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NaY molecular sieve/natural mineral composite material having multistage pore structure and preparation method thereof

A technology of natural minerals and composite materials, which is applied in the directions of crystalline aluminosilicate zeolite, octahedral crystalline aluminosilicate zeolite, etc., can solve the problems of high material preparation cost, long process route, pollution discharge, etc., and achieves reduction of synthesis cost, The effect of broadening the application field and reducing the preparation cost

Active Publication Date: 2013-04-17
PETROCHINA CO LTD +1
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AI Technical Summary

Problems solved by technology

[0011] The previously reported methods for synthesizing Y-type molecular sieve / natural mineral composite materials need to add an external silicon source or aluminum source to adjust the silicon-aluminum ratio of the synthesis system. Most of these chemical raw materials are produced from natural minerals through complicated reaction and separation processes. The process route is long, the consumption of energy and materials is high, and most of the processes have serious pollution emissions
In addition, few of the composite materials reported in the past have a multi-level pore structure composed of micropores, mesoporous pores, and macropores, and can only form composite materials of micropores and macropores or micropores and mesoporous pores, and the mesopores in the composites The formation is formed by the introduction or post-treatment of the template agent, the preparation process is complicated, and the cost of material preparation is relatively high

Method used

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  • NaY molecular sieve/natural mineral composite material having multistage pore structure and preparation method thereof
  • NaY molecular sieve/natural mineral composite material having multistage pore structure and preparation method thereof
  • NaY molecular sieve/natural mineral composite material having multistage pore structure and preparation method thereof

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preparation example Construction

[0024] The preparation method of the NaY molecular sieve / natural mineral composite material with hierarchical porous structure of the present invention comprises the following steps:

[0025] (1) Diatomite minerals and kaolin minerals are mixed according to the mass ratio of 1: 0.8 to 3;

[0026] (2) molding the mixture obtained in step (1) under the action of water, roasting the molded product at 650°C to 850°C, and then crushing and sieving to obtain mineral particle raw materials;

[0027](3) mixing the mineral particle raw material obtained in step (2) with a directing agent, sodium hydroxide and water, aging at 40°C to 65°C, and then hydrothermally crystallizing at 90°C to 110°C;

[0028] (4) cooling and filtering the crystallized product obtained in step (3) to remove the mother liquor, washing the filter cake with deionized water until the pH is below 10, and drying to obtain a NaY molecular sieve / natural mineral composite material with a hierarchical pore structure.

...

Embodiment 1

[0044] Dissolve 27.2 grams (g) of sodium hydroxide solid (produced by Beijing Chemical Plant, with a purity of 99%) in 38 g of water, cool to room temperature, and set aside. Get 26.66g aluminum sulfate (molecular formula: Al 2 (SO 4 ) 3 18H 2 (0, Beijing Yili Fine Chemicals Co., Ltd., with a purity of 99%) was dissolved in 38g of water, and the prepared aluminum sulfate solution was dissolved in sodium hydroxide solution to make a high-alkali sodium metaaluminate solution. With 96.63g sodium silicate (molecular formula: Na 2 SiO 3 9H 2 O, Beijing Modern Chemical Reagent Company, the purity is 99%) was dissolved in 115g water, added 82g silica sol (Qingdao Ocean Chemical Co., Ltd, SiO 2 The content is 30.0%, Na 2 O content is 0.06%), stirring rapidly for 2 hours. Then add high alkali sodium metaaluminate solution under stirring condition, mix evenly, stir and age at 30° C. for 4 hours, and stand and age at room temperature for 2 days to obtain a directing agent liquid....

Embodiment 2

[0049] The preparation of the directing agent liquid is the same as in Example 1.

[0050] Mix commercially available diatomite and kaolin at a mass ratio of 1:2, add water to extrude into strips, dry the strips and break them into particles with a particle size of 50 to 100 μm, and bake them at 820°C for 4 hours. spare.

[0051] Dissolve 6.2g of sodium hydroxide solid (produced by Beijing Chemical Plant, with a purity of 99%) in 40g of distilled water, add 7.8g of directing agent liquid, mix with 6g of the above-mentioned roasted particles, stir for about 1 hour, and heat at 60°C Let stand and age for 15 hours.

[0052]The above mixture was poured into a stainless steel crystallization kettle lined with polytetrafluoroethylene, heated to 95°C, and left to stand for crystallization for 20 hours. After the crystallization is completed, the mother liquor is removed by cooling and filtering, and the solid phase product is washed and dried to obtain a crystallized product. Acco...

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Abstract

The invention belongs to the technical field of petrochemical industry, and relates to a NaY molecular sieve / natural mineral composite material having a multistage pore structure and a preparation method thereof. The composite material is a crystal product formed through in-situ crystallization by taking a natural kaolin mineral and a natural kieselguhr mineral as entire silicon sources and aluminum sources for molecular sieve synthesis and using the minerals as substrates for molecular sieve growth. In the composite material, the mass percent of the NaY molecular sieve is 25-50%, and the silicon-aluminum ratio of the NaY molecular sieve is 3-5.5. The invention widens the raw material sources in the preparation of the molecular sieve / natural mineral composite material through an in-situ synthesis method, and can simultaneously greatly lower the production cost of the molecular sieve / natural mineral composite material.

Description

technical field [0001] The invention belongs to the field of petrochemical industry, and relates to a NaY molecular sieve / natural mineral composite material with a multi-level pore structure and a preparation method thereof, wherein the natural minerals are kaolin minerals and diatomite minerals, which provide all the materials required for the synthesis of NaY molecular sieves It is a source of silicon and aluminum, and it is used as a matrix or carrier material for the preparation of composite materials. Background technique [0002] The in-situ crystallization technology is the chemically reactive SiO in natural minerals 2 and Al 2 o 3 As part of the silicon source and aluminum source for the synthesis of molecular sieves, it is a synthetic process of growing molecular sieves on the outer surface and inner pore surface of natural minerals together with the external silicon source and aluminum source under certain conditions. [0003] The composite material prepared by ...

Claims

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Application Information

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IPC IPC(8): C01B39/24
Inventor 鲍晓军李铁森刘海燕范煜石冈
Owner PETROCHINA CO LTD
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