JPH06206721A - Production of amorphous aluminosilicate - Google Patents
Production of amorphous aluminosilicateInfo
- Publication number
- JPH06206721A JPH06206721A JP205793A JP205793A JPH06206721A JP H06206721 A JPH06206721 A JP H06206721A JP 205793 A JP205793 A JP 205793A JP 205793 A JP205793 A JP 205793A JP H06206721 A JPH06206721 A JP H06206721A
- Authority
- JP
- Japan
- Prior art keywords
- mol
- aqueous solution
- concentration
- ion
- amorphous aluminosilicate
- 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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- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、ゴム用，樹脂用，紙
用，塗料用などの無機充填剤やイオン交換剤，触媒や脱
臭剤の担体またはゼオライトの合成原料等に用いられる
無定形アルミノシリケートの製造方法に関するものであ
り、アルミン酸アルカリ金属塩水溶液とケイ酸アルカリ
金属塩水溶液をを連続的に又は回分式に混合して反応さ
せて凝集した粒子の比較的少ない無定形アルミノシリケ
ートを製造する方法に関するものである。更に詳しく述
べると、イオン交換体としてはそのイオン交換性能が、
２００ｍｇＣａＣＯ3／ｇ以上の性能を有し、また、油
状物質の担体としては、２ｃｃ／ｇ以上の油状物質吸収
性を有する無定形アルミノシリケートを製造する方法に
関するものである。BACKGROUND OF THE INVENTION The present invention relates to an amorphous alumino, which is used as an inorganic filler for rubber, resin, paper, paint, an ion exchanger, a carrier for catalysts and deodorants, or a synthetic raw material for zeolite. The present invention relates to a method for producing a silicate, which produces an amorphous aluminosilicate having relatively few agglomerated particles by continuously or batchwise mixing and reacting an aqueous alkali metal aluminate solution and an aqueous alkali metal silicate solution. It is about how to do it. More specifically, the ion exchange performance of the ion exchanger is
The present invention relates to a method for producing an amorphous aluminosilicate having a performance of 200 mgCaCO 3 / g or more and having an oil substance absorbency of 2 cc / g or more as a carrier for an oil substance.
【０００２】[0002]
【従来の技術】無定形アルミノシリケートは従来一般的
にアルミン酸ナトリウム水溶液と、ケイ酸ナトリウム水
溶液とを混合し、また必要に応じて追加の水酸化ナトリ
ウム水溶液を混合し製造されていた。具体的な例を上げ
ると、例えば特開昭４９−６４６００号公報には無定形
アルミノシリケートの合成方法が詳しく述べられている
が、このものはゼオライトを合成する為の原料としてで
あり、イオン交換特性などの特徴については特に問題に
していない。また、特開昭５２−５８０９９号公報で
は、生成物のイオン交換能はかなり高いものではあるが
まだ不十分であるし、その他の特性として、油吸収性は
７５ｃｃ／１００ｇと、非常に低いものである。この様
な方法においてはその生産性を高めるために、希薄な溶
液とはいいながらも実質的にはかなり高い濃度のアルミ
ン酸ナトリウムとケイ酸ナトリウムとを混合している。
そのため、それぞれの溶解度を高めるために必然的に高
い水酸化物イオン濃度の領域で反応する必要が有り、こ
れらの原料を混合して得られる無定形アルミノシリケー
トのイオン交換特性は限られた範囲にとどまる。2. Description of the Related Art Amorphous aluminosilicates have hitherto been generally produced by mixing an aqueous solution of sodium aluminate and an aqueous solution of sodium silicate, and optionally an additional aqueous solution of sodium hydroxide. As a specific example, for example, JP-A-49-64600 describes in detail a method for synthesizing an amorphous aluminosilicate, which is a raw material for synthesizing zeolite and is ion-exchanged. Characteristics such as characteristics are not particularly a problem. Further, in JP-A-52-58099, the ion exchange capacity of the product is quite high but is still insufficient, and as another characteristic, the oil absorption is as low as 75 cc / 100 g. Is. In such a method, in order to increase the productivity, although it is a dilute solution, sodium aluminate and sodium silicate having substantially high concentrations are mixed.
Therefore, in order to increase the solubility of each, it is necessary to react in the region of high hydroxide ion concentration inevitably, the ion exchange characteristics of the amorphous aluminosilicate obtained by mixing these raw materials is limited to a limited range. Stay
【０００３】[0003]
【発明が解決しようとする課題】従来の方法で調製した
無定型アルミノシリケートは、例えば触媒等に利用する
場合は、均一に触媒としての修飾を行うこと（例えば有
用な金属イオンとのイオン交換や、それらの担持等）が
困難であり、触媒としても均一な性能が得られにくい。
また、イオン交換体として使用する際は、そのイオン交
換性能が十分とはいえない。また、油状の物質を含浸さ
せる場合にも、その吸収量が不十分なものであった。When the amorphous aluminosilicate prepared by the conventional method is used as a catalyst, for example, it should be uniformly modified as a catalyst (for example, ion exchange with a useful metal ion or However, it is difficult to obtain uniform performance as a catalyst.
