JPH0832557B2 - Method for producing sodium trititanate fine particle powder - Google Patents
Method for producing sodium trititanate fine particle powderInfo
- Publication number
- JPH0832557B2 JPH0832557B2 JP62086687A JP8668787A JPH0832557B2 JP H0832557 B2 JPH0832557 B2 JP H0832557B2 JP 62086687 A JP62086687 A JP 62086687A JP 8668787 A JP8668787 A JP 8668787A JP H0832557 B2 JPH0832557 B2 JP H0832557B2
- Authority
- JP
- Japan
- Prior art keywords
- sodium
- trititanate
- sodium trititanate
- fine particle
- particle powder
- 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 - Fee Related
Links
- 239000011734 sodium Substances 0.000 title claims description 35
- 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 title claims description 28
- 229910052708 sodium Inorganic materials 0.000 title claims description 28
- 239000010419 fine particle Substances 0.000 title claims description 13
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 239000000843 powder Substances 0.000 title claims description 12
- 239000002245 particle Substances 0.000 claims description 21
- 150000001875 compounds Chemical class 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 4
- 239000011268 mixed slurry Substances 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 14
- 238000010304 firing Methods 0.000 description 11
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 238000009826 distribution Methods 0.000 description 8
- 239000003463 adsorbent Substances 0.000 description 5
- 238000005342 ion exchange Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000004408 titanium dioxide Substances 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 235000008708 Morus alba Nutrition 0.000 description 1
- 240000000249 Morus alba Species 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Description
【発明の詳細な説明】 産業上の利用分野 本発明は、イオン交換材あるいは吸着材として有用な
三チタン酸ナトリウム微細粒子粉末の製造法に関するも
のである。Description: TECHNICAL FIELD The present invention relates to a method for producing sodium trititanate fine particle powder useful as an ion exchange material or an adsorbent.
従来の技術およびその問題点 従来、三チタン酸ナトリウム微細粒子粉末の製造法と
しては焼成法（吉川他、窯業協会誌、94,7,1986）が知
られている。即ちこの製造方法は、二酸化チタンと炭酸
ナトリウムとを乾式混合して、800℃で20時間焼成した
後、粉砕、混合し、更に800℃で20時間追焼成するとい
う方法である。2. Description of the Related Art Conventional technology and its problems Conventionally, a firing method (Yoshikawa et al., Journal of Ceramic Industry, 94, 7, 1986) is known as a method for producing sodium trititanate fine particle powder. That is, this manufacturing method is a method in which titanium dioxide and sodium carbonate are dry-mixed, calcined at 800 ° C. for 20 hours, crushed and mixed, and additionally calcined at 800 ° C. for 20 hours.
本発明者らもこの製造方法により三チタン酸ナトリウ
ム微細粒子粉末の単一相の合成を試みたが、三チタン酸
ナトリウムの単一相は得られたものの、粒子径は0.5〜1
0μｍであつて粒度分布範囲が広く、そのためイオン交
換材あるいは吸着材用として好ましいものではなかつ
た。即ち、三チタン酸ナトリウムは各種アルカリ金属イ
オンへの交換反応速度差を利用して水溶液中のリチウム
イオンを濃縮させるためのイオン交換体の原料としての
検討が進められているが、このように反応速度差を利用
してある特定成分を濃縮させようとする場合、最高の分
離効率を示す反応時間が粒子径により異ることから、特
性を充分に発揮させるためにはイオン交換材あるいは吸
着材は狭い粒度分布を有する必要がある。The inventors of the present invention also attempted to synthesize a single phase of sodium trititanate fine particle powder by this production method, but although a single phase of sodium trititanate was obtained, the particle size was 0.5 to 1
Since it is 0 μm and has a wide particle size distribution range, it is not preferable as an ion exchange material or an adsorbent. That is, sodium trititanate is being studied as a raw material of an ion exchanger for concentrating lithium ions in an aqueous solution by utilizing the difference in exchange reaction rate to various alkali metal ions. When attempting to concentrate a specific component using the speed difference, the reaction time showing the highest separation efficiency depends on the particle size. Must have a narrow particle size distribution.
また、前記従来法により単一相を得るためには、焼
成、粉砕、混合、焼成と、２度の焼成を必要とし、かつ
各焼成時間も20時間という長時間を要するなど、工業的
製造法として利用が困難である。Further, in order to obtain a single phase by the above-mentioned conventional method, firing, pulverization, mixing, firing and two firings are required, and each firing time requires a long time of 20 hours. Is difficult to use.
