Method and system for energy-saving separation of DCB-NMP mixture

A technology of DCB-NMP and separation method, applied in the field of PPS device and resource recovery, which can solve the problems of high cost, unreasonable energy utilization, large amount of heat transfer oil, etc.

Active Publication Date: 2020-01-10
南京佳华科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Chinese patent CN 106478481A discloses an ultra-high-purity separation and purification process for wastewater containing N-methylpyrrolidone and p-dichlorobenzene. The raw materials of this invention are all liquid phases, and a pressurized rectification system with a three-tower series structure is used. High-purity NMP is extracted from the bottom of the first tower, and DCB is extracted from the bottom of the third tower after two condensations at the top of the tower. The azeotrope of DCB and water is repeatedly heated and condensed, and its energy utilization is not Reasonable
Since both the fractionation tower and the NMP rectification tower are heated by heat transfer oil, and the boiling points of NMP and heavy components are both greater than 200°C, the traditional technical solution requires a large amount of heat transfer oil and a high heat load, resulting in excessive natural gas consumption for the heat transfer oil heating furnace. big, cost too much

Method used

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  • Method and system for energy-saving separation of DCB-NMP mixture
  • Method and system for energy-saving separation of DCB-NMP mixture
  • Method and system for energy-saving separation of DCB-NMP mixture

Examples

Experimental program
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Effect test

Embodiment 3

[0059] like figure 2 As shown, a DCB-NMP mixture double-effect rectification separation system adopts a high-pressure dehydration tower and a low-pressure dehydration tower in parallel, including a fractionation tower 1, a fractionation tower condenser 2, a phase separation tank 3, and a fractionation tower reboiler 9 , low pressure dehydration tower 4, low pressure dehydration tower condenser 5, first low pressure dehydration tower reboiler 10, second low pressure dehydration tower reboiler 11, high pressure dehydration tower 6, first high pressure dehydration tower reboiler 12, rectification Tower 7, rectifying tower reboiler 14; The tower top gas outlet of described fractionating tower 1 is connected with the inlet of phase-separating tank 3 through fractionating tower condenser 2, and the water phase outlet of phase-separating tank 3 is refluxed with fractionating tower 1 The liquid inlet is connected, the oil phase outlet of the phase separation tank 3 is used to extract...

Embodiment 2

[0066] The DCB-NMP mixture (same as Example 1) is separated and recovered based on the DCB-NMP mixture double-effect rectification separation system of Example 1, including the following steps:

[0067] Step (1), fractionation treatment: the DCB-NMP mixture is sent to fractionation tower 1 (the number of theoretical plates is 52), the operating pressure of the fractionation tower is controlled to be 0.13MPa, the operating temperature is 80°C, and the reflux ratio is 2.1; The tower condenser 2 enters the phase separation tank 2, and the non-condensable gas (H 2 S) Discharge from the top of the tank, absorb H with water or lye 2 S, the oil phase is extracted from the oil phase outlet to obtain DCB with a purity of 99.8%, the DCB yield is 99.55%, and the water phase is discharged from the water phase outlet and refluxed to the fractionation tower;

[0068] Step (2), double-effect rectification dehydration: step (1) the liquid phase extracted from the fractionating tower still is...

Embodiment 4

[0076] The DCB-NMP mixture (same as Example 1) is separated and recovered based on the DCB-NMP mixture double-effect rectification separation system of Example 1, including the following steps:

[0077] Step (1), fractionation treatment: the DCB-NMP mixture is sent to fractionation tower 1 (the number of theoretical plates is 47), the operating pressure of the fractionation tower is controlled to be 0.14MPa, the operating temperature is 90°C, and the reflux ratio is 2.3; the gas phase at the top of the tower is fractionated. The tower condenser 2 enters the phase separation tank 2, and the non-condensable gas (H 2 S) Discharge from the top of the tank, absorb H with water or lye 2 S, the oil phase is extracted from the oil phase outlet to obtain DCB with a purity of 99.8%, the DCB yield is 99.55%, and the water phase is discharged from the water phase outlet and refluxed to the fractionation tower;

[0078] Step (2), double-effect rectification and dehydration: the liquid pha...

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Abstract

The invention belongs to the field of resource recovery, and discloses a method for energy-saving separation of a DCB-NMP mixture. The method comprises the following steps: (1) fractionating: enablingcooled or uncooled gas-phase raw material containing DCB and NMP and/or liquid-phase raw material containing DCB and NMP to enter a fractionating tower, performing azeotropic treatment on water and DCB, condensing a tower top gas phase, allowing the condensed tower top gas phase to enter a phase separation tank for layering to achieve a separation effect and obtain an oil phase and a water phase,and enabling the water phase to flow back into the fractionating tower; (2) dehydrating: feeding a material flow at the bottom of the fractionating tower into a dehydration system, and performing dehydration; and (3) rectifying: feeding the dehydrated mixture into a rectifying tower to separate NMP from heavy components, and obtaining a high-purity NMP product from the top of the rectifying tower. The invention further provides a system for energy-saving separation of the DCB-NMP mixture. The method has the advantages of small investment, low energy consumption, reduction of environmental pollution, and deeply recovery of ultra-pure DCB and NMP products.

Description

technical field [0001] The invention belongs to the field of resource recovery, in particular to the field of PPS devices, in particular to the recovery of NMP therein, and relates to an energy-saving separation method and system for a DCB-NMP mixture. Background technique [0002] PPS (polyphenylene sulfide, Polyphenylene sulfide) is a crystalline high-rigidity white powder polymer, which is a special engineering plastic with excellent comprehensive properties. PPS has the characteristics of excellent high temperature resistance, corrosion resistance, radiation resistance, flame retardancy, balanced physical and mechanical properties, excellent dimensional stability and excellent electrical properties, and is widely used as a structural polymer material. It is widely used as a special engineering plastic after being stabilized. At the same time, it can also be made into various functional films, coatings and composite materials, and has been successfully applied in the fie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/267C07C17/383C07C25/08
CPCC07D207/267C07C17/383C07C25/08Y02P20/10
Inventor 刘琼黄小康赵怡谢佳华
Owner 南京佳华科技股份有限公司
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