JPS62252302A - Production of aqueous solution of titanium hydroperoxide of high purity - Google Patents

Production of aqueous solution of titanium hydroperoxide of high purity

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Publication number
JPS62252302A
JPS62252302A JP9358486A JP9358486A JPS62252302A JP S62252302 A JPS62252302 A JP S62252302A JP 9358486 A JP9358486 A JP 9358486A JP 9358486 A JP9358486 A JP 9358486A JP S62252302 A JPS62252302 A JP S62252302A
Authority
JP
Japan
Prior art keywords
titanium
hydrogen peroxide
aqueous solution
purity
high purity
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
Application number
JP9358486A
Other languages
Japanese (ja)
Other versions
JPH0369843B2 (en
Inventor
Masaru Shioda
塩田 勝
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
National Institute for Research in Inorganic Material
Original Assignee
National Institute for Research in Inorganic Material
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by National Institute for Research in Inorganic Material filed Critical National Institute for Research in Inorganic Material
Priority to JP9358486A priority Critical patent/JPS62252302A/en
Publication of JPS62252302A publication Critical patent/JPS62252302A/en
Publication of JPH0369843B2 publication Critical patent/JPH0369843B2/ja
Granted legal-status Critical Current

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Abstract

PURPOSE:A fine powder of titanium hydride is dissolved in aqueous hydrogen peroxide to enable the easy production of aqueous solution of titanium hydroperoxide high purity which is used for making powder, film or fiber of high-purity titanium dioxide. CONSTITUTION:Titanium hydride is crushed in an non-oxidizing atmosphere and then resultant fine particles are dissolved in an aqueous hydrogen peroxide to give the objective aqueous solution of titanium hydroperoxide of high purity. When the resultant aqueous solution is allowed to stand at room temperature, the gradual condensation reaction of the hydroperoxide occurs to form a gel. A solid body is coated with the gel and dried with air to form a coating layer. Then, the gel is dried and heat-treated to give a powder of titanium oxide. Thus, the starting materials include only titanium, hydrogen and oxygen, resulting in production of titanium oxide of high purity without admixture of impurities.

Description

【発明の詳細な説明】 産業上の利用分野 本発明は高純度酸化チタンの粉末、膜、繊維構造体を作
るのに有用な高純度過酸化水素化チタン水溶液の製造法
に関するものである。
DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for producing a high-purity titanium hydrogen peroxide aqueous solution useful for producing high-purity titanium oxide powder, membranes, and fibrous structures.

従来技術 従来の水酸化チタン又は酸化チタンの製造法としては、
塩化チタン、硫酸チタン或いはアルコキシチタン等のチ
タン塩を原料に用いて、加水分解する方法、又は酸化す
る方法、もしくは両者の併用が知られている。これらの
方法によると水酸化チタン或いは酸化チタンの生成の場
に於いて、不純分の原因となる成分即ち硫酸塩、塩化物
、塩素。
Prior Art Conventional methods for producing titanium hydroxide or titanium oxide include:
A method of hydrolyzing or oxidizing a titanium salt such as titanium chloride, titanium sulfate, or alkoxytitanium as a raw material, or a combination of both is known. According to these methods, in the production of titanium hydroxide or titanium oxide, components that cause impurities, such as sulfates, chlorides, and chlorine, are removed.

或いはアルコールのいずれかが存在している。そのため
、これらの物質は水酸化チタン又は酸化チタンに取り込
まれて、これらを不純にしていた。
or alcohol is present. Therefore, these substances were incorporated into titanium hydroxide or titanium oxide, making them impure.

又過酸化水素化チタン水溶液としては高濃度塩酸酸性の
塩化チタンおよび高濃度硫酸酸性硫酸チタンに過酸化水
素水を加えたものが知られているが、これらを分解して
も前記と同じ理由で、不純な水酸化チタンが得られる。
In addition, titanium hydrogen peroxide aqueous solutions are known to include highly concentrated hydrochloric acid acidic titanium chloride and highly concentrated sulfuric acid acidic titanium sulfate with hydrogen peroxide solution added, but even if these are decomposed, it will not work for the same reason as above. , impure titanium hydroxide is obtained.

