JPH0413293B2 - - Google Patents
Info
- Publication number
- JPH0413293B2 JPH0413293B2 JP60288257A JP28825785A JPH0413293B2 JP H0413293 B2 JPH0413293 B2 JP H0413293B2 JP 60288257 A JP60288257 A JP 60288257A JP 28825785 A JP28825785 A JP 28825785A JP H0413293 B2 JPH0413293 B2 JP H0413293B2
- Authority
- JP
- Japan
- Prior art keywords
- solution
- water
- silica spheres
- silica
- present
- 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 - Lifetime
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 40
- 239000000377 silicon dioxide Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000006228 supernatant Substances 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 4
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 125000003545 alkoxy group Chemical group 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
- -1 and in particular Chemical compound 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000012778 molding material Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
- Silicon Polymers (AREA)
Description
【発明の詳細な説明】
本発明は有機溶剤中でエチルシリケートを加水
分解して単分散状態の微小球シリカを製造する方
法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing monodisperse microspherical silica by hydrolyzing ethyl silicate in an organic solvent.
エチルシリケートをアンモニア水のエタノール
溶液中で加水分解するとシリカ球分散液が得られ
るが、液から分離した状態のシリカ球を得るため
には長時間遠心分離しなければならない。遠心分
離をせずに長時間放置してもシリカ球を液から分
離することは困難である。 When ethyl silicate is hydrolyzed in an aqueous ammonia solution in ethanol, a silica sphere dispersion can be obtained, but in order to obtain the silica spheres separated from the liquid, centrifugation must be performed for a long time. It is difficult to separate the silica spheres from the liquid even if the liquid is left for a long time without centrifugation.
本発明者らはエチルシリケートより単分散状態
の微粒状シリカ球を得る方法について鋭意検討を
重ねた結果、エタノールより炭素数が多く、水を
溶解することのできる有機溶剤を用いてエチルシ
リケートを加水分解すると容易に単分散状態のシ
リカ球が得られることを知り本発明に到達したも
のである。 The inventors of the present invention have conducted intensive studies on a method for obtaining monodispersed microgranular silica spheres from ethyl silicate, and found that ethyl silicate is hydrated using an organic solvent that has more carbon atoms than ethanol and can dissolve water. The present invention was arrived at after discovering that monodisperse silica spheres can be easily obtained by decomposition.
すなわち本発明は水を溶解することのできる炭
素数３または４の有機溶剤にアンモニア水を溶解
させた後テトラアルコキシシランまたはその部分
縮合物の溶液を加えてアルコキシシランを加水分
解させることを特徴とするシリカの製法を提供せ
んとするものである。 That is, the present invention is characterized in that aqueous ammonia is dissolved in an organic solvent having 3 or 4 carbon atoms that can dissolve water, and then a solution of tetraalkoxysilane or a partial condensate thereof is added to hydrolyze the alkoxysilane. The purpose of this invention is to provide a method for producing silica.
本発明における水を溶解することのできる炭素
数３または４の有機溶剤としてはプロパノール、
イソプロパノール、第３級ブタノール、アセト
ン、メチルエチルケトン、ジオキサンあるいはテ
トラヒドロフランなどがあり、これらを単独ある
いは混合して用いることができる。 In the present invention, the organic solvent having 3 or 4 carbon atoms that can dissolve water includes propanol,
Examples include isopropanol, tertiary butanol, acetone, methyl ethyl ketone, dioxane, and tetrahydrofuran, and these can be used alone or in combination.
これらの有機溶剤にアンモニア水を溶解させた
後テトラアルコキシシランまたはその部分縮合物
の溶液を混合するとアルコキシシランは加水分解
され、白濁状態あるいは沈降性シリカ球を得るこ
とができる。白独状態のものも数日放置すると沈
降性のシリカ球となる。 When aqueous ammonia is dissolved in these organic solvents and then a solution of tetraalkoxysilane or its partial condensate is mixed, the alkoxysilane is hydrolyzed and cloudy white or precipitated silica spheres can be obtained. Even if it is left in a white state for a few days, it becomes a sedimentary silica sphere.
ここでテトラアルコキシシランまたはその部分
縮合物としては四塩化ケイ素とアルコールから容
易に製造されるものであり、特にテトラエトキシ
シラン（エチルシリケート）またはその部分縮合
物は市販品として容易に入手することができ、本
発明に用いられるものである。 Here, tetraalkoxysilane or its partial condensate is easily produced from silicon tetrachloride and alcohol, and in particular, tetraethoxysilane (ethyl silicate) or its partial condensate is easily available as a commercial product. It can be used in the present invention.
これを加水分解するために水を加えるが、その
量はアルコキシ基に対して当量以上が必要であ
り、アルコキシ基を完全に加水分解するためには
過剰の水を用いる必要がある。 Water is added to hydrolyze this, but the amount needs to be at least equivalent to the alkoxy group, and in order to completely hydrolyze the alkoxy group, it is necessary to use an excess of water.
本発明のシリカ球は例えばアンモニア水の第３
級ブタノール溶液にエチルシリケート（テトラエ
トキシシラン）の第３級ブタノールの溶液を加え
て放置し、上澄液が透明になつた後上澄液を除
き、沈殿を乾燥して得ることができる。このシリ
カ球の直径は約0.5μであり、よく分散した状態で
得られる。 The silica spheres of the present invention can be used, for example, in ammonia water.
A tertiary-butanol solution of ethyl silicate (tetraethoxysilane) is added to a tertiary-butanol solution, the mixture is left to stand, and after the supernatant becomes transparent, the supernatant is removed and the precipitate is dried. The diameter of these silica spheres is approximately 0.5μ, and they are obtained in a well-dispersed state.
