JPH0513892B2 - - Google Patents
Info
- Publication number
- JPH0513892B2 JPH0513892B2 JP19672185A JP19672185A JPH0513892B2 JP H0513892 B2 JPH0513892 B2 JP H0513892B2 JP 19672185 A JP19672185 A JP 19672185A JP 19672185 A JP19672185 A JP 19672185A JP H0513892 B2 JPH0513892 B2 JP H0513892B2
- Authority
- JP
- Japan
- Prior art keywords
- alumina sol
- acetic acid
- alumina
- temperature
- transmittance
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 36
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 32
- 238000002834 transmittance Methods 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 229910052782 aluminium Inorganic materials 0.000 claims description 11
- -1 aluminum alkoxide Chemical class 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 238000001935 peptisation Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 229910001593 boehmite Inorganic materials 0.000 claims description 3
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 claims description 3
- 150000004682 monohydrates Chemical class 0.000 claims description 3
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010408 film Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- JPUHCPXFQIXLMW-UHFFFAOYSA-N aluminium triethoxide Chemical compound CCO[Al](OCC)OCC JPUHCPXFQIXLMW-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 244000309464 bull Species 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- UAEJRRZPRZCUBE-UHFFFAOYSA-N trimethoxyalumane Chemical compound [Al+3].[O-]C.[O-]C.[O-]C UAEJRRZPRZCUBE-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
- C01F7/36—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts from organic aluminium salts
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Description
【発明の詳細な説明】
産業上の利用分野
本発明は特に透明性の優れたアルミナゾルの製
造方法に関するものである。
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
チツク工業等に用いられており、特に最近ではニ
ユーセラミツクスの原料として急速に伸びている
従来の技術
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2656321号公報（1963）
Bulent I.Yolds，Am.Ceramic Soc.Bull.，
54，289（1975）
日特開昭57−88074号公報
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かならずしも
満足な結果を与えるものではなく、かつ反応所用
時間も長くかかる欠点を有している。近年は電子
材料関係等において特に優れた透明性が要求され
てきており、そのようなアルミナゾルの安定供給
が望まれている。
発明が解決しようとする問題点
本発明は特に透明性に優れたアルミナゾルの製
造方法を提供するものである。具体的にはアルミ
ナを１〜9wt％含有するアルミナゾルにおいて
540nmの光の透過率が95％以上であるアルミナゾ
ルを低温でしかも短時間に製造する方法に関する
ものである。
問題点を解決するための手段
本発明者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
る際の反応条件およ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
れしかも比較的短時間のアルミナゾルの製造方法
をみいだした。
即ち本発明は、アルミニウムアルコキシドを希
酢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、ついで硝酸を加えて解膠し、
かつ全工程を100℃以下の温度で行うことを特徴
とする透明性の優れたアルミナゾルの製造方法で
ある。本発明の要点は加水分解時には酢酸、解膠
時には硝酸をそれぞれ使用することにあり、他の
酸を単純もしくは別の組み合わせで併用しても良
い透明性は得られない。従来の文献では塩酸、硝
酸、硫酸、燐酸、酢酸、蟻酸、過塩素酸等が単独
もしくは併用で使用されてはいるが透明性との論
議はされておらず、本発明のみいだした事実は全
くの新規なものである。
また更に反応条件を検討した結果、特定の酸の
量と特定の温度条件において極めて透明性の優れ
たアルミナゾルがえられることがわかつた。即ち
加水分解時における酢酸の濃度は0.9〜1.25％の
