CN101254985B - PTA refined mother liquor reclaiming method and system - Google Patents
PTA refined mother liquor reclaiming method and system Download PDFInfo
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- CN101254985B CN101254985B CN 200810103270 CN200810103270A CN101254985B CN 101254985 B CN101254985 B CN 101254985B CN 200810103270 CN200810103270 CN 200810103270 CN 200810103270 A CN200810103270 A CN 200810103270A CN 101254985 B CN101254985 B CN 101254985B
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Abstract
The invention relates to a PTA device refined mother liquor recovery method and a PTA device refined mother liquor recovery system. The method comprises the steps that refined mother liquor is cooled through a heat exchange method and is processed through an ultrafiltration method, ultrafiltration concentrated liquor is delivered to an ultrafiltration concentrated tank and is delivered to an ion exchange system, Co and Mn ion which can be used as a catalyzer and Fe, Ni , Na and other meallic ion are respectively removed from the liquor, and Co ion elutriant and Mn ion elutriant which can be used as the catalyzer are recycled, the liquor after being treated by ion exchange in a liquor pot is partially returned to a refined system to be used, and part of the liquor after being heated is delivered to a reverse osmosis system to perform the reverse osmosis treatment, reverse osmosis concentrated liquor is mixed into the refined mother liquor which is not treated by ultrafiltration to be treated again, and the reverse osmosis filtered liquor can be used as reuse water. The system is composed of the heat exchange system, the ultrafiltration system, the iron exchange system and the reverse osmosis system. The invention effectively recovers and utilizes the effective content in the refined mother liquor and reduces the pollution, and can be matched with the PTA device.
Description
Technical field
The present invention relates to a kind of PTA device of refining mother liquor reclaiming method, also relate to a kind of PTA device of refining mother liquor recovery system that adopts this method, belong to chemical industry and environmental technology field.
Background technology
The refined unit of PTA (pure terephthalic acid) device is to be solvent with water, and crude terephthalic acid (CTA) is entered the refining reaction device after the making beating heating for dissolving, in the presence of catalyzer, with hydrogen (H
2) make that major impurity is reduced into water-soluble p-methylbenzoic acid (p-TA) to carboxyl benzaldehyde (4-CBA) in the slurry, again by crystallization, filtration or technological processs such as centrifugation, drying, make product pure terephthalic acid (PTA).In TA filtration or centrifugal separation processes, isolate a large amount of aqueous solution (refinement mother liquor), contain TA, p-TA, HAC and little amount of catalyst (cat), 4-CBA and other metal ion in this solution, refinement mother liquor in traditional PTA device is directly to enter the sewage-farm, wherein useful component and water is not reclaimed, cause material consumption, the energy consumption height of device thus, and bring difficulty to sewage disposal.
Along with social development, people's environmental consciousness strengthens, and enterprise presses for and reduces material consumption, minimizing energy consumption for reducing cost, improve product competitiveness simultaneously.In recent years, the PTA device is mostly set up the refinement mother liquor recvery facility, adopts various filters that TA, p-TA in the mother liquor are recycled, and makes the product material consumption reduce, alleviate treatment pressure of sewage.Though these recvery facilities all have certain actual effect, incomplete to the recovery of useful component, device still has the large amount of sewage that contains more TA, p-TA and other impurity to efflux, and environment is polluted.
Summary of the invention
For overcoming the above-mentioned defective of prior art, the invention provides a kind of PTA device of refining mother liquor reclaiming method and a kind of PTA device of refining mother liquor recovery system, so that reclaim and utilize various useful components and heat energy in the refinement mother liquor effectively, reduce the quantity discharged of pollutent, reduce the PTA production cost.
