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Device and method for crystallizing (meth)acrylic acid

A crystallization device, acrylic acid technology, applied in solution crystallization, heat exchange cooling crystallization, crystallization adjustment/control, etc., can solve the problem that the blockage of the heat exchanger cannot be suppressed

Active Publication Date: 2012-05-23
NIPPON SHOKUBAI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the problem of pressure rise in the reactor is a completely different problem from the problem of blockage in the crystallization unit, and the problem of blockage in the heat exchanger cannot be suppressed by this technology.

Method used

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  • Device and method for crystallizing (meth)acrylic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] (1) Preparation of crude acrylic acid solution

[0056] Propylene was supplied to the gas-phase catalytic oxidation reaction in the reactor, and the obtained reaction gas was introduced into the absorption tower and brought into contact with the absorption liquid, and a crude acrylic acid solution was obtained at the bottom of the absorption tower. Analysis of the obtained crude acrylic acid solution revealed that it contained: 90.0% by mass of acrylic acid, 3.2% by mass of water, 1.9% by mass of acetic acid, 0.6% by mass of maleic acid, 1.5% by mass of acrylic acid dimer, 0.07% by mass of furfural, 0.27% by mass of benzaldehyde, 0.06% by mass of formaldehyde, 0.1% by mass of hydroquinone, and 2.3% by mass of other impurities. In addition, the temperature of the bottom liquid of the absorption tower at this time, that is, the temperature of the crude acrylic acid solution immediately discharged from the absorption tower was 91°C. The resulting crude acrylic acid was us...

Embodiment 2

[0070] Acrylic acid was produced in the same manner as in Example 1 above, except that the pressure of the circulation supply pipe 8 was maintained in the range of 0.10 MPa to 0.16 MPa in the crystallization process. At this time, the difference between the maximum value and the minimum value of the measured pressure value was 0.06 MPa within 100% of the minimum value.

[0071] Analysis of the obtained purified acrylic acid showed that the purity of acrylic acid was 99.89% by mass, and in addition, it contained 153 mass ppm of water, 710 mass ppm of acetic acid, 4 mass ppm of maleic acid, and 100 mass ppm of acrylic acid dimer , furfural 0.5 mass ppm, benzaldehyde 0.4 mass ppm, no formaldehyde was detected. In addition, the production efficiency after the above process is 9.98kg / hour.

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Abstract

The objective of the present invention is to provide a crystallization device and a crystallization process for obtaining (meth) acrylic acid with higher purity without causing leakage of a crude solution by preventing complete clogging in a crystallization tube from occurring. The device for crystallizing (meth)acrylic acid according to the present invention is characterized in comprising a crude (meth)acrylic acid solution supply part, a crystallization tube, a heat medium supply tube, a heat medium discharge tube, a storage part of a crude (meth)acrylic acid solution passed through the crystallization tube, a tube for circulating and supplying the crude (meth)acrylic acid solution to the supply part from the storage part, and a pump for circulating and supplying the crude (meth) acrylic acid solution to the supply part from the storage part; and further comprising a pressure meter in the circulate-supply tube; wherein the device is used for carrying out dynamic crystallization in a batch manner by circulating the crude (meth)acrylic acid solution to flow the crude solution downward along the inner wall of the crystallization tube in a coating film-like state.

Description

technical field [0001] The present invention relates to a device for refining (meth)acrylic acid by crystallization and a method for crystallizing (meth)acrylic acid. Background technique [0002] (Meth)acrylic acid is generally prepared by the following method: the gas containing (meth)acrylic acid obtained by gas-phase catalytic oxidation reaction is introduced into a condensation tower or an absorption tower to obtain a crude (meth)acrylic acid solution, and then refined. As the purification method described above, crystallization is used in addition to distillation, desorption (Japanese original: dispersal), extraction, and the like. [0003] Crystallization may also be performed only by cooling a crude (meth)acrylic acid solution, but in industrial mass production, dynamic crystallization is mainly used. The dynamic crystallization is a method in which a film-like crude (meth)acrylic acid solution flows down on a heat transfer surface that is in contact with a medium o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/43B01D9/02C07C57/07
CPCB01D9/0013C07C51/43B01D9/0063C07C57/04
Inventor 坂元一彦上野晃嗣石井良武北浦正次
Owner NIPPON SHOKUBAI CO LTD
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