JPH0524835A - Production of highly pure amorphous zinc stannate powder - Google Patents
Production of highly pure amorphous zinc stannate powderInfo
- Publication number
- JPH0524835A JPH0524835A JP20139591A JP20139591A JPH0524835A JP H0524835 A JPH0524835 A JP H0524835A JP 20139591 A JP20139591 A JP 20139591A JP 20139591 A JP20139591 A JP 20139591A JP H0524835 A JPH0524835 A JP H0524835A
- Authority
- JP
- Japan
- Prior art keywords
- aqueous solution
- zinc stannate
- amorphous zinc
- powder
- zinc
- 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
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は高純度の無定形錫酸亜鉛
粉末を容易に製造する方法に関する。本発明で得られる
粉末は難燃剤として利用することができ、ポリマーに添
加分散させることにより優れた難燃性や有毒ガスの発煙
抑制効果を達成することができる。FIELD OF THE INVENTION The present invention relates to a method for easily producing high-purity amorphous zinc stannate powder. The powder obtained in the present invention can be used as a flame retardant, and by adding and dispersing it in a polymer, excellent flame retardancy and toxic gas smoke suppressing effect can be achieved.
【０００２】[0002]
【従来技術】無定形錫酸亜鉛粉末は、添加型難燃剤とし
てポリマー中に分散させることにより、ポリマーに難燃
性および有毒ガス発煙抑制効果を与えることが報告され
ている。従来、無定形錫酸亜鉛は、まずヒドロキシ錫酸
Naを得、次にこのNaを亜鉛に置換する方法によって製造
されている。具体的には、ヒドロキシ錫酸Na水溶液と亜
鉛塩水溶液を混合して、ヒドロキシ錫酸亜鉛沈殿を生成
させ、この沈殿を濾別し乾燥後、400℃に焼成すること
により無定形錫酸亜鉛粉末を製造している。ところが、
この方法では、生成するヒドロキシ錫酸亜鉛が微細化し
易いため、デカンテーションや濾別の際に遠心分離など
の機械的操作や凝集剤の添加などの化学的操作が必要で
ある。またヒドロキシ錫酸Naを経てヒドロキシ錫酸亜鉛
を製造するので製造工程が煩雑である。またヒドロキシ
錫酸Naを原料として直接用いるとヒドロキシ錫酸Naのコ
ストが高いので量産に向かず、工業的な実施に適さな
い。2. Description of the Related Art It has been reported that amorphous zinc stannate powder, when dispersed in a polymer as an additive flame retardant, imparts flame retardancy and toxic gas smoke suppression effects to the polymer. Conventionally, amorphous zinc stannate was first prepared from hydroxystannic acid.
It is produced by the method of obtaining Na and then replacing this Na with zinc. Specifically, a sodium hydroxystannate aqueous solution and a zinc salt aqueous solution are mixed to form a zinc hydroxystannate precipitate, which precipitate is separated by filtration, dried, and then baked at 400 ° C. to form an amorphous zinc stannate powder. Are manufactured. However,
In this method, since zinc hydroxystannate to be produced is easily micronized, mechanical operations such as centrifugation and chemical operations such as addition of a flocculant are required at the time of decantation or filtration. Further, since zinc hydroxystannate is produced through Na hydroxystannate, the manufacturing process is complicated. Further, if Na hydroxystannate is directly used as a raw material, the cost of Na hydroxystannate is high, so that it is not suitable for mass production and is not suitable for industrial implementation.
【０００３】[0003]
【発明の解決課題】以上のように従来の製造方法は製造
工程が煩雑であり、コスト面からも工業的実施に適さな
い問題がある。本発明は従来の製造方法における上記問
題を解決するものであって、安価な原料を用い、水溶液
中で直接に無定形錫酸亜鉛沈殿を生成させ、容易に無定
形錫酸亜鉛粉末を製造できる方法を提供することを目的
とする。As described above, the conventional manufacturing method has a problem that the manufacturing process is complicated and is not suitable for industrial implementation from the viewpoint of cost. The present invention solves the above-mentioned problems in the conventional manufacturing method, and by using an inexpensive raw material, an amorphous zinc stannate precipitate can be directly produced in an aqueous solution to easily produce an amorphous zinc stannate powder. The purpose is to provide a method.
