JP2009227484A - Method for producing lithium-type zeolite - Google Patents

Method for producing lithium-type zeolite Download PDF

Info

Publication number
JP2009227484A
JP2009227484A JP2008072014A JP2008072014A JP2009227484A JP 2009227484 A JP2009227484 A JP 2009227484A JP 2008072014 A JP2008072014 A JP 2008072014A JP 2008072014 A JP2008072014 A JP 2008072014A JP 2009227484 A JP2009227484 A JP 2009227484A
Authority
JP
Japan
Prior art keywords
lithium
zeolite
producing
type zeolite
aqueous solution
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.)
Granted
Application number
JP2008072014A
Other languages
Japanese (ja)
Other versions
JP5594710B2 (en
Inventor
Kiyoshi Mizuno
清 水野
Motoki Uehara
元樹 上原
Taiji Matsumoto
泰治 松本
Yoshiaki Goto
義昭 後藤
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.)
Tochigi Prefecture
Railway Technical Research Institute
Ryukoku University
Original Assignee
Tochigi Prefecture
Railway Technical Research Institute
Ryukoku University
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 Tochigi Prefecture, Railway Technical Research Institute, Ryukoku University filed Critical Tochigi Prefecture
Priority to JP2008072014A priority Critical patent/JP5594710B2/en
Publication of JP2009227484A publication Critical patent/JP2009227484A/en
Application granted granted Critical
Publication of JP5594710B2 publication Critical patent/JP5594710B2/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for producing a lithium-type zeolite by which the lithium-type zeolite can be produced at a synthesis temperature in a range of 20-50°C, in such a very low lithium hydroxide, that is, alkali concentration as 1 M (1 mol) and in a short synthesis time. <P>SOLUTION: The method for producing the lithium-type zeolite comprises adding an aqueous lithium hydroxide solution to metakaolin obtained by firing and activating kaolinite which is a natural clay mineral, and bringing those into a reaction at a low temperature of 20-50°C, whereby the lithium-type zeolite is produced in a low alkali concentration and in a short synthesis time. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

本発明は、天然カオリナイトを焼成したメタカリオンを使用した、リチウム型ゼオライトの製造方法に係り、特に、アルカリ骨材反応を抑制するコンクリート材料に適するリチウム型ゼオライトの製造方法に関するものである。   The present invention relates to a method for producing a lithium type zeolite using metakalion obtained by calcining natural kaolinite, and more particularly to a method for producing a lithium type zeolite suitable for a concrete material that suppresses alkali aggregate reaction.

アルカリ骨材反応とは、コンクリート中の骨材の特定の鉱物とアルカリ性細孔溶液との間の化学反応によって、局部的な容積膨張が生じ、コンクリートにひび割れを生じさせるとともに、強度低下あるいは弾性の低下という物性の変化が生じる現象であり、道路・橋梁・トンネル・ビル等のコンクリート構造物の崩壊をもたらすことから社会的な問題となっている。この対策として、リチウム型ゼオライトがアルカリ骨材反応抑制に有効なことが報告されている。   Alkali-aggregate reaction refers to local volume expansion caused by a chemical reaction between a specific mineral of aggregate in the concrete and the alkaline pore solution, causing cracks in the concrete and reducing strength or elasticity. This is a phenomenon that causes a change in physical properties, such as a decline, and it is a social problem because it causes the collapse of concrete structures such as roads, bridges, tunnels, and buildings. As a countermeasure, it has been reported that lithium-type zeolite is effective in suppressing alkali-aggregate reaction.

