JP4568418B2 - Method for producing organopolysiloxane - Google Patents
Method for producing organopolysiloxane Download PDFInfo
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- JP4568418B2 JP4568418B2 JP2000328497A JP2000328497A JP4568418B2 JP 4568418 B2 JP4568418 B2 JP 4568418B2 JP 2000328497 A JP2000328497 A JP 2000328497A JP 2000328497 A JP2000328497 A JP 2000328497A JP 4568418 B2 JP4568418 B2 JP 4568418B2
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- organopolysiloxane
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Description
【０００１】
【発明の属する技術分野】
本発明は、オルガノポリシロキサンの製造方法に関し、詳しくは、線状または環状のオルガノ(ポリ)シロキサンを酸活性固体触媒を用いて増粘ないし重合させたオルガノポリシロキサンの経時での増粘、ゲル化を抑制することができる、オルガノポリシロキサンの製造方法に関する。
【０００２】
【従来の技術】
線状または環状のオルガノ(ポリ)シロキサンを酸活性固体触媒を用いて増粘ないし重合させてオルガノポリシロキサンを製造する方法は周知である(特公昭５６−２６２４８号公報、および特公昭６３−１４０１５号公報参照)。酸活性固体触媒を濾別することにより、得られるオルガノポリシロキサンの増粘を停止することができる。
【０００３】
しかしながら、本発明者らは、得られるオルガノポリシロキサンが経時的に増粘、あるいはゲル化してしまうという問題があることに気付いた。特に、ケイ素原子結合水素原子を有するオルガノ(ポリ)シロキサンを酸活性固体触媒を用いて増粘させたオルガノポリシロキサンは経時での増粘、ゲル化が著しいという問題があることに気付いた。
【０００４】
【発明が解決しようとする課題】
本発明者らは、上記の課題を解決するために鋭意検討した結果、本発明に到達した。
すなわち、本発明の目的は、線状または環状のオルガノ(ポリ)シロキサンを酸活性固体触媒を用いて増粘ないし重合させたオルガノポリシロキサンの経時での増粘、ゲル化を抑制することができる、オルガノポリシロキサンの製造方法を提供することにある。
【０００５】
【課題を解決するための手段】
本発明のオルガノポリシロキサンの製造方法は、線状または環状のオルガノ（ポリ）シロキサンを酸活性固体触媒を用いて増粘ないし重合させた後、酸活性固体触媒とオルガノポリシロキサンとの混合物に、平均孔径が１〜１００Åであり、気孔率が４０〜７０％である少なくとも１種のゼオライト系固体吸着剤を、オルガノポリシロキサン１００重量部に対して０.５〜２０重量部となる量添加した後、該吸着剤および酸活性固体触媒を濾別することを特徴とする。
【０００６】
【発明の実施の形態】
本発明のオルガノポリシロキサンの製造方法を詳細に説明する。
本発明のオルガノポリシロキサンの製造方法では、線状または環状のオルガノ(ポリ)シロキサンを酸活性固体触媒を用いて増粘ないし重合させる。この線状または環状のオルガノ(ポリ)シロキサンとしては、分子鎖両末端シラノール基封鎖ジメチルシロキサンオリゴマー、分子鎖両末端トリメチルシロキシ基封鎖ジメチルシロキサンオリゴマー等のジメチルシロキサンオリゴマー、あるいはこれらのジメチルシロキサンオリゴマーのメチル基の一部を水素原子；エチル基、プロピル基、tert−ブチル基、２−エチルヘキシル基、ドデシル基、オクタデシル基等のアルキル基；ビニル基、アリル基、ヘキセニル基等のアルケニル基；フェニル基、ナフチル基等のアリール基；クロルメチル基、３,３,３−トリフルオロプロピル基、３,３,４,４,５,５,５−ヘプタフルオロペンチル基、ジフルオロモノクロルプロピル基等のハロゲン化アルキル基等で置換した線状のオルガノシロキサンオリゴマー；分子鎖両末端シラノール基封鎖ジメチルポリシロキサン、分子鎖両末端トリメチルシロキシ基封鎖ジメチルポリシロキサン等のジメチルポリシロキサン、あるいはこれらのジメチルポリシロキサンのメチル基の一部を前記と同様の原子または基で置換した線状のオルガノポリシロキサン；オクタメチルシクロテトラシロキサン、デカメチルシクロペンタシロキサン等のジメチルシクロシロキサンオリゴマー、あるいはこれらのジメチルシクロシロキサンオリゴマーのメチル基の一部を前記と同様の原子または基で置換した環状のオルガノシロキサンオリゴマーが例示される。特に、本発明の製造方法では、ケイ素原子結合水素原子を有するオルガノ(ポリ)シロキサンを増粘ないし重合させた後、経時的な増粘、ゲル化を著しく抑制することができるので好ましい。
