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A kind of preparation method of hedgehog spherical suz-4

A SUZ-4, spherical technology, applied in the field of silicon, can solve problems such as no recurrence, and achieve the effect of reducing production costs

Active Publication Date: 2020-07-03
CHINA CATALYST HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] So far, there have been no reports on the synthesis of SUZ-4 molecular sieves for the synthesis of new templates

Method used

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  • A kind of preparation method of hedgehog spherical suz-4
  • A kind of preparation method of hedgehog spherical suz-4
  • A kind of preparation method of hedgehog spherical suz-4

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 2.48g of aluminum isopropoxide and 5.82g of KOH (85%) to 37.96g of deionized water to form solution A, and stir for 0.5h to completely dissolve the aluminum source. Add 30.01 g of silica sol (40%), 2.55 g of ethylenediamine, and 6.01 g of cyclohexylamine into 30 g of deionized water, mix and stir evenly to form solution B. Then A solution and B solution were mixed and stirred for 1 h to form a white gel. The formed gel was transferred to a 170ml polytetrafluoroethylene reactor, dynamically rotated at a speed of 20r / min, and crystallized at 150°C for 4 days. The obtained sample was washed, dried at 120°C, and calcined at 550°C for 6 hours to obtain SUZ-4 molecular sieve with a crystallinity of 85%. Its XRD spectrum is attached figure 1 .

[0028] Initial gel molar composition: 33.3SiO 2 :Al 2 o 3 :14.7KOH:7EDA:10CHA:798H 2 o

Embodiment 2

[0030] Add 2.48g of aluminum isopropoxide and 5.82g of KOH (85%) to 37.96g of deionized water to form solution A, and stir for 0.5h to completely dissolve the aluminum source. Add 30.01 g of silica sol (40%), 2.19 g of ethylenediamine, and 6.01 g of cyclohexylamine into 30 g of deionized water, mix and stir evenly to form solution B. Then A solution and B solution were mixed and stirred for 1 h to form a white gel. The formed gel was transferred to a 170ml polytetrafluoroethylene reactor, dynamically rotated at a speed of 20r / min, and crystallized at 150°C for 4 days. The obtained sample was washed, dried at 120°C, and calcined at 550°C for 6 hours to obtain a pure SUZ-4 molecular sieve with a crystallinity of 98%, and a Si / Al ratio of 15.6 as measured by an X-ray fluorescence spectrometer. attached figure 2 The XRD spectrum of the sample obtained in this example is given. attached image 3 The SEM image of the sample obtained in this example is given.

[0031] Initial g...

Embodiment 3

[0033] Add 2.48g of aluminum isopropoxide and 5.82g of KOH (85%) to 37.96g of deionized water to form solution A, and stir for 0.5h to completely dissolve the aluminum source. Add 30.01 g of silica sol (40%), 1.82 g of ethylenediamine, and 6.01 g of cyclohexylamine into 30 g of deionized water, mix and stir evenly to form solution B. Then A solution and B solution were mixed and stirred for 1 h to form a white gel. The formed gel was transferred to a 170ml polytetrafluoroethylene reactor, dynamically rotated at a speed of 20r / min, and crystallized at 150°C for 4 days. The obtained sample was washed, dried at 120° C., and calcined at 550° C. for 6 hours. The spectrum of the sample in this experiment was the same as in Example 2, except that the crystallinity was 80%.

[0034] Initial gel molar composition: 33.3SiO 2 :Al 2 o 3 :14.7KOH:5EDA:10CHA:798H 2 o

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Abstract

The invention aims to provide a preparation method for synthesizing a SUZ-4 molecular sieve by using a novel cheap template agent. Firstly, preparing a silicon-aluminum mixed glue solution, and then adding a template agent of ethylenediamine (EDA) and cyclic ethylamine (CHA) into the mixed glue solution according to an arbitrary ratio for mixing, then adding the mixture into a reaction kettle forhigh-temperature crystallization growth; wherein the crystallization temperature is 130-170 DEG C, and the crystallization time is 2-5 days, and finally synthesizing the hedgehog spherical SUZ-4 molecular sieve generated by the cheap template agent. The method is simple in process and convenient to operate, not only greatly reduces the synthesis cost of the molecular sieve, but also obtains the hedgehog spherical SUZ-4 molecular sieve.

Description

technical field [0001] The invention belongs to the technical field of silicon and aluminum oxide molecular sieves, and in particular relates to the preparation of hedgehog-shaped SUZ-4 by mixing two relatively cheap templates. [0002] technical background [0003] In 1992, the British BP company first discovered and prepared SUZ-4 molecular sieve. Barri et al. in containing Si0 2 ,Al 2 0 3 , The initial gel of KOH and NaOH mixture was added with organic tetraethyl hydroxide (TEAOH) and quinuclidine as templates to synthesize SUZ-4 molecular sieves. This is the first synthesis of this molecular sieve, but the poor repeatability of the synthesis method hinders the research and development of SUZ-4 molecular sieve to a certain extent. [0004] In 1999, Asensi et al. improved the reproducibility of SUZ-4 molecular sieve synthesis. They used a new initial gel ratio - 21.2Si0 at a temperature of 150 °C. 2 :Al 2 0 3 :7.9KOH:2.6TEAOH:498.6H 2 0 (molar ratio), there is no Na...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/48
CPCC01B39/48C01P2002/72
Inventor 蒋山高晓坤王炳春李进王建青
Owner CHINA CATALYST HLDG CO LTD
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