JPH0457611B2 - - Google Patents
Info
- Publication number
- JPH0457611B2 JPH0457611B2 JP58153465A JP15346583A JPH0457611B2 JP H0457611 B2 JPH0457611 B2 JP H0457611B2 JP 58153465 A JP58153465 A JP 58153465A JP 15346583 A JP15346583 A JP 15346583A JP H0457611 B2 JPH0457611 B2 JP H0457611B2
- Authority
- JP
- Japan
- Prior art keywords
- boehmite
- weight
- parts
- compound
- hydrothermal treatment
- 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
Links
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
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/447—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by wet processes
- C01F7/448—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by wet processes using superatmospheric pressure, e.g. hydrothermal conversion of gibbsite into boehmite
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)
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】
本発明はベーマイトの製造方法に関する。ベー
マイトは通常ギブサイトを水熱処理することによ
つて製造される。しかして、ベーマイトを工業的
規模において経済的有利に製造するためには、水
熱処理の温度を低く抑えてユーテイリテイーを削
減することが重要である。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing boehmite. Boehmite is usually produced by hydrothermally treating gibbsite. Therefore, in order to economically advantageously produce boehmite on an industrial scale, it is important to keep the temperature of the hydrothermal treatment low to reduce utility.
本発明者らは、上記実情に鑑み鋭意検討を行な
つた結果、ベーマイト形成化合物の水スラリー中
に特定の化合物を存在させて水熱処理を行なうな
らば、この反応の温度を著しく低下し得るとの知
見を得て、本発明を完成した。 The inventors of the present invention have conducted intensive studies in view of the above circumstances, and have found that the temperature of this reaction can be significantly lowered if a specific compound is present in the aqueous slurry of boehmite-forming compounds and hydrothermal treatment is carried out. The present invention was completed based on these findings.
すなわち、本発明の要旨は、ベーマイト形成化
合物の水スラリーを、該ベーマイト形成化合物を
Al2O3に換算してその100重量部に対し、Ca換算
で少なくとも0.05重量部のカルシウム化合物の存
在下に水熱処理することを特徴とするベーマイト
の製造方法に存する。以下、本発明を詳細に説明
する。 That is, the gist of the present invention is to provide an aqueous slurry of a boehmite-forming compound to a water slurry containing the boehmite-forming compound.
A method for producing boehmite , which comprises hydrothermally treating 100 parts by weight of boehmite in the presence of at least 0.05 parts by weight of a calcium compound in terms of Ca. The present invention will be explained in detail below.
本発明で使用するベーマイト形成化合物として
は、例えば、ギブサイト、バイヤライト、ρ−ア
ルミナ等の100℃以上の温度で水熱処理条件下、
ベーマイトを生成するアルミニウム含有化合物が
用いられる。これは単独でも2種以上の混合物と
しても使用できる。水の使用量は、通常、ベーマ
イト形成化合物100重量部に対して30〜300重量部
の範囲から選ばれる。水の量が少なすぎると水ス
ラリーの粘度が高くなり、攪拌等の操作が困難に
なり、また多すぎると水熱処理中に無用な熱源の
増加を招き経済的ではない。 Boehmite-forming compounds used in the present invention include, for example, gibbsite, bayerite, ρ-alumina, etc. under hydrothermal treatment conditions at a temperature of 100°C or higher.
Aluminum-containing compounds are used that produce boehmite. These can be used alone or as a mixture of two or more. The amount of water used is usually selected from the range of 30 to 300 parts by weight per 100 parts by weight of the boehmite-forming compound. If the amount of water is too small, the viscosity of the water slurry will become high, making operations such as stirring difficult, while if it is too large, an unnecessary heat source will increase during the hydrothermal treatment, which is not economical.
カルシウム化合物としては、CaO、Ca(CH)2、
CaAl2O4等の水熱処理に際しカルシウムイオンを
水スラリー中に供給するカルシウム化合物が用い
られ、その量はベーマイト形成化合物のAl2O3換
算の100重量部に対してCa換算で少くとも0.05重
量部である。Caの量をあまりに多くすると得ら
れるベーマイトを成形体とした場合、その耐熱
性、耐薬品性に低下するので、Caの量は0.05〜20
重量部、好ましくは0.1〜10重量部である。 Calcium compounds include CaO, Ca(CH) 2 ,
A calcium compound is used that supplies calcium ions into the water slurry during the hydrothermal treatment of CaAl 2 O 4 , etc., and the amount thereof is at least 0.05 parts by weight in terms of Ca per 100 parts by weight in terms of Al 2 O 3 of the boehmite-forming compound. Department. If the boehmite obtained is made into a molded product if the amount of Ca is too large, its heat resistance and chemical resistance will decrease, so the amount of Ca should be 0.05 to 20.
parts by weight, preferably 0.1 to 10 parts by weight.
