JPS63252927A - Production of fine particle powder of sodium hexatitanate - Google Patents
Production of fine particle powder of sodium hexatitanateInfo
- Publication number
- JPS63252927A JPS63252927A JP8668887A JP8668887A JPS63252927A JP S63252927 A JPS63252927 A JP S63252927A JP 8668887 A JP8668887 A JP 8668887A JP 8668887 A JP8668887 A JP 8668887A JP S63252927 A JPS63252927 A JP S63252927A
- Authority
- JP
- Japan
- Prior art keywords
- sodium
- raw material
- slurry
- material compound
- fine particles
- 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
- 239000011734 sodium Substances 0.000 title claims abstract description 43
- 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 abstract description 42
- 229910052708 sodium Inorganic materials 0.000 title claims abstract description 42
- 239000010419 fine particle Substances 0.000 title claims abstract description 26
- 239000000843 powder Substances 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000002245 particle Substances 0.000 claims abstract description 29
- GROMGGTZECPEKN-UHFFFAOYSA-N sodium metatitanate Chemical compound [Na+].[Na+].[O-][Ti](=O)O[Ti](=O)O[Ti]([O-])=O GROMGGTZECPEKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002994 raw material Substances 0.000 claims abstract description 23
- 150000001875 compounds Chemical class 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 11
- 239000010936 titanium Substances 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 239000011268 mixed slurry Substances 0.000 claims abstract description 6
- 238000001694 spray drying Methods 0.000 claims abstract description 4
- 239000008187 granular material Substances 0.000 claims abstract description 3
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract description 9
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 238000010304 firing Methods 0.000 description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- 239000003973 paint Substances 0.000 description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 6
- 208000005156 Dehydration Diseases 0.000 description 5
- 239000000919 ceramic Substances 0.000 description 5
- 230000018044 dehydration Effects 0.000 description 5
- 238000006297 dehydration reaction Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000007716 flux method Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
本発明は、断熱塗料、断熱シート及びセラミックス用等
の原料として有用な六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。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing fine particle powder of sodium hexatitanate, which is useful as a raw material for heat insulating paints, heat insulating sheets, ceramics, and the like.
従来、六チタン酸ナトリウムの製造方法については水熱
法及びフラックス法等が報告されているが、これらは総
べて繊維状のチタン酸ナトリウムの製造方法に関するも
のである。例えば水熱法〔滝貞男、田中桂子；工業化学
雑誌、第６６巻、第４号、１９６３）では、酸化チタン
をＩＮ−水酸化ナトリウム水溶液中に分散した後、銀ラ
イニングを施したオートクレーブに仕込み、３２５〜３
５０℃で５〜２４時間処理することにより、２００〜１
，０００μｍ程度の長さの六チタン酸ナトリウム繊維が
生成するとされており、又フラックス法（特開昭４６−
４３７０号参照）では、酸化チタンと炭酸ナトリウムと
をモル比で６＝１で混合後、更にフラックスとして硫酸
ナトリウムを添加して、９８０℃で２時間加熱溶融する
ことにより、ｌＯ〜１００μｍ程度の長さの六チタン酸
ナトリウム繊維が生成するとされている。しかしながら
これら繊維状のチタン酸ナトリウム粒子は、断熱塗料、
断熱シートあるいはセラミックス等の原料としては下記
のような理由で好ましくない。Hitherto, hydrothermal methods, flux methods, and the like have been reported as methods for producing sodium hexatitanate, but all of these relate to methods for producing fibrous sodium titanate. For example, in the hydrothermal method [Sadao Taki, Keiko Tanaka; Industrial Chemistry Magazine, Vol. 66, No. 4, 1963], titanium oxide is dispersed in an IN-sodium hydroxide aqueous solution and then charged into a silver-lined autoclave. , 325-3
200-1 by processing at 50°C for 5-24 hours.
