JPH07291609A - Production of aqueous solution of aluminum phosphate - Google Patents

Production of aqueous solution of aluminum phosphate

Info

Publication number
JPH07291609A
JPH07291609A JP6090898A JP9089894A JPH07291609A JP H07291609 A JPH07291609 A JP H07291609A JP 6090898 A JP6090898 A JP 6090898A JP 9089894 A JP9089894 A JP 9089894A JP H07291609 A JPH07291609 A JP H07291609A
Authority
JP
Japan
Prior art keywords
aluminum
aluminum phosphate
reaction
aqueous solution
concentration
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
JP6090898A
Other languages
Japanese (ja)
Inventor
Motoi Takenaga
基 武永
Yukihiro Yoda
幸廣 與田
Yukio Takahashi
幸男 高橋
Osamu Matsubara
修 松原
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.)
Mitsui Toatsu Chemicals Inc
Original Assignee
Mitsui Toatsu Chemicals Inc
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 Mitsui Toatsu Chemicals Inc filed Critical Mitsui Toatsu Chemicals Inc
Priority to JP6090898A priority Critical patent/JPH07291609A/en
Publication of JPH07291609A publication Critical patent/JPH07291609A/en
Pending legal-status Critical Current

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  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

PURPOSE:To stably produce an aqueous solution of aluminum phosphate having excellent storage stability in a molar ratio of PO2O5/Al2O3 Of 2.2 to 2.8 CONSTITUTION:A solution of phosphoric acid is reacted with aluminum hydroxide and/or aluminum oxide under heating in a high-temperature range to form a transparent solution of aluminum phosphate having 60-75wt.% aluminum phosphate concentration and the molar ratio of P2O5/Al2O3 of 2.2 to 2.8 once. Then water is added to the solution and the concentration is adjusted to produce an aqueous solution of aluminum phosphate in a molar ratio of P2O5/Al2O3 of 2.2 to 2.8.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、燐酸アルミニウム水溶
液の製造方法に関し、特には、第一燐酸アルミニウムを
主成分としP2O5/Al2O3モル比2.2〜2.8である、ア
ルミニウム成分が高く、かつ安定性の高い燐酸アルミニ
ウム水溶液の製造方法に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an aqueous solution of aluminum phosphate, and in particular, it has a primary aluminum phosphate as a main component and a P 2 O 5 / Al 2 O 3 molar ratio of 2.2 to 2.8. The present invention relates to a method for producing an aluminum phosphate aqueous solution having a high aluminum component and high stability.

【0002】[0002]

【従来の技術】燐酸アルミニウムには、種々の化合物が
知られており、第一燐酸アルミニウムAl(H2PO4)3 、第
二燐酸アルミニウム Al2(HPO4)3 、第三燐酸アルミニウ
ム AlPO4、セスキ燐酸アルミニウム AlH3(PO4)2 、トリ
ポリ燐酸アルミニウム AlH2P3O 10、メタ燐酸アルミニウ
ム Al(PO3)3 などが一般的に使用されている。
2. Description of the Related Art Various compounds are contained in aluminum phosphate.
It is known that aluminum monophosphate Al (H2POFour)3, First
Aluminum diphosphate Al2(HPOFour)3Aluminum triphosphate
Mu AlPOFour, Aluminum sesquiphosphate AlH3(POFour)2,bird
Aluminum polyphosphate AlH2P3O Ten, Aluminum metaphosphate
Mu Al (PO3)3Are commonly used.

【0003】燐酸アルミニウム化合物の中で、第一燐酸
アルミニウムは、水溶性の化合物であるため水溶液とし
てしばしば使用される。また、粉末状のものも使用され
ているが、その強い吸湿性のため敬遠されることも多
い。
Among aluminum phosphate compounds, monobasic aluminum phosphate is often used as an aqueous solution because it is a water-soluble compound. Although powdery ones are also used, they are often shunned due to their strong hygroscopicity.

【0004】第一燐酸アルミニウムを主成分とする燐酸
アルミニウム水溶液は、不安定であることがすでに知ら
れており、長期保存が出来ないと言う問題点を内蔵して
いる。燐酸アルミニウム水溶液は保管中に、沈澱物が生
成し使用に不都合をきたすことがしばしばある。この沈
澱物は、第三燐酸アルミニウム、またはセスキ燐酸アル
ミニウムと言われている。燐酸アルミニウム水溶液は、
P2O5/Al2O3モル比が高いほど長期保存性が高く、一般に
はP2O5/Al2O3モル比が、2.9〜3.0のものが使用さ
れている。
It has been already known that an aqueous solution of aluminum phosphate containing aluminum monophosphate as a main component is unstable, and it has a problem that it cannot be stored for a long period of time. An aqueous solution of aluminum phosphate often causes inconvenience in use because a precipitate is formed during storage. This precipitate is called aluminum triphosphate or aluminum sesquiphosphate. Aqueous aluminum phosphate solution
The higher the P 2 O 5 / Al 2 O 3 molar ratio, the higher the long-term storage stability, and in general, the P 2 O 5 / Al 2 O 3 molar ratio of 2.9 to 3.0 is used.

【0005】燐酸アルミニウム水溶液は、耐火物結合
剤、金属表面処理剤などに幅広く使用されている。従来
の燐酸アルミニウム水溶液は、使用目的により各種の濃
度に調整され供されているが、50重量%程度のものが
一般的である。
Aqueous aluminum phosphate solutions are widely used as refractory binders, metal surface treatment agents and the like. The conventional aluminum phosphate aqueous solution is adjusted to various concentrations depending on the purpose of use, and is generally provided at about 50% by weight.