発明の目的 本発明は従来法における欠点を解消するために行ったも
ので、第一の目的は高純度水酸化チタンおよび高純度酸
化チタンを得るために、不純物の原因となる成分を含ま
ない原料としての高純度の過酸化水素化チタン水溶液の
製造法を提供することである。第二の目的は高純度水酸
化チタンおよび高純度酸化チタンを得るにさいして、環
境を汚染する物質を発生しない原料としての高純度の過
酸化水素化チタン水溶液の製造法を提供することである
。第三の目的は高純度水酸化チタンおよび高純度酸化チ
タンを得るにさいして、これらの形状を膜状、繊維状、
微粉末状に容易に得ることが出来る高純度過酸化水素化
チタン水溶液の製造法を提供することである。
Purpose of the Invention The present invention was carried out to eliminate the drawbacks of conventional methods, and the first purpose is to produce raw materials that do not contain components that cause impurities, in order to obtain high-purity titanium hydroxide and high-purity titanium oxide. An object of the present invention is to provide a method for producing a highly pure aqueous titanium peroxide solution. The second purpose is to provide a method for producing a high-purity titanium peroxide aqueous solution as a raw material that does not generate substances that pollute the environment when obtaining high-purity titanium hydroxide and high-purity titanium oxide. . The third purpose is to obtain high-purity titanium hydroxide and high-purity titanium oxide, which can be shaped into membranes, fibers, or
An object of the present invention is to provide a method for producing a high-purity titanium hydrogen peroxide aqueous solution that can be easily obtained in the form of a fine powder.

発明の構成 本発明者は、前記目的を達成するために研究した結果、
水素化チタン微粉末と過酸化水素水溶液とを混合して、
溶解させると、高純度の水酸化チタン並びに高純度酸化
チタンの製造原料として好適な高純度過酸化水素化チタ
ン水溶液が得られることを見出した。この知見に基づい
て本発明を完成したものである。
Structure of the Invention As a result of research to achieve the above object, the present inventor has discovered that
Mix titanium hydride fine powder and hydrogen peroxide aqueous solution,
It has been found that when dissolved, a high-purity titanium hydrogen peroxide aqueous solution suitable as a raw material for producing high-purity titanium hydroxide and high-purity titanium oxide can be obtained. The present invention was completed based on this knowledge.

本発明の要旨は、 水素化チタン微粉末と過酸化水素水溶液とを混合して、
溶解させることを特徴とする高純度過酸化水素化チタン
水溶液の製造法にある。
The gist of the present invention is to mix titanium hydride fine powder and a hydrogen peroxide aqueous solution,
The present invention provides a method for producing a high-purity titanium hydrogen peroxide aqueous solution, which is characterized by dissolving it.

本発明で使用する水素化チタン微粉末は通常入手出来る
塊状乃至粗粒状の水素化チタンを非酸化性雰囲気下、例
えば水中で粉砕し、微粉の泥状として得るか、或いは常
温で泥状を風乾して乾燥微粉末として得る。なお、水素
化チタンは非常に砕は易く、粉砕して容易に微粉末とす
ることが出来るが、同時に酸化も容易である。なお、水
素化チタンは高純度スポンヂチタンに高純度水素を約4
00 ’Cで接触させても容易に得ることが出来る。
The fine titanium hydride powder used in the present invention is obtained by grinding normally available lump or coarse titanium hydride in a non-oxidizing atmosphere, for example in water, or by air-drying the slurry at room temperature. It is obtained as a dry fine powder. Incidentally, titanium hydride is very easily crushed and can be easily ground into fine powder, but at the same time it is easily oxidized. In addition, titanium hydride is made by adding about 4% of high-purity hydrogen to high-purity sponge titanium.
It can be easily obtained by contacting at 00'C.

