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Combined process for treatment of PTA (pure terephthalic acid) refined waste water

A technology for terephthalic acid and refined wastewater, applied in natural water treatment, water/sewage multi-stage treatment, water/sludge/sewage treatment, etc., can solve the problem of increasing treatment difficulty, affecting hydrogenation reaction, and affecting product purity and other issues to achieve the effect of reducing overall emissions

Inactive Publication Date: 2013-01-16
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In recent years, there have been patent reports on the method of recycling useful components in wastewater in the process of treating PTA refining wastewater. CN102139970A discloses a method for recycling purified terephthalic acid production wastewater, which uses microfiltration-membrane extraction-resin adsorption The combined process treats the PTA refined wastewater to make the wastewater meet the water standard of the refining unit, but the unpretreated PTA refined wastewater contains more solid suspended particles, which makes the operating load of the microfiltration membrane larger and the operation cycle shorter; and in the membrane The extraction step needs to add an extraction accelerator, which will contain the accelerator in the treated water, and if it is reused, it will affect the purity of the product
CN101723531B provides a method for the treatment and reuse of purified terephthalic acid wastewater, using "neutralization + solid-liquid separation" as pre-membrane pretreatment, and adopting "ultrafiltration + two-stage reverse osmosis" double-membrane process for membrane treatment, so that the treated wastewater meets the water requirements of the refining unit of the production system, but the neutralization reaction of this process requires the addition of lye, which introduces more sodium ions, which increases the difficulty of subsequent treatment, and does not consider the reuse of aromatic acids. serious waste of resources
CN101544429B has introduced a kind of method of extraction-ultrafiltration-reverse osmosis combination treatment PTA refining wastewater, adopt p-xylene to extract the purified wastewater of purified terephthalic acid, the extraction phase is returned in the preparation process of purified terephthalic acid, and the raffinate phase After ultrafiltration and reverse osmosis treatment, the permeated water reaches the reuse standard. However, since the PX dissolved in the water is not treated in this method, returning to the system will affect the hydrogenation reaction and thus affect the product purity.

Method used

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  • Combined process for treatment of PTA (pure terephthalic acid) refined waste water

Examples

Experimental program
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Embodiment 1

[0019] The method adopted in this embodiment is as figure 1 shown.

[0020] PTA refined wastewater enters the sieve plate extraction tower from the top of the tower, PX enters from the bottom of the tower, the volume ratio of PX to wastewater is 1:4, the extraction temperature is 30°C, the two phases are in countercurrent contact in the extraction tower, and the waste water in the extraction tower The residence time is 8min. The extract phase is cut out from the top of the tower and sent to the PTA oxidation system as the reaction raw material. The raffinate phase enters the microfiltration membrane separation device through the circulation pump. The membrane material is porous alumina ceramic membrane with a membrane pore size of 0.05 μm and an operating pressure of 0.2 MPa. The resin adsorption device is equipped with styrene-based macroporous adsorption resin (model LS105), and the residence time of the permeate in the resin bed is about 0.5h. The ion exchange device is e...

Embodiment 2

[0022] PTA refined wastewater enters the rotary extraction tower from the top of the tower, PX enters from the bottom of the tower, the volume ratio of PX to wastewater is 1:8, the extraction temperature is 40°C, the two phases are in countercurrent contact in the extraction tower, and the wastewater stays in the extraction tower The time is 6 minutes. The extract phase is cut out from the top of the tower and sent to the PTA oxidation system as the reaction raw material. The raffinate phase enters the microfiltration membrane separation device through the circulation pump. The membrane material is a sintered stainless steel powder membrane with a pore size of 0.1 μm and an operating pressure of 0.1 MPa. The resin adsorption device is equipped with styrene-based macroporous adsorption resin (model LS100), and the residence time of the permeate in the resin bed is about 0.75h. The ion exchange device is equipped with styrene-based strong acid cation exchange resin (model Amberj...

Embodiment 3

[0024] PTA refined wastewater enters the rotary extraction tower from the top of the tower, PX enters from the bottom of the tower, the volume ratio of PX to wastewater is 1:12, the extraction temperature is 50°C, the two phases are in countercurrent contact in the extraction tower, and the wastewater stays in the extraction tower The time is 4 minutes. The extract phase is cut out from the top of the tower and sent to the PTA oxidation system as the reaction raw material. The raffinate phase enters the microfiltration membrane separation device through the circulating pump. The membrane material is polyethylene hollow fiber membrane with a membrane pore size of 0.1 μm and an operating pressure of 0.4 MPa. The resin adsorption device is equipped with styrene-based anion exchange resin (model D301), and the residence time of the permeate in the resin bed is about 1 hour. The ion exchange device is equipped with styrene-based strongly acidic cation exchange resin (model D001), a...

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Abstract

A combined process for treatment of PTA (pure terephthalic acid) refined waste water comprises the following steps: firstly, aromatic acid in the PAT refined waste water is extracted in an extraction column by using para-xylene into an extract phase, and the extract phase is conveyed to an oxidation unit to serve as a reaction raw material; a raffinate phase is conveyed to a micro-filtration membrane separation device, so that solid suspension particles in the raffinate phase are removed; and a penetrating fluid enters a resin adsorption device and an ion exchange device, so that residual aromatic acid and metal ions in the penetrating fluid are removed, and treated water meets the water standard of a PAT refining unit. According to the method, the water and the aromatic acid therein are recycled, so as to reduce the unit consumption of products and water consumption, and bring remarkable economic benefits.

Description

technical field [0001] The invention belongs to the field of waste water treatment, and in particular relates to a treatment method for terephthalic acid refining waste water. technical background [0002] PTA is one of the important basic organic chemical raw materials, mainly used in the production of polyester fiber, polyester film and so on. The production of PTA generally uses p-xylene as a raw material, acetic acid as a solvent, catalytic oxidation at a certain temperature and pressure to generate crude terephthalic acid (TA), and then refined into high-purity PTA. In the TA hydrorefining process, a large amount of water needs to be used as the dissolving water of TA. After crystallization and centrifugal filtration, a large amount of waste water will be generated. The waste water contains the incompletely reacted intermediate product p-toluic acid (PT acid), P-carboxybenzaldehyde and its product terephthalic acid have the characteristics of high COD, low pH, many imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/04C02F103/36
Inventor 管国锋万辉李钢
Owner NANJING UNIV OF TECH
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