JPH0317852B2 - - Google Patents
Info
- Publication number
- JPH0317852B2 JPH0317852B2 JP24854189A JP24854189A JPH0317852B2 JP H0317852 B2 JPH0317852 B2 JP H0317852B2 JP 24854189 A JP24854189 A JP 24854189A JP 24854189 A JP24854189 A JP 24854189A JP H0317852 B2 JPH0317852 B2 JP H0317852B2
- Authority
- JP
- Japan
- Prior art keywords
- titanium
- silicic acid
- polymer
- titanosiloxane
- oxyquinolinate
- 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
- 229920000642 polymer Polymers 0.000 claims description 21
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 13
- 235000012239 silicon dioxide Nutrition 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 10
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 7
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 150000003609 titanium compounds Chemical class 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000011541 reaction mixture Substances 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 229910052719 titanium Inorganic materials 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 125000004432 carbon atom Chemical group C* 0.000 claims description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 8
- 239000000243 solution Substances 0.000 description 8
- 239000003960 organic solvent Substances 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000006482 condensation reaction Methods 0.000 description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- BTANRVKWQNVYAZ-UHFFFAOYSA-N butan-2-ol Chemical compound CCC(C)O BTANRVKWQNVYAZ-UHFFFAOYSA-N 0.000 description 3
- KVIKMJYUMZPZFU-UHFFFAOYSA-N propan-2-ol;titanium Chemical compound [Ti].CC(C)O.CC(C)O KVIKMJYUMZPZFU-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 2
- MBMKFKOVXPKXCV-UHFFFAOYSA-N CCO[Ti]OCC Chemical compound CCO[Ti]OCC MBMKFKOVXPKXCV-UHFFFAOYSA-N 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- IJKVHSBPTUYDLN-UHFFFAOYSA-N dihydroxy(oxo)silane Chemical compound O[Si](O)=O IJKVHSBPTUYDLN-UHFFFAOYSA-N 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000012784 inorganic fiber Substances 0.000 description 2
- ZXEKIIBDNHEJCQ-UHFFFAOYSA-N isobutanol Chemical compound CC(C)CO ZXEKIIBDNHEJCQ-UHFFFAOYSA-N 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- FIPWRIJSWJWJAI-UHFFFAOYSA-N Butyl carbitol 6-propylpiperonyl ether Chemical compound C1=C(CCC)C(COCCOCCOCCCC)=CC2=C1OCO2 FIPWRIJSWJWJAI-UHFFFAOYSA-N 0.000 description 1
- 229910003849 O-Si Inorganic materials 0.000 description 1
- 229910003872 O—Si Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000004115 Sodium Silicate Substances 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229960005235 piperonyl butoxide Drugs 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000012260 resinous material Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 235000019795 sodium metasilicate Nutrition 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Silicon Polymers (AREA)
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、新規のチタノシロキサン重合体の製
造法に関する。本発明で得られるチタノシロキサ
ン重合体は、常温で有機溶媒可溶性の固体であつ
て急激な有機溶媒不溶化を起さない安定性を有す
る。この重合体は、更に加水分解及び縮合反応さ
せることにより、或いは加熱下縮合反応させるこ
とにより、チタン原子、珪素原子及び酸素原子か
らなる無機質の酸化物硬化体に変る性質を有し、
無機繊維、無機コーテイング剤、無機接着剤、無
機結合剤等の原料又はその成分として用いられ
る。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a novel method for producing titanosiloxane polymers. The titanosiloxane polymer obtained in the present invention is a solid that is soluble in organic solvents at room temperature and has stability that does not cause rapid insolubilization in organic solvents. This polymer has the property of converting into an inorganic oxide cured product consisting of titanium atoms, silicon atoms, and oxygen atoms by further hydrolysis and condensation reaction, or by condensation reaction under heating,
It is used as a raw material or component of inorganic fibers, inorganic coating agents, inorganic adhesives, inorganic binders, etc.