このように従来の製造法は、イオン交換材あるいは吸
着材として有用な、狭い粒度分布を有する三チタン酸ナ
トリウムを合成できないのみならず、製造法が煩雑であ
り、経済的にも不利である等の欠点があつた。Thus, the conventional manufacturing method is not only not possible to synthesize sodium trititanate having a narrow particle size distribution, which is useful as an ion-exchange material or an adsorbent, but the manufacturing method is complicated and economically disadvantageous. There was a drawback of.
そこで本発明はイオン交換材あるいは吸着材として有
用な、狭い粒度分布を有する三チタン酸ナトリウム微細
粒子粉末の経済的製造法を提供することを目的とする。Therefore, an object of the present invention is to provide an economical production method of sodium trititanate fine particle powder having a narrow particle size distribution, which is useful as an ion-exchange material or an adsorbent.
問題点を解決するための手段 本発明者らは狭い粒度分布を有する三チタン酸ナトリ
ウム微細粒子粉末の経済的製造法を開発せんものと鋭意
研究の結果、TiO2対Na2Oのモル比が3:1の割合で配合さ
れているチタン原料化合物とナトリウム原料化合物との
混合スラリーを噴霧乾燥して、チタン原料化合物の粒子
表面にナトリウム原料化合物を均一に付着させた後、焼
成することにより、狭い粒度分布を有する三チタン酸ナ
トリウム微細粒子からなる粒状物が得られ、次いで該粒
状物を水又は温水中に浸漬することにより、単一粒子に
分離した三チタン酸ナトリウム微細粒子粉末が得られる
ことを発見し、本発明を完成したものである。Means for Solving the Problems The present inventors have developed an economical production method of sodium trititanate fine particle powder having a narrow particle size distribution. As a result of intensive research, the inventors have found that the molar ratio of TiO 2 to Na 2 O is By spray-drying a mixed slurry of a titanium raw material compound and a sodium raw material compound, which are blended in a ratio of 3: 1, and uniformly adhering the sodium raw material compound to the particle surface of the titanium raw material compound, and then firing. A granule consisting of sodium trititanate fine particles having a narrow particle size distribution is obtained, and by dipping the granule in water or warm water, a sodium trititanate fine particle powder separated into single particles is obtained. The inventors have discovered the above and completed the present invention.
即ち、本発明の方法は、TiO2対Na2Oのモル比が3:1の
割合で配合されているチタン原料化合物とナトリウム原
料化合物との混合スラリーを噴霧乾燥した後、700〜1,1
00℃で焼成して、三チタン酸ナトリウム微細粒子からな
る粒状物を生成せしめ、次いで該粒状生成物を水又は温
水中に浸漬して、微細単一粒子に分離することを特徴と
する。That is, the method of the present invention, after spray-drying a mixed slurry of titanium raw material compound and sodium raw material compound that are mixed at a molar ratio of TiO 2 to Na 2 O of 3: 1, 700-1,1,1
It is characterized in that it is calcined at 00 ° C. to form granules composed of fine particles of sodium trititanate, and then the granulated product is immersed in water or warm water to be separated into fine single particles.
本発明で使用されるチタン原料化合物としては二酸化
チタン及び含水酸化チタンなどを挙げることができ、ナ
トリウム原料化合物としては焼成時にNa2Oを生じる化合
物、例えばNa2O、NaOH、Na2CO3、NaHCO3、Na2C2O4及びNaNO3
などを挙げることができる。Examples of the titanium raw material compound used in the present invention may include titanium dioxide and hydrous titanium oxide, and the sodium raw material compound may be a compound that produces Na 2 O upon firing, such as Na 2 O, NaOH, Na 2 CO 3 , NaHCO 3 , Na 2 C 2 O 4 and NaNO 3
And so on.
焼成温度は700〜1,100℃、好ましくは800〜1,000℃で
ある。即ち焼成温度が1,100℃より高い場合には、三チ
タン酸ナトリウムの単一相を得ることができず、一方焼
成温度が700℃よりも低いと、反応速度が遅く、実用的
でない。The firing temperature is 700 to 1,100 ° C, preferably 800 to 1,000 ° C. That is, when the firing temperature is higher than 1,100 ° C, a single phase of sodium trititanate cannot be obtained, while when the firing temperature is lower than 700 ° C, the reaction rate is slow and it is not practical.
