JPH0710535A - Production of alumina sol excellent in transparency and having satisfactory viscosity stability - Google Patents
Production of alumina sol excellent in transparency and having satisfactory viscosity stabilityInfo
- Publication number
- JPH0710535A JPH0710535A JP18184293A JP18184293A JPH0710535A JP H0710535 A JPH0710535 A JP H0710535A JP 18184293 A JP18184293 A JP 18184293A JP 18184293 A JP18184293 A JP 18184293A JP H0710535 A JPH0710535 A JP H0710535A
- Authority
- JP
- Japan
- Prior art keywords
- alumina sol
- acid
- alumina
- transparency
- amount
- 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)
- Colloid Chemistry (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は特に透明性の優れた、粘
度安定性の良いアルミナゾル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 alumina sol having excellent transparency and excellent viscosity stability.
【０００２】[0002]
【従来の技術】アルミナゾルは製紙工業や繊維工業の表
面処理剤、各種耐火物のバインダー、触媒担体、プラス
チック工業等に用いられており、特に最近ではニューセ
ラミックスの原料、各種フィルムの表面改質剤として急
速にその需要が高まってきている。2. Description of the Related Art Alumina sol is used as a surface treatment agent in the paper and textile industries, a binder for various refractories, a catalyst carrier, a plastics industry and the like. In particular, recently, a raw material for new ceramics and a surface modifier for various films. As demand for it is increasing rapidly.
【０００３】アルミニウムアルコキシドを原料として透
明なアルミナゾルを製造する例は、すでに下記の文献が
知られている。 米国特許第2,656,321号公報（1963） Bulent E.Yolds,Am.Ceramic Soc.Bull.,54,289（19
75） 日特開昭５７−８８０７４号公報The following documents have already been known as examples of producing a transparent alumina sol using aluminum alkoxide as a raw material. U.S. Patent No. 2,656,321 (1963) Bulent E. Yolds, Am. Ceramic Soc. Bull., 54,289 (19
75) JP-A-57-88074
【０００４】しかし、これらの文献に記載された技術で
製造したアルミナゾルは透明性において必ずしも満足な
結果を与えるものではなく、かつ反応所要時間も長くか
かる欠点を有している。また、100 ℃以下の温度で解膠
するため、酸の使用量が多くなり、10％以上の濃度では
粘度安定性が悪いといった欠点もある。However, the alumina sols produced by the techniques described in these documents have the disadvantages that they do not always give satisfactory results in terms of transparency and that the reaction time is long. Further, since the peptization occurs at a temperature of 100 ° C. or lower, the amount of acid used increases, and at a concentration of 10% or higher, the viscosity stability is poor.
【０００５】また、日特開昭５９−７８９２５号公報に
記載されているアルミナゾルは、粒子の大きさが直径10
nm，長さ200nm 以下の針状結晶であり、かなり大きな粒
子を含んでいる。しかも、製造方法はアルミニウム粉末
を原料としており、解膠の際添加する酸の使用量が多
く、低濃度で反応時間も長いといった上記と同様な欠点
を有している。また、日特開昭６２−５６３２１号公報
に記載されているアルミナゾルは、透明性に優れている
が、これも解膠の際添加する酸の使用量が多いため粘度
安定性に欠けており長期保存ができず、高濃度にすると
ゲル化する欠点がある。The alumina sol described in JP-A-59-78925 has a particle size of 10 mm in diameter.
It is a needle-shaped crystal with a size of nm and a length of 200 nm or less, and contains fairly large particles. Moreover, the manufacturing method uses aluminum powder as a raw material, and has the same drawbacks as the above, such as a large amount of acid added during peptization, a low concentration, and a long reaction time. Further, the alumina sol described in JP-A-62-56321 has excellent transparency, but this also lacks viscosity stability due to the large amount of acid added during deflocculation, which results in long-term It has the drawback that it cannot be stored and gels at high concentrations.
