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A kind of fluorine-modified titanium aluminum phosphate molecular sieve f-tapo-5 and preparation method thereof

A technology of F-TAPO-5, titanium aluminum phosphate, applied in the direction of molecular sieve characteristic aluminum phosphate, molecular sieve catalyst, molecular sieve and alkali exchange phosphate, etc., to achieve the effect of easy process, low price and less time-consuming

Active Publication Date: 2018-10-26
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Research work on this aspect has not been reported in the literature

Method used

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  • A kind of fluorine-modified titanium aluminum phosphate molecular sieve f-tapo-5 and preparation method thereof
  • A kind of fluorine-modified titanium aluminum phosphate molecular sieve f-tapo-5 and preparation method thereof
  • A kind of fluorine-modified titanium aluminum phosphate molecular sieve f-tapo-5 and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0039] 4.151g H 3 PO 4 and 10.0 g H 2 O was stirred and mixed at 30°C, and 2.7648g Al(OH) was weighed 3 The powder was added to the above system, and after stirring for 0.5h, 0.191g N 2 h 8 TiF 6 Powder is added to the system. Then 3.751g MCHA is slowly added dropwise in the above-mentioned suspension, finally add 10.0g water, the molar ratio of raw materials is Al(OH) 3 :H 3 PO 4 :N 2 h 8 TiF 6 :MCHA:H 2 O=0.96:1.5:0.04:0.8:50, continue to stir vigorously for 1 hour, then transfer it to a stainless steel crystallization kettle lined with polytetrafluoroethylene, and crystallize at 180°C for 24 hours. After the crystallization is completed, centrifuge and wash with distilled water until neutral, and dry at 110°C for 12 hours to obtain the original powder of F-TAPO-5. The obtained F-TAPO-5 raw powder was calcined in a tube furnace at 575° C. for 6 hours in an oxygen atmosphere to remove the structure-directing agent and obtain a molecular sieve, labeled as: F-TAPO-...

Embodiment 2

[0041]4.151g H 3 PO 4 and 10.0 g H 2 O was stirred and mixed at 30°C, and 2.7648g Al(OH) was weighed 3 The powder was added to the above system, and after stirring for 0.5h, 0.764g N 2 h 8 TiF 6 Powder is added to the system. Then 3.751g MCHA is slowly added dropwise in the above-mentioned suspension, finally add 10.0g water, the molar ratio of raw materials is Al(OH) 3 :H 3 PO 4 :N 2 h 8 TiF 6 :MCHA:H 2 O=0.96:1.5:0.1:0.8:50, continue to stir vigorously for 1 hour, then transfer it to a stainless steel crystallization kettle lined with polytetrafluoroethylene, and crystallize at 180°C for 24 hours. After the crystallization is completed, centrifuge and wash with distilled water until neutral, and dry at 110°C for 12 hours to obtain the original powder of F-TAPO-5. The obtained F-TAPO-5 raw powder was calcined in a tube furnace at 575° C. for 6 hours in an oxygen atmosphere to remove the structure-directing agent and obtain a molecular sieve, labeled as: F-TAPO-5 ...

Embodiment 3

[0043] 4.151g H 3 PO 4 and 10.0 g H 2 O was stirred and mixed at 30°C, and 2.7648g Al(OH) was weighed 3 The powder was added to the above system, and after stirring for 0.5h, 1.528g N 2 h 8 TiF 6 Powder is added to the system. Then 3.751g MCHA is slowly added dropwise in the above-mentioned suspension, finally add 10.0g water, the molar ratio of raw materials is Al(OH) 3 :H 3 PO 4 :N 2 h 8 TiF 6 :MCHA:H 2 O=0.96:1.5:0.2:0.8:50, continue to stir vigorously for 1 hour, then transfer it to a stainless steel crystallization kettle lined with polytetrafluoroethylene, and crystallize at 180°C for 24 hours. After the crystallization is completed, centrifuge and wash with distilled water until neutral, and dry at 110°C for 12 hours to obtain the original powder of F-TAPO-5. The obtained F-TAPO-5 raw powder was calcined in an air atmosphere at 575° C. for 6 hours to remove the structure directing agent in a muffle furnace to obtain a molecular sieve, labeled as: F-TAPO-5 (...

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Abstract

The invention provides a fluorine-modified titanium and aluminum phosphate molecular sieve F-TAPO-5 and a preparation method thereof. The preparation method comprises the steps that 1, a phosphorus source, an aluminum source, a fluorine-containing titanium source, a templating agent and deionized water are mixed to be uniform according to the molar ratio of 0.96:1.5:(0.04-0.3):0.8:50 under vigorous stirring, stirring is conducted for 20-40 min at the temperature of 25-35 DEG C, and molecular sieve precursor sol is obtained; the precursor sol is converted into a hydrothermal reactor with a PTFE lining, crystallization treatment is conducted for 18-30 h at the temperature of 160-185 DEG C, after crystallization is finished, solids are separated out through centrifugation, the solids are washed with distilled water and then dried by 10-15 h at the temperature of 90-110 DEG C, and fluorine-containing titanium and aluminum phosphate molecular sieve raw powder is obtained; 2, the molecular sieve raw powder obtained in the step 1 is put into a tubular furnace constant temperature area, calcination is conducted for 4-8 h at the temperature of 500-650 DEG C in an oxygen atmosphere to remove the templating agent, and the fluorine-modified titanium and aluminum phosphate molecular sieve F-TAPO-5 is obtained. The fluorine-modified titanium and aluminum phosphate molecular sieve F-TAPO-5 obtained through the method has high Lewis acid and surface hydrophobicity and can be applied in a catalytic cyclohexanone ammoximation reaction.

Description

technical field [0001] The invention relates to an aluminum phosphate molecular sieve, in particular to a fluorine-modified titanium aluminum phosphate molecular sieve F-TAPO-5 and its preparation method and application. Background technique [0002] In the early 1980s, Italian Enichem Company developed titanium-silicon molecular sieve TS-1. The catalytic system composed of TS-1 and low-concentration hydrogen peroxide can realize the selective oxidation of organic compounds such as alcohols, phenols and olefins under mild conditions, among which phenol hydroxylation, cyclohexanone ammoximation and propylene epoxidation have been realized Industrialization makes TS-1 a milestone in the field of molecular sieves. Subsequently, the researchers introduced titanium into various molecular sieves to prepare new titanium-containing molecular sieves with different structures and compositions. According to the composition of these molecular sieves can be divided into two categories:...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/54C01B37/06B01J29/84C07C249/04C07C251/44
CPCB01J29/84C01B37/06C01B39/54C01P2002/72C01P2002/82C01P2002/85C01P2006/90C07C249/04C07C251/44
Inventor 高鹏飞赵永祥张鸿喜赵丽丽李恒杰
Owner SHANXI UNIV
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