尚、焼成時間は0.5〜10時間、好ましくは１〜４時間
である。粒状生成物を単一の三チタン酸ナトリウム微細
粒子に分離する操作は、焼成物を適量の水又は温水中に
投入して、0.5〜10時間浸漬後、攪拌することによりな
される。The firing time is 0.5 to 10 hours, preferably 1 to 4 hours. The operation of separating the granular product into a single fine particle of sodium trititanate is performed by charging the calcined product in an appropriate amount of water or warm water, immersing it for 0.5 to 10 hours, and then stirring it.
以下、実施例及び比較例により、本発明を更に詳しく
説明する。Hereinafter, the present invention will be described in more detail with reference to Examples and Comparative Examples.
実施例1. アナターゼ型二酸化チタン1,000g及び炭酸ナトリウム
442gを秤量し、2.5Lの水を添加後、よく攪拌した。この
スラリーを入口温度270〜280℃、出口温度80〜85℃の条
件で噴霧乾燥した。Example 1. 1,000 g of anatase type titanium dioxide and sodium carbonate
After weighing 442 g and adding 2.5 L of water, the mixture was well stirred. This slurry was spray-dried under conditions of an inlet temperature of 270 to 280 ° C and an outlet temperature of 80 to 85 ° C.
次に、この乾燥物をアルミナ製ルツボに入れ、電気炉
中で昇温速度200℃／時、焼成温度850℃、保持時間４時
間の条件で焼成した後、200℃／時の速度で降温した。Next, this dried product was put into an alumina crucible, and baked in an electric furnace at a temperature rising rate of 200 ° C./hour, a baking temperature of 850 ° C., and a holding time of 4 hours, and then cooled at a speed of 200 ° C./hour. .
焼成物をステンレス製容器中の10Lの温水に投入し
て、３時間浸漬した後ホモミキサーで１時間攪拌し、次
いでろ過、洗浄、乾燥して、チタン酸ナトリウム微細粉
末を得た。The fired product was put into 10 L of warm water in a stainless steel container, immersed for 3 hours, stirred with a homomixer for 1 hour, then filtered, washed and dried to obtain sodium titanate fine powder.
この生成物をＸ線回折により同定したところ、三チタ
ン酸ナトリウムの単一相であつた。又走査型電子顕微鏡
により観察したところ、粒子径0.4〜0.7μｍ、粒子長２
〜４μｍの柱状結晶であつた。The product was identified by X-ray diffraction and was a single phase of sodium trititanate. Observation with a scanning electron microscope revealed that the particle diameter was 0.4 to 0.7 μm and the particle length was 2
It was a columnar crystal of ˜4 μm.
実施例2. TiO231.4％、SO32.3％を含む含水酸化チタンスラリー
2,600gを攪拌しながら、炭酸ナトリウム粉末440gを添加
した。このスラリーを実施例1.と同様な条件で噴霧乾燥
した。Example 2. Hydrous titanium oxide slurry containing TiO 2 31.4% and SO 3 2.3%
While stirring 2,600 g, 440 g of sodium carbonate powder was added. This slurry was spray-dried under the same conditions as in Example 1.
次にこの乾燥物をアルミナ製ルツボに入れ、電気炉で
昇温速度200℃／時、焼成温度1,000℃、保持時間２時間
の条件で焼成した後、200℃／時の速度で降温した。Next, this dried product was put into an alumina crucible and baked in an electric furnace under the conditions of a heating rate of 200 ° C./hour, a baking temperature of 1,000 ° C. and a holding time of 2 hours, and then the temperature was lowered at a speed of 200 ° C./hour.
焼成物をステンレス製容器中の8Lの温水に投入して、
５時間浸漬した後、ホモミキサーで１時間攪拌し、次い
でろ過、洗浄、乾燥して、チタン酸ナトリウム微細粉末
を得た。Add the fired product to 8 L of warm water in a stainless steel container,
After soaking for 5 hours, the mixture was stirred for 1 hour with a homomixer, then filtered, washed and dried to obtain sodium titanate fine powder.
この生成物をＸ線回折により同定したところ、三チタ
ン酸ナトリウムの単一相であつた。又走査型電子顕微鏡
により観察したところ、粒子径0.8〜1.3μｍ、粒子長３
〜５μｍの柱状結晶であつた。The product was identified by X-ray diffraction and was a single phase of sodium trititanate. Observation with a scanning electron microscope revealed that the particle diameter was 0.8 to 1.3 μm and the particle length was 3
It was a columnar crystal of ˜5 μm.
