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Method for preparing beta zeolite molecular sieves with excess chiral polymorph a under acidic conditions

A technology of beta zeolite and acidic conditions, which is applied in the field of Beta zeolite molecular sieve preparation, and can solve problems such as high cost, harsh conditions, and complicated operation

Active Publication Date: 2017-01-11
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 sieves with excess chiral polymorph a under acidic conditions
  • Method for preparing beta zeolite molecular sieves with excess chiral polymorph a under acidic conditions
  • Method for preparing beta zeolite molecular sieves with excess chiral polymorph a under acidic conditions

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Experimental program
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Effect test

Embodiment 1

[0025] Embodiment 1: take citric acid as acid auxiliary agent

[0026] In a plastic beaker, weigh 4.50g ethyl orthosilicate and 2.22g aqueous solution of tetraethylammonium hydroxide with a mass fraction of 35%, add 4g of distilled water, seal the beaker with parafilm and stir for 5 hours to make ethyl orthosilicate Esters are completely hydrolyzed. Remove the sealing film, continue to stir in the fume hood for 6 hours, volatilize the ethanol and water in the system to form a jelly, transfer to freezing (material temperature 20°C, cold trap temperature -60°C, the temperature has no obvious influence on the experimental system, Dehydration is a key factor) freeze-drying in the drier 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 quality is 2.4 g.

[0027] Mix 2.4g of solid rubber 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 stainles...

Embodiment 2

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

[0030] In a plastic beaker, weigh 4.50g ethyl orthosilicate and 2.22g aqueous solution of tetraethylammonium hydroxide with a mass fraction of 35%, add 4g of distilled water, seal the beaker with parafilm and stir for 5 hours to make ethyl orthosilicate Esters are completely hydrolyzed. Remove the sealing film, continue to stir in the fume hood for 6h, volatilize the ethanol and water in the system to form a jelly, and transfer it to a freeze dryer (material temperature 20°C, cold trap temperature -60°C, the temperature has no significant effect on the experimental system. Influence, water removal is the key factor) freeze-dried 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 quality is 2.4 g.

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

Embodiment 3

[0033] Embodiment 3: Take oxalic acid as acid auxiliary agent

[0034] In a plastic beaker, weigh 4.50g ethyl orthosilicate and 2.22g aqueous solution of tetraethylammonium hydroxide with a mass fraction of 35%, add 3g of distilled water, seal the beaker with parafilm and stir for 5 hours to make ethyl orthosilicate Esters are completely hydrolyzed. Remove the sealing film, continue to stir in the fume hood for 6h, volatilize the ethanol and water in the system to form a jelly, and transfer it to a freeze dryer (material temperature 20°C, cold trap temperature -60°C, the temperature has no significant effect on the experimental system. Influence, water removal is the key factor) freeze-dried 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 quality is 2.4 g.

[0035]Mix 2.4g of solid rubber 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 po...

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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, in particular to a method for preparing chiral polymorph A-excess Beta zeolite molecular sieves under specific acidic conditions by adding acidic additives to initial gel. Background technique [0002] Beta zeolite is the only high-silica zeolite with a three-dimensional twelve-membered ring intersecting channel structure. Due to its unique topological structure and good thermal stability, hydrothermal stability, acidity and hydrophobicity, it has been widely used in petrochemical, fine chemical and other fields. a wide range of applications. [0003] In 1967, Mobil Petroleum Company synthesized Beta zeolite from silica-alumina gel containing tetraethylammonium hydroxide and sodium ions for the first time, 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 trans...

Claims

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Application Information

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Patent Type & Authority Patents(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