JPS6034574B2 - Method for producing organosilicon polymer - Google Patents
Method for producing organosilicon polymerInfo
- Publication number
- JPS6034574B2 JPS6034574B2 JP12150877A JP12150877A JPS6034574B2 JP S6034574 B2 JPS6034574 B2 JP S6034574B2 JP 12150877 A JP12150877 A JP 12150877A JP 12150877 A JP12150877 A JP 12150877A JP S6034574 B2 JPS6034574 B2 JP S6034574B2
- Authority
- JP
- Japan
- Prior art keywords
- siloxysilanol
- water
- liquid
- organosilicon
- zeolite
- Prior art date
- Legal status (The legal status 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 status listed.)
- Expired
Links
- 229920001558 organosilicon polymer Polymers 0.000 title claims description 5
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 150000003961 organosilicon compounds Chemical class 0.000 claims description 5
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 239000010457 zeolite Substances 0.000 description 12
- 229910021536 Zeolite Inorganic materials 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 11
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 11
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 10
- 235000019353 potassium silicate Nutrition 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 4
- 239000003208 petroleum Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 2
- BYLOHCRAPOSXLY-UHFFFAOYSA-N dichloro(diethyl)silane Chemical compound CC[Si](Cl)(Cl)CC BYLOHCRAPOSXLY-UHFFFAOYSA-N 0.000 description 2
- 239000010436 fluorite Substances 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- POWFTOSLLWLEBN-UHFFFAOYSA-N tetrasodium;silicate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-][Si]([O-])([O-])[O-] POWFTOSLLWLEBN-UHFFFAOYSA-N 0.000 description 2
- 239000005051 trimethylchlorosilane Substances 0.000 description 2
- WNEODWDFDXWOLU-QHCPKHFHSA-N 3-[3-(hydroxymethyl)-4-[1-methyl-5-[[5-[(2s)-2-methyl-4-(oxetan-3-yl)piperazin-1-yl]pyridin-2-yl]amino]-6-oxopyridin-3-yl]pyridin-2-yl]-7,7-dimethyl-1,2,6,8-tetrahydrocyclopenta[3,4]pyrrolo[3,5-b]pyrazin-4-one Chemical compound C([C@@H](N(CC1)C=2C=NC(NC=3C(N(C)C=C(C=3)C=3C(=C(N4C(C5=CC=6CC(C)(C)CC=6N5CC4)=O)N=CC=3)CO)=O)=CC=2)C)N1C1COC1 WNEODWDFDXWOLU-QHCPKHFHSA-N 0.000 description 1
- 235000003392 Curcuma domestica Nutrition 0.000 description 1
- 244000008991 Curcuma longa Species 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- JEWHCPOELGJVCB-UHFFFAOYSA-N aluminum;calcium;oxido-[oxido(oxo)silyl]oxy-oxosilane;potassium;sodium;tridecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.O.[Na].[Al].[K].[Ca].[O-][Si](=O)O[Si]([O-])=O JEWHCPOELGJVCB-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- DMEXFOUCEOWRGD-UHFFFAOYSA-N chloro-[chloro(dimethyl)silyl]oxy-dimethylsilane Chemical compound C[Si](C)(Cl)O[Si](C)(C)Cl DMEXFOUCEOWRGD-UHFFFAOYSA-N 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 235000003373 curcuma longa Nutrition 0.000 description 1
- QFLLWLFOOHGSBE-UHFFFAOYSA-N dichloro-methyl-trimethylsilyloxysilane Chemical compound C[Si](C)(C)O[Si](C)(Cl)Cl QFLLWLFOOHGSBE-UHFFFAOYSA-N 0.000 description 1
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 229910001683 gmelinite Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 229910001723 mesolite Inorganic materials 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910001743 phillipsite Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- WVMSIBFANXCZKT-UHFFFAOYSA-N triethyl(hydroxy)silane Chemical compound CC[Si](O)(CC)CC WVMSIBFANXCZKT-UHFFFAOYSA-N 0.000 description 1
- AAPLIUHOKVUFCC-UHFFFAOYSA-N trimethylsilanol Chemical compound C[Si](C)(C)O AAPLIUHOKVUFCC-UHFFFAOYSA-N 0.000 description 1
- 235000013976 turmeric Nutrition 0.000 description 1
Landscapes
- Silicon Polymers (AREA)
Description
【発明の詳細な説明】
本発明はシロキシシラノールとオルガノシリル化剤との
反応による溌水性に富む有機珪素化合物の製造方法に関
する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing an organosilicon compound with high water repellency by reacting a siloxysilanol with an organosilylating agent.
