JPH0627001B2 - Method for producing trimagnesium phosphate powder - Google Patents

Method for producing trimagnesium phosphate powder

Info

Publication number
JPH0627001B2
JPH0627001B2 JP2079793A JP7979390A JPH0627001B2 JP H0627001 B2 JPH0627001 B2 JP H0627001B2 JP 2079793 A JP2079793 A JP 2079793A JP 7979390 A JP7979390 A JP 7979390A JP H0627001 B2 JPH0627001 B2 JP H0627001B2
Authority
JP
Japan
Prior art keywords
trimagnesium phosphate
magnesium
producing
water
phosphate
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 - Lifetime
Application number
JP2079793A
Other languages
Japanese (ja)
Other versions
JPH03279205A (en
Inventor
善之 横川
資三 川村
ゆかり 河本
素弘 鳥山
高広 鈴木
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 of Advanced Industrial Science and Technology AIST
Original Assignee
Agency of Industrial Science and Technology
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 Agency of Industrial Science and Technology filed Critical Agency of Industrial Science and Technology
Priority to JP2079793A priority Critical patent/JPH0627001B2/en
Publication of JPH03279205A publication Critical patent/JPH03279205A/en
Publication of JPH0627001B2 publication Critical patent/JPH0627001B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Compositions Of Oxide Ceramics (AREA)
  • Materials For Medical Uses (AREA)

Description

【発明の詳細な説明】 3.1産業上の利用分野 この発明は、リン酸三マグネシウム粉体の製造法に関す
るものである。
TECHNICAL FIELD The present invention relates to a method for producing trimagnesium phosphate powder.

リン酸三マグネシウムは王水難溶性などの特性を持ち、
その8水和物はCaHPO4・2H2Oの安定剤として工業的に重
要な化合物である。
Trimagnesium phosphate has characteristics such as poor solubility in aqua regia,
The octahydrate is an industrially important compound as a stabilizer of CaHPO 4 .2H 2 O.

この明細書において、「リン酸マグネシウム化合物」な
る用語は、リン酸水素マグネシウムあるいは酸化マグネ
シウム、炭酸マグネシウム等の所要割合での反応の結果
として生成せられる化合物を意味し、その代表例として
はMg3(PO4)2すなわちトリマグネシウムホスフェイト
(以下TMPと記述する)およびその多水和物Mg3(PO4)
2・8H2O(以下、TMP8と記述する)、Mg3(PO4)2・22
H2O(いか、TMP22と記述する)が挙げられる。
In this specification, the term "magnesium phosphate compound" means a compound formed as a result of a reaction of magnesium hydrogen phosphate, magnesium oxide, magnesium carbonate, etc. in a required ratio, and a typical example thereof is Mg 3 (PO 4 ) 2 or Trimagnesium Phosphate (hereinafter referred to as TMP) and its polyhydrate Mg 3 (PO 4 ).
2 · 8H 2 O (hereinafter, referred to as TMP8), Mg 3 (PO 4 ) 2 · 22
H 2 O (squid, described as TMP22) can be mentioned.

またこの明細書において割合を表わす%はすべて重量に
基づいて計算した値である。
Further, in this specification, all percentages that represent ratios are values calculated based on weight.

3.2従来技術及びその問題点 リン酸三マグネシウムの製造法としてはアンモニアアル
カリ溶液中でMgNH4PO4・6H2Oより22水和物をへて8水和
物を得る方法が一般的であるが、この方法では目的物の
生成に約2ケ月という非常に長時間を要する。またNa2H
PO4とMgSO4を水溶液中で80-90℃で2-48時間加熱するこ
とにより8水和物を得る方法もあるが、反応開始時にpH
を6.4-7.0に調節する必要がある。そのため簡便にリン
酸三マグネシウム粉体を製造する技術を開発することが
期待されるものである。
3.2 Prior art and its problems The general method for producing trimagnesium phosphate is to obtain octahydrate by converting 22 hydrate from MgNH 4 PO 4 .6H 2 O in an alkaline solution of ammonia. However, in this method, it takes a very long time of about 2 months to produce the target substance. Also Na 2 H
There is also a method of obtaining octahydrate by heating PO 4 and MgSO 4 in an aqueous solution at 80-90 ° C for 2-48 hours.
Need to be adjusted to 6.4-7.0. Therefore, it is expected to develop a technology for easily producing trimagnesium phosphate powder.

この発明は、上記のような実状からなされたものであっ
て、リン酸三マグネシウム粉体を簡便に合成する製造技
術を提供することを目的とする。
The present invention has been made in the above-mentioned circumstances, and an object thereof is to provide a manufacturing technique for easily synthesizing trimagnesium phosphate powder.

3.3問題の解決手段 この発明によるリン酸三マグネシウム粉体の合成法は、
上記目的の達成のために、比較的短時間に、かつpH調節
等の操作を必要としない製造法を提供することを目的と
する。
3.3 Solution to Problem The method for synthesizing trimagnesium phosphate powder according to the present invention is
In order to achieve the above object, it is an object of the present invention to provide a production method that does not require operations such as pH adjustment in a relatively short time.

