CN102698675A - Recovery tower and recovery process for benzoic acid in pure terephthalic acid (PTA) residues - Google Patents
Recovery tower and recovery process for benzoic acid in pure terephthalic acid (PTA) residues Download PDFInfo
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- CN102698675A CN102698675A CN2012102033814A CN201210203381A CN102698675A CN 102698675 A CN102698675 A CN 102698675A CN 2012102033814 A CN2012102033814 A CN 2012102033814A CN 201210203381 A CN201210203381 A CN 201210203381A CN 102698675 A CN102698675 A CN 102698675A
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Abstract
The invention discloses a recovery tower and recovery process for benzoic acid in pure terephthalic acid (PTA) residues. The recovery tower for the benzoic acid in the PTA residues comprises an overhead heat exchanger, a packed tower and a reaction kettle, wherein the overhead heat exchanger, the packed tower and the reaction kettle are arranged vertically and are connected in sequence; the packed tower is formed by connecting a plurality of delivery pipes head to tail; the upper part of the overhead heat exchanger is provided with a feeding hole; the bottom part of the reaction kettle is provided with a discharge hole; and the interior of at least one delivery pipe is provided with a latticed grid tray. As the recovery tower for the benzoic acid in the PTA residues consists of the overhead heat exchanger, the packed tower and the reaction kettle which are connected in sequence, all processing steps of dissolving residue hot water required by recovering the benzoic acid in the PTA residues to coarse benzoic acid to remove water can be completed only by the recovery tower. The recovery tower is simple in structure, easy in assembling, low in cost and high in utilization rate of equipment. According to the recovery tower disclosed by the invention, the oxidation residues can be repeatedly heated and dissolved, and thus, the waste of the benzoic acid is reduced, the delivery pipes of the packed tower cannot be blocked; and the benzoic acid recovery rate reaches up to 85 percent.
Description
Technical field
The present invention relates to a kind of recovery tower and reclaim technology, be specifically related to benzoic recovery tower and recovery technology in a kind of PTA residue.
Background technology
P-phthalic acid (PTA) is the important source material of polyester industrial; Large-scale industrial production, PTA by paraxylene through oxidation, refining forming, in the oxidation reaction except that generating the principal product terephthalic acid (TPA); Still there is multiple accessory substance to generate; In order to guarantee the quality of PTA product, prevent that harmful substance from accumulating in generation system, oxidation section needs regularly to discharge oxidation residua; Per 1,000,000 tons of PTA discharge moisture 60% oxidation residua at 07～10,000 ton, and the main component of oxidation residua has: water, benzoic acid, terephthalic acid (TPA), M-phthalic acid etc.
The present main method of disposal of oxidation residua has: (1) gets into the PTA sewage disposal system with it with alkali dissolving back, and the characteristics of this method are to handle very thoroughly, but cost is high, has high input, not by extensive employing; (2) carry out recycling, the solid portion of oxidation residua is separated, behind separating technology, be processed into useful product, the COD amount that gets into the PTA sewerage like this can reduce about 70%, significantly reduces processing cost.
Chinese invention patent CN101870648A discloses a kind of benzoic method that from the PTA oxidation residua, reclaims; Comprise that residue hot water dissolving, filtration, hot filtrate cooling, crude benzol formic acid dope filtration, crude benzol formic acid dewater, six processes of crude benzol formic acid rectifying; Make technical benzene formic acid and pure mixed phthalic acid product; Its job step is following: a) with oxidation residua and water heating for dissolving, obtain the hot slurries of oxidation residua, solution temperature is 70～140 ℃; B) the hot slurries of oxidation residua are through the filtering slag, and filtrating is cooled off in cooled containers, is cooled to be no more than 10 ℃ of room temperatures, obtains crude benzol formic acid slurries; C) crude benzol formic acid slurries get crude benzol formic acid filter cake and waste water through press filtration, and the waste water major part is returned dissolution process, and the back of releasing on a small quantity gets into sewage-treatment plant and handles; D) crude benzol formic acid filter cake distilled water, the temperature terminal point is 115～130 ℃; E) crude benzol formic acid rectifying, pressure is controlled at 0.001～0.1mpa, and the still temperature is no more than 250 ℃.Utilize said method, the benzoic acid rate of recovery is high, meets the requirement of technical benzene formic acid.About 70% COD changes into useful product in the oxidation residua, turns waste into wealth, and has reduced the COD discharge capacity significantly.