【0006】近年、耐火物結合剤、金属表面処理剤など
の用途において、アルミニウム成分の高い燐酸アルミニ
ウム水溶液の要望が高くなってきている。耐火物結合剤
ではその耐火性向上が叫ばれている中で、このアルミニ
ウム成分の高い燐酸アルミニウム水溶液の使用は耐火性
向上もさることながら、耐スポーリング性の向上も達成
できる優位性を持っている。本発明者らは、これは高温
度下での燐酸の縮合に伴う縮合水の発生が抑制されるた
めと推察している。また、金属表面処理剤では金属表面
に塗布し、加熱処理された際、生成する縮合燐酸による
表面のベタつき問題点として上げられていたが、アルミ
ニウム成分を高くすることにより、この問題点は解消で
きるのである。
In recent years, there has been an increasing demand for an aluminum phosphate aqueous solution having a high aluminum content in applications such as refractory binders and metal surface treatment agents. While refractory binders are required to improve their fire resistance, the use of an aqueous solution of aluminum phosphate having a high aluminum content has the advantage of improving fire resistance as well as spalling resistance. There is. The present inventors speculate that this is because generation of condensed water accompanying the condensation of phosphoric acid at high temperature is suppressed. Further, the metal surface treatment agent has been mentioned as a problem of stickiness of the surface due to condensed phosphoric acid generated when it is applied to a metal surface and heat-treated, but this problem can be solved by increasing the aluminum component. Of.

【0007】[0007]

【発明が解決しようとする課題】しかしながら、このア
ルミニウム成分を高くすること即ち、P2O5/Al2O3モル比
を低くすると、次の問題点があり供給の妨げとなってい
る。
However, if the aluminum component is increased, that is, the P 2 O 5 / Al 2 O 3 molar ratio is lowered, the following problems occur and supply is hindered.

【0008】従来のP2O5/Al2O3モル比2.9〜3.0の
燐酸アルミニウム水溶液は、約54重量%の燐酸液に水
酸化アルミニウムをP2O5/Al2O3モル比2.9〜3.0と
なる量混合し、90〜100℃に加熱反応させることに
より得られる。この方法でP2O5/Al2O3モル比2.2〜
2.8の燐酸アルミニウム水溶液を製造した場合、沈澱
物が生じ透明な燐酸アルミニウム水溶液が得られず、生
産性が著しく低下する。仮に透明な燐酸アルミニウム水
溶液が得られたとしても、保存安定性が低く、30日以
内に第三燐酸アルミニウム、またはセスキ燐酸アルミニ
ウムが生成、沈澱し使用に不都合をきたす。
A conventional aluminum phosphate aqueous solution having a molar ratio of P 2 O 5 / Al 2 O 3 of 2.9 to 3.0 is prepared by adding aluminum hydroxide to P 2 O 5 / Al 2 O 3 in a phosphoric acid solution of about 54% by weight. It can be obtained by mixing in a molar ratio of 2.9 to 3.0 and reacting by heating at 90 to 100 ° C. In this way, the molar ratio of P 2 O 5 / Al 2 O 3 is 2.2 to
When the 2.8 aluminum phosphate aqueous solution is produced, a precipitate is formed and a transparent aluminum phosphate aqueous solution cannot be obtained, resulting in a marked decrease in productivity. Even if a transparent aqueous solution of aluminum phosphate is obtained, the storage stability is low, and aluminum triphosphate or aluminum sesquiphosphate is formed and precipitated within 30 days, which causes inconvenience in use.

【0009】この原因として、本発明者等は透明な燐酸
アルミニウム水溶液であっても極微細な第三燐酸アルミ
ニウム、またはセスキ燐酸アルミニウムの結晶がすでに
生成していて経日とともに結晶が成長し沈澱するためと
推察している。
As a cause of this, the inventors of the present invention have already formed ultrafine aluminum triphosphate or aluminum sesquiphosphate crystals even in a transparent aqueous solution of aluminum phosphate, and the crystals grow and precipitate with the passage of time. It is supposed to be because.

【0010】[0010]

【課題を解決するための手段】本発明者等はこの様な問
題点を解決するために鋭意検討を重ねた結果、高濃度の
燐酸液に水酸化アルミニウムをP2O5/Al2O3モル比を2.
2〜2.8となる量混合して高濃度域で反応をおこな
い、透明な燐酸アルミニウム水溶液を一旦生成させ、後
で所定の濃度となる量水を添加することにより、保存安
定性の優れた燐酸アルミニウム水溶液を得ることが可能
であることを見出だし、本発明を完成させたものであ
る。
Means for Solving the Problems As a result of intensive studies made by the present inventors to solve such problems, as a result, aluminum hydroxide was added to a high-concentration phosphoric acid solution with P 2 O 5 / Al 2 O 3 The molar ratio is 2.
The mixture was mixed in an amount of 2 to 2.8 to cause a reaction in a high concentration range, a transparent aluminum phosphate aqueous solution was once generated, and then water was added to a predetermined concentration to give excellent storage stability. They have found that it is possible to obtain an aqueous solution of aluminum phosphate, and have completed the present invention.

【0011】即ち、本発明は燐酸液と水酸化アルミニウ
ム及び/又は酸化アルミニウムとを加熱反応させて、燐
酸アルミニウム濃度が60〜75重量%でP2O5/Al2O3
ル比2.2〜2.8の透明な燐酸アルミニウム水溶液を
生成させ、その後水を添加して濃度調節を行うことを特
徴とするP2O5/Al2O3モル比2.2〜2.8の燐酸アルミ
ニウム水溶液の製造方法である。
That is, according to the present invention, a phosphoric acid solution is heated and reacted with aluminum hydroxide and / or aluminum oxide to give an aluminum phosphate concentration of 60 to 75% by weight and a P 2 O 5 / Al 2 O 3 molar ratio of 2.2. To produce a transparent aqueous solution of aluminum phosphate having a concentration of P 2 O 5 / Al 2 O 3 of 2.2 to 2.8. It is a method for producing an aqueous solution.

