Method for preparing ZSM-5 molecular sieves

A technology of ZSM-5 and molecular sieve, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problem of synthetic molecular sieve materials that have not yet been seen from silicon-aluminum sources, and achieve the purpose of broadening the range of raw materials, Effects of improving performance and reducing manufacturing cost

Active Publication Date: 2010-06-09
邵武绿闽环保科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Take rectorite as raw material to prepare the research of catalytic material at present and mainly focus on utilizing its interlayer to have the characteristic of exchangeable cation to prepare layer pillar clay material (such as Chinese patent publication CN1071945A, CN1211608A, CN1353012A etc.), do not yet see rectorite as A report on the synthesis of molecular sieve materials by providing some or all of the silicon and aluminum sources as raw materials

Method used

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  • Method for preparing ZSM-5 molecular sieves

Examples

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Effect test

Embodiment 1

[0040] Using commercially available rectorite (produced by Hubei Mingliu Rectorite Co., Ltd., see Table 1 for its chemical composition) as raw material, 0.69 g was roasted in a muffle furnace at 800° C. for 2 h, and then used.

[0041] Water glass (containing SiO 2 26wt.%, Na 2 O 8wt.%) 19.7g, TPABr 2.04g, distilled water 95g, concentration is that the rectorite after the sulfuric acid aqueous solution 2.3g of 3M and roasting process joins in the beaker, mixes and stirs 1h and obtains mixture gel (this moment system pH value is about for 9). The components in the gel are calculated as oxides, and the molar ratio is SiO 2 / Al 2 o 3 ≈35, (Na 2 O+K 2 O) / SiO 2 =0.2,H 2 O / SiO 2 =70, TPABr / SiO 2 = 0.09. The mixed gel was moved into a stainless steel crystallization kettle lined with polytetrafluoroethylene, heated to 170°C, and statically crystallized for 72 hours. After the crystallization is completed, the mother liquor is removed by cooling and filtering, and then th...

Embodiment 2

[0046] Commercially available rectorite was used as raw material, and 0.9 g was calcined in a muffle furnace at 900° C. for 4 h before use.

[0047] Water glass (containing SiO 2 26wt%, Na 2 O 8wt%) 18g, TPABr 1.03g, distilled water 59g, concentration is that the sulfuric acid aqueous solution 2g of 3M and the rectorite after roasting process join in the beaker, mix and stir 1h to obtain mixture gel (this moment system pH value is about 10) . The components in the gel are calculated as oxides, and the molar ratio is SiO 2 / Al 2 o 3 ≈22, (Na 2 O+K 2 O) / SiO 2 =0.2,H 2 O / SiO 2 =50, TPABr / SiO 2 = 0.05. Move the mixture gel into a stainless steel crystallization kettle lined with polytetrafluoroethylene, raise the temperature to 175°C, and crystallize statically for 48 hours, then cool and filter to remove the mother liquor, then wash, dry, and roast at 550°C to remove the template agent A crystallized product was obtained.

[0048] According to XRD measurement, the p...

Embodiment 3

[0050] Commercially available rectorite was used as raw material, and 0.5 g was calcined in a muffle furnace at 1000° C. for 1 h, and then used.

[0051] Water glass (containing SiO 2 26wt%, Na 2 O 8wt%) 25g, TPABr 1.15g, distilled water 65g, concentration is that 3M sulfuric acid aqueous solution 2g and the rectorite after roasting process join in the beaker, mix and stir 1h to obtain mixture gel (this moment system pH value is about 10) . Each component in the gel is SiO according to its oxide molar ratio 2 / Al 2 o 3 ≈50, (Na 2 O+K 2 O) / SiO 2 =0.3,H 2 O / SiO 2 =42, TPABr / SiO 2 = 0.04. Move the mixed gel into a stainless steel crystallization kettle lined with polytetrafluoroethylene, raise the temperature to 165°C, and crystallize statically for 72 hours, then cool and filter to remove the mother liquor, then wash, dry, and roast at 550°C to remove the template agent A crystallized product was obtained.

[0052] According to XRD measurement, the phase of the pro...

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Abstract

The invention provides a method for preparing ZSM-5 molecular sieves, which are prepared by using a natural rectorite mineral to provide an aluminum source and part of silicon source for synthesizing molecular sieves, and by adding a template agent to perform crystallization reaction under a hydrothermal condition. The implementation of the method of the invention expands the range of the raw materials for synthesizing the ZSM-5 molecular sieves, opens a new application field of natural rectorite and provides the ZSM-5 molecular sieves with high stability.

Description

technical field [0001] The invention belongs to the field of petrochemical industry, and relates to a preparation technology of ZSM-5 molecular sieve, in particular to using natural minerals to provide all the aluminum sources and part of the silicon sources required for synthesizing ZSM-5 molecular sieves, and synthesizing ZSM-5 type molecular sieves by using templates at the same time craft. Background technique [0002] ZSM-5 molecular sieve is a molecular sieve with a high-silicon three-dimensional straight channel structure first reported by Mobil Corporation of the United States in 1972 (USP3702886). The unique pore structure of ZSM-5 molecular sieve makes it have the effect of shape-selective catalysis, and it is widely used in reactions such as alkylation, isomerization, disproportionation, catalytic cracking, methanol to gasoline, heavy oil deep cracking, methanol to olefins, etc. catalyst or catalyst support. Since the pores of the ZSM-5 molecular sieve only allo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38
Inventor 刘海燕鲍晓军曹丽媛范煜石冈
Owner 邵武绿闽环保科技有限公司
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