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A method for synthesizing sapo-34 molecular sieves by utilizing industrial phosphate fertilizer by-product fluosilicic acid and its application

A technology of SAPO-34 and molecular sieve, which is applied in the field of comprehensive utilization of resources, can solve the problems of high price, high cost, and restrictions on wide application, and achieve the effects of strong reproducibility, high crystallinity, and overcoming process defects

Active Publication Date: 2022-06-07
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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  • A method for synthesizing sapo-34 molecular sieves by utilizing industrial phosphate fertilizer by-product fluosilicic acid and its application
  • A method for synthesizing sapo-34 molecular sieves by utilizing industrial phosphate fertilizer by-product fluosilicic acid and its application
  • A method for synthesizing sapo-34 molecular sieves by utilizing industrial phosphate fertilizer by-product fluosilicic acid and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 1) Add 25g of distilled water to the polytetrafluoroethylene lining, add 5.07g of 85% phosphoric acid and 2.4g of pseudo-boehmite in sequence under stirring conditions, and then add 9.51g of triethylamine after thorough mixing, and stir for 2h each time. , stir until the body phase is uniform to obtain solution I;

[0034] 2) Add 2.88g of 30wt% industrial fluorosilicic 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 liquid in it into a high temperature and high pressure reaction kettle, 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 un...

Embodiment 2

[0046] 1) Add 25g of distilled water to the polytetrafluoroethylene lining, add 5.07g of 85% phosphoric acid and 2.4g of pseudo-boehmite in sequence under stirring at room temperature, and then add 9.51g of triethylamine after mixing thoroughly, and stir for 2h each time. , stir until the body phase is uniform to obtain solution I;

[0047] 2) Add 3.46g of 25wt% industrial fluorosilicic acid to 3g of triethylamine and stir to obtain solution II, and add the solution II to the solution I and stir to obtain a precursor solution, and add the solution to the precursor solution according to the method of Example 1 The prepared SAPO-34 seed crystal was used as a crystal guide agent and stirred for 1 h. The addition amount of the crystal guide agent was 2% of the mass 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 polytetrafluoroe...

Embodiment 3

[0052] 1) Add 25g of distilled water to the polytetrafluoroethylene lining, add 5.07g of 85% phosphoric acid and 2.4g of pseudo-boehmite in sequence under stirring conditions, and then add 9.51g of triethylamine after thorough mixing, and stir for 2h each time. , stir until the body phase is uniform to obtain solution I;

[0053] 2) Add 3.09g of 28wt% industrial fluorosilicic acid to 3g of triethylamine and fully stir 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 lining with the precursor liquid in it into a high temperature and high pressure reaction kettle, 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 wa...

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Abstract

The invention provides a method for synthesizing SAPO‑34 molecular sieves by using fluosilicic acid, a by-product of industrial phosphate fertilizers, and its application, belonging to the technical field of comprehensive utilization of resources. The method includes the following steps: 1) adding phosphorus source and aluminum source to water, stirring and adding triethylamine to obtain solution I; 2) mixing industrial fluosilicic acid and triethylamine to obtain solution II, and adding solution II to the The precursor solution is obtained in the solution I, and the molar ratio of the substance in the precursor solution is Al2O3: SiO2: P2O5: H2O: TEA=1:0.3-0.6:1-1.1:70-90:3.2-9.5; 3) the precursor 4) Roasting the SAPO-34 molecular sieve precursor to obtain microporous SAPO-34 molecular sieve. An application based on the SAPO-34 molecular sieve described above, the SAPO-34 molecular sieve is loaded into a chromatography column, crude phosphoric acid is added, and vacuum filtration is performed to defluorinate the crude phosphoric acid. The SAPO-34 molecular sieve prepared by the present invention has large crystal grains, high crystallinity, good purity, and less impurity phases, can defluorinate more than 65% of fluorine-containing 6g / L crude phosphoric acid, and the fluorine adsorption capacity of the molecular sieve can reach 350mg / g .

Description

technical field [0001] The invention belongs to the technical field of comprehensive utilization of resources, and particularly relates to a method for synthesizing SAPO-34 molecular sieve by utilizing fluorosilicic acid, a by-product of industrial phosphate fertilizer, and application thereof. Background technique [0002] In the production process of wet-process phosphoric acid and phosphate fertilizer, a large amount of fluorine-containing gas is produced, which is absorbed by water to form industrial fluorosilicic acid. As a by-product of the development of the phosphate fertilizer industry, the output of fluorosilicic acid in my country is huge, but it is usually only processed into products with small demand such as fluoride 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 molecular sieves by us...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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