温度在40~60 度,待滴加完成后,40~60度保温7小时后降至室温,加入金属吸附剂,室温搅拌5小时,将产物A滤出待用。 [0018] Example 1: To a dry 500ml three-necked flask 112 g divinyl silane, heating is started, the catalyst is added 1. 5ppm at 40 degrees, was added dropwise with stirring for 5min dihydro-tetramethyl disiloxane 134g was added dropwise for 1 hour and the reaction temperature is controlled at 40 to 60 degrees, until the completion of the dropwise addition, 40 to 60 degrees after 7 hours incubation cooled to room temperature, adding metal adsorbent, stirred at room temperature for 5 hours the product was filtered off standby A . 向500ml干燥的三口瓶中加入产物A135g、八甲基四硅氧烷130g、四甲基二乙烯基二硅氧烷〇.41g、三氟甲烷磺酸0.llg平衡聚合12小时。 The product A135g were added to 500ml dry three-neck flask, octamethyltetrasiloxane 130g, tetramethyl divinyl disiloxane 〇.41g trifluoromethanesulfonate 0.llg balance polymerized for 12 hours. 平衡后,加六甲基二硅氮烷40g中和后,抽滤,除去低组分得到无色透明液体,即为产物。 After equilibration, bis (trimethylsilyl) amine and 40g after suction filtration, to remove low fraction obtained colorless transparent liquid, i.e. product. 测得粘度8220mpas,乙烯基质量百分含量〇. 09%,挥发份(150°C/2hr) 0. 33%。 The measured viscosity of 8220mpas, the mass percentage of vinyl billion. 09%, volatile matter (150 ° C / 2hr) 0. 33%.

[0019] 实施例2 : 向500ml干燥的三口瓶中加入二乙烯基硅烷112g,开始加热,在45度下加入催化剂1. 5ppm,搅拌5min后滴加四甲基二氢基二硅氧烷134g,滴加1小时,控制反应温度在40~60 度,待滴加完成后,40~60度保温9小时后降至室温,加入金属吸附剂,室温揽样5小时,将产物A滤出待用。 [0019] Example 2: To a dry 500ml three-necked flask 112 g divinyl silane, heating is started, the catalyst was added at 45 degrees 1. 5ppm, dropwise stirring for 5min dihydro-tetramethyl disiloxane 134g was added dropwise for 1 hour and the reaction temperature is controlled at 40 to 60 degrees, until the completion of the dropwise addition, 40 to 60 degrees down to 9 hours after incubation at room temperature, adding metal sorbent, football-like at room temperature for 5 hours and the product filtered off to be A use. 向500ml干燥的三口瓶中加入产物A134g、八甲基四硅氧烷121g、四甲基二乙烯基二硅氧烷〇.34g、三氟甲烷磺酸0.lg平衡聚合12小时。 The product A134g were added to 500ml dry three-neck flask, 121g octamethyl cyclotetrasiloxane, tetramethyl divinyl disiloxane 〇.34g trifluoromethanesulfonate 0.lg balance polymerized for 12 hours. 平衡后,加六甲基二硅氮烷40g中和后,抽滤,除去低组分得到无色透明液体,即为产物。 After equilibration, bis (trimethylsilyl) amine and 40g after suction filtration, to remove low fraction obtained colorless transparent liquid, i.e. product. 测得粘度4160mpas,乙烯基质量百分含量〇. 15%,挥发份(150°C/2hr) 0. 61%。 The measured viscosity of 4160mpas, the mass percentage of vinyl billion. 15%, volatile matter (150 ° C / 2hr) 0. 61%.