比較例1. アナターゼ型二酸化チタン100gと炭酸ナトリウム44.2
gを秤量し、石川式擂漬機で湿式混合した後、アルミナ
製ルツボに入れ、電気炉中で昇温速度200℃／時、焼成
温度800℃、保持時間20時間の条件で焼成した後、200℃
／時の速度で降温した。Comparative Example 1. Anatase type titanium dioxide 100g and sodium carbonate 44.2
After weighing g and wet-mixing with an Ishikawa type mulberry picker, the mixture was placed in an alumina crucible and baked in an electric furnace under the conditions of a heating rate of 200 ° C / hour, a baking temperature of 800 ° C, and a holding time of 20 hours, 200 ° C
The temperature was lowered at a speed of / hour.
焼成物をＸ線回折により同定したところ、三チタン酸
ナトリウム、六チタン酸ナトリウム及び二酸化チタンか
らなる混合相であつた。When the calcined product was identified by X-ray diffraction, it was a mixed phase consisting of sodium trititanate, sodium hexatitanate and titanium dioxide.
次に、この焼成物を石川式擂漬機で粉砕、混合した
後、１回目と同様な条件で追焼成した。これにより得ら
れた生成物はＸ線回折により三チタン酸ナトリウムの単
一相であることが判つた。又走査型電子顕微鏡により観
察したところ、0.5〜２μｍの大きさの粒状粒子と粒子
径１〜２μｍ、長さ５〜10μｍの柱状粒子との混合物で
あり、実施例1.及び2.で得られた生成物よりも明らかに
粒度分布の悪いものであつた。Next, this fired product was crushed and mixed with an Ishikawa type glazed machine, and then additionally fired under the same conditions as the first time. The product thus obtained was found by X-ray diffraction to be a single phase of sodium trititanate. Further, when observed by a scanning electron microscope, it was a mixture of granular particles having a size of 0.5 to 2 μm and columnar particles having a particle diameter of 1 to 2 μm and a length of 5 to 10 μm, which were obtained in Examples 1 and 2. The product had a significantly worse particle size distribution than the product.
発明の効果 本発明による製造法は従来法よりも経済的に有利のみ
ならず、本発明の製造法により得られる三チタン酸ナト
リウム微細粉末は、従来法により得られる三チタン酸ナ
トリウム微細粒子よりも狭い粒度分布を有する為、イオ
ン交換材及び吸着材用として好適である。EFFECTS OF THE INVENTION The production method according to the present invention is not only economically advantageous over the conventional method, but the sodium trititanate fine powder obtained by the production method of the present invention is superior to the sodium trititanate fine particles obtained by the conventional method. Since it has a narrow particle size distribution, it is suitable for ion exchange materials and adsorbents.
Claims (1)
れているチタン原料化合物とナトリウム原料化合物との
混合スラリーを噴霧乾燥した後、700〜1,100℃で焼成し
て、三チタン酸ナトリウム微細粒子からなる粒状物を生
成せしめ、次いで該粒状生成物を水又は温水中に浸漬し
て、単一粒子に分離することを特徴とする、三チタン酸
ナトリウム微細粒子粉末の製造法。1. A mixed slurry of a titanium raw material compound and a sodium raw material compound mixed in a molar ratio of TiO 2 to Na 2 O of 3: 1 is spray-dried and then fired at 700 to 1,100 ° C. , Sodium trititanate fine particles, and then soaking the granular product in water or warm water to separate into single particles, sodium trititanate fine particle powder, Manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62086687A JPH0832557B2 (en) | 1987-04-08 | 1987-04-08 | Method for producing sodium trititanate fine particle powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62086687A JPH0832557B2 (en) | 1987-04-08 | 1987-04-08 | Method for producing sodium trititanate fine particle powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63252926A JPS63252926A (en) | 1988-10-20 |
| JPH0832557B2 true JPH0832557B2 (en) | 1996-03-29 |
Family
ID=13893900
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62086687A Expired - Fee Related JPH0832557B2 (en) | 1987-04-08 | 1987-04-08 | Method for producing sodium trititanate fine particle powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0832557B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7013067B1 (en) * | 2020-11-02 | 2022-01-31 | 国立大学法人信州大学 | Filtration material, manufacturing method of filtration material, water treatment material and water purifier |
| WO2022091514A1 (en) * | 2020-11-02 | 2022-05-05 | 国立大学法人信州大学 | Filter material, production method for filter material, water treatment material, and water purifier |
-
1987
- 1987-04-08 JP JP62086687A patent/JPH0832557B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63252926A (en) | 1988-10-20 |
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