The present invention realizes that the technical scheme of above-mentioned purpose is:
A kind of PTA device of refining mother liquor reclaiming method comprises the following steps:
(1) adopt heat change method that refinement mother liquor is lowered the temperature;
(2) the employing hyperfiltration process is handled the refinement mother liquor after lowering the temperature, and the ultrafiltration and concentration liquid that obtains after the ultrafiltration is sent in the ultrafiltration and concentration flow container, recycles in order to sending into occasions such as oxidation unit;
(3) the ultrafiltration filtrate that obtains after the ultrafiltration is sent into ion exchange system, remove Co, Mn ion and the metal ions such as Fe, Ni, Na of useful as catalysts in the liquid respectively by ion-exchange techniques, wherein contain Co, Mn ionic elutriant is sent in the catalyzer flow container, recycle in order to sending into occasion such as oxidation unit; The elutriant that contains metal ions such as Fe, Ni, Na effluxes, and can send into the sewage-farm and handle; Exchange back liquid is sent into from handing over the back liquid tank;
(4) will be from handing over using in the liquid tank of back from handing over the back liquid portion to return refining system, part is carried out reverse-osmosis treated through sending into reverse osmosis system after heating, the reverse osmosis concentrated liquid that obtains is sneaked into without the refinement mother liquor of uf processing and is handled again, the reverse osmosis filtrate that obtains is sent into the reuse water pot, is used in order to sending into occasions such as refined unit.
In the described step (1), by placed in-line first interchanger and second interchanger carry out twice heat exchange cooling successively, wherein first interchanger can adopt step (4) to need the liquid after handing over of heating, the heat energy that utilizes refinement mother liquor will be to entering these liquid heat of reverse osmosis system, control is 72～77 ℃ from the temperature of the refinement mother liquor that first interchanger comes out, the temperature of the refinement mother liquor that comes out from second interchanger is 40～45 ℃, and the temperature from handing over back liquid of coming out from first interchanger is 70～75 ℃.
The preferred precision of filter material of used ultrafiltration system can reach the coated TiO of sintering metal of 50～100 nanometers in the described step (2)
2Film, filter type adopt cross-flow to concentrate, and the concentrated solution solid content is 15-20%.
The ion exchange system of described step (3) by the Co that sets gradually, Mn from presentate unit and Fe, Ni, Na from presentate unit, can be used as Co, Mn ion and the metal cations Fe of catalyzer, the ion-exchange of Ni, Na etc. successively, and carry out regeneration of ion-exchange resin by acid washing method, and obtain corresponding ionic elutriant, wherein Co, Mn adopt HBr to carry out pickling from presentate unit, and Fe, Ni, Na adopt HCl to carry out pickling from presentate unit.
In step (4), the reverse osmosis precision is controlled at 0.5～1nm scope, only allows small molecules H basically
2O passes through, the HAC of larger molecular weight, TA, p-TA and metal ion etc. are held back the formation concentrated solution by reverse osmosis membrane, account for 1/3 liquid measure, the filtrate of reverse osmosis is about 2/3 liquid measure, meet the quality of reused water requirement, according to PTA quality product and systematic water balance requirement, concentrated solution also can be discharged on a small quantity, enters the sewage-farm.
A kind of PTA device of refining mother liquor recovery system, comprise heat-exchange system, ultrafiltration system, ion exchange system and reverse osmosis system, the heat release medium import of described heat-exchange system is the refinement mother liquor import, outlet connects the import of ultrafiltration system, the filtrate outlet of described ultrafiltration system connects the import of described ion exchange system, and the liquid outlet connects described reverse osmosis system import after the exchange of described ion exchange system.
Described heat-exchange system comprises first interchanger and second interchanger at least, between the outlet of the heat-absorbing medium passage of described first interchanger serial connection ion exchange system on the pipeline.
Described second interchanger is connected on the back of described first interchanger, and its heat-absorbing medium passage connects cooling water pipeline.
The preferred cross-flow of described ultrafiltration system concentrates structure, the coated TiO of the preferred sintering metal of used filter material
2The membrane structure filter material.
The ultrafiltration and concentration liquid outlet of described ultrafiltration system connects the import of ultrafiltration and concentration flow container, has agitator in the described ultrafiltration and concentration flow container, and its outlet is provided with ultrafiltration and concentration liquid and sends pump, and described ultrafiltration and concentration liquid is sent the pump discharge pipeline can insert oxidation system.
(1) described ultrafiltration system filtrate outlet leaches flow container and ion-exchange fresh feed pump with being provided with successively on the connecting tube of described ion exchange system import, the inlet pipeline of described ion exchange system is provided with the ion-exchange feed heater, described ion-exchange feed heater preferred lower pressure steam heater.
