CN112744955A - Integrated device and integrated process for resource utilization of purified terephthalic acid mother solid waste liquid - Google Patents

Integrated device and integrated process for resource utilization of purified terephthalic acid mother solid waste liquid Download PDF

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CN112744955A
CN112744955A CN202110095506.5A CN202110095506A CN112744955A CN 112744955 A CN112744955 A CN 112744955A CN 202110095506 A CN202110095506 A CN 202110095506A CN 112744955 A CN112744955 A CN 112744955A
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waste liquid
terephthalic acid
solid waste
reverse osmosis
silicon carbide
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李光辉
李毓亮
孙德虎
靳建光
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Zhejiang Cathayripe Environmental Engineering Co ltd
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Zhejiang Cathayripe Environmental Engineering Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42—Separation; Purification; Stabilisation; Use of additives
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/42—Treatment of water, waste water, or sewage by ion-exchange
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/02—Temperature
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/06—Controlling or monitoring parameters in water treatment pH
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00—General aspects of water treatment
    • C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals
    • C02F2303/16—Regeneration of sorbents, filters
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A20/00—Water conservation; Efficient water supply; Efficient water use
    • Y02A20/124—Water desalination
    • Y02A20/131—Reverse-osmosis
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Treatment Of Water By Ion Exchange (AREA)

Abstract

The invention discloses a resource utilization integrated device of purified terephthalic acid mother solid waste liquid, which comprises a fixed base, an adsorption tank, a flow guide pipe and a high-temperature-resistant temperature sensor, wherein the top end of the fixed base is fixedly connected with a reverse osmosis mechanism, one side of the fixed base is fixedly connected with a centrifugal machine, the top end of the centrifugal machine is provided with the high-temperature-resistant temperature sensor, and the top end of the high-temperature-resistant temperature sensor is fixedly connected with the adsorption tank. The method comprises the steps of cooling PTA mother solid waste liquid to 40 ℃ through a cooling drainage tube, separating out terephthalic acid into tiny particles, filtering and concentrating by adopting a silicon carbide film, separating out terephthalic acid solid, enabling the silicon carbide film to filter produced water through a diversion tube to enter an adsorption unit, adsorbing dissolved PT acid, enabling thick slurry of the silicon carbide film to enter a centrifuge, enabling effluent to enter an ion exchanger, and separating manganese and cobalt ions through exchange resin; and the produced water after ion exchange enters two stages of reverse osmosis, and is separated by a reverse osmosis membrane to obtain desalted water.

Description

Integrated device and integrated process for resource utilization of purified terephthalic acid mother solid waste liquid
Technical Field
The invention relates to the technical field of resource utilization, in particular to a resource utilization integrated device for mother solid waste liquid of purified terephthalic acid.
Background
The integrated device for recycling the purified terephthalic acid mother solid waste liquid has the advantages that the required desalted water or other substances are obtained from the waste liquid through separation and processing, but the existing integrated device for recycling the purified terephthalic acid mother solid waste liquid has many problems or defects:
firstly, the traditional integrated device for recycling purified terephthalic acid mother solid waste liquid is inconvenient for cooling the PTA mother solid waste liquid to a certain temperature, and the terephthalic acid is separated out into tiny particles, and the separated terephthalic acid solid is separated out, so that the traditional device has insufficient operation rigidness;
secondly, the traditional integrated device for resource utilization of the purified terephthalic acid mother solid waste liquid cannot enable the silicon carbide film to be circulated under the action of a circulating pump at a large flow and a low pressure, and the concentration multiple cannot be controlled by adjusting the proportion of produced water and slurry;
thirdly, the traditional resource utilization integrated device for the mother solid waste liquid of the purified terephthalic acid is inconvenient for carrying out two-stage reverse osmosis on the produced water after ion exchange, and the desalted water cannot be obtained.
Disclosure of Invention
A first technical object of the present invention is to provide an integrated device for recycling purified terephthalic acid mother solid waste liquid, so as to solve the problems in the background art that it is inconvenient to cool PTA (purified terephthalic acid) mother solid waste liquid to a certain temperature, it is not possible to circulate a silicon carbide film at a high flow rate and a low pressure under the action of a circulation pump, and it is inconvenient to perform two-stage reverse osmosis on the produced water after ion exchange.