【0012】本発明を更に詳しく説明する。本発明で
は、燐酸液と水酸化アルミニウム及び/又は酸化アルミ
ニウムを高濃度域で加熱反応させて、燐酸アルミニウム
濃度が60〜75重量%でP2O5/Al2O3モル比2.2〜
2.8の透明な燐酸アルミニウム水溶液を一旦生成させ
る。
The present invention will be described in more detail. In the present invention, the phosphoric acid solution and aluminum hydroxide and / or aluminum oxide are heated and reacted in a high concentration range to give an aluminum phosphate concentration of 60 to 75% by weight and a P 2 O 5 / Al 2 O 3 molar ratio of 2.2.
A transparent aluminum phosphate aqueous solution of 2.8 is once generated.

【0013】このとき燐酸液として、75重量%以上の
燐酸液を使用することが好適であり、通常市販の75
%、85%の燐酸液がそのまま使用できる。75重量%
より低いと、高濃度の燐酸アルミニウム水溶液を生成さ
せることが出来ない場合がある。また、水酸化アルミニ
ウム及び酸化アルミニウムは通常市販のものが使用でき
る。
At this time, it is preferable to use a phosphoric acid solution of 75% by weight or more as the phosphoric acid solution, which is usually commercially available.
%, 85% phosphoric acid solution can be used as it is. 75% by weight
If it is lower, it may not be possible to generate a high-concentration aluminum phosphate aqueous solution. Commercially available aluminum hydroxide and aluminum oxide can be used.

【0014】また、燐酸液と水酸化アルミニウム及び/
又は酸化アルミニウムとを反応させる際、水酸化アルミ
ニウム及び/又は酸化アルミニウムの燐酸液への添加方
法としては、燐酸液中に所定のP2O5/Al2O3モル比に必要
な量を一括して添加するという一般的な方法が利用でき
る。また反応熱による急激な温度上昇を防ぐため、操作
上有効な反応温度を保持可能な添加速度で、所定量を連
続的にあるいは分割して添加する方法も好ましい方法で
ある。
Further, phosphoric acid solution and aluminum hydroxide and /
Alternatively, when reacting with aluminum oxide, as a method of adding aluminum hydroxide and / or aluminum oxide to the phosphoric acid solution, an amount necessary for a predetermined P 2 O 5 / Al 2 O 3 molar ratio in the phosphoric acid solution is collectively included. Then, a general method of adding the compound can be used. Further, in order to prevent a rapid temperature rise due to the heat of reaction, a method of adding a predetermined amount continuously or in a divided manner at an addition rate capable of maintaining a reaction temperature effective in operation is also a preferable method.

【0015】本発明では燐酸アルミニウム濃度が60〜75
重量%の燐酸アルミニウム水溶液を一旦生成させる。本
発明でいう燐酸アルミニウム濃度とは、原料燐酸の全量
を第一燐酸アルミニウムとした場合の第一燐酸アルミニ
ウム濃度である。濃度が60重量%未満では、保存安定
性の優れた燐酸アルミニウム水溶液が得られず、また7
5重量%を越えると、反応液の粘度が高くなり撹拌操作
が不可能となるため好ましくない。
In the present invention, the aluminum phosphate concentration is 60 to 75
A weight percent aluminum phosphate aqueous solution is once generated. The aluminum phosphate concentration in the present invention is the aluminum phosphate monobasic concentration when the total amount of the raw material phosphoric acid is aluminum monophosphate. If the concentration is less than 60% by weight, an aluminum phosphate aqueous solution having excellent storage stability cannot be obtained.
If it exceeds 5% by weight, the viscosity of the reaction solution becomes high and the stirring operation becomes impossible, which is not preferable.

【0016】加熱反応させる際の温度は70〜120℃
が好ましく、特に好ましくは80〜90℃である。70
℃より低いと透明な燐酸アルミニウム水溶液が得られな
いことがあり、120℃より高いと反応液の沸点とな
り、操作が困難である。また、本発明の反応は反応熱が
生じるため、50℃程度まで加熱して反応を開始させ、
反応熱により70〜120℃まで上昇させ、反応を進行
させることも好ましい。
The temperature during the heating reaction is 70 to 120 ° C.
Is preferred, and particularly preferably 80 to 90 ° C. 70
If the temperature is lower than 0 ° C, a transparent aluminum phosphate aqueous solution may not be obtained, and if it is higher than 120 ° C, the boiling point of the reaction liquid is reached, which makes the operation difficult. Further, since the reaction of the present invention generates reaction heat, it is heated to about 50 ° C. to start the reaction,
It is also preferable to raise the temperature to 70 to 120 ° C. by the heat of reaction to allow the reaction to proceed.

【0017】本発明では燐酸アルミニウム濃度が60〜
75重量%という高濃度燐酸アルミニウム水溶液を製造
し、液が透明になった後、水を添加して濃度を調節す
る。この際、液が透明になった後、4時間以内に水を添
加するのが好ましい。濃度調整用の水の添加時間が4時
間を越えた場合、透明な燐酸アルミニウム水溶液が得ら
れない場合がある。
In the present invention, the aluminum phosphate concentration is 60 to
A high-concentration aluminum phosphate aqueous solution of 75% by weight is produced, and after the solution becomes transparent, water is added to adjust the concentration. At this time, it is preferable to add water within 4 hours after the liquid becomes transparent. If the addition time of the concentration adjusting water exceeds 4 hours, a transparent aluminum phosphate aqueous solution may not be obtained in some cases.

