Synthetic method of MgSAPO-31 molecular sieve

A synthesis method, the technology of mgsapo-31, is applied in the direction of molecular sieve and alkali-exchanged phosphate, molecular sieve characteristic silicoaluminophosphate, etc., which can solve the problem of easy formation of miscellaneous crystals in crystallization products, and achieve flexible modulation and high acid site density. , the effect of high purity

Inactive Publication Date: 2014-01-01
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to solve the problem that only MgAPO-31 or SAPO-31 molecular sieves with one acidic site can be synthesized by traditional silicon and aluminum sources, and miscellaneous crystals are easily formed in crystallized products, and provide a simultaneous Synthesis of MgSAPO-31 Novel Molecular Sieves with Two Acid Sites with Different Acid Strengths

Method used

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  • Synthetic method of MgSAPO-31 molecular sieve
  • Synthetic method of MgSAPO-31 molecular sieve
  • Synthetic method of MgSAPO-31 molecular sieve

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specific Embodiment approach 1

[0022] Specific embodiment one: the synthetic method of present embodiment MgSAPO-31 molecular sieve is implemented according to the following steps:

[0023] 1. Disperse NaX molecular sieves in magnesium nitrate solution or magnesium acetate solution, and perform ion exchange at a temperature of 50-80 ° C. The number of exchanges is 1-4 times, and each exchange is 1-6 hours to obtain Mg / NaX molecular sieves;

[0024] Two, the mass fraction is 85% phosphoric acid, pseudo-boehmite, Mg / NaX molecular sieve obtained in step 1, di-n-butylamine and deionized water according to 1: (0-0.7): (0.05-1.2): ( 0.5~1.5): (2~7.0) for mixing in parts by weight, fully stirring at a speed of 500~1000r / min for 3~7 hours to obtain an initial gel;

[0025] 3. Place the initial gel obtained in step 2 in a crystallization kettle lined with polytetrafluoroethylene, crystallize at 170-190°C for 12-48 hours, and then cool to room temperature. The crystallized product is centrifuged, washed, and After d...

specific Embodiment approach 2

[0029] Embodiment 2: This embodiment differs from Embodiment 1 in that the concentration of the magnesium nitrate solution or magnesium acetate solution described in Step 1 is 0.1-0.4 mol / L. Other steps and parameters are the same as those in Embodiment 1.

specific Embodiment approach 3

[0030] Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that in step 1, the NaX molecular sieve is dispersed in the magnesium nitrate solution or the magnesium acetate solution according to the solid-to-liquid ratio of 1:20-40. Other steps and parameters are the same as those in Embodiment 1 or Embodiment 2.

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Abstract

The invention discloses a synthetic method of a MgSAPO-31 molecular sieve, relating to a synthetic method of a molecular sieve, and aiming to solve the problems that only a molecular sieve with an acid site can be synthesized at present by adopting the conventional silicon source and aluminum source and mixed crystals are easily formed in a crystallized product. The synthetic method comprises the steps of 1, dispersing a NaX molecular sieve into a magnesium nitrate solution or magnesium acetate solution to perform ion exchange, and controlling the exchange frequency and exchange time to obtain a Mg/NaX molecular sieve; 2, mixing phosphoric acid, pseudo-boehmite, the Mg/NaX molecular sieve, di-n-butylamine and deionized water, and stirring to obtain an initial gel; 3, putting the initial gel into a crystallization kettle, performing crystallization at 170-190 DEG C, performing centrifugal separation, washing and drying on a crystallization product, and then roasting to obtain a molecular sieve. According to the synthetic method disclosed by the invention, a molecular sieve framework contains two acid sites of Si and Mg with different strengths at the same time, the preparation purity is high, and the molecular sieve can be used as a catalyst applied to the fields of petrochemical industry and the like.

Description

technical field [0001] The invention relates to a synthesis method of molecular sieves, in particular to a method for simultaneously replacing aluminum phosphate molecular sieves AlPO with Mg and Si 4 The preparation method of the MgSAPO-31 molecular sieve of -31. Background technique [0002] In 1984, Lok et al. successfully introduced Si into AlPO 4 Among the series of molecular sieves, a series of silicoaluminophosphate molecular sieves (SAPO-n) with negatively charged skeletons, exchangeable cations and proton acidity were synthesized. Among them, the mesoporous SAPO-31 molecular sieve has suitable pore size and temperature acidity, As a catalyst for alkylation, amination and isomerization reactions, it has broad application prospects in petroleum refining, petrochemical and other fields. U.S. Patent USP4,1984,440:871 and the synthesis of the SAPO-31 molecular sieve of follow-up work report usually adopt dipropylamine to make template agent, take aluminum isopropoxide ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/08
Inventor 吴伟戚维欣
Owner HEILONGJIANG UNIV
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