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Modified beta molecular sieve as well as preparation method and application thereof

A β molecular sieve and modification technology, which is applied in the direction of molecular sieves and base exchange compounds, molecular sieve catalysts, carboxylate preparation, etc., can solve the problems of easy loss of active components, loss of sulfonic acid groups, and high temperature resistance of resin catalysts.

Active Publication Date: 2018-07-27
SHANDONG QILU HUAXIN HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the production process of strong acidic cation exchange resin, there will be problems such as loss of sulfonic acid group and broken resin particles, which will cause catalyst deactivation, and the resin catalyst is not resistant to high temperature and difficult to regenerate; There is the shortcoming that active component is easy to lose in; The β molecular sieve of reported lanthanum nitrate modification, HY molecular sieve and mordenite catalyst are all low to the conversion rate and the selectivity of butene

Method used

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  • Modified beta molecular sieve as well as preparation method and application thereof
  • Modified beta molecular sieve as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Put 30g of 20-40 mesh commercial hydrogen-type β-molecular sieves in a quartz cup and put them in the constant temperature section of the hydrothermal aging device. 0.5h; heat up to 480°C at 30°C / min, and keep the temperature constant for 0.5h for every 30°C rise; heat up to 500°C at 25°C / min, keep the temperature for 3h. After processing, naturally cool to room temperature and set aside.

[0046] Using 5g of the modified β molecular sieve prepared above as a catalyst, the esterification reaction of acetic acid and butene was evaluated. The reaction temperature was 110°C, the reaction pressure was 2MPa, and the weight hourly space velocity was 2.0h -1 , the molar ratio of acetic acid and butene is 1.5. The results show that the conversion rate of butene is 40.8%, and the selectivity of sec-butyl acetate is 100%.

Embodiment 2

[0048] Put 30g of 20-40 mesh commercial hydrogen-type β-molecular sieves in a quartz cup and put them in the constant temperature section of the hydrothermal aging device. 0.5h; heat up to 560°C at 30°C / min, and keep the temperature constant for 0.5h for every 40°C rise; heat up to 600°C at 25°C / min, keep the temperature constant for 5h. Then, adopt equal volume impregnation method to load 10% zirconium sulfate thereon (thermogravimetric curve such as figure 2 shown), dried, baked at 200°C for 3h, cooled naturally to room temperature, and set aside.

[0049] Using 5g of the modified β molecular sieve prepared above as a catalyst, the esterification reaction of acetic acid and butene was evaluated. The reaction temperature was 130°C, the reaction pressure was 2MPa, and the weight hourly space velocity was 1.0h -1 , the molar ratio of acetic acid and butene is 1.5. The results show that the conversion rate of butene is 46.8%, and the selectivity of sec-butyl acetate is 100%. ...

Embodiment 3

[0051] Put 30g of 20-40 mesh commercial hydrogen-type β-molecular sieves into a quartz cup and place them in the constant temperature section of the hydrothermal aging device. 1h; the temperature was raised to 550°C at 35°C / min, and the temperature was kept constant for 1h for every 30°C rise; the temperature was raised to 600°C at 30°C / min, and the temperature was kept constant for 5h. Then, 20% zirconium sulfate was loaded on it by an equal volume impregnation method, dried, calcined at 200° C. for 3 hours, cooled naturally to room temperature, and set aside.

[0052] Using 5g of the modified β molecular sieve prepared above as a catalyst, the esterification reaction of acetic acid and butene was evaluated. The reaction temperature was 120°C, the reaction pressure was 3MPa, and the weight hourly space velocity was 2.0h -1 , the molar ratio of acetic acid and butene is 2.0. The results show that the conversion rate of butene is 59.0%, and the selectivity of sec-butyl acetate...

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Abstract

The invention provides a modified beta molecular sieve as well as a preparation method and an application thereof. The method comprises a step of performing water vapor modification treatment on a hydrogen type beta molecular sieve and a step of loading the water vapor modified hydrogen type beta molecular sieve with zirconium sulfate to obtain the modified beta molecular sieve, wherein water vapor modification treatment is performed at the temperature of 400-800 DEG C for 2-6 h; the load of zirconium sulfate is 0-50% of the mass of the water vapor modified hydrogen type beta molecular sieve.The defects that traditional ion exchange resin is difficult to regenerate, heteropolyacid and active components of a solid super acidic catalyst are easy to lose and the activity and selectivity of currently reported catalysts such as a beta molecular sieve, an HY molecular sieve and mordenite are low and the like can be overcome.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular, the invention relates to a modified β molecular sieve and its preparation method and application. Background technique [0002] Second-butyl acetate, also known as second-butyl acetate and second-butyl acetate, is one of the four isomers of butyl acetate. It is a light yellow transparent liquid with a special fruity aroma and belongs to the acetate solvent. The application range of sec-butyl acetate is very wide, suitable for spices, reaction medium, metal cleaning agent, extractant, medicine and solvent, and can also replace methyl tert-butyl ether (MTBE), as a gasoline additive, is a kind of use Wide range of fine chemicals. [0003] The traditional method of producing sec-butyl acetate at home and abroad is to adopt a batch tank reactor, and use concentrated sulfuric acid as a catalyst to catalyze the esterification reaction of acetic acid and butanol. Such as, CN1844076A has...

Claims

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Application Information

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IPC IPC(8): C01B39/02B01J29/70B01J37/10B01J37/02B01J37/08C07C67/04C07C69/14
CPCB01J29/7057B01J37/0201B01J37/08B01J37/10B01J2229/18C01B39/026C01P2006/12C07C67/04C07C69/14
Inventor 刘海燕李建华安婷婷李飞杰鲍晓军岳源源
Owner SHANDONG QILU HUAXIN HIGH TECH
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