[0020] 实施例3 : 向500ml干燥的三口瓶中加入四甲基二乙烯基二硅氧烷186g,开始加热,在40度下加入催化剂1. 5ppm,搅拌5min后滴加四甲基二氢基二硅氧烷134g,滴加1小时,控制反应温度在40~60度,待滴加完成后,40~60度保温7小时后降至室温,加入金属吸附剂,室温搅拌5小时,将产物A滤出待用。 [0020] Example 3: To a dried three-necked 500ml flask tetramethyl divinyl disiloxane 186 g of, heating is started, the catalyst was added at 40 degrees 1. 5ppm After 5min stirring dropwise tetramethyl-dihydro- disiloxane 134g, dropping one hour, the reaction temperature is controlled at 40 to 60 degrees, until the completion of the dropwise addition, 40 to 60 degrees after 7 hours incubation cooled to room temperature, adding metal adsorbent, stirred at room temperature for 5 hours, A product was filtered off and set aside. 向500ml干燥的三口瓶中加入产物A113g、八甲基四硅氧烷87g、四甲基二乙烯基二硅氧烷0. 24g、浓硫酸3. 2g平衡聚合12小时。 It was added to a 500ml three-necked flask dried product A113g, octamethyltetrasiloxane 87g, tetramethyl divinyl disiloxane 0. 24g, 3. 2g of concentrated sulfuric acid balance polymerized for 12 hours. 平衡后,加碳酸氢钠4. 8g中和后,抽滤,除去低组分得到无色透明液体,即为产物。 After equilibration, 4. 8g of sodium bicarbonate and after suction filtration, to remove low fraction obtained colorless transparent liquid, i.e. product. 测得粘度3533mpas,乙烯基质量百分含量〇. 17%,挥发份(150°C/2hr) 0. 25%。 The measured viscosity of 3533mpas, the mass percentage of vinyl billion. 17%, volatile matter (150 ° C / 2hr) 0. 25%.

[0021] 实施例4: 向500ml干燥的三口瓶中加入四甲基二乙烯基二硅氧烷186g,开始加热,在40度下加入催化剂1. 5ppm,搅拌5min后滴加四甲基二氢基二硅氧烷134g,滴加1小时,控制反应温度在40~60度,待滴加完成后,40~60度保温7小时后降至室温,加入金属吸附剂,室温搅拌5小时,将产物A滤出待用。 [0021] Example 4: To a dried three-necked 500ml flask tetramethyl divinyl disiloxane 186 g of, heating is started, the catalyst was added at 40 degrees 1. 5ppm After 5min stirring dropwise tetramethyl-dihydro- disiloxane 134g, dropping one hour, the reaction temperature is controlled at 40 to 60 degrees, until the completion of the dropwise addition, 40 to 60 degrees after 7 hours incubation cooled to room temperature, adding metal adsorbent, stirred at room temperature for 5 hours, A product was filtered off and set aside. 向500ml干燥的三口瓶中加入产物A113g、八甲基四硅氧烷87g、四甲基二乙烯基二硅氧烷1. 03g、四甲基四乙烯基环四硅氧烷3. 23g、浓硫酸3. 3g平衡聚合8小时。 The product A113g were added to 500ml dry three-neck flask, 87g octamethyl cyclotetrasiloxane, tetramethyl divinyl disiloxane 1. 03g, tetramethyl tetravinyl cyclotetrasiloxane 3. 23g, conc. 3. 3g sulfuric equilibrium polymerization for 8 hours. 平衡后,加碳酸氢钠4. 9g中和后,抽滤,除去低组分得到无色透明液体,即为产物。 After equilibration, 4. 9g of sodium bicarbonate and after suction filtration, to remove low fraction obtained colorless transparent liquid, i.e. product. 测得粘度5190mpas,乙烯基质量百分含量0. 64%,挥发份(150°C/2hr) 0. 38%。 The measured viscosity of 5190mpas, vinyl mass percentage of 0.64%, volatile matter (150 ° C / 2hr) 0. 38%.

