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Preparation method of shape-selective catalyst used for p-dialkyl benzene synthesis process

The technology of p-dialkylbenzene and catalyst is applied in the field of preparation of shape-selective catalysts in the process of synthesizing p-dialkylbenzene, and can solve the problems of complicated operation, lowering of acidity in pores, lowering of acidity of outer surface, etc. The effect of improving shape selection performance and improving selectivity

Active Publication Date: 2012-06-27
溧阳常大技术转移中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method of silicon deposition can effectively improve the shape-selective performance of molecular sieve catalysts, due to the weak force between the hydroxyl groups on the surface of molecular sieves and the sediments, it often takes 3-4 times of deposition to achieve better results, so the operation is more cumbersome , higher energy consumption
Pre-coking can also improve the shape-selective performance of molecular sieve catalysts, but since the regenerated catalyst must be pre-coked again, the operation is cumbersome, and it is currently limited to laboratory research
It is very simple to use metal oxide modification to cover the acid sites on the outer surface of molecular sieves, and a good covering effect can be achieved in one operation. Can be used on a large scale

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take magnesium nitrate (2.44g), add it in (29.9ml) dehydrated alcohol, wherein the mass ratio of magnesium nitrate and dehydrated alcohol is 1:10, treat that it dissolves completely and then add complex ligand citric acid (3.16g), wherein the molar ratio of citric acid and magnesium ions in magnesium nitrate is 1:1, stir well, then add microporous molecular sieve MCM-22 (4.0g) wherein, magnesium ion in magnesium nitrate and microporous molecular sieve The mass ratio of MCM-22 is 1:10, then stir evenly, let it stand at room temperature for 24 hours, put it in a 60°C water bath to dry, then transfer to an oven to dry at 120°C for 6 hours, and then put it in a muffle furnace for roasting , the temperature was raised to 550 °C at 10 °C / min and kept for 6 h, and the desired shape-selective catalyst with a magnesium ion loading of 10% was obtained. The catalyst was used in the process of alkylation of toluene and dimethyl carbonate to synthesize p-xylene, the molar ratio was ...

Embodiment 2

[0017] Compared with Example 1, the molar ratio of magnesium ions in citric acid and magnesium nitrate is changed to 2:1, and the others are the same. The catalyst was used in the process of alkylation of toluene and dimethyl carbonate to synthesize p-xylene, the molar ratio was toluene: dimethyl carbonate 4:1, the reaction temperature was 380 °C, and the mass space velocity of the raw material was 1 h -1 , the conversion rate of toluene reached 33.9%, and the selectivity of p-dimethylbenzene was 77.1%.

Embodiment 3

[0019] Compared with Example 1, the molar ratio of magnesium ions in citric acid and magnesium nitrate is changed to 3:1, and the others are the same. The catalyst was used in the process of alkylation of toluene and dimethyl carbonate to synthesize p-xylene, the molar ratio was toluene: dimethyl carbonate 4:1, the reaction temperature was 380 °C, and the mass space velocity of the raw material was 1 h -1 , the conversion rate of toluene reached 35.2%, and the selectivity of p-xylene was 75.4%.

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PUM

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Abstract

The invention relates to a preparation method of a shape-selective catalyst used for a p-dialkyl benzene synthesis process, and relates to the technical field of preparation of a high-performance catalyst for an alkylation process. The preparation method comprises the steps of: weighing a metal nitrate, adding to absolute ethanol at a mass ratio of metal nitrate to absolute ethanol being 1:10 for completely dissolving, then adding a complex ligand at a molar ratio of the complex ligand to metal ions in the metal nitrate being (1:1)-(3:1), uniformly stirring, adding a microporous molecular sieve at a mass ratio of the metal ions in the metal nitrate to the microporous molecular sieve being (1:100)-(1:10), uniformly stirring, standing at room temperature for 24h, drying in a 60 DEG C water bath, then transferring to an oven, drying at 120 DEG C for 6h, baking in a muffle furnace, heating to 550 DEG C at a speed of 10 DEG C / min, and maintaining the temperature for 6h to obtain the required shape-selective catalyst. The preparation method is simple and low in cost; and the obtained shape-selective catalyst has high shape selective performance.

Description

technical field [0001] The invention relates to the technical field of preparing a high-performance catalyst in an alkylation process, in particular to a preparation method for a shape-selective catalyst in the process of synthesizing p-dialkylbenzene. Background technique [0002] P-dialkylbenzenes such as p-xylene and p-diethylbenzene are important chemical raw materials, and their traditional synthesis methods are mainly obtained through the disproportionation process of toluene or ethylbenzene, but because the disproportionation process requires a strong acidic catalyst and a high The reaction temperature is higher, so the catalyst deactivation is faster. In recent years, the synthesis of p-xylene and p-diethylbenzene by direct alkylation of toluene or ethylbenzene has become a research hotspot. [0003] The commonly used catalysts in the alkylation process of toluene and ethylbenzene are microporous molecular sieves such as ZSM-5 or MCM-22. The alkylation reaction can ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/40B01J29/70C07C2/86C07C15/08C07C15/02
CPCY02P20/52
Inventor 李永昕薛冰许杰刘平张卫红
Owner 溧阳常大技术转移中心有限公司
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