It is said that sodium hexatitanate fibers with a length of about ,000 μm are produced, and the flux method
No. 4370), after mixing titanium oxide and sodium carbonate at a molar ratio of 6=1, adding sodium sulfate as a flux and heating and melting at 980°C for 2 hours, a length of about 10 to 100 μm is obtained. It is said that sodium hexatitanate fibers are produced. However, these fibrous sodium titanate particles can be used in insulation coatings,
It is not preferred as a raw material for heat insulating sheets or ceramics for the following reasons.
■ 断熱塗料用途・・・繊維状でかつ嵩高い為に塗料中
での分散が難しい。又吸油量が大きいので、塗料中での
チタン酸ナトリウムの濃度を高くすることができず、断
熱性の良好な塗膜が得られない。■ Use in insulation paints: Difficult to disperse in paints because they are fibrous and bulky. Furthermore, since the amount of oil absorbed is large, it is not possible to increase the concentration of sodium titanate in the paint, and a coating film with good heat insulation properties cannot be obtained.
■ 断熱シート・・嵩高い為に樹脂中への練り込みが困
難となり、生産性が悪い。■ Insulating sheet: Because it is bulky, it is difficult to knead it into the resin, resulting in poor productivity.
■ セラミックス用途・・・粒子が大きく、かつ嵩高い
為に緻密な焼結体を得ることができない。■ Ceramics applications: Because the particles are large and bulky, dense sintered bodies cannot be obtained.
以上述べたように、従来報告されているチタン酸す）
ＩＪウム繊維は断熱塗料、断熱シート及びセラミックス
等の原料としては好ましいものではない０
そこで本発明は上記用途向として、分散性が良く、かつ
狭い粒度分布を有するチタノ酸ナトリウム微細粒子つ末
の経済的製造法を提供することを目的とする。As mentioned above, the previously reported titanic acid
IJum fibers are not preferable as raw materials for heat insulating paints, heat insulating sheets, ceramics, etc. Therefore, the present invention is an economical method for producing fine powders of sodium titanoate with good dispersibility and narrow particle size distribution for the above-mentioned applications. The purpose is to provide a manufacturing method for
問題点を解決するための手段
本発明者らは、分散性が良好で、かつ狭い粒度分布を有
する六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、一般式Ｎａ２０ｅ
ｎＴｉ０ｚ （ただしｎ＝２〜４）で示される割合で配
合された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五チタン酸四
ナトリウム、三チタン酸ナトリウム、及び六チタン酸ナ
トリウム等からなるチタン酸ナトリウム混合相の微細粒
子粉末が得られること、次いでこれを酸水溶液で処理し
てチタン酸ナトリウム微細粒子粉末中のＮ ａ ２０成
分の一部を抽出した後、加熱脱水処理する方法で、分散
性が良好で、かつ粒度分布の狭い六チタン酸ナトリウム
微細粒子粉末の単−相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 sought to develop an economical method for producing fine particle powder of sodium hexatitanate, which has good dispersibility and a narrow particle size distribution, and as a result of intensive research, the general formula Na20e
A mixed slurry of a titanium raw material compound and a sodium raw material compound blended in a ratio shown by nTi0z (where n = 2 to 4) was spray-dried to uniformly adhere the sodium raw material compound to the particle surface of the titanium raw material compound. After that, by calcination, a fine particle powder of a sodium titanate mixed phase consisting of tetrasodium pentatitanate, sodium trititanate, sodium hexatitanate, etc. having a narrow particle size distribution is obtained, and then this is dissolved in an acid aqueous solution. A part of the Na 20 component in the sodium titanate fine particle powder is extracted by heating and dehydrating the sodium hexatitanate fine particle powder, which has good dispersibility and a narrow particle size distribution. He discovered that a single phase could be obtained and completed the present invention.