The preferred continuous ionic exchange system of described ion exchange system, comprise the Co, the Mn that set gradually from presentate unit and Fe, Ni, Na from presentate unit, described Co, Mn are from handing over unitary Co, the outlet of Mn desorbed solution to enter catalyst tank, the outlet of described catalyst tank is sent pump by catalyzer and is inserted oxidation system, and described Fe, Ni, Na are from handing over unitary Fe, Ni, the outlet of Na desorbed solution to insert the sewage-farm by pipeline.
On exporting with the connecting tube of described reverse osmosis system import, the liquid after handing over of described ion exchange system is provided with successively from handing over the back flow container and transferpump after handing over, the described heat-absorbing medium import that connects described first interchanger from the outlet conduit of handing over the back transferpump, on the connecting tube of handing over back transferpump outlet and the described first interchanger heat-absorbing medium import, also be provided with one from handing over back liquid branch road described, should be from handing over back liquid branch road to be connected in refining system.
Described reverse osmosis system concentrated solution outlet is connected with two reverse osmosis concentrated liquid output channels, one of them reverse osmosis concentrated liquid output channel inserts the sewage-farm, and another reverse osmosis concentrated liquid output channel inserts the connecting tube between the described first interchanger heat release media outlet and the second interchanger heat release medium import.
Described reverse osmosis system is provided with the film cleaning system.
Described ion exchange system is provided with regeneration such as the rinsing that is used for regenerated HBr input channel and HCl input channel liquid input tube road.
The invention has the beneficial effects as follows:
(1) realized the recycling of TA, P-TA, Co, Mn, water and heat energy in the refinement mother liquor, wherein the recovery utilization rate of TA, P-TA can reach 70-80%, the recovery utilization rate of Co, Mn can reach about 90%, the recovery utilization rate of water can reach about 70-80%, and the required heating heat energy of native system is all provided by the used heat of system's refinement mother liquor;
(2) reduced pollutant discharge amount significantly;
(3) economic benefit is obvious, and system's payback period is reduced to about 1.5 by about 3.5 years under the prior art;
(4) technical process is reasonable, helps reducing facility investment, handled easily and maintenance;
(5) with existing PTA system support, the various materials of recovery can be sent into the PTA system basically and be used, and not only help simplifying this body structure of PTA system thus, reduce investment and occupation of land, but also have guaranteed effective utilization of native system recovered material.
Description of drawings
Fig. 1 is a process principle figure of the present invention;
Fig. 2 is system architecture of the present invention and process flow diagram.
Embodiment
Referring to Fig. 1 and Fig. 2, concrete enforcement of the present invention can be given unnecessary details no longer one by one according to technique scheme.Only as follows with regard to characteristics of the present invention and main contents combined process process explanation:
1, technical characterstic:
PTA device of refining mother liquor major impurity is: TA 0.5～1%, p-TA～0.2%, small amount of H AC and 4CBA, Cat and other metal ion.The conventional processes of PTA device of refining mother liquor is earlier mother liquor to be cooled to about 50 ℃ at present, dissolved TA in the mother liquor, p-TA crystallization are separated out, form trickle solid particulate, then by various filters (for example candle wick formula, vane-type, sintered metal tube etc.), adopt intermittently vertical filter type, TA, p-TA is partially recycled.The filtering accuracy of filter screen mostly is micron (μ m) level, adopts the filtering accuracy of sintering metal can reach 0.2～0.5 μ m.This type of filter type solid recovery rate is lower, and operation is also relatively more difficult, only filter cake (TA, p-TA) is recycled, and filtrate still all enters the sewage-farm, and the environmental improvement effect is still relatively poor.
The treatment process that this patent is new is to adopt ultra-filtration technique to reclaim TA, p-TA fine particle, and filter material is the coated TiO of sintering metal
2Film, precision can reach 50～100 nanometers (nm), and filter type is that cross-flow concentrates, and the rate of recovery is higher, concentrated solution solid content 15-20%, but direct reuse is in production system; Operate also relatively easy.To the ultrafiltration rear filtrate, adopt ion exchange resin that catalyst cobalt in the filtrate (CO), manganese (Mn) are selected absorption earlier, take off suction with the HBr aqueous solution then, take off imbibition (Cat) and return the production system use.Remove filtrate behind Co, the Mn metal, again through the primary ions resin absorption, remove other metal ion (Fe, Ni, Na etc.), then the direct retrieval system of～1/3 liquid measure is used, other 2/3 liquid measure enters reverse osmosis (RO) system.The reverse osmosis precision only allows small molecules H basically in 0.5～1nm scope
2O passes through, and HAC, TA, p-TA and the metal ion etc. of larger molecular weight are held back the formation dope by reverse osmosis membrane.The reverse osmosis water of about 2/3 liquid measure directly returns production system and uses; About 1/3 liquid measure hold back concentrated solution, major ingredient is TA and p-TA (5000-8000PPM), returns the refinement mother liquor charging, once more through cooling, crystallization, separation, further reclaims TA, p-TA.According to quality product and systematic water balance, concentrated solution also can be discharged on a small quantity, enters the sewage-farm.