Conventional, for implementing above-mentioned technology, all corresponding special equipment of each step connects into benzoic recovery tower with each equipment then, but this apparatus structure is complicated, cost is high, and take bigger space, assembling is difficult for.
For solving the problems of the technologies described above, a kind ofly can concentrate the equipment of realizing to become the technical barrier of benzoic recovery in the PTA residue multiplex's step of planting, it is existing to need to be resolved hurrily.
Summary of the invention
The object of the invention provides benzoic recovery tower and recovery technology in a kind of PTA residue; Utilize this device and technology; A plurality of steps in the benzoic acid removal process can be accomplished in same equipment, simple in structure, be prone to assembling, cost is low, and production capacity is big, the rate of recovery is high.
For achieving the above object; The technical scheme that the present invention adopts is: benzoic recovery tower in a kind of PTA residue; Comprise the cat head heat exchanger, packed tower and the agitated reactor that are provided with and connect successively up and down, said packed tower is formed by connecting the complex root carrier pipe from beginning to end, and the top of said cat head heat exchanger is provided with charging aperture; The bottom of agitated reactor is provided with drain hole, is provided with latticed screen at least one carrier pipe.
In the technique scheme; Said cat head heat exchanger comprises housing and the heat-exchanging tube bundle that is plugged in this housing; The below of this heat-exchanging tube bundle is provided with end socket; The concave surface of end socket is connected with discharging opening over against the heat-exchanging tube bundle tail end on the said end socket, and the heat exchanger inner space of the recessed side of end socket is through this discharging opening and external communications.
In the technique scheme, the lower housing portion of said cat head heat exchanger is provided with two temperatures meter interface, and the not-go-end of two temperatures meter interface lays respectively at the concave, convex side of said end socket.
Further technical scheme, the gusset that said end socket utilization plural number piece circumferentially is uniformly distributed with is fixedly connected with the heat exchanger shell inwall.
Further technical scheme, said packed tower is formed by connecting the long root carrier pipe of 4 2.5m～3m from beginning to end, is provided with a said screen in each carrier pipe, and screen utilizes gripper shoe to be fixedly connected with the carrier pipe inwall.
In the technique scheme, connect through flange seal between said cat head heat exchanger, packed tower and the agitated reactor.
In the technique scheme, the outside of said agitated reactor is arranged with spacer, is provided with the conduction oil that circulates between spacer and the agitated reactor outer wall.
Preferably; Said cat head heat exchanger is vertical titanium heat exchanger, and said heat-exchanging tube bundle is a U type heat-exchanging tube bundle, has circulated heat transferring medium in it; The head of this U type heat-exchanging tube bundle utilizes flange to be connected with the oral area of heat exchanger shell, and said end socket is located at the below of U type heat-exchanging tube bundle.
Cat head heat exchanger, packed tower and the agitated reactor of this recovery tower are all selected titanium material, good corrosion resistance for use.
The solution temperature of oxidation residua is 70～140 ℃, but more than 80 ℃, along with temperature is high more, benzoic solubility absolute value is exponential type and rises, and the water of required adding reduces rapidly, causes the benzoic acid concentration of ordinary dissolution excessive.In the said structure, dissolve fully, the temperature of heat transferring medium in the U type heat-exchanging tube bundle is set at 200～270 ℃ for making oxidation residua; But the interbank temperature of U type heat-exchanging tube bundle is higher than the temperature between heat-exchanging tube bundle and the heat exchanger shell inwall, and the mixture between heat-exchanging tube bundle of flowing through is heated many, and benzoic acid solubility is excessive; The benzoic acid that remains in the slurries is too much; If directly carry out technologies such as follow-up filtration, distillation, rectifying, the benzoic acid rate of recovery is low, and waste is serious; Simultaneously; The filter plant easy scale formation, the cleaning frequency increases sharply the carrier pipe easy blocking; So the discharging opening that is provided with in cat head heat exchanger bottom can be drawn the cat head heat exchanger by hot slurries with the oxidation residua that end socket converges; After charging aperture is sent this cat head heat exchanger to, repeat heating for dissolving in cat head heat exchanger outside thin up again, improve the benzoic rate of recovery.