即ち、本発明の方法は、一般式Ｎａ２Ｏ・ｎＴｆｃ）２
（ただしｎ ＝ ２〜４）で示される割合で配合された
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五チタン酸四ナトリウ
ム、三チタン酸ナトリウム、及び六チタン酸ナトリウム
等からなるチタン酸ナトリウム混合相の微相粒子粉末が
得られること、次いでこれを酸水溶液で処理してチタン
酸ナトリウム微細粒子粉末中のＮａ２Ｏ成分の一部を抽
出した後、加熱脱水処理する方法で、分散性が良好で、
かつ粒度分布の狭い六チタン酸ナトリウム微細粒子粉末
の単−相が得られることを発見し、本発明を完成したも
のである。That is, the method of the present invention uses the general formula Na2O.nTfc)2
(However, n = 2 to 4) After spray-drying the mixed slurry of the titanium raw material compound and the sodium raw material compound blended in the ratio shown by n = 2 to 4 to uniformly adhere the sodium raw material compound to the particle surface of the titanium raw material compound. By calcination, a fine-phase powder of sodium titanate mixed phase consisting of tetrasodium pentatitanate, sodium trititanate, sodium hexatitanate, etc. having a narrow particle size distribution is obtained, and then this is dissolved in an acid aqueous solution. After treatment with sodium titanate to extract a part of the Na2O component in the fine particle powder of sodium titanate, a heating dehydration treatment is performed, resulting in good dispersibility.
The present invention was completed based on the discovery that a single phase of fine particle powder of sodium hexatitanate with a narrow particle size distribution could be obtained.
即ち、本発明の方法は、一般式Ｎ＆２０・ｎＴｉＯ２（
ｎ＝２〜４）で示される割合で配合されたチタン原料化
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、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チタン酸ナト
リウム微細粒子を単一の粒子に分離した後、該スラリー
に酸を添加してｐＨを７．５〜８．５に調整することに
より、チタン酸ナトリウム微細粒子組成がＮｎ２０・６
Ｔｉ０２・ｎＨ２Ｏの組成となるように組成変換処理し
、更に５００℃以上に加熱することを特徴とする。That is, the method of the present invention uses the general formula N&20.nTiO2 (
After spray-drying a mixed slurry of a titanium raw material compound and a sodium raw material compound blended in the ratio shown by n = 2 to 4), it is fired at 700 to 1,100°C to form granules consisting of fine particles of sodium titanate. After the granular product is soaked in water or hot water to separate the sodium titanate fine particles into single particles, acid is added to the slurry to adjust the pH to 7.5-8. 5, the sodium titanate fine particle composition becomes Nn20.6.
It is characterized in that it undergoes a composition conversion treatment so that it has a composition of Ti02.nH2O, and is further heated to 500° C. or higher.
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、含水酸化チタン、ルチル鉱石などを挙げることが
でき、その粒子形状はなるべく微粒子が好ましい。又本
発明で使用される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Ｎａ２０ＳＮａＯＨ
，ＮａｚＣＯａ、ＮａＨＣＯ３、ＮａｚＣ２０４及びＮ
ａＮＯ３などを挙げることができる。Examples of the titanium raw material compound used in the present invention include titanium dioxide, hydrous titanium oxide, and rutile ore, and the particle shape thereof is preferably as fine as possible. In addition, the sodium raw material compounds used in the present invention include compounds that generate Na2O during firing, such as Na20SNaOH.
, NazCOa, NaHCO3, NazC204 and N
Examples include aNO3.
チタン原料化合物とす） ＩＪウム原料化合物との配合
割合は、一般式Ｎａ２Ｏ・ｎＴｉＯ２で表わした場合の
ｎ値が２〜４の範囲、好ましくは２．５〜３．５である
。ｎが４よりも大きい場合、焼成により得られるチタン
酸ナトリウム混合相中の六チタン酸ナトリウムの含有率
が多くなり、その為に水又は温水中に浸漬してもチタン
酸ナトリウム微細粒子を単一粒子に分離することができ
なくなる。The blending ratio of titanium with the IJium raw material compound is such that the n value when expressed by the general formula Na2O.nTiO2 is in the range of 2 to 4, preferably 2.5 to 3.5. When n is larger than 4, the content of sodium hexatitanate in the sodium titanate mixed phase obtained by calcination increases, and therefore, even when immersed in water or hot water, the sodium titanate fine particles cannot be separated into single particles. It becomes impossible to separate into particles.