2, equipment and technical process:
PTA device of refining unit separating and filtering waste water (refinement mother liquor) through heat exchange and cooling to design temperature, enters stainless steel membrane ultra-filtration and separation device, by recycle pump pressurization thickening filtration.The stainless steel membrane tripping device is held back TA and the p-TA suspended solids that crystallization is separated out in the waste water, and the concentrated solution of holding back suspended solids formation is collected in the ultrafiltration and concentration liquid storage tank, recycles to be pumped into PTA device oxidation unit again.Stainless steel membrane tripping device filtrate enters into ultrafiltration and leaches flow container, then by being pumped into the ion-exchange feed heater, enters continuous ionic exchange catalysts recovery system (ion exchange system) after making its temperature microlitre.Ion exchange resin is selected adsorption and enrichment to cobalt and manganese, adsorbs saturated back and resolves with rare HBr aqueous solution, obtains cobalt-manganese catalyst solution, and desorbed solution enters catalyst tank, again to be pumped into the oxidation system reuse.The ion exchange resin water outlet to other adsorption of metal ions, is taken off suction with dilute hydrochloric acid once more through ion exchange resin then, and stripping liquid enters sewage disposal.The liquid stream that removes metal ion is introduced into from handing over the back liquid tank, send with transferpump again, use from handing over back liquid directly to return refining system on a small quantity, most of liquid makes its temperature rise to 70～75 ℃ through the refinement mother liquor heat exchange of first interchanger and about 100 ℃, enter the reverse osmosis (RO) system then, by the RO film molten Jie's organic matter and metal ion are efficiently held back removal, filtrate satisfies the quality of reused water requirement, is back to the refined unit water spot.The reverse osmosis membrane concentrated solution returns the refinement mother liquor charging, and according to the device situation, a small amount of concentrated solution intermittently enters sewage disposal.
Regularly wash and matting flushing and Cleaning Wastewater discharging for the film system; Ion exchange system is regularly carried out rinsing and acid, alkali regeneration, regenerative wastewater discharging.
Substantially realized that by above-mentioned facility refinement mother liquor waste water step uses and closed cycle, has stepped major step to the waste water zero emission target.
3, exemplifying embodiment
Refinement mother liquor is reduced to about 100 ℃ through temperature after the flash distillation, this moment mother liquor in P-TA concentration at 2000～2500PPM, TA content is approximately 0.5～1.0%Wt, through first interchanger and liquid heat-exchange after handing over, make its temperature reduce to 72～75 ℃, cool off with recirculated cooling water through water cooler (second interchanger) again, make mother liquor be cooled to 40～45 ℃, P-TA nearly 65% separates out in the mother liquor at this moment, and TA finishes substantially and separates out (more than 95%), and the mother liquor solid content is greatly about 0.6～1.0%Wt.Cooling back mother liquor being pumped into the stainless steel membrane ultrafiltration system, and concentrates its circulating filtration with recycle pump through mother liquor tank, and when being concentrated into solid content 16～18%Wt, concentrated solution is extracted out, drains into the concentrated flow container that band stirs, and then recycles to be pumped to oxidation unit.The ultrafiltration system filtrate then enters ultrafiltration and leaches flow container, heat with low-pressure steam to be pumped into the ion-exchange feed heater again, it is warming up to enters continuous ionic exchange catalysts recovery system about 45 ℃, by ion exchange resin adsorption of cobalt manganese metal ion optionally, adsorb the HBr aqueous solution desorb of saturated resin, desorbed solution recycles with the pumped back oxidation system through catalyst tank.Logistics enters the secondary ions resin-column after removing Co, Mn ion, to other adsorption of metal ions, and takes off suction with dilute hydrochloric acid, and metal ion is taken off imbibition and is discharged into sewage disposal.From handing over back liquid to pump out, about 1/3 liquid measure is used as PTA drying machine eluting column spray liquid from handing over back liquid directly to deliver