JPH0891824A - Production of zirconium silicate - Google Patents
Production of zirconium silicateInfo
- Publication number
- JPH0891824A JPH0891824A JP26433894A JP26433894A JPH0891824A JP H0891824 A JPH0891824 A JP H0891824A JP 26433894 A JP26433894 A JP 26433894A JP 26433894 A JP26433894 A JP 26433894A JP H0891824 A JPH0891824 A JP H0891824A
- Authority
- JP
- Japan
- Prior art keywords
- zirconium
- silicate
- solution
- zirconium silicate
- sio
- 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.)
- Pending
Links
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 17
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 15
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 15
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 11
- 238000001354 calcination Methods 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 7
- 239000012670 alkaline solution Substances 0.000 claims description 6
- 230000003301 hydrolyzing effect Effects 0.000 claims description 5
- 239000007858 starting material Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 7
- 239000012265 solid product Substances 0.000 abstract description 5
- 229910052726 zirconium Inorganic materials 0.000 abstract description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 abstract description 3
- 239000003513 alkali Substances 0.000 abstract 1
- 229910052710 silicon Inorganic materials 0.000 abstract 1
- 239000010703 silicon Substances 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 description 9
- 239000000047 product Substances 0.000 description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 229910006501 ZrSiO Inorganic materials 0.000 description 4
- 229910007735 Zr—Si Inorganic materials 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000010908 decantation Methods 0.000 description 3
- 150000003377 silicon compounds Chemical class 0.000 description 3
- 150000003755 zirconium compounds Chemical class 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 150000004703 alkoxides Chemical class 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000005304 optical glass Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- ZGSOBQAJAUGRBK-UHFFFAOYSA-N propan-2-olate;zirconium(4+) Chemical compound [Zr+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] ZGSOBQAJAUGRBK-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- -1 zirconium silicates Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、ケイ酸ジルコニウム
（ＺｒＳｉＯ４化合物あるいはＺｒＳｉＯ４にＳｉＯ２
および／またはＺｒＯ２の混合したもので以下単にケイ
酸ジルコニウムという）の製造法に関し、詳しくは安価
なケイ酸ナトリウムとオキシ塩化ジルコニウムとを原料
として光学用ガラス用等として使用される高純度なケイ
酸ジルコニウムを工業的かつ安価に製造する方法に関す
るものである。The present invention relates to zirconium silicate (ZrSiO 4 compound or ZrSiO 4 and SiO 2
And / or a mixture of ZrO 2 and hereinafter simply referred to as zirconium silicate), more specifically, a high-purity silica used for optical glass or the like using inexpensive sodium silicate and zirconium oxychloride as raw materials. The present invention relates to a method for industrially and inexpensively producing zirconium acid.
【０００２】[0002]
【従来の技術】従来、ケイ酸ジルコニウムの製造法とし
ては、次の２法が主として研究され提案されている。 （１）ケイ酸エチル（Ｓｉ（ＯＣ２Ｈ５）４），オキシ
塩化ジルコニウム（ＺｒＯＣｌ２・８Ｈ２Ｏ）を使用し
たゾルーゲル法及び水熱合成法による方法。 （２）金属アルコキシドを出発原料としたジルコニウム
テトライソプロポキシド（Ｚｒ（ＯＰｒｉ）４）とケイ
酸エチル（Ｓｉ（ＯＣ２Ｈ５）４），Ｚｒ（ＯＰｒｉ）
４）−ＳｉＯ２ゾル，ＺｒＯＣｌ２・８Ｈ２Ｏ−Ｓｉ
（ＯＣ２Ｈ５）４及びＺｒＯＣｌ２・８Ｈ２Ｏ−ＳｉＯ
２ゾルの組合せによるゾルーゲル法。2. Description of the Related Art Conventionally, the following two methods have been mainly studied and proposed as a method for producing zirconium silicate. (1) A method by a sol-gel method and a hydrothermal synthesis method using ethyl silicate (Si (OC 2 H 5 ) 4 ), zirconium oxychloride (ZrOCl 2 · 8H 2 O). (2) Zirconium tetraisopropoxide (Zr (OPr i ) 4 ) and ethyl silicate (Si (OC 2 H 5 ) 4 ), Zr (OPr i ) starting from metal alkoxide
4) -SiO 2 sol, ZrOCl 2 · 8H 2 O- Si
(OC 2 H 5) 4 and ZrOCl 2 · 8H 2 O-SiO
Sol-gel method with a combination of two sols.
