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Method for synthesizing SAPO-34 molecular sieve by using industrial phosphate fertilizer byproduct fluosilicic acid and application of SAPO-34 molecular sieve

A SAPO-34, molecular sieve technology, applied in the field of comprehensive utilization of resources, can solve the problems of high price, high cost, limited wide application, etc., and achieve the effect of strong regeneration, high crystallinity and overcoming process defects

Active Publication Date: 2021-09-24
WUHAN INSTITUTE OF TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN108675317A prolongs the single-pass life of SAPO-34 molecular sieve through post-treatment process, making the industrial cost of methanol synthesis olefin (MTO) reduced, but the silicon source used in its synthetic molecular sieve is organosilicon source, although it is more organic template agent triethylamine Easy to disperse in synthetic systems, but more expensive
Therefore, the cost of SAPO-34 synthesized from organosilicon sources is relatively high. Although it can be used as a catalyst for the synthesis of olefins from methanol, it limits its wide application in industrial wastewater treatment and other industrial fields with less economic added value.

Method used

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  • Method for synthesizing SAPO-34 molecular sieve by using industrial phosphate fertilizer byproduct fluosilicic acid and application of SAPO-34 molecular sieve
  • Method for synthesizing SAPO-34 molecular sieve by using industrial phosphate fertilizer byproduct fluosilicic acid and application of SAPO-34 molecular sieve
  • Method for synthesizing SAPO-34 molecular sieve by using industrial phosphate fertilizer byproduct fluosilicic acid and application of SAPO-34 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1) Add 25g of distilled water to the PTFE lining, add 5.07g of 85% phosphoric acid and 2.4g of pseudo-boehmite in turn under stirring conditions, mix well and then add 9.51g of triethylamine, and stir for 2 hours each time , and stir until the bulk phase is uniform to obtain solution I;

[0034] 2) Add 2.88g of 30wt% industrial fluosilicic acid to 3g of triethylamine and stir well to obtain solution II, add solution II to solution I, and stir at room temperature for 2h to obtain a precursor solution. At this time, the molar composition ratio of each substance in the precursor solution is Al 2 o 3 : SiO 2 :P 2 o 5 :H 2 O:TEA=1:0.3:1.1:70:6.2;

[0035] 3) Put the polytetrafluoroethylene liner with the precursor solution into a high-temperature and high-pressure reactor, and statically crystallize it in an oven at 200°C for 1 day; the obtained mother liquor is recovered, and the solid product is washed with deionized water until neutral, and filtered , and dried to ...

Embodiment 2

[0046] 1) Add 25g of distilled water to the PTFE lining, add 5.07g of 85% phosphoric acid and 2.4g of pseudo-boehmite in turn under stirring at room temperature, mix well and then add 9.51g of triethylamine, and stir for 2 hours each time , and stir until the bulk phase is uniform to obtain solution I;

[0047] 2) Add 3.46g of 25wt% industrial fluosilicic acid to 3g of triethylamine and stir well to obtain solution II, and add the solution II to the solution I and stir thoroughly to obtain a precursor solution, and add to the precursor solution according to the method in Example 1 The prepared SAPO-34 seed crystal was used as a crystal guide agent, stirred for 1h, and the addition amount of the crystal guide agent was 2% of the quality of the precursor solution. At this time, the molar composition ratio of each substance in the precursor solution was Al 2 o 3 : SiO 2 :P 2 o 5 :H 2 O:TEA:seed=1:0.3:1.1:90:5.7;

[0048] 3) Put the polytetrafluoroethylene lining with the pr...

Embodiment 3

[0052] 1) Add 25g of distilled water to the PTFE lining, add 5.07g of 85% phosphoric acid and 2.4g of pseudo-boehmite in turn under stirring conditions, mix well and then add 9.51g of triethylamine, and stir for 2 hours each time , and stir until the bulk phase is uniform to obtain solution I;

[0053] 2) Add 3.09g of 28wt% industrial fluosilicic acid to 3g of triethylamine and stir well to obtain solution II, add solution II to solution I, and stir at room temperature for 2h to obtain a precursor solution. At this time, the molar composition ratio of each substance in the precursor solution is Al 2 o 3 : SiO 2 :P 2 o 5 :H 2 O:TEA=1:0.3:1.1:70:6.2;

[0054] 3) Put the polytetrafluoroethylene liner with the precursor solution into a high-temperature and high-pressure reactor, and statically crystallize it in an oven at 220°C for 2 hours; the obtained mother liquor is recovered, and the solid product is washed with deionized water until neutral, filtered, Dry to obtain SA...

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Abstract

The invention provides a method for synthesizing an SAPO-34 molecular sieve by using an industrial phosphate fertilizer byproduct fluosilicic acid and application of the SAPO-34 molecular sieve, and belongs to the technical field of comprehensive utilization of resources. The method comprises the steps of 1) adding a phosphorus source and an aluminum source into water, stirring, and adding triethylamine to obtain a solution I; (2) mixing industrial fluosilicic acid and triethylamine to obtain a solution II, and adding the solution II into the solution I to obtain a precursor solution, wherein the molar ratio of Al2O3 to SiO2 to P2O5 to H2O to TEA in the precursor solution is 1: (0.3-0.6): (1-1.1): (70-90): (3.2-9.5); 3) performing hydrothermal crystallization on the precursor solution to obtain an SAPO-34 molecular sieve precursor; and (4) roasting the SAPO-34 molecular sieve precursor so as to obtain the microporous SAPO-34 molecular sieve. According to the application of the SAPO-34 molecular sieve, the SAPO-34 molecular sieve is loaded into a chromatographic column, crude phosphoric acid is added, reduced pressure suction filtration is carried out, and defluorination is conducted on the crude phosphoric acid. The prepared SAPO-34 molecular sieve is large in crystal grain, high in crystallinity, good in purity and less in impurity phase, the defluorination rate of crude phosphoric acid containing 6 g / L of fluorine can be 65% or above, and the fluorine adsorption capacity of the molecular sieve can reach 350 mg / g.

Description

technical field [0001] The invention belongs to the technical field of comprehensive utilization of resources, and in particular relates to a method for synthesizing SAPO-34 molecular sieves by utilizing fluosilicic acid, a by-product of industrial phosphate fertilizers, and an application thereof. Background technique [0002] During the production process of wet-process phosphoric acid and phosphate fertilizer, a large amount of fluorine-containing gas will be produced, which will form industrial fluosilicic acid after being absorbed by water. As a by-product of the development of the phosphate fertilizer industry, the output of fluosilicic acid in my country is huge, but it is usually only processed into products with small demand such as fluorine salts, and the abundant resources such as silicon, aluminum, and phosphorus have not been fully utilized. [0003] The published Chinese patent with publication number CN105271244A provides a method for synthesizing mesoporous m...

Claims

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Application Information

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IPC IPC(8): C01B37/08C01B39/54B01J20/18B01J20/30B01D15/08C01B25/237
CPCC01B37/08C01B39/54B01J20/186B01D15/08C01B25/2372C01P2002/72C01P2004/03C01P2004/61Y02P20/52
Inventor 金放许冶吴桂英田承涛肖林波
Owner WUHAN INSTITUTE OF TECHNOLOGY
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