JPH04175218A - Production of high-purity silica - Google Patents
Production of high-purity silicaInfo
- Publication number
- JPH04175218A JPH04175218A JP30286390A JP30286390A JPH04175218A JP H04175218 A JPH04175218 A JP H04175218A JP 30286390 A JP30286390 A JP 30286390A JP 30286390 A JP30286390 A JP 30286390A JP H04175218 A JPH04175218 A JP H04175218A
- Authority
- JP
- Japan
- Prior art keywords
- silica
- acid
- acid component
- ammonia
- slurry
- 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.)
- Granted
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000002253 acid Substances 0.000 claims abstract description 35
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000012535 impurity Substances 0.000 claims abstract description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000012736 aqueous medium Substances 0.000 claims abstract description 5
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- LRCFXGAMWKDGLA-UHFFFAOYSA-N dioxosilane;hydrate Chemical compound O.O=[Si]=O LRCFXGAMWKDGLA-UHFFFAOYSA-N 0.000 claims 1
- 229940070337 ammonium silicofluoride Drugs 0.000 abstract 2
- 239000000843 powder Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 7
- 239000002002 slurry Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 150000001450 anions Chemical class 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000004993 emission spectroscopy Methods 0.000 description 2
- 239000012065 filter cake Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000003456 ion exchange resin Substances 0.000 description 2
- 229920003303 ion-exchange polymer Polymers 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 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
- 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
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は珪弗化水素酸、珪弗化アンモニウムまたはこれ
らの混合物を反応原料とし、この珪弗化物とアンモニア
とを水性媒体中で反応させて得られるシリカスラリーま
たはシリカケーキに酸成分を添加して不純物を除去する
ことを特徴とする高純度シリカの製造法に関する。高純
度シリカは石英原料、セラミックス原料、塗料、充填剤
等の各種機能材料として有用である。[Detailed Description of the Invention] [Industrial Application Field] The present invention uses hydrofluorosilicic acid, ammonium fluorosilicide, or a mixture thereof as a reaction raw material, and reacts this silicofluoride with ammonia in an aqueous medium. The present invention relates to a method for producing high-purity silica, which is characterized by adding an acid component to a silica slurry or silica cake obtained by removing impurities. High-purity silica is useful as a variety of functional materials such as quartz raw materials, ceramic raw materials, paints, and fillers.
従来、シリカ粉末の製造方法としては、珪酸ソーダを酸
やイオン交換樹脂を用いて中和する方法（珪酸ソーダを
原料とする湿式法）か−船釣であるか、この方法は低コ
ストである反面、ナトリウム、アルミニウム、鉄等の金
属性不純物か混入する為、高純度を要求される分野には
供し得ない。Traditionally, silica powder has been produced by neutralizing sodium silicate with acid or ion exchange resin (wet method using sodium silicate as raw material), or by boat fishing, which is a low-cost method. On the other hand, it cannot be used in fields that require high purity because it is contaminated with metallic impurities such as sodium, aluminum, and iron.
また、乾式法として四塩化珪素を酸素と水素の存在下、
高温燃焼させる方法かあるが、特殊な製造装置を要する
上、高コストのため用途か限定される。また得られるシ
リカの物性も湿式法シリカとは異なる。In addition, as a dry method, silicon tetrachloride is mixed in the presence of oxygen and hydrogen.
There is a method of high-temperature combustion, but its use is limited because it requires special manufacturing equipment and is expensive. The physical properties of the obtained silica are also different from those of wet-process silica.
また更に、珪弗化水素酸のアンモニア中和により比較的
高純度の高いシリカが得られることか知られているか（
特開昭５８−２０８１２５、特開昭５８−２０８１２６
、特開昭５９−１４１４１３、特開昭６２−１５３１１
１）、通常の方法では本発明の如き高純度のシリカは得
られない。即ち、原料の珪弗化水素酸、珪弗化アンモニ
ウムまたはこれらの混合物中にアルミニウム、カルシウ
ム、ナトリウム、鉄等の金属不純分か含有しており、こ
れらの金属成分は珪弗化物とアンモニウムとを水性媒体
中で反応させてシリカを得る際、大半か製品シリカ中に
そのまま不純物として混入する。また、反応副原料であ
るアンモニアも生成シリカ内部及び表面部に強く吸着さ
れ、通常の水洗処理では除去不能である。製品シリカ中
にこれらの不純物が残留すると、シリカの実用場面で問
題となる。Furthermore, is it known that silica of relatively high purity can be obtained by neutralizing hydrosilicofluoric acid with ammonia?
