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JPH09227116A - Production of layered silicic acid salt - Google Patents

Production of layered silicic acid salt

Info

Publication number
JPH09227116A
JPH09227116A JP6190096A JP6190096A JPH09227116A JP H09227116 A JPH09227116 A JP H09227116A JP 6190096 A JP6190096 A JP 6190096A JP 6190096 A JP6190096 A JP 6190096A JP H09227116 A JPH09227116 A JP H09227116A
Authority
JP
Japan
Prior art keywords
silicic acid
aqueous solution
acid compound
hydrothermal reaction
sodium
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
JP6190096A
Other languages
Japanese (ja)
Inventor
Katsunori Kosuge
勝典 小菅
Motohiko Tanaka
元彦 田中
Takeshi Fujita
武 藤田
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
National Institute of Advanced Industrial Science and Technology AIST
Sakai Chemical Industry Co Ltd
Original Assignee
Agency of Industrial Science and Technology
Sakai Chemical Industry Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Agency of Industrial Science and Technology, Sakai Chemical Industry Co Ltd filed Critical Agency of Industrial Science and Technology
Priority to JP6190096A priority Critical patent/JPH09227116A/en
Publication of JPH09227116A publication Critical patent/JPH09227116A/en
Pending legal-status Critical Current

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  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

PROBLEM TO BE SOLVED: To obtain an ilerite-type layered silicic acid salt effectively at a low cost and industrially advantageously by using an inexpensive silicic acid compound and by performing a hydrothermal reaction of an aqueous solution of a silicic acid compound. SOLUTION: This layered silicic acid salt is obtained by performing a hydrothermal reaction of an aqueous solution of a silicic acid compound such as an aqueous solution of sodium silicate and potassium silicate an aqueous solution of crystals of sodium orthosilicate or sodium metasilicate, having 10-60wt.% solid portion concentration by using the silicic acid compound by 1mol SiO2 to 5-30mol water in a molar ratio with water and based on SiO2 in the silicic acid compound, at 100-150 deg.C, while agitating. As necessary, in order to obtain an ilerite-type layered silicic acid salt having better crystalline properties, a seed crystal or a part of the previous batch is added. The hydrothermal reaction is performed in the presence of an alkali, and an oxide or a hydroxide of sodium, potassium, etc., is added by 0.2-0.8mol based on 1mol SiO2 . The solid material obtained by the hydrothermal reaction is separated from mother liquor thereof, and recovered by drying after washing.

Description

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

【0001】[0001]

【発明の属する技術分野】本発明は、アイラアイト型層
状ケイ酸塩の工業的な水熱合成による製造方法に関す
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an ilaito type layered silicate by industrial hydrothermal synthesis.

【0002】[0002]

【従来の技術】層状ケイ酸塩は、その特殊構造に基づい
て機能性材料への応用が期待されている物質の1つであ
る。これ自体、触媒、充填剤、吸着剤等の種々の用途開
発がなされているが、更に、層状ケイ酸塩を用いたイン
ターカレーションによる層間修飾では、新規な触媒や多
孔材料をはじめとした機能性材料の開発が行われてお
り、発展が期待されている分野である。
2. Description of the Related Art Layered silicates are one of the substances that are expected to be applied to functional materials due to their special structure. As such, various applications such as catalysts, fillers, and adsorbents have been developed. In addition, in inter-layer modification by intercalation using layered silicates, new catalysts and porous materials and other functions have been developed. Is being developed, and is a field that is expected to grow.

【0003】機能性材料の開発に用いられている層状ケ
イ酸塩としては、アイラアイト型層状ケイ酸塩のほか、
天然のスメクタイト系粘土鉱物、膨潤性フッ素雲母等が
挙げられる。アイラアイト型層状ケイ酸塩とは、Na2
Si8 17・nH2 Oで表される天然には産出しない、
新しいタイプのケイ酸塩化合物であり、オクトシリケー
トとも呼ばれる。
As the layered silicate used for the development of the functional material, in addition to the ilaite type layered silicate,
Examples include natural smectite clay minerals and swelling fluoromica. Iraite type layered silicate means Na 2
Naturally represented by Si 8 O 17 · nH 2 O does not occur naturally,
A new type of silicate compound, also called octosilicate.