【０００７】
また、酸活性固体触媒としては、日本活性白土社製のＫ−５００、トンシル社製のトンシルＡＣ、フィルトロール社製のフィルトロール ウルトラ等で知られている酸活性白土；その他、酸活性ケイ酸アルミニウム、酸活性活性炭が例示される。
【０００８】
本発明の製造方法では、上記の線状または環状のオルガノ(ポリ)シロキサンと上記の酸活性固体触媒を攪拌下、通常、６０℃〜１００℃の温度で４〜２４時間加熱することにより、上記のオルガノ(ポリ)シロキサンを増粘ないし重合させることができる。
【０００９】
本発明の製造方法では、前記の酸活性固体触媒とオルガノポリシロキサンとの混合物に前記のゼオライト系固体吸着剤を添加することを特徴とする。このゼオライト系固体吸着剤は、オルガノポリシロキサンの経時での増粘、ゲル化を抑制するためのものであり、ペレット、ビーズ、メッシュ、パウダー等の形状を有するものを用いることができる。このゼオライト系固体吸着剤としては、天然のゼオライトや合成のゼオライトが例示される。このようなゼオライト系固体吸着剤は平均孔径が１〜１００Åであり、このゼオライト系固体吸着剤の気孔率が４０〜７０％である。
【００１０】
本発明の製造方法において、上記のゼオライト系固体吸着剤の添加量は、オルガノポリシロキサン１００重量部に対して０.５〜２０重量部であり、特に、１.０〜２０重量部であることが好ましい。これは、ゼオライト系固体吸着剤の添加量が上記範囲の下限未満であると、得られるオルガノポリシロキサンの経時的な増粘、ゲル化を十分に抑制することができなくなるおそれがあるからであり、一方、上記範囲の上限をこえても著しい効果を奏することができないからである。
【００１１】
本発明の製造方法では、上記のゼオライト系固体吸着剤は、得られるオルガノポリシロキサンから濾別することが必要である。さらに、必要に応じて、得られるオルガノポリシロキサンから低揮発成分を留去してもよい。このようにして得られたオルガノポリシロキサンは、貯蔵中に著しく増粘したり、あるいはゲル化することがないという特徴がある。また、このようにして得られたケイ素原子結合水素原子を有するオルガノポリシロキサンは、ヒドロシリル化反応硬化型オルガノポリシロキサン組成物の架橋剤、特には、剥離性硬化皮膜形成用のヒドロシリル化反応硬化型オルガノポリシロキサン組成物の架橋剤として有用である。
【００１２】
【実施例】
本発明のオルガノポリシロキサンの製造方法を実施例により説明する。なお、オルガノポリシロキサンの粘度は２５℃において、回転型粘度計ビスメトロンＶＡ型により、ローターNo.１を用いて１２rpmにおいて測定した値である。
【００１３】
［実施例１］
２００Ｌの反応釜に、粘度２０mPa・sの分子鎖両末端トリメチルシロキシ基封鎖メチルハイドロジェンポリシロキサン１４０kg、および酸活性固体触媒(日本活性白土社製のＫ−５００)４kgを仕込み、窒素でバブリングしながら均一に混合し、８０〜９０℃で１９.５時間攪拌した。次に、これを冷却し、平均孔径４Å、気孔率５２％、平均粒径１.６mmのペレット状のゼオライト系固体吸着剤９.８kgを仕込み、２時間攪拌した後、フィルタープレスにて濾過した。得られたオルガノポリシロキサンの濾過直後の粘度、および室温で５ヵ月放置した後の粘度を測定し、それらの結果を表１に示した。
【００１４】
［実施例２］
２００Ｌの反応釜に、粘度２０mPa・sの分子鎖両末端トリメチルシロキシ基封鎖メチルハイドロジェンポリシロキサン１４０kg、および酸活性固体触媒(日本活性白土社製のＫ−５００)４kgを仕込み、窒素でバブリングしながら均一に混合し、８０〜９０℃で１９.５時間攪拌した。次に、これを冷却し、平均孔径４Å、気孔率５１％、平均粒径３mmのペレット状ゼオライト系固体吸着剤９.８kgを仕込み、２時間攪拌した後、フィルタープレスにて濾過した。得られたオルガノポリシロキサンの濾過直後の粘度、および室温で５ヵ月放置した後の粘度を測定し、それらの結果を表１に示した。
