JPS58161911A - Manufacture of beta-form calcium tertiary phosphate - Google Patents

Manufacture of beta-form calcium tertiary phosphate

Info

Publication number
JPS58161911A
JPS58161911A JP4545482A JP4545482A JPS58161911A JP S58161911 A JPS58161911 A JP S58161911A JP 4545482 A JP4545482 A JP 4545482A JP 4545482 A JP4545482 A JP 4545482A JP S58161911 A JPS58161911 A JP S58161911A
Authority
JP
Japan
Prior art keywords
neutralization reaction
calcination
calcium phosphate
temperature
carried out
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
Application number
JP4545482A
Other languages
Japanese (ja)
Inventor
Isao Tetsuka
手束 功
Michiteru Miyoshi
三好 通曜
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.)
Taihei Chemical Industrial Co Ltd
Original Assignee
Taihei Chemical Industrial Co Ltd
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 Taihei Chemical Industrial Co Ltd filed Critical Taihei Chemical Industrial Co Ltd
Priority to JP4545482A priority Critical patent/JPS58161911A/en
Publication of JPS58161911A publication Critical patent/JPS58161911A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To manufacture the titled compound of high purity in a high yield by carrying out the neutralization reaction of CaO with H3PO4 at a low temp. and calcining a specified intermediate as a neutralization reaction product at a low temp. for a short time. CONSTITUTION:A phosphoric acid soln. is slowly added to an aqueous suspension of calcium oxide with stirring to carry out a neutralization reaction, and the resulting hydroxyapatite (calcium phosphate) is converted into beta-form calcium tertiary phosphate by calcination. At this time, the neutralization reaction is carried out at <=60 deg.C, and the calcination is carried out at >=750 deg.C. By carrying out the neutralization reaction at such a low temp., the calcination temp. of the hydroxyapatite as an intermediate is reduced, the calcination time is shortened, and a high purity product can be obtd. in a high yield. The manufacturing cost can be also reduced.

Description

【発明の詳細な説明】 この発明は、酸化カルシウムとリン酸の中和反応により
ハイドロオキシアパタイトリン酸カルシウムを得、これ
を焼成してβ型第3リン酸カルシウムに変換するβ型第
3リン酸カルシウムの製造方法に関する。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing β-type tribasic calcium phosphate, which involves obtaining hydroxyapatite calcium phosphate through a neutralization reaction between calcium oxide and phosphoric acid, and converting it into β-type tribasic calcium phosphate by firing. .

β型第3リン酸カルシウムは、近年窯業関係の原料とし
て多量に用いられるよう番こなり、高純度で且つ安価な
ものが求められている。従来、この化合物は、酸化カル
シウムとリン酸の中和反応を60℃以上特に100℃前
後の温度で行ない、得られたハイドロオキシアパタイト
リン酸カルシウムの焼成を900℃以上特に1200℃
前後の高温で数時間特に6時間前後行なうことにより製
造されていた。しかしこの場合、中和反応の温度が高い
ため、中間体ハイドロオキシアパタイトリン酸カルシウ
ムの焼成(こ高温および長時間を要して、熱コスト的に
はなはだ不経済である上に、変換率が低くて中間体ハイ
ドロオキシアパタイトリン酸カルシウムが残留し、この
点でも製品のコスト高をまねくという問題があった。
In recent years, β-type tertiary calcium phosphate has been used in large quantities as a raw material for ceramics, and there is a demand for high purity and low cost. Conventionally, this compound has been produced by carrying out a neutralization reaction of calcium oxide and phosphoric acid at a temperature of 60°C or higher, especially around 100°C, and then firing the obtained hydroxyapatite calcium phosphate at a temperature of 900°C or higher, especially 1200°C.
It was manufactured by performing the process at a high temperature for several hours, especially around 6 hours. However, in this case, since the temperature of the neutralization reaction is high, the calcination of the intermediate hydroxyapatite calcium phosphate (this requires high temperature and a long time, is very uneconomical in terms of heat cost, and the conversion rate is low, resulting in intermediate There is a problem in that hydroxyapatite calcium phosphate remains in the body, which also increases the cost of the product.