[0022] 实施例5 : 向500ml干燥的三口瓶中加入二乙烯基硅烷112g,开始加热,在40度下加入催化剂1. 5ppm,搅拌5min后滴加四甲基二氢基二硅氧烷134g,滴加1小时,控制反应温度在40~60 度,待滴加完成后,40~60度保温7小时后降至室温,加入吸附炭黑,室温搅拌5小时,将产物A滤出待用。 [0022] Example 5: divinyl silane was added to 112g dried 500ml three-necked flask, heating is started, the catalyst is added 1. 5ppm at 40 degrees, was added dropwise with stirring for 5min dihydro-tetramethyl disiloxane 134g was added dropwise for 1 hour and the reaction temperature is controlled at 40 to 60 degrees, until the completion of the dropwise addition, 40 to 60 degrees down to room temperature and after 7 hours incubation, the adsorption of carbon black was added, was stirred room temperature for 5 hours, the product was filtered off standby A . 向500ml干燥的三口瓶中加入产物A150g、八甲基四硅氧烷120g、四甲基四乙烯基环四硅氧烷3. 08g、六甲基二硅氧烷1. 5g、浓硫酸4. 4g平衡聚合8小时。 The product A150g were added to 500ml dry three-neck flask, octamethyltetrasiloxane 120g, tetramethyl tetravinyl cyclotetrasiloxane 3. 08g, hexamethyldisiloxane 1. 5g, 4 of concentrated sulfuric acid. 4g equilibrium polymerization for 8 hours. 平衡后,加碳酸氢钠6. 6g中和后,抽滤,除去低组分得到无色透明液体,即为产物。 After equilibration, sodium bicarbonate and 6. 6g after suction filtration, to remove low fraction obtained colorless transparent liquid, i.e. product. 测得粘度6050mpas, 乙烯基质量百分含量〇. 35%,挥发份(150°C/2hr) 0. 42%。 The measured viscosity of 6050mpas, the mass percentage of vinyl billion. 35%, volatile matter (150 ° C / 2hr) 0. 42%.

Claims (10)

