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Preparation method of low-silicon SAPO-34 molecular sieve

A technology of molecular sieve and silicon source, which is applied in the field of preparation of SAPO-34 molecular sieve, can solve the problems of shortening the induction period, poor repeatability, and difficulty in synthesis, and achieve the effect of shortening the induction period, simplifying the preparation process, and good amplification repeatability

Active Publication Date: 2015-04-29
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Therefore, the present invention aims at the shortcomings of difficult synthesis, poor repeatability, and many steps in the prior art, and provides a method for synthesizing low-silicon SAPO-34 molecular sieves. The synthesized SAPO-34 molecular sieves can shorten the induction period

Method used

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  • Preparation method of low-silicon SAPO-34 molecular sieve
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  • Preparation method of low-silicon SAPO-34 molecular sieve

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preparation example Construction

[0019] The preparation method of the low-silicon SAPO-34 molecular sieve provided by the present invention is characterized in that it comprises the following steps: (1) according to (0.7~2)P 2 o 5 :(0.01~0.2)SiO2 2 :Al 2 o 3 :(20~100)H 2 The molar ratio of O, mix the silicon source, phosphorus source and aluminum source evenly, and dry to obtain a silicon-phosphor-aluminum dry glue with a solid content of not less than 60%; (2) contact and mix the silicon-phosphorus-aluminum dry glue with a template agent to obtain a mixture , wherein, 1 mole of Al in silicon phosphorus aluminum dry glue 2 o 3 In other words, the amount of template added is 1 to 2.5 moles; (3) the mixture B is placed in a closed reactor to crystallize under autogenous pressure and the product is recovered, wherein the crystallization is from low to high The temperature range is divided into three sections sequentially. The crystallization temperature of the adjacent two sections is different and the cry...

Embodiment 1

[0039] The same proportion and steps as Comparative Example 3, the difference is that the crystallization of the mixture is crystallized in stages, after aging at room temperature for 10 hours, crystallization at 150°C for 10 hours, and crystallization at 200°C for 40 hours, take out the crystallization when the temperature of the reactor drops to room temperature The product, the sample is filtered or centrifuged and washed with deionized water until neutral, the sample is dried in a constant temperature drying oven at 80-120°C, and finally placed in a roasting furnace at a constant temperature of 550°C for 5 hours.

[0040] Gained sample is measured through XRD diffraction and scanning electron microscope, and its XRD diffraction pattern is shown in image 3 , SEM photo see Figure 4 . The XRD spectrum shows that it is a pure-phase SAPO-34 molecular sieve; the SEM photo shows that the grains are regular, the grains are cubic, and the average grain size is 500nm.

Embodiment 2

[0042] Weigh 7g of SB powder and dissolve it in 25g of deionized water, stir rapidly for 1 hour, mix with the solution formed by adding 9.2g of 85% orthophosphoric acid into 30g of deionized water and stir evenly, then add 1g of 30% acidic silica sol, and stir rapidly to obtain a mixture , stirred in a constant temperature water bath at 70°C for 12h, and dried the mixture at 100°C for 24h to obtain a silicon-phosphoraluminum glue with a solid content of 85%.

[0043] Transfer the silica-phosphoraluminum glue to a 100 mL stainless steel autoclave, add 27 g of tetraethylammonium hydroxide and 2 g of triethylamine, and stir for 2 h to obtain a mixture. Segmented crystallization: aging at room temperature for 10 hours, crystallization at 150°C for 10 hours, and crystallization at 200°C for 40 hours. When the temperature of the autoclave dropped to room temperature, the crystallized product was taken out, filtered or centrifuged and washed with deionized water until neutral, and the...

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Abstract

The invention discloses a preparation method of a low-silicon SAPO-34 molecular sieve, which is characterized by comprising the following steps: (1) uniformly mixing a silicon source, a phosphorus source and an aluminum source according to the mol ratio of (0.7-2)P2O5:(0.01-0.2)SiO2:Al2O3:(20-100)H2O, and drying to obtain silicon phosphorus aluminum dry glue with the solid content of not lower than 60%; (2) uniformly contacting and mixing the silicon phosphorus aluminum dry glue with a template and a silicon source to obtain a mixture, wherein the addition amount of the template is 1-2.5 mol on the basis of 1 mol of Al2O3 in the silicon phosphorus aluminum dry glue; and (3) putting the mixture in a closed reaction kettle, sectionally crystallizing under autogenous pressure, and recovering the product.

Description

technical field [0001] The present invention relates to a kind of preparation method of SAPO-34 molecular sieve, relate to a kind of preparation method of low silicon SAPO-34 molecular sieve more specifically. Background technique [0002] SAPO-34 molecular sieve is a phosphorus silicon aluminum molecular sieve developed by United Carbide Chemical Company in 1984. It belongs to the eight-membered ring chabazite CHA structure, cubic crystal system, the eight-membered ring pore size is 0.43nm, and the molecular dynamics of ethylene and propylene The diameter is similar. SAPO-34 molecular sieve has suitable acid strength, total acid content and good hydrothermal stability, and exhibits excellent catalytic performance in methanol to light olefins (MTO). [0003] In the past thirty years, researchers at home and abroad have done a lot of work on the synthesis of SAPO-34 molecular sieves. There are many methods for the synthesis of SAPO-34 molecular sieve, such as hydrothermal s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08B01J29/85C07C1/20C07C11/02
Inventor 杨冬清王永睿慕旭宏舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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