Preparation method of Al modified SBA-15 and application of Al modified SBA-15 in catalyzing alkynol dehydration reaction

A technology of SBA-15 and dehydration reaction, which is applied in the direction of catalyst, sulfide preparation, halogenated hydrocarbon preparation, etc. It can solve the problems of difficult formation, metal hydrolysis and polymerization speed mismatch, etc., and achieve the effect of enhancing controllability and reducing raw material cost

Active Publication Date: 2021-06-11
CHINA THREE GORGES UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Compared with the post-synthesis method (loading), the direct hydrothermal synthesis method (doping) requires stronger acidity during the synthesis of metal-doped SBA-15, but under acidic conditions, the metal mainly exists in the form of cations, and metal-oxygen- Silicon (M-O-Si) bonds are difficult to form, and the metal hydrolytic polymerization rate does not match the silicon source

Method used

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  • Preparation method of Al modified SBA-15 and application of Al modified SBA-15 in catalyzing alkynol dehydration reaction
  • Preparation method of Al modified SBA-15 and application of Al modified SBA-15 in catalyzing alkynol dehydration reaction
  • Preparation method of Al modified SBA-15 and application of Al modified SBA-15 in catalyzing alkynol dehydration reaction

Examples

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Embodiment 2

[0038] A preparation method of Al-modified SBA-15 containing only four-coordinated aluminum skeleton - mixing and stirring for 6 hours, crystallization at 120°C, the following is the specific implementation method:

[0039] Weigh 1.23g Al(NO 3 ) 3 9H 2 O aluminum source, it is added in the round bottom flask that fills the deionized water of 120mL, stirs under normal temperature, until Al(NO 3 ) 3 9H 2 O is completely dissolved until the solution is clear, then adjust the pH value of the solution, and the pH value of the solution is 2; then weigh 2 g of the prepared spherical SBA-15 mesoporous molecular sieve, slowly stir it into the aluminum-containing source solution, and continuously Stir, mix and stir for 6 hours and then stop stirring; transfer the obtained mixed solution into a polytetrafluoroethylene-lined crystallization kettle, and continue crystallization at 120°C for 24 hours; wash the crystallized solid with deionized water and absolute ethanol After washing a...

Embodiment 3

[0043] A preparation method of a terminal enyne compound - But-3-en-1-yne-1,3-diyldibenzene, the following is the specific implementation method (catalyst dosage 6mg):

[0044] Weigh compound acetylenic alcohol 1a 0.0222g (0.1mmol) (substituent R 1 , R 2 , R 3 Respectively phenyl, hydrogen, phenyl) are placed in a round-bottomed flask, measure 3mL of anhydrous toluene as a reaction solvent and pour it into it, stir to completely dissolve the acetylenic alcohol, weigh the Al / SBA-15 medium prepared in Example 1 Add 6mg of porous material catalyst into the reaction system, stir at a constant temperature in an oil bath at 110°C, condense and reflux; monitor the reaction with TCL, after 15 minutes the reaction of compound acetylenic alcohol 1a is complete, the system is cooled to room temperature and the solvent toluene is evaporated under reduced pressure, and the reaction system is passed through a silica gel column Column chromatography separation was carried out to obtain the...

Embodiment 4

[0049] A preparation method of a terminal enyne compound - But-3-en-1-yne-1,3-diyldibenzene, the following is the specific implementation method (catalyst dosage 3mg):

[0050] Weigh compound acetylenic alcohol 1a 0.0222g (0.1mmol) (substituent R 1 , R 2 , R 3 Respectively phenyl, hydrogen, phenyl) are placed in a round-bottomed flask, measure 3mL of anhydrous toluene as a reaction solvent and pour it into it, stir to completely dissolve the acetylenic alcohol, weigh the Al / SBA-15 medium prepared in Example 1 Add 3 mg of porous material catalyst to the reaction system, stir at a constant temperature in an oil bath at 110°C, condense and reflux; monitor the reaction with TCL, after 15 minutes the reaction of the compound acetylenic alcohol 1a is complete, the system is cooled to room temperature and the solvent toluene is evaporated under reduced pressure, and the reaction system is passed through a silica gel column The target product enyne 2a was obtained by column chromato...

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Abstract

The invention relates to a preparation method of Al-modified SBA-15 and application of the Al-modified SBA-15 in catalyzing alkynol dehydration reaction. A spherical SBA-15 mesoporous molecular sieve is used as a loading substrate, aluminum nitrate nonahydrate is used as an aluminum source, and H2O is used as a synthesis solvent. The method comprises the steps of synthesizing an SBA-15 mesoporous molecular sieve with spherical morphology, and regulating and controlling the pH value, stirring time, crystallization temperature and crystallization time of a mixed solution of an aluminum source and the spherical SBA-15 to prepare a target product Al / SBA-15 only containing tetra-coordinated framework aluminum. According to the invention, two-step synthesis is adopted, an NF4F hydrolysis catalyst does not need to be added like a doping method to improve modification loading failure caused by mismatching of hydrolytic polymerization speeds of an aluminum source and a silicon source, and other solvents are not used in the modification loading process. The method is simple in production process, relatively high in experimental controllability, green and environment-friendly, the catalyst is low in preparation cost, the types of raw materials are simplified, the yield of terminal eneyne preparation participating in catalysis can reach 92%, and the catalyst is easy to separate and recycle and can be repeatedly used.

Description

technical field [0001] The invention relates to a preparation method of Al-modified SBA-15 and its application in catalyzing the dehydration reaction of acetylenic alcohols. Background technique [0002] SBA-15 is a mesoporous silicon-based molecular sieve with a two-dimensional hexagonal structure synthesized under acidic conditions using P123 triblock copolymer as a template. High specific surface area and thick pore wall, not only as a new catalyst, but also as a carrier have attracted extensive attention of many researchers in this field. Compared with traditional zeolite molecular sieves, SBA-15 mesoporous molecular sieves are based on amorphous SiO 2 , in the catalyzed high-temperature reaction, water molecules are easy to attack the Si-OH bond, causing the Si-O-Si bond to be hydrolyzed and broken, resulting in the collapse of the two-dimensional hexagonal structure inside SBA-15, so its hydrothermal stability is low, which is also to a certain extent This limits its...

Claims

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Application Information

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IPC IPC(8): C01B37/02B01J29/04C07C1/24C07C15/50C07C17/35C07C25/24C07C319/14C07C323/20
CPCC01B37/02B01J29/041C07C1/24C07C17/35C07C319/14C01P2002/72C01P2004/03C01P2004/04C01P2002/86C01P2002/82B01J2229/186C07C2529/04C07C15/50C07C25/24C07C323/20
Inventor 王龙罗享豪王华胡为民李德莹
Owner CHINA THREE GORGES UNIV
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