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Method for synthesizing paraxylene through toluene and methanol shape-selective alkylation

A technology of p-xylene and chemical synthesis, applied in the direction of chemical instruments and methods, hydrocarbons, hydrocarbons, etc., can solve the problems of poor catalyst stability and low product selectivity

Active Publication Date: 2016-04-20
SHANGHAI HUAYI GRP CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is the problem of low product selectivity and poor catalyst stability in the prior art, and a new method for synthesizing p-xylene by shape-selective alkylation of toluene and methanol is provided

Method used

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  • Method for synthesizing paraxylene through toluene and methanol shape-selective alkylation
  • Method for synthesizing paraxylene through toluene and methanol shape-selective alkylation
  • Method for synthesizing paraxylene through toluene and methanol shape-selective alkylation

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Experimental program
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Effect test

Embodiment 1

[0030] Set the mass to 80g, and SiO 2 / Al 2 o 3 After mixing 60g of HZSM-35 molecular sieve with a molar ratio of 200 and 20g of EU-1 molecular sieve evenly, put it into a solution of tetrapropylammonium hydroxide with a concentration of 0.1M, stir for 12 hours, then suction filter, wash, acid exchange, and dry Dry it, and then place it in a muffle furnace for calcination at 550°C for 4h. Mix the alkali-treated HZSM-35 and EU-1 molecular sieves with 20g of alumina, then add Tianqing powder and dilute nitric acid and knead them evenly, carry out extrusion molding, dry at 80°C, and roast at 540°C to obtain the shaped ZSM -35 / EU-1 molecular sieve; pre-vacuumize 50g of ZSM-35 / EU-1 molecular sieve formed, after vacuum impregnation in aqueous solution of calcium nitrate, filter off excess solution, dry at 80°C for 24 hours, then Roast at 540°C for 4 hours to obtain a catalyst loaded with calcium oxide; then vacuum impregnate with the prepared aqueous solution of palladium chlorid...

Embodiment 2

[0032] Set the mass to 60g, and SiO 2 / Al 2 o 3After mixing 45g of HZSM-5 molecular sieve with a molar ratio of 60 and 15g of MCM-22 molecular sieve evenly, put it into a sodium hydroxide solution with a concentration of 0.3M, stir for 0.5 hours, then suction filter, wash, acid exchange, and dry, then Place it in a muffle furnace for calcination at 550°C for 4h. Mix the alkali-treated HZSM-5 and MCM-22 molecular sieves with 20g of alumina, then add Tianqing powder and dilute nitric acid and knead them evenly, then extrude them into strips, dry them at 80°C, and roast them at 540°C to obtain the shaped ZSM -5 / MCM-22 molecular sieve; Add 50g of methanol, 35g of ethanol, 60g of hydrazine hydrate, 25g of sodium hydroxide, 5g of distilled water and 30g of potassium borohydride in a three-necked flask, and the above 50g of formed ZSM-5 / MCM-22 Add the catalyst into a three-necked flask, keep stirring at 80°C for 30 minutes, take out the catalyst and wash it three times with distil...

Embodiment 3

[0034] Set the mass to 80g, and SiO 2 / Al 2 o 3 Put the HZSM-5 molecular sieve with a molar ratio of 200 into the tetraethylammonium hydroxide solution with a concentration of 0.4M, stir for 1 hour, then filter with suction, wash, acid exchange, and dry, and then place it in a muffle furnace at 550°C Calcination 4h. Mix the alkali-treated HZSM-5 with 20g of alumina, add methyl cellulose and dilute nitric acid and knead evenly, carry out extrusion molding, dry at 80°C, and roast at 540°C to make ZSM-5 molecular sieve catalyst; The obtained 50g ZSM-5 molecular sieve was vacuum-impregnated in cerium nitrate solution, and after filtering off the excess solution, it was dried at 80°C for 24 hours, and then roasted at 540°C for 4 hours to obtain a catalyst supporting cerium oxide. After vacuum impregnation in petroleum ether solution, let stand after impregnation until the solvent is completely volatilized, dry and bake at 540°C for 4 hours; repeat the above methyl hydroxy silico...

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Abstract

The invention relates to a method for synthesizing paraxylene through toluene and methanol shape-selective alkylation and mainly solves the problems that in the prior art, a product is low in selectivity, and a catalyst is poor in stability. According to the method for synthesizing paraxylene through toluene and methanol shape-selective alkylation, toluene and methanol raw materials are in contact with a catalyst in a reaction container, and a product containing the paraxylene is generated under certain operation conditions; according to the operation conditions, the reaction temperature is 400-600 DEG C, the reaction gage pressure is 0-2.0 MPa, the diluent gas / hydrocarbon mole ratio is 0.5-10, the water / hydrocarbon mole ratio is 0.1-5, the toluene / methanol mole ratio is 1-10, and the mass space velocity is 0.1-5<-1> hour. By means of the technical scheme of the method, the mentioned problems are solved, and the method can be used for synthesizing paraxylene through toluene and methanol shape-selective alkylation.

Description

technical field [0001] The invention relates to a method for synthesizing p-xylene by shape-selective alkylation of toluene and methanol. Background technique [0002] P-xylene is an important chemical raw material, and its demand has been growing continuously. However, the main industrial production methods - xylene isomerization separation and toluene shape-selective disproportionation have low xylene yield and raw material utilization respectively. low problem. The catalytic alkylation of toluene and methanol to xylene through molecular sieves has been considered as a production method that can replace the above two traditional processes. However, the problem of carbon deposition in the catalyst results in poor reaction stability, which limits its industrial application. [0003] The document US7060864 discloses that the introduction of water during the alkylation reaction of toluene and methanol can effectively improve the stability of the catalyst, and explains that it...

Claims

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Application Information

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IPC IPC(8): C07C15/08C07C2/86B01J29/80B01J29/48
CPCY02P20/52C07C2/864B01J29/44B01J29/46B01J29/48B01J29/67B01J29/68B01J29/7492B01J29/7646B01J29/7676B01J29/80C07C2529/48C07C2529/80C07C15/08
Inventor 唐建远宁春利李永刚赵成文娄报华张春雷
Owner SHANGHAI HUAYI GRP CO
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