かかるリチウム型ゼオライトはこれまでに、ABWゼオライトやEDIゼオライトなどの合成が報告されている(下記非特許文献1〜4参照)が、これらを製造するためには、アルミナゾル、シリカゾル、水酸化リチウムから調製したゲル、あるいは天然の粘土鉱物であるカオリナイトを焼成し活性化したメタカオリンあるいは天然粘土鉱物であるアロフェンに水酸化リチウム水溶液を加え、60℃〜200℃程度の高温条件下で合成された。あるいは、リチウム以外の金属を含むゼオライト(例えば、ナトリウム型ゼオライトA)を塩化リチウムなどのリチウム塩溶液中でイオン交換処理を数回繰り返した後、塩化物イオンを洗浄することにより製造されていた(下記特許文献1参照)。
特開平11−226429号 「アルミナゾル、シリカゾル、水酸化リチウムからのリチウム型EDIゼオライトの合成方法」,T.Matsumoto,T.Miyazaki,and Y.Goto:J.Eur.Ceram.Soc., 26,455−458,(2006) 「メタカオリンからのLi型ABWゼオライトの合成方法」,R.Barrer,and D.E.Mainwaring:J.Chem.Soc.Dalton.,1972,2534−2546,(1972) 「カオリナイトからのLi型ABWゼオライトの合成方法」,A.A.Kosorukov,L.G.Nadel,and A.S.Chirkov,Russian J.lnorg.Chem. ,31,503,(1986) 「アロフェンからのリチウム型ABWゼオライトとリチウム型EDIゼオライトの合成方法」,興野雄亮、吉葉光雄、星佳宏、磯文夫,渡辺雄二郎、小松優、守吉佑介、無機マテリアル学会第112回学術講演会要旨集、p.8−9、(2006)
So far, such lithium-type zeolite has been reported to be synthesized such as ABW zeolite and EDI zeolite (see Non-Patent Documents 1 to 4 below). In order to produce these, alumina sol, silica sol, lithium hydroxide is used. A lithium hydroxide aqueous solution was added to the prepared gel or metakaolin obtained by calcination and activation of kaolinite, which is a natural clay mineral, or allophane, which was a natural clay mineral, and synthesized under a high temperature condition of about 60 ° C to 200 ° C. Alternatively, a zeolite containing a metal other than lithium (for example, sodium-type zeolite A) was produced by repeating ion exchange treatment several times in a lithium salt solution such as lithium chloride and then washing chloride ions ( See Patent Document 1 below).
JP-A-11-226429 “Method for synthesizing lithium-type EDI zeolite from alumina sol, silica sol and lithium hydroxide”, T.W. Matsumoto, T .; Miyazaki, and Y.M. Goto: J.M. Eur. Ceram. Soc. , 26, 455-458, (2006) “Synthesis of Li-type ABW zeolite from metakaolin”, R.A. Barrer, and D.B. E. Mainwaring: J.M. Chem. Soc. Dalton. , 1972, 2534-2546, (1972) “Synthesis of Li-type ABW zeolite from kaolinite”, A. A. Kosorukov, L.M. G. Nadel, and A.M. S. Kirkov, Russian J. et al. lorg. Chem., 31, 503, (1986) "Synthesis of Lithium-type ABW Zeolite and Lithium-Type EDI Zeolite from Allophane", Yusuke Okino, Mitsuo Yoshiba, Yoshihiro Hoshi, Fumio Tsuji, Yujiro Watanabe, Yu Komatsu, Yusuke Moriyoshi, Abstracts of the 112th Annual Meeting of the Society of Inorganic Materials Shu, p. 8-9, (2006)

しかしながら、従来のリチウム型ゼオライトの製造方法は、合成法においては高温条件下にすることが必要であり、イオン交換法においてはイオン交換操作の回数が多いため、コストが高いという問題があった。   However, the conventional method for producing lithium zeolite requires a high temperature condition in the synthesis method, and in the ion exchange method, the number of ion exchange operations is large.

また、リチウム型に限らず、ゼオライトの合成温度は80℃以上の報告が殆どであり、20℃〜50℃でのゼオライトの合成例は数少なく、それも極めて高いアルカリ濃度が必要か、あるいは合成時間が数カ月かち数年という極めて長くかかることから、工業的には現実的でないとされていた。   Moreover, not only the lithium type, the synthesis temperature of zeolite is mostly reported to be 80 ° C. or higher, and there are few examples of zeolite synthesis at 20 ° C. to 50 ° C., which also requires a very high alkali concentration, or the synthesis time. However, it took a very long time of several months to several years, so it was considered unrealistic industrially.