A second technical objective of the present invention is to provide an integrated process for recycling purified terephthalic acid mother solid waste liquid, so as to solve the problems of inconvenience in cooling PTA (purified terephthalic acid) mother solid waste liquid to a certain temperature, inability to circulate a silicon carbide film at a high flow rate and a low pressure under the action of a circulation pump, and inconvenience in performing two-stage reverse osmosis on the produced water after ion exchange, which are proposed in the background art.
In order to achieve the first technical object, the present invention provides the following technical solutions:
a resource utilization integrated device for purified terephthalic acid mother solid waste liquid comprises a fixed base, an adsorption tank, a flow guide pipe and a high-temperature-resistant temperature sensor, wherein the top end of the fixed base is fixedly connected with a reverse osmosis mechanism, one side of the fixed base is fixedly connected with a centrifugal machine, the top end of the centrifugal machine is provided with the high-temperature-resistant temperature sensor, and the top end of the high-temperature-resistant temperature sensor is fixedly connected with the adsorption tank;
the inside of reverse osmosis mechanism has set gradually circulating pump, transfer line, second grade reverse osmosis unit, one-level reverse osmosis unit and tubular carborundum film, the top through connection of circulating pump has the transfer line, and one side of transfer line has run through tubular carborundum film, through connection between one side of circulating pump and the tubular carborundum film.
The invention creatively adopts the silicon carbide film integrated device to carry out resource utilization of the mother solid waste liquid of the pure terephthalic acid; the special device of the invention endows and strengthens the advantages of silicon carbide film filtration, strengthens the acid resistance and concentration functions of the whole device system, and ensures that the concentrated water enters the water again and becomes more concentrated, thereby facilitating the recovery of phthalic acid particles by a centrifuge; meanwhile, PT acid in an ionic state at a water production end is concentrated and enters water production, and the water production enters an adsorption device to adsorb the PT acid; PT acid concentration means that the pH value is lower and lower, the smaller the pH value is, the more favorable the adsorption is, and the phthalic acid particles at the concentrated water end can be recovered conveniently, so that the resource utilization integrated synergistic effect is formed.
Preferably, one side inside the tubular silicon carbide film is fixedly connected with a second-level reverse osmosis unit, the other side inside the tubular silicon carbide film is fixedly connected with a first-level reverse osmosis unit, and the second-level reverse osmosis unit, the first-level reverse osmosis unit and the tubular silicon carbide film are fixedly connected through clamping blocks.
Preferably, the centrifuge is a table centrifuge, the top end of the table centrifuge is fixedly connected with water guide pipes, the water guide pipes are arranged in two groups and are symmetrically distributed about the central axis of the table centrifuge, and the water guide pipes are spiral hollow pipe bodies.
Preferably, one side of the adsorption tank is fixedly connected with a flow guide pipe, and the reverse osmosis mechanism is in through connection with the adsorption tank through the flow guide pipe; an ion exchanger is arranged between the adsorption tank and the guide pipe.
Preferably, the top fixedly connected with cooling drainage tube of adsorption tanks, and cooling drainage tube is the appearance of "snakelike" distribution, through cooling drainage tube through connection between adsorption tanks and the discharge gate.
Preferably, the silicon carbide film filtering water production end is provided with a heat exchanger connected with a PTA mother solid waste liquid heat energy recovery pipe. The structure can partially utilize the heat energy recovered during PTA cooling, and the heat exchanger heats the produced water at the adsorption end, so that the analysis is more facilitated, and the recovery of phthalic acid particles at the concentrated water end is facilitated.
In order to achieve the second technical object, the present invention provides the following technical solutions:
the integrated process for recycling the purified terephthalic acid mother solid waste liquid is completed by adopting the integrated device for recycling the purified terephthalic acid mother solid waste liquid, and comprises the following specific processes:
(1) cooling the PTA mother solid waste liquid to 35-45 ℃, separating out terephthalic acid into tiny particles, filtering and concentrating by adopting a silicon carbide film, and separating out terephthalic acid solid;
(2) the water produced by filtering the silicon carbide film enters an adsorption unit to adsorb the dissolved PT acid;
(3) the water after adsorption enters an ion exchanger, and manganese and cobalt ions are adsorbed and separated by exchange resin;
(4) and the produced water after ion exchange enters two stages of reverse osmosis, and the final produced water is desalted water after separation of a reverse osmosis membrane.