本発明で使用する過酸化水素水は市販品でよく、これに
は多種の純度品があるが、最も好ましくは安定剤の入っ
ていない最高純度品であるが、これに限るものではない
。過酸化水素濃度は0.1%以上で溶解出来るが、濃度
が高いほど溶解速度は早くなり、また分解する分もある
ので、30%程度が好ましく、溶解後は水で稀釈しても
差し支えがない。
The hydrogen peroxide solution used in the present invention may be a commercially available product, and there are various purity products, but the most preferred is the highest purity product that does not contain stabilizers, but it is not limited to this. Hydrogen peroxide can be dissolved at a concentration of 0.1% or more, but the higher the concentration, the faster the dissolution rate, and some decomposition occurs, so a hydrogen peroxide concentration of about 30% is preferable, and after dissolution it can be diluted with water. do not have.

水素化チタン微粉末と過酸化水素水とを混合して、けん
濁させると、常温以下で容易に溶解して、黄色系色調の
高純度過酸化水素化チタン水溶液が得られる。
When fine titanium hydride powder and aqueous hydrogen peroxide are mixed and suspended, they are easily dissolved at room temperature or below, yielding a yellowish-colored high-purity aqueous titanium peroxide solution.

なお、水素化チタンは過酸化水素水との溶解反応以外に
、過酸化水素の分解反応および先に生じた過酸化水素化
チタンの縮合反応に触媒作用を持ち、両反応を促進する
。溶解反応を優先させるために、微粉末として使用する
ことが高濃度溶液を得るためには必要で、且つ室温以下
で攪拌して速やかに溶解させて、不要の水素化チタンは
出来るだけ系中に存在させないことが好ましい。
In addition to the dissolution reaction with the hydrogen peroxide solution, titanium hydride has a catalytic effect on the decomposition reaction of hydrogen peroxide and the condensation reaction of titanium hydrogen peroxide that occurs previously, promoting both reactions. In order to give priority to the dissolution reaction, it is necessary to use it as a fine powder to obtain a highly concentrated solution, and to quickly dissolve it by stirring at room temperature or below, as much as possible of unnecessary titanium hydride is removed from the system. Preferably, it is not present.

得られた高純度過酸化水素化チタン水溶液から熱分解に
よって高純度過酸化水素化チタンおよび高純度酸化チタ
ンを得ることが出来る。その過程は以下の通りである。
High purity titanium hydrogen peroxide and high purity titanium oxide can be obtained from the obtained high purity titanium hydrogen peroxide aqueous solution by thermal decomposition. The process is as follows.

高純度過酸化水素化チタン水溶液は冷温下では準安定で
あるが、室温程度では、最初に遊離の過酸化水素を分解
して多量の酸素ガスを放出する。
High-purity titanium hydrogen peroxide aqueous solution is metastable at cold temperatures, but at room temperature it first decomposes free hydrogen peroxide and releases a large amount of oxygen gas.

同時に膣液の色調の黄色は時間と共に薄くなる。At the same time, the yellow color of the vaginal fluid becomes lighter over time.

続いて過酸化水素化チタンの縮合が生じ、その縮合度を
徐々に増して行き、粘ちょう性の増加として見られ、ゼ
リー状を示すようになる。一般的には、室温下では数時
間から数日間、或いは100℃下では数分間から数時間
にわたって、この状態が続く。遂には縮合過酸化水素化
チタンが沈降する、最終的には沈降物は水酸化チタンに
変化する。
Subsequently, condensation of titanium hydrogen peroxide occurs, and the degree of condensation gradually increases, which is seen as an increase in viscosity and a jelly-like appearance. Generally, this state continues for several hours to several days at room temperature, or for several minutes to several hours at 100°C. Eventually, condensed titanium hydrogen peroxide precipitates, and finally the precipitate changes to titanium hydroxide.