本発明は、上記状況に鑑みて、合成温度が20℃〜50℃の範囲で、しかも水酸化リチウムのアルカリ濃度が1M(1モル)と極めて希薄な濃度であり、短い合成時間で製造することができるリチウム型ゼオライトの製造方法を提供することを目的とする。   In view of the above situation, the present invention is manufactured in a short synthesis time with a synthesis temperature in the range of 20 ° C. to 50 ° C. and an alkali concentration of lithium hydroxide of 1M (1 mol). An object of the present invention is to provide a method for producing a lithium-type zeolite that can be used.

本発明は、上記目的を達成するために、
〔1〕リチウム型ゼオライトの製造方法において、天然の粘土鉱物であるカオリナイトを焼成し活性化したメタカオリンに水酸化リチウム水溶液を加え、20℃〜50℃の低温下の反応によって、アルカリ濃度が低く、しかも短い合成時間でリチウム型ゼオライトを製造することを特徴とする。
In order to achieve the above object, the present invention provides
[1] In a method for producing lithium zeolite, an aqueous lithium hydroxide solution is added to metakaolin obtained by calcining and activating kaolinite, a natural clay mineral, and the alkali concentration is lowered by a reaction at a low temperature of 20 ° C to 50 ° C. Moreover, it is characterized in that lithium zeolite is produced in a short synthesis time.

〔2〕上記〔1〕記載のリチウム型ゼオライトの製造方法において、前記メタカオリン1に対して、10倍量の1M(モル)水酸化リチウム水溶液を加えることを特徴とする。   [2] The method for producing a lithium zeolite according to [1] above, wherein 10 times the amount of 1M (mol) lithium hydroxide aqueous solution is added to the metakaolin 1.

〔3〕上記〔1〕又は〔2〕記載のリチウム型ゼオライトの製造方法において、前記水酸化リチウム水溶液を20℃〜50℃に調整した雰囲気中で24時間から120時間保持することを特徴とする。   [3] The method for producing a lithium zeolite according to [1] or [2], wherein the lithium hydroxide aqueous solution is maintained in an atmosphere adjusted to 20 ° C. to 50 ° C. for 24 hours to 120 hours. .

〔4〕上記〔1〕、〔2〕又は〔3〕記載のリチウム型ゼオライトの製造方法において、前記メタカオリン1に対して10倍量の1M(モル)水酸化リチウム水溶液を加え、密閉容器に入れ、この密閉容器を20℃〜50℃に調整した雰囲気中で24時間から120時間保持し、該保持時間が経過した後、得られた沈殿物を常温でろ過・洗浄・乾燥し、白色粉末からなるリチウム型ゼオライトを得ることを特徴とする。   [4] In the method for producing a lithium-type zeolite described in [1], [2] or [3] above, 10 times the amount of 1M (mol) lithium hydroxide aqueous solution is added to the metakaolin 1, and the mixture is placed in a sealed container. The sealed container is held in an atmosphere adjusted to 20 ° C. to 50 ° C. for 24 to 120 hours, and after the holding time has elapsed, the resulting precipitate is filtered, washed and dried at room temperature to obtain a white powder. A lithium type zeolite is obtained.

本発明によれば、次のような効果を奏することができる。   According to the present invention, the following effects can be achieved.

(1)20℃〜50℃という極めて低温でリチウム型ゼオライトが合成できる。   (1) Lithium-type zeolite can be synthesized at an extremely low temperature of 20 ° C to 50 ° C.

(2)メタカオリンは安価(100〜150円/kg)であり、合成コストが低い。   (2) Metakaolin is inexpensive (100 to 150 yen / kg) and the synthesis cost is low.

(3)メタカオリンは鉄等の着色不純物が極めて少ないため、白色度の高い、リチウム型ゼオライトが得られる。   (3) Since metakaolin has very little colored impurities such as iron, a lithium zeolite with high whiteness can be obtained.