【０００４】[0004]
【課題の解決手段：発明の構成】本発明によれば、第二
錫イオンと亜鉛イオンを含む酸性水溶液と炭酸アンモニ
ウムまたは炭酸水素アンモニウム水溶液とを混合し、水
溶液中で直接に無定形錫酸亜鉛沈殿を生成させ、該沈殿
を濾別し乾燥させることを特徴とする高純度無定形錫酸
亜鉛粉末の製造方法が提供される。According to the present invention, an acidic aqueous solution containing stannic ions and zinc ions is mixed with an aqueous solution of ammonium carbonate or ammonium hydrogencarbonate, and the amorphous zinc stannate is directly added to the aqueous solution. Provided is a method for producing a high-purity amorphous zinc stannate powder, which comprises producing a precipitate, filtering the precipitate, and drying.
【０００５】本発明は、第二錫イオンと亜鉛イオンを含
む酸性水溶液と炭酸アンモニウム水溶液または炭酸水素
アンモニウム水溶液を原料として用いる。第二錫イオン
源としては、塩化第二錫、金属錫などが用いられる。な
お第一錫イオンを用いると良好な錫酸亜鉛沈殿を得るこ
とができない。亜鉛イオン源としては酸化亜鉛、硫酸亜
鉛、金属亜鉛などが用いられる。これら塩化第二錫、酸
化亜鉛などを塩酸あるいは濃塩酸、硫酸などに溶解した
錫／亜鉛酸性水溶液が用いられる。In the present invention, an acidic aqueous solution containing stannic and zinc ions and an aqueous solution of ammonium carbonate or an aqueous solution of ammonium hydrogen carbonate are used as raw materials. As the stannic ion source, stannic chloride, metallic tin, etc. are used. If stannous ions are used, a good zinc stannate precipitate cannot be obtained. As the zinc ion source, zinc oxide, zinc sulfate, metallic zinc, etc. are used. A tin / zinc acidic aqueous solution obtained by dissolving these stannic chloride, zinc oxide, etc. in hydrochloric acid, concentrated hydrochloric acid, sulfuric acid or the like is used.
【０００６】第二錫イオンと亜鉛イオンを含む酸性水溶
液と、炭酸アンモニウムないし炭酸水素アンモニウム水
溶液とを混合すると、水溶液中で直接に無定形の錫酸亜
鉛の沈殿が生じる。錫／亜鉛酸性水溶液と炭酸アンモニ
ウム水溶液または炭酸水素アンモニウム水溶液とを混合
する場合、両液を同時に混合してもよく、又は、何れか
一方を他方に滴下してもよい。生成した無定形錫酸亜鉛
沈殿の粒径は0.2〜0.4 μmであり、デカンテーションに
適し、かつポリマーに分散させるのに適当な大きさであ
る。更に上記沈殿はデカンテーションによって残留する
塩分を容易に除去することができるので、残留塩分によ
って表面処理が妨害されることがなく、得られた無定形
錫酸亜鉛粒子の表面処理も容易になる。必要に応じて粒
子の表面処理を適宜行なうことによりポリマーに対する
分散性を高めることができる。また本発明の方法によれ
ば、アルカリ溶液として炭酸アンモニウム水溶液または
炭酸水素アンモニウム水溶液を用いるので、沈澱中にア
ルカリ金属が残留する虞がなく高純度の無定形錫酸亜鉛
粉末を製造することができる。本発明の無定形錫酸亜鉛
粉末は不純物の混入を嫌う電子材料の封止剤などに対す
る難燃剤として用いると非常に効果的である。When an acidic aqueous solution containing stannic and zinc ions is mixed with an ammonium carbonate or ammonium hydrogen carbonate aqueous solution, amorphous zinc stannate precipitates directly in the aqueous solution. When the tin / zinc acidic aqueous solution and the ammonium carbonate aqueous solution or the ammonium hydrogen carbonate aqueous solution are mixed, both solutions may be mixed at the same time, or one of them may be dropped into the other. The particle size of the formed amorphous zinc stannate precipitate is 0.2 to 0.4 μm, which is suitable for decantation and suitable for dispersion in the polymer. Further, since the above-mentioned precipitation can easily remove the residual salt content by decantation, the surface treatment is not disturbed by the residual salt content, and the surface treatment of the obtained amorphous zinc stannate particles is also facilitated. The dispersibility in the polymer can be enhanced by appropriately performing the surface treatment of the particles, if necessary. Further, according to the method of the present invention, since an aqueous solution of ammonium carbonate or an aqueous solution of ammonium hydrogen carbonate is used as the alkaline solution, it is possible to produce a high-purity amorphous zinc stannate powder without the risk of alkali metal remaining during precipitation. . The amorphous zinc stannate powder of the present invention is very effective when used as a flame retardant for an electronic material sealant and the like, which does not want to contain impurities.