  1. 1. 一种乙烯基硅油,其特征在于,所述的硅油结构为以下结构式中的一种或两种的混合: A vinyl silicone oil, wherein the silicone oils of the following structural formulas or a mixture of two:
    Figure CN104817699AC00021
    上述的nl、n2、n3分别为大于等于O的正整数且不能够全部为0,上述的ml、m2分别为大于等于〇的正整数且不能够全部为〇, q为大于等于1的正整数。 Above nl, n2, n3 are positive integers greater than or equal to O and not all can be 0, the above-described ml, m2 are positive integers greater than or equal square and not all can be square, q is a positive integer greater than or equal to 1 .
  2. 2. 根据权利要求1所述的一种乙烯基硅油,其特征在于,nl、n2、n3为1~100的正整数, ml、m2分别为1~100的正整数,q为1~100的正整数。 The one vinyl silicone oil according to claim 1, wherein, nl, n2, n3 is a positive integer of 1 to 100, ml, m2 are each a positive integer of 1 to 100, q is from 1 to 100 a positive integer.
  3. 3. 根据权利要求1所述的一种乙烯基硅油,其特征在于,nl、n2、n3为2~50的正整数, ml、m2分别为2~50的正整数,q为2~50的正整数。 The one vinyl silicone oil according to claim 1, wherein, nl, n2, n3 is a positive integer of 2 to 50, ml, m2 are each a positive integer of 2 to 50, q is 2 to 50 a positive integer.
  4. 4. 一种制备权利要求1~3任意一项权利要求所述的一种乙烯基硅油的制备方法,其特征在于该方法包括以下的步骤: 1) 聚硅氧烷A的制备: 将氢硅氧烷与含烯基的硅烷或硅氧烷,在铂催化剂作用下,加成反应得下列结构式产 A method for preparing a vinyl silicone oil is 1 to 3, any one of claim 4. A preparation as claimed in claim, characterized in that the method comprises the following steps: 1) Preparation of Polysiloxane A is: hydrogen silicon alumoxane and alkenyl-containing silane or siloxane, platinum catalyst in the addition reaction to give the following structural formula yield
    Figure CN104817699AC00022
    上述的n为大于等于1的正整数; 2) 由上述步骤1)产物,再与八甲基环四硅氧烷及1,1,3,3 -四甲基_1,3 -二乙烯基二硅氧烷,在酸催化下,平衡聚合;除去低挥发份组份,得以下结构式(1)和(2)的产物: The above n is a positive integer greater than or equal to 1; 2) the above Step 1) product, and the octamethyl cyclotetrasiloxane and 1,1,3,3 - tetramethyl _1,3 - divinyl disiloxane, under acid catalysis, the polymerization balance; removing low-volatile ingredients, have the following structural formula (1) (2) and the product of:
    Figure CN104817699AC00031
    3)由上述结构式(1)和/或(2)的产物,与八甲基环四硅氧烷,四甲基四乙烯基环四硅氧烷,六甲基二硅氧烷,在酸催化下,平衡聚合;得含亚烷基结构的乙烯基硅油,除去低挥发份组份,得结构式(5)和/或(6)所示的含亚烷基结构的乙烯基硅油产物。 3) the product of the above formula (1) and / or (2), and the octamethyl cyclotetrasiloxane, tetramethyl tetravinyl cyclotetrasiloxane, hexamethyldisiloxane, in acid catalysis under equilibrium polymerization; vinyl-containing silicone oil have an alkylene structure, removing low volatile ingredients to give structural formulas (5) and / or vinyl silicone oil product containing alkylene group represented by structure (6).
  5. 5. 根据权利要求4所述的制备方法,其特征在于,结构产物A1、A2的原料为1,1,3, 3-四甲基-1,3- 二氛基^硅氧烷,^乙條基硅烷,I,1,3, 3-四甲基-1,3- 二乙條基^娃氧烷,在铂催化剂作用下,进行加成反应制得。 The production method according to claim 4, characterized in that the structure of the product A1, A2 starting material is 1,1,3,3-tetramethyl-1,3-siloxane atmosphere yl ^ ^ B Article silane, I, 1,3, 3- tetramethyl-1,3-diethyl-yl article Wa ^ siloxane, platinum catalyst in, an addition reaction.
  6. 6. 根据权利要求5所述的制备方法,其特征在于,结构产物Al、A2合成采用的催化剂为铂催化剂,作为优选,铂催化剂选用铂-乙烯基硅氧烷配合物或铂-醇溶液。 The production method according to claim 5, characterized in that the structure of the product Al, A2 synthesis catalyst employed is a platinum catalyst, preferably a platinum catalyst selected a platinum - vinylsiloxane complex or a platinum - alcoholic solution.
  7. 7. 根据权利要求5所述的制备方法,其特征在于,结构产物Al、A2合成采用的所述反应温度:40~120°C,所述反应时间:5~24小时。 The production method according to claim 5, characterized in that the structure of the product Al, A2 synthesized by the reaction temperature: 40 ~ 120 ° C, the reaction time: 5 to 24 hours.
  8. 8. 根据权利要求5所述的制备方法,其特征在于,结构产物A1、A2合成反应结束,除去催化剂,除去铂催化剂的方法,选择金属吸附剂或吸附炭黑。 8. The production method according to claim 5, characterized in that the structure of the product A1, A2 end of the synthesis reaction, the catalyst was removed, the method of removing the platinum catalyst, adsorbent or adsorbent carbon black selected metal.
  9. 9. 根据权利要求5所述的制备方法,其特征在于,结构式(5)和/或(6)合成所述酸催化剂选用三氟甲烷磺酸,浓硫酸或盐酸;所述反应温度30~100°C ;所述反应时间4~48小时;反应结束,除去催化剂。 9. The production method according to claim 5, characterized in that the structure of formula (5) and / or (6) Synthesis of the acid catalyst selected trifluoromethanesulfonic acid, concentrated sulfuric acid or hydrochloric acid; the reaction temperature of 30 to 100 ° C; the reaction time is 4 to 48 hours; the reaction was completed, the catalyst was removed.
  10. 10. 根据权利要求9所述的制备方法,其特征在于,除催化剂方法,选用中和过滤,中和剂选用碳酸钠,碳酸氢钠或六甲基二硅氮烷。 10. The production method according to claim 9, characterized in that the method of catalyst addition, and the choice of filter, the choice of neutralizing agent sodium carbonate, sodium bicarbonate or hexamethyl disilazane.
CN 201510199209 2015-04-24 2015-04-24 Vinyl silicone oil and preparation method thereof CN104817699A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 201510199209 CN104817699A (en) 2015-04-24 2015-04-24 Vinyl silicone oil and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 201510199209 CN104817699A (en) 2015-04-24 2015-04-24 Vinyl silicone oil and preparation method thereof

