A device and method for preparing durene by using methanol and mixing C4

A technology of mesitylene and methanol, applied in the field of petrochemical product synthesis, can solve the problems of high separation cost, many by-products, and high raw material cost, and achieve the effects of reducing the content of by-products, reducing the separation cost, and simplifying the production process

Active Publication Date: 2021-06-29
潍坊弘润新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The C10 component crystallization / adsorption separation method has complicated process, high energy consumption, low yield and purity of durene, and the raw material sources of heavy aromatics rich in durene are limited, which cannot satisfy downstream pyromellitic dianhydride Or the market growth demand of polyimide; the process of producing durene by isomerization of partial toluene also has the defects of limited source of raw materials, catalyst deactivation, and insufficient stability; The toluene chloromethylation method has high cost of raw materials, limited sources, unsatisfactory catalyst activity, selectivity and stability, severe corrosion, and environmental pollution; the reaction conditions of the gas-phase isomerization and disproportionation of methylene trimethylbenzene are harsh, and industrialization has not yet been realized. ;Using methanol as raw material to synthesize durene can solve the problem of limited raw materials in the upstream of durene, but the traditional method for preparing durene from methanol has the disadvantages of many by-products, complicated process, difficulty in controlling the degree of alkylation, and high separation cost

Method used

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  • A device and method for preparing durene by using methanol and mixing C4

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Effect test

Embodiment 1

[0051] A device that utilizes methanol and mixed C4 to prepare durene, such as figure 1 As shown, it includes an alkylation reactor 1, an oil-water separator 2, a de-C5 rectification tower 3, a de-C9 rectification tower 4, an alkylation reactor 5 and a freeze crystallization device 6, and the alkylation reactor 1 is vertically arranged, The alkylation reactor 1 is divided into the first section, the second section and the third section from top to bottom, the top, the first section and the second section of the alkylation reactor 1 have methanol inlets, and the second section of the alkylation reactor 1 The mixed C4 inlet is opened in the first section, and the product outlet is opened at the bottom of the alkylation reactor 1. The first section is filled with H-ZSM-5 after hydrothermal treatment, the second section is filled with Ag modified H-ZSM-5, and the third section is filled with Filled with Ni modified H-ZSM-5;

[0052] Methanol and mixed C4 enter the alkylation reac...

Embodiment 2

[0056] This embodiment is the same as Embodiment 1, the difference is:

[0057] The molar ratio of methanol and mixed C4 feed is 3:1 (methanol is the total amount entering the alkylation reactor; the proportion of methanol entering the top of the reactor, the first section, and the second section is required to be 50%, 10%, and 40% ), the three-stage reaction conditions of the alkylation reactor: temperature 390°C, pressure 3MPa, mass space velocity 2h -1 , the residence time is 2s; the reaction conditions of the alkylation reactor: the reaction temperature is 380°C, the reaction pressure is 3.0MPa, and the mass space velocity is 2h -1 . The durene with a purity of 98% was obtained, and the yield of durene was 28%.

Embodiment 3

[0059] This embodiment is the same as Embodiment 1, the difference is:

[0060] The molar ratio of methanol and mixed C4 feed is 4:1, and the three-stage reaction conditions of the alkylation reactor are: temperature 400°C, pressure 4MPa, mass space velocity 3h -1 , the residence time is 4s; the reaction conditions of the alkylation reactor: the reaction temperature is 400°C, the reaction pressure is 4.0MPa, and the mass space velocity is 4h -1 . Freeze and crystallize at -15°C. After crystallization, centrifuge at 1500 r / min to obtain durene with a purity of 97%, and the yield of durene is 27%.

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Abstract

The invention discloses a device and a method for preparing durene by utilizing methanol and mixed C4. The alkylation reactor is divided into the first section, the second section and the third section from top to bottom. The top, the first section and the second section of the alkylation reactor are provided with methanol inlet, and the second section of the alkylation reactor is provided with a mixing C4 inlet, the product outlet is opened at the bottom of the alkylation reactor, the first section is filled with H-ZSM-5 after hydrothermal treatment, the second section is filled with Ag-modified H-ZSM-5, and the third section is filled with Ni-modified H‑ZSM‑5; the product of the alkylation reactor enters the oil-water separator, the product in the oil-water separator is separated to remove dry gas and water, and enters the de-C5 rectification tower, and the bottom material of the de-C5 rectification tower enters the de-C9 rectification tower Distillation tower, the bottom material of the C9 rectification tower enters the cooling crystallization equipment, the tower top of the C9 rectification tower is connected to the alkylation reactor through the C9 pipeline, and the C9 pipeline opens a methanol inlet, and the tower top of the C9 rectification tower The material is mixed with methanol and enters the alkylation reactor, and the product of the alkylation reactor enters the oil-water separator.

Description

technical field [0001] The invention belongs to the field of synthesis of petrochemical products, in particular to a device and method for preparing durene by using methanol and mixed C4. Background technique [0002] Durene, that is, 1,2,4,5-tetramethylbenzene, is an important fine chemical raw material, and is an important raw material for medicine, powder coating matting agent, dye, pesticide, and surfactant. The most important use is to produce pyromellitic dianhydride and further produce polyimide. Polyimide has the advantages of thermal oxidation stability and good insulation, and is widely used in aerospace, electrical insulation, atomic energy industry, satellite, nuclear submarine, microelectronics and other precision machinery. [0003] At present, the production process of durene is mainly divided into two types: separation method and synthesis method. The separation method includes: C10 heavy aromatics crystallization separation method, C10 heavy aromatics disti...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07C2/86C07C15/02C08G73/10
CPCC07C2/864C07D493/04C08G73/1003C07C15/02
Inventor曲延涛张范赵汝臣朱文聪
Owner潍坊弘润新材料有限公司