The invention creatively adopts the silicon carbide film integrated device to carry out resource utilization of the mother solid waste liquid of the pure terephthalic acid; the specific device and the process of the invention endow and strengthen the advantages of silicon carbide film filtration, strengthen the acid resistance and the concentration function of the whole device system, make the concentrated water enter the water again, make the concentrated water more concentrated, facilitate the recovery of phthalic acid particles by the centrifuge; meanwhile, PT acid in an ionic state at a water production end is concentrated and enters water production, and the water production enters an adsorption device to adsorb the PT acid; PT acid concentration means that the pH value is lower and lower, the smaller the pH value is, the more favorable the adsorption is, and the convenience is brought to the recovery of phthalic acid particles at the concentrated water end; thereby forming the combined advantageous effect of low-temperature cooling process of PTA mother solid waste liquid and continuous cycle treatment to lower and lower the pH value of the pure terephthalic acid mother solid waste liquid, being more beneficial to recycling phthalic acid particles, and forming the synergistic effect of resource utilization integration.
Preferably, the particle size of the particles in the PTA solid waste liquid in the step (1) is mainly distributed in a micron grade of 0.8-1.8 μm, and the components are undissolved terephthalic acid, and the content is 0.3-0.8 wt%.
Preferably, the particle size of the particles in the PTA solid waste liquid in the step (1) is mainly distributed in a micron grade of 0.8-1.8 μm, and the components are undissolved terephthalic acid, and the content is 0.5 wt%.
Preferably, the aperture of the silicon carbide film is 0.08-0.12 micron, and the flow channel of the silicon carbide film is 5-7 mm.
The silicon carbide film is formed by high-temperature sintering by adopting a recrystallization technology, a flow passage is formed by a porous supporting layer, a transition layer and a microporous layer, the cross section of the flow passage is asymmetrically distributed, the flow passage is a circular hole passage with the diameter of 5-7mm, the aperture is large, smooth and not easy to pollute. The PTA mother liquor carrying particulate matters flows in a flow channel in a cross mode at a high speed, so that the pollution and blockage to membrane pores are reduced.
Preferably, the aperture of the silicon carbide film is 0.1 micron, and the flow channel of the silicon carbide film is 6 mm.
The flow channel is a silicon carbide film round hole channel with the diameter of 6mm, the aperture is large and smooth, and pollution is not easy to occur; the PTA mother liquor carrying particulate matters flows in the flow channel in a cross way at a high speed, which is more favorable for reducing the pollution and blockage to membrane pores.
Compared with the prior art, the invention has the beneficial effects that: this solid waste liquid's of pure terephthalic acid mother resource utilization integrated device has not only realized being convenient for to cool to the uniform temperature with the solid waste liquid of PTA mother, has realized to have made the carborundum film carry out the circulation of large-traffic low pressure under the circulating pump effect, has realized being convenient for to carry out the two-stage reverse osmosis to the product water after the ion exchange moreover:
(1) cooling the PTA mother solid waste liquid to 35-45 ℃ through a cooling drainage tube, separating out tiny particles from terephthalic acid, filtering, concentrating and reprocessing the tiny particles by adopting a silicon carbide film again, and separating out a terephthalic acid solid raw material so as to facilitate reprocessing in the later period;
(2) the silicon carbide film is filtered through a guide pipe to produce water, the water enters an adsorption unit to adsorb dissolved PT acid, the thick slurry of the silicon carbide film enters a desk centrifuge, manganese and cobalt ions are adsorbed and separated through exchange resin, the silicon carbide film can be subjected to high-flow low-pressure circulation under the action of a circulating pump, and the concentration multiple can be controlled by adjusting the proportion of the produced water and the slurry;
(3) the water produced after ion exchange enters two-stage reverse osmosis through a second-stage reverse osmosis unit and a first-stage reverse osmosis unit, and the final water produced is desalted water after reverse osmosis membrane separation;
(4) the invention creatively adopts the silicon carbide film integrated device to carry out resource utilization of the mother solid waste liquid of the pure terephthalic acid; the specific device and the process of the invention endow and strengthen the advantages of silicon carbide film filtration, strengthen the acid resistance and the concentration function of the whole device system, make the concentrated water enter the water again, make the concentrated water more concentrated, facilitate the recovery of phthalic acid particles by the centrifuge; meanwhile, PT acid in an ionic state is concentrated and enters a water production end to produce water, and the produced water enters an adsorption device to adsorb the PT acid; PT acid concentration means that the pH value is lower and lower, the smaller the pH value is, the more favorable the adsorption is, and the convenience is brought to the recovery of phthalic acid particles at the concentrated water end; thereby forming the combined advantageous effect of low-temperature cooling process of PTA mother solid waste liquid and continuous cycle treatment to lower and lower the pH value of the pure terephthalic acid mother solid waste liquid, being more beneficial to recycling phthalic acid particles, and forming the synergistic effect of resource utilization integration.