即ち粒状生成物を水又は温水に浸漬して、単一のチタン
酸ナトリウム微細粒子に分離する操作は、層状構造を有
する五チタン酸四ナトリウム及び三チタン酸ナトリウム
に対し有効な手段ではあるが、トンネル構造を有する六
チタン酸ナトリウムに対しては有効な手段とはならない
からである。一方ｎが２よりも小さい場合には、狭い粒
度分布を有するチタン酸ナトリウム微細粒子を得ること
ができないためである。That is, immersing the granular product in water or hot water to separate it into single fine particles of sodium titanate is an effective method for tetrasodium pentatitanate and sodium trititanate, which have a layered structure. This is because it is not an effective means for sodium hexatitanate having a tunnel structure. On the other hand, if n is smaller than 2, it is impossible to obtain sodium titanate fine particles having a narrow particle size distribution.
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、得られるチタン酸ナトリウムの粒子径が大
きくなるのみならず、粒子間子の焼結が進み水又は温水
中に浸漬しても粒状生成物を単一粒子に分離することが
できない。又焼成温度が７００℃よりも低い場合は反応
速度が遅く、実用的でない。尚焼成時間は０．５〜１０
時間、好ましくは１〜４時間である。焼成により合成さ
れる相は一般式Ｎａ２Ｏ、ｎＴｉＯ２のｎの値により異
なる。即ち２ （ｎ （３の場合には五チタン酸四ナト
リウムと三チタン酸ナトリウムとの混合相、ｎ＝３の場
合には三チタン酸ナトリウムの単独相、３ （’ｎ （
４の場合には三チタン酸ナトリウムと六チタン酸ナトリ
ウムの混合相として得られる。Firing temperature is 700~1,100℃, preferably 800~
The temperature is 1,000°C. In other words, when the calcination temperature is higher than 1,100°C, not only does the particle size of the obtained sodium titanate become large, but also the sintering of the particles progresses and the granular product cannot be easily separated even when immersed in water or hot water. It cannot be separated into single particles. Further, if the firing temperature is lower than 700°C, the reaction rate is slow and it is not practical. The firing time is 0.5 to 10
time, preferably 1 to 4 hours. The phase synthesized by firing differs depending on the value of n in the general formulas Na2O and nTiO2. That is, 2 (n
In the case of No. 4, it is obtained as a mixed phase of sodium trititanate and sodium hexatitanate.
粒状生成物を単一の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。単
一粒子に分離後のスラリーのｐＩ（はスラリー濃度によ
り異なるが通常１１〜１２程度であり、チタン酸ナトリ
ウム微細粒子は五チタン酸四ナトリウムと三チタン酸ナ
トリウムとの混合相、三チタン酸ナトリウムの単独相あ
るいは三チタン酸ナトリウムと六チタン酸ナトリウムの
混合相等の状態にある。従って、その状態でろ過、洗浄
、乾燥、及び焼成の操作を行なっても六チタン酸ナトリ
ウムの単独相は得られない。The operation of separating the granular product into single fine particles of sodium titanate is to pour the fired product into an appropriate amount of water or hot water, and then
．． This is done by stirring after soaking for 5 to 10 hours. The pI of the slurry after separation into single particles varies depending on the slurry concentration, but is usually about 11 to 12. Sodium titanate fine particles are a mixed phase of tetrasodium pentitanate and sodium trititanate, sodium trititanate. Sodium trititanate and sodium hexatitanate are in a single phase or a mixed phase of sodium hexatitanate.Therefore, even if filtration, washing, drying, and calcination operations are performed in this state, a single phase of sodium hexatitanate cannot be obtained. do not have.
