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Synthetic process of SAPO-11 Molecular sieve

A technique for the synthesis of SAPO-11, which is applied in the field of synthesis of SAPO-11 molecular sieves, can solve the problems of difficult operation, complex process, and high synthesis cost, and achieve the effects of safe and convenient operation, strong process economy, and low synthesis cost

Inactive Publication Date: 2006-09-20
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of these hydrothermal synthesis processes are that the molecular sieve crystallization process is carried out under high pressure, the investment in reaction equipment is large, the process is complicated, and the operation is difficult; the molecular sieve crystallization process requires the use of organic templates, which are expensive, cannot be recycled, and the synthesis cost is high; After the reaction, the molecular sieve product needs to be filtered and washed. The reaction waste liquid containing phosphoric acid and organic templates, surfactants and organic alcohols cannot be recovered, and it will pollute the environment after being directly discharged.

Method used

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  • Synthetic process of SAPO-11 Molecular sieve
  • Synthetic process of SAPO-11 Molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Add 80g of 1-ethyl-3-methylimidazole bromide into a three-necked flask, heat up to 100°C, add 3.2g of phosphoric acid with a concentration of 85wt%, stir well, then add 2.1g of aluminum isopropoxide, stir well, Then add 0.5g ethyl orthosilicate, stir evenly, then add 0.3g hydrofluoric acid with a concentration of 40wt%, stir evenly, heat up to 150°C, keep for 68 hours, then cool the reaction mixture to room temperature, add 150ml water, stir uniform, then the reaction mixture was filtered to obtain a brown powder, which was washed with 100ml of acetone to obtain a white powder, which was tested by XRD to be SAPO-11 molecular sieve and contained a small amount of unknown miscellaneous crystals. The water in the washed filtrate and the solvent for washing the molecular sieves are evaporated in a rotary evaporator to recover the ionic liquid.

Embodiment 2

[0024] Add 200g of 1-ethyl-3-methylimidazole bromide into a three-necked flask, heat up to 80°C, add 3.2g of phosphoric acid with a concentration of 85wt%, stir well, then add 2.1g of aluminum isopropoxide, stir well, Then add 0.5g ethyl orthosilicate, stir evenly, then add 0.3g hydrofluoric acid with a concentration of 40wt%, stir evenly, heat up to 150°C, keep for 68 hours, then cool the reaction mixture to room temperature, add 150ml water, stir uniform, then the reaction mixture was filtered to obtain a brown powder, which was washed with 100ml of acetone to obtain a white powder, which was tested by XRD to be SAPO-11 molecular sieve and contained a small amount of unknown miscellaneous crystals.

Embodiment 3

[0026] Add 40g of 1-ethyl-3-methylimidazole bromide into a three-necked flask, heat up to 150°C, add 3.2g of phosphoric acid with a concentration of 85wt%, stir well, then add 2.1g of aluminum isopropoxide, stir well, Then add 0.5g ethyl orthosilicate, stir evenly, then add 0.3g hydrofluoric acid with a concentration of 40wt%, stir evenly, heat up to 150°C, keep for 68 hours, then cool the reaction mixture to room temperature, add 150ml water, stir uniform, then the reaction mixture was filtered to obtain a brown powder, which was washed with 100ml of acetone to obtain a white powder, which was tested by XRD to be SAPO-11 molecular sieve and contained a small amount of unknown miscellaneous crystals.

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Abstract

This invention relates to a method to synthesize SAPO-11 molecular sieves, which conquers the disadvantages of hydrothermal high-pressure procedure, expensive organic reagents adopted and acid and alkali waste liquid discharge in conventional methods. It has the characteristics that during the synthesis, ionic liquid with a low vapor pressure is adopted as solvent and template and thus the crystallization can be carried out under normal pressure. And as the ionic liquid can be recycled, no expensive organic template is necessary, which greatly cuts down the cost. Besides, no acid or alkali waste liquid is discharged and this method is environmentally friendly.

Description

technical field [0001] The invention relates to a method for synthesizing molecular sieves, in particular to a method for synthesizing SAPO-11 molecular sieves. Background technique [0002] SAPO-11 molecular sieve is a silicon-containing aluminophosphate molecular sieve with AEL topology. This type of molecular sieve has a one-dimensional ten-membered ring straight pore structure, the channel is elliptical, the size is 0.39×0.63nm, and it has exchangeable cations. Silicon-free AEL-type aluminophosphate molecular sieves have no acid sites due to the charge balance of the framework composed of aluminum-oxygen tetrahedrons and phosphorus-oxygen tetrahedrons. SAPO-11 molecular sieves have extended the use of this type of molecular sieves, especially in alkane hydroisomerization reactions, due to the introduction of silicon species into the molecular sieve framework to generate acid sites, but SAPO-11 molecular sieves have excellent catalytic performance in noble metals. [00...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08B01J27/182
Inventor 田志坚徐云鹏徐竹生王炳春曲炜李鹏
Owner PETROCHINA CO LTD
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