CN-117181285-B - Modification method of H beta zeolite and application of modified H beta zeolite

Abstract

The invention provides a modification method of H beta zeolite and application of the modified H beta zeolite in isomerization reaction to prepare mesitylene. The modification method of the H beta zeolite comprises the steps of high-temperature calcination, alkali treatment, ammonium chloride treatment and active component loading of molybdenum and nickel sequentially, wherein mordenite is mixed with NaOH solution during alkali treatment and reacts at 50-80 ℃, and the active component loading step comprises the step of placing the H beta zeolite into a soluble salt mixed solution of molybdenum and nickel and reacting at 50-80 ℃. The application of the mordenite improves the mesitylene resource amount in the reformed carbon nine.

Inventors

• WANG YANG
• GU ZHENGGUI
• CHEN SHAOHUI
• WANG BAOZHENG
• HU WEIQIANG

Assignees

• 中国石化扬子石油化工有限公司
• 中国石油化工股份有限公司

Dates

Publication Date

20260512

Application Date

20220530

Claims (5)

1. 1. The application of an isomerization catalyst in preparing mesitylene by catalyzing the isomerization reaction of the pseudocumene and the o-methyl ethylbenzene is characterized in that the isomerization catalyst is obtained by sequentially treating H beta zeolite through high-temperature calcination, alkali treatment, ammonium chloride treatment and molybdenum and nickel active component loading, wherein the H beta zeolite is mixed with NaOH solution during the alkali treatment and reacts at 50-80 ℃, and the active component loading step is to put the H beta zeolite into a soluble salt mixed solution of molybdenum and nickel and react at 50-80 ℃; The concentration of the soluble salt solution of the molybdenum is 0.2-1M, the concentration of the soluble salt of the nickel is 0.2-1M, and 1g of H beta zeolite is placed in 20-50mL of the soluble salt mixed solution; The concentration of NaOH solution is 0.1-0.3M,1gH beta zeolite is placed in 15-50mLNaOH solution during alkali treatment; The reaction temperature in the application is 200-300 ℃, the reaction pressure is 1.0-1.5MPa, the reaction space velocity is 0.5-1.5h -1 , and the hydrogen-oil mole ratio is 5-10.
2. 2. Use according to claim 1, characterized in that the H beta zeolite is reacted with NaOH solution during the alkaline treatment to obtain a suspension, the suspension is filtered and washed with water to ph=7 and then dried.
3. 3. Use according to claim 2, characterized in that the alkali-treated H beta zeolite is mixed with the ammonium chloride solution during the ammonium chloride treatment to obtain a suspension, the suspension is filtered and washed free of chloride ions, and then dried.
4. 4. Use according to claim 3, characterized in that the concentration of the ammonium chloride solution is 0.2-1M, and the mixing is carried out according to the proportion of 1g H beta zeolite per 15-50mL of ammonium chloride solution.
5. 5. The method according to claim 4, wherein the modified H.beta.zeolite is obtained by calcining the H.beta.zeolite treated with ammonium chloride for 4 hours at a calcination temperature of 400-600 ℃.

Description

Modification method of H beta zeolite and application of modified H beta zeolite Technical Field The invention relates to a method for reforming carbon nine isomerization, in particular to a method for modifying H beta zeolite and a method for generating mesitylene by catalyzing the isomerization reaction of pseudocumene and o-methyl ethylbenzene by the modified H beta zeolite. Background The reformed C9 aromatic hydrocarbon resources in China are quite rich, and the reformed C9 aromatic hydrocarbon accounts for about 10% of the total oil refining amount. . In reforming C9, mesitylene accounts for 8%, which most refineries use as a gasoline blending component or as a raw material for the disproportionation of aromatic hydrocarbon to produce xylene. In recent years, with the advanced development of carbon nonaarenes, mesitylene is an important raw material for producing mesitylene, antioxidant Ethanox330, herbicide, ultraviolet absorber for plastics and rubber, and the like. In recent years, with the success of development of many downstream products, the demand has increased greatly. The related researches include Zhang Pengfei and the like in petrochemical industry, 2005.5, the best process conditions for obtaining isomerization reaction in the process for preparing the mesitylene by using the M-2 composite mordenite to catalyze the liquid phase non-hydroisomerization of the mesitylene, the single pass conversion of the mesitylene can reach 39 percent under the conditions of the reaction temperature of 310-320 ℃, the reaction pressure of 1.5-2.0 MPa and the liquid space velocity of 1.0-1.5 and h -1, the selectivity of the mesitylene can reach 66.29 percent, zhang Weijiang and the like in chemical engineering newspaper, 2002.3, the optimal process conditions for obtaining isomerization reaction in the process for producing the mesitylene by using mixed aromatic hydrocarbon are that the composition is controlled to be about 21.8 percent of dimethylbenzene, about 50.3 percent of mesitylene, about 0.4 percent of durene (including 3 isomers) and about 24.3 percent of durene (other components are light components brought by raw materials, such as benzene, toluene and the like), the reaction temperature is about 21.8 percent of dimethylbenzene, and the reaction time is about 5 percent of the reaction time of the trimeitylene is more than that the trimeitylene is produced by using the method of the trimeitylene which is developed by using the method of the trimeitylene which has the three-phase of the reaction of the trimeitylene. Disclosure of Invention The invention aims at overcoming the defects of the prior art and provides a modification method of H beta and application of H beta zeolite in preparing mesitylene through catalytic isomerization reaction. The technical scheme of the invention is as follows: A process for modifying H beta zeolite includes such steps as calcining at high temp, alkali treating, ammonium chloride treating, loading active components of Mo and Ni, mixing mordenite with NaOH solution, and reacting at 50-80 deg.C, and loading active components as H beta zeolite in the solution of soluble salt of Mo and Ni, reacting at 50-80 deg.C, and mixing Mo and Ni for better interaction between active centers. As a further improvement of the technical scheme, in order to improve the loading effect, the concentration of the molybdenum soluble salt solution is 0.2-1M, the concentration of the nickel soluble salt is 0.2-1M,1g of H beta zeolite is placed in 20-50ml of soluble salt mixed solution, and the soluble salt of each metal can be one or a mixture of ammonium salt and nitrate. As a further improvement of the technical scheme, in order to improve the desilication effect, the concentration of the NaOH solution is 0.1-0.3M during alkali treatment, and 1gH beta zeolite is placed in 15-50mlNaOH solution. As a further improvement of the technical scheme, the H beta zeolite is reacted with NaOH solution to obtain a suspension during the alkali treatment, the suspension is filtered and washed with water to ph=7, and then dried. As a further improvement of the technical scheme, in order to change sodium zeolite into hydrogen zeolite, the alkali-treated H beta zeolite is mixed with an ammonium chloride solution to obtain a suspension during the ammonium chloride treatment, and the suspension is filtered, washed with water until no chloride ions exist, and then dried. As a further improvement of the technical scheme, the concentration of the ammonium chloride solution is 0.2-1M, and the ammonium chloride solution is mixed according to the proportion of 1g H beta zeolite per 15-50 ml. As a further improvement of the technical scheme, the H beta zeolite after the ammonium chloride treatment is roasted for 4 hours at the roasting temperature of 400-600 ℃ to obtain the modified H beta zeolite. As a further improvement of the technical scheme, in order to improve the activation effect, the activation condition i