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Catalyst for converting alcohol ether into high p-xylene content aromatic hydrocarbon, preparation method and reaction process thereof

A para-xylene, high-content technology, applied in physical/chemical process catalysts, molecular sieve catalysts, chemical instruments and methods, etc., can solve the unstable catalyst reaction conditions, increase the difficulty and cost of operation, and difficult to treat alcohol-containing wastewater, etc. problems, to achieve the effect of broadening the applicability of raw materials, saving equipment investment, and reducing operating costs

Active Publication Date: 2014-12-24
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the conversion rate of methanol is lower than 90%, resulting in difficulties in the treatment of alcohol-containing wastewater and an increase in the recovery cost of unreacted methanol
At the same time, due to the relationship between the preparation method, this type of catalyst is unstable under the reaction conditions, and silicon components need to be added regularly, which increases the difficulty and cost of the operation of the process.
Moreover, the above-mentioned patents can only convert methanol, dimethyl ether, and methanol and dimethyl ether containing a small amount of aromatics, but cannot convert methanol or dimethyl ether containing water and a small amount of impurities such as other alcohols, ketones, acids, esters, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Immerse zinc nitrate with a concentration of 0.2 mol / L, phosphoric acid with a concentration of 0.3 mol / L and lanthanum nitrate with a concentration of 1 mol / L on ZSM-5 molecular sieves in sequence, filter each step, and dry at 110°C Dry for 2 hours, and finally bake at 700°C for 2 hours; soak the ZSM-5 molecular sieve loaded with zinc, phosphorus and lanthanum in silane, soak at 20°C for 0.5 hour, then filter, and dry at 90°C for 24 hours, and then roasted at 350°C for 24 hours; the above particles were immersed in zirconium chloride sol, treated at 50°C for 0.5 hours, then sprayed and granulated at 300°C, and dried for 2 hours, and then heated at 700°C Roast at low temperature for 3 hours; soak the above particles in benzene at room temperature for 3 hours, then filter, rinse with hydrochloric acid with a concentration of 0.1mol / L for 10 seconds, then quickly filter, wash, and dry at 90°C 24 hours, and finally calcined at 350°C for 24 hours to obtain the final catalys...

Embodiment 2

[0027] Mix a sufficient amount of silver nitrate with a concentration of 2mol / L, manganese nitrate with a concentration of 0.1mol / L, diamine hydrogen phosphate with a concentration of 1mol / L, lanthanum nitrate with a concentration of 0.2mol / L and nitric acid with a concentration of 0.3mol / L Cerium was sequentially impregnated on ZSM-5 molecular sieves, filtered each step, dried at 90°C for 24 hours, and finally calcined at 600°C for 10 hours; then ZSM-5 loaded with silver, manganese, phosphorus, lanthanum and cerium Molecular sieves were immersed in tetraethyl orthosilicate, treated at 50°C for 0.5 hours, then filtered, then dried at 100°C for 2 hours, and then roasted at 500°C for 4 hours; the above particles were immersed in titanium chloride sol, Treat at 20°C for 10 hours, then extrude, and then bake at 600°C for 5 hours; soak the above particles in toluene at room temperature for 1 hour, then filter, and use a concentration of 0.1mol / L Nitric acid solution was rinsed for ...

Embodiment 3

[0030] Zinc acetate with a concentration of 1mol / L, cobalt nitrate with a concentration of 0.5mol / L, phosphoric acid with a concentration of 2mol / L and cerium chloride with a concentration of 1mol / L are impregnated on the ZSM-5 molecular sieve in sequence, and filtered at each step , and dried at 100°C for 8 hours, and finally roasted at 650°C for 4 hours; the ZSM-5 molecular sieve loaded with zinc, cobalt, phosphorus and cerium was immersed in tetraethyl orthosilicate, and treated at 20°C 1 hour, then filtered, dried at 110°C for 8 hours, and then calcined at 550°C for 8 hours. The above particles were immersed in zirconium chloride sol, treated at 30°C for 4 hours, then sprayed and granulated at 200°C, dried for 10 hours, and then calcined at 650°C for 8 hours; the above particles were dissolved in xylene , soaked at room temperature for 0.5 hours, then filtered, and rinsed with a nitric acid solution with a concentration of 1mol / L for 0.1 second; then quickly filtered, wash...

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Abstract

The invention belongs to the technical field of chemical industry catalysis, and particularly relates to a catalyst for converting an alcohol ether into a high p-xylene content aromatic hydrocarbon, a preparation method and a reaction process thereof. According to the present invention, a molecular sieve loading a metal, phosphorus and rare earth and other reinforcing components are adopted to form high mechanical strength particles, and the surface acid sites are 0.01-1% (molar fraction) of the total acid sites of the catalyst; the preparation method relates to a method for forming composite particles through multiple forming and controlling acid of the surface of the composite particles; and the catalyst can be applicable for fixed beds, moving beds and fluidized beds, and can be provided for converting methanol or dimethyl ether raw materials containing water and a small amount of high carbon alcohol and ester, wherein one-time conversion efficiency of the methanol or the dimethyl ether at a temperature of 450-520 DEG C and a space velocity of 0.2-30 h <-1> is more than 99.9%, the total (carbon-base) yield of the aromatic hydrocarbon is more than 60%, and the mass fraction of the p-xylene in the xylene is more than 90%.

Description

technical field [0001] The invention belongs to the technical field of chemical catalysis, and in particular relates to a catalyst for converting alcohol ethers into aromatic hydrocarbons with a high content of p-xylene, a preparation method and a reaction process thereof. Background technique [0002] Using coal or natural gas to prepare methanol, and then preparing various olefins or aromatic chemicals from methanol is an important chemical technology route at present, and it is a beneficial supplement to the traditional production route that uses petroleum as raw material. Among them, modifying ZSM-5 molecular sieve and loading metals can effectively prepare aromatics, and obtain mixed aromatics mainly composed of benzene, toluene and xylene, wherein the obtained xylene is a mixture, p-xylene, o-xylene and m-xylene It is in a balanced composition (mass percentage is 23:24:53). However, p-xylene has the greatest use. To obtain a relatively large amount of p-xylene, the in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/40B01J29/48B01J29/46C07C15/08C07C1/20
CPCY02P20/52
Inventor 骞伟中张金贵孔垂岩魏飞
Owner TSINGHUA UNIV
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