Drawings
FIG. 1 is a schematic front sectional view of the present invention;
FIG. 2 is a partially enlarged schematic view of a reverse osmosis mechanism of the present invention;
fig. 3 is an enlarged schematic view of a portion a in fig. 1 according to the present invention.
In the figure: 1. a fixed base; 2. a reverse osmosis mechanism; 201. a circulation pump; 202. a transfusion tube; 203. a secondary reverse osmosis unit; 204. a first-stage reverse osmosis unit; 205. a tubular silicon carbide film; 3. cooling the drainage tube; 4. an adsorption tank; 5. a flow guide pipe; 6. a temperature sensor; 7. a water conduit; 8. a centrifugal machine.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The resource utilization integrated process of the purified terephthalic acid mother solid waste liquid is completed by adopting a resource utilization integrated device of the purified terephthalic acid mother solid waste liquid, and the specific process is as follows:
(1) cooling the PTA mother solid waste liquid to 45 ℃, separating out terephthalic acid into tiny particles, filtering and concentrating by adopting a silicon carbide film, and separating out terephthalic acid solid; wherein, the particle size of the particles in the PTA mother solid waste liquid is mainly distributed in the micron level of 1.8 μm, the component is undissolved terephthalic acid, and the content is 0.8 wt%;
(2) the water produced by filtering the silicon carbide film enters an adsorption unit to adsorb the dissolved PT acid; wherein the aperture of the silicon carbide film is 0.12 micron, and the flow channel of the silicon carbide film is 7 mm;
(3) the water after adsorption enters an ion exchanger, and manganese and cobalt ions are adsorbed and separated by exchange resin;
(4) and the produced water after ion exchange enters two stages of reverse osmosis, and the final produced water is desalted water after separation of a reverse osmosis membrane.
Referring to fig. 1-3, the device for recycling purified terephthalic acid mother solid waste liquid comprises a fixed base 1, an adsorption tank 4, a flow guide pipe 5 and a high temperature resistant temperature sensor 6, wherein the top end of the fixed base 1 is fixedly connected with a reverse osmosis mechanism 2;
the reverse osmosis mechanism 2 is internally provided with a circulating pump 201, an infusion tube 202, a secondary reverse osmosis unit 203, a primary reverse osmosis unit 204 and a tubular silicon carbide film 205 in sequence, the top end of the circulating pump 201 is connected with the infusion tube 202 in a penetrating manner, one side of the infusion tube 202 is provided with the tubular silicon carbide film 205 in a penetrating manner, one side of the circulating pump 201 is connected with the tubular silicon carbide film 205 in a penetrating manner, one side of the inside of the tubular silicon carbide film 205 is fixedly connected with the secondary reverse osmosis unit 203, the other side of the inside of the tubular silicon carbide film 205 is fixedly connected with the primary reverse osmosis unit 204, and the secondary reverse osmosis unit 203, the primary reverse;
specifically, as shown in fig. 1 and 2, when the mechanism is used, firstly, the water produced after ion exchange enters two-stage reverse osmosis through a second-stage reverse osmosis unit 203 and a first-stage reverse osmosis unit 204, and the water produced finally is the desalted water after separation through a reverse osmosis membrane;
one side of the fixed base 1 is fixedly connected with a centrifugal machine 8, the type of the centrifugal machine 8 can be JIDI-20D, the top end of the centrifugal machine 8 is fixedly connected with a water guide pipe 7, the water guide pipe 7 is provided with two groups and is symmetrically distributed about the central axis of the centrifugal machine 8, the water guide pipe 7 is a spiral hollowed pipe body, one side of the adsorption tank 4 is fixedly connected with a flow guide pipe 5, and the reverse osmosis mechanism 2 is in through connection with the adsorption tank 4 through the flow guide pipe 5;
