WO2021254169A1 - 一种有机硅消泡组合物的制备方法 - Google Patents

一种有机硅消泡组合物的制备方法 Download PDF

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WO2021254169A1
WO2021254169A1 PCT/CN2021/098236 CN2021098236W WO2021254169A1 WO 2021254169 A1 WO2021254169 A1 WO 2021254169A1 CN 2021098236 W CN2021098236 W CN 2021098236W WO 2021254169 A1 WO2021254169 A1 WO 2021254169A1
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polyorganosiloxane
defoaming composition
silicone
reaction
composition
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PCT/CN2021/098236
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French (fr)
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杨有忠
黄伟
曹添
朱智
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江苏四新科技应用研究所股份有限公司
扬州四新新材料科技有限公司
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Publication of WO2021254169A1 publication Critical patent/WO2021254169A1/zh

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D19/00Degasification of liquids
    • B01D19/02Foam dispersion or prevention
    • B01D19/04Foam dispersion or prevention by addition of chemical substances
    • B01D19/0404Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D19/00Degasification of liquids
    • B01D19/02Foam dispersion or prevention
    • B01D19/04Foam dispersion or prevention by addition of chemical substances
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D19/00Degasification of liquids
    • B01D19/02Foam dispersion or prevention
    • B01D19/04Foam dispersion or prevention by addition of chemical substances
    • B01D19/0404Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance
    • B01D19/0409Foam dispersion or prevention by addition of chemical substances characterised by the nature of the chemical substance compounds containing Si-atoms
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/42Block-or graft-polymers containing polysiloxane sequences
    • C08G77/44Block-or graft-polymers containing polysiloxane sequences containing only polysiloxane sequences