【0018】[0018]

【実施例】以下、実施例を挙げて本発明を具体的に説明
するが、本発明の要旨をそれらに限定するものではな
い。以下、%は重量%を意味する。
EXAMPLES The present invention will be specifically described below with reference to examples, but the scope of the present invention is not limited thereto. Hereinafter,% means% by weight.

【0019】実施例1 75%燐酸1378gを撹拌機およびコンデンサーを具
備した2lセパラブルフラスコに仕込み、水酸化アルミ
ニウム(水分8.54%含有)324gを添加し、外部
加熱装置により50℃まで加熱した。反応が開始し反応
熱により、温度は107℃まで上昇した。外部加熱装置
を外し冷却水により80℃まで冷却しこの温度を保持し
た。反応開始から60分後、内部反応液が透明になった
ことを確認し、80℃を保持したまま水549gを60
分間で添加した。冷却水により40℃まで冷却して製品
とした。
Example 1 1378 g of 75% phosphoric acid was placed in a 2 liter separable flask equipped with a stirrer and a condenser, 324 g of aluminum hydroxide (containing 8.54% of water content) was added, and the mixture was heated to 50 ° C. by an external heating device. . The temperature rose to 107 ° C. due to the heat of reaction when the reaction started. The external heating device was removed and the temperature was maintained by cooling to 80 ° C. with cooling water. After 60 minutes from the start of the reaction, it was confirmed that the internal reaction solution became transparent.
Added in minutes. The product was cooled to 40 ° C. with cooling water.

【0020】水添加前の燐酸アルミニウム濃度は、6
5.7%である。製品の分析値は、P2 5 33.27
%、Al2 3 8.61%、P2O5/Al2O3モル比=2.7
7であった。燐酸アルミニウム濃度は、50%である。
保管温度40℃において、87日間透明性を保持した。
The concentration of aluminum phosphate before adding water is 6
It is 5.7%. The analytical value of the product is P 2 O 5 33.27.
%, Al 2 O 3 8.61%, P 2 O 5 / Al 2 O 3 molar ratio = 2.7
It was 7. The aluminum phosphate concentration is 50%.
The transparency was maintained for 87 days at a storage temperature of 40 ° C.

【0021】実施例2 75%燐酸1378gと水酸化アルミニウム(水分8.
54%含有)342gを実施例1同様の反応機に仕込み
添加し、外部加熱装置により50℃まで加熱した。反応
が開始し反応熱により、温度は110℃まで上昇した。
実施例1同様の操作により80℃まで冷却しこの温度を
保持した。反応開始から90分後、内部反応液が透明に
なったことを確認し、80℃を保持したまま水531g
を60分間で添加した。冷却水により40℃まで冷却し
て製品とした。
Example 2 1378 g of 75% phosphoric acid and aluminum hydroxide (water content: 8.
342 g (containing 54%) was charged into the same reactor as in Example 1 and added, and heated to 50 ° C. by an external heating device. The temperature started to rise to 110 ° C due to the reaction heat and the reaction heat.
By the same operation as in Example 1, the temperature was cooled to 80 ° C. and this temperature was maintained. After 90 minutes from the start of the reaction, it was confirmed that the internal reaction solution became transparent, and 531 g of water was maintained while maintaining 80 ° C.
Was added over 60 minutes. The product was cooled to 40 ° C. with cooling water.

【0022】水添加前の燐酸アルミニウム濃度は、6
5.0%である。製品の分析値は、P2 5 33.26
%、Al2 3 9.08%、P2O5/Al2O3モル比=2.6
3であった。燐酸アルミニウム濃度は、50%である。
保管温度40℃において、85日間透明性を保持した。
The concentration of aluminum phosphate before addition of water is 6
It is 5.0%. The analytical value of the product is P 2 O 5 33.26.
%, Al 2 O 3 9.08%, P 2 O 5 / Al 2 O 3 molar ratio = 2.6
It was 3. The aluminum phosphate concentration is 50%.
The transparency was maintained for 85 days at a storage temperature of 40 ° C.

【0023】実施例3 75%燐酸1378gと水酸化アルミニウム(水分8.
54%含有)360gを実施例1同様の反応機に仕込み
添加し、外部加熱装置により50℃まで加熱した。反応
が開始し反応熱により、温度は112℃まで上昇した。
実施例1同様の操作により80℃まで冷却しこの温度を
保持した。反応開始から180分後、内部反応液が透明
になったことを確認し、80℃を保持したまま水513
gを60分間で添加した。冷却水により40℃まで冷却
して製品とした。
Example 3 1378 g of 75% phosphoric acid and aluminum hydroxide (water content: 8.
In the same reactor as in Example 1, 360 g (containing 54%) was added and heated to 50 ° C. by an external heating device. The reaction started and the temperature rose to 112 ° C due to the heat of reaction.
By the same operation as in Example 1, the temperature was cooled to 80 ° C. and this temperature was maintained. After 180 minutes from the start of the reaction, it was confirmed that the internal reaction solution became transparent, and water 513 was added while maintaining 80 ° C.
g was added in 60 minutes. The product was cooled to 40 ° C. with cooling water.

【0024】水添加前の燐酸アルミニウム濃度は、6
4.3%である。製品の分析値は、P2 5 33.24
%、Al2 3 9.56%、P2O5/Al2O3モル比=2.5
0であった。燐酸アルミニウム濃度は、50%である。
保管温度40℃において、78日間透明性を保持した。
The concentration of aluminum phosphate before addition of water is 6
It is 4.3%. The analytical value of the product is P 2 O 5 33.24.
%, Al 2 O 3 9.56%, P 2 O 5 / Al 2 O 3 molar ratio = 2.5
It was 0. The aluminum phosphate concentration is 50%.
The transparency was maintained for 78 days at a storage temperature of 40 ° C.