従来シロキシシラノールとオルガノシリル化剤との反応
による有機珪素化合物は、特開昭５１一１２２１９８号
公報、特公階４９一４０６３ｙ号公報に示される方法で
合成されている。Conventionally, organosilicon compounds obtained by the reaction of siloxysilanol and an organosilylating agent have been synthesized by the method shown in Japanese Patent Application Laid-Open No. 51-122198 and Japanese Patent Publication No. 49-4063y.
これらの方法による生成物はいずれもガラス状の固形物
であるから、その利用範囲は著しく制限されている。例
えば、熱媒、潤滑油等の油状物質としての使用は不可能
である。本発明は上記公知の有機珪素重合体の製造方法
の欠点をを解消するために開発されたもので液状で低粘
度の有機珪素重合体を製造することを目的とする。Since the products produced by these methods are all glass-like solids, their range of use is severely limited. For example, it cannot be used as an oily substance such as a heating medium or lubricating oil. The present invention was developed to overcome the drawbacks of the above-mentioned known methods for producing organosilicon polymers, and its object is to produce a liquid, low-viscosity organosilicon polymer.
すなわち、本発明は水ガラスとかゼオラィトのようなシ
ロキシシラノールを鉱酸、水、水に可溶な有機溶剤およ
びオルガノシリル化剤からなる混合水溶液中に高速櫨辞
しながら徐々に添加し反応させることにより液状で低粘
度の有機珪素化合物を製造する方法を提供する。That is, the present invention involves gradually adding and reacting siloxysilanol such as water glass or zeolite to a mixed aqueous solution consisting of a mineral acid, water, a water-soluble organic solvent, and an organosilylation agent while stirring at high speed. A method for producing a liquid, low viscosity organosilicon compound is provided.
本発明に用いられる水に可溶な有機溶剤としては、通常
エーテル類、アルコール類、ケトン類等が用いられる。As the water-soluble organic solvent used in the present invention, ethers, alcohols, ketones, etc. are usually used.
具体例としては次のものがあげられる。メチルアルコー
ル、エチルアルコール、インプロピルアルコール、アセ
トン、メチルエーナル等である。シロキシシラソールと
しては、通常水ガラスもしくはゼオラィトを用いる。Specific examples include: These include methyl alcohol, ethyl alcohol, inpropyl alcohol, acetone, and methyl enal. As siloxysilazole, water glass or zeolite is usually used.
水ガラスは望ましくは〆タ珪酸ソーダ、オルソ珪酸ソー
ダ等低モル比のものが望ましいが、これらの限定される
ものではなく、ＪＩＳＩ号、ＪＩＳ２号、ＪＩＳ３号等
も有効である。シロキシシラノール源として、水ガラス
の他にその基本構造が低重合度のシロキサンから成るゼ
オラィトを用いる。本発明に用いるゼオラィトとしては
、下記の一般式で表わされる物質が有効である。（一般
式）
（ＭＬ ＭＯ）○・山２０３・ｎＳｉ０２・ｍＨ２０ｎ
：０くｎミ３の実数ｍ：正の実数
ＭＩ：１価の金属イオン
Ｍロ：２価の金属イオン
具体的には、ホウフツ石、ワィカラィト、ホージヤサイ
ト、リヨウフツ石、グメリナイト、オフレタイト、レビ
ナイト、メソライト、スコレサイト、トムソナイト、エ
ジングトナイト、ゴナルダイト、ジュウジフッ石、フィ
リップサイト、ジスモンドフッ石、菱フッ石、濁フッ石
、等の天然ゼオライトの他のゼオライトＸ、ゼオライト
Ｙ、ゼオラィトＡ、ゼオラィトＬ等の合成ゼオラィー・
用いられる。The water glass is preferably one with a low molar ratio such as sodium silicate or sodium orthosilicate, but is not limited to these, and JIS No. 2, JIS No. 2, JIS No. 3, etc. are also effective. As a siloxysilanol source, in addition to water glass, zeolite whose basic structure is composed of siloxane with a low degree of polymerization is used. As the zeolite used in the present invention, substances represented by the following general formula are effective. (General formula) (ML MO) ○・mountain 203・nSi02・mH20n
: 0 k n m 3 real number m : positive real number MI : monovalent metal ion M b : divalent metal ion Specifically, borovite, waicalite, hojiasite, leopardite, gmelinite, offretite, levinite, mesolite Synthesis of other natural zeolites such as , scolesite, thomsonite, edgingtonite, gonaldite, sedumite, phillipsite, jismundite, rhodofluorite, turbidite, etc., as well as zeolite X, zeolite Y, zeolite A, zeolite L, etc. Xeoray
used.
