CN100368370C - Recovery system of suspended substance in para dimethyl benzene oxidation mother liquor - Google Patents
Recovery system of suspended substance in para dimethyl benzene oxidation mother liquor Download PDFInfo
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- CN100368370C CN100368370C CNB2006100391689A CN200610039168A CN100368370C CN 100368370 C CN100368370 C CN 100368370C CN B2006100391689 A CNB2006100391689 A CN B2006100391689A CN 200610039168 A CN200610039168 A CN 200610039168A CN 100368370 C CN100368370 C CN 100368370C
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Abstract
The present invention discloses a recovery system for suspended objects in para dimethyl benzene oxidation mother liquor. The recovery system comprises a mother liquor tank, a feeding pump, a cooler, a filter and a control valve, wherein oxidation mother liquor in the mother liquor tank is conveyed to the cooler through the feeding pump; the cooled mother liquor is recovered by suspended objects and is filtered by the filter; the filtered clear liquor is conveyed to a solvent recovering system for recovering acetic acid, and the suspended objects are returned to the mother liquor tank along with the mother liquor; and then, the suspended objects are conveyed to a feeding and mixing tank through the mother liquor pump for continuing to be used, and the action of the control valve in a pipeline is controlled by a program. The recovery system effectively recovers the suspended objects in the oxidation mother liquor. A device which has the capability of producing 35 0000 tons of PTA per year uses the recovery system to recover 700 tons of PTA per year.
Description
One, technical field
The present invention relates to the resource recovering system in a kind of Chemicals production process, particularly a kind of pure terephthalic acid (PTA) is in the feedstock production PTA process with p-Xylol (PX) especially, to the recovery system of suspended substance in the PX oxidizing reaction mother liquor in producing.
Two, background technology
Pure terephthalic acid's (PTA) production generally is to be raw material with p-Xylol (PX), with Cobaltous diacetate and manganese acetate is catalyzer, Hydrogen bromide is a promotor, acetic acid is solvent, under certain temperature and pressure, utilizes the continuous oxidation of air to make terephthalic acid slurry, crystallization then, separation, drying, obtain crude terephthalic acid (TA), crude terephthalic acid is again through hydrogenation reaction, and crystallization, separation and drying can make the pure terephthalic acid (PTA) who is used to produce polyester.
Produce in the thick TA process in the PX oxidation, the acetate solvate of separating that is rich in catalyzer, other organism by products and inorganic impurity abbreviates mother liquor as.It can turn back to continues in the oxidation system to use, and in order to guarantee quality product, mother liquor only can have 90%～95% to get back to original system, and 5%～10% remaining mother liquor will be by the extraction system, outside this part mother liquor extraction system.The classical group of mother liquor becomes to see Table 1:
Table 1
| Form | Acetic acid | Catalyzer | By product/impurity | Suspended substance |
| Wt％ | 89 | 0.16 | 3.8 | 1～2％ |
Traditional technology is that the mother liquor of this part extraction is reclaimed wherein acetic acid by an evaporation subsystem, and remaining catalyzer, by product, suspended substance are all delivered to wastewater treatment.Suspended substance main component table 2 in the mother liquor:
Table 2
| Suspended substance is formed | Phenylformic acid | To carboxyl benzaldehyde | P-methylbenzoic acid | Terephthalic acid |
| Wt％ | 0.76 | 0.50 | 0.26 | 98 |
Suspended substance mainly consist of terephthalic acid, if directly deliver to wastewater treatment, not only lose terephthalic acid every year from here and be about 700 tons (for devices of 350,000 tons of/year PTA throughput), and increased the load of wastewater treatment, cause the wasting of resources.
The particle diameter of this suspended substance is about 5～20 μ m, and viscosity is higher, can not efficient recovery with common filter method, also be difficult to realize industrialized continuous production.
Three, summary of the invention
1, goal of the invention: the purpose of this invention is to provide the recovery system of suspended substance in a kind of p xylene oxidation mother liquor,, can reclaim the suspended substance in the oxidation mother liquor automatically by this recovery system.
2, technical scheme: for achieving the above object, the recovery system of suspended substance in the p xylene oxidation mother liquor of the present invention, it is characterized in that it comprises mother liquor tank, fresh feed pump, water cooler, strainer and by-pass valve control, oxidation mother liquor in the mother liquor tank is delivered to water cooler by fresh feed pump, cooled mother liquor reclaims strainer through suspended substance and filters, clear liquid after the filtration is delivered to solvent recovering system and is reclaimed acetic acid, suspended substance returns mother liquor tank with mother liquor, being pumped into the charging mixing tank by mother liquor then continues to use, the action of the by-pass valve control in the pipeline is by time variable control, according to the order of by-pass valve control action, and sequence of control is worked out in conjunction with the General Principle of programming.
Water cooler is connected with cooling water circuit system, is provided with the valve and the temperature regulator of controlled chilling discharge and temperature in cooling water circuit system.
Be provided with bypass conduit is connected with solvent recovering system with the charging mixing tank in the ingress of water cooler.
On the pipeline between strainer and the mother liquor tank, be provided with the valve of Control Circulation flow.
Between strainer and solvent recovering system, be provided with the valve of control clear liquid flow.
Be connected with the pipeline that strainer is cleaned on the strainer.
Strainer is connected with the normal pressure absorption tower by pipeline respectively with mother liquor tank.
Inlet at fresh feed pump is provided with flushing pipeline.
Described strainer is a tube shell type structure, is furnished with micropore on its tubulation.