【0004】以下の文献に記載されているように、アイ
ラアイト型層状ケイ酸塩の合成には、従来、シリカゲ
ル、シリカゾル等の高価な原料が用いられていた。ジー
・ボーベリー(G.Borbely)、エイチ・ケイ・
バイエル(H.K.Beyer)、エイチ・ジー・カル
ゲ(H.G.Karge)、ダブリュ・シュバイゲル
(W.Schwieger)、エイ・ブラント(A.B
randt)、ケイ・エイチ・ベルク(K.H.Ber
gk)著、クレイズ・アンド・クレイ・ミネラルズ(C
lays & Clay Minerals)39巻、
490頁(1991年);ケイ・コスゲ(K.Kosu
ge)、エイ・ツナシマ(A.Tsunashima)
著、ジャーナル・オブ・ザ・ケミカル・ソサエティー
(J.Chem.Soc.),ケミカル・コミュニケー
ションズ(Chem.Commun..)23巻、24
27頁(1995年)。
As described in the following documents, expensive raw materials such as silica gel and silica sol have hitherto been used for the synthesis of the ilaito type layered silicate. G. Borbury, H.K.
HK Beyer, H. G. Karge, W. Schwieger, A. Brandt (AB)
randt), KH Berg (KH Ber)
gk), Crazy and Clay Minerals (C
Lays & Clay Minerals) Vol. 39,
490 (1991); K. Kosu
ge), A. Tsunashima
Author, Journal of the Chemical Society (J. Chem. Soc.), Chemical Communications (Chem. Commun ..), 23, 24
Page 27 (1995).

【0005】層状ケイ酸塩を活用した機能性材料の開発
においては、より安価な原料を出発原料とした、効率の
よい合成プロセスが望まれている。しかしながら、アイ
ラアイト型層状ケイ酸塩は、上述したように原料が高価
であり、また、その製造は、効率のよいものではなかっ
た。
In developing functional materials utilizing layered silicates, efficient synthetic processes using cheaper raw materials as starting materials are desired. However, as described above, the raw materials of the ilaito type layered silicate are expensive, and the production thereof is not efficient.

【0006】[0006]

【発明が解決しようとする課題】本発明は、上記に鑑
み、工業的に有利であり、安価であるケイ酸化合物を使
用して、効率よく、安価にアイラアイト型層状ケイ酸塩
を製造することができる層状ケイ酸塩の製造方法を提供
することを目的とするものである。
DISCLOSURE OF THE INVENTION In view of the above, the present invention is to produce an ilaito type layered silicate efficiently and inexpensively using a silicic acid compound which is industrially advantageous and inexpensive. It is an object of the present invention to provide a method for producing a layered silicate capable of achieving the above.

【0007】[0007]

【課題を解決するための手段】本発明の要旨は、ケイ酸
化合物の水溶液を、100〜150℃で水熱反応させる
アイラアイト型層状ケイ酸塩の製造方法に存する。以下
に本発明を詳述する。
The gist of the present invention lies in a method for producing an ilaito type layered silicate by hydrothermally reacting an aqueous solution of a silicic acid compound at 100 to 150 ° C. Hereinafter, the present invention will be described in detail.

【0008】本発明で使用されるケイ酸化合物の水溶液
としては特に限定されず、例えば、水溶液状のケイ酸ソ
ーダ、水溶液状のケイ酸カリウム;オルソケイ酸ソー
ダ、メタケイ酸ソーダ等の結晶の水溶液等を挙げること
ができる。また、場合によっては、固体状のカレットを
水に溶解して使用してもよい。
The aqueous solution of the silicic acid compound used in the present invention is not particularly limited, and examples thereof include aqueous solution sodium silicate, aqueous solution potassium silicate; aqueous solution of crystals of sodium orthosilicate, sodium metasilicate and the like. Can be mentioned. In some cases, solid cullet may be dissolved in water before use.