そこで、層状構造である五チタン酸四ナトリウム及び三
チタン酸ナトリウム組成をＮａ２Ｏ・６Ｔｉ０２・ｎＨ
２Ｏに変化させることを目的として単一粒子に分離後、
スラリーに酸を添加してスラリーのｐＨを７．５〜８．
５に調整する。この時のｐＨが８．５よりも高い場合に
は五チタン酸四ナトリウム、及び三チタン酸ナトリウム
の組成を完全にＮａ２Ｏ・６ＴｉＯ２・ｎＨ２Ｏまで変
化させることができない為、最終製品に三チタン酸ナト
リウムが混在する。又ｐＨが７．５よりも低い場合には
ナトリウムイオンの抽出が進みすぎて最終製品に酸化チ
タンが混在する。Therefore, we changed the composition of tetrasodium pentitanate and sodium trititanate, which have a layered structure, to Na2O.6Ti02.nH.
After separation into single particles for the purpose of converting to 2O,
Add acid to the slurry to adjust the pH of the slurry to 7.5-8.
Adjust to 5. If the pH at this time is higher than 8.5, the composition of tetrasodium pentitanate and sodium trititanate cannot be completely changed to Na2O, 6TiO2, nH2O, so sodium trititanate is added to the final product. are mixed. If the pH is lower than 7.5, the extraction of sodium ions will proceed too much and titanium oxide will be mixed in the final product.
スラリーのｐＨを調整する為に添加する酸の種類として
は、硫酸、塩酸、リン酸、酢酸等が使用できる。As the type of acid added to adjust the pH of the slurry, sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, etc. can be used.
又組成変換を行なった後の加熱脱水処理は、５００℃〜
１，０００℃、好ましくは６００〜９００℃である。即
ち加熱脱水温度が１，０００℃を超える場合、粒子間に
焼結がおこり分散性が良好な六チタン酸ナトリウム微細
粒子粉末を得ることができず、又５００℃未満の場合加
熱脱水に要する時間が大巾に長くなり、工業的でない。In addition, the heating dehydration treatment after the composition conversion is performed at 500℃~
The temperature is 1,000°C, preferably 600-900°C. That is, if the heating dehydration temperature exceeds 1,000°C, sintering will occur between the particles, making it impossible to obtain fine particles of sodium hexatitanate with good dispersibility, and if the heating dehydration temperature is below 500°C, the time required for heating dehydration will decrease. It is very long and unindustrial.
以下、本発明を実施例によりさらに詳しく説明する。Hereinafter, the present invention will be explained in more detail with reference to Examples.
実施例１゜
アナターゼ型酸化チタン１，０００ｇ及び炭酸ナトリウ
ム４７４ｇ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 oxide and 474 g of sodium carbonate were weighed, and after adding 2.5 L of water, they were thoroughly 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 placed in an alumina crucible and fired in an electric furnace at a heating rate of 200°C/hour, a firing temperature of 850°C, and a holding time of 4 hours, and then the temperature was lowered at a rate of 200°C/hour. .
焼成物をステンレス製容器中のＩＯＬ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、４
Ｎ−硫酸を滴下してスラリーのｐＨを７．８に調整した
のち、ろ過、洗浄後、８００℃で１時間焼成した。The baked product was poured into IOL warm water in a stainless steel container, immersed for 3 hours, stirred for 1 hour with a homomixer,
After adjusting the pH of the slurry to 7.8 by dropping N-sulfuric acid, it was filtered, washed, and then baked at 800°C for 1 hour.
生成物をＸ線回折により同定したところ、六チタン酸ナ
トリウムの単−相であった。又走査凰電子顕微鏡により
観察したところ粒子径０．５〜０．７μｍ１ 粒子長２
〜４βｍの柱状結晶であった。The product was identified by X-ray diffraction as a single phase of sodium hexatitanate. Also, when observed using a scanning electron microscope, the particle size was 0.5 to 0.7 μm1 and the particle length was 2.
It was a columnar crystal of ~4βm.
