JPH03252309A - Synthesis of a type zeolite - Google Patents
Synthesis of a type zeoliteInfo
- Publication number
- JPH03252309A JPH03252309A JP4920490A JP4920490A JPH03252309A JP H03252309 A JPH03252309 A JP H03252309A JP 4920490 A JP4920490 A JP 4920490A JP 4920490 A JP4920490 A JP 4920490A JP H03252309 A JPH03252309 A JP H03252309A
- Authority
- JP
- Japan
- Prior art keywords
- aqueous solution
- crude ore
- diatomaceous earth
- composition
- zeolite
- 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
Links
- 239000010457 zeolite Substances 0.000 title claims abstract description 27
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 23
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 230000015572 biosynthetic process Effects 0.000 title description 6
- 238000003786 synthesis reaction Methods 0.000 title description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 19
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000000203 mixture Substances 0.000 claims abstract description 13
- 239000005909 Kieselgur Substances 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 10
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 6
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 229910001388 sodium aluminate Inorganic materials 0.000 claims abstract description 5
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 7
- 230000002194 synthesizing effect Effects 0.000 claims description 6
- JYIMWRSJCRRYNK-UHFFFAOYSA-N dialuminum;disodium;oxygen(2-);silicon(4+);hydrate Chemical compound O.[O-2].[O-2].[O-2].[O-2].[O-2].[O-2].[Na+].[Na+].[Al+3].[Al+3].[Si+4] JYIMWRSJCRRYNK-UHFFFAOYSA-N 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 abstract description 25
- 230000008025 crystallization Effects 0.000 abstract description 25
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 6
- KKCBUQHMOMHUOY-UHFFFAOYSA-N Na2O Inorganic materials [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 abstract description 5
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 229910052681 coesite Inorganic materials 0.000 abstract 3
- 229910052906 cristobalite Inorganic materials 0.000 abstract 3
- 239000000377 silicon dioxide Substances 0.000 abstract 3
- 229910052682 stishovite Inorganic materials 0.000 abstract 3
- 229910052905 tridymite Inorganic materials 0.000 abstract 3
- 238000002156 mixing Methods 0.000 abstract 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 description 9
- 238000005342 ion exchange Methods 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 101100348017 Drosophila melanogaster Nazo gene Proteins 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 230000006698 induction Effects 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- 229910021417 amorphous silicon Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000001493 electron microscopy Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 229910001948 sodium oxide Inorganic materials 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
- C01B33/28—Base exchange silicates, e.g. zeolites
- C01B33/2807—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures
- C01B33/2815—Zeolitic silicoaluminates with a tridimensional crystalline structure possessing molecular sieve properties; Isomorphous compounds wherein a part of the aluminium ore of the silicon present may be replaced by other elements such as gallium, germanium, phosphorus; Preparation of zeolitic molecular sieves from molecular sieves of another type or from preformed reacting mixtures of type A (UNION CARBIDE trade name; corresponds to GRACE's types Z-12 or Z-12L)
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Description
【発明の詳細な説明】
産業上の利用分野
本発明はＡ型ゼオライトの合成法に関するものであり、
特に珪藻土原鉱からＡ型ゼオライトを合成する方法に関
するものである。[Detailed Description of the Invention] Industrial Application Field The present invention relates to a method for synthesizing type A zeolite.
In particular, the present invention relates to a method for synthesizing type A zeolite from diatomaceous earth ore.
従来技術、発明の解決しようとする課題ゼオライトはそ
の吸着特性により分子ふるいや触媒として工業的利用価
値が高ので種々のゼオライトの合成が試みられてきた。PRIOR ART AND PROBLEMS TO BE SOLVED BY THE INVENTION Zeolites have high industrial utility value as molecular sieves and catalysts due to their adsorption properties, and attempts have been made to synthesize various zeolites.
しかし、ゼオライトは準安定相として存在し、必ずしも
安定相として存在しないなめにその結晶化機構は十分に
解明されていない。ゼオライトの生成条件および生成過
程を解明することは新種のゼオライトの合成法を開発す
るうえで重要である。However, since zeolite exists as a metastable phase and not necessarily as a stable phase, its crystallization mechanism has not been fully elucidated. Elucidating the conditions and process of zeolite formation is important in developing a method for synthesizing new types of zeolites.
本発明は、未利用資源として多量に存在する珪藻土の有
効利用として珪藻土中に含まれる非晶質酸化珪素分を利
用し、高度の結晶化特性を有するＡ型ゼオライトの合成
法を開発しようとするものである。The present invention aims to develop a method for synthesizing A-type zeolite having high crystallization properties by utilizing the amorphous silicon oxide content contained in diatomaceous earth as an effective use of diatomaceous earth, which exists in large amounts as an unused resource. It is something.