範囲にあり、かつその時の温度が10〜80℃が好ま
しい。また解膠時に加える硝酸の量はアルミニウ
ムアルコキシド１モルあたり0.08〜0.12モルの範
囲が良く、解膠温度は90〜95℃が良い結果を与え
る。これらの範囲を脱するとアルミナゾルの透明
性は悪くなり、また解膠に要する時間も長くな
る。また透明性を良くするためには充分な透過率
に達したら50℃以下に急冷することが望ましい。
必要以上に加熱を続けると透過率が低下するため
である。
本発明に使用するアルミニウムアルコキシドは
アルミニウムメトシキド、アルミニウムエトキシ
ドおよびアルミニウムイソプロポキシドのいずれ
を使用しても良い。アルミニウムアルコキシドの
純度は99％以上が望ましい。
次に本発明の一実施態様を示す。イオン交換水
に所定量の99％酢酸を加えて濃度0.9〜1.25％の
希酢酸水溶液を調製する。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
徐々に投入して加水分解する。投入終了後95℃前
後まで加熱して副生するアルコールを留出させ
る。ほぼ完全にアルコールを除去したのちアルミ
ニウムアルコキシド１モルあたり0.08〜0.12モル
の硝酸を３倍に希釈した水溶液を滴下し、液温を
90〜95℃に保つて良く攪拌し解膠させる。４〜12
時間保持して透過率が充分な透明度になつたら50
℃以下に急冷して透明なアルミナゾル溶液を得
る。
この実施態様に準じて製造したアルミナゾルは
アルミナ濃度が１〜9wt％の範囲において540nm
の波長光の透過率が何れも95％以上の値を示す。
また電子顕微鏡写真によればアルミナの粒径は10
〜100オングストロームと非常に小さいことがわ
かつた。また本発明のアルミナゾル溶液をテフロ
ン製容器に流しこみゆつくり乾燥させると製膜性
が良く透明性の優れた薄膜が得られた。
作 用
本発明の方法で何故透明性の優れたアルミナゾ
ルがえられるかは不明である。
以下実施例によつて本発明を更に詳しく説明す
る。
実施例 １
500ml４つ口フラスコにイオン交換水300gと99
％酢酸３mlを仕込み、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
24g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32gであつた。その後61％
硝酸1.21g（アルミニウムイソプロポキシドに対し
てモル比0.10）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℃に保ちつつ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つたところで液温
を50℃以下に急冷し攪拌をとめた。最高値到達時
間は硝酸溶液滴下後12時間であつた。得られたア
ルミナゾルのアルミナ濃度は2wt％であり、透過
率は340nmで92％、350nmで94％、420nmで97
％、540nmで99％であつた。
実施例２〜７
アルミニウムアルコキシドの使用量を下記の表
に示すように変化させ、アルミナ濃度の異なるア
ルミナゾルを製造した。その他の反応条件は全て
実施例１とほぼ同様に行つた。解膠所要時間と透
過率の結果を下記の表に示す。
【表】
フアインケミカル株式会社製）
実施例 ８
500ml４つ口フラスコにイオン交換水300gと99
％酢酸３mlを仕込んだ。液温は12℃であつた。次
にアルミニウムイソプロポキシド84gを投入し、
液温を80℃まで急上昇させその後徐々に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104gであつた。
その後61％硝酸4.25g（アルミニウムイソプロポキ
シドに対してモル比0.10）を３倍量のイオン交換
水で希釈してから滴下させた。液温は92〜95℃に
保ちつつ５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つた
ところで液温を50℃以下に急冷し攪拌をとめた。
最高値到達時間は硝酸溶液滴下後７時間であつ
た。得られたアルミナゾルの濃度は7wt％であ
り、透過率は340nmで77％、350nmで82％、
420nmで93％、540nmで97％であつた。
比較例 １
500ml４つ口フラスコにイオン交換水300gをと
り、塩酸を加えてPH３としてから液温を80℃まで
加温した。次いでアルミニウムイソプロポキシド
72gを投入し、加水分解を行つた。副生したイソ
プロピルアルコールを留出除去後、これに1N塩
酸水溶液35.2ml（アルミニウムイソプロポキシド
に対してモル比0.1相当）を加えて90〜95℃に保
持したまま16時間攪拌して解膠させた。この時の
アルミナ濃度は6wt％であり、透過率は350nmで
73％、420nmで85％、540nmで92％であつた。
比較例２〜３
比較例１において、塩酸に代えて各々酢酸、硝
酸を使用した他はほぼ同様に行つてアルミナゾル
を得た。下表に解膠時間と透過率の結果を記す。
【表】
発明の効果
本発明によつて今までになく透明性に優れたア
ルミナゾルを安定的に供給することが可能にな
る。 DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention particularly relates to a method for producing an alumina sol with excellent transparency. Alumina sol is used as a surface treatment agent in the paper and textile industries, as a binder for various refractories, as a catalyst carrier, and as a plastics industry.In recent years, it has been rapidly growing as a raw material for new ceramics.Aluminum alkoxide is used as a raw material. Examples of producing transparent alumina sol are already known in the following documents. U.S. Patent No. 2656321 (1963) Bulent I.Yolds, Am.Ceramic Soc.Bull.