It is a kind of that to utilize above-mentioned recovery tower to reclaim in the PTA residue benzoic processing step following:
(1) 200～270 ℃ hot water flows into, is circulated in heat-exchanging tube bundle by what the tube side outlet was flowed out from the tube side import of U type heat-exchanging tube bundle;
(2) 200～270 ℃ conduction oil flows into, is circulated between spacer and agitated reactor by what the conduction oil outlet was flowed out from heat conductive oil inlet;
(3) oxidation residua and water mix, and Total Water is 0.5～1.5 times according to the theoretical consumption of benzoic acid Calculation of Solubility gained in the pure water in the mixture;
(4) mixture that obtains in the step (3) is sent the cat head heat exchanger to through charging aperture, the heat of utilizing U type heat-exchanging tube bundle to shed, and oxidation residua progressively dissolves;
The hot slurries of oxidation residua of (5) flowing through between U type heat-exchanging tube bundle are converged by end socket, flow out the cat head heat exchanger via discharging opening then, after charging aperture is sent this cat head heat exchanger to, repeat heating for dissolving in cat head heat exchanger outside thin up again;
(6) the hot slurries of oxidation residua between U type heat-exchanging tube bundle and inner walls of flowing through flow into the packed tower of cat head heat exchanger below, and in each carrier pipe of packed tower, obtain crude benzol formic acid slurries after by the screen filter cleaner;
(7) crude benzol formic acid slurries get into agitated reactor, and distillation dehydration under the effect of conduction oil obtains the dry raw benzoic acid;
(8) the dry raw benzoic acid that obtains in the step (7) flows out recovery tower by drain hole, flows to the rectifier unit of peripheral hardware by pipeline, obtains required benzoic acid, and the benzoic acid recovery operation is accomplished in the PTA residue.
Because the technique scheme utilization, the advantage that the present invention compared with prior art has is:
1. the present invention is made up of the cat head heat exchanger, packed tower and the agitated reactor that connect successively; Reclaiming each processing step that the required residue hot water dissolving of benzoic acid dewaters to crude benzol formic acid in the PTA residue only needs this cover recovery tower to accomplish; Simple in structure, be prone to assembling, cost is low, utilization rate of equipment and installations is high.
The present invention will flow through between heat-exchanging tube bundle, residually have the hot slurries of too much benzoic oxidation residua to converge by end socket; Flow out the cat head heat exchanger via discharging opening then; After charging aperture is sent this cat head heat exchanger to, repeat heating for dissolving in cat head heat exchanger outside thin up again, reduce benzoic waste, do not cause the obstruction of packed tower carrier pipe; The benzoic acid rate of recovery is high, can reach 85%.
3. the present invention is provided with screen in carrier pipe, can in the process of each carrier pipe of packed tower, accomplish filter cleaner technology synchronously in the hot slurry stream of oxidation residua, and adopt the mode of multistage filtering, and slagging-off thoroughly problems such as fouling, obstruction can not take place.
Description of drawings
Fig. 1 is the front view of the embodiment of the invention one;
Fig. 2 is the front view of cat head heat exchanger among the embodiment one;
Fig. 3 is the front view of carrier pipe among the embodiment one;
Fig. 4 is the front view after the assembling of agitated reactor and spacer among the embodiment one;
Wherein: 1, cat head heat exchanger; 10, charging aperture; 11, end socket; 12, discharging opening; 13, thermometer boss; 14, thermometer boss; 2, carrier pipe; 20, screen; 3, agitated reactor; 30, drain hole; 4, heat-exchanging tube bundle; 5, spacer.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further described:
Embodiment one: referring to Fig. 1～shown in Figure 4; Benzoic recovery tower in a kind of PTA residue; Comprise the cat head heat exchanger 1, packed tower and the agitated reactor 3 that are provided with and connect successively up and down; Said packed tower is by long carrier pipe 2 end to end the forming of 4 2.5m, and said cat head heat exchanger 1, packed tower and agitated reactor 3 are all selected corrosion resistant titanium material for use, all connect through flange seal between cat head heat exchanger 1, packed tower and the agitated reactor 3.