本発明のリチウム型ゼオライトの製造方法は、天然の粘土鉱物であるカオリナイトを焼成し活性化したメタカオリンに水酸化リチウム水溶液を加え、20℃〜50℃の低温下の反応によって、リチウム型ゼオライトを製造する。   According to the method for producing a lithium zeolite of the present invention, a lithium hydroxide aqueous solution is added to metakaolin obtained by calcining and activating kaolinite, which is a natural clay mineral, and a reaction at a low temperature of 20 ° C. to 50 ° C. To manufacture.

以下、本発明の実施の形態について詳細に説明する。   Hereinafter, embodiments of the present invention will be described in detail.

本発明のリチウム型ゼオライトの製造方法は、天然の粘土鉱物であるカオリナイトを焼成し活性化したメタカオリンに水酸化リチウム水溶液を加え、20℃〜50℃の低温下の反応によって、リチウム型ゼオライトを製造する。   According to the method for producing a lithium zeolite of the present invention, a lithium hydroxide aqueous solution is added to metakaolin obtained by calcining and activating kaolinite, which is a natural clay mineral, and a reaction at a low temperature of 20 ° C. to 50 ° C. To manufacture.

図1は本発明の実施例に係るリチウム型ゼオライトの製造装置を示す図、図2は本発明の実施例のリチウム型ゼオライトの製造方法を示すフローチャートである。   FIG. 1 is a diagram showing an apparatus for producing a lithium zeolite according to an embodiment of the present invention, and FIG. 2 is a flowchart showing a method for producing a lithium zeolite according to an embodiment of the present invention.

図1において、1は密閉容器、2は密閉容器1内の沈殿物、3は電子制御装置、4は制御部、5は温度調整装置、6は計時装置、7は沈殿物2の排出口、7Aは電磁開閉弁、8はろ過・洗浄・乾燥処理装置、8Aは送出装置、9はろ過・洗浄・乾燥処理装置8の排出口、9はそのろ過・洗浄・乾燥処理装置8の排出口、10は排出口9から得られた白色粉末である。   In FIG. 1, 1 is an airtight container, 2 is a deposit in the airtight container 1, 3 is an electronic control device, 4 is a control unit, 5 is a temperature adjusting device, 6 is a timing device, 7 is an outlet for the precipitate 2, 7A is an electromagnetic on-off valve, 8 is a filtration / cleaning / drying processing device, 8A is a delivery device, 9 is an outlet of the filtration / cleaning / drying processing device 8, 9 is an outlet of the filtration / cleaning / drying processing device 8, Reference numeral 10 denotes a white powder obtained from the discharge port 9.

以下、リチウム型ゼオライトの製造方法について図2に示すフローチャートを参照しながら説明する。   Hereinafter, a method for producing lithium zeolite will be described with reference to the flowchart shown in FIG.

(1)まず、天然カオリナイトを焼成したメタカオリン(モル)1に対し、10倍量の水酸化リチウム(モル)の水溶液を、密閉容器1中で混合する(ステップS1)。   (1) First, 10 times the amount of lithium hydroxide (mol) aqueous solution is mixed in the closed container 1 with respect to metakaolin (mol) 1 obtained by firing natural kaolinite (step S1).

(2)この密閉容器1を温度調整装置5により20℃〜50℃に調整した雰囲気中で計時装置6で監視して24時間から120時間保持する(ステップS2)。   (2) The airtight container 1 is monitored by the time measuring device 6 in an atmosphere adjusted to 20 ° C. to 50 ° C. by the temperature adjusting device 5 and held for 24 to 120 hours (step S2).

(3)再び、天然カオリナイトを焼成したメタカオリン(モル)1に対し、10倍量の水酸化リチウム(モル)の水溶液を、密閉容器1中で混合する(ステップS3)。   (3) Again, an aqueous solution of 10 times the amount of lithium hydroxide (mol) is mixed in the closed container 1 with respect to metakaolin (mol) 1 obtained by firing natural kaolinite (step S3).

(4)所定の時間が経過した後、得られた沈殿物2をろ過・洗浄・乾燥処理装置8において常温でろ過・洗浄・乾燥する(ステップS4)。   (4) After a predetermined time has elapsed, the obtained precipitate 2 is filtered, washed and dried at room temperature in the filtration / washing / drying processing apparatus 8 (step S4).