水熱処理は、通常、100℃〜400℃で1Kg/cm2G
〜1000Kg/cm2Gの加圧下、0.1時間〜100時間行な
われるが、本発明方法によりベーマイト形成化合
物の水スラリーをカルシウム化合物の存在下に水
熱処理する場合は、ベーマイト形成化合物の水ス
ラリーをカルシウム化合物の不存在下に水熱処理
する場合より、処理時の温度、圧力、時間を低減
できる。 Hydrothermal treatment is usually 1Kg/ cm2G at 100℃ to 400℃
When hydrothermally treating an aqueous slurry of a boehmite-forming compound in the presence of a calcium compound according to the method of the present invention, the aqueous slurry of a boehmite - forming compound is treated with calcium. The temperature, pressure, and time during treatment can be reduced compared to when hydrothermal treatment is performed in the absence of a compound.
例えば、カルシウム化合物を存在させずにギブ
サイトを水熱処理する場合は、通常、180℃以上
の温度で数時間を要するが、本発明方法によれば
180℃より低い温度下でも3〜4時間で水熱処理
を行なうことができる。 For example, when gibbsite is hydrothermally treated without the presence of calcium compounds, it usually takes several hours at a temperature of 180°C or higher, but according to the method of the present invention,
Hydrothermal treatment can be carried out for 3 to 4 hours even at temperatures lower than 180°C.
また、本発明においては、ベーマイト形成化合
物の水熱処理をカルシウム化合物に加えてアルコ
ール性の水酸基を有する有機化合物の存在下に行
なうことにより得られるベーマイトの結晶形状を
変えることができる。 Furthermore, in the present invention, the crystal shape of the boehmite obtained can be changed by hydrothermally treating the boehmite-forming compound in the presence of an organic compound having an alcoholic hydroxyl group in addition to a calcium compound.
即ち、通常、ベーマイトの結晶外形は単斜柱状
で、そのc軸方向に垂直な相対する結晶面間の長
さ(以下、c軸方向の長さという)に対するa軸
方向の最長の長さの比(以下、a軸長/c軸長比
という)を大きくしたものは結晶性の悪いベーマ
イト或は擬ベーマイトであつた。結晶性の良好な
ベーマイトにおいてはa軸長/c軸長比を10以上
とし、かつ、a軸方向の最長の長さを2000Å以上
とすることはできなかつた。(即ち、従来公知の
ベーマイトにおいては、a軸方向の最長の長さを
2000Å以上としたものはa軸長/c軸長比は5以
下であつた。)しかしながら、本発明においては
水熱処理に際し、カルシウム化合物及びアルコー
ル性水酸基を有する有機化合物を存在させること
により、a軸長/c軸長比が10以上で、かつa軸
方向の最長の長さが2000Å以上のベーマイトが得
られる。 That is, normally, the crystal external shape of boehmite is monoclinic columnar, and the longest length in the a-axis direction is the length between opposing crystal planes perpendicular to the c-axis direction (hereinafter referred to as the length in the c-axis direction). Boehmite or pseudo-boehmite with a large ratio (hereinafter referred to as a-axis length/c-axis length ratio) had poor crystallinity. Boehmite with good crystallinity could not have an a-axis length/c-axis length ratio of 10 or more and a longest length in the a-axis direction of 2000 Å or more. (In other words, in conventionally known boehmite, the longest length in the a-axis direction is
When the thickness was 2000 Å or more, the a-axis length/c-axis length ratio was 5 or less. ) However, in the present invention, by making a calcium compound and an organic compound having an alcoholic hydroxyl group exist during hydrothermal treatment, the a-axis length/c-axis length ratio is 10 or more and the longest length in the a-axis direction is Boehmite with a thickness of over 2000Å can be obtained.
アルコール性の水酸基を有する有機化合物とし
ては各種の有機化合物を用い得るが、通常は、水
熱処理時の温度以上の沸点を有する化合物が採用
される。また、水酸基の数が1個のものも使用し
得るが、水酸基を2個以上有するものが好まし
く、具体例としては、エチレングリコール、ポリ
ビニルアルコール、ヒドロキシエチルセルロース
等が挙げられ、その使用量はベーマイト形成化合
物のAl2O3換算の100重量部に対して0.01〜100重
量部、好ましくは0.1〜50重量部の範囲から選ば
れる。本発明方法により得られるベーマイトはこ
れを成形体とした場合、耐熱性に優れ、かつ高強
度のものが得られる。以下、本発明を実施例によ
つて更に詳細に説明する。 Various organic compounds can be used as the organic compound having an alcoholic hydroxyl group, but usually a compound having a boiling point higher than the temperature during hydrothermal treatment is used. Furthermore, although those having one hydroxyl group may be used, those having two or more hydroxyl groups are preferable. Specific examples include ethylene glycol, polyvinyl alcohol, hydroxyethyl cellulose, etc., and the amount used is determined to form boehmite. It is selected from the range of 0.01 to 100 parts by weight, preferably 0.1 to 50 parts by weight, based on 100 parts by weight of the compound in terms of Al 2 O 3 . When the boehmite obtained by the method of the present invention is made into a molded product, it has excellent heat resistance and high strength. Hereinafter, the present invention will be explained in more detail with reference to Examples.