本発明によつて得られるシリカ球は従来にない
よく分散した状態の微細なシリカ球であり、気体
および液体クロマト用の充填剤として、またシリ
カ系セラミツクの成形材料としてその応用が期待
されるものである。 The silica spheres obtained by the present invention are fine silica spheres in a well-dispersed state that has never existed before, and are expected to be used as a filler for gas and liquid chromatography, and as a molding material for silica-based ceramics. It is.
本発明をさらに詳細に説明するため、つぎに例
をあげて説明する。 In order to explain the present invention in more detail, an example will be given below.
実施例 １
30％アンモニア水10mlと水７mlを第３級ブタノ
ール40mlに混合し、テトラエトキシシラン10mlと
第３級ブタノール40mlの溶液を加える。７日間放
置した後傾斜して上澄液を除き、沈殿を乾燥する
と約0.5μの分散したシリカ球が得られる。Example 1 10 ml of 30% aqueous ammonia and 7 ml of water are mixed with 40 ml of tertiary butanol, and a solution of 10 ml of tetraethoxysilane and 40 ml of tertiary butanol is added. After standing for 7 days, the supernatant liquid is removed by decanting, and the precipitate is dried to obtain dispersed silica spheres of about 0.5μ.
第３級ブタノールのかわりにエタノールを用い
ると上澄液が透明にならず、沈殿を分離すること
ができない。 If ethanol is used instead of tertiary butanol, the supernatant will not become transparent and the precipitate cannot be separated.
実施例 ２
30％アンモニア水10ml、水10mlとイソプロパノ
ール40mlの溶液にテトラエトキシシラン10mlとイ
ソプロパノールの溶液を加えると白濁状態とな
る。これを７日間放置した後、透明な上澄液を傾
斜して除き、沈殿を乾燥すると0.5〜0.7μの分散
したシリカ球を得る。Example 2 When a solution of 10 ml of tetraethoxysilane and isopropanol is added to a solution of 10 ml of 30% ammonia water, 10 ml of water, and 40 ml of isopropanol, the mixture becomes cloudy. After this was allowed to stand for 7 days, the clear supernatant liquid was decanted and the precipitate was dried to obtain dispersed silica spheres of 0.5-0.7μ.
実施例 ３
30％アンモニア水10ml、水７mlとアセトン40ml
の溶液にテトラエトキシシラン10mlとアセトン40
mlの溶液を加え、７日間法置した後上澄液を除い
て乾燥すると0.5〜1μのシリカ球が分散した状態
で得られる。Example 3 10ml of 30% ammonia water, 7ml of water and 40ml of acetone
10 ml of tetraethoxysilane and 40 ml of acetone in a solution of
ml of the solution is added, and after incubation for 7 days, the supernatant is removed and dried to obtain silica spheres of 0.5 to 1 μ in size dispersed.
実施例 ４
30％アンモニア水10ml、水７mlとジオキサン40
mlの溶液にテトラエトキシシラン10mlとジオキサ
ン40mlの溶液を混合すると液は白濁する。３日間
放置した後、炉過して乾燥すると小量の凝集した
シリカ球とともに分散したシリカ球を得る。Example 4 10ml of 30% ammonia water, 7ml of water and 40ml of dioxane
When a solution of 10 ml of tetraethoxysilane and 40 ml of dioxane is mixed with 1 ml of a solution, the liquid becomes cloudy. After being left for 3 days, it is filtered and dried to obtain dispersed silica spheres along with a small amount of aggregated silica spheres.
Claims (1)
の有機溶剤にアンモニア水を溶解させた後、テト
ラアルコキシシランまたはその部分縮合物の溶液
を加えて、アルコキシシランを加水分解させるこ
とを特徴とするシリカの製法。1 Carbon number 3 or 4 that can dissolve water
A method for producing silica, which comprises dissolving aqueous ammonia in an organic solvent, and then adding a solution of tetraalkoxysilane or a partial condensate thereof to hydrolyze the alkoxysilane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60288257A JPS62148316A (en) | 1985-12-20 | 1985-12-20 | Preparation of microspherical silica |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60288257A JPS62148316A (en) | 1985-12-20 | 1985-12-20 | Preparation of microspherical silica |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62148316A JPS62148316A (en) | 1987-07-02 |
| JPH0413293B2 true JPH0413293B2 (en) | 1992-03-09 |
Family
ID=17727853
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60288257A Granted JPS62148316A (en) | 1985-12-20 | 1985-12-20 | Preparation of microspherical silica |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62148316A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013115367A1 (en) * | 2012-02-02 | 2013-08-08 | 日産化学工業株式会社 | Low refractive index film-forming composition |
| US20250059050A1 (en) * | 2021-12-23 | 2025-02-20 | Fuso Chemical Co., Ltd. | Colloidal silica and production method therefor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5841810A (en) * | 1981-09-07 | 1983-03-11 | Tokuyama Soda Co Ltd | Composite reparative material |
| JPS58110414A (en) * | 1981-12-23 | 1983-07-01 | Tokuyama Soda Co Ltd | Inorganic oxide and its manufacture |
| JPS6252119A (en) * | 1985-08-29 | 1987-03-06 | Tokuyama Soda Co Ltd | Method for manufacturing silica particles |
-
1985
- 1985-12-20 JP JP60288257A patent/JPS62148316A/en active Granted
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5841810A (en) * | 1981-09-07 | 1983-03-11 | Tokuyama Soda Co Ltd | Composite reparative material |
| JPS58110414A (en) * | 1981-12-23 | 1983-07-01 | Tokuyama Soda Co Ltd | Inorganic oxide and its manufacture |
| JPS6252119A (en) * | 1985-08-29 | 1987-03-06 | Tokuyama Soda Co Ltd | Method for manufacturing silica particles |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62148316A (en) | 1987-07-02 |
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