(5)回収水酸化リチウム水溶液+未使用水酸化リチウム水溶液を再利用する(ステップS5)。   (5) The recovered lithium hydroxide aqueous solution + unused lithium hydroxide aqueous solution is reused (step S5).

(6)ステップS4により、白色粉末10が得られる(ステップS6)。   (6) The white powder 10 is obtained by step S4 (step S6).

このようにした製造された白色粉末10を、X線回折法により回折した結果、リチウム型ゼオライト(Li−EDI、Li−EDI+Li−ABW)であることを確認できた。   As a result of diffracting the produced white powder 10 by the X-ray diffraction method, it was confirmed that it was a lithium type zeolite (Li-EDI, Li-EDI + Li-ABW).

かかるリチウム型ゼオライトは、アルカリイオン捕集機能を有し、リチウムイオンの効果と相まってアルカリ骨材反応を抑制する材料(例えば、コンクリート材料)として好適である。
〔実施例1〕
メタカオリン1gに対し、1M(モル)の水酸化リチウム水溶液10mlを加え、テフロン(登録商標)性の密閉容器内で、30℃、24時間反応を行った。反応後、生成物を蒸留水で洗浄し、乾燥した。得られた生成物をX線回折により調べた結果、リチウム型EDIゼオライトの生成を確認した。
〔実施例2〕
メタカオリン1gに対し、1M(モル)の水酸化リチウム水溶液10mlを加え、テフロン(登録商標)性の密閉容器内で、50℃、120時間反応を行った。反応後、生成物を蒸留水で洗浄し、乾燥した。得られた生成物をX線回折により調べた結果、リチウム型ABWゼオライトとリチウム型EDIゼオライトの混合物であることを確認した。
Such lithium-type zeolite has an alkali ion collecting function and is suitable as a material (for example, a concrete material) that suppresses the alkali aggregate reaction in combination with the effect of lithium ions.
[Example 1]
To 1 g of metakaolin, 10 ml of a 1M (mol) lithium hydroxide aqueous solution was added, and the reaction was performed at 30 ° C. for 24 hours in a Teflon (registered trademark) sealed container. After the reaction, the product was washed with distilled water and dried. As a result of examining the obtained product by X-ray diffraction, it was confirmed that lithium type EDI zeolite was produced.
[Example 2]
To 1 g of metakaolin, 10 ml of a 1M (mol) lithium hydroxide aqueous solution was added, and the reaction was carried out at 50 ° C. for 120 hours in a Teflon (registered trademark) sealed container. After the reaction, the product was washed with distilled water and dried. As a result of examining the obtained product by X-ray diffraction, it was confirmed that it was a mixture of lithium ABW zeolite and lithium EDI zeolite.

これまでカオリナイトもしくはメタカオリンを原料とした、リチウム型ゼオライトの合成例において、EDIゼオライトは報告されておらず、本発明において初めてリチウム型EDIゼオライトの合成に成功した。また、その合成温度は、これまで化成原料(アルミナゾル、シリカゾル)やアロフェンからのEDIゼオライトの合成温度である60〜100℃よりも極めて低い、20℃〜50℃である。   So far, no EDI zeolite has been reported in the synthesis examples of lithium zeolite using kaolinite or metakaolin as a raw material, and for the first time in the present invention, lithium type EDI zeolite was successfully synthesized. The synthesis temperature is 20 ° C. to 50 ° C., which is much lower than 60 to 100 ° C., which is the synthesis temperature of EDI zeolite from chemical raw materials (alumina sol, silica sol) and allophane.

また、本発明ではリチウム型ABWゼオライトとリチウム型EDIゼオライトの混合物も得られているが、ABWゼオライトの合成温度に関しても、従来報告されている80℃〜200℃と比較して低い合成温度に成功している。   In the present invention, a mixture of lithium-type ABW zeolite and lithium-type EDI zeolite was also obtained, but the synthesis temperature of ABW zeolite was also successful at a low synthesis temperature compared to 80 ° C. to 200 ° C. reported conventionally. is doing.