Definitions

  • the invention relates to a method for preparing an organosilicon defoaming composition.
  • the obtained composition has excellent defoaming and suppressing properties in an anionic and non-ionic foaming system.
  • the invention belongs to the technical field of fine chemical preparations.
  • Bubbles are a common phenomenon in life and work. But in most industrial production, bubbles can bring great harm, such as reducing the efficiency of machines, delaying labor time, and affecting product quality. With the substantial increase in production scale and production efficiency of industrial enterprises, defoamers have been more widely used. At present, defoamers have been widely used in papermaking, textile printing and dyeing, petroleum extraction and refining, coatings, emulsion polymerization, sewage treatment, metal cleaning and other industries, and defoamers have become indispensable functional additives in the production process.
  • Silicone defoaming agent is currently the most widely used defoaming agent on the market.
  • Silicone defoaming composition is the core of the defoaming agent. Its defoaming speed and anti-foaming performance directly affect the performance of the final product.
  • the improvement of the antifoaming performance of the composition is the direction for the improvement of silicone defoamers.
  • the most primitive silicone defoaming composition is obtained from polydimethylsiloxane and silicon dioxide through a specific processing technology, such as the defoaming composition introduced in US4639489.
  • due to its inability to sustain foam suppression that is, its poor foam suppression performance
  • researchers at home and abroad have carried out large-scale research on its performance.
  • US4338217A1 uses alkoxy polysiloxane instead of ordinary polysiloxane to mix with silica particles to prepare a defoaming composition
  • US5824739 introduces amino polysiloxane or carboxy polysiloxane as the main body of the defoaming composition, It is mixed with silicon dioxide to obtain a defoaming composition
  • CN1931417A discloses a high temperature and strong alkali resistant defoaming agent composition, which is obtained by the cross-linking reaction of polysiloxane and silicone resin, and the composition is prepared After the emulsion is formed into the black liquor, it has good foam suppression performance, but the defoaming speed needs to be further improved.
  • US5082590 discloses a method for dissolving MQ and polyorganosiloxane through xylene, and then steaming xylene. This method has a complicated synthesis process of organosilicon defoamer, and xylene is not easy to be completely removed, which is harmful to the environment and human body. , And affect the defoaming performance of silicone defoamers.
  • the degree of cross-linking of the silicone defoaming composition is low, and the viscosity is low, the foam suppression performance is poor, but the degree of cross-linking is high, resulting in the final composition being too viscous and difficult to emulsify, and the prepared silicone defoaming composition
  • the foaming agent is also easy to precipitate bleaching oil.
  • the inventor found through a large number of experiments that on the basis of preparing high-viscosity cross-linked silicone grease, the viscosity of the cross-linked silicone grease is adjusted by introducing a capping agent, which can effectively control the degree of cross-linking and give full play to the cross-linked silicone grease.
  • Foam-suppressing performance in the late fat stage; the obtained defoaming composition has excellent defoaming speed and foam-suppressing performance in anionic and non-ionic foaming systems.
  • the purpose of the present invention is to introduce a capping agent in the process of preparing cross-linked silicone grease to effectively control the degree of cross-linking, to ensure the consistency of the viscosity of the defoaming composition, and to improve the anti-foaming composition of the silicone defoaming composition.
  • the foaming performance is convenient for the late emulsification and use of the composition.
  • the defoaming composition can be widely used to eliminate harmful foams in industrial production.
  • the method for preparing an organosilicon defoaming composition is composed of the following materials:
  • the value of a is 1.9 to 2.2.
  • the R in the molecular structure is the same or different. It includes a hydrogen atom, a monovalent substituted or unsubstituted branched or straight chain alkyl group with 1 to 20 carbon atoms, specifically Including methyl, ethyl, propyl, n-propyl, butyl, isobutyl, pentyl, hexyl, octyl, decyl, dodecyl, tetradecyl, hexadecyl, Octadecyl and eicosyl, the polyorganosiloxane has a dynamic viscosity of 1,000 to 300,000 mPa ⁇ s at 25°C.
  • the polyorganosiloxane used in the present invention is trimethylsiloxy-terminated polydimethylsiloxane; the amount of polyorganosiloxane accounts for 40-70% of the total mass of the organosilicon defoaming composition.
  • R 1 groups are the same or different, and are alkyl groups with 1 to 30 carbon atoms, including methyl, ethyl, propyl, n-propyl, butyl, and isobutyl, preferably with 1 to 10 carbon atoms; Or aryl groups with 6 to 20 carbon atoms, including phenyl and benzyl; or aralkyl groups with 7 to 20 carbon atoms; subscript m is an integer from 500 to 3000; the amount of hydroxy polyorganosiloxane It accounts for 10-40% of the total mass of the silicone defoaming composition.
  • the fine filler particles are vapor-phase hydrophobic white carbon black, with a specific surface area of 50-500 m 2 /g, preferably 90-300 m 2 /g; the amount of fine filler particles accounts for 2-8 of the total mass of the silicone defoaming composition %.
  • the said silicone resin is an MQ resin composed of R 2 3 SiO l/2 (called M unit in silicone chemistry) and SiO 4/2 (Q unit), the molar ratio between the two 0.4: 1.0 to 0.4: 1.2; the same as M units of R 2 3 SiO l / 2 R 2, or different, and the same general structure polyorganosiloxane a value of R, include hydrogen atom,
  • M unit in silicone chemistry a silicad silicad silicad silicad silicad silica
  • SiO 4/2 the molar ratio between the two 0.4: 1.0 to 0.4: 1.2
  • the same as M units of R 2 3 SiO l / 2 R 2, or different and the same general structure polyorganosiloxane a value of R, include hydrogen atom
  • the amount of the silicone resin accounts for 2-10% of the total mass of the silicone defoaming composition.
  • Basic catalyst is used to accelerate the reaction between silicone resin and polyorganosiloxane. Selected from sodium hydroxide, potassium hydroxide, cesium hydroxide, potassium methyl siliconate, sodium methyl siliconate, sodium methoxide, potassium methoxide, sodium ethoxide, potassium ethoxide, ⁇ -hydroxyethyl trimethylamine, tetramethyl Base ammonium hydroxide; the amount of the alkaline catalyst accounts for 0.01%-0.2% of the total mass of the organosilicon defoaming composition.
  • the capping agent is selected from small molecular methyl silicone oil and small molecular hydroxy silicone oil, the dynamic viscosity at 25° C. is 20-100 mPa ⁇ s, and the amount of the capping agent accounts for 2-8% of the total mass of the silicone defoaming composition.
  • a preparation method of the organosilicon defoaming composition is as follows:
  • a 0.5% (mass percentage) sodium dodecylbenzene sulfonate aqueous solution was used as the foaming medium, and the flask was shaken for testing.
  • the test method is as follows: add 50mL of the above foaming medium to a 100mL graduated cylinder, and then add 0.050g of defoaming composition, shake 50 times in the vertical direction and then stand still, and record the time T 50 for the foam to disappear to the liquid surface , Shake 50 times to record the time T 100 from which the foam disappears to the surface of the liquid, until the total number of shakes reaches 400 times.
  • the shorter the time the better the antifoaming effect of the antifoaming agent composition.
  • Table 1 The results are shown in Table 1:

