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Method for preparing SAPO-34 molecular sieve by liquid phase crystallization method

A technology of SAPO-34 and molecular sieves, which is applied in the field of preparation of SAPO-34 molecular sieves, can solve problems such as small synthesis range, low crystallinity, complex equipment, etc., and achieve industrial scale production, good crystallinity, and simple preparation process Effect

Active Publication Date: 2008-02-20
HUALU ENG & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, compared with the hydrothermal synthesis method, this method has relatively low crystallinity, the synthesis range of the prepared molecular sieve silicon-aluminum ratio and phosphorus-aluminum ratio is small, and the equipment is complicated, and it is not easy to scale up.

Method used

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  • Method for preparing SAPO-34 molecular sieve by liquid phase crystallization method

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Experimental program
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Effect test

Embodiment 1

[0020] Mix 23.06g 85% orthophosphoric acid with 25ml H 2 O fully mixed, under vigorous stirring, add 32.57g of pseudo-boehmite into the mixed solution of phosphoric acid and water, add 25g of water, stir for 2h, then add 13.61g of SiO 2 26.45% silica sol. Wherein the molar composition of adding each component is: Al 2 o 3 :P 2 o 5 : 0.6SiO2 2 .

[0021] After stirring and reacting at room temperature for 2 h, the reaction temperature was gradually increased to 80° C., and the stirring reaction was continued for 6 to 18 h. With the evaporation of water during the reaction, the viscosity of the system gradually increases until finally it becomes dry glue. Grind the obtained dry glue into powder, take 24g of the powder and a mixed solution of 45.8g morpholine and 53.2g water (volume ratio is 1:1) and fully mix them under stirring, place in a stainless steel autoclave, and seal the autoclave Then crystallize at 180°C for 5 days. Finally, after cooling the autoclave to ro...

Embodiment 2

[0024] Mix 23.06g of 85% phosphoric acid with 25ml of H 2 O mixed thoroughly, under vigorous stirring, 32.57g of aluminum hydroxide was gradually added to the aqueous solution of phosphoric acid within 2h, and after stirring for 2h, 13.61g of SiO 2 26.45% silica sol. Prepare the precursor sol after stirring and reacting at room temperature for 4 hours, gradually increase the reaction temperature to 90°C, continue stirring and reacting for 4-6 hours, then place the precursor sol in the oven, and evaporate the water until it becomes a dry gel .

[0025] Grind the obtained dry glue into powder, take 24g of the powder and a mixed solution of 45.8g morpholine and 53.2g water (volume ratio is 1:1) and fully mix them under stirring, place in a stainless steel autoclave, and seal the autoclave Then crystallize at 180°C for 5 days. Finally, after cooling the autoclave to room temperature, the resulting mixture was fully washed with water, filtered, dried at 120°C for 4 hours, and ca...

Embodiment 3

[0028] According to the method and steps of Example 1, but changing the amount of silica sol, the molar ratio of each component in the precursor sol is respectively:

[0029] Al 2 o 3 :P 2 o 5 : SiO 2 =1:1:0.4, the rest are the same as in Example 1. The obtained sample was determined by X-diffraction, and the result was similar to Example 1, all of which were SAPO-34 molecular sieves, but the intensity of individual diffraction peaks was slightly different.

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Abstract

The invention discloses a method to prepare SAPO-34 molecule sieve through liquid phase crystallization: the precursor compounds of aluminum, silicon and phosphorous are prepared into dry gel, then the dry gel powder and a water solution of organic amine template are placed in a stainless steel high pressure vessel, and the SAPO-34 molecule sieve is synthesized through liquid crystallization. The molecule sieve after being treated can be used for a catalyst for transferring methanol into low carbon olefins. The method solves the wall sticking trouble of hydrothermal synthesis, and has the advantages of simple preparation process, good crystallization degree, simple equipments, and a normal high pressure stainless steel reaction boil can be adopted in the crystallization process, which is beneficial to industrialized mass production, and the organic amine template can be recycled.

Description

technical field [0001] The present invention relates to a kind of preparation method of SAPO-34 molecular sieve, specifically, the present invention relates to the method for preparing SAPO-34 molecular sieve by liquid phase crystallization method. Background technique [0002] Silicoaluminophosphate molecular sieves are another large class of molecular sieve catalytic materials besides silica-alumina zeolite molecular sieves. They have been widely used in petrochemical and petroleum processing. Among them, the SAPO-34 molecular sieve has a chabazite-like structure and belongs to small-pore zeolites, which can be used as adsorbents and catalysts, especially in the reaction of methanol to olefins (MTO), showing good catalytic activity and selectivity. The classic method for preparing SAPO-34 molecular sieve is the hydrothermal synthesis method (USP4440871, CN1037334C, CN1038125C, CN1048428C), that is, the crystallization of silicoaluminophosphate gel in a high temperature hyd...

Claims

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Application Information

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IPC IPC(8): C01B39/54C01B37/08
Inventor 张毅航张秀成程惠亭李建青段文杰陈立宇王晓梅
Owner HUALU ENG & TECH
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