このように、本発明によれば、天然カオリナイトを焼成したメタカオリンを使用して、これまでより安価にリチウム型ゼオライトを製造する条件を見出した。また、イオン種の異なるゼオライトを使用して煩雑なイオン交換、洗浄を繰り返す必要もない。   Thus, according to the present invention, the present inventors have found conditions for producing lithium-type zeolite at a lower cost than before by using metakaolin obtained by calcining natural kaolinite. Further, it is not necessary to repeat complicated ion exchange and washing using zeolites having different ionic species.

なお、本発明は上記実施例に限定されるものではなく、本発明の趣旨に基づいて種々の変形が可能であり、これらを本発明の範囲から排除するものではない。   In addition, this invention is not limited to the said Example, A various deformation | transformation is possible based on the meaning of this invention, and these are not excluded from the scope of the present invention.

本発明のリチウム型ゼオライトの製造方法は、安価にしかも容易にアルカリ骨材反応を抑制するコンクリート材料に適するリチウム型ゼオライトの製造を行うために利用することができる。   The method for producing a lithium-type zeolite of the present invention can be used for producing a lithium-type zeolite suitable for a concrete material that can easily inhibit the alkali-aggregate reaction at low cost.

本発明の実施例に係るリチウム型ゼオライトの製造装置を示す図である。It is a figure which shows the manufacturing apparatus of the lithium type zeolite which concerns on the Example of this invention. 本発明の実施例のリチウム型ゼオライトの製造方法を示すフローチャートである。It is a flowchart which shows the manufacturing method of the lithium type zeolite of the Example of this invention.

符号の説明Explanation of symbols

1 密閉容器
2 密閉容器内の沈殿物
3 電子制御装置
4 制御部
5 温度調整装置
6 計時装置
7 沈殿物の排出口
7A 電磁開閉弁
8 ろ過・洗浄・乾燥処理装置
8A 送出装置
9 ろ過・洗浄・乾燥処理装置の排出口
10 白色粉末
DESCRIPTION OF SYMBOLS 1 Airtight container 2 Precipitate in airtight container 3 Electronic control device 4 Control part 5 Temperature control device 6 Timekeeping device 7 Precipitate discharge port 7A Electromagnetic on-off valve 8 Filtration / washing / drying processing device 8A Delivery device 9 Filtration / washing / Drying equipment discharge port 10 White powder

Claims (4)

天然の粘土鉱物であるカオリナイトを焼成し活性化したメタカオリンに水酸化リチウム水溶液を加え、20℃〜50℃の低温下の反応によって、アルカリ濃度が低く、しかも短い合成時間でリチウム型ゼオライトを製造することを特徴とするリチウム型ゼオライトの製造方法。   Lithium zeolite aqueous solution is produced by adding lithium hydroxide aqueous solution to metakaolin activated by calcining kaolinite, a natural clay mineral, and reacting at low temperatures of 20 ° C to 50 ° C. A method for producing a lithium-type zeolite, characterized by comprising: 請求項1記載のリチウム型ゼオライトの製造方法において、前記メタカオリン1に対して、10倍量の1M(モル)水酸化リチウム水溶液を加えることを特徴とするリチウム型ゼオライトの製造方法。   2. The method for producing a lithium zeolite according to claim 1, wherein 10 times the amount of 1M (mol) lithium hydroxide aqueous solution is added to the metakaolin 1. 請求項1又は2記載のリチウム型ゼオライトの製造方法において、前記水酸化リチウム水溶液を20℃〜50℃に調整した雰囲気中で24時間から120時間保持することを特徴とするリチウム型ゼオライトの製造方法。   3. The method for producing a lithium zeolite according to claim 1, wherein the lithium hydroxide aqueous solution is held in an atmosphere adjusted to 20 to 50 ° C. for 24 to 120 hours. . 請求項1、2又は3記載のリチウム型ゼオライトの製造方法において、前記メタカオリン1に対して10倍量の1M(モル)水酸化リチウム水溶液を加え、密閉容器に入れ、該密閉容器を20℃〜50℃に調整した雰囲気中で24時間から120時間保持し、該保持時間が経過した後、得られた沈殿物を常温でろ過・洗浄・乾燥し、白色粉末からなるリチウム型ゼオライトを得ることを特徴とするリチウム型ゼオライトの製造方法。   The method for producing a lithium-type zeolite according to claim 1, 2, or 3, wherein 10 times the amount of 1M (mol) lithium hydroxide aqueous solution is added to the metakaolin 1 and placed in a sealed container, and the sealed container is placed at 20 ° C to 20 ° C. Holding for 24 hours to 120 hours in an atmosphere adjusted to 50 ° C. After the holding time has elapsed, the obtained precipitate is filtered, washed and dried at room temperature to obtain a lithium-type zeolite made of white powder. A method for producing a lithium-type zeolite.
JP2008072014A 2008-03-19 2008-03-19 Method for producing lithium-type zeolite Active JP5594710B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2008072014A JP5594710B2 (en) 2008-03-19 2008-03-19 Method for producing lithium-type zeolite

