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Supercritical carbon dioxide assisted periodic devolatilization process and device

A carbon dioxide and supercritical technology, which is applied in the production of bulk chemicals, chemical instruments and methods, and separation methods, can solve the problems of high-efficiency devolatilization and discharge in the vacuum devolatilization process, and promote rapid degassing and degassing volatilization, improve devolatilization efficiency, and save resources

Pending Publication Date: 2022-02-01
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to provide a supercritical carbon dioxide-assisted periodic devolatilization process and device, which solves the problem of inability to balance high-efficiency devolatilization and discharge in the vacuum devolatilization process in the prior art by periodically changing the pressure. Especially for heat-sensitive and / or high-viscosity polymers, it can effectively prevent the decomposition of polymers while efficiently devolatilizing under low temperature conditions, and can also have a good devolatilization effect for polymers containing high volatility

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  • Supercritical carbon dioxide assisted periodic devolatilization process and device
  • Supercritical carbon dioxide assisted periodic devolatilization process and device

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Embodiment 1

[0046] refer to figure 1 , the present embodiment provides a supercritical carbon dioxide-assisted periodical devolatilization device, comprising a devolatilization tank 1, a pressure sensor 7 and a vacuum pump 9; the top of the devolatilization tank 1 is provided with an exhaust port 11, and the exhaust port 11 is connected to The vacuum pump 9 is connected; the pressure sensor 7 is connected with the devolatilization tank 1 and the vacuum pump 9 respectively; the pressure sensor 7 is connected with the vacuum valve 8 of the vacuum pump 9, and the critical pressure of the pressure sensor 7 is set, and when the pressure in the devolatilization tank 1 reaches the critical pressure, The vacuum valve 8 is opened or closed, and the vacuum pump 9 starts / stops working. Preferably, the outer wall of the devolatilization tank 1 is provided with a heat preservation jacket, and a circulating heat medium / cold medium is arranged in the heat preservation jacket,

[0047] The top of the de...

Embodiment 2

[0067] This embodiment takes high-viscosity polymers as an example, specifically including but not limited to SAN resin, polymethyl methacrylate (PMMA), polyacrylonitrile (PAN), etc. The devolatilization characteristic of high-viscosity polymers is that bubbles Many but not easy to completely remove, this embodiment is a periodic devolatilization process, including multiple pressure cycles, with carbon dioxide as the supercritical medium, the pressure first increases and then decreases during the pressure cycle, so that the carbon dioxide is in a supercritical state Change between gaseous and gaseous states to achieve polymer devolatilization.

[0068] Specifically, this embodiment takes PMMA as an example. The devolatilization process of PMMA in the prior art mostly adopts extruder extruding mode to carry out devolatilization. Chinese invention patent CN113459324A discloses a devolatilization screw extruder device and a method for producing PMMA using the device, which uses ...

Embodiment 3

[0078] This embodiment takes polystyrene (PS) as an example to further illustrate the technical solution of the present invention.

[0079] Chinese invention patent CN10220109A discloses a supercritical fluid devolatilization method for polystyrene, which includes using carbon dioxide as a supercritical medium to realize the devolatilization process of polystyrene, which can reduce the residual monomer in the polymer to 1ppm the following. However, the devolatilization process takes a long time and can be completed in at least 6 hours, and the devolatilization efficiency is low. And it uses polystyrene resin particles as raw material, intermittent fixed bed for devolatilization, that is, the product is devolatilized after the production is completed, the effect is better for polystyrene resin particles with small particle size, and for the requirements particle size, this process cannot complete the devolatilization process. Therefore, the practical significance is limited. ...

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Abstract

The invention discloses a supercritical carbon dioxide assisted periodic devolatilization process which comprises a plurality of pressure cycle periods, carbon dioxide is taken as a supercritical medium, and the pressure is firstly increased and then reduced in the pressure cycle periods, so that the carbon dioxide is converted between a supercritical state and a gaseous state, and polymer devolatilization is realized. The devolatilization process is carried out on the thermosensitive polymer according to the principle that the solubility of volatile components in supercritical CO2 is larger than that of the volatile components in the polymer and periodic pressure is adopted to promote bubble breaking, high-efficiency devolatilization can be carried out under the low-temperature condition, the devolatilization time is short, devolatilization and discharging can be carried out at the same time, the content of volatile components in the devolatilized high polymer is reduced to below 50ppm, and the efficiency is high.

Description

technical field [0001] The invention relates to the technical field of fluid devolatilization, in particular to a supercritical carbon dioxide assisted periodic devolatilization process and device. Background technique [0002] Devolatilization is a technology that removes one or more monomers or solvents that have not participated in the reaction from the polymer through heating and volatilization. During the devolatilization process, effective heating must be considered to increase the heating temperature to volatilize the monomers and solvents and raise the temperature of the polymer. It reaches above the softening point and has fluidity, but at the same time it is not overheated and does not damage the molecular weight, color and other properties of the polymer. Apparently, the polymer devolatilization process is essentially a process of thermal melting and controlled separation of polymers, and the key points are the control of pressure, temperature and heating time. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F6/00C08F112/08C08F120/14C08F114/06C08F236/06C08F236/08B01D1/14
CPCC08F6/005B01D1/14C08L25/06C08L33/12C08L27/06C08L9/00Y02P20/54C08C2/02
Inventor 仇枭逸奚桢浩赵鸣黄剑清王雪松张林李响
Owner EAST CHINA UNIV OF SCI & TECH
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