【０００６】[0006]
【発明が解決しようとする課題】本発明は、特に透明性
に優れかつ粘度安定性の良いアルミナゾルの製造方法を
提供するものである。具体的には、アルミナを10〜25wt
％含有する高濃度アルミナゾルにおいて３ヶ月以上安定
に粘度100cps以下の水媒体として保存可能であり、かつ
アルミナを10％含有するアルミナゾルに調製した場合に
おいて、540nm の光の透過率が70％以上であるアルミナ
ゾルを工業的に有利に製造する方法に関するものであ
る。DISCLOSURE OF THE INVENTION The present invention provides a method for producing an alumina sol which is particularly excellent in transparency and viscosity stability. Specifically, 10-25 wt% alumina
% High-concentration alumina sol can be stably stored as an aqueous medium with a viscosity of 100 cps or less for 3 months or more, and when prepared in an alumina sol containing 10% alumina, the transmittance of light at 540 nm is 70% or more. The present invention relates to a method for industrially producing alumina sol.
【０００７】[0007]
【課題を解決するための手段】本発明者らは、アルミニ
ウムアルコキシドを加水分解してアルミナ１水和物（ベ
ーマイト）を製造する際の反応条件、及び酸を加えて解
膠する際の反応条件について鋭意研究の結果、特に透明
性に優れしかも粘度安定性の良いアルミナゾルを比較的
短時間に製造する方法を見いだした。Means for Solving the Problems The present inventors have proposed reaction conditions for producing aluminum monohydrate (boehmite) by hydrolyzing aluminum alkoxide, and reaction conditions for peptizing by adding an acid. As a result of earnest research on the above, a method for producing an alumina sol having excellent transparency and good viscosity stability was found in a relatively short time.
【０００８】即ち本発明は、アルミニウムアルコキシド
を希酸水溶液中で加水分解してアルミナ１水和物（ベー
マイト）とし、その際生成したアルコールを留去した
後、酸を加えて高温、加圧下解膠する事を特徴とする透
明性の優れた粘度安定性の良いアルミナゾルの製造方法
である。本発明で使用されるアルミニウムアルコキシド
は一般式 Ａｌ（ＯＲ1）（ＯＲ2）（ＯＲ3） で示されるものであり、式中のＲ1，Ｒ2，Ｒ3は炭素数
２から５までのアルキル基を表すが、好ましくは炭素数
３のアルミニウムイソプロポキサイドないし炭素数４の
アルミニウムイソブトキサイドが良い。また、これらの
アルミニウムアルコキシドの性状は、液体よりも粉末な
いし顆粒状が好ましく、純度は99％以上が望ましい。That is, according to the present invention, aluminum alkoxide is hydrolyzed in a dilute aqueous acid solution to form alumina monohydrate (boehmite), and the alcohol produced at that time is distilled off. It is a method for producing an alumina sol having excellent transparency and excellent transparency, which is characterized by sticking. The aluminum alkoxide used in the present invention is represented by the general formula Al (OR 1 ) (OR 2 ) (OR 3 ), and R 1 , R 2 and R 3 in the formula have 2 to 5 carbon atoms. It represents an alkyl group, but is preferably aluminum isopropoxide having 3 carbon atoms or aluminum isobutoxide having 4 carbon atoms. The properties of these aluminum alkoxides are preferably powdery or granular rather than liquid, and the purity is preferably 99% or more.