課題を解決するための手段
本発明は、珪藻土原鉱を乾燥、分級後シュウ酸水溶液に
て処理し、６００〜８００″Ｃにて焼成したものを合成
原料の酸化珪素として使用し、これに水酸化ナトリウム
水溶液およびアルミン酸すトリウムを混合して次の組成
ＮａｚＯＡ１２０３−Ｓ ｉ ０ａ−ＨＪＩＯ（Ｎ
ａｚｏ／ Ｓ ｉ ０２＝１，０〜１．４． ５ｉＣ）
ａ／ＡＩａＯ３＝１．２〜２．０ ＨａＯ／Ｎａｇ
Ｏ＝２０．０〜６００）を有するＡ型ゼオライト組成物
を作り、これを温度５０〜１００℃、０．５〜３０時間
結晶化処理するＡ型ゼオライトの合成法に関するもので
ある。シュウ酸水溶液の濃度は原鉱に含まれる鉄分によ
って異なるが、奸才しくは０２規定以上、処理温度とし
ては７０℃以上が望ましい。焼成温度は６００〜８００
°Ｃであるが１好ましくは６５０〜８００℃で、８００
℃以上では結晶化の進行度が大きいので好ましくない。Means for Solving the Problems The present invention uses diatomaceous earth ore which is dried, classified, treated with an oxalic acid aqueous solution, and calcined at 600 to 800"C as a synthetic raw material, silicon oxide, which is then added with water. Aqueous sodium oxide solution and sodium aluminate are mixed to form the following composition NazOA1203-S i 0a-HJIO (N
azo/S i 02=1,0-1.4. 5iC)
a/AIaO3=1.2~2.0 HaO/Nag
The present invention relates to a method for synthesizing type A zeolite, in which a type A zeolite composition having a zeolite (O = 20.0 to 600) is prepared and the composition is crystallized at a temperature of 50 to 100°C for 0.5 to 30 hours. The concentration of the oxalic acid aqueous solution varies depending on the iron content in the raw ore, but it is preferably 0.2N or higher and the treatment temperature is preferably 70°C or higher. Firing temperature is 600-800
°C, preferably 650-800 °C, 800 °C
If the temperature is higher than 0.degree. C., crystallization progresses to a large extent, which is not preferable.
Ｋ電忽
珪藻土原鉱は秋田県北秋田郡森吉町寄延沢採掘場より採
取した珪藻土原鉱を使用した。原鉱を粉砕し、１１０℃
で乾燥し、４２メツシユのフルイを用いて分級し、これ
を０．２規定シユウ酸水溶液で処理して鉄分を除去した
後６５０℃で２時間焼成して合成原料とした。The K-den diatomaceous earth ore used was diatomaceous earth ore collected from the Yorinobuzawa mining site, Moriyoshi-cho, Kitaakita-gun, Akita Prefecture. Crush raw ore and heat to 110℃
The mixture was dried using a 42-mesh sieve, classified using a 42-mesh sieve, treated with a 0.2 N oxalic acid aqueous solution to remove iron, and then calcined at 650° C. for 2 hours to obtain a synthetic raw material.
原料の組成（ｗ ｔ％）は、 Ｓ ｉ Ｏａ＝ ８３．
９０、Ａ ＩＪＩ０３＝９．３０．ＮａｚＯ＝０．３３
、Ｆ ｅ ａｓｓ” ０．４ Ｂ 、Ｋａ○＝０．４
７゜Ｉｇ、１ｏｓｓ＝０．５０．Ｔｏｔａｌ 〜９４゜
９３である０次に酸処理珪藻±（ＳｉＯ２）に水酸化ナ
トリウム（ＮａＯＨ）水溶液、アルミン酸ナトリウム（
Ｎ ａ Ａ Ｉ Ｏ２）を加え２合成を次の範囲で行っ
た。The composition (wt%) of the raw material is S i Oa = 83.
90, A IJI03=9.30. NazO=0.33
, F e ass” 0.4 B , Ka○=0.4
7°Ig, 1oss=0.50. Aqueous solution of sodium hydroxide (NaOH), sodium aluminate (
2 synthesis was carried out in the following range.
Ｎ ａ ｘ Ｏ／ Ｓ ｉＯ２＝ １ 、０〜１ 、４
３１０ ａ ／ Ａ １２０ ｓ ＝ １ 、２〜２．
０ＨｇＯ／Ｎ ａ２０＝ ２０．０〜６０．０結晶化温
度５０．６５．８０℃および時間０．５〜２８時間を変
えて実験を行った。Na x O/S iO2 = 1, 0~1, 4
310 a / A 120 s = 1, 2-2.
