JPH07291609A - Production of aqueous solution of aluminum phosphate - Google Patents
Production of aqueous solution of aluminum phosphateInfo
- 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.)
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- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
Description
【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 Ｏ5 ３３．２７
％、Ａｌ2 Ｏ3 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 Ｏ5 ３３．２６
％、Ａｌ2 Ｏ3 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 Ｏ5 ３３．２４
％、Ａｌ2 Ｏ3 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 Ｏ5 ３３．２６
％、Ａｌ2 Ｏ3 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 Ｏ5 ３３．２５
％、Ａｌ2 Ｏ3 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 Ｏ5 ３３．２５
％、Ａｌ2 Ｏ3 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 Ｏ5 ３３．２６
％、Ａｌ2 Ｏ3 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 Ｏ5 ３３．２５
％、Ａｌ2 Ｏ3 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 Ｏ5 ３３．２４
％、Ａｌ2 Ｏ3 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 Ｏ5 ３３．２７％、
Ａｌ2 Ｏ3 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)
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.
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.
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.
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.
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) |
Cited By (5)
| 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 |
| 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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1994
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| 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 |
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| 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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