【0025】実施例4 75%燐酸1378gと水酸化アルミニウム(水分8.
54%含有)378gを実施例1同様の反応機に仕込み
添加し、外部加熱装置により50℃まで加熱した。反応
が開始し反応熱により、温度は112℃まで上昇した。
実施例1同様の操作により80℃まで冷却しこの温度を
保持した。反応開始から270分後、内部反応液が透明
になったことを確認し、80℃を保持したまま水495
gを60分間で添加した。冷却水により40℃まで冷却
して製品とした。
Example 4 1378 g of 75% phosphoric acid and aluminum hydroxide (water content: 8.
378 g (containing 54%) was charged into the same reactor as in Example 1 and added, and heated to 50 ° C. by an external heating device. The reaction started and the temperature rose to 112 ° C due to the heat of reaction.
By the same operation as in Example 1, the temperature was cooled to 80 ° C. and this temperature was maintained. After 270 minutes from the start of the reaction, it was confirmed that the internal reaction solution became transparent, and while maintaining the temperature at 80 ° C, water 495 was added.
g was added in 60 minutes. The product was cooled to 40 ° C. with cooling water.

【0026】水添加前の燐酸アルミニウム濃度は、6
3.7%である。製品の分析値は、P2 5 33.26
%、Al2 3 10.04%、P2O5/Al2O3モル比=2.
38であった。燐酸アルミニウム濃度は、50%であ
る。保管温度40℃において、70日間透明性を保持し
た。
The concentration of aluminum phosphate before addition of water is 6
It is 3.7%. The analytical value of the product is P 2 O 5 33.26.
%, Al 2 O 3 10.04%, P 2 O 5 / Al 2 O 3 molar ratio = 2.
It was 38. The aluminum phosphate concentration is 50%. The transparency was maintained for 70 days at a storage temperature of 40 ° C.

【0027】実施例5 75%燐酸1378gと水酸化アルミニウム(水分8.
54%含有)396gを実施例1同様の反応機に仕込み
添加し、外部加熱装置により50℃まで加熱した。反応
が開始し反応熱により、温度は112℃まで上昇した。
実施例1同様の操作により80℃まで冷却しこの温度を
保持した。反応開始から400分後、内部反応液が透明
になったことを確認し、80℃を保持したまま水477
gを60分間で添加した。冷却水により40℃まで冷却
して製品とした。
Example 5 1378 g of 75% phosphoric acid and aluminum hydroxide (water content: 8.
396 g (containing 54%) was charged into the same reactor as in Example 1 and added, and heated to 50 ° C. by an external heating device. The reaction started and the temperature rose to 112 ° C due to the heat of reaction.
By the same operation as in Example 1, the temperature was cooled to 80 ° C. and this temperature was maintained. After 400 minutes from the start of the reaction, it was confirmed that the internal reaction solution became transparent, and while maintaining the temperature at 80 ° C, water 477 was added.
g was added in 60 minutes. The product was cooled to 40 ° C. with cooling water.

【0028】水添加前の燐酸アルミニウム濃度は、6
3.0%である。製品の分析値は、P2 5 33.25
%、Al2 3 10.52%、P2O5/Al2O3モル比=2.
27であった。燐酸アルミニウム濃度は、50%であ
る。保管温度40℃において、70日間透明性を保持し
た。
The concentration of aluminum phosphate before addition of water is 6
It is 3.0%. The analytical value of the product is P 2 O 5 33.25.
%, Al 2 O 3 10.52%, P 2 O 5 / Al 2 O 3 molar ratio = 2.
It was 27. The aluminum phosphate concentration is 50%. The transparency was maintained for 70 days at a storage temperature of 40 ° C.

【0029】実施例6 85%燐酸1216gと水酸化アルミニウム(水分8.
54%含有)396gを実施例1同様の反応機に仕込み
添加し、外部加熱装置により50℃まで加熱した。反応
が開始し反応熱により、温度は110℃まで上昇した。
実施例1同様の操作により80℃まで冷却しこの温度を
保持した。反応開始から90分後、内部反応液が透明に
なったことを確認し、80℃を保持したまま水639g
を60分間で添加した。冷却水により40℃まで冷却し
て製品とした。
Example 6 1216 g of 85% phosphoric acid and aluminum hydroxide (water content: 8.
396 g (containing 54%) was charged into the same reactor as in Example 1 and added, and heated to 50 ° C. by an external heating device. The temperature started to rise to 110 ° C due to the reaction heat and the reaction heat.
By the same operation as in Example 1, the temperature was cooled to 80 ° C. and this temperature was maintained. After 90 minutes from the start of the reaction, it was confirmed that the internal reaction solution became transparent, and while keeping the temperature at 80 ° C, 639 g of water was added.
Was added over 60 minutes. The product was cooled to 40 ° C. with cooling water.

【0030】水添加前の燐酸アルミニウム濃度は、6
9.4%である。製品の分析値は、P2 5 33.25
%、Al2 3 10.52%、P2O5/Al2O3モル比=2.
27であった。燐酸アルミニウム濃度は、50%であ
る。保管温度40℃において、85日間透明性を保持し
た。
The concentration of aluminum phosphate before adding water is 6
It is 9.4%. The analytical value of the product is P 2 O 5 33.25.
%, Al 2 O 3 10.52%, P 2 O 5 / Al 2 O 3 molar ratio = 2.
It was 27. The aluminum phosphate concentration is 50%. The transparency was maintained for 85 days at a storage temperature of 40 ° C.

