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Ti-SBA-15 molecular sieve, modified Ti-SBA-15 molecular sieve, their preparation methods and preparation method of epoxy propane

A technology of ti-sba-15 and molecular sieve, which is applied in the field of preparation of propylene oxide, achieves the effects of increased yield, low preparation cost and improved selectivity

Active Publication Date: 2013-01-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the defect that titanium species are not easy to enter the molecular sieve skeleton when using conventional inorganic titanium sources and / or organic titanates to obtain Ti-SBA-15 molecular sieves using a liquid-phase grafting synthesis method in the prior art, and provide A method for preparing Ti-SBA-15 molecular sieve with simple method, low cost and efficient entry of titanium source into mesoporous molecular sieve framework

Method used

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  • Ti-SBA-15 molecular sieve, modified Ti-SBA-15 molecular sieve, their preparation methods and preparation method of epoxy propane
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  • Ti-SBA-15 molecular sieve, modified Ti-SBA-15 molecular sieve, their preparation methods and preparation method of epoxy propane

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preparation example Construction

[0023] According to the method for preparing Ti-SBA-15 molecular sieve of the present invention, the method comprises:

[0024] (1) Under the reaction conditions of introducing titanium by liquid phase grafting and in the presence of the first organic solvent, the titanium source and SBA-15 molecular sieve are contacted and reacted in the presence of 100-300W ultrasonic waves, and the product after the contact reaction is solid-liquid separation;

[0025] (2) washing, drying, and roasting the solid product obtained in step (1) from solid-liquid separation,

[0026] Wherein, the titanium source is a general formula of Ti(OR) 4 titanate and / or inorganic titanium source; the first organic solvent is an alcohol compound with the general formula R'OH, where R' is an alkyl group with 1-5 carbon atoms.

[0027] The above-mentioned method for preparing Ti-SBA-15 molecular sieve mainly involves introducing the titanium source into the SBA-15 molecular sieve, selecting common and easy...

Embodiment 1

[0075] (1) Preparation of SBA-15 molecular sieve

[0076] Add 24.0g of nonionic surfactant P123 to 600g of 2M hydrochloric acid aqueous solution, stir at 35°C for 1 hour; add 51.2g of tetraethyl orthosilicate to the above solution, and stir at 35°C for 24 hours; transfer the above mixture to water Hot pot, hydrothermal crystallization at 100°C for 24 hours. After the hydrothermal reaction, the solid product was separated from the mother liquor, washed with deionized water until neutral, and dried at 110° C. for 3 hours to obtain the original powder of SBA-15. Mix 20.0 g of SBA-15 raw powder with 200 ml of acidified methanol (the volume ratio of methanol to concentrated hydrochloric acid is 20:1), reflux extraction at 80°C for 10 hours, then filter, wash, and vacuum dry at 120°C for 3 hours to obtain SBA -15 molecular sieves. Its X-ray diffraction pattern (XRD) is as figure 1 As shown in (a), it can be seen that the sample has typical SBA-15 molecular sieve mesoporous struct...

Embodiment 2

[0089] (1) Preparation of SBA-15 molecular sieve

[0090] Add 30.6g of nonionic surfactant P123 to 400g of 1M hydrochloric acid aqueous solution, stir at 40°C for 1 hour; add 40.1g of methyl orthosilicate dropwise to the above solution, and stir at 40°C for 24 hours; transfer the above mixture To a hydrothermal kettle, hydrothermal crystallization at 100°C for 24 hours. After the hydrothermal reaction, the solid product was separated from the mother liquor, washed with deionized water until neutral, and dried at 110° C. for 3 hours to obtain the original powder of SBA-15. Mix 20.0 g of SBA-15 raw powder with 200 g of tetrahydrofuran, reflux extraction at 70°C for 6 hours, then filter, wash, and vacuum dry at 120°C for 3 hours to obtain SBA-15 molecular sieve.

[0091] (2) Preparation of Ti-SBA-15 molecular sieve

[0092] Dissolve 6.3g of titanium tetrachloride in 1000g of ethanol, mix with 10.0g of the above-mentioned SBA-15 molecular sieve, and react with stirring for 60 mi...

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Abstract

The invention discloses a Ti-SBA-15 molecular sieve and its preparation method. The method includes: (1) under the reaction conditions of titanium introduction through liquid phase grafting and in the presence of a first organic solvent, subjecting a titanium source and an SBA-15 molecular sieve to a contact reaction in the presence of 100-300W ultrasonic waves, and conducting solid-liquid separation on a product of the contact reaction; and (2) carrying out washing, drying and roasting on a solid product obtained in step (1). Specifically, the titanium source is titanate with a general formula as Ti(OR)4 and / or an inorganic titanium source, and the first organic solvent is an alcohol compound with a general formula as R' OH, wherein R' is an alkyl group with a carbon atom number of 1-5. The invention also provides a modified Ti-SBA-15, its preparation method, and a preparation method of epoxy propane. The Ti-SBA-15 molecular sieve and the modified Ti-SBA-15 molecular sieve prepared in the invention can present good catalytic performance when applied to preparation of epoxy propane.

Description

technical field [0001] The invention relates to a Ti-SBA-15 molecular sieve and a preparation method thereof, a modified Ti-SBA-15 molecular sieve and a preparation method thereof, and a preparation method of propylene oxide. Background technique [0002] Propylene oxide (PO) is an important basic chemical raw material, widely used in petrochemical, light industry, pharmaceutical, food and textile industries. At present, the main production method of propylene oxide is to use propylene as raw material, organic peroxide as oxidant, and co-oxidation method. According to the characteristics of the propylene epoxidation reaction, it is generally believed that the most suitable catalyst for this reaction is a titanium-silicon mesoporous molecular sieve with a suitable pore structure, and the most widely used Ti-MCM-41 molecular sieve (US6323147, US6639085, US6646138, US6838570 ). However, because the quaternary ammonium salt template used in the synthesis of MCM-41 mesoporous m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89B01J31/02B01J37/34C07D301/19C07D303/04
CPCY02P20/52
Inventor 刘红梅张明森柯丽
Owner CHINA PETROLEUM & CHEM CORP
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