はじめにリン酸水素マグネシウムと酸化マグネシウムあ
るいは炭酸マグネシウムをモル比で2:1の割合で秤量
し、水を重量比で10%以上加えポットミル中、室温で撹
拌する。得られたスラリーを50〜60℃で乾燥し、リン酸
三マグネシウムの多水和物が得られる。水に難溶性のリ
ン酸水素マグネシウムと酸化マグネシウムあるいは炭酸
マグネシウムを出発原料に用い、ポットミル中、水の存
在下で機械的な力を加えることで、徐々に反応が進行す
るが、この反応は数時間で完了する。このように特にpH
調節を行わず比較的短時間に、リン酸三マグネシウムの
多水和物が合成できる。
First, magnesium hydrogen phosphate and magnesium oxide or magnesium carbonate are weighed at a molar ratio of 2: 1, water is added at 10% or more by weight ratio, and the mixture is stirred at room temperature in a pot mill. The obtained slurry is dried at 50 to 60 ° C to obtain a polyhydrate of trimagnesium phosphate. The reaction proceeds gradually by applying mechanical force in the presence of water in a pot mill using magnesium hydrogen phosphate and magnesium oxide or magnesium carbonate, which are sparingly soluble in water, as starting materials. Complete in time. Thus especially pH
Polyhydrate of trimagnesium phosphate can be synthesized in a relatively short time without adjustment.

次に、700〜800℃の仮焼処理を行うことで無水のリン酸
三マグネシウムが得られる。
Then, an anhydrous trimagnesium phosphate is obtained by performing a calcination treatment at 700 to 800 ° C.

3.4作用 リン酸水素マグネシウムと酸化マグネシウムあるいは炭
酸マグネシウムを2:1の割合で秤量し、水を重量比で30%
以上加えポットミル中、室温で数時間撹拌する。水に難
溶性の粉末を出発原料に用い、ポットミル中、水の存在
下で機械的な力を加えることで、いわゆるメカノケミカ
ル的な反応が起こりTMP8が得られた。一方、水を加
えないとポットミル中で撹拌しても出発物質のまま変化
はみられず、また水の重量比を10%と少なくするとTM
P22が得られた。
3.4 Action Magnesium hydrogen phosphate and magnesium oxide or magnesium carbonate are weighed in a ratio of 2: 1 and water is 30% by weight.
Add the above and stir at room temperature for several hours in a pot mill. TMP8 was obtained by using a powder that is hardly soluble in water as a starting material and applying a mechanical force in the presence of water in a pot mill to cause a so-called mechanochemical reaction. On the other hand, if water is not added, the starting material remains unchanged even if stirred in a pot mill, and if the weight ratio of water is reduced to 10%, TM
P22 was obtained.

得られたリン酸三マグネシウム多水和物のスラリーを乾
燥後、加熱するとまず50〜200℃で構造水等の脱離によ
り非晶質となり、更に約650〜700℃で結晶化し(熱分析
で確認)、結晶質リン酸三マグネシウム粉体が得られ
る。そのため仮焼処理は、700〜800℃で行うのが望まし
い。
When the obtained slurry of trimagnesium phosphate polyhydrate is dried and heated, it first becomes amorphous at 50 to 200 ° C due to the elimination of structural water, etc., and crystallizes at about 650 to 700 ° C (by thermal analysis. Confirmation), crystalline trimagnesium phosphate powder is obtained. Therefore, it is desirable that the calcination process be performed at 700 to 800 ° C.

3.5発明の効果 以上の次第で、この発明によるリン酸三マグネシウム化
合物セラミックスの製造技術は、出発原料をポットミル
中で数時間以上撹拌し、その後仮焼するもので、比較的
簡便にリン酸三マグネシウム粉体を合成することができ
る。
3.5 Effects of the Invention According to the above, in the technology for producing a trimagnesium phosphate compound ceramics according to the present invention, the starting material is stirred in a pot mill for several hours or more and then calcined. Trimagnesium powder can be synthesized.

またこの発明によれば、冒頭で説明したようにpH調節等
の操作が必要なく、また比較的短時間で合成が可能であ
るため、製品の製造においてランニングコストダウンを
果たすことができる。
Further, according to the present invention, as described at the beginning, operations such as pH adjustment are not necessary and the synthesis can be performed in a relatively short time, so that the running cost can be reduced in the production of the product.

3.6実施例 次にこの発明の効果を実証するために実施例を示す。3.6 Example Next, an example will be shown in order to demonstrate the effect of the present invention.

実施例 1 リン酸水素マグネシウムと酸化マグネシウムをモル比で
2:1の割合に秤量し、重量比で10%以上になるように水を
加え、ポットミル中、室温下において毎分50回転で撹拌
する。撹拌後、乾燥し得られた粉体を700〜800℃で仮焼
すると目的とするTMPが得られる。
Example 1 Magnesium hydrogen phosphate and magnesium oxide in a molar ratio
Weigh it at a ratio of 2: 1, add water so that the weight ratio becomes 10% or more, and stir at 50 rpm at room temperature in a pot mill. After stirring, the powder obtained by drying is calcined at 700 to 800 ° C. to obtain the target TMP.

