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Solid-phase synthesizing method of flaky lamellar SAPO-34

A SAPO-34, solid-phase synthesis technology, applied in chemical instruments and methods, hydrocarbon production from oxygen-containing organic compounds, molecular sieves and alkali-exchanged phosphate, etc., can solve poor stability, low crystallinity in solid-phase production, crystallinity Low-level problems, to achieve the effect of strong anti-carbon deposition, high crystallinity, and prolonged catalytic life

Active Publication Date: 2016-10-26
CHIA TAI ENERGY MATERIALS DALIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the addition of fluoride during hydrothermal synthesis will inevitably bring serious environmental problems. Therefore, most colleagues want to use the solid-phase method to open up a green and efficient path. However, the traditional solid-phase synthesis has low crystallinity and poor stability. The present invention Clever use of the solid-phase method, adding fluoride to the initial gel, effectively avoids a series of problems caused by the mother liquor in the liquid phase, and solves the problems of low crystallinity and poor stability in solid-phase production. Solid Phase Synthesis Pushes to Industrialized Production

Method used

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  • Solid-phase synthesizing method of flaky lamellar SAPO-34
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  • Solid-phase synthesizing method of flaky lamellar SAPO-34

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] With the initial gel molar ratio as 50H 2 O: 0.2SiO 2 (Silica sol): 1.0Al 2 o 3 (pseudoboehmite): 1.0P 2 o 5 : 0.5TEA: 0.05NaF to prepare a gel (code S-0.05NaF), age at room temperature for 8 hours, then transfer to a 90°C oven to dry overnight to obtain a dry gel, crush the dry gel, weigh 20g and place it in a polyamide Fluoride beaker. Take a 200ml reaction kettle, add 10gH to the bottom of the kettle 20, 5g TEA, place the polytetrafluoro beaker with dry glue on the upper layer of the kettle liquid, seal it and place it in a 200°C oven for crystallization for 48h, and place the dry powder sample in a 550°C muffle furnace for 300min roasting after the reaction , the final product can be obtained.

[0038] The S-0.05NaF obtained in Example 1 was granulated, and 1.0 g of 40-60 mesh particle samples were weighed for the fixed-bed methanol-to-olefin reaction. The samples were loaded into the constant temperature zone of the reactor, and both ends were filled with qu...

Embodiment 2

[0040] With the initial gel molar ratio as 50H 2 O: 0.2SiO 2 (Silica): 1.0Al 2 o 3 (pseudoboehmite): 1.0P 2 o 5 :0.5TEA: x NH 4 F prepares gel, wherein x=0(S-ONH 4 F), x=0.05(S-0.05NH 4 F), x=0.10(S-0.10NH 4 F), x=0.15(S-0.15NH 4 F), aged at room temperature for 8 hours, then transferred to an oven at 90°C to dry overnight to obtain dry glue, crushed dry glue, weighed 20 g and placed it in a polytetrafluoro beaker. Take a 200ml reaction kettle, add 10gH to the bottom of the kettle 2 0. 5gTEA, place the polytetrafluoro beaker with dry glue on the upper layer of the kettle liquid, seal it and place it in a 200°C oven for crystallization for 48h, and place the dry powder sample in a 550°C muffle furnace for roasting for 300min after the reaction. The final product can be obtained, and its SEM analysis is as follows: figure 2 shown.

Embodiment 3

[0042] With the initial gel molar ratio as 50H 2 O: 0.15TEOS (orthoethyl silicate): 1.0Al 2 o 3 (Aluminum isopropoxide): 1.0P 2 o 5 :1.0DEA:x NH 4 F Prepare the gel. x=0(S-0NH 4 F'), x=0.05(S-0.05NH 4 F') Aging at room temperature for 8 hours, and then transferred to a 90°C oven to dry overnight to obtain dry glue. After crushing the dry glue, weigh 20 g and place it in a polytetrafluoro beaker. Take a 200ml reaction kettle, add 10g H2O and 5g TEA to the bottom of the kettle, place a polytetrafluoro beaker with dry glue on the upper layer of the kettle liquid, seal it and place it in a 200°C oven for crystallization for 48h, after the reaction is over, put the dry powder The sample is placed in a muffle furnace at 550°C and roasted for 300 minutes to obtain the final product. The XRD analysis is as follows: image 3 As shown, the NH3-TPD analysis is as follows Figure 4 shown.

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Abstract

The invention relates to a solid-phase synthesizing method of flaky lamellar SAPO-34. The synthesizing method includes: mixing deionized water, silicon source, aluminum source, phosphorus source, fluoride and template agent, and stirring for 5-8 hours under room temperature to obtain initial gel; aging the initial gel under room temperature for 8-12 hours, and drying the aged gel under 90-120 DEG C overnight to obtain dry gel; adding mixed liquid of water and triethylamine to the bottom of a reaction kettle, crushing the dry gel and placing into a teflon beaker, placing the beaker on the liquid in the kettle, and performing reaction under 170-200 DEG C for 2-3 days to obtain SAPO-34 molecular sieve. The flaky lamellar SAPO-34 is good in stability, high in crystallinity and good in selectivity.

Description

technical field [0001] The invention belongs to a synthesis method of SAPO-34, and in particular relates to a solid-phase synthesis method of lamellar SAPO-34. Background technique [0002] In 1982, UCC Corporation 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 co...

Claims

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Application Information

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IPC IPC(8): C01B37/08C01B39/54B01J29/85C07C1/20C07C11/04C07C11/06
CPCB01J29/85C01B37/08C01B39/54C01P2002/72C01P2004/03C01P2004/20C07C1/20C07C11/04C07C11/06Y02P20/52Y02P30/20Y02P30/40
Inventor 李晓峰李志宏狄春雨王平何祖光窦涛
Owner CHIA TAI ENERGY MATERIALS DALIAN
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