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P-xylene fluid catalyst prepared by performing alkylation of methylbenzene methyl alcohol and preparation method thereof

A xylene fluidized bed and alkylation technology, applied in the chemical industry, can solve problems such as difficult industrialization, high cost, and high cost, and achieve the effects of easy wastewater treatment, low equipment requirements, and low cost

Active Publication Date: 2014-03-19
陕西煤化工技术工程中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although these technologies reported above have obtained relatively high toluene conversion and PX selectivity, they have the following disadvantages: (1) the reaction is carried out on a fixed bed device, and the catalyst is not easy to regenerate; (2) toluene conversion and PX selectivity Cannot have both, and methanol conversion rate is not mentioned; (3) The molar ratio of water / (toluene+methanol) is too high, the energy consumption is extremely high, the waste water is more and difficult to handle; (4) The hydrogen reaction, and the ratio of hydrogen to hydrocarbon Too high, dangerous to operate, more waste gas, difficult to recycle hydrogen, high cost; (5) pressurized reaction, high requirements for equipment; (6) In addition, the patent CN101485994B is modified with precious metal Pt, which is expensive and difficult industrialization
However, the conversion rate of toluene on this catalyst is 20.1%, and the selectivity of PX is 99.1%, but the selectivity of xylene is only 65%, and the yield of PX is very low, only 12.95%.

Method used

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  • P-xylene fluid catalyst prepared by performing alkylation of methylbenzene methyl alcohol and preparation method thereof
  • P-xylene fluid catalyst prepared by performing alkylation of methylbenzene methyl alcohol and preparation method thereof

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preparation example Construction

[0033] The present invention also relates to a method for preparing a fluidized-bed catalyst for producing p-xylene through the alkylation of toluene with methanol, comprising the following steps:

[0034] a) Mix 20-70wt% ZSM-5 molecular sieve, 20-60wt% matrix, 5-50wt% binder and water to form a slurry with a solid content of 10-50% for spray molding to form a particle diameter Spherical particles between 10-300μm, calcination at 350-600°C for 2-20h to form the original powder;

[0035]b) Mix the original powder obtained in step a) with the aqueous solution of the modified element precursor in equal volumes, the mass of the precursor is 0-15wt% of the original powder by the amount of Mg, Ca, and Sr introduced, and the amount of P is 0-15wt% of the original powder. 0-10wt% of the mass and 0-10wt% of the mass of La and Ce accounted for the mass of the original powder. Under the condition of 10-90°C, impregnated and modified for 1-24h, the obtained material was dried and then roa...

Embodiment 1

[0039] 21.36kg demineralized water, 5.21kg ZSM-5 molecular sieve (SiO 2 / Al 2 o 3 The molar ratio is 20), 5.64kg of pseudo-boehmite, 7.79kg of silica sol, mixed, stirred for 2 hours, and then spray-dried to obtain microsphere particle products. The product is calcined at 500°C for 5 hours in an air atmosphere to obtain the original catalyst powder.

[0040] Stir 400g of the above catalyst raw powder, 112.9g of phosphoric acid, and 187.1g of water evenly, keep the temperature at 10°C for 24h, dry, and calcinate at 500°C for 5h to obtain a P-modified catalyst. Stir 400g of P-modified catalyst and 300g of tetramethylsilicate evenly, let it stand at room temperature for 1 hour, dry it, and roast it at 400°C for 6 hours to obtain P and Si-modified catalyst (referred to as DP-1).

Embodiment 2

[0042] 21.52kg demineralized water, 10.64kg ZSM-5 molecular sieve (SiO 2 / Al 2 o 3 The molar ratio is 25), 3.29kg of montmorillonite, 4.55kg of aluminum sol, mixed, stirred for 2 hours, and then spray-dried to obtain microsphere particle products. The product is calcined at 600°C for 2 hours in an air atmosphere to obtain the original catalyst powder.

[0043] 400g of the above-mentioned catalyst raw powder, 20g of lanthanum nitrate, and 280g of water were stirred evenly, kept at a constant temperature of 30°C for 15h, dried, and calcined at 350°C for 10h to obtain a La-modified catalyst. Stir 400g of La modified catalyst, 150g of phenylmethylpolysiloxane, and 150g of absolute ethanol evenly, let stand at room temperature for 10h, dry, and roast at 650°C for 2h to obtain La and Si modified catalyst (referred to as DP -2).

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Abstract

The invention discloses a p-xylene fluid catalyst prepared by performing alkylation of methylbenzene methyl alcohol and a preparation method of the p-xylene fluid catalyst. The p-xylene fluid catalyst is prepared by modeling mixed spray of ZSM-5, matrix and amorphous binding agent, modifying by alkaline-earth metals, non-metals or / and rare earth metals and modifying by a siloxy group compound to prepare corresponding catalysts. The catalyst is used in methylbenzene methyl alcohol alkylation reaction; based on full conversion of methanol, methylbenzene conversion rate is more than 20 percent, and the once through yield of p-xylene in the product is up to 25 percent.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering, and relates to a fluidized bed catalyst for p-xylene, in particular to a fluidized-bed catalyst for producing p-xylene by alkylation of toluene with methanol and a preparation method thereof. Background technique [0002] As the main raw material for PTA production, p-xylene (PX) is widely used in many fields. With the rapid development of my country's textile industry, the production capacity of PTA has expanded rapidly in recent years. PX is far from being able to meet the demand. Judging from the situation in recent years, about 40% of the domestic consumption of PX needs to be imported. [0003] In contrast to the insufficient production capacity of PX, there is currently a serious excess of domestic methanol production capacity. Due to the rapid development of the coal chemical industry in recent years, a large number of domestic coal-to-methanol plants have been built and operat...

Claims

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Application Information

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IPC IPC(8): B01J29/40C07C15/08C07C2/86
CPCY02P20/52
Inventor 张世刚汪彩彩辛玉冰闵小建张军民刘建斌侯翠利张变玲
Owner 陕西煤化工技术工程中心有限公司
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