オルガノシリル化剤としては下記の一般式で表わされる
物質が有効である。As the organosilylating agent, substances represented by the following general formula are effective.
（一般式）
ＳＩＲｎＸ４‐ｎ、
Ｘ（Ｒ２Ｓｉ○）ｍＳｉＲ２×、
Ｒ３ＳｉＯＳｊＲ３、
Ｒ：アルキル基
Ｘ：ハロゲン、アルコキシ基又は水酸
基、
ｎ：０又は４以下の正の整数
ｍ：１以上の正の数
具体的にはトリメチルクロルシラソ、トリエチルクロル
シヒン、ヘキサメチルジシロキサン、トリメチルシラノ
ール、トリエチルシラノール、ジメチルジクロルシラン
、ジエチルジクロルシラン、１，３−ジクロロテトラメ
チルジシロキサン等が用いられる。(General formula) SIRnX4-n, X(R2Si○)mSiR2x, R3SiOSjR3, R: alkyl group X: halogen, alkoxy group or hydroxyl group, n: 0 or a positive integer of 4 or less m: a positive number of 1 or more Specific Specifically, trimethylchlorosilaso, triethylchlorocihin, hexamethyldisiloxane, trimethylsilanol, triethylsilanol, dimethyldichlorosilane, diethyldichlorosilane, 1,3-dichlorotetramethyldisiloxane, etc. are used.
本発明の方法は一般に以下に示すようにして行なう。The method of the invention is generally carried out as described below.
まず塩酸や硫酸のような鉱酸、水に可溶な有機溶剤、オ
ルガノシリル化剤の所定量を混合し、次にこの混合液を
高速で損拝しながらこれに所定濃度の水ガラス水溶液ま
たは粉末状ゼオラィトを徐々に添加し、該オルガノシリ
ル化剤と反応させる。この場合、反応温度は０〜９００
０、好ましくは１０〜３０００としＰＨは３以下が望ま
しい。この時オルガノシリル化剤の濃度は０．１〜５．
０％、好ましくは０．３〜３．０％、鍵酸の濃度は５〜
５０％、好ましくは１０〜３０％とし、また水溶性有機
溶剤は任意の星で反応を進め得るが、望ましくは全溶液
量の２０〜８０％、特に３０％〜５０％の添加量が最も
経済的かつ充分な収率を与える。また水ガラス水溶液の
濃度は０．１〜２．０％、好ましくは０．１〜５．０％
（Ｓｉ０２として）、添加速度は、酸、水落性有機溶剤
、オルガノシリル化剤の混合液の量に対して約５の【／
分・ク以下であることが望ましい。擬拝速度は約２０仇
ｐｍ以上とするのが望ましい。反応速度は温度に関係な
く、通常反応は１０〜２０時間で終了する。酸、水に可
溶な有機溶剤、オルガノシリル化剤の混合液を高速櫨拝
しながら水ガラス水溶液を徐々に添加すると、水ガラス
は高重合度のシロキシシラノールにはならないでオルガ
ノシリル化剤と反応し低重合度の液体状の有機珪素重合
体が得られる。反応終了後、非水溶性有機溶剤を添加し
、充分蝿拝した後に有機溶剤層を分取し、精製、乾燥し
て生成物を得る。First, a predetermined amount of a mineral acid such as hydrochloric acid or sulfuric acid, a water-soluble organic solvent, and an organosilylating agent are mixed together, and then this mixed solution is poured at high speed while adding a water glass aqueous solution of a predetermined concentration or Powdered zeolite is gradually added and allowed to react with the organosilylating agent. In this case, the reaction temperature is 0 to 900
0, preferably 10 to 3000, and the pH is desirably 3 or less. At this time, the concentration of the organosilylating agent is 0.1 to 5.