to refined unit; Amount refinement mother liquor of 100 ℃ after handing over back liquid to send into interchanger and flash distillation carries out heat exchange in addition～2/3, makes it be warming up to 70～75 ℃, enters the reverse osmosis water recovery system thereafter.This strand liquid multistage reverse osmosis (RO) system that flows through holds back concentrated, the amount that sees through the peace and quiet water of permeable membrane (filtrate) is approximately 2/3 of inlet, p-TA content is lower than 200PPM in this liquid, directly returns refining system, can be used as one washing lotion of filter cake or as PTA drying machine eluting column spray liquid.RO system concentrated solution is approximately 1/3 of inlet amount, wherein contain p-TA 2500～3500PPM, contain TA 1000～2000PPM, and contain very metal ion such as small amount of Fe, Na, refinement mother liquor is mainly returned in this burst logistics, recycle once more, according to metal ion situation and systematic water balance in the system, this concentrated solution can intermittently be discharged into sewage disposal.
Ultrafiltration, from hand over, reverse osmosis system all has the back flushing facility, regularly with acid, alkali, RO water cleaning anti-blocking, washing lotion also is discharged to sewage disposal.
Claims (9)
1. pure terephthalic acid's device of refining mother liquor reclaiming method is characterized in that comprising the following steps:
(1) adopt heat change method that refinement mother liquor is lowered the temperature;
(2) the employing hyperfiltration process is handled the refinement mother liquor after lowering the temperature, and the ultrafiltration and concentration liquid that obtains after the ultrafiltration is sent in the ultrafiltration and concentration flow container, recycles in order to sending into the oxidation unit occasion;
(3) the ultrafiltration filtrate that obtains after the ultrafiltration is sent into ion exchange system, remove Co, Mn ion and Fe, Ni, the Na metal ion that is used as catalyzer in the liquid respectively by ion-exchange techniques, wherein contain Co, Mn ionic elutriant is sent in the catalyzer flow container, recycle in order to sending into the oxidation unit occasion; The elutriant that contains Fe, Ni, Na metal ion effluxes, and sends into the sewage-farm and handle; Exchange back liquid is sent into from handing over the back liquid tank;
(4) will be from handing over using in the liquid tank of back from handing over the back liquid portion to return refining system, part is carried out reverse-osmosis treated through sending into reverse osmosis system after heating, the reverse osmosis concentrated liquid that obtains is sneaked into without the refinement mother liquor of uf processing and is handled again, the reverse osmosis filtrate that obtains is sent into the reuse water pot, be used in order to sending into the refined unit occasion
In the described step (1), by placed in-line first interchanger and second interchanger carry out twice heat exchange cooling successively, wherein first interchanger adopts step (4) to need the liquid after handing over of heating, the heat energy that utilizes refinement mother liquor will be to entering these liquid heat of reverse osmosis system, control is 72～77 ℃ from the temperature of the refinement mother liquor that first interchanger comes out, the temperature of the refinement mother liquor that comes out from second interchanger is 40～45 ℃, and the temperature from handing over back liquid of coming out from first interchanger is 70～75 ℃.
2. pure terephthalic acid's device of refining mother liquor reclaiming method as claimed in claim 1 is characterized in that:
The filter material of used ultrafiltration system is the coated TiO of sintering metal that precision reaches 50～100 nanometers in the described step (2)
2Film, filter type adopt cross-flow to concentrate, and the concentrated solution solid content is 15-20%.
3. pure terephthalic acid's device of refining mother liquor reclaiming method as claimed in claim 1 is characterized in that:
The ion exchange system of described step (3) by the Co that sets gradually, Mn from presentate unit and Fe, Ni, Na from presentate unit, be used as Co, Mn ion and the metal cations Fe of catalyzer, the ion-exchange of Ni, Na successively, and carry out regeneration of ion-exchange resin by acid washing method, and obtain corresponding ionic elutriant, wherein Co, Mn adopt HBr to carry out pickling from presentate unit, and Fe, Ni, Na adopt HCl to carry out pickling from presentate unit.
