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Microwave-enhanced esterification rectifying device and process

A technology of esterification reaction and microwave, which is applied in the field of microwave-enhanced esterification reaction distillation equipment, to achieve the effects of reducing production energy consumption, increasing speed, and reducing energy consumption

Inactive Publication Date: 2014-04-16
INST OF METAL RESEARCH - CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the problem that the existing reactive distillation process is difficult to apply to the high boiling target product (the bubble point temperature of the target product is higher than the reaction temperature) and the production process of strong endothermic reaction. Using microwave heating to quickly supply energy to the reaction system, so that the temperature in the reactive distillation tower can meet the needs of the reaction process, so as to give full play to the advantages of efficient reaction and separation of reactive distillation, and realize energy saving and consumption reduction in the chemical process

Method used

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  • Microwave-enhanced esterification rectifying device and process
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  • Microwave-enhanced esterification rectifying device and process

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Such as figure 1 As shown, the diameter of the wave-transparent reaction material channel 1 is D=10cm, and the operating frequency of the microwave source is 2.45×109Hz. Considering the size of the waveguide port and the corresponding flange for feeding microwave energy, and taking into account the certain expansion space after microwave feeding, The minimum size of the corresponding microwave heating cavity is 60×60×32.5 cm (length×width×height). That is, the cross-sectional size of the microwave heating cavity is fixed, and the height is 32.5 cm or a multiple of 32.5 cm. The length and width of the partition are the same as the cross-sectional size of the microwave heating chamber, a=b=6.12cm, c=2cm, and the placement interval is 65cm.

[0043] The diameter of the small hole in the microwave cut-off section is 0.5 cm, and the length is 0.6 cm; the diameter of the large hole is 4 cm, and the length is 6 cm.

Embodiment 2

[0045] The diameter of the wave reaction material channel 1 is D = 30cm, and the operating frequency of the microwave source is 915MHz. Considering the size of the waveguide and the corresponding flange size for feeding microwave energy, and taking into account the certain expansion space after microwave feeding, a rectangular microwave heating cavity is used. The height h=4*19.5=78cm. It is the 334 resonance mode, and the minimum size of the corresponding microwave heating cavity is 120×120×78cm (length×width×height). That is, the cross-sectional size of the microwave heating cavity is fixed, and the height is 78cm or a multiple of 78cm. The length and width of the partition are the same as the cross-sectional size of the microwave heating cavity, a=b=16.4cm, c=6cm, and the placement interval is 78cm.

[0046] The size of the small hole in the microwave cut-off section is 1.5 cm, and the length is 2 cm; the size of the large hole is 8 cm, and the length is 10 cm.

Embodiment 3

[0048] Weigh 15 kg of citric acid and 37.5 kg of butanol, mix and heat citric acid and 15 kg of butanol until fully dissolved, and add the mixed solution of citric acid and butanol from the reaction mass at a rate of 55 kg / hour with a metering pump Port 19 is injected into the liquid-phase reaction material distributor 20, and the remaining butanol is injected into the microwave esterification reaction rectification tower from the alcohol vapor pipeline 12 by steam, and the reflux ratio of the microwave esterification reaction rectification tower top alcohol is 1 / 3. Control the reaction temperature at 235°C by controlling the power of the microwave, and the acid value of the product extracted from the bottom kettle is 0.3mg / 100gKOH. In order to compare with the conventional tank reactor, the same amount of citric acid and butanol were mixed and placed in a 100L oil bath reactor, and the oil bath temperature of the reactor was controlled at 240°C, reacted for 3.5 hours, and too...

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Abstract

The invention relates to the esterification field, in particular to a microwave-enhanced esterification rectifying device heated by microwaves and used for producing high-boiling-point esterification products, as well as a corresponding process, and solves the problem that the reactive rectification process has difficulty in being applied to the high-boiling-point target product and strong endothermic reaction manufacturing process. A microwave esterification rectifying tower consists of one or more cubic microwave multimode resonance heating cavities connected in series, a reactant passage with wave transmittance is mounted in a microwave heating cavity, and a structured packing with the same wave transmittance is arranged in the reactant passage; and the microwave esterification rectifying tower is connected with a conventional heating bottom kettle and an alcohol steam pipeline, and the upper end of the microwave esterification rectifying tower is connected with a conventional rectifying tower. The conventional rectifying tower is mainly used for alcohol and water separation, the microwave esterification rectifying tower is mainly used for esterification and rectification, and the reactants, namely alcohol and acid, enter the microwave esterification rectifying tower from the lower end and the upper end of the microwave esterification rectifying tower respectively. By adopting the invention, a high esterification effect can be obtained.

Description

technical field [0001] The invention relates to the design of a microwave heating chemical reaction device and the field of organic chemical synthesis in which an enhanced esterification reaction process is realized through reactive distillation, specifically a microwave-enhanced esterification reaction essence applied to the production of high-boiling point esterification products. Distillation equipment and corresponding processes. Background technique [0002] Esterification is an important reaction type in the organic chemical synthesis industry, and it is widely used in the production of bulk chemicals (such as plasticizers) and fine chemicals (such as flavors, fragrances, and pharmaceutical intermediates). The current main problems of esterification reaction are long reaction time (high energy consumption) and serious environmental pollution caused by sewage discharge. [0003] The long reaction time and high energy consumption are caused by the following two aspects....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/08C07C67/54B01J19/12B01D3/32B01J8/02
CPCY02P20/10
Inventor 张劲松刘志宇孙博孙家言刘强杨永进李鑫钢高鑫崔峰刘延华刘建军孙长春
Owner INST OF METAL RESEARCH - CHINESE ACAD OF SCI