0HgO/N a20 = 20.0-60.0 Experiments were carried out by changing the crystallization temperature of 50.65.80°C and the time of 0.5-28 hours.
結果：
（イ） Ｓ ｉ Ｏ２／ Ａ ｌ ２０ ：ａ比の結晶
化におよぼす影響
結晶化温度６５℃、 Ｓ ｉ Ｏａ／ Ａ Ｉ ２０３
比を１．２ １．６．２．０と変えて調べた。その結果
は第１Ａ図、第１Ｂ図、第１Ｃ図に示す。図よりＳ ｉ
Ｏ，／Ａ ｌ ２Ｏｓ比が高くなるにつれて。Results: (a) Effect of S i O2/ A l 20 :a ratio on crystallization Crystallization temperature 65°C, S i Oa/ A I 203
The investigation was conducted by changing the ratio to 1.2, 1.6, and 2.0. The results are shown in FIGS. 1A, 1B, and 1C. From the figure, S i
As the O,/A l 2Os ratio increases.
誘導期が減少し、その後結晶化速度が増大することがわ
かった。It was found that the induction period was decreased and the crystallization rate was subsequently increased.
（ロ）ＮａｚＯ／Ｓ ｉＯａ比の結晶化におよぼす影響
結晶化温度６５℃、Ｎａ、Ｏ／Ｓ ｉ Ｏ，比を１．０
．１．２，１．４に変えて調べた。その結果は 第２Ａ
図、第２Ｂ図、第２Ｃ図に示す。(b) Effect of NazO/S iOa ratio on crystallization Crystallization temperature 65°C, Na, O/S iO ratio 1.0
．． I changed it to 1.2 and 1.4 and investigated. The result is 2A
2B and 2C.
Ｎ ａ ２０ ／ Ｓ ｉ Ｏａ比が高くなるにつれて
誘導期が減少し、結晶化速度が増大することがわかった
。It was found that as the Na 20 /S i Oa ratio increases, the induction period decreases and the crystallization rate increases.
（ハ）Ｈ２０／Ｎａ２Ｏ比の結晶化におよぼす影響
結晶化温度６５℃、Ｈ２０／ＮａａＯ比を２０．４０．
６０に変えて調べた。その結果は第３図に示す０図より
Ｈ２０／Ｎａ、Ｏ比の減少と共に結晶化速度は増大する
が、Ｈ２０／Ｎａ、Ｏ比が２０の場合のみ２４時間後の
結晶化速度は減少することがわかった。(c) Effect of H20/Na2O ratio on crystallization Crystallization temperature 65°C, H20/NaaO ratio 20.40.
I changed it to 60 and checked. As shown in Figure 3, the results show that as the H20/Na, O ratio decreases, the crystallization rate increases, but only when the H20/Na, O ratio is 20, the crystallization rate after 24 hours decreases. I understand.
（ニ）結晶化温度の結晶化におよぼす影響’ ＮａｚＯ
／５ｉＯａ＝１．４．Ｓｉ○２／Ａ１．０３＝ １．６
．Ｈ，Ｏ／ＮａｚＯ＝４０の組成の合成ゼオライトを用
い、結晶化温度５０，６５．８０℃に変えて調べ、その
結果を、第４図に示す０図より、温度が減少するにつれ
て誘導期は減少し、結晶化速度は増加することがわかっ
た。(d) Effect of crystallization temperature on crystallization' NazO
/5iOa=1.4. Si○2/A1.03= 1.6
．． Using a synthetic zeolite with a composition of H, O/NazO = 40, the crystallization temperature was changed to 50 and 65.80°C, and the results are shown in Figure 4. As the temperature decreases, the induction period increases. It was found that the crystallization rate decreased and the crystallization rate increased.
（ホ）ガス吸着量およびイオン交換能（ＣＥＣ）の変化
上記組成の合成ゼオライトを用い、結晶化温度６５℃で
ガス吸着量およびイオン交換能の経時変化を調べた。そ
の結果を第５図に示す。図よりイオン交換能は結晶化速
度に対応して変化することがわかった。またガス吸着量
は結晶化構造の発達と共に増加することがわかった。(e) Changes in gas adsorption amount and ion exchange capacity (CEC) Using the synthetic zeolite having the above composition, changes over time in gas adsorption amount and ion exchange capacity were investigated at a crystallization temperature of 65°C. The results are shown in FIG. The figure shows that the ion exchange capacity changes depending on the crystallization rate. It was also found that the amount of gas adsorption increases with the development of the crystallized structure.