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Toxicology (AREA)
  • Dispersion Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Degasification And Air Bubble Elimination (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Silicon Polymers (AREA)

Abstract

本发明提供了一种有机硅消泡组合物的制备方法,其目的是在制备交联硅脂的过程中,引入封头剂,有效地控制交联的程度,保证了消泡组合物粘度的一致性,提高了有机硅消泡组合物的消抑泡性能,便于组合物后期乳化使用。消泡组合物可广泛用于消除工业生产中的有害泡沫。

Description

一种有机硅消泡组合物的制备方法 技术领域
本发明涉及一种有机硅消泡组合物的制备方法,得到的组合物在阴离子、非离子起泡体系中有优异的消抑泡性能。本发明属于精细化工制剂技术领域。
背景技术
泡沫是生活和工作中常见的现象。但在绝大多数工业生产中泡沫会带来极大的危害,例如降低机器的工作效率、延误劳动时间、影响产品的质量等。随着工业企业生产规模和生产效率的大幅提高,消泡剂得到更加广泛的应用。目前,消泡剂已经广泛应用于造纸、纺织印染、石油开采和炼制、涂料、乳液聚合、污水处理、金属清洗等行业中,消泡剂已成为生产过程中不可缺少的功能性助剂。
有机硅消泡剂是目前市场上应用最为广泛的消泡剂,有机硅消泡组合物是消泡剂的核心,它的消泡速度和抑泡性能直接影响最终产品的性能。对于有机硅类的消泡剂而言,其组合物的消抑泡性能的改进是有机硅消泡剂的改进方向。最原始的有机硅消泡组合物是由聚二甲基硅氧烷和二氧化硅经过特定加工工艺处理得到的,如US4639489介绍的消泡剂组合物就是这样的。但是由于其不能够持久抑泡,即抑泡性能差,因此,国内外的研究人员都对其性能进行了大规模的拓展研究。US4338217A1用烷氧基聚硅氧烷代替普通聚硅氧烷与二氧化硅粒子混合处理制得消泡组合物;US5824739引入氨基聚硅氧烷或羧基聚 硅氧烷作为消泡组合物的主体,与二氧化硅混合处理得到消泡组合物;CN1931417A公开了一种耐高温耐强碱的消泡剂组合物,它是由聚硅氧烷和有机硅树脂交联反应得到的,将组合物制备成乳液后在黑液中鼓泡测试性能,其具有较好的抑泡性能,但消泡速度有待进一步提高,而且,由于消泡组合物粘度较大,分散在水中相当困难。US5082590公开了一种通过二甲苯溶解MQ和聚有机硅氧烷,然后再蒸出二甲苯,这种方法合成有机硅消泡剂的工艺复杂,而且二甲苯不易完全去除,对环境和人体有危害,并影响有机硅消泡剂消抑泡性能。
综上所述,有机硅消泡组合物的交联程度低,粘度小,则抑泡性能差,但是交联程度多高,导致最终的组合物粘度过大,不易乳化,制备的有机硅消泡剂也容易析出漂油。
本发明人通过大量的实验发现,在制备高粘度交联硅脂的基础上,通过引入封头剂来调节交联硅脂的粘度,这样既能有效控制交联程度,又充分发挥交联硅脂后期的抑泡性能;得到的消泡组合物在阴离子、非离子起泡体系中具有优良的消泡速度和抑泡性能。
发明内容
本发明的目的是在制备交联硅脂的过程中,引入封头剂,有效地控制交联的程度,保证了消泡组合物粘度的一致性,提高了有机硅消泡组合物的消抑泡性能,便于组合物后期乳化使用。消泡组合物可广泛用于消除工业生产中的有害泡沫。
技术方案
所述的一种有机硅消泡组合物的制备方法,由以下物质组成:
A、聚有机硅氧烷
聚有机硅氧烷的结构通式如下:
R aSiO (4-a)/2
