• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    A METHOD FOR OBTAINING A ZEOLITE TYPE L5 M5 by reacting at 150-200 ° C a reaction mixture consisting of a source of silicon dioxide, a source of alumina, alkali and a dihydric alcohol, with a polar ratio of components: SiOg / AgjO 40-120 Me O / SiO 0 , 1-0.25 K (OH) 2 / Ae203 10-50 -HjO / Me O-10-1000 where Me is an alkali metal; R (OH) 2 is a dihydric alcohol, characterized in that, in order to increase the phase purity of the product, S as a dihydric alcohol is used 1,6-gx xdiol or tetramethyl ethylene glycol, or 2,2-dimethyl-1, 3-propanediol, or 1, 12-dode Candiol. .
    公开号:SU1118284A3
    申请号:SU813298450
    申请日:1981-06-11
    公开日:1984-10-07
    发明作者:Леонелло Каски Джон；Милнер Лоув Барри；Винсент Виттэм Томас
    申请人:Империал Кемикал Индастриз Лимитед (Фирма)；
    IPC主号:
    专利说明:

    This invention relates to methods for producing LSM type zeolites. A known method for producing zeolite by crystallization in the presence of quaternary ammonium compounds lj. However, these compounds are quite expensive. The closest in technical essence and the achieved result is a method of producing zeolite bSM-5, including the crystallization of a mixture consisting of a source of silicon dioxide, a source of alkali alumina and a diatomic alcohol izj. The disadvantage of this method is that the target product has an insufficient phase purity due to the presence of kenyanite impurity in it. The aim of the invention is to increase the phase purity of the product. This goal is achieved by the proposed method of obtaining a zeolite of the LSM-5 type by reacting at 150-200 with a reaction mixture consisting of a source of silica dioxide, a source of alkali alumina and a dihydric alcohol, with a molar ratio of 51G2 / Ae20e 40-120 Me O / SiO 0.1-0.25 R (OH) / AbgO, 10-50 H20 / Me20 10-1000 where is a wicker metal; R (OH) /; dihydric alcohol, with 1,6-hexanediol or tetramethyl ethylene glycol, or 2,2-dimethyl-1, 3-propanediol, or 1,12-dodecay diol as dihydric alcohol. Example 1. The reaction mixture has the following molar composition: NajO 10, R (OH) 2 20, ASgO, Si02 60, HjO 3000. 23.2 g of Si02 is dispersed in 300 g of water. In this dispersion, a solution containing 1.5 g of sodium aluminate (1.25 NajOA6.20; j, 3), 4.5 g of sodium oxide, 15.2 g of 1,6-hexavdiol and 41, is stirred in while mixing; 7 g of water. The suspension obtained is reacted at 200 ° C for 17 hours with stirring in a 500 ml stainless steel autoclave. The solid phase accumulates on the filter and is flushed with hot water and then dried at 120 ° C. for 24 hours. The product is identified by X-ray diffraction as pure LSM-5 zeolite without amorphous and crystalline impurities. The crystals have a prismatic shape and an average size of 8x5x3 um Example 2 The reaction mixture has the following molar composition: K20 6.67; pinacol Yu, SiO 40, H2O 2000 22.6 g of SiO are dispersed in 300 g of water. Then, a solution containing 4.9 g of potassium aluminate (1.8 K, 18 HjO), 5.2 g of potassium hydroxide hydrate, 11.1 g of tetramethylethylene glycol (pinacol) and 35 g of water with simultaneous stirring is introduced into this dispersion. The suspension is reacted for 68 hours at 180 ° C. Then the procedures are carried out as in Example 1. The product is free of Kenyanite impurities. Example 3: The reaction mixture has the following molar composition: 20, LPRE 20, SiOg 120, H20 6000. 23.4 g of SiO M 5 is dissolved in 300 g of water and then introduced into this solution with simultaneous stirring. a solution containing 0.75 g of sodium aluminate, 4.9 g of sodium hydroxide, 6.9 g of 2: 2-dImethyl-1H3-propanediol and 50 g of water. After reaction for 64 h at 150 s, a pure LSM-5 product is obtained; however, with a reaction time of up to 71 h, a significant amount of LSM-5 disappears due to replacement with a product close to kyanianite. If the reaction lasts for 64,176 h, LSM-5 zeolite is gradually transformed into a product close to Kenyanite. Thus, although reactions involving 1: 3 substituted dols can lead to the formation of pure LSM-5 zeolite, the reaction time is more critical in this case than in the case of 1,6-hexanediol. Example 4. In carrying out the process according to this example, the problems that occur in example 3 are largely eliminated by using large quantities of 2: 2-dimethyl-1: 3-propanediol. The following composition of the reaction mixture was used: 10, AS20Z DMRD 30, SiOg 60, HgO 3000. The process is carried out as in Example 1, with the exception that instead of 1: 6-hexanediol, 20.5 g of 31 2: 2- Dimethyl-1: 3-propanediol. When the reaction proceeds for 68 hours at 150 ° C., pure LSM-5 zeolite is obtained. The reaction for a much longer time does not lead to the formation of a product close to kyanyanit. Froze This example shows that it is possible to obtain almost pure LSM-5 zeolite from 1: 12-dodecanediol. However, there is a tendency to form crystalline silica impurities, such as tridymite. The formation of such an impurity can be reduced to at least 11% due to crystallization at low temperatures, for example, at. The reaction mixture has the following composition: NagO 10, dodecanediol 20, AEjO, SiOj 60, H 6 3000. 46.4 g of silica KS 300 (5.09 NagO,. 728 Si02, 248 N, O) is dispersed in 200 g of water. Then, the solution, the contents of 1.5 g of sodium aluminate, 4.5 g of sodium hydroxide, 20.5 g of 1: 12-dodecanediol, and 247 g of water are introduced into this dispersion with simultaneous mixing. The suspension reacts during 17 hours at 200 C. The resulting 44 product is qeonHt LSM-5, containing approximately 10% tridymite. Example (by a known method). 112.5 g of 3.4 SiO liquid glass was dissolved in a mixture of 141 g of water and 18.6 g of p-pentan-1-ol. Solution A is obtained. Then, in a mixture of 192 g of water and 4, and g of sulfuric acid, 3.9 g of sulfate alkali 1 Ab are dissolved (Ab2P. 3 80, 16 HjOX; as a result, solution B is obtained. Solution B is introduced while stirring A (10 h) and held in an autoclave for 24 hours. The solid phase is filtered, washed and dried, as in Example 1. LSM-5 zeolite is obtained, contents of 20% kenianite impurity. method). The process is carried out as in Example 6, but 13.1 g of zthanediol are used as the alcohol. LSM-5 zeolite is obtained, containing 8% ken anitovoy impurities. Thus, the proposed method allows to obtain LSM-5 zeolite of high phase purity.
