JPH064486B2 - Zeolite synthesis method from fly ash - Google Patents

Zeolite synthesis method from fly ash

Info

Publication number
JPH064486B2
JPH064486B2 JP4647889A JP4647889A JPH064486B2 JP H064486 B2 JPH064486 B2 JP H064486B2 JP 4647889 A JP4647889 A JP 4647889A JP 4647889 A JP4647889 A JP 4647889A JP H064486 B2 JPH064486 B2 JP H064486B2
Authority
JP
Japan
Prior art keywords
fly ash
sio
zeolite
synthesis method
mixed slurry
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 - Lifetime
Application number
JP4647889A
Other languages
Japanese (ja)
Other versions
JPH02229709A (en
Inventor
淳介 春名
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.)
Nippon Steel Corp
Original Assignee
Nippon Steel Corp
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 Nippon Steel Corp filed Critical Nippon Steel Corp
Priority to JP4647889A priority Critical patent/JPH064486B2/en
Publication of JPH02229709A publication Critical patent/JPH02229709A/en
Publication of JPH064486B2 publication Critical patent/JPH064486B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は、フライアッシュからのゼオライト合成方法に
関するものである。
TECHNICAL FIELD The present invention relates to a method for synthesizing zeolite from fly ash.

(従来の技術と発明が解決しようとする課題) NaOH水溶液とフライアッシュの混合スラリーを煮沸
処理してゼオライト化すること知られている。
(Problems to be Solved by Prior Art and Invention) It is known that a mixed slurry of an aqueous NaOH solution and fly ash is boiled to form a zeolite.

このような処理においては、高塩基交換容量(250me
q/100g以上)を得るため、長時間の煮沸処理が必
要となる。
In such processing, high base exchange capacity (250me
In order to obtain q / 100 g or more), a long boiling process is required.

例えば、4N−NaOH水溶液100ccにフライアッシ
ュ50g添加したものを100℃で煮沸処理した場合の
ゼオライト生成は下表のごとくなる。
For example, when 100 g of 4N-NaOH aqueous solution added with 50 g of fly ash is boiled at 100 ° C., zeolite production is as shown in the table below.

上表のごとく、高塩基交換容量のゼオライトを得るため
には、煮沸処理時間は約15時間以上を必要とする。
As shown in the above table, in order to obtain a zeolite with a high base exchange capacity, a boiling treatment time of about 15 hours or more is required.

このようなことから生産性が極めて低く、又コスト的に
も不利であり、工業的規模での操業は不可能である等の
欠点がある。
For this reason, there are drawbacks such that productivity is extremely low, cost is disadvantageous, and operation on an industrial scale is impossible.

本発明はこのような欠点を有利に解決するためなされた
ものである。
The present invention has been made to advantageously solve these drawbacks.

(発明が解決するための手段、作用) 本発明は、NaOH水溶液とフライアッシュの混合スラ
リーに珪酸イオン20〜100g/(SiO換算)を
添加し、次いで煮沸処理すること及びNaOH水溶液と
フライアッシュの混合スラリーに反応性SiO含有岩
石を添加し、次いで煮沸処理することを特徴とするフラ
イアッシュからのゼオライト合成方法である。
(Means and Actions for Solving the Invention) The present invention is to add 20 to 100 g / (SiO 2 conversion) of silicate ions to a mixed slurry of an aqueous NaOH solution and fly ash, and then subject it to boiling treatment and an aqueous NaOH solution and fly ash. A method for synthesizing zeolite from fly ash, which comprises adding reactive SiO 2 -containing rock to the mixed slurry of, and then boiling the mixture.

こゝにおいて上記NaOH水溶液としては、従来知られ
ているフライアッシュとの混合スラリーを煮沸処理する
ものであればよく、例えばNaOH:80〜160g/
水溶液が適当であり、又フライアッシュとの混合割合と
しても、従来のゼオライト化の混合割合でよく、例えば
NaOH水溶液:フライアッシュの比が2:1〜3:2
が適当である。
Here, the above-mentioned NaOH aqueous solution may be any one that can boil a conventionally known mixed slurry with fly ash, for example, NaOH: 80 to 160 g /
An aqueous solution is suitable, and the mixing ratio with fly ash may be a conventional mixing ratio for zeoliticization.
Is appropriate.