【００１５】
［実施例３］
２００Ｌの反応釜に、粘度２０mPa・sの分子鎖両末端トリメチルシロキシ基封鎖メチルハイドロジェンポリシロキサン１１２kg、および酸活性固体触媒(日本活性白土社製のＫ−５００)３kgを仕込み、窒素でバブリングしながら均一に混合し、７８〜８０℃で７時間攪拌した。次に、これを冷却し、平均孔径１０Å、気孔率４５％、平均粒径１０μｍのパウダー状ゼオライト系固体吸着剤３kgを仕込み、２時間攪拌した後、フィルタープレスにて濾過した。得られたオルガノポリシロキサンの濾過直後の粘度、および室温で５ヵ月放置した後の粘度を測定し、それらの結果を表１に示した。
【００１６】
［比較例１］
２００Ｌの反応釜に、粘度２０mPa・sの分子鎖両末端トリメチルシロキシ基封鎖メチルハイドロジェンポリシロキサン１４０kg、および酸活性固体触媒(日本活性白土社製のＫ−５００)４kgを仕込み、窒素でバブリングしながら均一に混合し、８０〜９０℃で１９.５時間攪拌した。次に、これを冷却し、フィルタープレスにて濾過した。得られたオルガノポリシロキサンの濾過直後の粘度、および室温で５ヵ月放置した後の粘度を測定し、それらの結果を表１に示した。
【００１７】
［比較例２］
２００Ｌの反応釜に、粘度２０mPa・sの分子鎖両末端トリメチルシロキシ基封鎖メチルハイドロジェンポリシロキサン１１０kg、および酸活性固体触媒(日本活性白土社製のＫ−５００)３kgを仕込み、窒素でバブリングしながら均一に混合し、８０〜９０℃で７時間攪拌した。次に、これを冷却し、微粒子状の炭酸カルシウム８kgを仕込み、２時間攪拌した後、フィルタープレスにて濾過した。得られたオルガノポリシロキサンの濾過直後の粘度、および室温で５ヵ月放置した後の粘度を測定し、それらの結果を表１に示した。
【００１８】
［比較例３］
２００Ｌの反応釜に、粘度２０mPa・sの分子鎖両末端トリメチルシロキシ基封鎖メチルハイドロジェンポリシロキサン１４０kg、および酸活性固体触媒(日本活性白土社製のＫ−５００)４kgを仕込み、窒素でバブリングしながら均一に混合し、８０〜９０℃で１９.５時間攪拌した。次に、これを冷却し、ケイソウ土(昭和電工社製のラジオライト９００)５kgを仕込み、２時間攪拌した後、フィルタープレスにて濾過した。得られたオルガノポリシロキサンの濾過直後の粘度、および室温で５ヵ月放置した後の粘度を測定し、それらの結果を表１に示した。
【００１９】
【表１】
【発明の効果】
本発明のオルガノポリシロキサンの製造方法は、線状または環状のオルガノ(ポリ)シロキサンを酸活性固体触媒を用いて増粘ないし重合させたオルガノポリシロキサンの経時での増粘、ゲル化を抑制することができるという特徴がある。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for producing an organopolysiloxane, and more specifically, thickening or gelling of an organopolysiloxane obtained by thickening or polymerizing a linear or cyclic organo (poly) siloxane using an acid active solid catalyst. The present invention relates to a method for producing an organopolysiloxane capable of suppressing the conversion.
[0002]
[Prior art]
Methods for producing organopolysiloxanes by thickening or polymerizing linear or cyclic organo (poly) siloxanes using an acid-active solid catalyst are well known (Japanese Patent Publication No. 56-26248 and Japanese Patent Publication No. 63-14015). Issue gazette). The thickening of the resulting organopolysiloxane can be stopped by filtering off the acid active solid catalyst.