specifically, as shown in fig. 1, when the mechanism is used, firstly, the silicon carbide membrane filtration produced water enters an adsorption unit through a draft tube 5 to adsorb dissolved PT acid, the concentrated slurry of the silicon carbide membrane after adsorption enters a centrifuge 8, manganese cobalt ions are adsorbed and separated through exchange resin, so that the silicon carbide membrane can be circulated at a large flow and a low pressure under the action of a circulating pump 201, and the concentration multiple can be controlled by adjusting the proportion of the produced water and the slurry;
a high-temperature-resistant temperature sensor 6 is arranged at the top end of the centrifuge 8, an adsorption tank 4 is fixedly connected to the top end of the high-temperature-resistant temperature sensor 6, the type of the high-temperature-resistant temperature sensor 6 can be PT100, a cooling drainage tube 3 is fixedly connected to the top end of the adsorption tank 4, the cooling drainage tube 3 is in a shape of snake-shaped distribution, and the adsorption tank 4 is in through connection with a discharge port through the cooling drainage tube 3;
specifically, as shown in fig. 1 and 3, when the mechanism is used, firstly, the PTA-purified terephthalic acid mother solid waste liquid is cooled to 40 ℃ through the cooling drainage tube 3, the precipitated fine particles of terephthalic acid are filtered and concentrated by adopting a silicon carbide film, and the precipitated terephthalic acid solid raw material is separated, so that the later-stage re-processing is facilitated.
The working principle is as follows: when the device is used, mother solid waste liquid discharged from a refining working section is cooled by the cooling drainage tube 3, the temperature is conveniently measured by the high-temperature resistant temperature sensor 6, the pH value of the mother solid liquid is adjusted to 3-4, and the terephthalic acid is fully acidified; pumping mother solid liquid after acid precipitation into the tubular silicon carbide film 205, circulating the tubular silicon carbide film 205 at a large flow rate and a low pressure under the action of the circulating pump 201, wherein the flow rate of the film surface reaches 3-4m/s, the part penetrating through the film forms water production, and the retained part forms slurry. Controlling the concentration multiple by adjusting the proportion of the produced water and the slurry; returning the slurry to the refining process, and centrifugally separating the slurry by a centrifuge 8 to obtain a terephthalic acid solid; and (3) delivering produced water to an adsorption tank 4, adsorbing the dissolved PT acid and residual TA in the water, and desorbing by using a desorption agent after the adsorption is saturated. Obtaining the PT acid liquid with high concentration, and returning to the PTA oxidation process section. The water produced after adsorption is sent to an ion exchanger for manganese cobalt ion adsorption, and when the exchange resin is saturated, manganese cobalt is desorbed through regenerated liquid to obtain a manganese cobalt solution with high concentration; and after further treatment, the water is recycled to the oxidation process section, the water produced after ion exchange is pumped into the first-stage reverse osmosis unit 204 for primary membrane separation, the obtained water enters the second-stage reverse osmosis unit 203 for secondary membrane separation, and the water produced by the second-stage reverse osmosis unit 203 is high-quality desalted water and can be recycled to the refining process section. The concentrated water of the second-stage reverse osmosis is used as the inlet water of the first-stage reverse osmosis before returning to the first-stage reverse osmosis, so as to improve the recovery rate of the desalted water. The concentrated water of the first-stage reverse osmosis is subjected to standard discharge treatment or zero discharge treatment.
Through detection, the recovery rate of phthalic acid particles is 95-96wt%, the recovery rate of PT at the adsorption end is 99.68-99.88wt%, and the recovery rate of manganese cobalt ions in the mother solid waste liquid is 97.5-98.5 wt%.