低濃度、低縮合度のゲルを固体上に付着させて、これを
風乾すると被膜が形成される。ゲルを急速に凍結乾燥す
ると空隙を持った立体構造体が出来る。また、ゲルを徐
々に凍結すると粗大粒となる。
A film is formed by depositing a low concentration, low degree of condensation gel on a solid and air drying it. Rapid freeze-drying of the gel creates a three-dimensional structure with voids. Furthermore, when the gel is gradually frozen, it becomes coarse particles.

縮合過酸化水素化チタンのゲル液を乾燥したものを徐々
に昇温しでいくと、約100℃で脱水、吸熱が生じ、約
250〜320℃で脱水、脱酸素および発熱が生じ、4
50℃以上で加熱前の形状を保った酸化チタンとなる。
When the temperature of a dried gel solution of condensed titanium hydrogen peroxide is gradually raised, dehydration and endotherm occur at about 100°C, dehydration, deoxygenation, and heat generation occur at about 250 to 320°C.
At 50°C or higher, titanium oxide becomes titanium oxide that maintains its shape before heating.

急速に加熱すると、脱ガスによって以前の形状は壊れて
粉状となる。
When heated rapidly, degassing causes the former shape to collapse and become powder-like.

発明の効果 本発明の方法によるときは酸化チタンの製造原料として
、次ような優れた効果を有する。
Effects of the Invention The method of the present invention has the following excellent effects as a raw material for producing titanium oxide.

第一に、原料中に、チタン、水素、および酸素以外の元
素を含まないので、原料自体から不純物を発生しない、
また該原料に添加物を加える必要がなく、ただ熱的に分
解するだけでよいので、不純物の混入が避けられて、高
純度品が得られる。第二に、原料中に、チタン、水素、
および酸素以外の元素を含まないので、原料自体から不
純物を発生しない、また該原料に添加物を加える必要が
なく、ただ熱的に分解するだけでよいので、環境を汚染
する物質を発生しない。第三に高純度を保ちながら、形
状を膜状、繊維状、微粉末状に容易に得ることが出来る
First, the raw materials do not contain any elements other than titanium, hydrogen, and oxygen, so the raw materials themselves do not generate impurities.
Furthermore, since there is no need to add additives to the raw material and only thermal decomposition is required, contamination with impurities can be avoided and a highly pure product can be obtained. Second, the raw materials contain titanium, hydrogen,
Since it does not contain any elements other than oxygen, it does not generate impurities from the raw material itself, and there is no need to add additives to the raw material, and it only needs to be thermally decomposed, so it does not generate substances that pollute the environment. Thirdly, it can be easily formed into a film, fiber, or fine powder form while maintaining high purity.

実施例 塊状の水素化チタンを少量の水に浸しながら乳鉢中で粉
砕して、微粉の泥状として、これを風乾して乾燥微粉末
として、その微粉47■を10m1の30%高純度酸化
水素水に加え、混合して、しばらくすると溶解して、黄
色の高純度過酸化水素化チタン水溶液を得た。
Example: A block of titanium hydride is crushed in a mortar while soaked in a small amount of water to form a fine powder slurry, which is air-dried to form a dry fine powder. 47 cm of the fine powder is added to 10 ml of 30% high purity hydrogen oxide. It was added to water, mixed, and dissolved after a while to obtain a yellow high-purity titanium hydrogen peroxide aqueous solution.