【0009】上記水溶液の固形分濃度は、10〜60重
量%が好ましい。10重量%未満であると、経済的に不
利であり、60重量%を超えると、分離等を起こして、
工業的に問題を生じる。より好ましくは、15〜45重
量%である。
The solid concentration of the above aqueous solution is preferably 10 to 60% by weight. If it is less than 10% by weight, it is economically disadvantageous, and if it exceeds 60% by weight, separation or the like occurs,
It causes industrial problems. More preferably, it is 15 to 45% by weight.

【0010】上記ケイ酸化合物と水とのモル比は、上記
ケイ酸化合物を、SiO2 で換算した場合、SiO2
モルに対して5〜30モルが好ましい。5モル未満であ
ると、水が少なすぎて水熱反応が起こりにくく、30モ
ルを超えると、得られる層状ケイ酸塩の収率が悪くな
る。より好ましくは、7〜20モルである。
[0010] The molar ratio of the silicate compound and water, the silicate compound, when converted with SiO 2, SiO 2 1
5-30 mol is preferable with respect to mol. If it is less than 5 mol, the amount of water is too small to cause a hydrothermal reaction, and if it exceeds 30 mol, the yield of the obtained layered silicate is poor. More preferably, it is 7 to 20 mol.

【0011】本発明において、上記ケイ酸化合物の水溶
液は、水熱反応させる。上記水熱反応とは、高温高圧水
の存在下で反応させることである。上記水熱反応の反応
温度は、100〜150℃である。100℃未満である
と、反応に時間がかかり、150℃を超えると、クリス
トバライト、石英、あるいはマガディアイト等の不純物
が晶出するため上記範囲に限定される。好ましくは、1
00〜130℃である。上記水熱反応により得られた固
体物質は、常法により母液と分離され、水洗された後、
乾燥して回収される。
In the present invention, the aqueous solution of the silicic acid compound is hydrothermally reacted. The hydrothermal reaction is to react in the presence of high temperature and high pressure water. The reaction temperature of the hydrothermal reaction is 100 to 150 ° C. If the temperature is lower than 100 ° C., the reaction takes a long time, and if the temperature exceeds 150 ° C., impurities such as cristobalite, quartz, or magadiite crystallize out, and thus the range is limited to the above range. Preferably, 1
It is 00-130 degreeC. The solid substance obtained by the hydrothermal reaction is separated from the mother liquor by a conventional method and washed with water,
It is dried and collected.

【0012】本発明において、上記水熱反応中、ケイ酸
化合物の水溶液は、反応系の均一性を保持するために、
攪拌されていることが好ましい。上記水熱反応におい
て、より結晶性のよいアイラアイト型層状ケイ酸塩を得
るために、上記アイラアイト型層状ケイ酸塩の種子結晶
を添加してもよい。また、上記種子結晶を添加する代わ
りに、前バッチの一部を添加したり、反応容器に残して
おいたりしても同様の効果を得ることができる。
In the present invention, during the hydrothermal reaction, the aqueous solution of the silicic acid compound is used to maintain the homogeneity of the reaction system.
It is preferably stirred. In the hydrothermal reaction, seed crystals of the above-mentioned ilaito-type layered silicate may be added in order to obtain more crystalline ilaite-type layered silicate. Further, instead of adding the seed crystals, the same effect can be obtained by adding a part of the previous batch or leaving it in the reaction vessel.

【0013】本発明において、上記水熱反応は、アルカ
リ存在下で行うことが必要であり、上記アルカリとして
は特に限定されず、例えば、ナトリウム、カリウム、リ
チウム等の酸化物、水酸化物、あるいは炭酸塩等を挙げ
ることができる。これらは、単独で使用してもよく、2
種以上を併用してもよい。
In the present invention, the hydrothermal reaction needs to be carried out in the presence of an alkali, and the alkali is not particularly limited, and examples thereof include oxides such as sodium, potassium and lithium, hydroxides, or Carbonate etc. can be mentioned. These may be used alone or 2
More than one species may be used in combination.