Moreover, when used as an ion exchanger, its ion exchange performance is not sufficient. Further, even when impregnated with an oily substance, the amount absorbed was insufficient.
【０００４】このように、無定形アルミノシリケートの
イオン交換性能や、油状物質の吸収性を向上させること
は非常に重要な課題であった。As described above, it has been a very important subject to improve the ion exchange performance of amorphous aluminosilicate and the absorbability of oily substances.
【０００５】[0005]
【課題を解決するための手段】本発明者らは、無定形ア
ルミノシリケートの製造方法について鋭意検討を重ねた
結果、アルミン酸アルカリ金属塩溶液およびケイ酸アル
カリ金属塩溶液を原料として製造する際の遊離の水酸化
物イオンの濃度と得られる無定形アルミノシリケートの
イオン交換性や、油状物質吸収性との間に密接な関係を
見出し、本発明に至った。Means for Solving the Problems As a result of extensive studies on the method for producing an amorphous aluminosilicate, the present inventors have found that when an alkali metal aluminate solution and an alkali metal silicate solution are used as starting materials. The inventors have found a close relationship between the concentration of free hydroxide ion and the ion-exchange property of the obtained amorphous aluminosilicate and the absorbability of oily substance, and arrived at the present invention.
【０００６】すなわち、本発明は、アルミン酸アルカリ
金属塩水溶液とケイ酸アルカリ金属塩水溶液を反応させ
て無定形アルミノシリケートを製造する方法において、
前記両水溶液と水または水酸化ナトリウム水溶液を混合
して反応を起こさせる際の、水酸化物イオンの濃度が、
１．６ｍｏｌ／ｋｇ以下である反応条件下で反応させる
ことによって、得られる無定型アルミノシリケートのイ
オン交換性能が、２００ｍｇＣａＣＯ3／ｇ以上であ
り、かつ油状物質吸収性能が、２ｃｃ／ｇ以上の無定形
アルミノシリケートを製造する方法を提供するものであ
る。本明細書において、「水酸化物イオン濃度」とは、
下式によって求められるものをいう（式中、「Ｍ」はア
ルカリ金属を意味する。以下、同じ）。That is, the present invention provides a method for producing an amorphous aluminosilicate by reacting an aqueous solution of an alkali metal aluminate with an aqueous solution of an alkali metal silicate.
The concentration of hydroxide ions when the reaction is caused by mixing the both aqueous solutions and water or an aqueous sodium hydroxide solution,
By reacting under a reaction condition of 1.6 mol / kg or less, the ion exchange performance of the amorphous aluminosilicate obtained is 200 mgCaCO 3 / g or more, and the oily substance absorption performance is 2 cc / g or more. The present invention provides a method for producing a regular aluminosilicate. In the present specification, “hydroxide ion concentration” means
It means what is calculated by the following formula (in the formula, "M" means an alkali metal. The same applies hereinafter).
【０００７】水酸化物イオン濃度（ｍｏｌ／ｋｇ）＝Ｍ
2Ｏ（ｍｏｌ／ｋｇ）×２ −Ａｌ2Ｏ3（ｍｏｌ／ｋｇ）×２ −水酸イオン以外の陰イオンの濃度（グラムイオン／ｋ
ｇ） 本発明によれば生成する無定形アルミノシリケートは、
前述の様に高いイオン交換性と油状物質吸収性を合せも
つ。本発明で得られる無定形アルミノシリケートは、結
合水を含まないかたちで一般式 ０．８〜１．２（Ｍ2Ｏ）・Ａｌ2Ｏ3・２〜４（Ｓｉ
Ｏ2） で表わされるものである。Hydroxide ion concentration (mol / kg) = M
2 O (mol / kg) × 2-Al 2 O 3 (mol / kg) × 2-concentration of anions other than hydroxide ion (gram ion / k
g) The amorphous aluminosilicate produced according to the invention is
As mentioned above, it has both high ion exchange and oily substance absorption. The amorphous aluminosilicate obtained according to the present invention has the general formula of 0.8 to 1.2 (M 2 O) .Al 2 O 3 to 2 to 4 (Si
It is represented by O 2 ).
【０００８】以下本発明の内容を例を上げて詳細に説明
する。The contents of the present invention will be described in detail below with reference to examples.
【０００９】本発明に用いる原料は、アルミン酸アルカ
リ金属塩水溶液及びケイ酸アルカリ金属塩水溶液であ
る。また必要に応じて水酸化アルカリ塩水溶液で前記両
溶液を希釈して用いる。The raw materials used in the present invention are an aqueous solution of alkali metal aluminate and an aqueous solution of alkali metal silicate. If necessary, both solutions are diluted with an aqueous solution of alkali hydroxide and used.