（従来の技術）
ポリチタノシロキサンとしては、ポリチタノメ
チルシロキサン等耐熱性のポリチタノオルガノシ
ロキサンが既に、ジヤーナル・オブ・ポリマ−・
サイエンス（Journal of Polymer Science）第
52巻第257〜276頁（1961年）に記載されており、
また、窯業協会誌第84巻第614〜618頁（1976年）
にも、シリコンテトラエトキシドとチタンテトラ
イソプロポキシドとの共加水分解によつてポリチ
タノシロキサンが生成することが示されている。(Prior art) As polytitanosiloxanes, heat-resistant polytitanoorganosiloxanes such as polytitanomethylsiloxane are already available in the Journal of Polymers.
Science (Journal of Polymer Science) No.
52, pp. 257-276 (1961),
Also, Ceramics Association Journal, Vol. 84, pp. 614-618 (1976)
It has also been shown that polytitanosiloxane is produced by cohydrolysis of silicon tetraethoxide and titanium tetraisopropoxide.
また、日本化学会第52春季年会（1986年）の講
演予講集の第798頁には、ビス（アセチルアセ
トネート）チタンジイソプロポキシドと珪酸とを
反応させることによつて、曳糸性のポリチタノシ
ロキサンが得られることが示されている。 In addition, on page 798 of the pre-lecture lecture collection of the 52nd Spring Annual Meeting of the Chemical Society of Japan (1986), it is stated that by reacting bis(acetylacetonate) titanium diisopropoxide with silicic acid, It has been shown that polytitanosiloxanes with high properties can be obtained.
（発明が解決しようとする問題点）
ポリチタノオルガノシロキサンは、高価な有機
珪素化合物を原料とし、また、その生成反応及び
製造方法が複雑である。更にこのポリマーには、
炭素−珪素の直接結合が存するために、低温では
このポリマーを完全に無機化することができな
い。(Problems to be Solved by the Invention) Polytitanoorganosiloxane uses an expensive organic silicon compound as a raw material, and its production reaction and manufacturing method are complicated. Furthermore, this polymer has
Due to the presence of direct carbon-silicon bonds, this polymer cannot be completely mineralized at low temperatures.
一方、シリコンテトラエトキシドとチタンテト
ライソプロポキシドの共加水分解によつて生成す
るポリチタノシロキサンは、極めて不安定であつ
て、縮合反応の進行による溶媒不溶化を起し易
い。例えば、有用性が高い曳糸性を示す状態にあ
る期間は約１時間以内であるから、これを工業製
品として提供することは困難である。従つて、こ
れを用いることによつては、品質一定の無機繊
維、塗料、接着剤等は得られない。 On the other hand, polytitanosiloxane produced by cohydrolysis of silicone tetraethoxide and titanium tetraisopropoxide is extremely unstable and tends to become insolubilized in solvents due to the progress of the condensation reaction. For example, it is difficult to provide this as an industrial product because the period in which it is in a state where it exhibits highly useful stringiness is about one hour or less. Therefore, by using this, inorganic fibers, paints, adhesives, etc. of constant quality cannot be obtained.
上記日本化学会第52春季年会講演予講集には、
ビス（アセチルアセトネート）チタンジイソプロ
ポキシドと珪酸の反応によるポリチタノシロキサ
ンが示されているのみである。 The chemical society of Japan 52nd spring annual meeting lecture collection mentioned above includes:
Only polytitanosiloxanes produced by the reaction of bis(acetylacetonate)titanium diisopropoxide and silicic acid are shown.
従つて、本発明の目的は、常温の安定性は高い
が、容易に完全無機化せしめ得る新規の有機溶媒
可溶性チタノシロキサン重合体の製造法を提供す
ることにある。 Therefore, an object of the present invention is to provide a method for producing a novel organic solvent-soluble titanosiloxane polymer that is highly stable at room temperature but can be easily completely mineralized.
