Method for synthesizing B-beta-heteroatom molecular sieve

A heteroatomic molecular sieve and crystal seed technology, applied in the field of catalytic chemistry, can solve the problems of large particle size of solid products, long crystallization time, low production efficiency, etc., and achieve easy mass production, reduced product particle size, and crystallization time. reduced effect

Active Publication Date: 2014-06-25
DALIAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] The above method has problems such as complicated operation, long crystallization time, high crystallization temperature, low solid yield, and the particle size of the solid product is relatively large
High crystallization temperature and long crystallization time will result in high energy consumption and low production efficiency

Method used

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  • Method for synthesizing B-beta-heteroatom molecular sieve
  • Method for synthesizing B-beta-heteroatom molecular sieve
  • Method for synthesizing B-beta-heteroatom molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0059] Combine 0.48g borax, 0.15g NaOH, 0.93g NH 4 F was dissolved in 6.85g deionized water, 29.46g TEAOH was added to the above solution under mechanical stirring, after the solids were completely dissolved, 0.27g B-β molecular sieve seeds and 9.0g white carbon black were added to the above solution, continue After stirring for 2.5 h, put the above gel into a stainless steel reactor with PTFE lining, crystallize at 150℃ for 3 d, cool, centrifuge, wash, dry at 100℃ overnight, and then pass 540℃ The raw powder of B-β molecular sieve is obtained after roasting for 3 h. The solid yield is 80%. The characterization results are attached figure 1 , 2 .

Embodiment 2

[0061] Combine 0.48g borax, 0.15g NaOH, 0.74g NH 4 F was dissolved in 6.85g deionized water, 29.46g TEAOH was added to the above solution under mechanical stirring, after the solids were completely dissolved, 0.27g B-β molecular sieve seeds and 9.0g white carbon black were added to the above solution, continue After stirring for 2.5 h, put the above gel into a stainless steel reactor with PTFE lining, crystallize at 150℃ for 3 d, cool, centrifuge, wash, dry at 100℃ overnight, and then pass 540℃ The raw powder of B-β molecular sieve is obtained after roasting for 3 h. The solid yield is 85%. The characterization results are attached image 3 , 4 .

Embodiment 3

[0063] Combine 0.48g borax, 0.15g NaOH, 0.56g NH 4 F was dissolved in 6.85g deionized water, 29.46g TEAOH was added to the above solution under mechanical stirring, after the solids were completely dissolved, 0.27g B-β molecular sieve seeds and 9.0g white carbon black were added to the above solution, continue After stirring for 2.5 h, put the above gel into a stainless steel reactor with PTFE lining, crystallize at 150℃ for 3 d, cool, centrifuge, wash, dry at 100℃ overnight, and then pass 540℃ The raw powder of B-β molecular sieve is obtained after roasting for 3 hours. The solid yield is 67%. The characterization results are attached Figure 5 , 6 .

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Abstract

The invention discloses a method for synthesizing a B-beta-heteroatom molecular sieve, which comprises the following steps: proportionally and mechanically stirring a boron source, a template agent, an alkali source, fluoride and water at room temperature; after the solids are completely dissolved, adding a crystal seed and a silicon source to form an initial gel, stirring for some time, filling the mixture into a kettle, sealing, crystallizing at 120-170 DEG C for 2-5 days, and carrying out hydrothermal synthesis to obtain the B-beta-heteroatom molecular sieve with BEA structure. The method disclosed by the invention can greatly shorten the synthesis time, has the advantages of simple operating procedure and high solid yield, can easily implement large-scale production, and especially can synthesize the B-beta-heteroatom molecular sieve with small crystal grain size and regular appearance under the action of the fluoride.

Description

Technical field [0001] The invention relates to the technical field of catalytic chemistry, in particular to a method for synthesizing B-β heteroatom molecular sieve. Background technique [0002] Because of its unique pore structure and large specific surface area, molecular sieves are widely used in many fields such as ion exchange, adsorption separation, host and guest chemistry, and are widely used in fine chemical and petrochemical industries. In 1967, Mobil Company obtained β molecular sieve by hydrothermal synthesis (USP308069) in the tetraethylammonium hydroxide strong alkali system, which is the only high silica molecular sieve with a three-dimensional twelve-membered ring pore structure. Due to its unique topological structure, good thermal and hydrothermal stability, both acid catalytic activity and shape selectivity, it is widely used in petroleum refining and petroleum products such as alkylation, catalytic cracking, isomerization, disproportionation and reforming. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04
Inventor 郭新闻李宏伟代成义刘民张安峰
Owner DALIAN UNIV OF TECH
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