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Method for synthesizing Beta molecular sieve with low silica-alumina ratio by utilizing all-silicon Beta crystallization mother liquor

A low-silicon-aluminum ratio, crystallization mother liquor technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of increasing the cost of filter residue treatment, exceeding the standard of sewage suspended solids, and increasing the difficulty of sewage treatment, so as to reduce nucleation. The effect of activation energy, shortening synthesis time, and increasing nucleation rate

Pending Publication Date: 2019-11-22
JIANGSU TIANNUO NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the large amount of silicon in the mother liquor and the free silica is not easy to settle, it is very easy to cause the suspended solids in the sewage to exceed the standard, thereby increasing the difficulty of sewage treatment; and the Na in the crystallization mother liquor 2 O is high, increasing the cost of filter residue treatment

Method used

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  • Method for synthesizing Beta molecular sieve with low silica-alumina ratio by utilizing all-silicon Beta crystallization mother liquor
  • Method for synthesizing Beta molecular sieve with low silica-alumina ratio by utilizing all-silicon Beta crystallization mother liquor
  • Method for synthesizing Beta molecular sieve with low silica-alumina ratio by utilizing all-silicon Beta crystallization mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037]Mix 114.2g of the crystallization mother liquor (SiO2: 17.7g / L; Na2O: 23.3g / L) in Comparative Example 1 with 16g of water, add 3.7g of NaOH and 6.7g of sodium aluminate, and stir until a clear solution. Under magnetic stirring, slowly add 120g of silica sol dropwise to the above mixed solution to form silicate gel A; weigh a certain amount of tetraethylammonium bromide, and mix tetraethylammonium bromide and silicate gel The mass ratio of SiO2 is 1:0.25. Dissolve the above-mentioned tetraethylammonium bromide in 30.8g of deionized water and stir until it is completely dissolved to obtain a mixed solution B. Slowly add solution B to A gel under stirring conditions to mix Evenly, finally transfer the mixture into a polytetrafluoroethylene-lined stainless steel crystallization kettle, raise the temperature from room temperature to 120°C at 5°C / hour and keep it for 24h, then raise the temperature at 5°C / hour to 150°C and keep it for 36h, then at 150°C Crystallize at ℃ for 12...

Embodiment 2

[0039] 110.2g (SiO2: 17.7g / L; Na2O: 23.3g / L) of the crystallization mother liquor in Comparative Example 1 was mixed with 20g water, 3.9gNaOH and 10.2g aluminum hydroxide were added, and stirred until a clear solution. Under magnetic stirring, slowly add 125g of silica sol dropwise to the above mixed solution to form aluminosilicate gel A; weigh a certain amount of tetraethylammonium bromide, and add tetraethylammonium bromide and silicate The mass ratio of SiO2 in the gel is 1:0.25. Dissolve the above-mentioned tetraethylammonium bromide in 30.8g of deionized water and stir until completely dissolved to obtain a mixed solution B. Slowly add solution B to A gel under stirring conditions The mixture was mixed uniformly, and finally the mixture was transferred to a polytetrafluoroethylene-lined stainless steel crystallization kettle, and the temperature was raised from room temperature to 120°C at a rate of 5°C / hour for 24 hours, and then the temperature was raised to 150°C at a ...

Embodiment 3

[0041] 113.4g (SiO2: 65g / L; Na2O: 25.6g / L) of the crystallization mother liquor in Comparative Example 1 was mixed with 16.8g water, 4.1gNaOH and 9.5g alumina were added, and stirred until a clear solution. Slowly add 120g of silica sol dropwise into the above mixed solution under magnetic stirring to form silicate gel A; weigh a certain amount of tetraethylammonium bromide, and add tetraethylammonium bromide and silicate The mass ratio of SiO2 in the gel is 1:0.25. Dissolve the above-mentioned tetraethylammonium bromide in 30.8g of deionized water and stir until completely dissolved to obtain a mixed solution B. Slowly add solution B to A gel under stirring conditions Make the mixture uniform, and finally transfer the mixture into a polytetrafluoroethylene-lined stainless steel crystallization kettle, raise the temperature from room temperature to 120°C at 5°C / hour and keep it for 24h, then raise the temperature at 5°C / hour to 150°C and keep it for 36h, then in Crystallizatio...

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Abstract

The invention relates to a method for synthesizing a Beta molecular sieve with a low silica-alumina ratio by using all-silicon Beta crystallization mother liquor. Firstly, the components which do notparticipate in the reaction in the all-silicon Beta molecular sieve synthesis mother liquor are recycled, so that the discharge of synthesis waste liquor is avoided, the environmental pollution is reduced, the mother liquor is recycled, raw materials are saved, and the synthesis cost of the molecular sieve is reduced; secondly, microcrystals exist in mother liquor after the reaction, so that the nucleation speed and quantity of crystal nucleuses in the induction period of the crystallization process are greatly improved, the nucleation activation energy of the molecular sieve is reduced, the crystallization time can be shortened, the grain size of the molecular sieve is reduced, and the crystallinity of the synthesized molecular sieve is relatively high; therefore, the crystallization process of the molecular sieve is accelerated while the grain size of a sample is reduced, and the crystallization period is shortened.

Description

technical field [0001] The invention relates to the technical field of molecular sieve synthesis methods, in particular to a method for synthesizing a Beta molecular sieve with a low silicon-aluminum ratio by using an all-silicon Beta crystallization mother liquor. Background technique [0002] In 1967, mobil disclosed in the patent application USP3308069 that Beta molecular sieves were synthesized for the first time in a silica-alumina gel containing sodium ions using tetraethylammonium hydroxide as a template agent, which has a unique three-dimensional staggered macroporous structure. Compared with Y-type molecular sieves, the molar ratio of silicon-aluminum substances of Beta molecular sieves can be adjusted in the range of tens to hundreds. Beta molecular sieves have good structural selectivity, acid catalytic properties and hydrothermal stability, and it is Due to its excellent performance in adsorption and catalysis, it is widely used in various petrochemical processes...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
CPCC01B39/04C01P2002/72C01P2004/62
Inventor 孙先勇张伟
Owner JIANGSU TIANNUO NEW MATERIAL TECH
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