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Method for preparing Beta zeolite molecular sieve with excessive chiral polymorph A under acidic condition

A beta zeolite, acid condition technology, applied in the field of beta zeolite molecular sieve preparation, can solve the problems of high cost, harsh conditions, complicated operation, etc.

Active Publication Date: 2015-09-16
常州纳泰土壤修复技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN102190314A discloses a method for synthesizing pure silicon or metal-doped Beta zeolite under specific conditions by using an organic template. Form A, however, due to its harsh conditions, the repeatability of the experiment is poor; CN103601212A also discloses a method for preparing chiral polymorph A excess Beta zeolite by using a specific self-made template, which is complex in operation and high in cost

Method used

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  • Method for preparing Beta zeolite molecular sieve with excessive chiral polymorph A under acidic condition
  • Method for preparing Beta zeolite molecular sieve with excessive chiral polymorph A under acidic condition
  • Method for preparing Beta zeolite molecular sieve with excessive chiral polymorph A under acidic condition

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Example 1: Using citric acid as acid auxiliary

[0026] Weigh 4.50g of ethyl orthosilicate and 2.22g of 35% tetraethylammonium hydroxide aqueous solution in a plastic beaker in turn, add 4g of distilled water, seal the beaker with a sealing film and stir for 5 hours to make the ethyl orthosilicate The ester is completely hydrolyzed. Remove the sealing film, continue stirring for 6 hours in the fume hood, volatilize the ethanol and water in the system to form a gel, and transfer it to the freezer (material temperature 20 °C, cold trap temperature -60 °C, the temperature has no obvious effect on the experimental system, Water removal is the key factor) freeze-dried in a dryer for 3 days, at this time the H of the system 2 O and SiO 2 The molar ratio is less than 1, and the product mass is 2.4 g.

[0027] Mix 2.4g of solid glue block with 0.5g of citric acid and 0.2g of ammonium fluoride and grind it into a uniform powder (100 mesh), then transfer it to a stainless stee...

Embodiment 2

[0029] Embodiment 2: take acetic acid as acid auxiliary

[0030] Weigh 4.50g of ethyl orthosilicate and 2.22g of 35% tetraethylammonium hydroxide aqueous solution in a plastic beaker in turn, add 4g of distilled water, seal the beaker with a sealing film and stir for 5 hours to make the ethyl orthosilicate The ester is completely hydrolyzed. Remove the sealing film, continue stirring in the fume hood for 6 hours, volatilize the ethanol and water in the system to form a gel, and transfer it to a freeze dryer (material temperature 20 °C, cold trap temperature -60 °C, the temperature has no obvious effect on this experimental system. Influence, except water is the key factor) lyophilized for 3 days, at this time the H of the system 2 O and SiO 2 The molar ratio is less than 1, and the product mass is 2.4 g.

[0031] Grind 2.4g of solid gel blocks into powder (100 mesh), slowly add 120 μL of acetic acid and 225 μL of hydrofluoric acid (aqueous solution with a mass fraction of 4...

Embodiment 3

[0033] Embodiment 3: take oxalic acid as acid auxiliary

[0034] Weigh 4.50g of tetraethyl orthosilicate and 2.22g of 35% tetraethylammonium hydroxide aqueous solution in order in a plastic beaker, add 3g of distilled water, seal the beaker with a sealing film and stir for 5 hours to make the ethyl orthosilicate The ester is completely hydrolyzed. Remove the sealing film, continue stirring in the fume hood for 6 hours, volatilize the ethanol and water in the system to form a gel, and transfer it to a freeze dryer (material temperature 20 °C, cold trap temperature -60 °C, the temperature has no obvious effect on this experimental system. Influence, except water is the key factor) lyophilized for 3 days, at this time the H of the system 2 O and SiO 2 The molar ratio is less than 1, and the product mass is 2.4 g.

[0035]Mix 2.4g of solid glue block with 0.27g of oxalic acid and 0.19g of ammonium fluoride and grind it into a uniform powder (100 mesh), transfer it to a stainles...

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Abstract

The invention relates to the technical field of Beta zeolite molecular sieve preparation, and especially relates to a method of adding an acidic auxiliary agent in initial gel for preparing a Beta zeolite molecular sieve with excessive chiral polymorph A under a specific acidic condition. According to the invention, a silicon source, a fluorine source, tetraethyl ammonium hydroxide and the acidic auxiliary agent are adopted as raw materials; a hydrothermal synthesis reaction is carried out; an obtained product is subjected to suction filtration, and is washed to neutral; and after drying, the product is calcined for 4-6h under a temperature of 550-600 DEG C, such that the Beta zeolite molecular sieve with excessive A morphs is obtained. The added acidic auxiliary agent is a key factor for producing the Beta zeolite with excessive A morphs. The acidic auxiliary agent can be oxalic acid, citric acid, acetic acid, hydrofluoric acid, phosphoric acid or the like. Compared to conventional Beta zeolite, the Beta zeolite synthesized with the method contains more chiral polymorph A. The method can create significant application values in the fields of the researches on chiral catalysis and chiral separation.

Description

technical field [0001] The invention belongs to the technical field of preparation of Beta zeolite molecular sieves, and particularly relates to a method for preparing excess Beta zeolite molecular sieves of chiral polymorph A under specific acidic conditions by adding acidic auxiliary agents to initial gels. Background technique [0002] Beta zeolite is the only high-silica zeolite with a three-dimensional twelve-membered ring cross-channel structure. Due to its unique topology and good thermal stability, hydrothermal stability, acidity and hydrophobicity, it has been obtained in petrochemical, fine chemical and other fields. a wide range of applications. [0003] In 1967, Mobil Petroleum Company first synthesized Beta zeolite from silica-alumina gel containing tetraethylammonium hydroxide and sodium ions, but its structure was not obtained until 1988 by J.Newsam et al. and J.B.Higgins et al. with the help of X. - Ray diffraction analysis, high-resolution transmission elec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 闫文付鲁婷婷于吉红徐如人
Owner 常州纳泰土壤修复技术有限公司
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