Recycling method for SAPO-34 molecular-sieve synthesized mother liquid

A SAPO-34, a technology for synthesizing mother liquor, which is applied in the direction of molecular sieve and alkali exchange phosphate, molecular sieve characteristic silicoaluminophosphate, etc., can solve the problems affecting the performance of molding catalysts, difficult to use mother liquor at one time, and unfavorable industrial operation, etc., so as to reduce the synthesis Cost, high crystallinity, and the effect of reducing processing costs

Active Publication Date: 2016-06-15
山东齐鲁华信实业股份有限公司
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Problems solved by technology

[0004] In the method for the above-mentioned SAPO-34 mother liquor recycling, some use the mother liquor as a part of the synthesis system, and add corresponding raw materials according to the proportioning ratio. Because the mother liquor contains a large amount of water, it is difficult to use the mother liquor all at once, and when using the mother liquor At the same time, new crystallization mother liquor will also be produced, which is not conducive to industrial operation; some of them carry out the direct molding and beating process in the synthetic raw pulp or use the separated mother liquor as a binder for forming and beating, which inevitably makes the untreated mother liquor in the mother liquor Reactants clog the surface of the molecular sieve, thereby affecting the performance of the shaped catalyst

Method used

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  • Recycling method for SAPO-34 molecular-sieve synthesized mother liquid

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Experimental program
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Effect test

Embodiment 1

[0029] According to the ratio of raw materials 0.2SiO 2 :1.0Al 2 o 3 :1.0P 2 o 5 :2.0TEAOH:50H 2 O was sequentially added deionized water, pseudoboehmite, TEAOH, phosphoric acid, and silica sol, and stirred thoroughly to prepare an initial gel, which was then placed in a polytetrafluoroethylene-lined high-pressure crystallization kettle, and crystallized at 170°C for 24h. The solid product was separated, the mother liquor was recovered, the solid product was washed with deionized water until neutral, and dried at 110°C for 24 hours to obtain the original powder of SAPO-34 molecular sieve, marked as S-1. The X-ray diffraction analysis results are shown in the accompanying drawings, and the relative crystallinity is defined as 100%.

Embodiment 2

[0031] According to the ratio of raw materials 0.5SiO 2 :1.0Al 2 o 3 :1.0P 2 o 5 :0.5TEAOH:2.5TEA:90H 2 O Add deionized water, aluminum hydroxide, TEAOH, TEA, phosphoric acid, and ethyl orthosilicate in turn, stir well to prepare the initial gel, then put it into a polytetrafluoroethylene-lined high-pressure crystallization kettle, and crystallize at 150°C 36h. The solid product was separated, the mother liquor was recovered, the solid product was washed with deionized water until neutral, and dried at 110° C. for 24 hours to obtain the original powder of SAPO-34 molecular sieve, marked as S-2. X-ray diffraction analysis confirmed that the obtained solid product was SAPO-34 molecular sieve, and its relative crystallinity was 95%.

Embodiment 3

[0033] The mother liquor collected in Example 1 was concentrated, and the volume of the concentrated mother liquor was 25% of the recovered mother liquor volume. Use the formula in Example 1 to configure the initial gel, crystallize at 170°C for 24 hours, add the above-mentioned concentrated mother liquor, the addition amount is 6 times the mass of the initial gel, stir evenly and crystallize at 160°C for 30 hours, the solid product is separated, and the mother liquor After recovery, the solid product was washed with deionized water until it was neutral, and dried at 110°C for 24 hours to obtain the original powder of SAPO-34 molecular sieve, which was marked as S-3. X-ray diffraction analysis confirmed that the obtained solid product was SAPO-34 molecular sieve, and its relative crystallinity was 110%.

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Abstract

The invention relates to a recycling method for SAPO-34 molecular-sieve synthesized mother liquid, and belongs to the technical field of molecular sieve synthesis. The recycling method for the SAPO-34 molecular-sieve synthesized mother liquid includes the steps that concentrated mother liquid is treated as an independent whole, and is added into semi-crystallized crystallization liquid; particularly, a small amount of slurry of SAPO-34 molecular sieves is prepared to serve as primers, then a large amount of concentrated SAPO-34 molecular-sieve mother liquid is added, gel mixtures of the SAPO-34 molecular sieves are prepared and synthesized for next synthesis, and the molecular-sieve mother liquid is recycled. The recycling method is simple in technology and environmentally friendly, energy is saved, production cost is reduced, and recycling of the mother liquid and full using of active ingredients of the mother liquid are achieved.

Description

technical field [0001] The invention relates to a method for recycling a SAPO-34 molecular sieve synthetic mother liquid, and belongs to the technical field of molecular sieve synthesis. Background technique [0002] As important basic chemical raw materials, ethylene and propylene are becoming increasingly scarce, and the dwindling petroleum resources force people to seek alternative processes for the preparation of low-carbon olefins. At present, the most promising technology is methanol to low-carbon olefins (MTO) technology, and MTO The core of the technology is the preparation of MTO catalyst. Due to its suitable acidity, suitable pore structure, small pore size, large specific surface area, good hydrothermal stability and high selectivity of ethylene and propylene, SAPO-34 molecular sieve is currently developed for methanol-to-light olefins ( MTO) reaction catalyst of choice for molecular sieves. [0003] At present, the synthesis of SAPO-34 molecular sieve mainly ad...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
CPCC01B37/08C01B39/54C01P2002/72C01P2006/90
Inventor 梁光华明曰信刘环昌陈文勇
Owner 山东齐鲁华信实业股份有限公司
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