結晶化度は日本電子製ＪＸＷ−７Ｆ型Ｘ線回折装置によ
って行った。市販品の合成ゼオライト（水沢化学ジルト
ンＢ）の２θ＝２９．５〜３０２５の積分強度比を基準
として求めた。The crystallinity was measured using a JXW-7F model X-ray diffractometer manufactured by JEOL. It was determined based on the integrated intensity ratio of 2θ=29.5 to 3025 of a commercially available synthetic zeolite (Mizusawa Kagaku Jiruton B).
ガス吸着量は炭酸ガスを用い０℃における吸着量（吸着
表面積として評価）を測定した。The amount of gas adsorption was determined by measuring the adsorption amount (evaluated as adsorption surface area) at 0° C. using carbon dioxide gas.
イオン交換能（ＣＥＣ）は、Ｏ，１ｍｇのゼオライト試
料をカルシウム水溶液（塩化カルシウムＣａ ＣＩ ２
１９８ ｍ ｇを純水２５０ ｍ、 ｌに溶かしたもの
〉に分散させ２５℃一定で１０分間撹拌後０．４５μの
メンブランフィルタ−を使ってろ別してカルシウムイオ
ンを原子吸光で測定した。装置は日本ジャーレルアッシ
ュ（株）原子吸光／炎光共用分光測定装置ＡＡ−７８２
型を用いた。Ion exchange capacity (CEC) is determined by adding O.1 mg of zeolite sample to calcium aqueous solution (calcium chloride Ca CI 2
198 mg dissolved in 250 ml of pure water> was stirred at a constant temperature of 25° C. for 10 minutes, filtered using a 0.45 μm membrane filter, and calcium ions were measured by atomic absorption. The device is Japan Jarrell Ash Co., Ltd. atomic absorption/flame spectrometer AA-782.
A mold was used.
（１）電子顕微鏡（ＳＥＭ）観察
き成Ｉ、たゼオライトを走査型電子顕微鏡で観察し、そ
の結果を第６図（写真）（倍率１０，０００）に示す。(1) Electron microscopy (SEM) observation The prepared zeolite was observed using a scanning electron microscope, and the results are shown in FIG. 6 (photo) (magnification: 10,000).
ゼオライトＡは組成Ｎ ａ ２０ 、／ Ｓ ｉＯ２＝
１２．５ｉ０２／Ａｌ□０３＝ １．２．ＨｚＯｌＮ
ａ ＲＯ＝ ４０．結晶化温度８０℃１時間２４時間の
条件にて合成した。図より、ゼオライト結晶の成長が認
められた。Zeolite A has the composition N a 20 , / S iO2=
12.5i02/Al□03= 1.2. HzOIN
aRO=40. Synthesis was carried out at a crystallization temperature of 80° C. for 1 hour and 24 hours. From the figure, growth of zeolite crystals was observed.
発明の効果
本発明により１合成条件を変えることにより種々の異な
る炭酸ガス吸着能及びイオン交換能をもっなＡ型ゼオラ
イトを合成することができた。Effects of the Invention According to the present invention, A-type zeolites having various different carbon dioxide adsorption abilities and ion exchange abilities could be synthesized by changing one synthesis condition.
尚珪藻の核を残したまま該核上にゼオライトの結晶を形
成させることができた。Furthermore, it was possible to form zeolite crystals on the diatom core while leaving it intact.
第１Ａ図、第１Ｂ図、第１Ｃ図は合成ゼオライトのＳｉ
○２／ Ａ ｌ ２０３比と結晶化度との関係を経時的
に示した図。
第２Ａ図、第２Ｂ図、第２Ｃ図は合成ゼオライトのＮａ
、Ｏ／ＳｉＯ□比と結晶化度との関係を経時的に示した
図。
第３図は合成ゼオライトのＨ２０／Ｎａ２Ｏ比と結晶化
度との関係を経時的に示した図。
第４図は合成ゼオライトの合成温度と結晶化度との関係
を経時的に示した図。
第５図は合成ゼオライトのガス吸着量およびイオン交換
能と結晶化度との関係を経時的に示した図および第６図
は合成ゼオライトのＳＥＭ図（電子顕微鏡写真）である
。Figures 1A, 1B, and 1C show the Si of synthetic zeolite.
A diagram showing the relationship between the ○2/A l 203 ratio and the degree of crystallinity over time. Figures 2A, 2B, and 2C show the Na content of synthetic zeolite.
