Preparation method of p-diethylbenzene catalyst by using high-efficiency alkylation of ethylbenzene

A technology of diethylbenzene catalyst and p-diethylbenzene, which is applied in the direction of catalyst activation/preparation, carbon compound catalyst, physical/chemical process catalyst, etc., and can solve the problem of low ethylbenzene conversion rate, low ethanol utilization rate, and poor repeatability of catalyst regeneration problems such as simplification of impregnation steps, reduction of production costs, and improvement of catalyst stability

Active Publication Date: 2018-04-17
CNOOC TIANJIN CHEM RES & DESIGN INST +2
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Problems solved by technology

The catalyst prepared by this method has a selectivity of 95-98% to diethylbenzene in the alkylation reaction of ethyl phenylethanol, but the conversion rate of ethylbenzene is low (only 5-10%), and the performance in practical application The resulting catalyst has poor regeneration repeatability and is not suitable for industrial applications
[0005] CN200410020397.7 discloses a method for synthesizing p-diethylbenzene by the alkylation reaction of ethylbenzene and ethanol, using the HZSM-5 molecular sieve with SiO2/Al2O3=100 a

Method used

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  • Preparation method of p-diethylbenzene catalyst by using high-efficiency alkylation of ethylbenzene
  • Preparation method of p-diethylbenzene catalyst by using high-efficiency alkylation of ethylbenzene

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Embodiment 1

[0024] Weigh 133g of nano-hydrogen ZSM-5 molecular sieve with a grain size of 50-100nm, add 120g of pseudoboehmite and 3g of scallop powder, mix well, then add 21.45g of magnesium acetate, 42.24g of phosphoric acid and 117g of dilute nitric acid solution , kneaded and extruded to form a strip, dried at 550°C for 4 hours, and hydrothermally treated at 450°C for 6 hours. The obtained carrier was placed in a cyclohexane solution containing 34.22g of simethicone oil for equal volume impregnation for 6 hours. After drying, it was heated at 550 The p-diethylbenzene catalyst can be obtained by calcination at ℃ for 4 hours, and it is loaded into a fixed bed reactor to evaluate the alkylation reaction of ethylphenylethanol. The reaction temperature is 360°C, the reaction pressure is normal pressure, and the molar ratio of ethylbenzene to ethanol is 2:1, and the space velocity of the liquid phase raw material is 3h -1 , the conversion rate of ethylbenzene is 19.8%, the selectivity to di...

Embodiment 2

[0026] Weigh 266g of nano-hydrogen ZSM-5 molecular sieve, the grain size is 50-150nm, add 240g of pseudoboehmite, 6g of methyl cellulose, mix well, add 38.16g of magnesium nitrate, 45.4g of diammonium hydrogen phosphate and 235g of Dilute nitric acid solution, knead and extrude into strips, dry at 550°C for 4 hours, and hydrothermally treat at 500°C for 4 hours. The obtained carrier is placed in a methylcyclohexane solution containing 65.4g of tetraethyl orthosilicate for equal volume impregnation After drying for 4 hours at 550°C, the p-diethylbenzene catalyst can be obtained. Put it into a fixed-bed reactor to evaluate the alkylation reaction of ethyl styrene. The reaction temperature is 360°C, and the reaction pressure is normal pressure. The molar ratio of benzene to ethylene is 3:1, and the space velocity of the liquid phase raw material is 3h -1 , the conversion rate of ethylbenzene is 18.4%, the selectivity to diethylbenzene is 97.4%, and the reaction time is 323h.

Embodiment 3

[0028] Weigh 133g of nano-hydrogen ZSM-5 molecular sieve with a crystal grain size of 100-200nm, add 110g of pseudoboehmite and 3g of turnip powder, mix well, add 30.32g of magnesium sulfate, 42.58g of ammonium dihydrogen phosphate and 105g of dilute Nitric acid solution, kneaded and extruded to form a strip, dried at 550°C for 6h, and hydrothermally treated at 550°C for 3h, and the obtained carrier was placed in a cyclopentane solution containing 40.85g of diethyl silicone oil for 8h of equal volume. After drying After roasting at 550°C for 6 hours, the p-diethylbenzene catalyst can be obtained, and it is put into a fixed bed reactor to evaluate the alkylation reaction of ethylbenzene and ethanol. The reaction temperature is 380°C, the reaction pressure is normal pressure, and the ratio of ethylbenzene and ethanol The molar ratio is 8:1, and the space velocity of the liquid phase raw material is 8h -1 , the ethylbenzene conversion rate is 12.1%, the p-diethylbenzene selectivi...

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Abstract

The invention discloses a preparation method of a p-diethylbenzene catalyst by using high-efficiency alkylation of ethylbenzene, and belongs to the technical field of preparation of catalysts. The preparation method comprises the following steps of mixing a nanometer hydrogen type ZSM-5 molecular sieve, an adhesive and an extrusion additive; adding an inorganic acid solution and modified components of magnesium and phosphor in the kneading process, mixing, peptizing, extruding, forming, and treating by hydrothermal aging, so as to improve the stability of the catalyst; impregnating the modified component of silicon in the carrier by one step, so as to obtain the catalyst, wherein the pore size of the molecular sieve of the catalyst and the acidity at the outer surface are modified, and thereaction property and stability are obviously improved under the synergistic modifying function of magnesium, silicon and phosphor. The preparation method has the advantages that compared with the prior art, the modified components of magnesium and phosphor can be directly lead in the strip extruding process, so that the preparation process is simplified, and the industrial production cost is reduced; after the prepared catalyst is evaluated by a fixed bed miniature reaction device in a laboratory, the selectivity on p-diethylbenzene reaches 98.5%, the conversion rate of ethylbenzene reaches20%, and the stable running period is 350h.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a preparation method of a catalyst for efficiently alkylating ethylbenzene to produce p-diethylbenzene. Background technique [0002] P-diethylbenzene is an essential analytical agent in the process of adsorption and separation of p-xylene, and its synthesis has very important social benefits and practical value. The industry requirement for p-diethylbenzene as a p-xylene desorbent is that its purity is greater than 95%. However, due to the similar boiling points of p-diethylbenzene, o-diethylbenzene and m-diethylbenzene, the rectification method is used to purify p-diethylbenzene products from mixed diethylbenzene (p-diethylbenzene content 30%), and the separation energy consumption is high , the purity is also difficult to meet the requirements. At present, the industrial production of p-diethylbenzene generally adopts the catalyst with HZSM-5 as the main body, a...

Claims

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Application Information

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IPC IPC(8): B01J29/40C07C2/66C07C2/86C07C15/02
CPCB01J29/40B01J37/0207B01J37/10B01J2229/12B01J2229/18B01J2229/32B01J2229/37C07C2/66C07C2/864C07C2529/40C07C15/02
Inventor 王银斌汪洋郭春垒刘航孙振海于海斌臧甲忠隋芝宇李佳彭晓伟姜雪丹张永惠
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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