【０００３】上記の従来の製造法にあっては、ケイ素化
合物の出発原料がケイ酸エチル（Ｓｉ（ＯＣ
２Ｈ５）４）やＳｉＯ２ゾルを使用したジルコニウム化
合物との組合せによる方法であるため、 （イ）ケイ酸エチルが非常に高価であること。 （ロ）ＳｉＯ２ゾルは金属アルコキシドよりは安価であ
るがまだ非常に高価であること。 等の致命的な欠点があり、従って極めて高価なケイ酸ジ
ルコニウムしか製造できないという問題点があった。In the above conventional manufacturing method, the starting material of the silicon compound is ethyl silicate (Si (OC
(2 ) Ethyl silicate is very expensive because it is a method of combining 2 H 5 ) 4 ) and a zirconium compound using SiO 2 sol. (B) SiO 2 sol is cheaper than metal alkoxide, but still very expensive. However, there is a problem that only extremely expensive zirconium silicate can be produced.
【０００４】[0004]
【発明が解決しようとする課題】本発明は、従来法の問
題点を解決し、安価なケイ素化合物とジルコニウム化合
物とを出発原料として、しかもその製造工程も比較的単
純であり、安価でかつ高純度なケイ酸ジルコニウムを工
業的に量産できる製造法を提案するものである。DISCLOSURE OF THE INVENTION The present invention solves the problems of the conventional method, uses an inexpensive silicon compound and a zirconium compound as starting materials, and has a relatively simple manufacturing process, which is inexpensive and highly expensive. It proposes a manufacturing method capable of industrially mass-producing pure zirconium silicate.
【０００５】[0005]
【課題を解決するための手段】本発明者らは、上記課題
を解決すべく鋭意研究の結果、ケイ素化合物として工業
的に量産されている安価なケイ酸ナトリウムと、一方ジ
ルコニウム化合物としてオキシ塩化ジルコニウムを出発
原料として、両者を溶存する溶液を加水分解し、生成し
た固形生成物を所定温度でか焼することにより、高純度
なケイ酸ジルコニウムを安価に製造することができると
の知見を得て、本発明をなすに至ったのである。As a result of earnest research to solve the above problems, the present inventors have found that inexpensive sodium silicate that is industrially mass-produced as a silicon compound and zirconium oxychloride as a zirconium compound. As a starting material, by hydrolyzing a solution in which both are dissolved, and calcining the produced solid product at a predetermined temperature, it was found that it is possible to inexpensively produce high-purity zirconium silicate. Thus, the present invention has been completed.
【０００６】第１発明は、オキシ塩化ジルコニウムとケ
イ酸ナトリウムとを溶存する溶液を加水分解し、得られ
た固形分をか焼することを特徴とするケイ酸ジルコニウ
ムの製造法であり、The first invention is a method for producing zirconium silicate, which comprises hydrolyzing a solution in which zirconium oxychloride and sodium silicate are dissolved and calcining the obtained solid content,
【０００７】第２発明は、オキシ塩化ジルコニウムとケ
イ酸ナトリウムとを溶存する溶液をアルカリ溶液により
所定ｐＨ範囲に維持しながら加水分解し、得られた固形
分をか焼することを特徴とするケイ酸ジルコニウムの製
造法を提供するものである。A second invention is characterized in that a solution in which zirconium oxychloride and sodium silicate are dissolved is hydrolyzed with an alkaline solution while maintaining a predetermined pH range, and the obtained solid content is calcined. A method for producing zirconium acid is provided.
【０００８】上記第１，２発明において、か焼温度が１
０００℃以上であり、溶液中のオキシ塩化ジルコニウム
とケイ酸ナトリウムとがＺｒＯ２／ＳｉＯ２比で当量で
あることが好ましいのである。In the first and second inventions, the calcination temperature is 1
It is preferably 000 ° C. or higher, and zirconium oxychloride and sodium silicate in the solution are equivalent in ZrO 2 / SiO 2 ratio.
【０００９】即ち、本発明は、オキシ塩化ジルコニウム
（ＺｒＯＣｌ２・８Ｈ２Ｏ）とケイ酸ナトリウム（Ｎａ
２Ｏ・ｎＳｉＯ２・ｘＨ２Ｏ：ｎ＝２〜４）をそれぞれ
別個に水に溶解した水溶液をＺｒＯ２／ＳｉＯ２比が等
モルになるように混合し、該混合溶液を加水分解するこ
とにより得られた固形生成物を固液分離し、洗浄・乾燥
・粉砕した後、１０００℃以上の温度でか焼することを
特徴とするケイ酸ジルコニウムの製造法である。That is, according to the present invention, zirconium oxychloride (ZrOCl 2 .8H 2 O) and sodium silicate (Na) are used.