, A diagram showing the relationship between O/SiO□ ratio and crystallinity over time. FIG. 3 is a diagram showing the relationship between the H20/Na2O ratio and crystallinity of synthetic zeolite over time. FIG. 4 is a graph showing the relationship between synthesis temperature and crystallinity of synthetic zeolite over time. FIG. 5 is a diagram showing the relationship between the amount of gas adsorption, ion exchange capacity, and crystallinity of the synthetic zeolite over time, and FIG. 6 is an SEM diagram (electron micrograph) of the synthetic zeolite.
Claims (1)
６００〜８００℃にて焼成したものを合成原料の酸化珪
素として使用し、これに水酸化ナトリウム水溶液および
アルミン酸ナトリウムを混合して次の組成Ｎａ＿２Ｏ−
Ａｌ＿２Ｏ＿３−ＳｉＯ＿２−Ｈ＿２Ｏ（Ｎａ＿２Ｏ／
ＳｉＯ＿２＝１．０〜１．４、ＳｉＯ＿２／Ａｌ＿２Ｏ
＿３＝１．２〜２．０、Ｈ＿２Ｏ／Ｎａ＿２Ｏ＝２０．
０〜６０．０）を有するＡ型ゼオライト組成物を作り、
これを温度５０〜１００℃、０．５〜３０時間結晶化処
理することを特徴とするＡ型ゼオライトの合成法。After drying and classifying diatomaceous earth ore, it is treated with an oxalic acid aqueous solution,
Silicon oxide calcined at 600 to 800°C is used as a synthetic raw material, and an aqueous sodium hydroxide solution and sodium aluminate are mixed with it to form the following composition Na_2O-
Al_2O_3-SiO_2-H_2O(Na_2O/
SiO_2=1.0~1.4, SiO_2/Al_2O
_3=1.2-2.0, H_2O/Na_2O=20.
0 to 60.0),
A method for synthesizing type A zeolite, which comprises crystallizing the zeolite at a temperature of 50 to 100°C for 0.5 to 30 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4920490A JPH03252309A (en) | 1990-03-02 | 1990-03-02 | Synthesis of a type zeolite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4920490A JPH03252309A (en) | 1990-03-02 | 1990-03-02 | Synthesis of a type zeolite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03252309A true JPH03252309A (en) | 1991-11-11 |
Family
ID=12824462
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4920490A Pending JPH03252309A (en) | 1990-03-02 | 1990-03-02 | Synthesis of a type zeolite |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03252309A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6451282B1 (en) * | 1997-10-28 | 2002-09-17 | SIKLOSI PéTER | Process for production of zeolites from raw materials containing alkali alumino hydro-silicates |
| CZ302624B6 (en) * | 2009-11-05 | 2011-08-03 | Výzkumný ústav anorganické chemie, a. s. | Process for preparing zeolite beta from dried half-finished product |
| MD20110099A2 (en) * | 2011-03-18 | 2012-09-30 | Институт Прикладной Физики Академии Наук Молдовы | Sorption-filtering material for water purification and process for its production |
| CN102923724A (en) * | 2012-11-28 | 2013-02-13 | 东北大学 | Method for increasing specific surface area of diatomite and proportion of nanopore |
| CN104016370A (en) * | 2014-06-05 | 2014-09-03 | 诺威尔（天津）能源装备股份有限公司 | Method for preparing 5A molecular sieve from diatomite |
| CN105645540A (en) * | 2016-01-28 | 2016-06-08 | 肇庆市新荣昌工业环保有限公司 | Copper-containing waste liquid treatment method |
-
1990
- 1990-03-02 JP JP4920490A patent/JPH03252309A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6451282B1 (en) * | 1997-10-28 | 2002-09-17 | SIKLOSI PéTER | Process for production of zeolites from raw materials containing alkali alumino hydro-silicates |
| CZ302624B6 (en) * | 2009-11-05 | 2011-08-03 | Výzkumný ústav anorganické chemie, a. s. | Process for preparing zeolite beta from dried half-finished product |
| MD20110099A2 (en) * | 2011-03-18 | 2012-09-30 | Институт Прикладной Физики Академии Наук Молдовы | Sorption-filtering material for water purification and process for its production |
| CN102923724A (en) * | 2012-11-28 | 2013-02-13 | 东北大学 | Method for increasing specific surface area of diatomite and proportion of nanopore |
| CN104016370A (en) * | 2014-06-05 | 2014-09-03 | 诺威尔（天津）能源装备股份有限公司 | Method for preparing 5A molecular sieve from diatomite |
| CN105645540A (en) * | 2016-01-28 | 2016-06-08 | 肇庆市新荣昌工业环保有限公司 | Copper-containing waste liquid treatment method |
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