【００１０】また前記両水溶液は市販のアルミン酸アル
カリ金属塩水溶液や、ケイ酸アルカリ金属塩水溶液を用
いても良いし、水酸化アルミニウムなどのアルカリ源や
ケイ酸などのシリカ源をそれぞれに水酸化アルカリ金属
塩水溶液とともに加熱処理等を施して、両溶液を調製し
ても良い。使用するアルカリは通常ナトリウムが用いら
れるがナトリウムに特に限定されるものではない。As the both aqueous solutions, a commercially available aqueous solution of alkali metal aluminate or an aqueous solution of alkali metal silicate may be used, or an alkali source such as aluminum hydroxide or a silica source such as silicic acid may be used as a hydroxide. Both solutions may be prepared by performing a heat treatment or the like together with the alkali metal salt aqueous solution. The alkali used is usually sodium, but is not particularly limited to sodium.
【００１１】アルミン酸アルカリ金属塩水溶液の濃度は
特に限定されないが、一般的にはＡｌ２Ｏ３表示で３０
重量％以下の濃度で用いられ、またケイ酸アルカリ金属
塩水溶液の濃度も特に制限はないが一般的にはＳｉＯ2
表示で３０重量％以下である。これら両水溶液は反応系
に供給されるが、アルミン酸アルカリ金属塩水溶液とケ
イ酸アルカリ金属塩水溶液の添加割合は特に限定されな
いが、極端にＳｉＯ2／Ａｌ２Ｏ３の高い無定型アルミ
ノシリケートではイオン交換性が損われ、また、極端に
低いものは、油状物質吸収性が低下するので、ＳｉＯ2
／Ａｌ2Ｏ3のモル比に換算して０．５〜１０好ましくは
１．５〜４になるように供給される。しかし、これらの
比率は本発明の必須ではない。The concentration of the alkali metal aluminate salt aqueous solution is not particularly limited, but generally it is 30 in terms of Al2O3.
The concentration of the alkali metal silicate aqueous solution is not particularly limited, but it is generally SiO 2
It is 30% by weight or less in the display. Both of these aqueous solutions are supplied to the reaction system, but the addition ratio of the aqueous alkali metal aluminate solution and the aqueous alkali metal silicate solution is not particularly limited, but in the case of amorphous aluminosilicate having extremely high SiO 2 / Al 2 O 3, ion exchangeability is high. Is impaired, and when the content is extremely low, the absorption of oily substances decreases, so SiO 2
It is supplied so as to be 0.5 to 10 preferably 1.5 to 4 in terms of the molar ratio of / Al 2 O 3 . However, these ratios are not essential to the invention.
【００１２】この時、混合後の組成が（ＯＨ-）モル／
（合成仕込み全重量）ｋｇ＝１．６モル／ｋｇ以下にな
るように予めアルミン酸アルカリ金属塩水溶液またはケ
イ酸アルカリ金属塩水溶液の水酸化物イオン濃度を水や
希薄なアルカリ溶液などを添加して希釈するかまたは反
応槽に予め必要量の水または水酸化アルカリ金属塩水様
液を添加してそれにアルミン酸アルカリ金属塩水溶液及
びケイ酸アルカリ金属塩水溶液を同時に、または別々に
供給する。この様にして反応させることによって、これ
らの混合物はやがてスラリー状になるが、（ＯＨ-）モ
ル／（合成仕込み全重量）ｋｇ＝１．６モル／ｋｇ以下
の組成で反応させてスラリー化させることが本発明では
必須である。At this time, the composition after mixing is (OH − ) mol /
(Synthetic preparation total weight) The hydroxide ion concentration of the alkali metal aluminate aqueous solution or the alkali metal silicate aqueous solution was previously added with water or a dilute alkali solution such that the total weight of the mixture was not more than 1.6 mol / kg. Or a necessary amount of water or an aqueous solution of alkali metal hydroxide is added to the reaction tank in advance and an aqueous solution of alkali metal aluminate and an aqueous solution of alkali metal silicate are simultaneously or separately supplied. By reacting in this manner, these mixtures are eventually becomes a slurry, - thereby mol / reacted with (Synthesis charged total weight) kg = 1.6 mol / kg following composition slurried (OH) Is essential in the present invention.
【００１３】反応の温度は室温以上１００℃以下の範囲
で行われる。しかし、例えば得られた無定形アルミノシ
リケートをイオン交換剤として用いる場合には比較的低
温で行うことが好ましい。反応温度が高くなるとイオン
交換性能が低下し、好ましくない。また、高い温度で反
応を行うと無定型アルミノシリケートの一部がゼオライ
ト等に結晶化し、油状物質吸収性が著しく低下する。従
って、７０℃以下の温度が好ましい。The reaction temperature is from room temperature to 100 ° C. However, when the obtained amorphous aluminosilicate is used as an ion exchange agent, it is preferable to carry out at a relatively low temperature. When the reaction temperature is high, the ion exchange performance is deteriorated, which is not preferable. Further, when the reaction is carried out at a high temperature, a part of the amorphous aluminosilicate is crystallized into zeolite or the like, and the absorbability of the oily substance is significantly lowered. Therefore, a temperature of 70 ° C. or lower is preferable.
【００１４】反応の時間は１０分〜５時間が望ましい。
あまり長時間の反応時間を設定すると、低温で合成した
場合でも結晶化が進行し、上述の様な不都合が発生す
る。The reaction time is preferably 10 minutes to 5 hours.
