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A kind of highly dispersed small grain ZSM-5 molecular sieve and preparation method thereof

A ZSM-5, molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of irregular crystal form and easy agglomeration, and achieve regular crystal form and difficult to agglomerate. , increasing the effect of steric hindrance

Active Publication Date: 2017-09-01
PETROCHINA CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The present invention aims at the above-mentioned problems such as easy agglomeration of nanometer and submicron molecular sieves, and mainly solves the problem of low-silicon-aluminum-ratio small-grain ZSM-5 zeolite molecular sieves in the prior art, especially nanometer and submicron size, which have irregular crystal forms and are easy to agglomerate. Problem, provide a kind of highly dispersed small grain ZSM-5 molecular sieve and preparation method thereof

Method used

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  • A kind of highly dispersed small grain ZSM-5 molecular sieve and preparation method thereof
  • A kind of highly dispersed small grain ZSM-5 molecular sieve and preparation method thereof
  • A kind of highly dispersed small grain ZSM-5 molecular sieve and preparation method thereof

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Effect test

Embodiment 1

[0064] Take 6g of NaOH, add 80g of deionized water to it, make it fully dissolved, then add 10g of urea, stir and dissolve, put it in -20°C environment for 2 hours and refrigerate it for 2 hours; take 4g of cotton linter pulp, add the above NaOH / Degrade in urea / water solution, centrifuge to obtain degradation solution, and store at -10°C. Take 18g of sodium hydroxide, 4g of sodium metaaluminate, and 40g of tetrapropylammonium bromide, and dissolve them in 150g of deionized water; take 250g of silica sol and 30g of degradation solution, and slowly add them dropwise to the aluminum salt solution, and then add NaOH Adjust the pH value to 14; put the reaction mixture into a reaction kettle, crystallize at 100°C for 36 hours, then raise the temperature to 170°C, and crystallize for 24 hours. After filtering, washing and drying, the average grain size of the obtained product is About 100nm, SiO 2 / Al 2 o 3 for 30. Its XRD pattern is as figure 1 As shown, the SEM image is shown...

Embodiment 2

[0066] Take 7g of NaOH, add 80g of deionized water to it, make it fully dissolved, then add 12g of urea, stir and dissolve, put it in -20℃ for 2 hours; take 4g of cotton linter pulp, add the above NaOH / Degrade in urea / water solution, centrifuge to obtain degradation solution, and store at -10°C. Take 20g of sodium hydroxide, 6.8g of aluminum isopropoxide, and 40g of tetrapropylammonium bromide, and dissolve them with 250g of deionized water; take 100g of white carbon black and 30g of degradation solution, and slowly add them dropwise to the aluminum salt solution, and then Add NaOH to adjust the pH value to 14; put the reaction mixture into the reaction kettle, crystallize at 100°C for 36 hours, then raise the temperature to 170°C, and crystallize for 24 hours. After filtering, washing and drying, the average crystal grain The size is around 70nm, SiO 2 / Al 2 o 3 for 40.

Embodiment 3

[0068] Take 6g of NaOH, add 80g of deionized water to it, make it fully dissolved, then add 10g of urea, stir and dissolve, put it in -20°C environment for 2 hours and refrigerate it for 2 hours; take 4g of cotton linter pulp, add the above NaOH / Degrade in urea / water solution, centrifuge to obtain degradation solution, and store at -10°C. Take 20g of sodium hydroxide, 2g of sodium metaaluminate, and 40g of tetrapropylammonium bromide, and dissolve them in 250g of deionized water; take 100g of coarse-pore silica gel and 30g of degradation solution, and slowly add them dropwise to the aluminum salt solution, and then add Adjust the pH value to 14 with NaOH; put the reaction mixture into a reaction kettle, crystallize at 100°C for 36 hours, then raise the temperature to 170°C, and crystallize for 24 hours. After filtering, washing and drying, the average grain size of the obtained product is Around 100nm, SiO 2 / Al 2 o 3 for 50.

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Abstract

The invention discloses a highly-dispersed small grain ZSM-5 zeolite and a preparation method thereof. The ratio of silicate to aluminum of the zeolite is 20 to 150; the grain size of the zeolite is 50 to 500 nm. The method comprises the following steps: dissolving cellulose in a mixed solution of sodium hydroxide / urea / water, stirring to degrade, centrifuging to obtain a degradation solution A and standing; dissolving the sodium hydroxide, an aluminum salt and a template by using water to obtain an aluminum salt solution B; adding the degradation solution A into the aluminum salt solution B and mixing uniformly to enable the molar ratio of various components of the mixed solution to be that SiO2:Al2O3:H2O:the template is (20-150):1:(130-3,000):(1-20); then, adding the sodium hydroxide to regulate the pH value to be alkali; crystallizing a mixture of which the pH value is regulated; processing to obtain the ZSM-5 zeolite. The obtained ZSM-5 zeolite is uniform in grain size, and high in dispersibility.

Description

technical field [0001] The invention belongs to the field of molecular sieve synthesis, and in particular relates to a highly dispersed small-grain ZSM-5 molecular sieve and a preparation method thereof. Background technique [0002] ZSM-5 molecular sieve (USP 3702886) is an aluminosilicate zeolite molecular sieve developed by Mobil Corporation of the United States. It is bent in a Z shape, the corner of the channel is about 150°, and the hole diameter is The channel of the ten-membered ring parallel to the c-axis is linear, and the diameter of the elliptical channel is This special pore structure and size make it have good shape-selective properties, and at the same time have the advantages of adjustable silicon-aluminum ratio, lipophilicity, thermal stability and high catalytic activity, so it has become one of the most important molecular sieve catalytic materials at present. , Widely used in catalytic fields such as petroleum processing, coal chemical industry and fi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/40
Inventor 巩雁军马通王洪华王久江胡清勋赵红娟王宝杰张莉熊晓云赵晓争高永福刘明霞侯凯军曹庚振杨周侠田爱珍
Owner PETROCHINA CO LTD