其中a的取值为1.9~2.2,分子结构中的R相同或不同,它包括氢原子、一价的取代或非取代的碳原子数为1~20的支链或直链的烷基,具体包括甲基、乙基、丙基、正丙基、丁基、异丁基、戊基、己基、辛基、癸基、十二碳烷基、十四碳烷基、十六碳烷基、十八碳烷基、二十碳烷基,该聚有机硅氧烷在25℃时的动力粘度为1,000~300,000mPa·s。本发明采用的聚有机硅氧烷为三甲基硅氧基封端的聚二甲基硅氧烷;聚有机硅氧烷的用量占有机硅消泡组合物总质量的40-70%。
B、羟基聚有机硅氧烷
羟基聚有机硅氧烷的结构通式如下:
HO(SiR 1 2O) mH
式中R 1基相同或不同,为碳原子数1~30的烷基,包括甲基、乙基、丙基、正丙基、丁基、异丁基,优选碳原子数为1~10;或碳原子数为6~20的芳基,包括苯基、苯甲基;或碳原子数为7~20的芳烷基;下标m为500~3000的整数;羟基聚有机硅氧烷用量占有机硅消泡组合物总质量的10-40%。
C、精细填料颗粒
所述的精细填料颗粒是气相法疏水白炭黑,其比表面积为50~ 500m 2/g,优选90~300m 2/g;精细填料颗粒用量占有机硅消泡组合物总质量的2-8%。
D、有机硅树脂
所述的有机硅树脂为由链节R 2 3SiO l/2(有机硅化学中称为M单元)和链节SiO 4/2(Q单元)组成的MQ树脂,二者之间的摩尔比为0.4:1.0~0.4:1.2;所述的M单元R 2 3SiO l/2中的R 2相同或不同,取值和聚有机硅氧烷A的结构通式中R一致,包括氢原子、一价的取代或非取代的碳原子数为1~20的烷基,有机硅树脂用量占有机硅消泡组合物总质量的2-10%。
E、碱性催化剂
碱性催化剂是用来加快有机硅树脂和聚有机硅氧烷之间反应的。选自氢氧化钠、氢氧化钾、氢氧化铯、甲基硅醇钾、甲基硅醇钠、甲醇钠、甲醇钾、乙醇钠、乙醇钾、β-羟乙基三甲基胺、四甲基氢氧化铵;碱性催化剂用量占有机硅消泡组合物总质量0.01%-0.2%。
F、封头剂
封头剂选自小分子甲基硅油、小分子羟基硅油,在25℃时的动力粘度为20~100mPa·s,封头剂用量占有机硅消泡组合物总质量的2-8%。
一种有机硅消泡组合物的制备方法如下:
在反应容器中加入聚有机硅氧烷B、聚有机硅氧烷A和有机硅树脂D,升温至50-90℃,使之形成溶液;继续在反应容器中添加催化剂E,混合升温至60-120℃发生聚合反应,反应时间为1-4h;反应完毕后 加入精细填料粒子C、封头剂F混合均匀,在60-120℃,反应3-5h;反应完毕后,混合物在-0.01~-0.1MPa真空度下维持0.5~3h,最后,冷却到室温,得到机硅消泡组合物。
具体实施方式
实施例1
在反应容器中加入10g羟基聚有机硅氧烷HO(Si(CH 3) 2O) 500H、70g1,000mPa·s三甲基硅氧基封端的聚二甲基硅氧烷和9.99gMQ树脂(摩尔比为0.4:1.2),升温至50℃,使之形成溶液;继续在反应容器中添加0.01g氢氧化钠,混合升温至60℃发生聚合反应,反应时间为4h;反应完毕后加入8g气相法疏水白炭黑(比表面积为50m 2/g)、2g甲基硅油(20mPa·s)混合均匀,在60℃,反应5h;反应完毕后,混合物在-0.01MPa真空度下维持3h,最后,冷却到室温,得到机硅消泡组合物。
实施例2
在反应容器中加入40g羟基聚有机硅氧烷HO(Si(CH 3CH 2) 2O) 1000(Si(CH 3CH 2CH 2) 2O) 2000H、40g300,000mPa·s三甲基硅氧基封端的聚二甲基硅氧烷和9.8gMQ树脂(摩尔比为1.0:1.2),升温至90℃,使之形成溶液;继续在反应容器中添加0.2g氢氧化钾,混合升温至120℃发生聚合反应,反应时间为1h;反应完毕后加入2g气相法疏水白炭黑(比表面积为500m 2/g)、8g甲基硅油(100mPa·s)F混合均匀,在120℃,反应3h;反应完毕后,混合物在-0.1MPa真 空度下维持0.5h,最后,冷却到室温,得到机硅消泡组合物。
实施例3