この発明は、上記のような問題を克服すべくなされたも
ので、焼成温度を低くし且つ焼成時間を短縮し、高収率
で高純度の製品を得ることができ、その結果製造原価の
低廉化を果すことのできるβ厘第3リン酸カルシウムの
製造方法を提供することを目的とする。
This invention was made to overcome the above-mentioned problems, and it is possible to lower the firing temperature and shorten the firing time, thereby obtaining a high-yield and high-purity product, and as a result, the manufacturing cost can be reduced. An object of the present invention is to provide a method for producing β-tribasic calcium phosphate, which can achieve the following effects.

この発明Cζよるβ型第3リン酸カルシウムの製造方法
は、酸化カルシウムの水性懸濁液に撹拌下にリン酸液を
徐々に添加して中和反応を行ない、得られたハイドロオ
キシアパタイトリン酸カルシウムを焼成してβ型第3リ
ン酸カルシウムに変換するに当り、中和反応を60℃以
下の温度で行ない、焼成を750℃以上の温度で行なう
ことを特徴とする。
The method for producing β-type tertiary calcium phosphate according to this invention Cζ involves gradually adding a phosphoric acid solution to an aqueous suspension of calcium oxide under stirring to carry out a neutralization reaction, and calcining the obtained hydroxyapatite calcium phosphate. When converting into β-type tertiary calcium phosphate, the neutralization reaction is carried out at a temperature of 60°C or lower, and the calcination is carried out at a temperature of 750°C or higher.

中和反応において、反応温度が60℃以下に限定される
理由は、温度が60℃を越えると、得られた中間体ハイ
ドロオキシアパタイトリン酸カルシウムの焼成に高温お
よび長時間を要するからである。最適反応温度は室温〜
45℃である。中和反応の時間は約2時間で十分である
The reason why the reaction temperature in the neutralization reaction is limited to 60°C or lower is that if the temperature exceeds 60°C, it will take a high temperature and a long time to calcinate the obtained intermediate hydroxyapatite calcium phosphate. Optimal reaction temperature is room temperature ~
The temperature is 45°C. Approximately 2 hours is sufficient for the neutralization reaction.

中間体ハイドロオキシアパタイトリン酸カルシウムの焼
成において、焼成温度が750℃以上に限定される理由
は、750℃未満ではハイドロオキシアパタイトリン酸
カルシウムからβ型第3リン酸カルシウムへの変換が十
分になされないからである。最適温度は800℃以上で
ある。焼成時間は、温度とも関連するが、約30分で十
分である。
In the firing of the intermediate hydroxyapatite calcium phosphate, the reason why the firing temperature is limited to 750°C or higher is that at lower than 750°C, sufficient conversion from hydroxyapatite calcium phosphate to β-type tertiary calcium phosphate is not achieved. The optimum temperature is 800°C or higher. The firing time is related to the temperature, but about 30 minutes is sufficient.

この発明によるβ型第3リン酸カルシウムの製造方法は
、以上のとおり構成されているので、焼成温度を低くし
且つ焼成時間を短縮し、高収率で高純度の製品を得るこ
とができ、その結果製造原価の低廉化を果すことができ
る。
Since the method for producing β-type tertiary calcium phosphate according to the present invention is configured as described above, it is possible to lower the calcination temperature and shorten the calcination time, and obtain a high-yield and high-purity product. Manufacturing costs can be reduced.

実施例 00vに、リン酸−←中→v2を含む25チ水溶液を撹
拌下に徐々に添加し、反応温度を30℃に保って、中和
反応を2時間行なった。生成したハイドロオキシアパタ
イトリン酸カルシウム沈殿物を沖取し、乾燥した後、温
度800℃で1時間焼成した。β型第3リン酸カルシウ
ム421(収率97%)が得られた。粉末X線回折分析
の結果、製品中にはハイドロオキシアバタイ)IJン酸
カルシウムの残留は認められず、高純度のβ型iJ3リ
ン酸カルシウムが得られたことが確認された。
To Example 00v, a 25% aqueous solution containing phosphoric acid -←middle→v2 was gradually added under stirring, and the reaction temperature was maintained at 30°C, and the neutralization reaction was carried out for 2 hours. The produced hydroxyapatite calcium phosphate precipitate was collected, dried, and then fired at a temperature of 800° C. for 1 hour. β-type tertiary calcium phosphate 421 (yield 97%) was obtained. As a result of powder X-ray diffraction analysis, no residual calcium hydroxyabatai)IJ3 phosphate was found in the product, confirming that highly pure β-type iJ3 calcium phosphate was obtained.