実施例２゜
Ｔ １（）ｚ ３１．４％、ＳＯ３２，３俤を含む含水
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３９８ｇ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。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２０
０℃／時焼成温度ｉ、ｏｏｏ℃、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。Example 2 398 g of sodium carbonate powder was added while stirring 2,600 g of a hydrous titanium oxide slurry containing 31.4% T 1 ( ) z and 2,3 SO. This slurry was used in Example 1. Spray-dried under the same conditions. Next, this dried material was placed in an alumina crucible and placed in an electric furnace at a heating rate of 20
After firing at a firing temperature of 0° C./hour, ooo° C., and a holding time of 2 hours, the temperature was lowered at a rate of 200° C./hour.
焼成物をステンレス製容器中の８Ｌ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、３Ｎ−
塩酸を滴下してスラリーのｐＩ（を８．２に調整したの
ちろ過、洗浄後、７００℃で２時間焼成した。得られた
生成物をＸ線回折により同定したところ、六チタン酸ナ
トリウムの単−相であった。又走査型電子顕微鏡により
観察したところ、粒子径１〜１．５μｍ１粒子長３〜６
μｍの柱状結晶であった。Pour the baked product into 8L of warm water in a stainless steel container, and
After soaking for an hour, stir with a homomixer for 1 hour, and
Hydrochloric acid was added dropwise to adjust the pI of the slurry to 8.2, followed by filtration, washing, and calcining at 700°C for 2 hours.The resulting product was identified by X-ray diffraction, and it was found to be a monomer of sodium hexatitanate. - phase.When observed with a scanning electron microscope, the particle size was 1 to 1.5 μm, the particle length was 3 to 6
It was a columnar crystal of μm.
発明の効果
本発明により合成された六チタン酸ナトリウムは微細で
かつ狭い粒度分布を有する為、断熱塗料、断熱シート及
びセラミックス用原料として好適である。Effects of the Invention Since the sodium hexatitanate synthesized according to the present invention is fine and has a narrow particle size distribution, it is suitable as a raw material for heat-insulating paints, heat-insulating sheets, and ceramics.
特許出願人 チタン工業株式会社 （外５名）Patent applicant: Titanium Industries Co., Ltd. (5 other people)
Claims (1)
れる割合で配合された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、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チタン酸ナトリウム微細粒子を単
一粒子に分離した後、該スラリーに酸を添加してｐＨを
７．５〜８．５に調整することにより、チタン酸ナトリ
ウム微細粒子の組成がＮａ＿２Ｏ・６ＴｉＯ＿２、ｎＨ
＿２Ｏの組成となるように組成変換処理し、更に、５０
０℃以上に加熱することを特徴とする、六チタン酸ナト
リウム微細粒子粉末の製造法。After spray-drying a mixed slurry of a titanium raw material compound and a sodium raw material compound blended in the ratio represented by the general formula Na_2O・nTiO_2 (n=2-4), 700~
Calcining at 1,100° C. to produce granules consisting of fine particles of sodium titanate, and then immersing the granular product in water or hot water to separate the fine particles of sodium titanate into single particles; By adding acid to the slurry and adjusting the pH to 7.5 to 8.5, the composition of the sodium titanate fine particles is changed to Na_2O・6TiO_2, nH
The composition was converted to a composition of _2O, and then 50
A method for producing fine particle powder of sodium hexatitanate, which comprises heating to 0°C or higher.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62086688A JP2528462B2 (en) | 1987-04-08 | 1987-04-08 | Method for producing sodium hexatitanate fine particle powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62086688A JP2528462B2 (en) | 1987-04-08 | 1987-04-08 | Method for producing sodium hexatitanate fine particle powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63252927A true JPS63252927A (en) | 1988-10-20 |
| JP2528462B2 JP2528462B2 (en) | 1996-08-28 |
Family
ID=13893923
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62086688A Expired - Fee Related JP2528462B2 (en) | 1987-04-08 | 1987-04-08 | Method for producing sodium hexatitanate fine particle powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2528462B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006044992A (en) * | 2004-08-04 | 2006-02-16 | National Institute Of Advanced Industrial & Technology | Simple method for manufacturing titanium oxide nanotube structure and titanium oxide nanotube structure obtained by the same method |