Example 2
The integrated process for recycling the solid waste liquid of the purified terephthalic acid mother liquor is completed by adopting the integrated device for recycling the solid waste liquid of the purified terephthalic acid mother liquor in the same embodiment 1, and the specific process is as follows:
(1) cooling the PTA mother solid waste liquid to 35 ℃, separating out terephthalic acid into tiny particles, filtering and concentrating by adopting a silicon carbide film, and separating out terephthalic acid solid; wherein, the particle size of the particles in the PTA mother solid waste liquid is mainly distributed in the micron level of 0.8 μm, the component is undissolved terephthalic acid, and the content is 0.3 wt%;
(2) the water produced by filtering the silicon carbide film enters an adsorption unit to adsorb the dissolved PT acid; wherein the aperture of the silicon carbide film is 0.08 micron, and the flow channel of the silicon carbide film is 5 mm;
(3) the water after adsorption enters an ion exchanger, and manganese and cobalt ions are adsorbed and separated by exchange resin;
(4) and the produced water after ion exchange enters two stages of reverse osmosis, and the final produced water is desalted water after separation of a reverse osmosis membrane.
Through detection, the recovery rate of phthalic acid particles is 96-97wt%, the recovery rate of PT at the adsorption end is 99.89-99.95wt%, and the recovery rate of manganese cobalt ions in the mother solid waste liquid is 97.9-98.9 wt%.
Example 3
The integrated process for recycling the solid waste liquid of the purified terephthalic acid mother liquor is completed by adopting the integrated device for recycling the solid waste liquid of the purified terephthalic acid mother liquor in the same embodiment 1, and the specific process is as follows:
(1) cooling the PTA mother solid waste liquid to 40 ℃, separating out terephthalic acid into tiny particles, filtering and concentrating by adopting a silicon carbide film, and separating out terephthalic acid solid; wherein, the particle size of the particles in the PTA mother solid waste liquid is mainly distributed in the micron level of 0.1 μm, the component is undissolved terephthalic acid, and the content is 0.5 wt%;
(2) the water produced by filtering the silicon carbide film enters an adsorption unit to adsorb the dissolved PT acid; wherein the aperture of the silicon carbide film is 0.1 micron, and the flow channel of the silicon carbide film is 6 mm;
(3) the water after adsorption enters an ion exchanger, and manganese and cobalt ions are adsorbed and separated by exchange resin;
(4) and the produced water after ion exchange enters two stages of reverse osmosis, and the final produced water is desalted water after separation of a reverse osmosis membrane.
Through detection, the recovery rate of phthalic acid particles is 95-97wt%, the recovery rate of PT at the adsorption end is 99.91-99.93wt%, and the recovery rate of manganese cobalt ions in the mother solid waste liquid is 98.8-99.3 wt%.
Example 4
The same as example 1, except that the membrane filtration cycle times are doubled, the recovery rate of phthalic acid particles is 97-99wt%, the recovery rate of PT at the adsorption end is 99.95-99.98wt%, and the recovery rate of manganese cobalt ions in the mother solid waste liquid is 99.4-99.5 wt%.
Example 5
The same as example 2, except that the membrane filtration cycle times are doubled, the recovery rate of phthalic acid particles is 98-99wt%, the recovery rate of PT at the adsorption end is 99.97-99.99wt%, and the recovery rate of manganese cobalt ions in the mother solid waste liquid is 99.5-99.7 wt%.
Example 6
The same as example 3, except that the membrane filtration cycle times were doubled, the recovery rate of phthalic acid particles was 97 to 99wt%, the recovery rate of PT at the adsorption end was 99.97 to 99.99wt%, and the recovery rate of manganese cobalt ions in the mother solid waste liquid was 99.8 to 99.9 wt%.
Comparative example 1
The same as example 1, except that the apparatus for treating the mother solid waste liquid of purified terephthalic acid was a prior art apparatus.
Detection shows that the recovery rate of each effective component in the mother solid waste liquid is 80-85 wt%.
Comparative example 2
The difference from the example 2 is that the apparatus for treating the mother solid waste liquid of purified terephthalic acid adopts the apparatus of the prior art.
Detection shows that the recovery rate of each effective component in the mother solid waste liquid is 81-86 wt%.
Comparative example 3
The same as example 3, except that the apparatus for treating the mother solid waste liquid of purified terephthalic acid was a prior art apparatus.