手続補正書 昭和62年2月々り 特許庁長官 小 川 邦 夫 殿 1、事件の表示 昭和61年特許願第93584号 2、発明の名称 高純度過酸化水素化チタン水溶液の製造法3、補正をす
る者 事件との関係 特許出願人 瀬   高   信   ai、、゛    ・5、補
正により増加する発明の数 なし6、補正の対象 明細書の発明の詳細な説明の欄 7、補正の内容 別紙 (1)明細書第2頁6行「過酸化水素水」を「過酸化水
素水溶液」と訂正する。
Procedural amendment filed in February 1988 Kunio Ogawa, Commissioner of the Patent Office1, Indication of the case Patent Application No. 93584 filed in 19882, Name of the invention Process for producing a high-purity titanium hydrogen peroxide aqueous solution3, Amendment Relationship with the patent applicant Takanobu Sase ai,,゛・5, Number of inventions increased by the amendment None6, Detailed explanation of the invention in the specification subject to the amendment 7, Contents of the amendment attached sheet (1) ) On page 2 of the specification, line 6, "Hydrogen peroxide solution" is corrected to "Hydrogen peroxide solution."

(2)同第2頁11行「行ったもので、」を[行ったも
のである。]と訂正する。
(2) Page 2, line 11, “I did it,” means “I did it.” ] Correct.

(3)同第4頁5〜6行「過酸化水素水は市販品で・・
・・・・があるが」を「過酸化水素水溶液は市販品でよ
いが、これには多種の純度品があり、」と訂正する。
(3) Page 4, lines 5-6 “Hydrogen peroxide is a commercially available product...
``There is...'' was corrected to ``A commercially available hydrogen peroxide solution is fine, but there are many different purity products.''

(4)同第4真下から8行、同上から4行「過酸化水素
水」を「過酸化水素水溶液」と訂正する。
(4) Correct "hydrogen peroxide solution" to "hydrogen peroxide solution" in the 8th line from the bottom of the 4th line and the 4th line from the top.

(5)同第5頁6行「高純度過酸化水素化チタン」を「
高純度水酸化チタン」と訂正する。
(5) Page 5, line 6 “High purity titanium hydrogen peroxide”
"High purity titanium hydroxide".

(6)同第6頁12行「次ような」を「次のような」と
訂正する。
(6) On page 6, line 12, ``like the following'' is corrected to ``like the following''.

(7)同第6頁15行、および路行「添加物」を「分解
剤」と訂正する。
(7) On page 6, line 15, the word "additive" is corrected to "decomposer."

(8)同第7頁9行「高純度酸化水素水」を[高純度過
酸化水素水溶液]と訂正する。
(8) On page 7, line 9, "High purity hydrogen oxide solution" is corrected to "High purity hydrogen peroxide solution."

Claims (1)

【特許請求の範囲】[Claims] 水素化チタン微粉末と過酸化水素水溶液とを混合して、
溶解させることを特徴とする高純度過酸化水素化チタン
水溶液の製造法。
Mix titanium hydride fine powder and hydrogen peroxide aqueous solution,
A method for producing a high-purity titanium hydrogen peroxide aqueous solution, which is characterized by dissolving it.
JP9358486A 1986-04-23 1986-04-23 Production of aqueous solution of titanium hydroperoxide of high purity Granted JPS62252302A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP9358486A JPS62252302A (en) 1986-04-23 1986-04-23 Production of aqueous solution of titanium hydroperoxide of high purity

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP9358486A JPS62252302A (en) 1986-04-23 1986-04-23 Production of aqueous solution of titanium hydroperoxide of high purity

Publications (2)

Publication Number Publication Date
JPS62252302A true JPS62252302A (en) 1987-11-04
JPH0369843B2 JPH0369843B2 (en) 1991-11-05

Family

ID=14086329

Family Applications (1)

Application Number Title Priority Date Filing Date
JP9358486A Granted JPS62252302A (en) 1986-04-23 1986-04-23 Production of aqueous solution of titanium hydroperoxide of high purity

Country Status (1)

Country Link
JP (1) JPS62252302A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004196647A (en) * 2003-09-09 2004-07-15 Monet Associates:Kk Method of manufacturing titanium hydroperoxide solution

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004196647A (en) * 2003-09-09 2004-07-15 Monet Associates:Kk Method of manufacturing titanium hydroperoxide solution

Also Published As

Publication number Publication date
JPH0369843B2 (en) 1991-11-05

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