【０００９】加水分解に使用する酸としては、塩酸、硝
酸、過塩素酸、酢酸、プロピオン酸等の一価の酸なら鉱
酸でも有機酸でもよく、解膠時に加える酸についても同
様である。酸の使用量については、加水分解時及び解膠
時ともに使用する酸の種類によって異なり、ある特定の
範囲においてはじめて透明性の優れた粘度安定性の良い
アルミナゾルが得られる。即ち、加水分解前のpHが2.0
〜3.0 の範囲で酸の種類により適した量を加えて加水分
解する。また、解膠時に加える酸の量は、（酸根／Al）
のモル比が0.005 〜0.1 、好ましくは0.01〜0.05の範囲
で酸の種類によって反応が数時間以内に行なわれ、期待
される透明性が得られる最低量とする。この酸の量は、
得られるアルミナゾルの粘度安定性と密接な関係があ
り、多すぎると粘度安定性が悪く経時的に増粘しゲル化
したり、15％以上の高濃度品を製造する際には反応中に
ゲル化したりして製造不能となる。また、少なすぎると
解膠速度が遅く反応に長時間を必要とし期待される透明
性を得る事ができない。The acid used for hydrolysis may be a mineral acid or an organic acid as long as it is a monovalent acid such as hydrochloric acid, nitric acid, perchloric acid, acetic acid or propionic acid, and the same applies to the acid added at the time of peptization. The amount of acid used varies depending on the type of acid used both during hydrolysis and peptization, and an alumina sol having excellent transparency and excellent viscosity stability can be obtained only in a specific range. That is, the pH before hydrolysis is 2.0
Hydrolyze by adding an amount suitable for the type of acid within the range of to 3.0. The amount of acid added during peptization is (acid radical / Al)
With a molar ratio of 0.005 to 0.1, preferably 0.01 to 0.05, the reaction is carried out within a few hours depending on the kind of acid, and the minimum amount is that at which the expected transparency can be obtained. The amount of this acid is
It has a close relationship with the viscosity stability of the obtained alumina sol. If it is too large, the viscosity stability is poor and the viscosity increases over time, causing gelation, or when producing a high-concentration product of 15% or more, gelation occurs during the reaction. It becomes impossible to manufacture. On the other hand, if the amount is too small, the peptization rate is slow and it takes a long time for the reaction, and the expected transparency cannot be obtained.
【００１０】従来の方法では、アルミニウムアルコキサ
イドを原料としてアルミナゾルを製造する場合、100 ℃
以下の温度で解膠していたため、必然的に酸の使用量が
多くなり、粘度安定性が悪く高濃度品を製造することが
できなかった。我々はこの問題を解決する為に鋭意検討
した結果、上記原因を解明するとともに、圧力反応装置
を使用して解膠温度が100 ℃〜300 ℃、好ましくは120
〜170 ℃で解膠を行なう事によって、適度な酸の使用量
で短時間に解膠し満足な透明性及び粘度安定性を得る事
に成功した。According to the conventional method, when an alumina sol is produced from aluminum alkoxide as a raw material, 100 ° C.
Since the peptization was carried out at the temperature below, the amount of acid used was inevitably increased, and the viscosity stability was poor and a high concentration product could not be manufactured. As a result of intensive studies to solve this problem, we have elucidated the above-mentioned cause and, using a pressure reactor, have a peptization temperature of 100 ° C to 300 ° C, preferably 120 ° C.
By deflocculating at ˜170 ° C., deflocculation was achieved in a short time with a proper amount of acid, and satisfactory transparency and viscosity stability were successfully obtained.
【００１１】次に本発明の一実施態様を示す。イオン交
換水に60％硝酸を加えてpHを2.2 〜2.5 に調整する。こ
れを加温してから製造したいアルミナゾルの濃度を考慮
して必要量のアルミニウムアルコキシドの粉末を攪拌し
ながら徐々に投入し、加水分解する。投入終了後95℃前
後まで加熱して副生するアルコールを除去した後、加圧
反応装置に移しアルミニウムアルコキシド１モルあたり
0.02〜0.03モルの硝酸を３倍に希釈した水溶液を滴下
し、液温を140 〜160 ℃に保って良く攪拌しながら解膠
させる。４〜８時間この状態を保持して透過率が十分な
透明度になったら50℃以下に急冷して透明なアルミナゾ
ル溶液を得る。Next, one embodiment of the present invention will be described. Adjust the pH to 2.2-2.5 by adding 60% nitric acid to ion-exchanged water. After heating this, in consideration of the concentration of the alumina sol to be produced, a necessary amount of the powder of aluminum alkoxide is gradually added while stirring and hydrolyzed. After the addition is complete, the product is heated to around 95 ° C to remove the by-produced alcohol, and then transferred to a pressure reactor, where 1 mol of aluminum alkoxide
An aqueous solution prepared by diluting 0.02 to 0.03 mol of nitric acid 3 times is added dropwise, and the liquid temperature is kept at 140 to 160 ° C. to deflocculate while stirring well. While maintaining this state for 4 to 8 hours, when the transmittance reaches a sufficient transparency, it is rapidly cooled to 50 ° C. or lower to obtain a transparent alumina sol solution.