Detection shows that the recovery rate of each effective component in the mother solid waste liquid is 83-88 wt%.
Comparative example 4
The same as example 3, except that the PTA mother solid waste liquid was cooled to 40 ℃ in the step (1).
Detection shows that the recovery rate of each effective component in the mother solid waste liquid is 85-90 wt%.
Comparative example 5
The same as example 3, except that the step (2) was carried out by filtration and concentration using a silicon carbide film having a pore size of 0.12 μm.
Detection shows that the recovery rate of each effective component in the mother solid waste liquid is 84-89 wt%.
Examples and comparative examples data illustrate that:
1. the integrated device for recycling the purified terephthalic acid mother solid waste liquid not only realizes that the PTA mother solid waste liquid is cooled to a certain temperature conveniently, realizes that a silicon carbide film can perform large-flow low-pressure circulation under the action of a circulating pump, but also realizes that two-stage reverse osmosis can be performed on the produced water after ion exchange conveniently;
2. cooling the PTA mother solid waste liquid to 40 ℃ through a cooling drainage tube, separating out tiny particles from terephthalic acid, filtering, concentrating and reprocessing the tiny particles by adopting a silicon carbide film again, and separating out a terephthalic acid solid raw material so as to facilitate reprocessing in the later period;
3. according to the invention, the wide-flow-channel and high-precision silicon carbide film is introduced to filter and concentrate solid particles in PTA (pure terephthalic acid) mother solid-liquid waste liquid, the ceramic film has a pore size of 0.1 micron, can intercept more than 99% of particles in mother solid-liquid waste liquid, and can concentrate the particles into slurry with a solid content of 10%, and meanwhile, no particle residue exists in filtered produced water, so that subsequent adsorption, ion exchange and reverse osmosis units are prevented from being blocked by particles; the pollution is reduced by a ceramic membrane with a 6mm wide flow channel, and the stable flux can still be maintained after the mother solid is concentrated by 20 times;
4. the cooling temperature control and the silicon carbide film aperture control of the PTA mother solid waste liquid have great influence on the recovery rate of each effective component in the mother solid waste liquid and have great influence on the water production performance after filtration;
5. the recovery rate of the obtained phthalic acid particles and the recovery rate of PT at the adsorption end are higher according to the cycle times of different membrane processes, and the recovery rates of the two products are higher along with the increase of the cycle and the higher the concentration rate. The specific device and the process of the invention endow and strengthen the advantages of silicon carbide film filtration, strengthen the acid resistance and the concentration function of the whole device system, make the concentrated water enter the water again, make the concentrated water more concentrated, facilitate the recovery of phthalic acid particles by the centrifuge; meanwhile, PT acid in an ionic state is concentrated and enters a water production end to produce water, and the produced water enters an adsorption device to adsorb the PT acid; PT acid concentration means that the pH value is lower and lower, the smaller the pH value is, the more favorable the adsorption is, and the convenience is brought to the recovery of phthalic acid particles at the concentrated water end; thereby forming the combined advantageous effect of low-temperature cooling process of PTA mother solid waste liquid and continuous cycle treatment to lower and lower the pH value of the pure terephthalic acid mother solid waste liquid, being more beneficial to recycling phthalic acid particles, and forming the synergistic effect of resource utilization integration.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (10)

1. The utility model provides a utilization integrated device of fine terephthalic acid mother solid waste liquid which characterized in that: the device comprises a fixed base (1), an adsorption tank (4), a flow guide pipe (5) and a high-temperature-resistant temperature sensor (6), wherein the top end of the fixed base (1) is fixedly connected with a reverse osmosis mechanism (2), one side of the fixed base (1) is fixedly connected with a centrifugal machine (8), the top end of the centrifugal machine (8) is provided with the high-temperature-resistant temperature sensor (6), and the top end of the high-temperature-resistant temperature sensor (6) is fixedly connected with the adsorption tank (4);
the inside of reverse osmosis mechanism (2) has set gradually circulating pump (201), transfer line (202), second grade reverse osmosis unit (203), one-level reverse osmosis unit (204) and tubular carborundum membrane (205), the top through connection of circulating pump (201) has transfer line (202), and one side of transfer line (202) runs through tubular carborundum membrane (205), through connection between one side of circulating pump (201) and tubular carborundum membrane (205).