JP-A-58-208125, JP-A-58-208126
, JP-A-59-141413, JP-A-62-15311
1) High purity silica as in the present invention cannot be obtained by conventional methods. That is, the raw material hydrofluorosilicic acid, ammonium fluorosilicide, or a mixture thereof contains metal impurities such as aluminum, calcium, sodium, iron, etc., and these metal components combine fluorosilicide and ammonium. When silica is obtained by reacting in an aqueous medium, most of it is mixed directly into the product silica as an impurity. In addition, ammonia, which is a reaction auxiliary raw material, is also strongly adsorbed inside and on the surface of the produced silica, and cannot be removed by ordinary water washing treatment. If these impurities remain in the product silica, it becomes a problem in the practical use of silica.
上記の技術的課題につき本発明者等は鋭意研究を進めた
結果、本発明を完成した。本発明の方法によれば、通常
の水洗処理では除去不可能なアルミニウム、カルシウム
、ナトリウム、鉄等の金属不純物やアンモニアも除去さ
れ、産業上有用な高純度シリカを工業製品として入手し
得る珪弗化物を反応原料として、簡単な製造工程で容易
に得ることかできる。The present inventors have completed the present invention as a result of intensive research regarding the above technical problem. According to the method of the present invention, metal impurities such as aluminum, calcium, sodium, iron, etc., which cannot be removed by ordinary water washing treatment, and ammonia are also removed, and industrially useful high-purity silica can be obtained as an industrial product. It can be easily obtained through a simple manufacturing process using a compound as a reaction raw material.
本発明は、珪弗化水素酸、珪弗化アンモニウムまたはこ
れらの混合物とアンモニアとを水性媒体中で反応させて
得られるシリカスラリーまたはシリカケーキに酸成分を
添加して不純物を除去することを特徴とする高純度シリ
カの製造法に関する。The present invention is characterized in that an acid component is added to a silica slurry or a silica cake obtained by reacting hydrofluorosilicic acid, ammonium fluorosilicide, or a mixture thereof with ammonia in an aqueous medium to remove impurities. This invention relates to a method for producing high-purity silica.
本発明において用いる酸成分としては、塩酸、硫酸、硝
酸、燐酸、弗化水素酸、珪弗化水素酸、炭酸等の無機酸
、各種有機酸、イオン交換樹脂等が挙げられる。なかで
も無機酸が好ましく、特に弗化水素酸、珪弗化水素酸が
好ましい。Examples of the acid component used in the present invention include inorganic acids such as hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, hydrofluoric acid, hydrofluorosilicic acid, and carbonic acid, various organic acids, and ion exchange resins. Among them, inorganic acids are preferred, and hydrofluoric acid and hydrosilicofluoric acid are particularly preferred.
酸成分の添加方式はシリカスラリー中に攪拌下、常温も
しくは加温下行うことか望ましいか、場合によりケーキ
状態のシリカに酸成分の添加、例えば、ろ過ケーキ中へ
の希薄酸による貫通洗浄方式も可能である。It is preferable to add the acid component to the silica slurry under stirring at room temperature or under heating.In some cases, it is also possible to add the acid component to the silica in the form of a cake, for example, by penetrating the filter cake with diluted acid for washing. It is possible.
酸成分の添加量はシリカスラリーまたはケーキ中の金属
不純物の種類、含量、アンモニア含量、シリカ混合物の
ｐＨ等によるか、シリカスラリーに酸成分を添加する場
合には、通常酸成分添加後のスラリーのｐＨか７以下、
好ましくはｐＨか５以下となる添加量である。シリカケ
ーキの場合はスラリーの場合と同様のｐＨにするか、酸
成分の希薄溶液、好ましくは５％以下の濃度の酸成分溶
液て洗浄すれば良い。過度の酸成分添加は酸成分中のア
ニオン成分の増加や装置材質の腐食をもたらし望ましく
ない。また製品シリカ中に弗素以外のアニオン成分の混
入を避けたい場合は、酸成分として弗化水素酸、珪弗化
水素酸または炭酸を使用する。以下実施例にて本発明を
より具体的に説明する。The amount of the acid component added depends on the type and content of metal impurities in the silica slurry or cake, the ammonia content, the pH of the silica mixture, etc.When adding the acid component to the silica slurry, it is usually determined by the amount of the slurry after adding the acid component. pH is below 7,
Preferably, the amount added is such that the pH is 5 or less. In the case of a silica cake, it may be washed at the same pH as in the case of a slurry, or with a dilute acid component solution, preferably an acid component solution with a concentration of 5% or less. Excessive addition of the acid component is undesirable because it causes an increase in the anion component in the acid component and corrosion of the equipment material. Furthermore, when it is desired to avoid mixing of anion components other than fluorine into the product silica, hydrofluoric acid, hydrosilicofluoric acid, or carbonic acid is used as the acid component. The present invention will be explained in more detail below with reference to Examples.