0%, preferably 0.3-3.0%, the concentration of key acid is 5-3.0%
50%, preferably 10 to 30%, and the water-soluble organic solvent can proceed with the reaction in any desired amount, but the most economical addition amount is preferably 20 to 80%, particularly 30 to 50% of the total solution amount. gives a targeted and sufficient yield. The concentration of the water glass aqueous solution is 0.1 to 2.0%, preferably 0.1 to 5.0%.
(as SiO2), the addition rate is about 5/
It is desirable that it be less than 1 minute. It is desirable that the prayer speed be approximately 20 pm or more. The reaction rate is independent of temperature, and the reaction usually completes in 10 to 20 hours. When a water glass aqueous solution is gradually added to a mixture of an acid, a water-soluble organic solvent, and an organosilylating agent while stirring at high speed, the water glass does not turn into a highly polymerized siloxysilanol, but instead becomes the organosilylating agent. The reaction results in a liquid organosilicon polymer with a low degree of polymerization. After the reaction is completed, a water-insoluble organic solvent is added, and after sufficient mixing, the organic solvent layer is separated, purified, and dried to obtain a product.
生成物は透明な液体状物質で粘度は約８０比ｐｓであり
、また溌水性をもち、３００００以上の耐熱性を示す。
以下に、本発明を実施例によりさらに詳細に説明する。The product is a transparent liquid substance with a viscosity of about 80 ps, water repellency, and a heat resistance of 30,000 or higher.
EXAMPLES Below, the present invention will be explained in more detail with reference to Examples.
実施例 １３０％硫酸１５０ｍ‘、アセトン２５０私、
トリメチルクロルシラン２．８の‘を縄枠混合する。Example 130% sulfuric acid 150m', acetone 250m',
Mix 2.8' of trimethylchlorosilane in a rope frame.
オルソ珪酸ソーダの９％水溶液１００の‘、を前述の混
合液中に約２の‘／分の速度で、高速凝拝しながら滴下
する。このときの反応液のｐＨは０以下であり、磯拝速
度は約２０仇ｐｍである。滴下後室温でそのまま放置し
て反応を促進せしめ、反応終了後石油ベンジン５０の上
を加え振とう混合する。次いで石油ベンジン層を分離し
、精製後乾燥する。生成物は液体状で粘度は約８０比ｐ
ｓ（２０００）であった。Ｓｉ収率は８０％。実施例
２
実施例１と同じ方法で、シロキシシラノールとして３号
珪酸ソーダの１０％水溶液４０肌を用いた。100 ml of a 9% aqueous solution of sodium orthosilicate is dropped into the above-mentioned mixture at a rate of about 2 ml/min while stirring at high speed. At this time, the pH of the reaction solution is 0 or less, and the Isohei speed is about 20 pm. After dropping, the mixture was allowed to stand at room temperature to accelerate the reaction, and after the reaction was completed, petroleum benzine 50 was added and mixed by shaking. The petroleum benzine layer is then separated, purified and dried. The product is liquid and has a viscosity of approximately 80 p.
s (2000). Si yield is 80%. Example
2 In the same manner as in Example 1, a 10% aqueous solution of No. 3 sodium silicate 40 skin was used as the siloxysilanol.
生成物は液体状で粘度は約９０比ｐｓ（２０００）であ
った。Ｓｉ収率は７８％。実施例 ３
濃塩酸（３６％）１５０の‘、アセトン１５０地、トリ
メチルクロルシラン３．６の‘を縄梓混合する。The product was in liquid form with a viscosity of approximately 90 ps (2000). Si yield was 78%. Example 3 150 parts of concentrated hydrochloric acid (36%), 150 parts of acetone, and 3.6 parts of trimethylchlorosilane were mixed together.
粉末状の方フッ石３夕を前述の混合液中に投入し、室温
で約３時間燈枠する。このときの反応液のｐＨは０以下
であり、蝿杵速度は約２０仇ｐｍである。３時間後石油
ベンジンｌｏ０の‘を添加し、蝿拝混合する。Powdered turmeric was added to the above-mentioned mixture and allowed to stand at room temperature for about 3 hours. At this time, the pH of the reaction solution was 0 or less, and the fly speed was about 20 pm. After 3 hours, add petroleum benzine LO' and mix well.