【0014】上記アルカリの添加量は、水酸化ナトリウ
ム又は水酸化カリウムで換算した場合、SiO2 1モル
に対して、0.2〜0.8モルが好ましい。0.2モル
未満であると、アルカリ添加の効果を得ることができ
ず、0.8モルを超えると、反応を阻害する可能性があ
る。より好ましくは、0.4〜0.6モルである。
The amount of the above-mentioned alkali added is preferably 0.2 to 0.8 mol per 1 mol of SiO 2 when converted into sodium hydroxide or potassium hydroxide. If it is less than 0.2 mol, the effect of alkali addition cannot be obtained, and if it exceeds 0.8 mol, the reaction may be inhibited. More preferably, it is 0.4 to 0.6 mol.

【0015】本発明の層状ケイ酸塩の製造方法により製
造された層状ケイ酸塩は、公知の方法により得られるア
イラアイト型層状ケイ酸塩と何ら変わりのないものであ
る。
The layered silicate produced by the method for producing a layered silicate of the present invention is no different from the isolaite type layered silicate obtained by a known method.

【0016】[0016]

【実施例】以下に実施例を掲げて本発明を更に詳しく説
明するが、本発明はこれら実施例のみに限定されるもの
ではない。
The present invention will be described in more detail with reference to the following examples, but the present invention is not limited to these examples.

【0017】実施例1 SiO2 23.3重量%、Na2 O 6.2重量%
(モル比:NaOH/SiO2 =0.51/1.0)か
らなる水ガラス(4号ケイ酸ソーダ)700gを1Lオ
ートクレーブ中において、反応温度107℃の水熱条件
下で、280時間処理した。反応終了後、濾別して固相
を分離し、水洗した。得られた固体を80℃で一昼夜乾
燥後、X線回折法で測定したところ、アイラアイト型層
状ケイ酸塩と同一のパターンを示した。
Example 1 23.3% by weight of SiO 2 and 6.2% by weight of Na 2 O
700 g of water glass (sodium silicate No. 4) composed of (molar ratio: NaOH / SiO 2 = 0.51 / 1.0) was treated in a 1 L autoclave under hydrothermal conditions at a reaction temperature of 107 ° C. for 280 hours. . After the reaction was completed, the solid phase was separated by filtration and washed with water. The obtained solid was dried at 80 ° C. for a whole day and night, and then measured by X-ray diffractometry to show the same pattern as that of the ilaite type layered silicate.

【0018】実施例2 SiO2 27.6重量%、Na2 O 9.1重量%
(モル比:NaOH/SiO2 =0.64/1.0)か
らなる水ガラス(3号ケイ酸ソーダ)に硫酸を加え、N
aOH/SiO2 のモル比を0.60/1.0に調整し
た後、オートクレーブに移し、反応温度105℃の水熱
条件下で、360時間処理した。得られた結晶は、実施
例1と同様にアイラアイト型層状ケイ酸塩と同一のX線
回折パターンを示した。
Example 2 27.6% by weight of SiO 2 and 9.1% by weight of Na 2 O
Sulfuric acid was added to water glass (No. 3 sodium silicate) composed of (molar ratio: NaOH / SiO 2 = 0.64 / 1.0), and N was added.
After adjusting the molar ratio of aOH / SiO 2 to 0.60 / 1.0, it was transferred to an autoclave and treated under hydrothermal conditions at a reaction temperature of 105 ° C. for 360 hours. The obtained crystal showed the same X-ray diffraction pattern as that of the ilaite type layered silicate as in Example 1.

【0019】実施例3 実施例1と同様の条件に、実施例1で得られた反応生成
液35mlを加え、同じく1Lオートクレーブ中におい
て、反応温度110℃の水熱条件下で200時間処理し
た。得られた結晶は、実施例1と同様にアイラアイト型
層状ケイ酸塩と同一のX線回折パターンを示した。
Example 3 35 ml of the reaction product solution obtained in Example 1 was added to the same conditions as in Example 1, and the mixture was treated in the same 1 L autoclave for 200 hours under hydrothermal conditions at a reaction temperature of 110 ° C. The obtained crystal showed the same X-ray diffraction pattern as that of the ilaite type layered silicate as in Example 1.