以  上 特許出願人  太平化学産業株式会社 外4名that's all Patent applicant: Taihei Kagaku Sangyo Co., Ltd. 4 people outside

Claims (1)

【特許請求の範囲】 (1)  酸化カルシウムの水性懸濁液に撹拌下にリン
酸液を徐々に添加して中和反応を行ない、得られたハイ
ドロオキシアパタイトリン酸カルシウムを焼成してβ型
gJ3リン酸カルシウムに変換するに当り、中和反応を
60℃以下の温度で行ない、焼成を750℃以上の温度
で行なうことを特徴とするβ型第3リン酸カルシウムの
製造方法。 (2+  中和反応を室温〜45℃で行なう特許請求の
範囲第1項記載の方法。 (3)  中和反応を約2時間行なう特許請求の範囲第
1または2項記載の方法。 (4)焼成を800℃以上で行なう特許請求の範囲第1
〜3項のうちいずれか1項記載の方法。 (5)  焼成を約30分間行なう輸許請求の範囲第1
〜4項のうちいずれか1項記載の方法。
[Scope of Claims] (1) A phosphoric acid solution is gradually added to an aqueous suspension of calcium oxide while stirring to perform a neutralization reaction, and the obtained hydroxyapatite calcium phosphate is calcined to obtain β-type gJ3 calcium phosphate. 1. A method for producing β-type tricalcium phosphate, which comprises carrying out a neutralization reaction at a temperature of 60°C or lower and calcination at a temperature of 750°C or higher. (2+ The method according to claim 1, in which the neutralization reaction is carried out at room temperature to 45°C. (3) The method according to claim 1 or 2, in which the neutralization reaction is carried out for about 2 hours. (4) Claim 1 in which firing is performed at 800°C or higher
The method according to any one of 3 to 3. (5) The first patent claim in which firing is performed for about 30 minutes
4. The method according to any one of 4.
JP4545482A 1982-03-19 1982-03-19 Manufacture of beta-form calcium tertiary phosphate Pending JPS58161911A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP4545482A JPS58161911A (en) 1982-03-19 1982-03-19 Manufacture of beta-form calcium tertiary phosphate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP4545482A JPS58161911A (en) 1982-03-19 1982-03-19 Manufacture of beta-form calcium tertiary phosphate

Publications (1)

Publication Number Publication Date
JPS58161911A true JPS58161911A (en) 1983-09-26

Family

ID=12719790

Family Applications (1)

Application Number Title Priority Date Filing Date
JP4545482A Pending JPS58161911A (en) 1982-03-19 1982-03-19 Manufacture of beta-form calcium tertiary phosphate

Country Status (1)

Country Link
JP (1) JPS58161911A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04321507A (en) * 1991-04-23 1992-11-11 Mitsubishi Materials Corp Production of calcium tertiary phosphate and hydraulic calcium phosphate cement
JP2020105060A (en) * 2018-12-28 2020-07-09 株式会社バイオアパタイト HYDROXYAPATITE, ITS PRODUCTION METHOD AND METHOD FOR PRODUCING β-TCP

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5645814A (en) * 1979-09-25 1981-04-25 Kureha Chem Ind Co Ltd Hydroxyapatite, its ceramic material and its manufacture
JPS5654841A (en) * 1979-10-08 1981-05-15 Mitsubishi Mining & Cement Co Bone broken portion and filler for void portion and method of treating bone of animal using said filler

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5645814A (en) * 1979-09-25 1981-04-25 Kureha Chem Ind Co Ltd Hydroxyapatite, its ceramic material and its manufacture
JPS5654841A (en) * 1979-10-08 1981-05-15 Mitsubishi Mining & Cement Co Bone broken portion and filler for void portion and method of treating bone of animal using said filler

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04321507A (en) * 1991-04-23 1992-11-11 Mitsubishi Materials Corp Production of calcium tertiary phosphate and hydraulic calcium phosphate cement
JP2020105060A (en) * 2018-12-28 2020-07-09 株式会社バイオアパタイト HYDROXYAPATITE, ITS PRODUCTION METHOD AND METHOD FOR PRODUCING β-TCP

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