54, 289 (1975) Japanese Patent Publication No. 57-88074 However, the alumina sols produced by the techniques described in these documents do not always give satisfactory results in terms of transparency, and the reaction time is also long. It has drawbacks. In recent years, particularly excellent transparency has been required in electronic materials and the like, and a stable supply of such alumina sol is desired. Problems to be Solved by the Invention The present invention provides a method for producing an alumina sol with particularly excellent transparency. Specifically, in alumina sol containing 1 to 9 wt% alumina
The present invention relates to a method for producing alumina sol having a transmittance of 540 nm light of 95% or more at low temperatures and in a short time. Means for Solving the Problems The present inventor has conducted extensive research into the reaction conditions for producing alumina monohydrate (boehmite) by hydrolyzing aluminum alkoxide and the reaction conditions for peptizing it by adding acid. As a result, we discovered a method for producing alumina sol that has particularly excellent transparency and that takes a relatively short time. That is, the present invention hydrolyzes aluminum alkoxide in a dilute aqueous acetic acid solution to obtain alumina monohydrate (boehmite), then peptizes it by adding nitric acid,
This is a method for producing alumina sol with excellent transparency, characterized in that all steps are carried out at a temperature of 100°C or lower. The key point of the present invention is to use acetic acid during hydrolysis and nitric acid during peptization, and transparency cannot be obtained by using other acids simply or in combination in other combinations. In conventional literature, hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, acetic acid, formic acid, perchloric acid, etc. are used alone or in combination, but there is no discussion of transparency, and the fact discovered by the present invention is This is completely new. Furthermore, as a result of further investigation of the reaction conditions, it was found that an extremely transparent alumina sol could be obtained under specific acid amounts and specific temperature conditions. That is, the concentration of acetic acid during hydrolysis is preferably in the range of 0.9 to 1.25%, and the temperature at that time is preferably 10 to 80°C. The amount of nitric acid added during peptization is preferably in the range of 0.08 to 0.12 mol per mol of aluminum alkoxide, and the peptization temperature is 90 to 95°C to give good results. Outside these ranges, the transparency of the alumina sol deteriorates and the time required for peptization increases. Furthermore, in order to improve transparency, it is desirable to rapidly cool the film to 50° C. or lower once a sufficient transmittance is reached.
This is because if heating is continued for longer than necessary, the transmittance will decrease. The aluminum alkoxide used in the present invention may be any of aluminum methoxide, aluminum ethoxide, and aluminum isopropoxide. The purity of aluminum alkoxide is preferably 99% or higher. Next, one embodiment of the present invention will be described. Add a predetermined amount of 99% acetic acid to ion-exchanged water to prepare a dilute acetic acid aqueous solution with a concentration of 0.9 to 1.25%. After heating this, a necessary amount of aluminum alkoxide powder is gradually added while stirring, taking into consideration the concentration of the alumina sol to be produced, and hydrolysis is carried out. After the addition is complete, the mixture is heated to around 95°C to distill off the alcohol by-product. After almost completely removing the alcohol, a 3-fold diluted aqueous solution of 0.08 to 0.12 moles of nitric acid per mole of aluminum alkoxide was added dropwise, and the temperature of the solution was lowered.
Keep at 90-95℃ and stir well to deflocculate. 4～12
50 when the transmittance reaches sufficient transparency after holding for a while.