（問題点を解決するための手段）
本発明の新規なる有機溶媒可溶性チタノシロキ
サン重合体は、下記一般式（）
（但し、式中Ｒは、炭素原子数１〜４のアルキ
ル基を表わす。）
で示されるビス（８−オキシキノリナート）チタ
ニウムジアルコキシドと珪酸を、好ましくは
SiO2／TiO2モル比0.25〜４で、これらチタニウ
ム化合物と珪酸の可溶性溶媒中、常温〜反応混合
物の還流温度で反応させることによつて得られ
る。(Means for Solving the Problems) The novel organic solvent soluble titanosiloxane polymer of the present invention has the following general formula () (However, in the formula, R represents an alkyl group having 1 to 4 carbon atoms.) A bis(8-oxyquinolinate) titanium dialkoxide represented by the formula and silicic acid are preferably used.
It can be obtained by reacting these titanium compounds with silicic acid in a soluble solvent at room temperature to the reflux temperature of the reaction mixture at a SiO 2 /TiO 2 molar ratio of 0.25 to 4.
本発明に用いられる珪酸は、従来から知られて
いる方法によつて容易に得られ、例えば、水ガラ
ス、メタ珪酸ソーダ、珪酸アンモニウム等可溶性
珪酸塩の水溶液を酸によつて中和処理することに
より、或いは陽イオン交換樹脂で処理することに
より水溶液として得られる。 The silicic acid used in the present invention can be easily obtained by a conventionally known method, for example, by neutralizing an aqueous solution of a soluble silicate such as water glass, sodium metasilicate, or ammonium silicate with an acid. or by treatment with a cation exchange resin as an aqueous solution.
本発明のチタノシロキサン重合体の生成反応に
は、上記例示の如き処理で得られた水溶液を、塩
析後、例えば、テトラヒドロフラン、ｎ−プロピ
ルアルコール、ｉ−プロピルアルコール、第３級
ブチルアルコール等有機溶媒で抽出することによ
り得られる有機溶媒溶液が用いられる。その
SiO2濃度には特に制限はないが、通常２モル／
程度、或いは更にヘキサン処理によつて６モ
ル／程度の濃度も用いられる。 In the production reaction of the titanosiloxane polymer of the present invention, the aqueous solution obtained by the above-mentioned treatment is salted out, and then, for example, tetrahydrofuran, n-propyl alcohol, i-propyl alcohol, tertiary butyl alcohol, etc. An organic solvent solution obtained by extraction with an organic solvent is used. the
There is no particular limit to the SiO 2 concentration, but it is usually 2 mol/
Concentrations of about 6 mol/mole/mole/m are also used, or even by treatment with hexane.
本発明に用いられる前記一般式（）で示され
る化合物としては、ビス（８−オキシキノリナー
ト）チタニウムジエトキシド、ビス（８−オキシ
キノリナート）チタニウムジイソプロポキシド、
ビス（８−オキシキノリナート）チタニウムジノ
ルマルブトキシド等が例示される。 Examples of the compound represented by the general formula () used in the present invention include bis(8-oxyquinolinate) titanium diethoxide, bis(8-oxyquinolinate) titanium diisopropoxide,
Examples include bis(8-oxyquinolinate) titanium di-normal butoxide.
上記一般式（）で示されるチタン化合物と珪
酸との反応に用いられる溶媒の例としては、アセ
トン、メタノール、エタノール、１−プロパノー
ル、２−プロパノール、１−ブタノール、２−ブ
タノール、２−メチル−１−プロパノール、２−
メチル−２−プロパノール等が挙げられる。 Examples of solvents used in the reaction between the titanium compound represented by the above general formula () and silicic acid include acetone, methanol, ethanol, 1-propanol, 2-propanol, 1-butanol, 2-butanol, 2-methyl- 1-propanol, 2-
Examples include methyl-2-propanol.