【0031】実施例7 75%燐酸1378gを撹拌機およびコンデンサーを具
備した2lセパラブルフラスコに仕込み、外部加熱装置
により50℃まで加熱した。水酸化アルミニウム(水分
8.54%含有)342gをテーブルフィーダーを用い
て連続的に添加した。反応が開始し反応熱により、温度
は80℃まで上昇した。この温度を保つように水酸化ア
ルミニウムの添加速度および外部加熱装置により調節し
た。水酸化アルミニウム添加後60分後、内部反応液が
透明になったことを確認し、80℃を保持したまま水5
30gを60分間で添加した。冷却水により40℃まで
冷却して製品とした。
Example 7 1378 g of 75% phosphoric acid was charged into a 2 liter separable flask equipped with a stirrer and a condenser, and heated to 50 ° C. by an external heating device. 342 g of aluminum hydroxide (containing 8.54% of water content) was continuously added using a table feeder. The temperature rose to 80 ° C. due to the heat of reaction when the reaction started. The addition rate of aluminum hydroxide and an external heating device were adjusted to maintain this temperature. After 60 minutes from the addition of aluminum hydroxide, it was confirmed that the internal reaction solution became transparent.
30 g was added in 60 minutes. The product was cooled to 40 ° C. with cooling water.

【0032】水添加前の燐酸アルミニウム濃度は、6
5.0%である。製品の分析値は、P2 5 33.26
%、Al2 3 9.08%、P2O5/Al2O3モル比=2.6
3であった。燐酸アルミニウム濃度は、50%である。
保管温度40℃において、80日間透明性を保持した。
The concentration of aluminum phosphate before adding water is 6
It is 5.0%. The analytical value of the product is P 2 O 5 33.26.
%, Al 2 O 3 9.08%, P 2 O 5 / Al 2 O 3 molar ratio = 2.6
It was 3. The aluminum phosphate concentration is 50%.
The transparency was maintained for 80 days at a storage temperature of 40 ° C.

【0033】実施例8 75%燐酸1378gを撹拌機およびコンデンサーを具
備した2lセパラブルフラスコに仕込み、外部加熱装置
により60℃まで加熱した。水酸化アルミニウム(水分
8.54%含有)396gを3分割し、このうち132
gを添加した。反応が開始し反応熱により、温度は80
℃まで上昇した。20分後、内部反応液が透明になった
ことを確認し、60℃まで冷却し、水酸化アルミニウム
132gを添加した。反応が開始し反応熱により、温度
は80℃まで上昇した。80分後、内部反応液が透明に
なったことを確認し、60℃まで冷却し、水酸化アルミ
ニウム132gを添加した。反応が開始し反応熱によ
り、温度は80℃まで上昇した。180分後、内部反応
液が透明になったことを確認し、80℃を保ち、水47
7gを60分間で添加した。冷却水により40℃まで冷
却して製品とした。
Example 8 1378 g of 75% phosphoric acid was charged into a 2 liter separable flask equipped with a stirrer and a condenser, and heated to 60 ° C. by an external heating device. 396 g of aluminum hydroxide (containing 8.54% water) was divided into 3 parts, of which 132
g was added. The reaction starts and the heat of reaction raises the temperature to 80
It rose to ℃. After 20 minutes, it was confirmed that the internal reaction solution became transparent, cooled to 60 ° C., and 132 g of aluminum hydroxide was added. The temperature rose to 80 ° C. due to the heat of reaction when the reaction started. After 80 minutes, it was confirmed that the internal reaction solution became transparent, cooled to 60 ° C., and 132 g of aluminum hydroxide was added. The temperature rose to 80 ° C. due to the heat of reaction when the reaction started. After 180 minutes, make sure that the internal reaction solution became transparent, and keep it at 80 ° C with water 47
7g was added in 60 minutes. The product was cooled to 40 ° C. with cooling water.

【0034】水添加前の燐酸アルミニウム濃度は、6
3.0%である。製品の分析値は、P2 5 33.25
%、Al2 3 10.52%、P2O5/Al2O3モル比=2.
27であった。燐酸アルミニウム濃度は、50%であ
る。保管温度40℃において、72日間透明性を保持し
た。
The concentration of aluminum phosphate before addition of water is 6
It is 3.0%. The analytical value of the product is P 2 O 5 33.25.
%, Al 2 O 3 10.52%, P 2 O 5 / Al 2 O 3 molar ratio = 2.
It was 27. The aluminum phosphate concentration is 50%. The transparency was maintained for 72 days at a storage temperature of 40 ° C.

【0035】実施例9 75%燐酸1378gと酸化アルミニウム216gを実
施例1同様の反応機に仕込み添加し、外部加熱装置によ
り90℃まで加熱した。反応が開始し反応熱により、温
度は112℃まで上昇した。実施例1同様の操作により
80℃まで冷却しこの温度を保持した。反応開始から1
80分後、内部反応液が透明になったことを確認し、8
0℃を保持したまま水513gを60分間で添加した。
冷却水により40℃まで冷却して製品とした。
Example 9 1378 g of 75% phosphoric acid and 216 g of aluminum oxide were charged in the same reactor as in Example 1 and heated to 90 ° C. by an external heating device. The reaction started and the temperature rose to 112 ° C due to the heat of reaction. By the same operation as in Example 1, the temperature was cooled to 80 ° C. and this temperature was maintained. 1 from the start of the reaction
After 80 minutes, confirm that the internal reaction solution became transparent.
513 g of water was added over 60 minutes while maintaining 0 ° C.
The product was cooled to 40 ° C. with cooling water.