次いで石油ベンジン層を分取し、精製後乾燥する。生成
物は液体状で粘度は約１００比ｐｓ（２０℃）であった
。Ｓｉ収率は７０％。実施例 ４
実施例３と同じ方法で方フッ石の替りにＡ型合成ゼオラ
ィトを５タ添加し、反応させた。Next, the petroleum benzine layer is separated, purified and dried. The product was liquid and had a viscosity of about 100 ps (at 20° C.). Si yield is 70%. Example 4 In the same manner as in Example 3, 5 tons of A-type synthetic zeolite was added instead of fluorite and reacted.
生成物は液体状で、粘度は約８０比ｐｓ（２０℃）であ
つた。Ｓｊ収率は７３％。実施例 ５
実施例３と同じ方法で方フッ石の替りにＹ型合成ゼオラ
ィト３夕を添加し、反応させた。The product was liquid with a viscosity of about 80 ps (at 20° C.). Sj yield was 73%. Example 5 In the same manner as in Example 3, Y-type synthetic zeolite was added instead of fluorite and reacted.
生成物は液体で、粘度は約９０比ｐｓ（２０００）であ
った。Ｓｉ収率は７５％。実施例 ６
実施例１と同じ方法でオルガノシリル化剤としてへキサ
メチルジシロキサンを２．１の‘添加した。The product was a liquid with a viscosity of approximately 90 ps (2000). Si yield is 75%. Example 6 In the same manner as in Example 1, 2.1' of hexamethyldisiloxane was added as organosilylating agent.
生成物は液体状で粘度は約８０比ｐｓ（２０ｏｏ）であ
った。Ｓｉ収率は８２％。実施例 ７
実施例３と同じ方法で、オルガノシリル化剤としてへキ
サメチルジシロキサンを３．０泌添加した。The product was liquid and had a viscosity of about 80 ps (20 oo). Si yield was 82%. Example 7 In the same manner as in Example 3, 3.0 ml of hexamethyldisiloxane was added as an organosilylating agent.
生成物は液体状で粘度は約１００比ｐｓ（２０ｑｏ）で
あった。Ｓｉ収率は７４％。実施例 ８
実施例１と同じ方法で硫酸の添加量を変えた時のＳｉ収
率は下表のようになったり実施例 ９ ．
実施例７と同じ方法でオルガノシリル化剤として１，３
−ジクロロテトラメチルジシロキサンを３．０の【添加
した。The product was liquid and had a viscosity of about 100 ps (20 qo). Si yield was 74%. Example 8 When the amount of sulfuric acid added was changed using the same method as in Example 1, the Si yield was as shown in the table below. 1,3 as an organosilylating agent in the same manner as in Example 7.
-3.0 of dichlorotetramethyldisiloxane was added.
Claims (1)
せて有機珪素化合物を得る方法において、水に可容な有
機溶剤とオルガノシリル化剤を含む鉱酸水溶液中に徐々
にシロキシシラノールを添加し、それにより低重合度の
ままシロキシシラノールを有機珪素化して液体状の有機
珪素化合物を得ることを特徴とする有機珪素重合体の製
造方法。1 In a method for obtaining an organosilicon compound by reacting siloxysilanol with an organosilylating agent, siloxysilanol is gradually added to an aqueous mineral acid solution containing a water-soluble organic solvent and an organosilylating agent, thereby reducing the 1. A method for producing an organosilicon polymer, which comprises producing a liquid organosilicon compound by converting siloxysilanol to organosilicon while maintaining the degree of polymerization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12150877A JPS6034574B2 (en) | 1977-10-12 | 1977-10-12 | Method for producing organosilicon polymer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12150877A JPS6034574B2 (en) | 1977-10-12 | 1977-10-12 | Method for producing organosilicon polymer |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5455100A JPS5455100A (en) | 1979-05-01 |
| JPS6034574B2 true JPS6034574B2 (en) | 1985-08-09 |
Family
ID=14812922
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12150877A Expired JPS6034574B2 (en) | 1977-10-12 | 1977-10-12 | Method for producing organosilicon polymer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6034574B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63256628A (en) * | 1987-04-14 | 1988-10-24 | Shin Etsu Chem Co Ltd | Method for producing organopolysiloxane |
-
1977
- 1977-10-12 JP JP12150877A patent/JPS6034574B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5455100A (en) | 1979-05-01 |
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