[0003]
However, the present inventors have found that there is a problem that the resulting organopolysiloxane thickens or gels over time. In particular, it has been found that organopolysiloxanes obtained by thickening organo (poly) siloxanes having silicon-bonded hydrogen atoms using an acid-active solid catalyst have a problem of significant thickening and gelation over time.
[0004]
[Problems to be solved by the invention]
As a result of intensive studies to solve the above problems, the present inventors have reached the present invention.
That is, an object of the present invention is to suppress thickening and gelation of organopolysiloxane obtained by thickening or polymerizing linear or cyclic organo (poly) siloxane using an acid active solid catalyst over time. Another object of the present invention is to provide a method for producing an organopolysiloxane.
[0005]
[Means for Solving the Problems]
In the method for producing an organopolysiloxane of the present invention, a linear or cyclic organo (poly) siloxane is thickened or polymerized using an acid active solid catalyst, and then mixed into an acid active solid catalyst and organopolysiloxane mixture . At least one zeolitic solid adsorbent having an average pore diameter of 1 to 100 mm and a porosity of 40 to 70% was added in an amount of 0.5 to 20 parts by weight with respect to 100 parts by weight of the organopolysiloxane . Thereafter, the adsorbent and the acid active solid catalyst are filtered off.
[0006]
DETAILED DESCRIPTION OF THE INVENTION
The production method of the organopolysiloxane of the present invention will be described in detail.
In the method for producing an organopolysiloxane of the present invention, a linear or cyclic organo (poly) siloxane is thickened or polymerized using an acid active solid catalyst. Examples of the linear or cyclic organo (poly) siloxane include dimethylsiloxane oligomers such as silanol group-capped dimethylsiloxane oligomers at both ends of the molecular chain, trimethylsiloxy group-capped dimethylsiloxane oligomers at both ends of the molecular chain, and methyls of these dimethylsiloxane oligomers. A part of the group is a hydrogen atom; an alkyl group such as an ethyl group, a propyl group, a tert-butyl group, a 2-ethylhexyl group, a dodecyl group or an octadecyl group; an alkenyl group such as a vinyl group, an allyl group or a hexenyl group; a phenyl group; Aryl groups such as naphthyl group; halogenated alkyl groups such as chloromethyl group, 3,3,3-trifluoropropyl group, 3,3,4,4,5,5,5-heptafluoropentyl group, difluoromonochloropropyl group Linear organosiloxane oligomer substituted with Dimethylpolysiloxane blocked with silanol groups at both ends of the molecular chain, dimethylpolysiloxane blocked with trimethylsiloxy groups at both ends of the molecular chain, or a part of the methyl groups of these dimethylpolysiloxanes replaced with the same atoms or groups as described above Linear organopolysiloxane; dimethylcyclosiloxane oligomers such as octamethylcyclotetrasiloxane and decamethylcyclopentasiloxane, or a part of methyl groups of these dimethylcyclosiloxane oligomers were substituted with the same atoms or groups as described above Examples are cyclic organosiloxane oligomers. In particular, the production method of the present invention is preferable because it is possible to remarkably suppress the thickening and gelation with time after the organo (poly) siloxane having a silicon atom-bonded hydrogen atom is thickened or polymerized.
[0007]
Examples of the acid active solid catalyst include acid activated clay known as K-500 manufactured by Nippon Active White Co., Ltd., Tonsil AC manufactured by Tonsil Co., Ltd., Filtrol Ultra manufactured by Filtrol Co., etc .; Aluminum and acid activated activated carbon are exemplified.
[0008]
In the production method of the present invention, the above linear or cyclic organo (poly) siloxane and the above acid active solid catalyst are usually heated at a temperature of 60 ° C. to 100 ° C. for 4 to 24 hours with stirring. The organo (poly) siloxane can be thickened or polymerized.
[0009]
In the production method of the present invention, it is characterized by adding the zeolitic solid adsorbent to the mixture of the previous SL acid-active solid catalyst and an organopolysiloxane. This zeolitic solid adsorbent is for suppressing thickening and gelation of organopolysiloxane over time, and may be one having a shape such as pellets, beads, meshes, and powders. Examples of the zeolitic solid adsorbent include natural zeolite and synthetic zeolite. Such zeolitic solid adsorbent is flat Hitoshiana径is Ri 1~100Å der, Ru porosity of the zeolite solid adsorbent 4 0% to 70% der.