在反应容器中加入30gHO(Si(C 6H 5) 2O) 50(Si(CH 3CH 2CH 2) 2O) 600H、50g20,000mPa·s三甲基硅氧基封端的聚二甲基硅氧烷和10gMQ树脂(摩尔比为0.4:0.4),升温至70℃,使之形成溶液;继续在反应容器中添加0.1g甲基硅醇钾,混合升温至100℃发生聚合反应,反应时间为2h;反应完毕后加入5.9g气相法疏水白炭黑(比表面积为90m 2/g)、4g羟基硅油(60mPa·s)混合均匀,在70℃,反应4h;反应完毕后,混合物在-0.05MPa真空度下维持2h,最后,冷却到室温,得到机硅消泡组合物。
实施例4
在反应容器中加入32gHO(Si(C 6H 5CH 3) 2O) 50(Si(CH 3CH 2CH 2) 2O) 800H、60g5,000mPa·s三甲基硅氧基封端的聚二甲基硅氧烷和2gMQ树脂(摩尔比为0.8:0.6),升温至80℃,使之形成溶液;继续在反应容器中添加0.05g甲醇钠,混合升温至90℃发生聚合反应,反应时间为3h;反应完毕后加入3g气相法疏水白炭黑(比表面积为300m 2/g)、2.95g甲基硅油(50mPa·s)混合均匀,在80℃,反应3h;反应完毕后,混合物在-0.08MPa真空度下维持2h,最后,冷却到室温,得到机硅消泡组合物。
实施例5
在反应容器中加入20gHO(Si(CH 3) 2O) 500H、65g150,000mPa·s三甲基硅氧基封端的聚二甲基硅氧烷和5gMQ树脂(摩尔比为1.0:0.8), 升温至60℃,使之形成溶液;继续在反应容器中添加0.15g四甲基氢氧化铵,混合升温至110℃发生聚合反应,反应时间为2h;反应完毕后加入5g气相法疏水白炭黑(比表面积为200m 2/g)、4.85g羟基基硅油(40mPa·s)混合均匀,在110℃,反应4h;反应完毕后,混合物在-0.06MPa真空度下维持1.5h,最后,冷却到室温,得到机硅消泡组合物。
对比例1:去掉封头剂
在反应容器中加入10g羟基聚有机硅氧烷HO(Si(CH 3) 2O) 500H、70g1,000mPa·s三甲基硅氧基封端的聚二甲基硅氧烷和9.99gMQ树脂(摩尔比为0.4:1.2),升温至50℃,使之形成溶液;继续在反应容器中添加0.01g氢氧化钠,混合升温至60℃发生聚合反应,反应时间为4h;反应完毕后加入10g气相法疏水白炭黑(比表面积为50m 2/g)混合均匀,在60℃,反应5h;反应完毕后,混合物在-0.01MPa真空度下维持3h,最后,冷却到室温,得到机硅消泡组合物。
对比例2:不形成溶液,直接混合
在反应容器中加入40g羟基聚有机硅氧烷HO(Si(CH 3CH 2) 2O) 1000(Si(CH 3CH 2CH 2) 2O) 2000H、40g300,000mPa·s三甲基硅氧基封端的聚二甲基硅氧烷和9.8gMQ树脂(摩尔比为1.0:1.2),搅拌均匀;继续在反应容器中添加0.2g氢氧化钾,混合升温至120℃发生聚合反应,反应时间为1h;反应完毕后加入2g气相法疏水白炭黑(比表面积为500m 2/g)、8g甲基硅油(100mPa·s)F混合均匀,在120℃,反应3h;反应完毕后,混合物在-0.1MPa真空度下维持 0.5h,最后,冷却到室温,得到机硅消泡组合物。
有机硅消泡组合物的性能测试
消抑泡性能对比:
以0.5%(质量百分比)的十二烷基苯磺酸钠水溶液为起泡介质,采用摇瓶方法测试。测试方法如下:往100mL具塞量筒中加入上述起泡介质50mL,然后再加入0.050g的消泡组合物,在垂直方向上摇振50次后静置,记录泡沫消至出现液面时间T 50,再摇振50次记录泡沫消至液面出现的时间T 100,直至总摇瓶次数达到400次为止,时间越短,则消泡剂组合物消抑泡效果越好。结果如表1所示:
表1 有机硅消泡组合物的消抑泡性能对比
Figure PCTCN2021098236-appb-000001