する珪弗化アンモニウム水溶液２９００ｇを仕込み、２
５％アンモニア水９００ｇを２０℃で３０分かけて添加
し、ｐＨが９．９のシリカ含有スラリーを得た。このシ
リカ含有スラリーを減圧ろ過して得た１次シリカケーキ
４２０ｇをｌＯ分割し、各々１ｋｇの２％硝酸水溶液（
Ａ）、２％硫酸水溶液（Ｂ）、２％塩酸水溶液（Ｃ）を
用いて貫通洗浄した。尚、比較のため同量の純水でも貫
通洗浄をした。この洗浄した２次シリカケーキは各々更
に１ｋｇの純水で貫通洗浄後１０５°Ｃの熱風乾燥話中
で３時間乾燥し、シリカ粉を得た。得られたシリカ粉の
金属不純物含量をＩｃＰ発光分析法により測定した。測
定結果を表−１に示す。Prepare 2,900 g of ammonium silifluoride aqueous solution,
900 g of 5% ammonia water was added at 20° C. over 30 minutes to obtain a silica-containing slurry with a pH of 9.9. 420 g of the primary silica cake obtained by filtering this silica-containing slurry under reduced pressure was divided into lO portions, each containing 1 kg of a 2% nitric acid aqueous solution (
A), a 2% aqueous sulfuric acid solution (B), and a 2% aqueous hydrochloric acid solution (C) were used for penetration cleaning. For comparison, the same amount of pure water was also used for through-cleaning. Each of the washed secondary silica cakes was further washed through with 1 kg of pure water and then dried in a hot air dryer at 105°C for 3 hours to obtain silica powder. The metal impurity content of the obtained silica powder was measured by IcP emission spectrometry. The measurement results are shown in Table-1.
表−１
実施例２
実施例１て用いた１次シリカケーキ４２ｇに純水を加え
全量３００ｇのスラリーを得た。これに１０％硫酸１２
ｇを加え（Ｄ）、スラリーのｐＨを１とした。同様に１
次シリカケーキ４２ｇと純水２５８ｇからシリカスラリ
ーを調製し各々１０％硫酸（Ｅ）、１０％弗化水素酸（
Ｆ）、１０％珪弗化水素酸（Ｇ）を添加しスラリーのｐ
Ｈを４とした。Table 1 Example 2 Pure water was added to 42 g of the primary silica cake used in Example 1 to obtain a slurry with a total amount of 300 g. Add 10% sulfuric acid 12
g was added (D) to adjust the pH of the slurry to 1. Similarly 1
Next, silica slurry was prepared from 42 g of silica cake and 258 g of pure water, and 10% sulfuric acid (E) and 10% hydrofluoric acid (
F), 10% hydrofluorosilicic acid (G) was added to reduce the p of the slurry.
H was set to 4.