【００１２】この実施態様に準じて製造したアルミナゾ
ルはアルミナ濃度を10％に調整して測定した540nm の波
長光の透過率が85％以上の値を示した。また、この溶液
を20％濃度に濃縮したアルミナゾルでも３ヶ月以上安定
に粘度50cps 以下の水溶液として保存可能であった。ま
た電子顕微鏡写真によれば、アルミナの粒径は１〜10nm
と非常に小さい事が分かった。また、本発明のアルミゾ
ル溶液をテフロン製容器に流し込みゆっくり乾燥させる
と、製膜性が良く透明度の高い薄膜が得られた。The alumina sol produced according to this embodiment had a transmittance of 85% or more for light having a wavelength of 540 nm measured by adjusting the alumina concentration to 10%. Further, even an alumina sol obtained by concentrating this solution to a concentration of 20% could be stably stored as an aqueous solution having a viscosity of 50 cps or less for 3 months or more. According to the electron micrograph, the particle size of alumina is 1 to 10 nm.
It turned out to be very small. Further, when the aluminum sol solution of the present invention was poured into a Teflon container and slowly dried, a thin film having good film forming property and high transparency was obtained.
【００１３】[0013]
【作用】本発明の方法で、酸の使用量を調節する事によ
り粘度安定性を高めかつ透明性の優れたアルミナゾルを
得ることができたが、その理由は不明である。According to the method of the present invention, an alumina sol having improved viscosity stability and excellent transparency can be obtained by controlling the amount of acid used, but the reason is unknown.
【００１４】以下実施例によって本発明を更に詳しく説
明する。The present invention will be described in more detail with reference to the following examples.
【実施例】実施例−１ イオン交換水300gをビーカに取り、硝酸を加えてpH2.30
に調整した。この液を500ml オートクレーブに移し、攪
拌しながら液温を75℃に上昇させた。次にアルミニウム
イソプロポキシド60g を投入し、液温を徐々に95℃付近
まで昇温させて発生するイソプロピルアルコール（含
水）を留出させた。留出量は82g であった。その後61％
硝酸を0.91g （アルミニウムイソプロポキシドに対して
モル比0.03）を３倍量のイオン交換水で希釈してから滴
下した。続いて、反応容器を密閉にし、攪拌しながら14
5 〜150 ℃に昇温し解膠を行なった。反応は分光光度計
を用いて透過率を適宜測定し、透過率が92.1％になった
時点で液温を50℃以下に急冷し反応を終了した。この間
に要した反応時間は４時間であり、最高圧力は3.8kg/cm
2 であった。得られたアルミナゾルのアルミナ濃度は５
wt％であり、この溶液を20wt％まで減圧下濃縮した時の
波長540nm での透過率は62.5％であった。また、このア
ルミナ濃度20wt％溶液の粘度を測定したところ、製造直
後の32cps から３ヶ月経過した後でも46cps と殆ど増粘
していなかった。[Examples] Example-1 300 g of ion-exchanged water was placed in a beaker, and nitric acid was added to adjust the pH to 2.30.
Adjusted to. This liquid was transferred to a 500 ml autoclave, and the liquid temperature was raised to 75 ° C while stirring. Next, 60 g of aluminum isopropoxide was added, and the liquid temperature was gradually raised to around 95 ° C. to distill isopropyl alcohol (containing water) generated. The amount of distillate was 82 g. 61% thereafter
0.91 g of nitric acid (molar ratio 0.03 with respect to aluminum isopropoxide) was diluted with 3 times the amount of ion-exchanged water and then added dropwise. Then, seal the reaction vessel and
The temperature was raised to 5 to 150 ° C to perform peptization. For the reaction, the transmittance was appropriately measured using a spectrophotometer, and when the transmittance reached 92.1%, the liquid temperature was rapidly cooled to 50 ° C or lower to terminate the reaction. The reaction time required during this period was 4 hours, and the maximum pressure was 3.8 kg / cm.
Was 2 . The alumina concentration of the obtained alumina sol was 5
When this solution was concentrated to 20 wt% under reduced pressure, the transmittance at a wavelength of 540 nm was 62.5%. Further, the viscosity of this 20 wt% alumina solution was measured, and it was found that the viscosity was 46 cps, which was hardly increased even after 3 months passed from 32 cps immediately after the production.