本発明の新規チタノシロキサン重合体は、上記
珪酸の有機溶媒溶液と、上記一般式（）で示さ
れる化合物の上記有機溶媒溶液とを、好ましくは
SiO2／TiO2モル比0.25〜４の比率に混合し、好
ましくは反応混合物の還流温度で0.5〜12時間程
度反応させることにより、上記溶媒溶液として容
易に得られる。この溶液から、例えば、減圧下溶
媒の留去等により、溶媒を一部又は全部除くと、
本発明のポリチタノシロキサンが固体又は高粘性
液体として得られる。また、このポリチタノシロ
キサンは、メタノールに溶解させた後、得られた
溶液をヘキサン中に投入するとスラリー状に析出
するから、このスラリーから溶媒及びヘキサンを
分離除去することによつて、粉末状のポリチタノ
シロキサンが得られる。 The novel titanosiloxane polymer of the present invention preferably comprises a solution of the silicic acid in an organic solvent and a solution of the compound represented by the general formula () in an organic solvent.
The above solvent solution can be easily obtained by mixing SiO 2 /TiO 2 at a molar ratio of 0.25 to 4 and reacting preferably at the reflux temperature of the reaction mixture for about 0.5 to 12 hours. If some or all of the solvent is removed from this solution, for example by distilling off the solvent under reduced pressure,
The polytitanosiloxanes of the invention are obtained as solids or highly viscous liquids. In addition, when this polytitanosiloxane is dissolved in methanol and the resulting solution is poured into hexane, it precipitates in the form of a slurry, so by separating and removing the solvent and hexane from this slurry, it can be made into a powder. of polytitanosiloxane is obtained.
（作用）
上記一般式（）で示されるチタン化合物と珪
酸は共縮合反応を起して重合体が生成するが、そ
の反応によつてはチタン化合物の８−オキシキノ
リナート基が脱離しないから、溶媒不溶性重合体
の生成が起りにくい。そしてこれらの基を含有す
るチタノシロキサン重合体も、常温で水に接触し
たときこれらの基の脱離が起りにくいから安定で
ある。しかし、このチタン化合物と珪酸とを、
SiO2／TiO2モル比として４を越える比率で反応
させると溶媒不溶性重合体が生成し易い。(Function) The titanium compound represented by the above general formula () and silicic acid undergo a co-condensation reaction to form a polymer, but the 8-oxyquinolinate group of the titanium compound does not leave due to the reaction. Therefore, formation of solvent-insoluble polymers is less likely to occur. Titanosiloxane polymers containing these groups are also stable because these groups are less likely to be eliminated when they come into contact with water at room temperature. However, this titanium compound and silicic acid,
If the reaction is carried out at a SiO 2 /TiO 2 molar ratio exceeding 4, a solvent-insoluble polymer is likely to be produced.
本発明のチタノシロキサン重合体は、上記８−
オキシキノリナート基を含有するが、特別の加水
分解条件或いは高温下では、これらの基を容易に
放出するから、有機基を含まないか、或いはその
含有率が極めて低い無機チタノシロキサン重合体
に変る。 The titanosiloxane polymer of the present invention has the above 8-
Inorganic titanosiloxane polymers that contain oxyquinolinate groups, but do not contain organic groups or have extremely low organic groups because these groups are easily released under special hydrolysis conditions or high temperatures. Changes to
（実施例）
SiO2として0.6重量部を含有する珪酸のテトラ
ヒドロフラン溶液11.8重量部と、ビス（８−オキ
シキノリナート）チタニウム ジエトキシド4.2
重量部を含む２−プロパノール溶液50重量部を混
合し、撹拌下60分間、反応混合物とその還流温度
に保つた。次いで、減圧下溶媒を留去することに
より、樹脂状物4.6重量部を得た。この生成物の
分析結果は、SiO2／TiO2モル比が１であつた。
更に、得られた生成物は赤外線吸収スペクトルに
930cm-1の吸収を観測し、Ti−Ｏ−Si結合のチタ
ノシロキサンであることを認めた。また、この樹
脂状物は空気中でガラス棒の先端を接触させた
後、ガラス棒を引き上げると70cmの長さに曳糸で
き、空気中480時間放置後も溶媒不溶化せず、同
様の曳糸性を示した。(Example) 11.8 parts by weight of a solution of silicic acid in tetrahydrofuran containing 0.6 parts by weight as SiO 2 and 4.2 parts by weight of bis(8-oxyquinolinate) titanium diethoxide.