If the reaction time is set to be too long, crystallization will proceed even when the synthesis is performed at a low temperature, and the above-mentioned inconvenience will occur.
【００１５】この様にして得られたスラリーを必要に応
じて固液分離することで目的の性能を有する無定形アル
ミノシリケートが得られる。By subjecting the slurry thus obtained to solid-liquid separation as necessary, an amorphous aluminosilicate having the desired performance can be obtained.
【００１６】[0016]
【発明の効果】本発明の方法で無定形アルミノシリケー
トを合成すればイオン交換能２００ｍｇＣａＣＯ3／ｇ
以上かつ、油状物質吸収性が２ｃｃ／ｇ以上の性能を有
する無定形アルミノシリケートを合成することが可能に
なる。If the amorphous aluminosilicate is synthesized by the method of the present invention, the ion exchange capacity is 200 mgCaCO 3 / g.
As described above, it becomes possible to synthesize an amorphous aluminosilicate having a performance of absorbing an oily substance of 2 cc / g or more.
【００１７】[0017]
【実施例】次に、実施例で本発明をさらに詳述する。EXAMPLES Next, the present invention will be described in more detail with reference to Examples.
【００１８】実施例，比較例に於ける各測定方法は以下
の通りである。The measuring methods in the examples and comparative examples are as follows.
【００１９】イオン交換性能の測定方法 イオン交換能の測定は、塩化カルシウム水溶液（炭酸カ
ルシウム換算で５００ｍｇ／リットル）１リットルに、
無定形アルミノシリケートを無水換算で１ｇ添加し、２
５℃において１０分間攪拌した。次いで濾過により固形
分を分離した後濾液中に残存するカルシウムをＥＤＴＡ
水溶液による滴定で測定し、無定形アルミノシリケート
１ｇ（無水物）あたりのカルシウム交換量をＣａＣＯ3
に換算してもとめた。Method for Measuring Ion Exchange Performance The ion exchange performance is measured by adding 1 liter of an aqueous calcium chloride solution (500 mg / liter in terms of calcium carbonate).
Add 1 g of amorphous aluminosilicate on an anhydrous basis and add
Stir for 10 minutes at 5 ° C. Then, the solid content is separated by filtration, and the calcium remaining in the filtrate is removed by EDTA.
The amount of calcium exchanged per 1 g (anhydrous) of amorphous aluminosilicate measured by titration with an aqueous solution was CaCO 3
Even if converted to
【００２０】油状物質吸収性の測定方法 ＪＩＳ Ｋ ６２２１に基づいてアマニ油法で行った。Method for measuring absorbability of oily substance: The linseed oil method was used in accordance with JIS K6221.
【００２１】実施例１ 内容積５リットルの反応容器に水、２８９０ｇを投入
し、６５℃の温度に保ちながら、同容器にアルミン酸ナ
トリウム水溶液（Ｎａ2Ｏ＝１９．３重量％，Ａｌ2Ｏ3
＝２１．９重量％）と、ケイ酸ナトリウム水溶液（Ｎａ
2Ｏ＝４．０重量％，ＳｉＯ2＝１２．７重量％）を両液
の供給割合がＳｉＯ2／Ａｌ2Ｏ3のモル比に換算して
１．９０に成るようにそれぞれアルミン酸ナトリウム水
溶液を３５１ｇおよびケイ酸ナトリウム水溶液６８５ｇ
を同時に強く攪拌しながら、ポンプを用いて投入した。
投入の所要時間は約７分であった。投入後の水酸化物イ
オン濃度は、０．４０ｍｏｌ／ｋｇであった。また、Ｎ
ａ2Ｏ濃度は、０．３９ｍｏｌ／ｋｇ（２．４ｗｔ％）
であった。投入後５０分間攪拌を継続した。その後直ち
に得られたスラリーを濾過し、無定形アルミノシリケー
トを得た。さらにこのスラリー容積の２倍のイオン交換
水を用いて濾過器上でケーキを洗浄した。 得られたケ
ーキについて、１００℃，１５時間乾燥したものの、イ
オン交換性能及び油状物質吸収性を上記方法で測定し
た。測定の結果、それぞれ２５０ｍｇＣａＣＯ3／ｇお
よび２．４ｃｃ／ｇであった。Example 1 Water (2890 g) was placed in a reaction vessel having an internal volume of 5 liters, and while maintaining the temperature at 65 ° C., an aqueous sodium aluminate solution (Na 2 O = 19.3 wt%, Al 2 O) was placed in the vessel. 3
= 21.9% by weight) and an aqueous sodium silicate solution (Na
2 O = 4.0% by weight, SiO 2 = 12.7% by weight) so that the supply ratio of both solutions is 1.90 in terms of the molar ratio of SiO 2 / Al 2 O 3 respectively. 351 g of aqueous solution and 685 g of sodium silicate aqueous solution
While being strongly stirred at the same time, it was charged using a pump.
