Method for synthesizing flaky SAPO-34

A technology for the synthesis of SAPO-34, which is applied in chemical instruments and methods, hydrocarbon production from oxygen-containing organic compounds, molecular sieves and alkali-exchanged phosphates, etc., can solve the problem of inability to achieve zero emissions, product performance is not guaranteed, and cannot achieve complete Recycling and other problems, to achieve the effect of strong anti-carbon deposition, excellent MTO catalytic performance, and extended single-pass catalytic life

Active Publication Date: 2018-07-24
深圳科冠华太新材料技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In recent years, counterparts at home and abroad have conducted a lot of research on the reuse of crystallization mother liquor, but it is almost impossible to achieve zero discharge. If the mother liquor is directly reused in industry, on the one hand, the product performance will not be guaranteed, and on the other hand, it will not be able to achieve complete circulation. Some of them need to be discharged, but the mother liquor cannot be completely solved fundamentally.

Method used

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  • Method for synthesizing flaky SAPO-34
  • Method for synthesizing flaky SAPO-34
  • Method for synthesizing flaky SAPO-34

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Take the MY-0 mother liquor and distill off part of the water under reduced pressure at 100°C to increase the solid content of the mother liquor to 70%. Add raw materials so that the molar ratio of each species is 1.0P (phosphoric acid): 1.0Al (pseudoboehmite): 0.2Si (silica sol): 0.05F (NH 4 F), uniformly dispersed, sealed and placed in a 100°C oven for pre-crystallization for 5 hours to obtain a crystal nucleus solution; then add aluminum source, silicon source, organic amine template agent and phosphorus source to deionized water in sequence, the molar ratio of each material is 1.0P 2 o 5 (phosphoric acid): 1.2Al 2 o 3 (pseudoboehmite): 0.06SiO 2 (silica sol): 1.0TEAOH: 50H 2 After the O is fully dispersed, the initial gel is made; the crystal nucleus solution is added to the initial gel to form a gel, and the amount of the crystal nucleus solution accounts for 30% of the total mass of the gel. After the gel is evenly dispersed, it is sealed and placed in an ove...

Embodiment 2

[0036] Take the MY-1 mother liquor and distill off part of the water under reduced pressure at 80°C to increase the solid content of the mother liquor to 70%. Add raw materials so that the molar ratio of each species is 1.0P (phosphoric acid): 1.0Al (pseudoboehmite): 0.4Si (silica sol): 0.75F (NH 4 F), uniformly dispersed, sealed and placed in an oven at 100°C for pre-crystallization for 10 hours to obtain a crystal nucleus solution; add aluminum source, silicon source, organic amine template agent and phosphorus source to deionized water in sequence, and the molar ratio of each material is 1.0 P 2 o 5 (phosphoric acid): 1.0Al 2 o 3 (pseudoboehmite): 0.3SiO 2 (silica sol): 2.0TEA: 40H 2 O; Add the crystal nucleus solution to the initial gel to make a gel. The amount of the crystal nucleus solution accounts for 40% of the total mass of the gel. After the gel is evenly dispersed, it is sealed and placed in a 170°C oven for crystallization for 48 hours. After the reaction, c...

Embodiment 3

[0038]Take the MY-2 mother liquor and distill off part of the water under reduced pressure at 60°C to increase the solid content of the mother liquor to 60%. Add raw materials so that the molar ratio of each species is 1.0P (phosphoric acid): 1.0Al (pseudoboehmite): 0.6Si (silica sol): 0.2F (HF), after the dispersion is uniform, seal and place in a 140°C oven for pre-crystallization After melting for 5 hours, the crystal nucleus solution was obtained; the aluminum source, the silicon source, the organic amine template agent and the phosphorus source were added to the deionized water successively, and the molar ratio of each material was 1.0P 2 o 5 (phosphoric acid): 0.8Al 2 o 3 (pseudoboehmite): 0.6SiO 2 (Orthoethyl silicate): 2.DEA: 30H 2 O: Add the crystal nucleus solution to the initial gel to make a gel. The amount of crystal nucleus solution added is 50% of the total mass of the gel. After the gel is evenly dispersed, it is sealed and placed in a 200°C oven for crysta...

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Abstract

A method for synthesizing flaky SAPO-34 comprises the following steps: carrying out reduced pressure distillation on an SAPO-34 crystallization mother liquor, evaporating away a part of water, addingan aluminum source, a phosphorus source, a silicon source and fluoride, uniformly dispersing the added substances, adding the obtained solution into a kettle, and crystallizing the solution to obtaina crystal nucleus solution; sequentially adding the aluminum source, the silicon source, an organic amine template and the phosphorus source to deionized water, and fully dispersing the added substances to form an initial gel; and adding a crystal nucleus solution to the initial gel, uniformly dispersing the initial gel, adding the obtained solution to a high pressure reactor, crystallizing the solution, and centrifuging, washing, drying and calcining obtained crystals to obtain flaky SAPO-34 raw powder. The method effectively prolongs the MTO catalysis life of the SAPO-34 molecular sieve, andreuses a large amount of the crystallization mother liquor produced in the production process of the SAPO-34 molecular sieve.

Description

technical field [0001] The invention belongs to a method for synthesizing SAPO-34, in particular to a method for synthesizing flake-shaped SAPO-34 molecular sieves. Background technique [0002] In 1982, UCC developed a new class of phosphorus-containing molecular sieves——silicoaluminophosphate molecular sieves (SAPO), among which SAPO-34 showed good reactivity and ethylene-propylene selectivity to MTO. However, due to the rapid coking and deactivation of SAPO-34 molecular sieve in the MTO reaction, its application is greatly limited. By controlling the silicon distribution and silicon content of the SAPO-34 molecular sieve, the acid density and acid strength can be adjusted, and the traditional cubic block shape of SAPO-34 can be changed to form a stacked sheet-like layered shape, which is conducive to the rapid diffusion of the reaction product. Thereby improving the anti-coking ability of the catalyst. [0003] SAPO-34 molecular sieves are generally prepared by conventi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/08C01B39/54B82Y40/00B01J29/85C07C11/04C07C11/06
CPCB01J29/85B82Y40/00C01B37/08C01B39/54C01P2004/03C01P2004/24C01P2004/64C07C1/20C07C11/04C07C11/06Y02P20/52Y02P30/20Y02P30/40
Inventor 李志宏狄春雨梁光华李晓峰窦涛
Owner 深圳科冠华太新材料技术有限公司
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