【００１５】実施例−２ イオン交換水100kg を圧力反応釜に仕込み、硝酸を加え
てpH2.35に調整した後、攪拌しながら液温を75℃に上昇
させた。次にアルミニウムイソプロポキシド40kgを投入
し、液温を徐々に95℃付近まで昇温させて発生するイソ
プロピルアルコール（含水）を常圧下留出させた。留出
量は53kgであった。その後61％硝酸を0.5 kg（アルミニ
ウムイソプロポキシドに対してモル比0.025 ）を３倍量
のイオン交換水で希釈してから滴下した。続いて、反応
容器を密閉にし、攪拌しながら145 〜155 〜160 ℃に昇
温し解膠を行なった。反応は分光光度計を用いて透過率
を適宜測定し、透過率が78.6％になった時点で液温を50
℃以下に急冷し反応を終了した。この間に要した反応時
間は６時間であり、最高圧力は4.6 kg／cm2であった。
得られたアルミナゾルのアルミナ濃度は10wt％であり、
この溶液を20wt％まで減圧下濃縮した時の波長540nm で
の透過率は58.3％であった。また、このアルミナ濃度20
wt％溶液の粘度を測定したところ、製造直後の23cps か
ら３ヶ月経過した後でも42cps と殆ど増粘していなかっ
た。Example 2 100 kg of ion-exchanged water was charged into a pressure reaction vessel, nitric acid was added to adjust the pH to 2.35, and then the liquid temperature was raised to 75 ° C. with stirring. Next, 40 kg of aluminum isopropoxide was added, the liquid temperature was gradually raised to around 95 ° C., and isopropyl alcohol (containing water) generated was distilled off under normal pressure. The amount of distillate was 53 kg. Thereafter, 0.5 kg of 61% nitric acid (molar ratio 0.025 with respect to aluminum isopropoxide) was diluted with 3 times amount of ion-exchanged water and then added dropwise. Then, the reaction vessel was hermetically closed, and the temperature was raised to 145-155-160 ° C. with stirring to peptize. For the reaction, the transmittance was appropriately measured using a spectrophotometer, and when the transmittance reached 78.6%, the liquid temperature was adjusted to 50%.
The reaction was terminated by rapidly cooling to below ℃. The reaction time required during this period was 6 hours, and the maximum pressure was 4.6 kg / cm 2 .
The alumina concentration of the obtained alumina sol was 10 wt%,
When this solution was concentrated to 20 wt% under reduced pressure, the transmittance at a wavelength of 540 nm was 58.3%. Also, this alumina concentration 20
When the viscosity of the wt% solution was measured, it was found that 23 cps immediately after production and 42 cps had not been increased even after 3 months.
【００１６】実施例−３〜１０ イオン交換水600gをビーカに取り、硝酸を加えてpH2.30
に調整した。この液を800ml オートクレーブに移し、攪
拌しながら液温を75℃に上昇させた。次にアルミニウム
イソプロポキシド240gを投入し、液温を徐々に95℃付近
まで昇温させて発生するイソプロピルアルコール（含
水）を留出させた。留出量は297gであった。その後、所
定量の61％硝酸を３倍量のイオン交換水で希釈してから
滴下した。続いて、反応容器を密閉にし、攪拌しながら
所定の温度まで昇温し所定時間その温度を維持して解こ
うを行なった後、50℃以下に急冷し反応を終了した。こ
の時得られたアルミナゾルのアルミナ濃度は10wt％であ
り、分光光度計を用いて測定したこの溶液の透過率を表
−１に示す。Examples 3 to 10 600 g of ion-exchanged water was placed in a beaker and nitric acid was added to the beaker to adjust the pH to 2.30.
Adjusted to. This liquid was transferred to an 800 ml autoclave, and the liquid temperature was raised to 75 ° C while stirring. Next, 240 g of aluminum isopropoxide was added and the liquid temperature was gradually raised to around 95 ° C. to distill isopropyl alcohol (containing water) generated. The amount of distillate was 297 g. Then, a predetermined amount of 61% nitric acid was diluted with 3 times the amount of ion-exchanged water and then added dropwise. Then, the reaction vessel was hermetically closed, the temperature was raised to a predetermined temperature with stirring, the temperature was maintained for a predetermined time for thawing, and then the reaction was terminated by rapidly cooling to 50 ° C. or lower. The alumina concentration of the alumina sol obtained at this time was 10 wt%, and the transmittance of this solution measured using a spectrophotometer is shown in Table 1.