The time required for charging was about 7 minutes. The hydroxide ion concentration after charging was 0.40 mol / kg. Also, N
The a 2 O concentration is 0.39 mol / kg (2.4 wt%)
Met. After the addition, stirring was continued for 50 minutes. Immediately thereafter, the obtained slurry was filtered to obtain an amorphous aluminosilicate. Furthermore, the cake was washed on the filter with twice the volume of the slurry ion-exchanged water. The cake thus obtained was dried at 100 ° C. for 15 hours, and the ion exchange performance and the absorption of the oily substance were measured by the above methods. The measurement results were 250 mg CaCO 3 / g and 2.4 cc / g, respectively.
【００２２】実施例２ 内容積５リットルの反応容器に塩化ナトリウム水溶液
（Ｎａ2Ｏ＝６．６重量％）２，８９０ｇを投入し、６
５℃の温度に保ちながら、同容器に実施例１と同様の組
成をもつアルミン酸ナトリウム水溶液と、ケイ酸ナトリ
ウム水溶液をそれぞれアルミン酸ナトリウム水溶液を３
５１ｇおよびケイ酸ナトリウム水溶液６８５ｇを同時に
強く攪拌しながら、ポンプを用いて投入した。投入の所
要時間は約７分であった。投入後の水酸化物イオン濃度
は、０．４０ｍｏｌ／ｋｇであった。また、Ｎａ２Ｏ濃
度は、０．８１ｍｏｌ／ｋｇ（５．０ｗｔ％）であっ
た。投入後５０分間攪拌を継続した。その後直ちに得ら
れたスラリーを濾過し、無定形アルミノシリケートを得
た。さらにこのスラリー容積の２倍のイオン交換水を用
いて濾過器上でケーキを洗浄した。Example 2 2,890 g of an aqueous sodium chloride solution (Na 2 O = 6.6% by weight) was put into a reaction vessel having an internal volume of 5 liters to prepare 6
While keeping the temperature at 5 ° C., in the same container, an aqueous solution of sodium aluminate having the same composition as that of Example 1 and an aqueous solution of sodium silicate were respectively added to 3 aqueous solutions of sodium aluminate.
51 g and 685 g of an aqueous sodium silicate solution were simultaneously agitated with vigorous stirring. The time required for charging was about 7 minutes. The hydroxide ion concentration after charging was 0.40 mol / kg. The Na2O concentration was 0.81 mol / kg (5.0 wt%). After the addition, stirring was continued for 50 minutes. Immediately thereafter, the obtained slurry was filtered to obtain an amorphous aluminosilicate. Furthermore, the cake was washed on the filter with twice the volume of the slurry ion-exchanged water.
【００２３】得られたケーキについて、１００℃，１５
時間乾燥したものの、イオン交換性能及び油状物質吸収
性を上記方法で測定した。測定の結果、それぞれ２５１
ｍｇＣａＣＯ3／ｇおよび２．５ｃｃ／ｇであった。The cake obtained was heated at 100 ° C. for 15 minutes.
After being dried for an hour, the ion exchange performance and the absorption of oily substances were measured by the above-mentioned methods. 251 each as a result of measurement
It was mgCaCO 3 / g and 2.5 cc / g.
【００２４】実施例３ 内容積５リットルの反応容器に炭酸水素ナトリウム水溶
液（Ｎａ2Ｏ＝９．５重量％）２，８９０ｇを投入し、
６５℃の温度に保ちながら、同容器に実施例１と同様の
組成をもつアルミン酸ナトリウム水溶液と、ケイ酸ナト
リウム水溶液をそれぞれアルミン酸ナトリウム水溶液を
３５１ｇおよびケイ酸ナトリウム水溶液６８５ｇを同時
に強く攪拌しながら、ポンプを用いて投入した。投入の
所要時間は約７分であった。投入後の水酸化物イオン濃
度は、約０．００１ｍｏｌ／ｋｇであった。また、Ｎａ
2Ｏ濃度は、０．８１ｍｏｌ／ｋｇ（５．０ｗｔ％）で
あった。投入後５０分間攪拌を継続した。その後直ちに
得られたスラリーを濾過し、無定形アルミノシリケート
を得た。さらにこのスラリー容積の２倍のイオン交換水
を用いて濾過器上でケーキを洗浄した。 得られたケー
キについて、１００℃，１５時間乾燥したものの、イオ
ン交換性能及び油状物質吸収性を上記方法で測定した。
測定の結果、それぞれ２７３ｍｇＣａＣＯ3／ｇおよび
２．８ｃｃ／ｇであった。Example 3 2,890 g of an aqueous sodium hydrogen carbonate solution (Na 2 O = 9.5% by weight) was placed in a reaction vessel having an internal volume of 5 liters,
While maintaining the temperature at 65 ° C., 351 g of sodium aluminate aqueous solution and 351 g of sodium aluminate aqueous solution and 685 g of sodium silicate aqueous solution were stirred in the same container at the same time while vigorously stirring. , Using a pump. The time required for charging was about 7 minutes. The hydroxide ion concentration after the addition was about 0.001 mol / kg. In addition, Na
The 2 O concentration was 0.81 mol / kg (5.0 wt%). After the addition, stirring was continued for 50 minutes. Immediately thereafter, the obtained slurry was filtered to obtain an amorphous aluminosilicate. Furthermore, the cake was washed on the filter with twice the volume of the slurry ion-exchanged water. The cake thus obtained was dried at 100 ° C. for 15 hours, and the ion exchange performance and the absorption of the oily substance were measured by the above methods.