50 parts by weight of a 2-propanol solution were mixed and the reaction mixture was kept at its reflux temperature for 60 minutes under stirring. Then, the solvent was distilled off under reduced pressure to obtain 4.6 parts by weight of a resinous material. Analysis of this product revealed that the SiO 2 /TiO 2 molar ratio was 1.
Furthermore, the obtained product has an infrared absorption spectrum.
Absorption at 930 cm -1 was observed, and it was recognized that it was titanosiloxane with Ti-O-Si bonds. In addition, this resin-like material can be threaded into a length of 70 cm by touching the tip of a glass rod in the air and then pulling the glass rod up, and even after being left in the air for 480 hours, it did not become insolubilized in the solvent, and similar threads could be made. showed his sexuality.
（発明の効果）
本発明によると、簡易な製造法により、安定
な、かつ曳糸性を示す有機溶媒可溶性のチタノシ
ロキサン重合体を得ることができる。特に、本発
明に用いられるビス（８−オキシキノリナート）
チタニウムジアルコキシドの配位子が加水分解に
対して、アルコキシ基よりも格段に安定であるか
ら、珪酸との共縮合反応の操作の際にも仕込み原
料組成を一定にコントロールし易く、品質一定の
重合体を得ることができる。(Effects of the Invention) According to the present invention, an organic solvent-soluble titanosiloxane polymer that is stable and exhibits spinnability can be obtained by a simple production method. In particular, the bis(8-oxyquinolinate) used in the present invention
Since the ligand of titanium dialkoxide is much more stable than an alkoxy group against hydrolysis, it is easy to control the raw material composition to a constant level even during the co-condensation reaction with silicic acid, and it is possible to maintain constant quality. Polymers can be obtained.
また、本発明による新規の有機溶媒可溶性チタ
ノシロキサン重合体は、８−オキシキノリナート
基が高温では加水分解による脱離を起し易いか
ら、高温処理により容易に有機分を含まない無機
質のポリチタノシロキサンを生成させることがで
きる。 In addition, the novel organic solvent-soluble titanosiloxane polymer according to the present invention has an 8-oxyquinolinate group that is easily eliminated by hydrolysis at high temperatures. Polytitanosiloxane can be produced.
Claims (1)
基を表わす。） で示されるビス（８−オキシキノリナート）チタ
ニウムジアルコキシドと珪酸をSiO2／TiO2モル
比0.25〜４において、これらチタニウム化合物と
珪酸の可溶性溶媒中常温ないし反応混合物の還流
温度で反応させることを特徴とするビス（８−オ
キシキノリナート）チタノシロキサン結合を含有
する有機溶媒可溶性のビス（８−オキシキノリナ
ート）チタノシロキサン重合体の製造法。[Claims] 1. The following general formula () (However, in the formula, R represents an alkyl group having 1 to 4 carbon atoms.) Bis(8-oxyquinolinate) titanium dialkoxide represented by the formula and silicic acid at a SiO 2 /TiO 2 molar ratio of 0.25 to 4, These titanium compounds and silicic acid are reacted in a soluble solvent at room temperature to the reflux temperature of the reaction mixture. Nolinato) method for producing titanosiloxane polymer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24854189A JPH02117923A (en) | 1989-09-25 | 1989-09-25 | Novel titanosiloxane polymer and production thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24854189A JPH02117923A (en) | 1989-09-25 | 1989-09-25 | Novel titanosiloxane polymer and production thereof |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20087786A Division JPS6356530A (en) | 1986-08-27 | 1986-08-27 | Novel titanosiloxane polymer and production thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02117923A JPH02117923A (en) | 1990-05-02 |
| JPH0317852B2 true JPH0317852B2 (en) | 1991-03-11 |
Family
ID=17179717
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24854189A Granted JPH02117923A (en) | 1989-09-25 | 1989-09-25 | Novel titanosiloxane polymer and production thereof |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02117923A (en) |
-
1989
- 1989-09-25 JP JP24854189A patent/JPH02117923A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPH02117923A (en) | 1990-05-02 |
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