【０００７】実施例１ 第二塩化錫の60％塩酸溶液21.7g(錫 0.05mol相当)と、
酸化亜鉛4.0g(亜鉛0.05mol相当)と、濃塩酸 10 mlとを
混合して錫／亜鉛酸性水溶液を調製した。この溶液と3.
5mol/lの炭酸アンモニウム水溶液 150mlを混合して錫酸
亜鉛の沈殿を生成させた。沈殿生成後デカンテーション
により残留塩分を除去し、沈殿を濾別して風乾し、9.7g
の白色粉末を得た(収率 83.6％)。この粉末をＸ線回折
法により測定したところ図１に示されるように、結晶性
ヒドロキシ錫酸亜鉛や他の錫・亜鉛化合物を含まない、
無定形錫酸亜鉛であることが確認された。またその比表
面積は190 m2/gであった。この無定形錫酸亜鉛粉末を塩
化ビニル樹脂に混練し分散させてシートを製造し、この
シートの限界酸素指数(LOI)をJIS K7201の試験方法に従
って測定した。この結果を表１に示した。本実施例のシ
ートは上記無定形錫酸亜鉛粉末を混入しないものに比較
して LOI値が高く難燃性に優れる。Example 1 21.7 g of 60% hydrochloric acid solution of stannous chloride (corresponding to 0.05 mol of tin),
4.0 g of zinc oxide (corresponding to 0.05 mol of zinc) and 10 ml of concentrated hydrochloric acid were mixed to prepare a tin / zinc acidic aqueous solution. With this solution and 3.
150 ml of a 5 mol / l ammonium carbonate aqueous solution was mixed to form a precipitate of zinc stannate. After the precipitate is formed, the residual salt is removed by decantation, and the precipitate is filtered off and air-dried to give 9.7 g.
Was obtained as a white powder (yield 83.6%). When this powder was measured by an X-ray diffraction method, as shown in FIG. 1, crystalline zinc hydroxystannate and other tin-zinc compounds were not contained,
It was confirmed to be amorphous zinc stannate. The specific surface area was 190 m 2 / g. This amorphous zinc stannate powder was kneaded and dispersed in vinyl chloride resin to produce a sheet, and the limiting oxygen index (LOI) of this sheet was measured according to the test method of JIS K7201. The results are shown in Table 1. The sheet of this example has a high LOI value and excellent flame retardancy as compared with the sheet not mixed with the amorphous zinc stannate powder.
【０００８】実施例２ 第二塩化錫の60％塩酸溶液21.7g(錫 0.05mol相当)と、
酸化亜鉛4.0g(亜鉛0.05mol相当)と、濃塩酸10mlとを混
合して錫／亜鉛酸性水溶液を調製した。この溶液と1 mo
l/lの炭酸アンモニウム水溶液150mlを混合し、錫酸亜鉛
の沈殿を生成させた。沈殿生成後デカンテーションによ
り残留塩分を除去し、沈殿を濾別して風乾し、10.8gの
無定形錫酸亜鉛の白色粉末を得た(収率 93.1％)。得ら
れた錫酸亜鉛粉末の比表面積は170 m2/gであった。この
無定形錫酸亜鉛粉末を塩化ビニル樹脂に混練し分散させ
てシートを製造し、このシートの限界酸素指数(LOI)を
測定した。この結果を表１に示した。本実施例のシート
は上記無定形錫酸亜鉛粉末を混入しないものに比較して
LOI値が高く難燃性に優れる。Example 2 21.7 g of 60% hydrochloric acid solution of stannic chloride (corresponding to 0.05 mol of tin),
4.0 g of zinc oxide (corresponding to 0.05 mol of zinc) and 10 ml of concentrated hydrochloric acid were mixed to prepare a tin / zinc acidic aqueous solution. This solution and 1 mo
150 ml of a 1 / l ammonium carbonate aqueous solution was mixed to form a precipitate of zinc stannate. After the precipitate was formed, the residual salt was removed by decantation, and the precipitate was filtered off and air-dried to obtain 10.8 g of white powder of amorphous zinc stannate (yield 93.1%). The specific surface area of the obtained zinc stannate powder was 170 m 2 / g. This amorphous zinc stannate powder was kneaded and dispersed in vinyl chloride resin to produce a sheet, and the limiting oxygen index (LOI) of this sheet was measured. The results are shown in Table 1. The sheet of this example is compared with the sheet not mixed with the above-mentioned amorphous zinc stannate powder.
