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Nano-iron modified SBA-16 molecular sieve and preparation method and application thereof

A molecular sieve and nano-iron technology, which is applied in the field of molecular sieves, can solve the problems of metal particle agglomeration, molecular sieve channel blockage, specific surface area decrease, etc., and achieve the effect of large specific surface area and high selectivity

Active Publication Date: 2019-03-19
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Loading trivalent iron ions on SBA-16 molecular sieve can significantly improve the acid number and ion exchange capacity of the molecular sieve, and the prepared Fe / SBA-16 performs well in the oxidation of alkanes, alkylation of phenol and benzene However, the supported molecular sieve catalyst obtained by the conventional method is very easy to cause the agglomeration of metal particles in the process of drying and roasting, so that the pores of the molecular sieve are covered by a large number of metals and metal oxides, resulting in the blockage of the molecular sieve channels and the specific surface area. Decline

Method used

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  • Nano-iron modified SBA-16 molecular sieve and preparation method and application thereof
  • Nano-iron modified SBA-16 molecular sieve and preparation method and application thereof
  • Nano-iron modified SBA-16 molecular sieve and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] At 60°C, 3.2g F127(EO 106 PO 70 EO 106 ) and 70g of deionized water were added to the reactor in turn, stirred evenly, and then 50mL of 0.1mol / L hydrochloric acid solution was added, and after fully stirring until uniform, the complexation of 0.7g of ferrous chloride and 3.2g of ethylenediaminetetraacetic acid was added Continue to stir, slowly add 11g tetraethyl orthosilicate (TEOS) dropwise, and finally add 15g ethanol, the molar ratio of the obtained mixture is SiO 2 :73H 2 O:0.005R:0.1Fe:0.09H + , the mixture was transferred to a crystallization kettle, heated to 110° C., and crystallized at a constant temperature for 72 hours. After the crystallization is complete, when the temperature drops to room temperature, the reacted mixture is separated, washed, and dried at 110°C, and the dried sample is transferred to a muffle furnace for 4 hours at 500°C. , to obtain Fe-SBA-16 molecular sieve powder. Place the original powder of Fe-SBA-16 molecular sieve at the bot...

Embodiment 2

[0046] Same as Example 1, the difference is that the consumption of F127 is changed into 4.9g, the amount of deionized water is changed into 100g, the amount of hydrochloric acid is changed into 80mL, the iron source is changed into ferrous nitrate, and the consumption is 1.08g, B The amount of diamine tetraacetic acid is changed into 6.6g, silicon source is changed into silica sol (SW-25, silicon dioxide content is 25wt%), consumption is 9.6g, alcohol is changed into ethylene glycol, consumption is 23g, the mixture obtained The molar ratio of SiO 2 :139H 2 O:0.009R:0.15Fe:0.2H + , the crystallization temperature is 90°C, the crystallization time is 60h, the drying temperature is 120°C, the roasting temperature is 550°C, the roasting time is 5h, the hydrogen heating rate is changed to 4°C / min, the reduction temperature is changed to 500°C, and the reduction time Change it to 3h, keep the other components and synthesis conditions unchanged, and obtain nano-iron modified SBA-1...

Embodiment 3

[0049] Same as Example 1, the difference is that the organic template agent is changed to F108, the dosage is 3.7g, the amount of deionized water is changed to 80.6g, the acid is changed to nitric acid, the dosage is 90mL, and the iron source is changed to ferrocyanide Potassium chloride, the consumption is 3.6g, the silicon source is changed into sodium silicate, the consumption is 12.1g, the amount of ethanol is changed into 7.6g, the molar ratio of the mixture obtained is SiO 2 :104H 2 O:0.006R:0.2Fe:0.21H + , the crystallization temperature is 100°C, the crystallization time is 54h, the drying temperature is changed to 130°C, the roasting temperature is changed to 600°C, the roasting time is changed to 6h, the heating rate of hydrogen reduction is changed to 5°C / min, and the reduction temperature is changed to 550 ℃, the reduction time was changed to 4h, and the other components and synthesis conditions were unchanged, and the SBA-16 molecular sieve decorated with nano-ir...

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Abstract

The invention relates to a nano-iron modified SBA-16 molecular sieve, and further relates to a preparation method thereof. Nano-iron, in a simple substance form, is embedded in a framework of the molecular sieve; the preparation method includes the steps of S1, mixing a silicon source, water, an organic template, an iron-source complex, acid and alcohol to obtain a reaction mixture; S2, subjectingthe reaction mixture to hydrothermal crystallization, and performing after-treatment, to obtain a Fe-SBA-16 molecular sieve; S3, subjecting the Fe-SBA-16 molecular sieve to reduction treatment through hydrogen to obtain the nano-iron modified SBA-16 molecular sieve. The nano-iron modified SBA-16 molecular sieve still has cubic mesoporous channel structure and high specific surface area, and granularity of nano-iron in the framework ranges from 3nm to 4nm.

Description

technical field [0001] The invention belongs to the technical field of molecular sieves, and in particular relates to a nano-iron modified SBA-16 molecular sieve and a preparation method thereof. Background technique [0002] In recent years, the research on supported catalysts has made great progress. Supported catalysts not only solve the problem that homogeneous catalysts are difficult to recycle and reuse, but also overcome the problem of environmental pollution caused by metal loss. Mesoporous materials have high specific surface area and regular pore structure, which can ensure the highly dispersed active sites of supported catalysts and maintain the original catalytic activity and selectivity of homogeneous catalysts; in addition, there are abundant hydroxyl groups on the surface of mesoporous materials, which are easy to surface Functionalization, and mesoporous materials also have high chemical and mechanical stability, so this type of material is an ideal homogeneo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/06C07C37/60C07C39/04B01J29/04
CPCC01B39/065C07C37/60B01J29/044C01P2006/12C01P2002/85C01P2004/04C01P2002/72B01J2229/186B01J35/396B01J35/393C07C39/04Y02P20/52
Inventor 吴凯任行涛刘艳惠贾志光杨光
Owner CHINA PETROLEUM & CHEM CORP
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