【００１７】 ＊解膠圧力 150℃ 4.8kg/cm2 ，165℃ 6.8kg/cm2 [0017] * Peptizing pressure 150 ℃ 4.8kg / cm 2 , 165 ℃ 6.8kg / cm 2
【００１８】実施例−１１ イオン交換水600gをビーカに取り、硝酸を加えてpH2.30
に調整した。この液を1000mlオートクレーブに移し、攪
拌しながら液温を75℃に上昇させた。次にアルミニウム
イソプロポキシド120gを投入し、液温を徐々に95℃付近
まで昇温させて発生するイソプロピルアルコール（含
水）を留出させた。留出量は327gであった。その後氷酢
酸2.97g （アルミニウムイソプロポキシドに対してモル
比0.084 ）を３倍量のイオン交換水で希釈してから滴下
した。続いて、反応容器を密閉にし、攪拌しながら150
℃に昇温し解膠を行なった。反応は分光光度計を用いて
透過率を適宜測定し、透過率が79.1％になった時点で液
温を50℃以下に急冷し、反応を終了した。この間に要し
た反応時間は2.5 時間であり、最高圧力は4.8 kg／cm2
であった。得られたアルミナゾルのアルミナ濃度は５wt
％であり、この溶液の粘度を測定したところ6cps（25
℃）であった。Example 11 600 g of ion-exchanged water was placed in a beaker, nitric acid was added to the beaker to adjust the pH to 2.30.
Adjusted to. This liquid was transferred to a 1000 ml autoclave, and the liquid temperature was raised to 75 ° C while stirring. Next, 120 g of aluminum isopropoxide was added, and the liquid temperature was gradually raised to around 95 ° C. to distill the generated isopropyl alcohol (containing water). The amount of distillate was 327 g. Thereafter, 2.97 g of glacial acetic acid (molar ratio 0.084 with respect to aluminum isopropoxide) was diluted with 3 times the amount of ion-exchanged water and then added dropwise. Then, seal the reaction vessel and stir 150
The temperature was raised to ℃ and the peptization was performed. For the reaction, the transmittance was appropriately measured using a spectrophotometer, and when the transmittance reached 79.1%, the liquid temperature was rapidly cooled to 50 ° C. or lower to terminate the reaction. The reaction time required during this period was 2.5 hours, and the maximum pressure was 4.8 kg / cm 2
Met. The alumina concentration of the obtained alumina sol was 5 wt.
%, And the viscosity of this solution was measured to be 6 cps (25
℃).
【００１９】比較例−１〜２ １ ４つ口フラスコにイオン交換水600gを仕込み、99％
酢酸を加えてpH2.30に調整した。その後、攪拌しながら
液温を75℃に上昇させた。次にアルミニウムイソプロポ
キシドを所定量投入し、液温を徐々に95℃付近まで昇温
せて発生するイソプロピルアルコール（含水）を留出さ
せた。その後、所定量の61％硝酸を３倍量のイオン交換
水で希釈してから滴下した。液温は92〜95℃に保ち常圧
で８時間攪拌した。分光光度計を用いて透過率を適宜測
定し、透過率がほぼ最高値になったところで液温を50℃
以下に急冷し攪拌をとめた。 この溶液を20wt％まで減圧下濃縮しようと試みたが、何
れも12〜13％まで濃縮したところでゲル化してしまっ
た。また、比較例２のアルミナ濃度10％品でも３ヵ月保
存しておいたところゲル化してしまった。Comparative Examples-1 to 2 1 600 g of ion-exchanged water was charged into a four-necked flask, and 99%
The pH was adjusted to 2.30 by adding acetic acid. Then, the liquid temperature was raised to 75 ° C. while stirring. Next, a predetermined amount of aluminum isopropoxide was added, the liquid temperature was gradually raised to around 95 ° C., and isopropyl alcohol (containing water) generated was distilled off. Then, a predetermined amount of 61% nitric acid was diluted with 3 times the amount of ion-exchanged water and then added dropwise. The liquid temperature was maintained at 92 to 95 ° C. and the mixture was stirred at normal pressure for 8 hours. Measure the transmittance appropriately with a spectrophotometer, and when the transmittance reaches the maximum value, raise the liquid temperature to 50 ° C.