【0036】水添加前の燐酸アルミニウム濃度は、7
0.1%である。製品の分析値は、P2 5 33.24
%、Al2 3 9.56%、P2O5/Al2O3モル比=2.5
0であった。燐酸アルミニウム濃度は、50%である。
保管温度40℃において、78日間透明性を保持した。
The concentration of aluminum phosphate before the addition of water is 7
It is 0.1%. The analytical value of the product is P 2 O 5 33.24.
%, Al 2 O 3 9.56%, P 2 O 5 / Al 2 O 3 molar ratio = 2.5
It was 0. The aluminum phosphate concentration is 50%.
The transparency was maintained for 78 days at a storage temperature of 40 ° C.

【0037】比較例1 75%燐酸1378g、水酸化アルミニウム(水分8.
54%含有)324gおよび水549gを撹拌機および
コンデンサーを具備した2lセパラブルフラスコに仕込
み、外部加熱装置により80℃まで加熱した。反応が開
始し反応熱により、一時温度は85℃まで上昇したが、
80℃まで低下した。この温度を保持した。反応開始か
ら60分後、内部反応液が透明になったことを確認し、
冷却水により40℃まで冷却して製品とした。
Comparative Example 1 1378 g of 75% phosphoric acid, aluminum hydroxide (water content 8.
54% content) (324 g) and water (549 g) were placed in a 2-liter separable flask equipped with a stirrer and a condenser, and heated to 80 ° C. by an external heating device. The reaction started and the heat of reaction raised the temperature up to 85 ° C.
The temperature dropped to 80 ° C. This temperature was maintained. After 60 minutes from the start of the reaction, confirm that the internal reaction solution became transparent,
The product was cooled to 40 ° C. with cooling water.

【0038】製品の分析値は、P2 5 33.27%、
Al2 3 8.61%、P2O5/Al2O3モル比=2.77で
あった。燐酸アルミニウム濃度は、50%である。保管
温度40℃において、透明性を保持したのは20日間と
短かった。
The analytical value of the product is P 2 O 5 33.27%,
Al 2 O 3 was 8.61% and P 2 O 5 / Al 2 O 3 molar ratio was 2.77. The aluminum phosphate concentration is 50%. At the storage temperature of 40 ° C., the transparency was maintained for as short as 20 days.

【0039】比較例2 75%燐酸1378g、水酸化アルミニウム(水分8.
54%含有)378gおよび水495gを実施例1同様
の反応機に仕込み添加し、外部加熱装置により80℃ま
で加熱した。反応が開始し反応熱により、一時温度は9
0℃まで上昇したが、80℃まで低下した。この温度を
保持した。反応開始から400分後経過しても、内部反
応液は透明にならず、透明な燐酸アルミニウム水溶液
は、得られなかった。この時のP2O5/Al2O3モル比=2.
38であった。
Comparative Example 2 1378 g of 75% phosphoric acid, aluminum hydroxide (water content 8.
54% content) (378 g) and water (495 g) were added to the same reactor as in Example 1 and heated to 80 ° C. by an external heating device. The reaction starts and the heat of reaction causes a temporary temperature of 9
It rose to 0 ° C but dropped to 80 ° C. This temperature was maintained. Even after 400 minutes from the start of the reaction, the internal reaction solution did not become transparent and a transparent aluminum phosphate aqueous solution was not obtained. P 2 O 5 / Al 2 O 3 molar ratio at this time = 2.
It was 38.

【0040】比較例3 75%燐酸1378g、酸化アルミニウム226gおよ
び水495gを実施例1同様の反応機に仕込み添加し、
外部加熱装置により80℃まで加熱した。反応が開始し
反応熱により、一時温度は90℃まで上昇したが、80
℃まで低下した。この温度を保持した。反応開始から4
00分後経過しても、内部反応液は透明にならず、透明
な燐酸アルミニウム水溶液は、得られなかった。この時
のP2O5/Al2O3モル比=2.38であった。
Comparative Example 3 1378 g of 75% phosphoric acid, 226 g of aluminum oxide and 495 g of water were charged in the same reactor as in Example 1 and added.
It heated up to 80 degreeC with the external heating apparatus. The reaction started and the heat of reaction raised the temperature up to 90 ° C,
It fell to ℃. This temperature was maintained. 4 from the start of the reaction
The internal reaction solution did not become transparent even after 00 minutes, and a transparent aqueous solution of aluminum phosphate was not obtained. At this time, the P 2 O 5 / Al 2 O 3 molar ratio was 2.38.

【0041】[0041]

【発明の効果】本発明によれば、一旦、高濃度燐酸アル
ミニウム水溶液を製造するという簡単な方法で、従来製
造することが困難であった保存安定性の良好なP2O5/Al2
O3モル比2.2〜2.8の燐酸アルミニウム水溶液を安
定的に製造できる。従って、アルミニウム濃度が高い燐
酸アルミニウム水溶液の利用分野に対する貢献は大き
く、極めて有用な発明である。
EFFECTS OF THE INVENTION According to the present invention, P 2 O 5 / Al 2 having good storage stability, which has been difficult to produce by a simple method of once producing a high-concentration aluminum phosphate aqueous solution, has been obtained.
An aluminum phosphate aqueous solution having an O 3 molar ratio of 2.2 to 2.8 can be stably produced. Therefore, the invention greatly contributes to the field of use of the aluminum phosphate aqueous solution having a high aluminum concentration and is a very useful invention.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 松原 修 山口県下関市彦島迫町七丁目1番1号 三 井東圧化学株式会社内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Osamu Matsubara 7-1, 1-1 Hikoshimasako-cho, Shimonoseki-shi, Yamaguchi Prefecture Mitsui Toatsu Chemical Co., Ltd.