The measurement results were 273 mg CaCO 3 / g and 2.8 cc / g, respectively.
【００２５】実施例４ 内容積５リットルの反応容器に炭酸ナトリウム水溶液
（Ｎａ2Ｏ＝４．９重量％）２，８９０ｇを投入し、６
５℃の温度に保ちながら、同容器に実施例１と同様の組
成をもつアルミン酸ナトリウム水溶液と、ケイ酸ナトリ
ウム水溶液をそれぞれアルミン酸ナトリウム水溶液を３
５１ｇおよびケイ酸ナトリウム水溶液６８５ｇを同時に
強く攪拌しながら、ポンプを用いて投入した。投入の所
要時間は約７分であった。投入後の水酸化物イオン濃度
は、約０．４０ｍｏｌ／ｋｇであった。また、Ｎａ2Ｏ
濃度は、０．８１ｍｏｌ／ｋｇ５．０ｗｔ％）であっ
た。投入後５０分間攪拌を継続した。その後直ちに得ら
れたスラリーを濾過し、無定形アルミノシリケートを得
た。さらにこのスラリー容積の２倍のイオン交換水を用
いて濾過器上でケーキを洗浄した。Example 4 2,890 g of an aqueous sodium carbonate solution (Na 2 O = 4.9% by weight) was put into a reaction vessel having an internal volume of 5 liters, and 6
While keeping the temperature at 5 ° C., in the same container, an aqueous solution of sodium aluminate having the same composition as that of Example 1 and an aqueous solution of sodium silicate were respectively added to 3 aqueous solutions of sodium aluminate.
51 g and 685 g of an aqueous sodium silicate solution were simultaneously agitated with vigorous stirring. The time required for charging was about 7 minutes. The hydroxide ion concentration after the addition was about 0.40 mol / kg. Also, Na 2 O
The concentration was 0.81 mol / kg 5.0 wt%). After the addition, stirring was continued for 50 minutes. Immediately thereafter, the obtained slurry was filtered to obtain an amorphous aluminosilicate. Furthermore, the cake was washed on the filter with twice the volume of the slurry ion-exchanged water.
【００２６】得られたケーキについて、１００℃，１５
時間乾燥したものの、イオン交換性能及び油状物質吸収
性を上記方法で測定した。測定の結果、それぞれ２６０
ｍｇＣａＣＯ3／ｇおよび２．４ｃｃ／ｇであった。The obtained cake was heated at 100 ° C. for 15 minutes.
After being dried for an hour, the ion exchange performance and the absorption of oily substances were measured by the above-mentioned methods. As a result of measurement, 260 each
It was mgCaCO 3 / g and 2.4 cc / g.
【００２７】実施例５ 内容積５リットルの反応容器に水酸化ナトリウム水溶液
（Ｎａ2Ｏ＝６．５重量％）２，８９０ｇを投入し、６
５℃の温度に保ちながら、同容器にアルミン酸ナトリウ
ム水溶液（Ｎａ2Ｏ＝１９．３重量％，Ａｌ2Ｏ3＝２
１．９重量％）と、ケイ酸ナトリウム水溶液（Ｎａ2Ｏ
＝４．０重量％，ＳｉＯ2＝１２．７重量％）を両液の
供給割合がＳｉＯ2／Ａｌ2Ｏ3のモル比に換算して１．
９０に成るようにそれぞれアルミン酸ナトリウム水溶液
を３５１ｇおよびケイ酸ナトリウム水溶液６８５ｇを同
時に強く攪拌しながら、ポンプを用いて投入した。投入
の所要時間は約７分であった。投入後の水酸化物イオン
濃度は、１．２３ｍｏｌ／ｋｇであった。また、Ｎａ2
Ｏ濃度は、０．８１ｍｏｌ／ｋｇ（５．０ｗｔ％）であ
った。投入後５０分間攪拌を継続した。その後直ちに得
られたスラリーを濾過し、無定形アルミノシリケートを
得た。さらにこのスラリー容積の２倍のイオン交換水を
用いて濾過器上でケーキを洗浄した。Example 5 2,890 g of an aqueous sodium hydroxide solution (Na 2 O = 6.5% by weight) was placed in a reaction vessel having an internal volume of 5 liters, and 6
While maintaining the temperature at 5 ° C, an aqueous solution of sodium aluminate (Na 2 O = 19.3% by weight, Al 2 O 3 = 2) was placed in the same container.
1.9% by weight) and an aqueous sodium silicate solution (Na 2 O
= 4.0% by weight, SiO 2 = 12.7% by weight), and the supply ratio of both solutions is converted to a SiO 2 / Al 2 O 3 molar ratio of 1.