    权利要求:
    Claims (1)
    [1]
    METHOD FOR PRODUCING ZEOLITE TYPE LSM 5-way interaction at
    150-200 ° C of the reaction mixture, consisting of a source of silicon dioxide, a source of aluminum oxide, alkali and dihydric alcohol, with a polar ratio of components:
    Si0 2 / Ae 2 0 40-120
    Me 2 O / SiO 2 * 0.1-0.25
    R (OH) 2 / AB 2 O 3 10-50
    H 2 O / Me 2 About 10-1000 where Me is an alkaline metal;
    R (0H) 2 ~ dihydric alcohol, characterized in that, in order to increase the phase purity of the product, 1,6-hexanediol or tetramethylene glycol or 2,2-di-§-methyl-1,3-propanediol is used as the dihydric alcohol or 1.12-dodecandiol. .
    SU. m 1118284>
    1 1118284
    SiC 2 / Ae z O 3 Me ^ O / SiO r (oh) / le 2 о 2 'Н 2 О / Ме 2 О where Ее - alkaline
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    同族专利:
    公开号 | 公开日
    EP0042225B1|1984-02-01|
    DE3162102D1|1984-03-08|
    EP0042225A1|1981-12-23|
    DK255081A|1981-12-13|
    NZ197268A|1984-08-24|
    JPS5727921A|1982-02-15|
    JPH0151446B2|1989-11-02|
    AU543903B2|1985-05-09|
    ZA813861B|1982-09-29|
    AU7145181A|1981-12-17|
    CA1161417A|1984-01-31|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    GB1334243A|1969-10-10|1973-10-17|Mobil Oil Corp|Crystalline zeolite and method of preparing the same|
    US3702886A|1969-10-10|1972-11-14|Mobil Oil Corp|Crystalline zeolite zsm-5 and method of preparing the same|
    GB1553209A|1975-09-29|1979-09-26|Ici Ltd|Zeolites|
    DK155176C|1978-06-22|1989-07-17|Snam Progetti|PROCEDURE FOR THE PREPARATION OF ALUMINUM OXIDE MODIFIED SILICON Dioxide|
    IT1140784B|1980-03-13|1986-10-10|Anic Spa|METHOD FOR THE PRODUCTION OF ZEOLITHIC STRUCTURE ALUMINUM SILICATES|NZ202099A|1981-10-21|1986-07-11|Ici Plc|Preparation of zeolite nu-10|
    DE3210062A1|1982-03-19|1983-09-29|Basf Ag, 6700 Ludwigshafen|NIOBINE ALUMINO AND BOROSILICATE ZOLITHES, THE PRODUCTION AND USE THEREOF AS A CATALYST|
    DE3211433C2|1982-03-27|1984-12-13|Degussa Ag, 6000 Frankfurt|Crystalline aluminosilicate PZ 1 and process for its production|
    JPH0250045B2|1982-07-30|1990-11-01|Shinnenryoyu Kaihatsu Gijutsu Kenkyu Kumiai|
    DE3362700D1|1982-10-01|1986-04-30|Ici Plc|Zeolites|
    US4599475A|1983-09-28|1986-07-08|Mobil Oil Corporation|Process for xylene isomerization using ZSM-23 zeolite|
    DE3400130A1|1984-01-04|1985-07-11|Hoechst Ag, 6230 Frankfurt|CRYSTALLINE SILICA, ITS SALTS AND METHOD FOR THE PRODUCTION THEREOF|
    DE3400132A1|1984-01-04|1985-07-11|Hoechst Ag, 6230 Frankfurt|METHOD FOR PRODUCING CRYSTALLINE ALKALINE LAYER SILICATES|
    DE3569235D1|1984-06-02|1989-05-11|Hoechst Ag|Process for the isomerisation of mono- or dichlorotoluene|
    US4900529A|1984-09-04|1990-02-13|W. R. Grace & Co.-Conn.|Process for making crystalline siliceous materials|
    US4626421A|1985-06-28|1986-12-02|Chevron Research Company|Preparation of magadiite|
    CN102897790B|2011-07-29|2014-12-31|中国石油化工股份有限公司|Synthesis method for ZSM-5 molecular sieve|
    CN102897791B|2011-07-29|2014-12-31|中国石油化工股份有限公司|Synthesis method for ZSM-5 molecular sieve|
    CN103964467B|2013-01-24|2016-01-20|中国石油化工股份有限公司|A kind of preparation method of ZSM-5 molecular sieve|
    CN103964465B|2013-01-24|2015-11-25|中国石油化工股份有限公司|A kind of synthetic method of phosphorous ZSM-5 molecular sieve|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    GB8019212|1980-06-12|
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