このような混合スラリーに珪酸イオン20〜100g/
(SiO換算)を添加するものであるが、20g/未
満では、ほとんど効果がなく、100g/超にしなくと
も十分効果が得られる。
20 to 100 g of silicate ions /
Although (SiO 2 equivalent) is added, if it is less than 20 g /, there is almost no effect, and even if it does not exceed 100 g /, a sufficient effect is obtained.

又珪酸イオンとしては、例えばメタ珪酸ソーダ等が適当
である。
As the silicate ion, for example, sodium metasilicate is suitable.

このような珪酸イオの他、反応性SiO含有岩石を用
いることができる。SiO源として例えばクリストバ
ライト、珪酸塩ガラス等を含有する岩石を使用すること
ができ、添加量としてはフライアッシュに対して2〜1
0%で十分である。
In addition to such silicate io, rocks containing reactive SiO 2 can be used. As the SiO 2 source, rock containing cristobalite, silicate glass or the like can be used, and the addition amount is 2-1 to the fly ash.
0% is sufficient.

本発明におけるNaOH水溶液とフライアッシュの混合
スラリーに珪酸イオン又は反応性SiO含有岩石を添
加することによりゼオライト化が迅速になされる理由は
以下のごとく考えられる。
The reason why the zeoliticization is rapidly performed by adding the silicate ion or the reactive SiO 2 -containing rock to the mixed slurry of the NaOH aqueous solution and the fly ash in the present invention is considered as follows.

即ち、フライアッシュはムライト、石英、及び非晶質S
iO(ガラス)からなっている。
That is, fly ash includes mullite, quartz, and amorphous S.
It is made from iO 2 (glass).

フライアッシュの成分組成の一例を示すと、SiO
0%,Al15%,CaO0.6%,Na
0.4%,KO0.2%,T−C3.5%,MgO
0.4%、残その他であり、又鉱物組成(X線回折)の
一例を示すと、石英30%,ムライト17%,非晶質S
iO38%、残その他から成っている。
An example of the composition of fly ash is SiO 2 7
0%, Al 2 O 3 15%, CaO 0.6%, Na 2 O
0.4%, K 2 O 0.2%, TC 3.5%, MgO
0.4%, the balance is other, and an example of the mineral composition (X-ray diffraction) is as follows: quartz 30%, mullite 17%, amorphous S
It consists of 38% of iO 2, the balance of others.

この内非晶質SiO分はNaOH水溶液中での煮沸処
理により、一旦溶解する。溶解した非晶質SiOは珪
酸イオンとして水溶液に存在し、その珪酸イオンと残り
のフライアッシュとNaOイオンが反応してゼオライ
トが生成されるものであるが、フライアッシュは、この
非晶質SiOの溶解に長時間を要し、そのためにゼオ
ライト合成(生成)も長時間を要するのである。
Of this, the amorphous SiO 2 component is once dissolved by boiling treatment in an aqueous NaOH solution. The dissolved amorphous SiO 2 exists in the aqueous solution as silicate ions, and the silicate ions react with the remaining fly ash and Na 2 O ions to produce zeolite. It takes a long time to dissolve the high-quality SiO 2 , and therefore the zeolite synthesis (production) also takes a long time.

そこで本発明のごとく、煮沸処理前に上記の如き、珪酸
イオン又は反応性SiOを添加することにより珪酸イ
オンが水溶液中に存在するのに時間が短くなり、それだ
けゼオライトも合成され易くなり、短時間で、しかも高
塩基交換容量(約200meq/100g以上)のゼオラ
イトが安定して合成できるものである。
Therefore, as in the present invention, by adding the silicate ion or reactive SiO 2 before the boiling treatment as described above, the time required for the silicate ion to exist in the aqueous solution becomes shorter, and the zeolite is more likely to be synthesized. Zeolites with a high base exchange capacity (about 200 meq / 100 g or more) can be stably synthesized in a short time.

(実施例) 次に本発明の実施例を比較例とともに挙げる。(Example) Next, the Example of this invention is given with a comparative example.