A clear alumina sol solution is obtained by rapidly cooling to below ℃. The alumina sol produced according to this embodiment has an alumina concentration of 540 nm in the range of 1 to 9 wt%.
The transmittance of wavelength light of 95% or more is shown in each case.
Furthermore, according to electron micrographs, the particle size of alumina is 10
It was found to be extremely small, ~100 angstroms. Furthermore, when the alumina sol solution of the present invention was poured into a Teflon container and allowed to slowly dry, a thin film with good film formability and excellent transparency was obtained. Effect It is unclear why an alumina sol with excellent transparency can be obtained by the method of the present invention. The present invention will be explained in more detail below with reference to Examples. Example 1 300g of ion exchange water and 99g of ion exchange water in a 500ml 4-necked flask
% acetic acid was added, and the temperature of the solution was raised to 75°C while stirring. Then aluminum isopropoxide
24g was added, and the liquid temperature was gradually raised to around 95°C to distill out the generated isopropyl alcohol (hydrous). The distilled amount was 32g. then 61%
1.21 g of nitric acid (mole ratio 0.10 to aluminum isopropoxide) was diluted with 3 times the amount of ion-exchanged water and then added dropwise. The solution was stirred for 8 hours while maintaining the temperature at 92 to 95°C. Transmittance was appropriately measured using a spectrophotometer, and when the transmittance reached almost the maximum value, the liquid temperature was rapidly cooled to 50° C. or less and stirring was stopped. The time to reach the maximum value was 12 hours after dropping the nitric acid solution. The alumina concentration of the obtained alumina sol is 2wt%, and the transmittance is 92% at 340nm, 94% at 350nm, and 97 at 420nm.
%, and 99% at 540 nm. Examples 2 to 7 Alumina sols with different alumina concentrations were produced by varying the amount of aluminum alkoxide used as shown in the table below. All other reaction conditions were substantially the same as in Example 1. The results of the peptization time and transmittance are shown in the table below. [Table] Manufactured by Huain Chemical Co., Ltd.)
Example 8 300g of ion exchange water and 99g of ion exchange water in a 500ml 4-necked flask
% acetic acid was charged. The liquid temperature was 12°C. Next, add 84g of aluminum isopropoxide,
The liquid temperature was rapidly raised to 80°C and then gradually raised to around 95°C to distill out the generated isopropyl alcohol (containing water). The distillate amount was 104g.
Thereafter, 4.25 g of 61% nitric acid (mole ratio 0.10 to aluminum isopropoxide) was diluted with 3 times the amount of ion-exchanged water and then added dropwise. The solution was stirred for 5 hours while maintaining the temperature at 92 to 95°C. Transmittance was appropriately measured using a spectrophotometer, and when the transmittance reached almost the maximum value, the liquid temperature was rapidly cooled to 50° C. or less and stirring was stopped.
The time to reach the maximum value was 7 hours after dropping the nitric acid solution. The concentration of the obtained alumina sol was 7wt%, and the transmittance was 77% at 340nm, 82% at 350nm,
It was 93% at 420nm and 97% at 540nm. Comparative Example 1 300 g of ion-exchanged water was placed in a 500 ml four-necked flask, and after adding hydrochloric acid to adjust the pH to 3, the liquid temperature was heated to 80°C. Then aluminum isopropoxide
72g was added to perform hydrolysis. After removing the by-produced isopropyl alcohol by distillation, add 35.2 ml of 1N hydrochloric acid aqueous solution (equivalent to a molar ratio of 0.1 to aluminum isopropoxide) and stir for 16 hours while maintaining the temperature at 90 to 95°C to peptize the mixture. Ta. The alumina concentration at this time was 6wt%, and the transmittance was 350nm.
73%, 85% at 420nm, and 92% at 540nm. Comparative Examples 2 to 3 Alumina sol was obtained in substantially the same manner as in Comparative Example 1 except that acetic acid and nitric acid were used in place of hydrochloric acid. The table below shows the results of peptization time and transmittance. [Table] Effects of the Invention The present invention makes it possible to stably supply an alumina sol with unprecedented transparency.