4. pure terephthalic acid's device of refining mother liquor reclaiming method as claimed in claim 1 is characterized in that:
In step (4), the reverse osmosis precision is controlled at 0.5～1nm scope, only allows small molecules H basically
2O passes through, the acetic acid of larger molecular weight, terephthalic acid, p-methylbenzoic acid and metal ion are held back the formation concentrated solution by reverse osmosis membrane, account for 1/3 liquid measure, the filtrate of reverse osmosis is 2/3 liquid measure, meet the quality of reused water requirement, according to pure terephthalic acid's quality product and systematic water balance requirement, concentrated solution is discharged on a small quantity, enters the sewage-farm.
5. pure terephthalic acid's device of refining mother liquor recovery system, it is characterized in that comprising heat-exchange system, ultrafiltration system, ion exchange system and reverse osmosis system, the heat release medium import of described heat-exchange system is the refinement mother liquor import, outlet connects the import of ultrafiltration system, the filtrate outlet of described ultrafiltration system connects the import of described ion exchange system, and the liquid outlet connects described reverse osmosis system import after the exchange of described ion exchange system.
6. pure terephthalic acid's device of refining mother liquor recovery system as claimed in claim 5, it is characterized in that described heat-exchange system comprises first interchanger and second interchanger, the heat-absorbing medium passage of described first interchanger is serially connected on the ion exchange system outlet conduit, described second interchanger is connected on the back of described first interchanger, and its heat-absorbing medium passage connects cooling water pipeline.
7. pure terephthalic acid's device of refining mother liquor recovery system as claimed in claim 5 is characterized in that described ultrafiltration system adopts cross-flow to concentrate structure, and used filter material adopts the coated TiO of sintering metal
2Membrane structure, the ultrafiltration and concentration liquid outlet of described ultrafiltration system connects the import of ultrafiltration and concentration flow container, has agitator in the described ultrafiltration and concentration flow container, and its outlet is provided with ultrafiltration and concentration liquid and sends pump.
8. pure terephthalic acid's device of refining mother liquor recovery system as claimed in claim 5, it is characterized in that the preferred continuous ionic exchange system of described ion exchange system, comprise the Co, the Mn that set gradually from presentate unit and Fe, Ni, Na from presentate unit, described Co, Mn are from handing over unitary Co, the outlet of Mn desorbed solution to enter catalyst tank.
9. as claim 5,6,7 or 8 described pure terephthalic acid's device of refining mother liquor recovery systems, it is characterized in that described ultrafiltration system filtrate outlet leaches flow container and ion-exchange fresh feed pump with being provided with successively on the connecting tube of described ion exchange system import, the inlet pipeline of described ion exchange system is provided with the ion-exchange feed heater, described ion-exchange feed heater is the low-pressure steam well heater, on exporting with the connecting tube of described reverse osmosis system import, the liquid after handing over of described ion exchange system is provided with successively from handing over the back flow container and transferpump after handing over, the described heat-absorbing medium import that connects described first interchanger from the outlet conduit of handing over the back transferpump, on the connecting tube of handing over back transferpump outlet and the described first interchanger heat-absorbing medium import, also be provided with one from handing over back liquid branch road described, should be from handing over back liquid branch road to be connected in refining system, described reverse osmosis system concentrated solution outlet is connected with two reverse osmosis concentrated liquid output channels, one of them reverse osmosis concentrated liquid output channel inserts the sewage-farm, and another reverse osmosis concentrated liquid output channel inserts the connecting tube between the described first interchanger heat release media outlet and the second interchanger heat release medium import.
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| WO2014189786A1 (en) * | 2013-05-20 | 2014-11-27 | Invista Technologies S.A R.L. | Pure plant waste water purification and recycle |
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| CN110372116A (en) * | 2019-08-09 | 2019-10-25 | 大连凯信石化科技有限公司 | Method for recovering acetic acid in wastewater of PTA oxidation device |
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| CN113087081B (en) * | 2021-04-14 | 2022-04-26 | 南京依柯卡特排放技术股份有限公司 | PTA refining mother liquor recovery method based on ceramic membrane technology |
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| CN101254985A (en) | 2008-09-03 |
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