ｐＨを調製したシリカスラリーを減圧ろ過後、ろ過ケー
キを各々０．５ ｋ ｇの純水で洗浄し得られた２次シ
リカケーキを１０５°Ｃの熱風乾燥話中で３時間乾燥し
、シリカ粉を得た。得られたシリカ粉の金属不純物含量
をＩＣＰ発光分析法により測定した結果、Ａｆ、Ｃａ、
Ｎａはいずれもｔｐｐｍ以下であった。また、Ｄ−Ｇ各
々のシリカ粉及び上記比較例１のシリカ粉の熱水抽出液
をイオンクロマト分析すると、Ｄの硫酸イオン含量（Ｓ
ｉ０２固形分換算）は１１００ｐｐ以上、Ｅの硫酸イオ
ン含量は１０ｐｐｍ以上であったか、Ｆ、 Ｇ及び比較
例１硫酸イオン含量はｌｐｐｍ以下であった。また、各
々のシリカ粉の熱水抽出液をイオンクワマド法によりア
ンモニア含量（Ｓｉ○２固形分換算）を測定すると、比
較例１は１１０００ｐｐ以上、Ｄ−Ｆのシリカ粉は各々
１１００ｐｐ以下であった。After filtering the pH-adjusted silica slurry under reduced pressure, each filter cake was washed with 0.5 kg of pure water, and the resulting secondary silica cake was dried in a hot air dryer at 105°C for 3 hours to obtain silica powder. I got it. As a result of measuring the metal impurity content of the obtained silica powder by ICP emission spectrometry, it was found that Af, Ca,
Na content was below tppm in all cases. In addition, when the hot water extract of the silica powder of D-G and the silica powder of Comparative Example 1 was analyzed by ion chromatography, the sulfate ion content (S
The sulfate ion content of E was 10 ppm or more, and the sulfate ion content of F, G, and Comparative Example 1 was 1 ppm or less. Further, when the ammonia content (in terms of Si○2 solid content) of the hot water extract of each silica powder was measured by the ion quamado method, it was found to be 11,000 pp or more in Comparative Example 1, and 1,100 pp or less in each of the silica powders of D-F.
特許出願人 日産化学工業株式会社Patent applicant: Nissan Chemical Industries, Ltd.
Claims (4)
の混合物とアンモニアとを水性媒体中で反応させて得ら
れるシリカスラリーまたはシリカケーキに酸成分を添加
して不純物を除去することを特徴とする高純度シリカの
製造法。(1) Impurities are removed by adding an acid component to a silica slurry or silica cake obtained by reacting hydrofluorosilicic acid, ammonium fluorosilicide, or a mixture thereof with ammonia in an aqueous medium. A method for producing high-purity silica.
カの製造法。(2) The method for producing high-purity silica according to claim 1, wherein the acid component is an inorganic acid.
求項２記載の高純度シリカの製造法。(3) The method for producing high-purity silica according to claim 2, wherein the inorganic acid is hydrofluoric acid or hydrosilicic acid.
キのｐＨを５以下とする請求項１記載の高純度シリカの
製造法。(4) The method for producing high-purity silica according to claim 1, wherein the pH of the silica slurry or silica cake after addition of the acid component is set to 5 or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2302863A JP3063147B2 (en) | 1990-11-08 | 1990-11-08 | Manufacturing method of high purity silica |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2302863A JP3063147B2 (en) | 1990-11-08 | 1990-11-08 | Manufacturing method of high purity silica |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04175218A true JPH04175218A (en) | 1992-06-23 |
| JP3063147B2 JP3063147B2 (en) | 2000-07-12 |
Family
ID=17914003
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2302863A Expired - Fee Related JP3063147B2 (en) | 1990-11-08 | 1990-11-08 | Manufacturing method of high purity silica |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3063147B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007005346A (en) * | 2005-06-21 | 2007-01-11 | Sanyu Rec Co Ltd | Method of removing metallic foreign matter |
| WO2010004925A1 (en) * | 2008-07-09 | 2010-01-14 | Kiya Shigeru | Method of recovering silicon, titanium, and fluorine |
| CN102502669A (en) * | 2011-10-26 | 2012-06-20 | 瓮福（集团）有限责任公司 | Preparation method of nanometer silicon dioxide |
-
1990
- 1990-11-08 JP JP2302863A patent/JP3063147B2/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007005346A (en) * | 2005-06-21 | 2007-01-11 | Sanyu Rec Co Ltd | Method of removing metallic foreign matter |
| WO2010004925A1 (en) * | 2008-07-09 | 2010-01-14 | Kiya Shigeru | Method of recovering silicon, titanium, and fluorine |
| JPWO2010004925A1 (en) * | 2008-07-09 | 2012-01-05 | 滋 木谷 | Method for recovering silicon, titanium and fluorine |
| JP5392576B2 (en) * | 2008-07-09 | 2014-01-22 | 滋 木谷 | Method for recovering silicon, titanium and fluorine |
| CN102502669A (en) * | 2011-10-26 | 2012-06-20 | 瓮福（集团）有限责任公司 | Preparation method of nanometer silicon dioxide |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3063147B2 (en) | 2000-07-12 |
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