Claims (1)
で加水分解してアルミナ１水和物（ベーマイト）
とし、ついで硝酸を加えて解膠し、かつ全工程を
100℃以下の温度で行うことを特徴とする透明性
の優れたアルミナゾルの製造方法。 ２ 酢酸の濃度が0.9〜1.25％の範囲にある希酢
酸水溶液を使用することを特徴とする特許請求の
範囲第１項記載の方法。 ３ 硝酸量がアルミニウムアルコキシド１モルに
対して0.08〜0.12モルの範囲であることを特徴と
する特許請求の範囲第１項記載の製造方法。 ４ 解膠温度が90〜95℃であり、かつ充分な透過
率が得られたところで50℃以下に急冷することを
特徴とする特許請求の範囲第１項記載の製造方
法。[Claims] 1. Alumina monohydrate (boehmite) is produced by hydrolyzing aluminum alkoxide in a dilute acetic acid aqueous solution.
Then add nitric acid to deflocculate, and complete the entire process.
A method for producing alumina sol with excellent transparency, which is characterized by being carried out at a temperature of 100°C or less. 2. The method according to claim 1, characterized in that a dilute aqueous acetic acid solution having an acetic acid concentration in the range of 0.9 to 1.25% is used. 3. The manufacturing method according to claim 1, wherein the amount of nitric acid is in the range of 0.08 to 0.12 mol per mol of aluminum alkoxide. 4. The manufacturing method according to claim 1, wherein the peptization temperature is 90 to 95°C, and the process is rapidly cooled to 50°C or lower after sufficient transmittance is obtained.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19672185A JPS6256321A (en) | 1985-09-05 | 1985-09-05 | Production of alumina sol having excellent transparency |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19672185A JPS6256321A (en) | 1985-09-05 | 1985-09-05 | Production of alumina sol having excellent transparency |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6256321A JPS6256321A (en) | 1987-03-12 |
| JPH0513892B2 true JPH0513892B2 (en) | 1993-02-23 |
Family
ID=16362489
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19672185A Granted JPS6256321A (en) | 1985-09-05 | 1985-09-05 | Production of alumina sol having excellent transparency |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6256321A (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR930005318B1 (en) * | 1991-06-11 | 1993-06-17 | 한국과학기술연구원 | Process for preparation of alumina sol |
| JPH0658803U (en) * | 1993-01-28 | 1994-08-16 | 昭世 重永 | Ear cover for preventing stains during hair dyeing and perming work |
| US6565950B1 (en) | 1998-06-18 | 2003-05-20 | Canon Kabushiki Kaisha | Recording medium, image forming method utilizing the same, method for producing the same, alumina dispersion and method for producing the same |
| JP2002123026A (en) * | 2000-08-08 | 2002-04-26 | Canon Inc | Electrophotographic photoreceptor, method for manufacturing the electrophotographic photoreceptor, process cartridge and electrophotographic device |
| JP2008239461A (en) * | 2007-03-29 | 2008-10-09 | Fujifilm Corp | Metal oxide fine particle dispersion material and method for manufacturing the same |
| US20110206919A1 (en) * | 2008-10-29 | 2011-08-25 | Kawaken Fine Chemicals Co., Ltd. | Porous alumina free-standing film, alumina sol and methods for producing same |
| JP5429733B2 (en) * | 2008-12-08 | 2014-02-26 | 川研ファインケミカル株式会社 | Alumina sol and method for producing the same |
| JP5303695B2 (en) * | 2008-10-29 | 2013-10-02 | 川研ファインケミカル株式会社 | Alumina porous self-supporting membrane and method for producing the same |
| EP2663399A1 (en) * | 2011-01-12 | 2013-11-20 | BP Corporation North America Inc. | Method of making and using hydrocarbon conversion catalyst |
-
1985
- 1985-09-05 JP JP19672185A patent/JPS6256321A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6256321A (en) | 1987-03-12 |
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