High LOI value and excellent flame retardancy.
【０００９】実施例３ 第二塩化錫の60％塩酸溶液21.7g(錫 0.05mol相当)と、
酸化亜鉛4.0g(亜鉛0.05mol相当)と、濃塩酸10mlとを混
合して錫／亜鉛酸性水溶液を調製した。この溶液と 3.5
mol/lの炭酸水素アンモニウム水溶液150mlを混合し、錫
酸亜鉛の沈殿を生成させた。沈殿生成後デカンテーショ
ンにより残留塩分を除去し、沈殿を濾別して風乾し、1
0.6gの無定形錫酸亜鉛の白色粉末を得た(収率 91.4
％)。得られた錫酸亜鉛粉末の比表面積は190m2/gであっ
た。この無定形錫酸亜鉛粉末を塩化ビニル樹脂に混練し
分散させてシートを製造し、このシートの限界酸素指数
(LOI)を測定した。この結果を表１に示した。本実施例
のシートは上記無定形錫酸亜鉛粉末を混入しないものに
比較して LOI値が高く難燃性に優れる。Example 3 21.7 g of 60% hydrochloric acid solution of stannic chloride (corresponding to 0.05 mol of tin),
4.0 g of zinc oxide (corresponding to 0.05 mol of zinc) and 10 ml of concentrated hydrochloric acid were mixed to prepare a tin / zinc acidic aqueous solution. 3.5 with this solution
150 ml of a mol / l ammonium hydrogen carbonate aqueous solution was mixed to form a precipitate of zinc stannate. After the precipitate is formed, the residual salt is removed by decantation, and the precipitate is filtered off and air dried.
0.6 g of white zinc stannate powder was obtained (yield 91.4
%). The specific surface area of the obtained zinc stannate powder was 190 m 2 / g. This amorphous zinc stannate powder is kneaded and dispersed in vinyl chloride resin to produce a sheet, and the limiting oxygen index of this sheet
(LOI) was measured. The results are shown in Table 1. The sheet of this example has a high LOI value and excellent flame retardancy as compared with the sheet not mixed with the amorphous zinc stannate powder.
【００１０】[0010]
【表１】 ────────────────────────── 試料 ZnSn(OH)6添加量(wt%) 限界酸素指数(LOI) ────────────────────────── 実施例１ ２ 24.0 ５ 25.5 実施例２ ２ 24.0 ５ 25.5 実施例３ ２ 24.0 ５ 25.5 ────────────────────────── 比較例 − 22.5 ──────────────────────────[Table 1] ────────────────────────── Sample ZnSn (OH) 6 addition amount (wt%) Limiting oxygen index (LOI) ── ──────────────────────── Example 1 2 24.0 5 25.5 Example 2 2 24.0 5 25.5 Example 3 2 24.0 5 25.5 ───── ───────────────────── Comparative example −22.5 ────────────────────────── ─
【００１１】[0011]
【発明の効果】本発明の製造方法によれば、無定形錫酸
亜鉛を、錫／亜鉛酸性水溶液とアンモニア水溶液とを混
合する簡便な方法によって直接に水溶液中で沈殿生成で
き、従来不可欠であった焼成工程を必要とせずに無定形
錫酸亜鉛粉末を製造できる実用上大きな利点を有する。
しかも得られる沈殿の粒径もデカンテーションに適する
大きさであり、また残留塩類も容易に洗浄除去できるな
ど工業生産に適する利点を有する。更に生成する沈澱中
にアルカリ金属等が混入する虞がなく高純度の無定形錫
酸亜鉛粉末を得ることができる。EFFECTS OF THE INVENTION According to the production method of the present invention, amorphous zinc stannate can be directly precipitated in an aqueous solution by a simple method of mixing a tin / zinc acidic aqueous solution and an aqueous ammonia solution, which is indispensable conventionally. It has a great practical advantage that an amorphous zinc stannate powder can be produced without the need for a firing step.