【0020】[0020]

【発明の効果】本発明の層状ケイ酸塩の製造方法は上述
のとおりであり、従来の方法に比べて、効率よく、安価
にアイラアイト型層状ケイ酸塩を製造することができる
ので、アイラアイト型層状ケイ酸塩の製造方法として好
適である。
The method for producing the layered silicate of the present invention is as described above, and the isolaite type layered silicate can be produced more efficiently and cheaper than the conventional method. It is suitable as a method for producing a layered silicate.

【図面の簡単な説明】[Brief description of drawings]

【図1】実施例1で得られたアイラアイト型層状ケイ酸
塩のX線回折チャートである。縦軸は、X線強度(cp
s)であり、横軸は、回折角(2θ)である。
FIG. 1 is an X-ray diffraction chart of an islayite type layered silicate obtained in Example 1. The vertical axis represents the X-ray intensity (cp
s), and the horizontal axis is the diffraction angle (2θ).

【図2】アイラアイト型層状ケイ酸塩の電子顕微鏡写真
である。(5000倍)
FIG. 2 is an electron micrograph of an ilaito type layered silicate. (5000 times)

───────────────────────────────────────────────────── フロントページの続き (72)発明者 田中 元彦 堺市戎島町5丁1番地 堺化学工業株式会 社内 (72)発明者 藤田 武 堺市戎島町5丁1番地 堺化学工業株式会 社内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Motohiko Tanaka, 5-1, Ebishima-cho, Sakai City, Sakai Chemical Industry Co., Ltd. (72) Inventor, Takeshi Fujita 5-chome, Ebisu-machi, Sakai City, Sakai Chemical Industry Co., Ltd.

Claims (1)

【特許請求の範囲】[Claims] 【請求項1】 ケイ酸化合物の水溶液を、100〜15
0℃で水熱反応させることを特徴とするアイラアイト型
層状ケイ酸塩の製造方法。
1. An aqueous solution of a silicic acid compound is added in an amount of 100 to 15
A method for producing an ilaito type layered silicate, which comprises performing a hydrothermal reaction at 0 ° C.
JP6190096A 1996-02-23 1996-02-23 Production of layered silicic acid salt Pending JPH09227116A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP6190096A JPH09227116A (en) 1996-02-23 1996-02-23 Production of layered silicic acid salt

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP6190096A JPH09227116A (en) 1996-02-23 1996-02-23 Production of layered silicic acid salt

Publications (1)

Publication Number Publication Date
JPH09227116A true JPH09227116A (en) 1997-09-02

Family

ID=13184494

Family Applications (1)

Application Number Title Priority Date Filing Date
JP6190096A Pending JPH09227116A (en) 1996-02-23 1996-02-23 Production of layered silicic acid salt

Country Status (1)

Country Link
JP (1) JPH09227116A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007020894A1 (en) * 2005-08-12 2007-02-22 Shiseido Co., Ltd. Mesoporous silica and method for production thereof
JP2007045692A (en) * 2005-08-12 2007-02-22 Shiseido Co Ltd Method of manufacturing mesoporous silica and method of manufacturing the same
JP2012051759A (en) * 2010-09-01 2012-03-15 Osaka Prefecture Univ Method of manufacturing layer silicate compound
JP2013040066A (en) * 2011-08-12 2013-02-28 Osaka Prefecture Univ Method for manufacturing lamellar silicate compound

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007020894A1 (en) * 2005-08-12 2007-02-22 Shiseido Co., Ltd. Mesoporous silica and method for production thereof
JP2007045692A (en) * 2005-08-12 2007-02-22 Shiseido Co Ltd Method of manufacturing mesoporous silica and method of manufacturing the same
JP2012051759A (en) * 2010-09-01 2012-03-15 Osaka Prefecture Univ Method of manufacturing layer silicate compound
JP2013040066A (en) * 2011-08-12 2013-02-28 Osaka Prefecture Univ Method for manufacturing lamellar silicate compound

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