[0010]
In the production method of the present invention, the addition amount of the zeolitic solid adsorbent is Ri from 0.5 to 20 parts by weight der against 100 parts by weight of an organopolysiloxane, in particular, is 1.0 to 20 parts by weight It is preferable. This is because if the addition amount of the zeolitic solid adsorbent is less than the lower limit of the above range, the resulting organopolysiloxane may not be sufficiently thickened or gelled over time. On the other hand, even if the upper limit of the above range is exceeded, a remarkable effect cannot be obtained.
[0011]
In the production method of the present invention, the above zeolitic solid adsorbent needs to be separated from the resulting organopolysiloxane. Furthermore, you may distill a low volatile component from the obtained organopolysiloxane as needed. The organopolysiloxane thus obtained has a characteristic that it does not significantly thicken or gel during storage. The organopolysiloxane having silicon-bonded hydrogen atoms thus obtained is a crosslinking agent for a hydrosilylation reaction-curable organopolysiloxane composition, particularly a hydrosilylation reaction-curable type for forming a peelable cured film. It is useful as a cross-linking agent for organopolysiloxane compositions.
[0012]
【Example】
The production method of the organopolysiloxane of the present invention will be described with reference to examples. The viscosity of the organopolysiloxane is a value measured at 12 rpm using a rotor No. 1 at 25 ° C. with a rotational viscometer bismetron VA type.
[0013]
[Example 1]
A 200-liter reaction kettle is charged with 140 kg of methyl hydrogen polysiloxane blocked with both ends of a molecular chain with a viscosity of 20 mPa · s and 4 kg of an acid-active solid catalyst (K-500, manufactured by Nippon Kaohaku Soil Co., Ltd.), and bubbled with nitrogen. Then, the mixture was uniformly mixed and stirred at 80 to 90 ° C. for 19.5 hours. Next, this was cooled, charged with 9.8 kg of a pellet-shaped zeolite solid adsorbent having an average pore diameter of 4 mm, a porosity of 52%, and an average particle diameter of 1.6 mm, stirred for 2 hours, and then filtered with a filter press. . The viscosity of the resulting organopolysiloxane immediately after filtration and the viscosity after standing at room temperature for 5 months were measured, and the results are shown in Table 1.
[0014]
[Example 2]
A 200-liter reaction kettle is charged with 140 kg of methyl hydrogen polysiloxane blocked with both ends of a molecular chain with a viscosity of 20 mPa · s and 4 kg of an acid-active solid catalyst (K-500, manufactured by Nippon Kaohaku Soil Co., Ltd.), and bubbled with nitrogen. Then, the mixture was uniformly mixed and stirred at 80 to 90 ° C. for 19.5 hours. Next, this was cooled, charged with 9.8 kg of a pellet-shaped zeolite solid adsorbent having an average pore diameter of 4 mm, a porosity of 51%, and an average particle diameter of 3 mm, stirred for 2 hours, and filtered with a filter press. The viscosity of the resulting organopolysiloxane immediately after filtration and the viscosity after standing at room temperature for 5 months were measured, and the results are shown in Table 1.
[0015]
[Example 3]
A 200 L reaction kettle is charged with 112 kg of trimethylsiloxy group-blocked methylhydrogenpolysiloxane having a viscosity of 20 mPa · s and 3 kg of an acid active solid catalyst (K-500, manufactured by Nippon Active Shiratosha), and bubbled with nitrogen. The mixture was mixed uniformly and stirred at 78-80 ° C. for 7 hours. Next, this was cooled, charged with 3 kg of a powdery zeolite solid adsorbent having an average pore size of 10 mm, a porosity of 45%, and an average particle size of 10 μm, stirred for 2 hours, and then filtered with a filter press. The viscosity of the resulting organopolysiloxane immediately after filtration and the viscosity after standing at room temperature for 5 months were measured, and the results are shown in Table 1.
[0016]
[Comparative Example 1]
A 200-liter reaction kettle is charged with 140 kg of methyl hydrogen polysiloxane blocked with both ends of a molecular chain with a viscosity of 20 mPa · s and 4 kg of an acid-active solid catalyst (K-500, manufactured by Nippon Kaohaku Soil Co., Ltd.), and bubbled with nitrogen. Then, the mixture was uniformly mixed and stirred at 80 to 90 ° C. for 19.5 hours. Next, this was cooled and filtered with a filter press. The viscosity of the resulting organopolysiloxane immediately after filtration and the viscosity after standing at room temperature for 5 months were measured, and the results are shown in Table 1.