2. The resource utilization integrated device for the mother solid waste liquid of the purified terephthalic acid as claimed in claim 1, is characterized in that: inside one side fixedly connected with second grade reverse osmosis unit (203) of tubular carborundum membrane (205), the inside opposite side fixedly connected with one-level reverse osmosis unit (204) of tubular carborundum membrane (205), pass through fixture block fixed connection between second grade reverse osmosis unit (203), one-level reverse osmosis unit (204) and tubular carborundum membrane (205).
3. The resource utilization integrated device for the mother solid waste liquid of the purified terephthalic acid according to claim 2 is characterized in that: centrifuge (8) are desk centrifuge, desk centrifuge's top fixedly connected with aqueduct (7), and aqueduct (7) are provided with two sets ofly and about desk centrifuge (8) axis symmetric distribution, aqueduct (7) are "spiral" fretwork form body.
4. The resource utilization integrated device for the mother solid waste liquid of the purified terephthalic acid according to claim 3 is characterized in that: a flow guide pipe (5) is fixedly connected to one side of the adsorption tank (4), and the reverse osmosis mechanism (2) is in through connection with the adsorption tank (4) through the flow guide pipe (5); an ion exchanger is arranged between the adsorption tank (4) and the draft tube (5).
5. The resource utilization integrated device for the mother solid waste liquid of purified terephthalic acid according to claim 4, characterized in that: the top fixedly connected with cooling drainage tube (3) of adsorption tank (4), and cooling drainage tube (3) are the appearance of "snakelike" distribution, through cooling drainage tube (3) through connection between adsorption tank (4) and the discharge gate.
6. The resource utilization integrated device for the mother solid waste liquid of purified terephthalic acid according to claim 5, characterized in that: and the water filtering and producing end of the silicon carbide film (205) is provided with a heat exchanger connected with a PTA mother solid waste liquid heat energy recovery pipe.
7. A process for recycling and integrating solid waste liquid of purified terephthalic acid mother liquor, which is completed by adopting the integrated device for recycling and integrating the solid waste liquid of purified terephthalic acid mother liquor, which is disclosed by any one of claims 1 to 6, and is characterized by comprising the following steps:
cooling the PTA mother solid waste liquid to 35-45 ℃, separating out terephthalic acid into tiny particles, filtering and concentrating by adopting a silicon carbide film, and separating out terephthalic acid solid;
the water produced by filtering the silicon carbide film enters an adsorption unit to adsorb the dissolved PT acid;
the water after adsorption enters an ion exchanger, and manganese and cobalt ions are adsorbed and separated by exchange resin;
and the produced water after ion exchange enters two stages of reverse osmosis, and the final produced water is desalted water after separation of a reverse osmosis membrane.
8. The resource utilization integrated process of the mother solid waste liquid of the purified terephthalic acid according to claim 7 is characterized in that: the particle size of the particles in the PTA mother solid waste liquid in the step (1) is mainly distributed in a micron grade of 0.8-1.8 mu m, and the component is undissolved terephthalic acid with the content of 0.3-0.8 wt%.
9. The resource utilization integrated process of the purified terephthalic acid mother solid waste liquid according to claim 7 or 8, which is characterized in that: the aperture of the silicon carbide film is 0.08-0.12 micron, and the flow channel of the silicon carbide film is 5-7 mm.
10. The resource utilization integrated process of the mother solid waste liquid of the purified terephthalic acid according to claim 9, which is characterized in that: the aperture of the silicon carbide film is 0.1 micron, and the flow channel of the silicon carbide film is 6 mm.
CN202110095506.5A 2021-01-25 2021-01-25 Integrated device and integrated process for resource utilization of purified terephthalic acid mother solid waste liquid Pending CN112744955A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113731189A (en) * 2021-10-15 2021-12-03 山东华恩新材料科技有限公司 Silicon carbide ceramic filter membrane group for industrial cutting fluid regeneration

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113731189A (en) * 2021-10-15 2021-12-03 山东华恩新材料科技有限公司 Silicon carbide ceramic filter membrane group for industrial cutting fluid regeneration

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