| JP2008110918A (en) * | 2008-01-28 | 2008-05-15 | Jfe Mineral Co Ltd | Nonfibrous potassium titanate |
| WO2008123558A1 (en) * | 2007-03-29 | 2008-10-16 | Toho Titanium Co., Ltd. | Method for production of alkali titanate, method for production of hollow powder of alkali titanate, alkali titanate and hollow powder thereof produced by the methods, and friction material comprising the alkali titanate or the hollow powder thereof |
| JP2008266131A (en) * | 2007-03-29 | 2008-11-06 | Toho Titanium Co Ltd | Method for producing alkali titanate, alkali titanate produced by the method, and friction material comprising the alkali titanate |
| WO2008149845A1 (en) * | 2007-06-08 | 2008-12-11 | Otsuka Chemical Co., Ltd. | Sodium hexatitanate and method for production thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101488905B1 (en) | 2013-05-29 | 2015-02-03 | 주식회사 경남케미컬 | Sodium titanate for welding material and method for preparing the same |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS553370A (en) * | 1978-06-23 | 1980-01-11 | Natl Inst For Res In Inorg Mater | Production of alkali metal hexatitanate fiber |
| JPS60210529A (en) * | 1984-03-30 | 1985-10-23 | Otsuka Chem Co Ltd | Production of fibrous alkali metal titanate |
-
1987
- 1987-04-08 JP JP62086688A patent/JP2528462B2/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS553370A (en) * | 1978-06-23 | 1980-01-11 | Natl Inst For Res In Inorg Mater | Production of alkali metal hexatitanate fiber |
| JPS60210529A (en) * | 1984-03-30 | 1985-10-23 | Otsuka Chem Co Ltd | Production of fibrous alkali metal titanate |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006044992A (en) * | 2004-08-04 | 2006-02-16 | National Institute Of Advanced Industrial & Technology | Simple method for manufacturing titanium oxide nanotube structure and titanium oxide nanotube structure obtained by the same method |
| JP4706053B2 (en) * | 2004-08-04 | 2011-06-22 | 独立行政法人産業技術総合研究所 | Simple production method of titanium oxide nanotube structure and titanium oxide nanotube structure obtained by the production method |
| WO2008123558A1 (en) * | 2007-03-29 | 2008-10-16 | Toho Titanium Co., Ltd. | Method for production of alkali titanate, method for production of hollow powder of alkali titanate, alkali titanate and hollow powder thereof produced by the methods, and friction material comprising the alkali titanate or the hollow powder thereof |
| JP2008266131A (en) * | 2007-03-29 | 2008-11-06 | Toho Titanium Co Ltd | Method for producing alkali titanate, alkali titanate produced by the method, and friction material comprising the alkali titanate |
| US8398952B2 (en) | 2007-03-29 | 2013-03-19 | Toho Titanium Co., Ltd. | Method of manufacturing alkali metal titanate and hollow body particle thereof, product thereof, and friction material containing the product |
| WO2008149845A1 (en) * | 2007-06-08 | 2008-12-11 | Otsuka Chemical Co., Ltd. | Sodium hexatitanate and method for production thereof |
| JP2008303121A (en) * | 2007-06-08 | 2008-12-18 | Otsuka Chemical Co Ltd | Sodium hexatitanate and method for producing the same |
| US8877339B2 (en) | 2007-06-08 | 2014-11-04 | Otsuka Chemical Co., Ltd. | Sodium hexatitanate and method for production thereof |
| JP2008110918A (en) * | 2008-01-28 | 2008-05-15 | Jfe Mineral Co Ltd | Nonfibrous potassium titanate |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2528462B2 (en) | 1996-08-28 |
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