2 O · nSiO 2 · xH 2 O: n = 2~4) were mixed to an aqueous solution prepared by dissolving separately the water, respectively ZrO 2 / SiO 2 ratio is equimolar, hydrolyzing the mixed solution The method for producing zirconium silicate is characterized in that the solid product obtained in (1) is subjected to solid-liquid separation, washed, dried and pulverized, and then calcined at a temperature of 1000 ° C. or higher.
【００１０】本発明は上記のように構成されているの
で、従来法のように非常に高価なケイ酸エチルやＳｉＯ
２ゾルを使用することなく、工業的に量産されている安
価なケイ酸ナトリウムとオキシ塩化ジルコニウムを出発
原料として、しかも比較的簡単な製造工程で、安価にし
てかつ高純度なケイ酸ジルコニウムを製造することがで
きるのである。Since the present invention is constructed as described above, ethyl silicate and SiO, which are very expensive as in the conventional method, are used.
Manufacturing high-purity zirconium silicate at low cost by using inexpensive sodium silicate and zirconium oxychloride, which are industrially mass-produced, as starting materials and using a relatively simple manufacturing process without using 2 sol You can do it.
【００１１】[0011]
【作用】オキシ塩化ジルコニウム（ＺｒＯＣｌ２・８Ｈ
２Ｏ）とケイ酸ナトリウム（Ｎａ２Ｏ・ｎＳｉＯ２・ｘ
Ｈ２Ｏ：ｎ＝２〜４）とを出発原料として、各別々に水
に溶解して各水溶液を作製する。これら両水溶液をＺｒ
Ｏ２／ＳｉＯ２比が等モルになるように混合し、混合溶
液を作製する。この混合溶液はオキシ塩化ジルコニウム
が水に溶解すると、解離してＨＣｌを副生成するため酸
性を示す。[Action] zirconium oxychloride (ZrOCl 2 · 8H
2 O) and sodium silicate (Na 2 O ・ nSiO 2・ x
H 2 O: n = 2 to 4) as starting materials, and dissolved in water separately to prepare respective aqueous solutions. Zr of these two aqueous solutions
Mix so that the O 2 / SiO 2 ratio becomes equimolar to prepare a mixed solution. This mixed solution is acidic because zirconium oxychloride is dissolved in water and dissociates to generate HCl as a by-product.
【００１２】この混合溶液を別に準備したアルカリ性水
溶液中に添加し、該溶液が常にアルカリ性を維持するよ
うに調整することにより、加水分解させてＺｒ−Ｓｉ複
合生成物を生成させる。This mixed solution is added to an alkaline aqueous solution prepared separately, and the solution is adjusted so as to always maintain the alkaline property, whereby it is hydrolyzed to form a Zr-Si composite product.
【００１３】得られたＺｒ−Ｓｉ複合生成物をデカンテ
ーションにより洗浄した後、固液分離し、更に充分洗浄
してＮａ＋，Ｃｌ−等をほぼ完全に除去した後、乾燥す
る。この乾燥された固形生成物を粉砕し、１０００℃以
上でか焼してケイ酸ジルコニウムを製造する。[0013] The resulting Zr-Si composite product was washed by decantation, solid-liquid separation, Na + and washed more sufficiently, Cl - was removed almost completely and the like, and dried. The dried solid product is crushed and calcined at 1000 ° C. or higher to produce zirconium silicate.
【００１４】また、上記方法で作製したＺｒＯ２／Ｓｉ
Ｏ２比が等モルの混合溶液にアルカリ溶液を該混合溶液
がアルカリ性になるまで加えて、Ｚｒ−Ｓｉ複合生成物
を生成させる。このＺｒ−Ｓｉ複合生成物をデカンテー
ションにより洗浄した後、固液分離し、更に充分洗浄
し、上記同様にＮａ＋やＣｌ−をほぼ完全に除去した
後、乾燥する。Further, ZrO 2 / Si produced by the above method
An alkaline solution is added to a mixed solution having an equimolar ratio of O 2 until the mixed solution becomes alkaline to form a Zr—Si composite product. The Zr-Si composite product is washed by decantation, solid-liquid separated, further sufficiently washed, and Na + and Cl − are almost completely removed as in the above, and then dried.
