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Preparation method of SAPO-34 molecular sieve

A technology of SAPO-34 and molecular sieve, applied in the field of preparation of SAPO-34 molecular sieve, can solve the problems of difficult solid-liquid separation, material loss and high cost, and achieve the effects of large specific surface area, easy operation and simple steps

Active Publication Date: 2014-09-24
VALIANT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0013] The technical problem to be solved by the present invention is to provide a preparation method of SAPO-34 molecular sieve, which overcomes the high cost of the existing preparation method, and the preparation of particles with a grain size less than 5 μm has serious material leakage, solid-liquid separation is difficult, and the material Defects such as serious loss

Method used

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  • Preparation method of SAPO-34 molecular sieve

Examples

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Effect test

Embodiment 1

[0047] Under stirring at room temperature, 105.8g of pseudo-boehmite (Al 2 o 3 Content is 76.5%) drop into 500g deionized water, then add 183.0g orthophosphoric acid (H 3 PO 4 content is 85%) and 183.0g deionized water, increase the stirring speed to 600 rpm, after stirring for 2h, add 63.5g silica sol (SiO 2 content is 30%) and 38.5g deionized water, 186.7g morpholine, and 162.9g TMAmOH aqueous solution (TMAmOH content is 25%) and 40.0g deionized water, increase stirring speed to 800 rev / min, form uniform after stirring 5h Gel; then transfer the gel to a 2L crystallization kettle, add 3g of seed crystal mixture (0.95g of seed crystal content), set the stirring speed at 120 rpm, and heat up to 190°C for crystallization 24h. After the crystallization is completed, the mixed solution is filtered, washed, dried, roasted and other post-treatments to obtain the target product, which is named B. After XRD and SEM characterization tests, it is found that the target product B pre...

Embodiment 2

[0049] Under stirring at room temperature, 115.6g of aluminum hydroxide was dropped into 750g of deionized water, and then 170.8g of orthophosphoric acid (H 3 PO 4 content is 85%) and 170g deionized water, increase the stirring speed to 600 rpm, after stirring for 2h, add 88.9g silica sol (SiO 2 content is 30%) and 48.4g deionized water, 209.5g triethylamine, and 124.8g TMAdOH aqueous solution (TMAdOH content is 25%) and 50.0g deionized water, increase the stirring speed to 800 rpm, and form a uniform mixture after stirring for 2 hours Gel; then transfer the gel to a 2L crystallization kettle, add 3g of seed crystal mixture solution (seed crystal content is 0.76g), set the stirring speed to 100 rpm, and heat up to 180°C for crystallization 48h. After the crystallization is completed, the mixed solution is filtered, washed, dried, roasted and other post-treatments to obtain the target product, which is named C. After XRD and SEM characterization tests, it was found that the ...

Embodiment 3

[0051] Under stirring at room temperature, 123.8g of aluminum hydroxide was dropped into 600.0g of deionized water, and then 183.0g of orthophosphoric acid (H 3 PO 4 content is 85%) and 183.0g deionized water, increase the stirring speed to 600 rpm, after stirring for 2h, continuously add 95.2g silica sol (SiO 2 content is 30%) and 42.6g deionized water, 192.4g triethylamine, and 50.5g aqueous solution of N-methyl-3-quinoniol hydroxide (N-methyl-3-quinoniol hydroxide content is 25 %) and 30.0g deionized water, increase the stirring speed to 800 rpm, and form a uniform gel after stirring for 2h; then transfer the gel to a 2L crystallization kettle, and add 3g seed crystal mixed solution (seed crystal content 0.81g), the stirring speed was set at 80 rpm, and the temperature was raised to 180°C for 48 hours of crystallization. After the crystallization is completed, the mixed solution is filtered, washed, dried, roasted and other post-treatments to obtain the target product, wh...

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Abstract

The invention relates to a preparation method of a SAPO-34 molecular sieve. The raw materials are as followings: a template R, an auxiliary template R', a phosphorus source, a silicon source, an aluminum source and deionized water in the molar ratio of 1-3:0-0.3:1.8-2.2:0.3-0.6:1:50-180. The method comprises the steps of: (1) evenly mixing and stirring the aluminum source, phosphorus source and part of the deionized water; (2) sequentially adding the silicon source, template agent R, auxiliary template R' and the rest of the deionized water into the above mixed solution to obtain a gel; and (3) transferring the gel to a crystallization kettle, adding seed crystal, crystallizing, filtering, washing, drying and roasting to obtain the SAPO-34 molecular sieve. Due to the addition of the small amount of auxiliary template R 'and seed crystal, the prepared cubic crystal has high degree of crystallinity and structured crystal form, and the product has large specific surface area and high acid content, shows a great prospect for industrialization, and is expected to be used as a catalyst for low carbon olefin preparation from methanol and automobile tail gas treatment.

Description

technical field [0001] The invention relates to a preparation method of SAPO-34 molecular sieve, in particular to a method for preparing SAPO-34 molecular sieve with uniform grain size and adjustable within the range of 1-20 μm by using auxiliary template agent R'. Background technique [0002] In 1984, UCC developed a series of silicoaluminophosphate molecular sieves (SAPO-n), which are made of SiO 2 , AlO 2 ～ 、PO 2 + , a microporous crystal composed of three tetrahedral units, where n represents a different crystal structure. SAPO-34 is a member of the SAPO series of molecular sieves, and it is also the most eye-catching one. Its window aperture is between 0.43 and 0.50nm. The crystal structure of SAPO-34 is very similar to that of the natural product chabazite, and it belongs to the CHA structure according to the regulations of the International Zeolite and Molecular Sieve Association (IZA). Although SAPO-34 has not appeared for a long time, due to its suitable pore...

Claims

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Application Information

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IPC IPC(8): C01B39/54C03B37/08
Inventor 张文于成龙矫志陈士辉王春勇杨腾
Owner VALIANT CO LTD
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