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Method for synthesizing pure-phase SAPO-41 molecular sieve by use of crystallization mother liquid

A technology of SAPO-41 and crystallization mother liquor, which is applied in the direction of molecular sieve silicoaluminophosphate, molecular sieve and alkali exchange phosphate, etc., can solve the problems of raw material waste environment, high synthesis cost, and miscellaneous crystals in the product, so as to save raw materials , increase the nucleation speed and quantity, and avoid the effect of heterocrystalline phase

Inactive Publication Date: 2013-09-18
CHINA NAT OFFSHORE OIL CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the problems of high synthesis cost of SAPO-41 molecular sieve in the prior art, miscellaneous crystals in the product, waste of raw materials and environmental pollution caused by direct discharge of waste liquid, and provide a microwave-assisted synthesis of SAPO-41 molecular sieve using crystallization mother liquor. 41 molecular sieve method

Method used

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  • Method for synthesizing pure-phase SAPO-41 molecular sieve by use of crystallization mother liquid
  • Method for synthesizing pure-phase SAPO-41 molecular sieve by use of crystallization mother liquid
  • Method for synthesizing pure-phase SAPO-41 molecular sieve by use of crystallization mother liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 156g of pseudoboehmite into 600g of deionized water, and stir for 30min. Then under vigorous stirring, a solution formed by 272.1g of phosphoric acid (85wt%) and 401.1g of deionized water was slowly added dropwise, then 357.2g of di-n-propylamine (chemically pure, 97wt%) was added dropwise, and then silica sol (30wt% SiO 2 ) 24g to form a sol mixture, which was transferred into a stainless steel crystallization kettle and crystallized at 185°C under autogenous pressure for 38h. Cool after crystallization, filter the cooled solid-liquid mixture through a 0.1 μm membrane, recycle the mother liquor containing microcrystals, continue washing the solid product with water until neutral, and dry the solid product at 100°C for 17 hours to obtain Molecular sieve raw powder. The raw molecular sieve powder was calcined at 550°C for 10 hours in an air atmosphere to remove the template agent to obtain SAPO-41 molecular sieve. The X-ray diffractometer test results are shown in ...

Embodiment 2

[0025] The crystallization mother liquor recovered in Example 1 is used as a synthetic raw material, and after analyzing the component content, it is mixed with a certain amount of pseudo-boehmite, phosphoric acid, di-n-propylamine, silica sol, and deionized water to form a sol mixture, and the SAPO-41 Molecular sieve synthesis, the specific feeding is as follows:

[0026] Add 78g of pseudo-boehmite into 200g of deionized water, and stir for 30min. Then under vigorous stirring, a solution formed by 136g of phosphoric acid (85%) and 321g of deionized water was slowly added dropwise, and then 178.6g of di-n-propylamine (chemically pure, 97%) and 529.4g of crystallization containing 178.4g of di-n-propylamine were added dropwise. Mother liquor, then add silica sol (30wt% SiO 2 ) 24g to form a sol mixture, which was transferred into a stainless steel crystallization kettle and crystallized at 185°C for 36h under autogenous pressure. Cool after crystallization, filter the cooled ...

Embodiment 3

[0030] The crystallization mother liquor recovered in Example 2 is used as a synthetic raw material, and after analyzing the component content, it is mixed with a certain amount of pseudoboehmite, phosphoric acid, di-n-propylamine, silica sol, and deionized water to form a sol mixture, and the sol is assisted by microwave After heat treatment, carry out SAPO-41 molecular sieve synthesis, specific feeding and operation are as follows:

[0031] Add 49.9g of pseudo-boehmite into 300g of deionized water, and stir for 30min. Then under vigorous stirring, a solution formed by 87g of phosphoric acid (85%) and 48.1g of deionized water was slowly added dropwise, and then 114.3g of di-n-propylamine (chemically pure, 97%) and 720g of a crystallization solution containing 242.6g of di-n-propylamine were added dropwise. Mother liquor, then add silica sol (30wt% SiO 2) 24g to form a sol mixture, and the sol was heated under microwave-assisted heating (heating temperature 55° C.), and the i...

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Abstract

The invention discloses a method for synthesizing a pure-phase SAPO-41 molecular sieve by use of crystallization mother liquid, relating to the technical field of molecular sieve synthesis. The mother liquid obtained by filtration after the crystallization of an SAPO-41 molecular sieve is used as one part of the raw material for the synthesis of the same type of molecular sieve, and a corresponding new raw material is supplemented proportionally to prepare a sol mixture for synthesizing a molecular sieve. The method disclosed by the invention can make full use of the microcrystal and the component not involved in reaction in the SAPO-41 molecular sieve synthesis mother liquid; on one hand, the heating is assisted by microwaves, thus the generation of a hybrid crystal phase in the molecular sieve is eliminated, and the crystallinity and purity of the SAPO-41 molecular sieve are improved; and on the other hand, by use of the mother liquid and microcrystal seed therein, the crystallization time is shortened, the grain size of the molecular sieve is reduced, zero emission of the crystallization mother liquid is realized, environmental pollution is reduced, and the synthesis cost of the molecular sieve is lowered.

Description

technical field [0001] The invention belongs to the technical field of synthesis of silicoaluminophosphate molecular sieves, and in particular relates to a microwave-assisted method for synthesizing SAPO-41 molecular sieves by using crystallization mother liquor. Background technique [0002] Mesoporous SAPO-41 molecular sieve is a silicoaluminophosphate mesoporous molecular sieve with AFO structure, and the one-dimensional elliptical channel size composed of ten-membered rings is 0.43mm×0.70mm. The framework of SAPO-41 molecular sieve is composed of Si, P, Al and O elements, and belongs to the orthorhombic crystal system. The unit cell size is a=0.97nm, b=2.55nm, c=0.84nm. Its typical structural parameters are: pore diameter 0.60nm, pore volume 0.22mL g -1 . Due to the appropriate pore structure and moderate acidity, it exhibits high activity and isomerization selectivity in isomerization reactions of normal paraffins such as isomerization dewaxing. [0003] U.S. Patent ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54
Inventor 张耀日于海斌裴仁彦李孝国费亚南孙国方李佳隋芝宇张永惠赵甲霍志萍
Owner CHINA NAT OFFSHORE OIL CORP
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