【００１５】この乾燥物を粉砕した後、１０００℃以上
でか焼することにより、ケイ酸ジルコニウムを製造して
もよい。Zirconium silicate may be produced by pulverizing the dried product and calcining it at 1000 ° C. or higher.
【００１６】上記の混合溶液のＺｒＯ２／ＳｉＯ２のモ
ル比がずれると、その分ＺｒＯ２あるいはＳｉＯ２が過
剰となる。また、か焼温度が１０００℃未満ではケイ酸
ジルコニウムが生成され難い。以下、本発明の実施例を
説明する。If the ZrO 2 / SiO 2 molar ratio of the mixed solution deviates, ZrO 2 or SiO 2 becomes excessive by that much. Further, if the calcination temperature is less than 1000 ° C, zirconium silicate is difficult to be generated. Examples of the present invention will be described below.
【００１７】[0017]
実施例１ まず、オキシ塩化ジルコニウム（ＺｒＯＣｌ２・８Ｈ２
Ｏ）を水に溶解し、ＺｒＯ２が５０ｇ／ｌになるように
調整し、オキシ塩化ジルコニウム溶存溶液を作製した。Example 1 First, zirconium oxychloride (ZrOCl 2 .8H 2
O) was dissolved in water and adjusted so that ZrO 2 was 50 g / l to prepare a zirconium oxychloride dissolved solution.
【００１８】次に、ケイ酸ナトリウム３号（ＳｉＯ２：
２８．７３％，Ｎａ２Ｏ：９．３％）を水に溶解させ、
ＳｉＯ２が１２．２ｇ／ｌになるように調整し、ケイ酸
ナトリウム溶存溶液を作製した。Next, sodium silicate No. 3 (SiO 2 :
28.73%, Na 2 O: 9.3%) in water,
SiO 2 was adjusted to 12.2 g / l to prepare a sodium silicate dissolved solution.
【００１９】これらの溶液をＺｒＯ２／ＳｉＯ２比が等
モルになるように混合して、混合溶液を作製した。These solutions were mixed so that the ZrO 2 / SiO 2 ratio was equimolar to prepare a mixed solution.
【００２０】次に、別にアンモニア水（ＮＨ４ＯＨ）に
よりｐＨ９に調整したアルカリ性溶液を１ｌ作り、この
アルカリ性溶液中に撹拌しなから上記混合溶液を添加す
ると共に、この反応系アルカリ性溶液のｐＨを常に９に
保持するためにアンモニア水を同時に添加し調整した。Next, separately prepare 1 liter of an alkaline solution adjusted to pH 9 with aqueous ammonia (NH 4 OH), add the above mixed solution to the alkaline solution without stirring, and adjust the pH of this reaction system alkaline solution. Ammonia water was added at the same time so as to keep the value at 9 at all times.
【００２１】上記反応系内で加水分解反応により生成し
た固形生成物をデカンテーションにより洗浄し、固液分
離した後、更に洗浄水中にＮａ＋やＣｌ−が検出されな
くなるまで洗浄し乾燥した。この乾燥物を粉砕し１１５
０℃でか焼した。The solid product produced by the hydrolysis reaction in the above reaction system was washed by decantation, solid-liquid separated, and further washed and dried until Na + and Cl − were not detected in the wash water. The dried product is crushed to 115
It was calcined at 0 ° C.
【００２２】得られたか焼物をＸ綿回析により同定した
結果、ＺｒＳｉＯ４が生成されていることが確認され
た。As a result of identifying the obtained calcined product by X-cotton diffraction, it was confirmed that ZrSiO 4 was produced.
【００２３】比較例 酸化ジルコニウム（ＺｒＯ２）と二酸化ケイ素（ＳｉＯ
２）を等モル計量し、試験用振動ボールミルに装入し、
粉砕・混合を行なった。この混合粉体をるつぼに入れ１
５００℃でか焼した。Comparative Example Zirconium oxide (ZrO 2 ) and silicon dioxide (SiO 2
2 ) are weighed equimolarly, charged into a test vibration ball mill,
It was crushed and mixed. Put this mixed powder in a crucible 1
It was calcined at 500 ° C.
【００２４】得られたか焼粉体をＸ線回析により同定し
た結果、ＺｒＯ２とＳｉＯ２それぞれのピークがでてお
り、ＺｒＳｉＯ４は同定されなかった。The obtained calcined powder was identified by X-ray diffraction. As a result, peaks of ZrO 2 and SiO 2 were observed, and ZrSiO 4 was not identified.