Claims (4)

【特許請求の範囲】[Claims] 【請求項1】 燐酸液と水酸化アルミニウム及び/又は
酸化アルミニウムとを加熱反応させて、燐酸アルミニウ
ム濃度が60〜75重量%でP2O5/Al2O3モル比2.2〜
2.8の透明な燐酸アルミニウム水溶液を生成させ、そ
の後水を添加して濃度調節を行うことを特徴とするP2O5
/Al2O3モル比2.2〜2.8の燐酸アルミニウム水溶液
の製造方法。
1. A phosphoric acid solution and an aluminum hydroxide and / or aluminum oxide are heated and reacted to give an aluminum phosphate concentration of 60 to 75% by weight and a P 2 O 5 / Al 2 O 3 molar ratio of 2.2.
P 2 O 5 characterized by producing a transparent aluminum phosphate aqueous solution of 2.8, and then adding water to adjust the concentration.
/ Al 2 O 3 A method for producing an aluminum phosphate aqueous solution having a molar ratio of 2.2 to 2.8.
【請求項2】 上記水の添加を、透明な燐酸アルミニウ
ム水溶液が生成した後4 時間以内に行う請求項1記載の
方法。
2. The method according to claim 1, wherein the addition of water is performed within 4 hours after the formation of the transparent aluminum phosphate aqueous solution.
【請求項3】 燐酸液と水酸化アルミニウム及び/又は
酸化アルミニウムとを反応させる際、燐酸液に水酸化ア
ルミニウム及び/又は酸化アルミニウムを一括して添加
する請求項1記載の方法。
3. The method according to claim 1, wherein when the phosphoric acid solution is reacted with aluminum hydroxide and / or aluminum oxide, aluminum hydroxide and / or aluminum oxide is added all at once to the phosphoric acid solution.
【請求項4】 燐酸液と水酸化アルミニウム及び/又は
酸化アルミニウムとを反応させる際、燐酸液に水酸化ア
ルミニウム及び/又は酸化アルミニウムを連続してまた
は分割して添加する請求項1記載の方法。
4. The method according to claim 1, wherein when the phosphoric acid solution is reacted with aluminum hydroxide and / or aluminum oxide, aluminum hydroxide and / or aluminum oxide is continuously or dividedly added to the phosphoric acid solution.
JP6090898A 1994-04-28 1994-04-28 Production of aqueous solution of aluminum phosphate Pending JPH07291609A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP6090898A JPH07291609A (en) 1994-04-28 1994-04-28 Production of aqueous solution of aluminum phosphate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP6090898A JPH07291609A (en) 1994-04-28 1994-04-28 Production of aqueous solution of aluminum phosphate

Publications (1)

Publication Number Publication Date
JPH07291609A true JPH07291609A (en) 1995-11-07

Family

ID=14011229

Family Applications (1)

Application Number Title Priority Date Filing Date
JP6090898A Pending JPH07291609A (en) 1994-04-28 1994-04-28 Production of aqueous solution of aluminum phosphate

Country Status (1)

Country Link
JP (1) JPH07291609A (en)

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* Cited by examiner, † Cited by third party
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WO2008072375A1 (en) * 2006-12-13 2008-06-19 Taki Chemical Co., Ltd. Temperature-sensitive aluminum phosphate solution, method for production thereof, and use thereof
JP2010089003A (en) * 2008-10-07 2010-04-22 Ryoko Lime Industry Co Ltd Method of manufacturing heavy metal stabilization composition
JP2011511867A (en) * 2008-02-12 2011-04-14 ブンゲ フェルチルザンテス エス.エー. Aluminum phosphate slurry
CN104603211A (en) * 2012-04-16 2015-05-06 柏格阿莫菲克索录森斯有限公司 Aluminum phosphates, compositions comprising aluminum phosphate, and methods for making the same
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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008072375A1 (en) * 2006-12-13 2008-06-19 Taki Chemical Co., Ltd. Temperature-sensitive aluminum phosphate solution, method for production thereof, and use thereof
JPWO2008072375A1 (en) * 2006-12-13 2010-03-25 多木化学株式会社 Temperature-sensitive aluminum phosphate solution, production method thereof and use thereof
US8025725B2 (en) 2006-12-13 2011-09-27 Taki Chemical Co., Ltd. Temperature-sensitive aluminum phosphate solution, a process for producing the same and the use thereof
JP2011511867A (en) * 2008-02-12 2011-04-14 ブンゲ フェルチルザンテス エス.エー. Aluminum phosphate slurry
JP2015091958A (en) * 2008-02-12 2015-05-14 ブンゲ フェルチリザンテス エス.エー. Aluminum phosphate slurry
JP2010089003A (en) * 2008-10-07 2010-04-22 Ryoko Lime Industry Co Ltd Method of manufacturing heavy metal stabilization composition
JP4573893B2 (en) * 2008-10-07 2010-11-04 菱光石灰工業株式会社 Method for producing heavy metal stabilizing composition
CN104603211A (en) * 2012-04-16 2015-05-06 柏格阿莫菲克索录森斯有限公司 Aluminum phosphates, compositions comprising aluminum phosphate, and methods for making the same
CN104603211B (en) * 2012-04-16 2017-11-14 柏格阿莫菲克索录森斯有限公司 Aluminum phosphate, phosphoric acid aluminium composition and preparation method thereof
CN116693271A (en) * 2023-04-27 2023-09-05 中国民航大学 Preparation method of special silicon-boron-carbon-zirconium modified aluminum zirconium phosphate high-temperature adhesive for zirconia ceramics
CN116693271B (en) * 2023-04-27 2024-03-19 中国民航大学 Preparation method of special silicon-boron-carbon-zirconium modified aluminum zirconium phosphate high-temperature adhesive for zirconia ceramics

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