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2008072014A JP5594710B2 (en) 2008-03-19 2008-03-19 Method for producing lithium-type zeolite

Publications (2)

Publication Number Publication Date
JP2009227484A true JP2009227484A (en) 2009-10-08
JP5594710B2 JP5594710B2 (en) 2014-09-24

Family

ID=41243326

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2008072014A Active JP5594710B2 (en) 2008-03-19 2008-03-19 Method for producing lithium-type zeolite

Country Status (1)

Country Link
JP (1) JP5594710B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013237585A (en) * 2012-05-15 2013-11-28 Tochigi Prefecture Abw type zeolite, alkali-silica reaction inhibiting material using the same, and production methods thereof
CN113264538A (en) * 2021-05-29 2021-08-17 山西腾茂科技股份有限公司 Preparation method and application of molecular sieve adsorbent based on LiNaKLSX

Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS52124000A (en) * 1976-04-09 1977-10-18 Grace W R & Co Method of making 4a and 5a aluminosilicate zeolite extrusions
JPS5316398A (en) * 1976-06-07 1978-02-15 Ethyl Corp Process for preparing zeoliteea
JPS62162615A (en) * 1985-10-15 1987-07-18 エクソン ケミカル パテンツ インコ−ポレ−テツド Improved zeolite l
JPH07109117A (en) * 1993-10-04 1995-04-25 Agency Of Ind Science & Technol Production of type a zeolite
JPH11226429A (en) * 1998-02-20 1999-08-24 Tosoh Corp Ion exchanging method
JP2004002132A (en) * 2002-04-11 2004-01-08 Sekisui Chem Co Ltd Zeolite powder granule and its manufacturing method
JP2006521986A (en) * 2003-04-04 2006-09-28 ナノケム ホールディングズ プロプライエタリー リミテッド Aluminosilicate with zeolite N structure
JP2006256876A (en) * 2005-03-15 2006-09-28 Tochigi Prefecture Molded product of zeolite and its manufacturing method
JP2008247640A (en) * 2007-03-29 2008-10-16 Denki Kagaku Kogyo Kk Method for synthesizing lithium-containing edi-type zeolite

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS52124000A (en) * 1976-04-09 1977-10-18 Grace W R & Co Method of making 4a and 5a aluminosilicate zeolite extrusions
JPS5316398A (en) * 1976-06-07 1978-02-15 Ethyl Corp Process for preparing zeoliteea
JPS62162615A (en) * 1985-10-15 1987-07-18 エクソン ケミカル パテンツ インコ−ポレ−テツド Improved zeolite l
JPH07109117A (en) * 1993-10-04 1995-04-25 Agency Of Ind Science & Technol Production of type a zeolite
JPH11226429A (en) * 1998-02-20 1999-08-24 Tosoh Corp Ion exchanging method
JP2004002132A (en) * 2002-04-11 2004-01-08 Sekisui Chem Co Ltd Zeolite powder granule and its manufacturing method
JP2006521986A (en) * 2003-04-04 2006-09-28 ナノケム ホールディングズ プロプライエタリー リミテッド Aluminosilicate with zeolite N structure
JP2006256876A (en) * 2005-03-15 2006-09-28 Tochigi Prefecture Molded product of zeolite and its manufacturing method
JP2008247640A (en) * 2007-03-29 2008-10-16 Denki Kagaku Kogyo Kk Method for synthesizing lithium-containing edi-type zeolite