注1:SiO添加量は、実施例1〜3は珪酸イオン
(メタ珪酸ソーダ)(SiO換算)を添加、実施例4
〜6は、反応性SiOイオンとしてクリストバライト
90%含有岩石粉(44μ>)を添加。
Note 1: The amount of SiO 2 added is silicate ion (sodium metasilicate) (SiO 2 conversion) added in Examples 1 to 3, and Example 4
For Nos. 6 to 6, rock powder (44 μ>) containing 90% of cristobalite was added as a reactive SiO 2 ion.

注2:煮沸は100℃ 注3:フライアッシュ組成(%)は、SiO:72.
0,Al:15.3,CaO:0.6,Na
O:0.4,KO:0.2,T−C:3.5,Mg
O:0.4。
Note 2: Boiling is 100 ° C. Note 3: Fly ash composition (%) is SiO 2 : 72.
0, Al 2 O 3 : 15.3, CaO: 0.6, Na
2 O: 0.4, K 2 O: 0.2, TC: 3.5, Mg
O: 0.4.

注4:フライアッシュ鉱物組成(%)は、石英:30.
4,ムライト:17.1,非晶質SiO:38.4,
その他14.1。
Note 4: Fly ash mineral composition (%) is quartz: 30.
4, mullite: 17.1, amorphous SiO 2 : 38.4,
Other 14.1.

注5:CPSは、phillipsiteのX線回折ピークのうち
2θ=12.5゜の回折強度。
Note 5: CPS is the diffraction intensity of 2θ = 12.5 ° in the X-ray diffraction peak of phillipsite.

注5:meq/100gは、塩基交換容量。Note 5: meq / 100g is base exchange capacity.

(発明の効果) 本発明によれば、塩基交換容量の高いゼオライトが安定
して得られる。又短時間の煮沸で生産できることから高
生産性を維持しつつ製造でき、工業的に大きな効果を奏
することができる等の優れた効果が得られる。
(Effect of the invention) According to the present invention, a zeolite having a high base exchange capacity can be stably obtained. In addition, since it can be produced by boiling for a short time, it can be produced while maintaining high productivity, and excellent effects such as a great industrial effect can be obtained.

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】NaOH水溶液とフライアッシュの混合ス
ラリーに珪酸イオン20〜100g/(SiO換算)
を添加し、次いで煮沸処理することを特徴とするフライ
アッシュからのゼオライト合成方法。
1. Silica ion 20 to 100 g / (SiO 2 conversion) in a mixed slurry of NaOH aqueous solution and fly ash.
A method for synthesizing zeolite from fly ash, which comprises adding water, followed by boiling treatment.
【請求項2】NaOH水溶液とフライアッシュの混合ス
ラリーに反応性SiO含有岩石を添加し、次いで煮沸
処理することを特徴とするフライアッシュからのゼオラ
イト合成方法。
2. A method for synthesizing zeolite from fly ash, which comprises adding reactive SiO 2 -containing rock to a mixed slurry of an aqueous NaOH solution and fly ash, and then performing boiling treatment.
JP4647889A 1989-03-01 1989-03-01 Zeolite synthesis method from fly ash Expired - Lifetime JPH064486B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP4647889A JPH064486B2 (en) 1989-03-01 1989-03-01 Zeolite synthesis method from fly ash

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP4647889A JPH064486B2 (en) 1989-03-01 1989-03-01 Zeolite synthesis method from fly ash

Publications (2)

Publication Number Publication Date
JPH02229709A JPH02229709A (en) 1990-09-12
JPH064486B2 true JPH064486B2 (en) 1994-01-19

Family

ID=12748305

Family Applications (1)

Application Number Title Priority Date Filing Date
JP4647889A Expired - Lifetime JPH064486B2 (en) 1989-03-01 1989-03-01 Zeolite synthesis method from fly ash

Country Status (1)

Country Link
JP (1) JPH064486B2 (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL1004729C2 (en) * 1996-12-09 1998-06-18 Kema Nv Method for manufacturing zeolite from fly ash.
US6299854B1 (en) 1998-06-12 2001-10-09 Teruo Henmi Method of producing artificial zeolite
US6599494B2 (en) 1999-08-19 2003-07-29 K.E.M. Corporation Process for preparing artificial zeolite by a slurry reaction method

Also Published As

Publication number Publication date
JPH02229709A (en) 1990-09-12

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