Heat-exchanging tube bundle 4 is plugged in the housing of cat head heat exchanger 1; The top of said housing is provided with charging aperture 10; The below of heat-exchanging tube bundle 4 is provided with end socket 11, and the gusset that end socket 11 utilizes plural piece circumferentially to be uniformly distributed with is fixedly connected with inner walls, and the concave surface of this end socket 11 is over against heat-exchanging tube bundle 4 tail ends; Be connected with discharging opening 12 on the said end socket 11, the heat exchanger inner space of end socket 11 recessed sides is through this discharging opening 12 and external communications.
The lower housing portion of cat head heat exchanger 1 is provided with two temperatures meter interface, is respectively recessed side thermometer boss 13 of end socket and the protruding side thermometer boss 14 of end socket, and the not-go-end of two temperatures meter interface lays respectively at the concave, convex side of end socket 11.
In the present embodiment, the cat head heat exchanger is vertical titanium heat exchanger.Heat-exchanging tube bundle 4 is a U type heat-exchanging tube bundle, has circulated heat transferring medium in it, and the temperature of heat transferring medium is 200～270 ℃.
Be provided with in every carrier pipe 2 one utilize gripper shoe to be fixedly connected with the carrier pipe inwall latticed screen 20, be used for the filter cleaner of the hot slurries of oxidation residua.
The bottom of said agitated reactor 3 is provided with drain hole 30, and the outside of agitated reactor 3 is arranged with spacer 5, is provided with the conduction oil that circulates between spacer 5 and agitated reactor 3 outer walls, and the temperature of conduction oil is 200～270 ℃.
The solution temperature of oxidation residua is 70～140 ℃, but more than 80 ℃, along with temperature is high more, benzoic solubility absolute value is exponential type and rises, and the water of required adding reduces rapidly, causes the benzoic acid concentration of ordinary dissolution excessive.In the said structure, dissolve fully, the temperature of heat transferring medium in the U type heat-exchanging tube bundle is set at 200～270 ℃ for making oxidation residua; But the interbank temperature of U type heat-exchanging tube bundle is higher than the temperature between heat-exchanging tube bundle and the heat exchanger shell inwall, and the mixture between heat-exchanging tube bundle of flowing through is heated many, and benzoic acid solubility is excessive; The benzoic acid that remains in the slurries is too much; If directly carry out technologies such as follow-up filtration, distillation, rectifying, the benzoic acid rate of recovery is low, and waste is serious; Simultaneously; The filter plant easy scale formation, the cleaning frequency increases sharply the carrier pipe easy blocking; So the discharging opening that is provided with in cat head heat exchanger bottom can be drawn the cat head heat exchanger by hot slurries with the oxidation residua that end socket converges; After charging aperture is sent this cat head heat exchanger to, repeat heating for dissolving in cat head heat exchanger outside thin up again, improve the benzoic rate of recovery.
