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Method for synthesizing molecular sieve by using silicon, aluminum and phosphorus elements in by-product fluosilicic acid in industrial phosphoric acid preparation process and application of molecular sieve

A technology for the preparation process and industrial phosphoric acid, which is applied in the field of comprehensive utilization of resources, can solve the problem that phosphorus is not well utilized, and achieve the effects of increasing added value, strong regeneration, and improving utilization rate

Pending Publication Date: 2021-10-08
HUBEI SANNING CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the fluosilicic acid by-product of wet-process phosphoric acid also contains a small amount of phosphorus and aluminum. In these two methods, phosphorus has not been well utilized. Therefore, molecular sieves in the comprehensive utilization of by-product fluosilicic acid have great development. Prospects and approaches to breakthrough innovation

Method used

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  • Method for synthesizing molecular sieve by using silicon, aluminum and phosphorus elements in by-product fluosilicic acid in industrial phosphoric acid preparation process and application of molecular sieve
  • Method for synthesizing molecular sieve by using silicon, aluminum and phosphorus elements in by-product fluosilicic acid in industrial phosphoric acid preparation process and application of molecular sieve
  • Method for synthesizing molecular sieve by using silicon, aluminum and phosphorus elements in by-product fluosilicic acid in industrial phosphoric acid preparation process and application of molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0050] A method for synthesizing molecular sieves using silicon, aluminum and phosphorus elements in the by-product fluosilicic acid in the preparation process of industrial phosphoric acid, comprising the following steps:

[0051] The first step: ammoniated silicon dioxide

[0052] (1) Take 150ml of industrial fluosilicic acid and add it to a cleaned three-necked flask, heat it to 45°C, start adding 40ml of ammonia water to the three-necked flask at a rate of 2ml / min, react for 30min, measure the final temperature of the reaction at 47°C, measure pH=6.80, aged for 30min, filtered, the filtrate was set aside, the filter cake was dried and weighed, the mass was 20g;

[0053] The second step: Synthesis of SAPO-34 molecular sieve

[0054] (2) Add 26.5ml of deionized water into the beaker, weigh 2.1729g of 85% phosphoric acid, add 6 drops / min for about 30 minutes, and stir for 2 hours;

[0055] (3) Weighing 2.4g of high-purity pseudo-boehmite, adding and stirring for 2 hours, th...

Embodiment 2

[0060] The preparation method is the same as in Example 1, the difference is that the ratio of raw materials becomes SiO 2 :Al 2 o 3 :P 2 o 5 :TEA:H 2 O=0.3:1:1.1:4.7:70. At this time, the pH of the precursor solution was reduced to 8.25. Product XRD detection result shows as pure phase SAPO-34 ( figure 1 -(B))

Embodiment 3

[0062] The preparation method is the same as in Example 1, the difference is that the ratio of raw materials becomes SiO 2 :Al 2 o 3 :P 2 o 5 :TEA:H 2 O=0.3:1:1.1:4.3:70. At this time, the pH of the precursor solution was reduced to 7.56. The XRD test result of the product shows that it is a mixed phase of SAPO-34 and SAPO-5 molecular sieves, and the content of SAPO-5 is relatively small. ( figure 1 -(C))

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Abstract

The invention discloses a method for synthesizing a molecular sieve by using silicon, aluminum and phosphorus elements in a by-product fluosilicic acid in an industrial phosphoric acid preparation process and application of the molecular sieve. The method comprises the steps of: preparing silicon dioxide by a fluosilicic acid ammonification method: adding industrial fluosilicic acid, heating, then adding ammonia water, reacting, measuring the final temperature of the reaction, measuring the pH value, aging, filtering, and drying and weighing a filter cake to obtain silicon dioxide; and synthesizing an SAPO-34 / SAPO-5 molecular sieve. The industrial by-product fluosilicic acid of a phosphorus fertilizer is used as a silicon source, an aluminum source, a phosphorus source and a fluorine source in the molecular sieve, so that the utilization rate of the fluosilicic acid is increased, and the added value of the silicon element in the in the fluosilicic acid as a phosphoric acid by-product is increased. In addition, the prepared molecular sieve is applied to industrial wastewater defluorination of recovered wastewater in a phosphorus fertilizer byproduct ardealite warehouse slag field, and circular economy is realized.

Description

technical field [0001] The invention belongs to the field of comprehensive utilization of resources, and specifically relates to a method and application for synthesizing molecular sieves by utilizing silicon, aluminum and phosphorus elements in fluosilicic acid, a by-product in the preparation process of industrial phosphoric acid. Background technique [0002] In 1982, Barrer R M and other colleagues from United Carbide Corporation (U.C.C.) synthesized and developed AlPO 4 -n aluminum phosphate molecular sieve, n represents a different skeleton structure, the molecular sieve is synthesized under hydrothermal conditions, using quaternary ammonium salt cations or organic amines as templates, different arrangements of aluminum oxide and phosphorus oxide skeletons will form different structures molecular sieve crystals. The synthesized aluminum phosphate molecular sieve is composed of P-O-Al connection, which makes the framework of the molecular sieve electrically neutral, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54B01J20/18B01J20/30C02F1/28C02F101/14
CPCC01B37/08C01B39/54B01J20/18C02F1/281C02F2101/14
Inventor 金放陈晋林田承涛肖林波许冶吴桂英
Owner HUBEI SANNING CHEM
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