Publications (1)

Publication Number Publication Date
CN104817699A true true CN104817699A (en) 2015-08-05

Family

ID=53728194

Family Applications (1)

Application Number Title Priority Date Filing Date
CN 201510199209 CN104817699A (en) 2015-04-24 2015-04-24 Vinyl silicone oil and preparation method thereof

Country Status (1)

Country Link
CN (1) CN104817699A (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5442083A (en) * 1993-09-03 1995-08-15 Dow Corning Toray Silicone Company, Ltd. Method for the preparation of organosilicon polymer
US6080829A (en) * 1998-06-24 2000-06-27 Medtronic, Inc. Silalkylenesiloxane copolymer materials and methods for their preparation
CN101955587A (en) * 2009-07-17 2011-01-26 信越化学工业株式会社 Organohydrogenpolysiloxane, making method, and addition-cure silicone composition
CN102596970A (en) * 2009-11-03 2012-07-18 道康宁公司 A process for the production of polysilalkylenesiloxanes

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5442083A (en) * 1993-09-03 1995-08-15 Dow Corning Toray Silicone Company, Ltd. Method for the preparation of organosilicon polymer
US6080829A (en) * 1998-06-24 2000-06-27 Medtronic, Inc. Silalkylenesiloxane copolymer materials and methods for their preparation
CN101955587A (en) * 2009-07-17 2011-01-26 信越化学工业株式会社 Organohydrogenpolysiloxane, making method, and addition-cure silicone composition
CN102596970A (en) * 2009-11-03 2012-07-18 道康宁公司 A process for the production of polysilalkylenesiloxanes

Similar Documents

Publication Publication Date Title
US4087585A (en) Self-adhering silicone compositions and preparations thereof
US3539530A (en) Flame resistant organopolysiloxane compositions
WO2009065644A1 (en) Method for producing branched sih functional polysiloxanes and the use thereof for producting sic- and sioc-linked, branched organomodified polysiloxanes
US4398010A (en) Method for accelerating the activity of a hydrosilation catalyst
JP2005307015A (en) Curable composition for sealing optical material
JP2000154252A (en) Novel silsequioxane-containing polymer and its production
CN101891893A (en) Preparation method of phenyl-based hydrogen-based silicone resin for encapsulating LED
CN101356214A (en) Thermally stable transparent silicone resin compositions and methods for their preparation and use
CN101659748A (en) Hyper-branched silicone resin containing active functional group and preparation method thereof
WO2011145638A1 (en) Novel organosilicon compound and thermosetting resin composition, cured resin, and semiconductor sealing material containing said organosilicon compound
US20080220266A1 (en) Silicone resin composition
CN101899159A (en) Silicone resin for one-component LED packaging materials and preparation method thereof
JP2010116462A (en) Siloxane polymer, siloxane-based crosslinkable composition and silicone membrane
US6828355B1 (en) Resin-reinforced UV, moisture and UV/moisture dual curable silicone compositions
WO2007001039A1 (en) Curable organopolysiloxane resin composition and optical part molded therefrom
JPH0739547B2 (en) RTV organopolysiloxane compositions
JP2009227863A (en) Cage structure-containing curable silicone copolymer, method for producing the same, curable resin composition using cage structure-containing curable silicone copolymer, and cured product thereof
WO2004035661A1 (en) Silicone resins
CN102234431A (en) High adhesiveness silicone resin composition and an optical semiconductor device provided with a cured product thereof
US8158265B2 (en) Addition-curable silicone composition that produces cured product having high refractive index, and optical element encapsulating material formed from the composition
JP2011190413A (en) Siloxane polymer crosslinking-cured product
JP2010280766A (en) Organosilicon compound, thermocurable composition containing the organosilicon compound, and sealing material for optical semiconductor
US3458469A (en) Curing system for room temperature vulcanizing organopolysiloxane elastomers
JP2013010881A (en) Addition curing silicone composition, and optical device
CN102850804A (en) Transparent two-component organic silicon pouring sealant for LED and preparation method thereof

Legal Events

Date Code Title Description
C06 Publication
EXSB Decision made by sipo to initiate substantive examination