It is following to utilize present embodiment to reclaim in the PTA residue benzoic processing step:
(1) 200～270 ℃ hot water flows into, is circulated in heat-exchanging tube bundle by what the tube side outlet was flowed out from the tube side import of U type heat-exchanging tube bundle;
(2) 200～270 ℃ conduction oil flows into, is circulated between spacer and agitated reactor by what the conduction oil outlet was flowed out from heat conductive oil inlet;
(3) oxidation residua and water mix, and Total Water is 0.5～1.5 times according to the theoretical consumption of benzoic acid Calculation of Solubility gained in the pure water in the mixture;
(4) mixture that obtains in the step (3) is sent the cat head heat exchanger to through charging aperture, the heat of utilizing U type heat-exchanging tube bundle to shed, and oxidation residua progressively dissolves;
The hot slurries of oxidation residua of (5) flowing through between U type heat-exchanging tube bundle are converged by end socket, flow out the cat head heat exchanger via discharging opening then, after charging aperture is sent this cat head heat exchanger to, repeat heating for dissolving in cat head heat exchanger outside thin up again;
(6) the hot slurries of oxidation residua between U type heat-exchanging tube bundle and inner walls of flowing through flow into the packed tower of cat head heat exchanger below, and in each carrier pipe of packed tower, obtain crude benzol formic acid slurries after by the screen filter cleaner;
(7) crude benzol formic acid slurries get into agitated reactor, and distillation dehydration under the effect of conduction oil obtains the dry raw benzoic acid;
(8) the dry raw benzoic acid that obtains in the step (7) flows out recovery tower by drain hole, flows to the rectifier unit of peripheral hardware by pipeline, obtains required benzoic acid, and the benzoic acid recovery operation is accomplished in the PTA residue.
The foregoing description is not the qualification to purposes of the present invention, and the present invention can also be as the equipment that reclaims terephthaldehyde's acid residue or other occasions that is suitable for.
Claims (10)
1. benzoic recovery tower in the PTA residue; It is characterized in that: comprise the cat head heat exchanger (1), packed tower and the agitated reactor (3) that are provided with and connect successively up and down; Said packed tower is formed by connecting complex root carrier pipe (2) head and the tail; The top of said cat head heat exchanger (1) is provided with charging aperture (10), and the bottom of agitated reactor (3) is provided with drain hole (30), is provided with latticed screen (20) at least one carrier pipe (2).
2. benzoic recovery tower in the PTA residue according to claim 1; It is characterized in that: said cat head heat exchanger (1) comprises housing and the heat-exchanging tube bundle (4) that is plugged in this housing; The below of this heat-exchanging tube bundle (4) is provided with end socket (11); The concave surface of end socket (11) is connected with discharging opening (12) over against heat-exchanging tube bundle (4) tail end on the said end socket (11), the heat exchanger inner space of the recessed side of end socket (11) is through this discharging opening (12) and external communications.
3. benzoic recovery tower in the PTA residue according to claim 2; It is characterized in that: the lower housing portion of said cat head heat exchanger (1) is provided with two temperatures meter interface (13; 14), the not-go-end of two temperatures meter interface (13,14) lays respectively at the concave, convex side of said end socket (11).
4. according to benzoic recovery tower in claim 2 or the 3 described PTA residues, it is characterized in that: the gusset that said end socket (11) utilizes plural piece circumferentially to be uniformly distributed with is fixedly connected with the heat exchanger shell inwall.
5. benzoic recovery tower in the PTA residue according to claim 1; It is characterized in that: said packed tower is formed by connecting long root carrier pipe (2) head and the tail of 4 2.5m～3m; Be provided with a said screen (20) in each carrier pipe (2), screen (20) utilizes gripper shoe to be fixedly connected with the carrier pipe inwall.
6. benzoic recovery tower in the PTA residue according to claim 1 is characterized in that: connect through flange seal between said cat head heat exchanger (1), packed tower and the agitated reactor (3).
7. benzoic recovery tower in the PTA residue according to claim 1 is characterized in that: the outside of said agitated reactor (3) is arranged with spacer (5), is provided with the conduction oil that circulates between spacer (5) and agitated reactor (3) outer wall.
8. according to benzoic recovery tower in claim 2 or the 3 described PTA residues; It is characterized in that: said cat head heat exchanger (1) is vertical titanium heat exchanger; Said heat-exchanging tube bundle (4) is a U type heat-exchanging tube bundle; Circulated heat transferring medium in it, the head of this U type heat-exchanging tube bundle (4) utilizes flange to be connected with the oral area of heat exchanger shell, and said end socket (11) is located at the below of U type heat-exchanging tube bundle (4).
9. benzoic recovery tower in the PTA residue according to claim 1 and 2 is characterized in that: said cat head heat exchanger (1), packed tower and agitated reactor (3) are all selected the titanium material for use.