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2013237585A (en) * 2012-05-15 2013-11-28 Tochigi Prefecture Abw type zeolite, alkali-silica reaction inhibiting material using the same, and production methods thereof
CN113264538A (en) * 2021-05-29 2021-08-17 山西腾茂科技股份有限公司 Preparation method and application of molecular sieve adsorbent based on LiNaKLSX

Also Published As

Publication number Publication date
JP5594710B2 (en) 2014-09-24

Similar Documents

Publication Publication Date Title
Tong et al. Use of Vietnamese rice husk ash for the production of sodium silicate as the activator for alkali-activated binders
Winnefeld et al. Further studies of the hydration of MgO-hydromagnesite blends
Lee et al. Synthesis of mesoporous geopolymers containing zeolite phases by a hydrothermal treatment
Walling et al. Structure and properties of binder gels formed in the system Mg (OH) 2–SiO 2–H 2 O for immobilisation of Magnox sludge
Lancellotti et al. Inorganic polymers from alkali activation of metakaolin: Effect of setting and curing on structure
Bakharev Resistance of geopolymer materials to acid attack
Aldabsheh et al. Dissolution behavior of Jordanian clay-rich materials in alkaline solutions for alkali activation purpose. Part I
Li et al. The role of MgO in the thermal behavior of MgO–silica fume pastes
Hosseini et al. Investigating the effect of the Mg2+/Ca2+ molar ratio on the carbonate speciation during the mild mineral carbonation process at atmospheric pressure
CN105967201A (en) Method for producing P-type zeolite from fly ash acid sludge
Fernández et al. Geochemical constraints on the stability of zeolites and C–S–H in the high pH reaction of bentonite
JP5594710B2 (en) Method for producing lithium-type zeolite
JP2013237585A (en) Abw type zeolite, alkali-silica reaction inhibiting material using the same, and production methods thereof
JP2017057095A (en) Production method of zeolite
Polat et al. Effects of tricarballylic acid on phase transformation of calcium sulfate hemihydrate to the dihydrate form
Leškevičienė α-Hemihydrate gypsum from flue gas desulphurization gypsum
Bajare et al. Alkali diffusion in porous alkali activated materials
Doneliene et al. The effect of synthetic hydrated calcium aluminate additive on the hydration properties of OPC
KR101619584B1 (en) Manufacturing method of geopolymer having high strength by using slag from waste spent catalyst
Bumanis et al. The Effect of Heat Treatment on Alkali Activated Materials
Prudďhomme et al. Impact of Alkaline Solution And Curing Temperature On Microstructure And Mechanical Properties Of Alkali‐Activated Blast Furnace Slag
Ferreiro et al. Influence of activated art paper sludge‐lime ratio on hydration kinetics and mechanical behavior in mixtures cured at 20° C
JPH08301638A (en) Solidification and materialization of kaolin powder with geopolymer
TWI577634B (en) Calcium Desulphurization by-product Formation Method for Calcium Sulfate Dihydrate
BR102014009507A2 (en) boussingaultite production process from liquid effluents containing magnesium sulphate

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20110218

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20110218

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20121213

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20130219

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20130411

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20131022

A521 Request for written amendment filed

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20131119

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20140701

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20140730

R150 Certificate of patent or registration of utility model

Ref document number: 5594710

Country of ref document: JP

Free format text: JAPANESE INTERMEDIATE CODE: R150

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

S111 Request for change of ownership or part of ownership

Free format text: JAPANESE INTERMEDIATE CODE: R313117

R350 Written notification of registration of transfer

Free format text: JAPANESE INTERMEDIATE CODE: R350

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250