It was rapidly cooled to the following and stirring was stopped. Attempts were made to concentrate this solution to 20 wt% under reduced pressure, but all gelled when concentrated to 12 to 13%. Further, even the product having a 10% alumina concentration of Comparative Example 2 gelled when stored for 3 months.
【００２０】[0020]
【発明の効果】本発明の方法で、酸の使用量を調節する
事により粘度安定性を高め、かつ透明性の優れたアルミ
ナゾルを得ることができた。INDUSTRIAL APPLICABILITY According to the method of the present invention, it was possible to obtain an alumina sol having improved viscosity stability and excellent transparency by adjusting the amount of acid used.
Claims (3)
５までのアルキル基を表す。］で表されるアルミニウム
アルコキシドを、希酸水溶液中で加水分解して得られた
アルミナ１水和物（ベーマイト）を、新たに酸を加えて
から水熱処理して解膠する事を特徴とする、アルミナゾ
ルの製造方法。1. The following general formula Al (OR 1 ) (OR 2 ) (OR 3 ), wherein R 1 , R 2 and R 3 each independently represent an alkyl group having 2 to 5 carbon atoms. ] Alumina monohydrate (boehmite) obtained by hydrolyzing an aluminum alkoxide represented by the following in a dilute aqueous acid solution is characterized by adding a new acid and then hydrothermally treating it for peptization. , Alumina sol manufacturing method.
ニウムに対してモル比で0.005 〜0.1 である特許請求の
範囲第１項記載のアルミナゾルの製造方法。2. The method for producing an alumina sol according to claim 1, wherein the amount of the acid added at the time of peptization is 0.005 to 0.1 in terms of molar ratio with respect to aluminum.
請求の範囲第一項記載の製造方法。3. The production method according to claim 1, wherein the peptization temperature is 100 ° C. to 300 ° C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18184293A JP3462891B2 (en) | 1993-06-28 | 1993-06-28 | Method for producing alumina sol with excellent transparency and good viscosity stability |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18184293A JP3462891B2 (en) | 1993-06-28 | 1993-06-28 | Method for producing alumina sol with excellent transparency and good viscosity stability |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0710535A true JPH0710535A (en) | 1995-01-13 |
| JP3462891B2 JP3462891B2 (en) | 2003-11-05 |
Family
ID=16107773
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18184293A Expired - Lifetime JP3462891B2 (en) | 1993-06-28 | 1993-06-28 | Method for producing alumina sol with excellent transparency and good viscosity stability |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3462891B2 (en) |
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|---|---|---|---|---|
| WO1997032817A1 (en) | 1996-03-05 | 1997-09-12 | Goro Sato | Alumina sol, process for preparing the same, process for preparing alumina molding using the same, and alumina-based catalyst prepared thereby |
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- 1993-06-28 JP JP18184293A patent/JP3462891B2/en not_active Expired - Lifetime
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1997032817A1 (en) | 1996-03-05 | 1997-09-12 | Goro Sato | Alumina sol, process for preparing the same, process for preparing alumina molding using the same, and alumina-based catalyst prepared thereby |
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| JP2008007379A (en) * | 2006-06-30 | 2008-01-17 | Kawaken Fine Chem Co Ltd | Liquid dispersion of alumina glycol and manufacturing method therefor |
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| WO2010050225A1 (en) * | 2008-10-29 | 2010-05-06 | 川研ファインケミカル株式会社 | Porous alumina free-standing film, alumina sol and methods for producing same |
| JP2010105846A (en) * | 2008-10-29 | 2010-05-13 | Kawaken Fine Chem Co Ltd | Alumina porous self-supported film and method for manufacturing the same |
| JP2010132519A (en) * | 2008-12-08 | 2010-06-17 | Kawaken Fine Chem Co Ltd | Alumina sol and method for producing the same |
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