10. a recovery technology of utilizing benzoic acid recovery tower in claim 1 or the described PTA residue is characterized in that: comprise the steps:
(1) 200～270 ℃ hot water flows into, is circulated in heat-exchanging tube bundle by what the tube side outlet was flowed out from the tube side import of U type heat-exchanging tube bundle;
(2) 200～270 ℃ conduction oil flows into, is circulated between spacer and agitated reactor by what the conduction oil outlet was flowed out from heat conductive oil inlet;
(3) oxidation residua and water mix, and Total Water is 0.5～1.5 times according to the theoretical consumption of benzoic acid Calculation of Solubility gained in the pure water in the mixture;
(4) mixture that obtains in the step (3) is sent the cat head heat exchanger to through charging aperture, the heat of utilizing U type heat-exchanging tube bundle to shed, and oxidation residua progressively dissolves;
The hot slurries of oxidation residua of (5) flowing through between U type heat-exchanging tube bundle are converged by end socket, flow out the cat head heat exchanger via discharging opening then, after charging aperture is sent this cat head heat exchanger to, repeat heating for dissolving in cat head heat exchanger outside thin up again;
(6) the hot slurries of oxidation residua between U type heat-exchanging tube bundle and inner walls of flowing through flow into the packed tower of cat head heat exchanger below, and in each carrier pipe of packed tower, obtain crude benzol formic acid slurries after by the screen filter cleaner;
(7) crude benzol formic acid slurries get into agitated reactor, and distillation dehydration under the effect of conduction oil obtains the dry raw benzoic acid;
(8) the dry raw benzoic acid that obtains in the step (7) flows out recovery tower by drain hole, flows to the rectifier unit of peripheral hardware by pipeline, obtains required benzoic acid, and the benzoic acid recovery operation is accomplished in the PTA residue.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102033814A CN102698675A (en) | 2012-06-20 | 2012-06-20 | Recovery tower and recovery process for benzoic acid in pure terephthalic acid (PTA) residues |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012102033814A CN102698675A (en) | 2012-06-20 | 2012-06-20 | Recovery tower and recovery process for benzoic acid in pure terephthalic acid (PTA) residues |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102961984A (en) * | 2012-12-06 | 2013-03-13 | 天津开发区渤海东大药业有限公司 | Dissolution tank for drug level benzoic acid production and operation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100409A (en) * | 1993-03-30 | 1995-03-22 | 三井石油化学工业株式会社 | Process and apparatus for producing terephthalic acid |
| CN101402564A (en) * | 2008-05-15 | 2009-04-08 | 厦门海湾化工有限公司 | Dissolution processing method for CTA draff in PTA production |
| CN101513641A (en) * | 2008-04-03 | 2009-08-26 | 沈福昌 | Resource treatment method for fine terephthalic acid waste residue |
| CN202666841U (en) * | 2012-06-20 | 2013-01-16 | 苏州龙峰钛镍设备有限公司 | Recovery tower for benzoic acid in PTA (Pure Terephthalic Acid) residues |
-
2012
- 2012-06-20 CN CN2012102033814A patent/CN102698675A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1100409A (en) * | 1993-03-30 | 1995-03-22 | 三井石油化学工业株式会社 | Process and apparatus for producing terephthalic acid |
| CN101513641A (en) * | 2008-04-03 | 2009-08-26 | 沈福昌 | Resource treatment method for fine terephthalic acid waste residue |
| CN101402564A (en) * | 2008-05-15 | 2009-04-08 | 厦门海湾化工有限公司 | Dissolution processing method for CTA draff in PTA production |
| CN202666841U (en) * | 2012-06-20 | 2013-01-16 | 苏州龙峰钛镍设备有限公司 | Recovery tower for benzoic acid in PTA (Pure Terephthalic Acid) residues |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102961984A (en) * | 2012-12-06 | 2013-03-13 | 天津开发区渤海东大药业有限公司 | Dissolution tank for drug level benzoic acid production and operation method |
| CN102961984B (en) * | 2012-12-06 | 2015-04-15 | 天津开发区渤海东大药业有限公司 | Dissolution tank for drug level benzoic acid production and operation method |
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Application publication date: 20121003 |