Moreover, the particle size of the obtained precipitate is suitable for decantation, and residual salts can be easily washed and removed, which is an advantage suitable for industrial production. Further, it is possible to obtain a high-purity amorphous zinc stannate powder without fear that an alkali metal or the like is mixed in the generated precipitate.
【図１】 実施例１で製造した無定形錫酸亜鉛粉末のＸ
線回折図。1 is the X of the amorphous zinc stannate powder produced in Example 1.
Line diffraction diagram.
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成４年４月１３日[Submission date] April 13, 1992
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１０[Correction target item name] 0010
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００１０】[0010]
【表１】 [Table 1]
【手続補正２】[Procedure Amendment 2]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１１[Correction target item name] 0011
【補正方法】変更[Correction method] Change
【補正内容】[Correction content]
【００１１】[0011]
【発明の効果】本発明の製造方法によれば、無定形錫酸
亜鉛を、錫／亜鉛酸性水溶液と炭酸アンモニウム又は炭
酸水素アンモニウム水溶液とを混合する簡便な方法によ
って直接に水溶液中で沈殿生成でき、従来不可欠であっ
た焼成工程を必要とせずに無定形錫酸亜鉛粉末を製造で
きる実用上大きな利点を有する。しかも得られる沈殿の
粒径もデカンテーションに適する大きさであり、また残
留塩類も容易に洗浄除去できるなど工業生産に適する利
点を有する。更に生成する沈澱中にアルカリ金属等が混
入する虞がなく高純度の無定形錫酸亜鉛粉末を得ること
ができる。According to the production method of the present invention, amorphous zinc stannate can be directly precipitated in an aqueous solution by a simple method of mixing tin / zinc acidic aqueous solution with ammonium carbonate or ammonium hydrogencarbonate aqueous solution. However, there is a great practical advantage that an amorphous zinc stannate powder can be produced without requiring a firing step which has been conventionally indispensable. Moreover, the particle size of the obtained precipitate is suitable for decantation, and residual salts can be easily washed and removed, which is an advantage suitable for industrial production. Further, it is possible to obtain a high-purity amorphous zinc stannate powder without fear that an alkali metal or the like is mixed in the generated precipitate.
Claims (1)
溶液と炭酸アンモニウムまたは炭酸水素アンモニウム水
溶液とを混合し、水溶液中で直接に無定形錫酸亜鉛沈殿
を生成させ、該沈殿を濾別し乾燥させることを特徴とす
る高純度無定形錫酸亜鉛粉末の製造方法。Claims: 1. An acidic aqueous solution containing stannic and zinc ions is mixed with an aqueous solution of ammonium carbonate or ammonium hydrogen carbonate to directly form an amorphous zinc stannate precipitate in the aqueous solution, A method for producing a high-purity amorphous zinc stannate powder, characterized in that the precipitate is filtered off and dried.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20139591A JP3166013B2 (en) | 1991-07-16 | 1991-07-16 | Method for producing high-purity amorphous zinc stannate powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP20139591A JP3166013B2 (en) | 1991-07-16 | 1991-07-16 | Method for producing high-purity amorphous zinc stannate powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0524835A true JPH0524835A (en) | 1993-02-02 |
| JP3166013B2 JP3166013B2 (en) | 2001-05-14 |
Family
ID=16440383
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP20139591A Expired - Fee Related JP3166013B2 (en) | 1991-07-16 | 1991-07-16 | Method for producing high-purity amorphous zinc stannate powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3166013B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0748768A1 (en) * | 1995-06-13 | 1996-12-18 | Nissan Chemical Industries Ltd. | Hydrated zinc stannate sols, coating compositions and optical elements |
| US20190177177A1 (en) * | 2016-08-12 | 2019-06-13 | William Blythe Limited | Synthesis of and Uses of Alkaline Earth Metal Stannates |
-
1991
- 1991-07-16 JP JP20139591A patent/JP3166013B2/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0748768A1 (en) * | 1995-06-13 | 1996-12-18 | Nissan Chemical Industries Ltd. | Hydrated zinc stannate sols, coating compositions and optical elements |
| US20190177177A1 (en) * | 2016-08-12 | 2019-06-13 | William Blythe Limited | Synthesis of and Uses of Alkaline Earth Metal Stannates |
| US11834344B2 (en) * | 2016-08-12 | 2023-12-05 | William Blythe Limited | Synthesis of and uses of alkaline earth metal stannates |
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| Publication number | Publication date |
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| JP3166013B2 (en) | 2001-05-14 |
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