【００２５】[0025]
【発明の効果】ケイ酸ジルコニウムは、光学用硝子とし
て使用するためには、着色不純物の共存がほどんどない
高純度のものが要求される。その合成法は極めて難し
く、余り研究されておらず、また前記のように非常に高
価な出発原料を使用しなくてはならず、天然産のものも
要求に適合した品質のものは、その量も限られており、
安価で工業的に使用可能なケイ酸ジルコニウムは、現在
市場に全く見当たらない。In order to use zirconium silicate as an optical glass, it is required that the zirconium silicate has a high degree of purity and is free from the coexistence of colored impurities. Its synthetic method is extremely difficult, has not been well researched, and as mentioned above, it has to use very expensive starting materials. Is also limited,
No inexpensive and industrially usable zirconium silicates are currently found on the market.
【００２６】本発明によれば、出発原料として従来のよ
うに非常に高価なケイ酸エチルやＳｉＯ２ゾル等を使用
することなく、工業的に量産されているケイ酸ナトリウ
ムとオキシ塩化ジルコニウムを出発原料とし、しかもそ
の製造工程も比較的単純であり、高純度なケイ酸ジルコ
ニウムを工業的に安価に製造することができるのであ
る。According to the present invention, industrially mass-produced sodium silicate and zirconium oxychloride are used as starting materials without using very expensive ethyl silicate, SiO 2 sol and the like as in the past. As a raw material, and the manufacturing process thereof is relatively simple, high-purity zirconium silicate can be industrially manufactured at low cost.
Claims (5)
ウムとを溶存する溶液を加水分解し、得られた固形分を
か焼することを特徴とするケイ酸ジルコニウムの製造
法。1. A method for producing zirconium silicate, which comprises hydrolyzing a solution in which zirconium oxychloride and sodium silicate are dissolved and calcining the obtained solid content.
ウムとを溶存する溶液をアルカリ溶液により所定ｐＨ範
囲に維持しながら加水分解し、得られた固形分をか焼す
ることを特徴とするケイ酸ジルコニウムの製造法。2. A zirconium silicate characterized by hydrolyzing a solution in which zirconium oxychloride and sodium silicate are dissolved in an alkaline solution while maintaining a predetermined pH range and calcining the obtained solid content. Manufacturing method.
とを特徴とする請求項１又は２記載のケイ酸ジルコニウ
ムの製造法。3. The method for producing zirconium silicate according to claim 1, wherein the calcination temperature is 1000 ° C. or higher.
ケイ酸ナトリウムとがＺｒＯ２／ＳｉＯ２比で当量であ
ることを特徴とする請求項１，２又は３記載のケイ酸ジ
ルコニウムの製造法。4. The method for producing zirconium silicate according to claim 1, wherein zirconium oxychloride and sodium silicate in the solution are equivalent in ZrO 2 / SiO 2 ratio.
・乾燥及び粉砕することを特徴とする請求項１，２，３
又は４記載のケイ酸ジルコニウムの製造法。5. The solid content is separated from the solid content before calcination, and the solid content is washed, dried and pulverized.
Alternatively, the method for producing zirconium silicate according to item 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26433894A JPH0891824A (en) | 1994-09-21 | 1994-09-21 | Production of zirconium silicate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP26433894A JPH0891824A (en) | 1994-09-21 | 1994-09-21 | Production of zirconium silicate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0891824A true JPH0891824A (en) | 1996-04-09 |
Family
ID=17401790
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP26433894A Pending JPH0891824A (en) | 1994-09-21 | 1994-09-21 | Production of zirconium silicate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0891824A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116751467A (en) * | 2023-06-28 | 2023-09-15 | 景德镇陶瓷大学 | A method for preparing zirconium silicate-based wrapped pigments by non-aqueous precipitation method |
| CN119736736A (en) * | 2025-02-28 | 2025-04-01 | 上海南极星高科技股份有限公司 | Preparation method of high-temperature-resistant zirconium silicate nanofiber |
-
1994
- 1994-09-21 JP JP26433894A patent/JPH0891824A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116751467A (en) * | 2023-06-28 | 2023-09-15 | 景德镇陶瓷大学 | A method for preparing zirconium silicate-based wrapped pigments by non-aqueous precipitation method |
| CN119736736A (en) * | 2025-02-28 | 2025-04-01 | 上海南极星高科技股份有限公司 | Preparation method of high-temperature-resistant zirconium silicate nanofiber |
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