351 g of the sodium aluminate aqueous solution and 685 g of the sodium silicate aqueous solution were simultaneously stirred strongly so as to be 90, and were introduced by using a pump. The time required for charging was about 7 minutes. The hydroxide ion concentration after the addition was 1.23 mol / kg. In addition, Na 2
The O concentration was 0.81 mol / kg (5.0 wt%). After the addition, stirring was continued for 50 minutes. Immediately thereafter, the obtained slurry was filtered to obtain an amorphous aluminosilicate. Furthermore, the cake was washed on the filter with twice the volume of the slurry ion-exchanged water.
【００２８】得られたケーキについて、１００℃，１５
時間乾燥したものの、イオン交換性能及び油状物質吸収
性を上記方法で測定した。測定の結果、それぞれ２０５
ｍｇＣａＣＯ3／ｇおよび２．１ｃｃ／ｇであった。The cake obtained was heated at 100 ° C. for 15 minutes.
After being dried for an hour, the ion exchange performance and the absorption of oily substances were measured by the above-mentioned methods. 205 of each measurement result
It was mgCaCO 3 / g and 2.1 cc / g.
【００２９】実施例６ 内容積５リットルの反応容器に水酸化ナトリウム水溶液
（Ｎａ2Ｏ＝６．５重量％）１６８ｇを投入し、６５℃
の温度に保ちながら、同容器にアルミン酸ナトリウム水
溶液（Ｎａ2Ｏ＝１９．３重量％，Ａｌ2Ｏ3＝２１．９
重量％）と、ケイ酸ナトリウム水溶液Ｎａ2Ｏ＝４．０
重量％，ＳｉＯ2＝１２．７重量％）を両液の供給割合
がＳｉＯ2／Ａｌ2Ｏ3のモル比に換算して１．９０に成
るようにそれぞれアルミン酸ナトリウム水溶液を３５１
ｇおよびケイ酸ナトリウム水溶液６８５ｇを同時に強く
攪拌しながら、ポンプを用いて投入した。投入の所要時
間は約７分であった。投入後の水酸化物イオン濃度は、
１．５９ｍｏｌ／ｋｇであった。また、Ｎａ2Ｏ濃度
は、１．４２ｍｏｌ／ｋｇ（８．８ｗｔ％）であった。
投入後５０分間攪拌を継続した。その後直ちに得られた
スラリーを濾過し、無定形アルミノシリケートを得た。
さらにこのスラリー容積の２倍のイオン交換水を用いて
濾過器上でケーキを洗浄した。Example 6 168 g of an aqueous sodium hydroxide solution (Na 2 O = 6.5% by weight) was placed in a reaction vessel having an internal volume of 5 liters, and the temperature was 65 ° C.
While maintaining the temperature of the above, an aqueous solution of sodium aluminate (Na 2 O = 19.3 wt%, Al 2 O 3 = 21.9) was placed in the same container.
Wt%) and sodium silicate aqueous solution Na 2 O = 4.0
% By weight, and SiO 2 = 12.7% by weight), so that the supply ratio of both solutions is 1.90 in terms of the molar ratio of SiO 2 / Al 2 O 3 so that each of the aqueous solutions of sodium aluminate is 351.
g and 685 g of sodium silicate aqueous solution were simultaneously stirred with vigorous stirring, and charged with a pump. The time required for charging was about 7 minutes. The hydroxide ion concentration after charging is
It was 1.59 mol / kg. The Na 2 O concentration was 1.42 mol / kg (8.8 wt%).
After the addition, stirring was continued for 50 minutes. Immediately thereafter, the obtained slurry was filtered to obtain an amorphous aluminosilicate.
Furthermore, the cake was washed on the filter with twice the volume of the slurry ion-exchanged water.
【００３０】得られたケーキについて、１００℃，１５
時間乾燥したものの、イオン交換性能及び油状物質吸収
性を上記方法で測定した。測定の結果、それぞれ２０２
ｍｇＣａＣＯ3／ｇおよび２．１ｃｃ／ｇであった。The cake obtained was heated at 100 ° C. for 15 minutes.
After being dried for an hour, the ion exchange performance and the absorption of oily substances were measured by the above-mentioned methods. The result of the measurement is 202
It was mgCaCO 3 / g and 2.1 cc / g.
【００３１】比較例１ 内容積５リットルの反応容器に水酸化ナトリウム水溶液
（Ｎａ2Ｏ＝６．５重量％）２，８９０ｇを投入し、６
５℃の温度に保ちながら、同容器に比較例１と同じ組成
をもつアルミン酸ナトリウム水溶液と、ケイ酸ナトリウ
ム水溶液をそれぞれ３５１ｇおよび６８５ｇを同時に強
く攪拌しながら、ポンプを用いて投入した。投入の所要
時間は約７分であった。投入後の水酸化物イオン濃度
は、１．９４ｍｏｌ／ｋｇであった。また、Ｎａ2Ｏ濃
度は、１．１６ｍｏｌ／ｋｇ（７．２ｗｔ％）であっ
た。投入後５０分間攪拌を継続した。その後直ちに得ら
れたスラリーを濾過し、無定形アルミノシリケートを得
た。さらにこのスラリー容積の２倍のイオン交換水を用
いて濾過器上でケーキを洗浄した。Comparative Example 1 2,890 g of an aqueous sodium hydroxide solution (Na 2 O = 6.5% by weight) was placed in a reaction vessel having an internal volume of 5 liters, and 6
While maintaining the temperature at 5 ° C., 351 g and 685 g of an aqueous solution of sodium aluminate and an aqueous solution of sodium silicate having the same composition as in Comparative Example 1 were simultaneously poured into the container by using a pump while vigorously stirring. The time required for charging was about 7 minutes. The hydroxide ion concentration after the addition was 1.94 mol / kg. The Na 2 O concentration was 1.16 mol / kg (7.2 wt%). After the addition, stirring was continued for 50 minutes. Immediately thereafter, the obtained slurry was filtered to obtain an amorphous aluminosilicate. Furthermore, the cake was washed on the filter with twice the volume of the slurry ion-exchanged water.