Claims (3)

  1. 一种有机硅消泡组合物的制备方法,其特征在于所述的有机硅消泡组合物由以下组分组成:
    A.聚有机硅氧烷
    聚有机硅氧烷的结构通式如下:
    R aSiO (4-a)/2
    其中a的取值为1.9~2.2,分子结构中的R相同或不同,它包括氢原子、一价的取代或非取代的碳原子数为1~20的支链或直链的烷基,具体包括甲基、乙基、丙基、正丙基、丁基、异丁基、戊基、己基、辛基、癸基、十二碳烷基、十四碳烷基、十六碳烷基、十八碳烷基、二十碳烷基,该聚有机硅氧烷在25℃时的动力粘度为1,000~300,000mPa·s,所述的聚有机硅氧烷为三甲基硅氧基封端的聚二甲基硅氧烷;聚有机硅氧烷的用量占有机硅消泡组合物总质量的40-70%;
    B、羟基聚有机硅氧烷
    羟基聚有机硅氧烷的结构通式如下:
    HO(SiR 1 2O) mH
    式中R 1基相同或不同,为碳原子数1~30的烷基,包括甲基、乙基、丙基、正丙基、丁基、异丁基;或碳原子数为6~20的芳基,包括苯基、苯甲基;或碳原子数为7~20的芳烷基;下标m为500~3000的整数;羟基聚有机硅氧烷用量占有机硅消泡组合物总质量的10-40%;
    C、精细填料颗粒
    所述的精细填料颗粒是气相法疏水白炭黑,其比表面积为50~500m 2/g,精细填料颗粒用量占有机硅消泡组合物总质量的2-8%;
    D、有机硅树脂
    所述的有机硅树脂为由链节R 2 3SiO l/2(有机硅化学中称为M单元)和链节SiO 4/2(Q单元)组成的MQ树脂,二者之间的摩尔比为0.4:1.0~0.4:1.2;所述的M单元R 2 3SiO l/2中的R 2相同或不同,取值和聚有机硅氧烷A的结构通式中R一致,包括氢原子、一价的取代或非取代的碳原子数为1~20的烷基,有机硅树脂用量占有机硅消泡组合物总质量的2-10%;
    E、碱性催化剂
    碱性催化剂是用来加快有机硅树脂和聚有机硅氧烷之间反应的;选自氢氧化钠、氢氧化钾、氢氧化铯、甲基硅醇钾、甲基硅醇钠、甲醇钠、甲醇钾、乙醇钠、乙醇钾、β-羟乙基三甲基胺、四甲基氢氧化铵;碱性催化剂用量占有机硅消泡组合物总质量0.01%-0.2%;
    F、封头剂
    封头剂选自小分子甲基硅油、小分子羟基硅油,在25℃时的动力粘度为20~100mPa·s,封头剂用量占有机硅消泡组合物总质量的2-8%
    所述的有机硅消泡组合物的制备方法,具体操作步骤为:
    在反应容器中加入聚有机硅氧烷B、聚有机硅氧烷A和有机硅树脂D,升温至50-90℃,使之形成溶液;继续在反应容器中添加催化剂E, 混合升温至60-120℃发生聚合反应,反应时间为1-4h;反应完毕后加入精细填料粒子C、封头剂F混合均匀,在60-120℃,反应3-5h;反应完毕后,混合物在-0.01~-0.1MPa真空度下维持0.5~3h,最后,冷却到室温,得到机硅消泡组合物。
  2. 根据权利要求1所述的一种有机硅消泡组合物的制备方法,其特征在于所述的羟基聚有机硅氧烷中R 1为烷基时,优选碳原子数为1~10。
  3. 根据权利要求1所述的一种有机硅消泡组合物的制备方法,其特征在于所述的精细填料颗粒比表面积优选90~300m 2/g。
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