実施例 1
ギブサイト100重量部、水酸化カルシウム0.8重
量部および水90重量部を室温下で攪拌して水スラ
リーを得た。この水スラリーを金型に注型した
後、167℃、6.5Kg/cm2Gの条件で4時間水熱処理
を行ない、その後、100℃で24時間乾燥してベー
マイト成形体を得た。成形体中のギブサイトの残
存量をX線回折で求めたところtrace程度であり、
167℃4時間の水熱処理でギブサイトの全量がベ
ーマイトに変換していた。Example 1 100 parts by weight of gibbsite, 0.8 parts by weight of calcium hydroxide and 90 parts by weight of water were stirred at room temperature to obtain a water slurry. After this water slurry was cast into a mold, it was subjected to hydrothermal treatment at 167°C and 6.5 kg/cm 2 G for 4 hours, and then dried at 100°C for 24 hours to obtain a boehmite molded body. The remaining amount of gibbsite in the molded body was determined by X-ray diffraction, and it was only a trace.
The entire amount of gibbsite was converted to boehmite by hydrothermal treatment at 167°C for 4 hours.
実施例 2
ギブサイト100重量部、水酸化カルシウム0.8重
量部およびポリビニルアルコールの10%水溶液
100重量部を室温下で攪拌して水スラリーを得た。
この水スラリーを実施例1と同様に処理してベー
マイト成形体を得た。成形体中のギブサイト残存
量を実施例1と同様にして求めたところ、ギブサ
イトは実質的に残存していなかつた。Example 2 100 parts by weight of gibbsite, 0.8 parts by weight of calcium hydroxide and 10% aqueous solution of polyvinyl alcohol
100 parts by weight was stirred at room temperature to obtain a water slurry.
This water slurry was treated in the same manner as in Example 1 to obtain a boehmite molded body. When the remaining amount of gibbsite in the molded article was determined in the same manner as in Example 1, it was found that substantially no gibbsite remained.
また、こうして得られたベーマイトの結晶外形
は、c軸に垂直な相対する結晶面間の長さは約
800Åであり、a軸方向の最長長さは平均的に約
20000Åであり、前者に対する後者の比は25.0で
ある。 In addition, the crystal outline of the boehmite obtained in this way has a length between opposing crystal planes perpendicular to the c-axis of approximately
800 Å, and the longest length in the a-axis direction is approximately
20000 Å, and the ratio of the latter to the former is 25.0.
比較例 1
ギブサイト100重量部、水90重量部を室温下で
攪拌して水スラリーを得た。このスラリーを実施
例1と同様に処理したが、ベーマイトはまつたく
得られず、ギブサイトが残存していた。Comparative Example 1 100 parts by weight of gibbsite and 90 parts by weight of water were stirred at room temperature to obtain a water slurry. This slurry was treated in the same manner as in Example 1, but no boehmite was obtained, and gibbsite remained.
なお、この水スラリーを4時間の水熱処理でベ
ーマイトに転換したときの処理温度は183℃であ
つた。 Note that the treatment temperature when this water slurry was converted to boehmite by hydrothermal treatment for 4 hours was 183°C.
Claims (1)
ーマイト形成化合物をAl2O3に換算してその100
重量部に対し、Ca換算で少なくとも0.05重量部の
カルシウム化合物の存在下に水熱処理することを
特徴とするベーマイトの製造方法。1. The water slurry of the boehmite-forming compound is converted into 100% of the boehmite-forming compound in terms of Al2O3 .
A method for producing boehmite, which comprises hydrothermally treating the boehmite in the presence of at least 0.05 parts by weight of a calcium compound calculated as Ca.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58153465A JPS6046922A (en) | 1983-08-23 | 1983-08-23 | Production of boehmite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58153465A JPS6046922A (en) | 1983-08-23 | 1983-08-23 | Production of boehmite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6046922A JPS6046922A (en) | 1985-03-14 |
| JPH0457611B2 true JPH0457611B2 (en) | 1992-09-14 |
Family
ID=15563153
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58153465A Granted JPS6046922A (en) | 1983-08-23 | 1983-08-23 | Production of boehmite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6046922A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3283475B2 (en) | 1998-09-16 | 2002-05-20 | 河合石灰工業株式会社 | Plate-like boehmite, plate-like alumina, and methods for producing them |
| CN1207208C (en) † | 1999-08-11 | 2005-06-22 | 阿克佐诺贝尔公司 | Process for preparation of quasi-crystalline boehmites from inexpensive precursors |
| WO2020235277A1 (en) * | 2019-05-20 | 2020-11-26 | パナソニックIpマネジメント株式会社 | Boehmite structure and method for producing same |
| US20240417330A1 (en) * | 2021-10-19 | 2024-12-19 | Panasonic Intellectual Property Management Co., Ltd. | Boehmite structure and method for producing same |
-
1983
- 1983-08-23 JP JP58153465A patent/JPS6046922A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6046922A (en) | 1985-03-14 |
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