【００３２】得られたケーキについて、１００℃，１５
時間乾燥したものの、イオン交換性能及び油状物質吸収
性を上記方法で測定した。測定の結果、それぞれ３７ｍ
ｇＣａＣＯ3／ｇおよび１．２ｃｃ／ｇであった。The obtained cake was heated at 100 ° C. for 15 minutes.
After being dried for an hour, the ion exchange performance and the absorption of oily substances were measured by the above-mentioned methods. As a result of measurement, each is 37m
It was gCaCO 3 / g and 1.2 cc / g.
【００３３】比較例２ 内容積５リットルの反応容器に水酸化ナトリウム水溶液
（Ｎａ2Ｏ＝１９．５重量％）１６８ｇを投入し、６５
℃の温度に保ちながら、同容器に比較例１と同じ組成を
もつアルミン酸ナトリウム水溶液と、ケイ酸ナトリウム
水溶液をそれぞれ３５１ｇおよび６８５ｇを同時に強く
攪拌しながら、ポンプを用いて投入した。投入の所要時
間は約７分であった。投入後の水酸化物イオン濃度は、
２．１８ｍｏｌ／ｋｇであった。また、Ｎａ2Ｏ濃度
は、１．７１ｍｏｌ／ｋｇ（１０．６ｗｔ％）であっ
た。投入後５０分間攪拌を継続した。その後直ちに得ら
れたスラリーを濾過し、無定形アルミノシリケートを得
た。さらにこのスラリー容積の２倍のイオン交換水を用
いて濾過器上でケーキを洗浄した。Comparative Example 2 A reaction vessel having an internal volume of 5 liters was charged with 168 g of an aqueous sodium hydroxide solution (Na 2 O = 19.5% by weight) and charged to 65
While keeping the temperature at 0 ° C., 351 g and 685 g of an aqueous solution of sodium aluminate and an aqueous solution of sodium silicate having the same composition as in Comparative Example 1 were simultaneously poured into the container by using a pump while vigorously stirring. The time required for charging was about 7 minutes. The hydroxide ion concentration after charging is
It was 2.18 mol / kg. The Na 2 O concentration was 1.71 mol / kg (10.6 wt%). After the addition, stirring was continued for 50 minutes. Immediately thereafter, the obtained slurry was filtered to obtain an amorphous aluminosilicate. Furthermore, the cake was washed on the filter with twice the volume of the slurry ion-exchanged water.
【００３４】得られたケーキについて、１００℃，１５
時間乾燥したものの、イオン交換性能及び油状物質吸収
性を上記方法で測定した。測定の結果、それぞれ３３ｍ
ｇＣａＣＯ3／ｇおよび１．３ｃｃ／ｇであった。The obtained cake was heated at 100 ° C. for 15 minutes.
After being dried for an hour, the ion exchange performance and the absorption of oily substances were measured by the above-mentioned methods. 33m each as a result of measurement
It was gCaCO 3 / g and 1.3 cc / g.
Claims (1)
酸アルカリ金属塩の水溶液を連続的又は回分式に混合す
ることによって無定形アルミノシリケートを製造する方
法において、反応系に含まれる水酸化物イオン濃度が、
１．６ｍｏｌ／ｋｇ以下であることを特徴とする無定形
アルミノシリケートの製造法。1. A method for producing an amorphous aluminosilicate by continuously or batchwise mixing an aqueous solution of an alkali metal aluminate and an aqueous solution of an alkali metal silicate, wherein a hydroxide ion contained in a reaction system is used. Concentration
A method for producing an amorphous aluminosilicate, which is 1.6 mol / kg or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP205793A JPH06206721A (en) | 1993-01-08 | 1993-01-08 | Production of amorphous aluminosilicate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP205793A JPH06206721A (en) | 1993-01-08 | 1993-01-08 | Production of amorphous aluminosilicate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH06206721A true JPH06206721A (en) | 1994-07-26 |
Family
ID=11518712
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP205793A Pending JPH06206721A (en) | 1993-01-08 | 1993-01-08 | Production of amorphous aluminosilicate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06206721A (en) |
-
1993
- 1993-01-08 JP JP205793A patent/JPH06206721A/en active Pending
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