実施例 2 リン酸水素マグネシウムと炭酸マグネシウムをモル比で
2:1の割合に秤量し、重量比で10%以上になるように水を
加え、ポットミル中、室温下において毎分50回転で撹拌
する。撹拌後、乾燥し得られた粉体を700〜800℃で仮焼
すると目的とするTMPが得られる。
Example 2 Magnesium hydrogen phosphate and magnesium carbonate in a molar ratio
Weigh it at a ratio of 2: 1, add water so that the weight ratio becomes 10% or more, and stir at 50 rpm at room temperature in a pot mill. After stirring, the powder obtained by drying is calcined at 700 to 800 ° C. to obtain the target TMP.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 鈴木 高広 愛知県名古屋市北区八代町2丁目109番地 八代寮101号 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Takahiro Suzuki 2-109, 2-chome, Yatsushiro-cho, Kita-ku, Nagoya-shi, Aichi Yatsushiro 101

Claims (4)

【特許請求の範囲】[Claims] 【請求項1】リン酸水素マグネシウムと酸化マグネシウ
ムあるいは炭酸マグネシウムを秤量し水を適当量加え、
ポットミル中室温で撹拌する。得られたスラリーを乾燥
し、多水和物のリン酸三マグネシウム粉末を得る。さら
に仮焼することにより無水のリン酸三マグネシウムを得
ることを特徴とする、リン酸三マグネシウム化合物セラ
ミックスの製造法。
1. Magnesium hydrogen phosphate and magnesium oxide or magnesium carbonate are weighed and an appropriate amount of water is added,
Stir in a pot mill at room temperature. The obtained slurry is dried to obtain a polyhydrated trimagnesium phosphate powder. A method for producing trimagnesium phosphate compound ceramics, characterized in that anhydrous trimagnesium phosphate is obtained by calcination.
【請求項2】リン酸水素マグネシウムと酸化マグネシウ
ムあるいは炭酸マグネシウムを秤量するが、その割合は
モル比で2:1であり、水は重量比で10%以上で行われる特
許請求の範囲第一項記載の製造法。
2. Magnesium hydrogen phosphate and magnesium oxide or magnesium carbonate are weighed, the ratio is 2: 1 by molar ratio, and water is 10% or more by weight ratio. The manufacturing method described.
【請求項3】ポットミル中で撹拌するが、撹拌時間は1
時間以上が必要である。得られたスラリーは乾燥するが
好ましくは50〜60℃以下で行われる特許請求の範囲第一
項記載の製造法。
3. Stir in a pot mill, but the stirring time is 1
Need more time. The obtained slurry is dried, but preferably the production method according to claim 1, which is performed at 50 to 60 ° C or lower.
【請求項4】仮焼温度は600〜1200℃とする特許請求の
範囲第一項記載の製造法。
4. The production method according to claim 1, wherein the calcination temperature is 600 to 1200 ° C.
JP2079793A 1990-03-28 1990-03-28 Method for producing trimagnesium phosphate powder Expired - Lifetime JPH0627001B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2079793A JPH0627001B2 (en) 1990-03-28 1990-03-28 Method for producing trimagnesium phosphate powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2079793A JPH0627001B2 (en) 1990-03-28 1990-03-28 Method for producing trimagnesium phosphate powder

Publications (2)

Publication Number Publication Date
JPH03279205A JPH03279205A (en) 1991-12-10
JPH0627001B2 true JPH0627001B2 (en) 1994-04-13

Family

ID=13700097

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2079793A Expired - Lifetime JPH0627001B2 (en) 1990-03-28 1990-03-28 Method for producing trimagnesium phosphate powder

Country Status (1)

Country Link
JP (1) JPH0627001B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106829904A (en) * 2017-02-28 2017-06-13 连云港市德邦精细化工有限公司 A kind of preparation method of graininess calcium phosphate dibasic anhydrous

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4562512B2 (en) * 2004-12-20 2010-10-13 宇部マテリアルズ株式会社 Method for producing high purity trimagnesium phosphate
JP4758112B2 (en) * 2005-02-24 2011-08-24 メタウォーター株式会社 Method for regenerating ammonia and / or ammonium ion absorbent and method for recovering ammonia and / or ammonium ion using regenerated absorbent

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106829904A (en) * 2017-02-28 2017-06-13 连云港市德邦精细化工有限公司 A kind of preparation method of graininess calcium phosphate dibasic anhydrous
CN106829904B (en) * 2017-02-28 2019-02-12 连云港市德邦精细化工有限公司 A kind of preparation method of graininess calcium phosphate dibasic anhydrous

Also Published As

Publication number Publication date
JPH03279205A (en) 1991-12-10

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