[0017]
[Comparative Example 2]
A 200-liter reaction kettle is charged with 110 kg of both ends of a trimethylsiloxy group-blocked methylhydrogenpolysiloxane having a viscosity of 20 mPa · s, and 3 kg of an acid-active solid catalyst (K-500, manufactured by Nippon Active Shiratosha), and bubbled with nitrogen. The mixture was uniformly mixed while stirring at 80 to 90 ° C. for 7 hours. Next, this was cooled, charged with 8 kg of fine particle calcium carbonate, stirred for 2 hours, and then filtered with a filter press. The viscosity of the resulting organopolysiloxane immediately after filtration and the viscosity after standing at room temperature for 5 months were measured, and the results are shown in Table 1.
[0018]
[Comparative Example 3]
A 200-liter reaction kettle is charged with 140 kg of methyl hydrogen polysiloxane blocked with both ends of a molecular chain with a viscosity of 20 mPa · s and 4 kg of an acid-active solid catalyst (K-500, manufactured by Nippon Kaohaku Soil Co., Ltd.), and bubbled with nitrogen. Then, the mixture was uniformly mixed and stirred at 80 to 90 ° C. for 19.5 hours. Next, this was cooled, charged with 5 kg of diatomaceous earth (Radiolite 900 manufactured by Showa Denko KK), stirred for 2 hours, and then filtered with a filter press. The viscosity of the resulting organopolysiloxane immediately after filtration and the viscosity after standing at room temperature for 5 months were measured, and the results are shown in Table 1.
[0019]
[Table 1]
【The invention's effect】
The method for producing an organopolysiloxane of the present invention suppresses thickening and gelation of an organopolysiloxane obtained by thickening or polymerizing a linear or cyclic organo (poly) siloxane using an acid active solid catalyst over time. There is a feature that can be.
Claims (3)
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| JP2000328497A JP4568418B2 (en) | 1999-11-25 | 2000-10-27 | Method for producing organopolysiloxane |
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| JP33441699 | 1999-11-25 | ||
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| JP2000328497A JP4568418B2 (en) | 1999-11-25 | 2000-10-27 | Method for producing organopolysiloxane |
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| EP2980122B1 (en) * | 2013-03-29 | 2018-08-08 | Idemitsu Kosan Co., Ltd | Polyorganosiloxane production method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US3853934A (en) * | 1974-01-14 | 1974-12-10 | Gen Electric | Continuous process for producing polysiloxane oils |
| JPS62227930A (en) * | 1986-03-28 | 1987-10-06 | ワツカ−−ケミ−・ゲゼルシヤフト・ミツト・ベシユレンクテル・ハフツング | Method for continuously changing molecular weight of linear or cyclic organo(poly)siloxane |
| DE3727182A1 (en) * | 1987-08-14 | 1989-02-23 | Wacker Chemie Gmbh | PRODUCTION AND PROCESSING OF MIXTURES WITH A HIGH CONTENT OF ORGANOCYCLOSILOXANES |
| US5276173A (en) * | 1992-10-05 | 1994-01-04 | Dow Corning Corporation | Method for removal for ionic chloride from hydroxyl-terminated siloxanes |
| DE4422813A1 (en) * | 1994-06-29 | 1996-01-04 | Wacker Chemie Gmbh | Process for stabilizing organpolysiloxanes |
| JPH08319352A (en) * | 1995-05-25 | 1996-12-03 | Toray Dow Corning Silicone Co Ltd | Purification of organopolysiloxane |
| JPH09324052A (en) * | 1996-04-03 | 1997-12-16 | Sumitomo Chem Co Ltd | Silicon resin manufacturing method, silicon resin and coating liquid for forming insulating film |
| JPH10298289A (en) * | 1997-04-25 | 1998-11-10 | Mitsubishi Chem Corp | Method for producing siloxane polymer |
| JP3703254B2 (en) * | 1997-06-19 | 2005-10-05 | ジーイー東芝シリコーン株式会社 | Method for producing Si-H bond-containing cyclic methylsiloxane oligomer |
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