Principle of work of the present invention is: the oxidation mother liquor in the mother liquor tank is delivered to water cooler by fresh feed pump, by regulating water coolant backwater amount control mother liquor temperature, cooled mother liquor reclaims strainer through suspended substance and filters, regulate flow by regulating strainer circular flow control valve, clear liquid after the filtration is delivered to solvent recovering system and is reclaimed acetic acid, regulate flow by valve 3, suspended substance returns mother liquor tank with mother liquor, is pumped into the charging mixing tank with mother liquor and continues to use.
3, beneficial effect: remarkable advantage of the present invention is the device for 350,000 tons of/year PTA throughput, adopt to reclaim the PTA700 ton every year of the present invention, difference according to device capability, the processing power of strainer can be handled 5～15 tons/hour of suspended substance liquid, and the size of processing power depends on the area of strainer.Simple in structure, the stable performance of native system.
Four, description of drawings
Accompanying drawing is a flowage structure schematic diagram of the present invention.
Five, embodiment
As shown in the figure, the fresh feed pump ingress is provided with flushing line, and flushing medium has alkali, acetic acid or water, and the fresh feed pump outlet is provided with tensimeter.Valve 1 is the cooling backwater control valve, and valve 2 place pipelines are the filter bypass pipeline, keeps the solvent recovering system works better by bypass, and whole strainer is in to be prepared or the cleaning state.Valve 4 is the strainer feed valve, and valve 5 is the circular flow control valve, and PT1 is a strainer feed entrance pressure, and valve 7 is the filter bottom blow-off valve, and valve 6 is a strainer cleaner liquid shutdown valve, and PT2 is a strainer purified liquor outlet pressure.Valve 8 is the strainer blow-off valve, is used for the exhaust and the release of strainer, and residual air is delivered to the normal pressure absorption tower and reclaimed.Valve 9 is the nitrogen equalizer valve, is used for the cleaning of strainer, and the cleaning medium of strainer also has alkali, acetic acid and water.Valve event is moved automatically by time variable control.
Suspended substance reclaims the similar tube and shell heat exchanger of strainer, divide tube side and shell side, be furnished with the isodiametric micropore of 2 μ m on its tubulation, mother liquor is walked tube side, reclaim in the strainer at suspended substance, this filtering recovering system adopts and extrudes filter type, and charging directly flows to lower ending opening from the upper end open of filter core, and the opening of the upper and lower end of its filter core is welded on respectively on the tube sheet of two ends.Clean filtrate is then extruded from the filter core outside, and the suspended substance solid in the mother liquor is stayed in the mother liquor, and clean filtrate is sent to solvent recovering system through the mouth of pipe of strainer shell, to remove the impurity in the mother liquor and to reclaim acetic acid.In the process of continuous filtration, owing to constantly on the tube wall of strainer, deposit the suspended substance in the mother liquor, influence filter effect, therefore need carry out on-line cleaning to strainer by cleaning system, by regulating water coolant backwater amount (valve 1), the temperature of control mother liquor is so that mother liquor can reach suitable viscosity, pressure reduction according to the filter tube shell side, strainer is carried out online blow-back, acetic acid cleaning, and the acetic acid scavenging solution utilizes gravity to flow back in the mother liquor tank, carries out next flow process again.Strainer of the present invention is the accurate filter of sintering metal system, in conjunction with time variable control, by automatic temp control, has effectively realized the recovery of suspended substance in the oxidation mother liquor.
The invention provides following program controlled mode:
1, temperature control: temperature transmitter is measured the temperature of mother liquor, 30～80 ℃ of the temperature ranges of temperature regulator TIC control mother liquor, the flow of temperature control valve (TCV) TV controlled chilling device recirculated cooling water, according to the relation of mother liquor viscosity and temperature, under suitable temperature, can obtain helping filtering mother liquor viscosity.
2, automatic sequence control step:
The first step: press automatic button, valve enters state separately.Remove over by-pass valve and the stripping tower flowrate control valve, all the other valves all are in closing condition.The effect of this step is to keep the stripping tower works better by bypass, and whole strainer is in ready state.
Second step: feed valve, bottom discharge valve and circular flow control valve are opened, and fill in advance.The effect of this step is to fill in advance; Expectation keeps the stripping tower works better by bypass.
The 3rd step: the stripping tower flowrate control valve cuts out, and by-pass valve cuts out.The effect of this step is before pre-end-of-fill, and realization stripping tower flowrate control valve delays opens (preventing that filter core is subjected to big flow attack of moment).
The 4th step: the cleaner liquid shutdown valve is opened, and the stripping tower flowrate control valve opens 5%, and emptying simultaneously.The effect of this step is slow reaching the standard grade, and begins to filter; And emptying, the gas in the strainer of draining.
The 5th step: close blow-off valve.
The 6th step: after the stripping tower flowrate control valve opens 10%, open 10% again, open with the speed of per minute 10% then.The effect of this step is to make the stripping tower flowrate control valve reach flow set point.
The 7th step: filtration end point.Bottom discharge valve cuts out; By-pass valve is opened; Circular flow control valve standard-sized sheet.
The 8th step: inlet valve cuts out.
The 9th step: close the cleaner liquid shutdown valve, open blow-off valve, lay down the pressure in the strainer.
The tenth step: close blow-off valve, open the nitrogen equalizer valve and carry out pressurising.
The 11 step: open bottom discharge valve, carry out discharge.
The 12 step: close equalizer valve, open blow-off valve and carry out release.It should be noted that if form negative pressure in filter interior in the strainer discharge process, then might have foul to be inhaled into strainer, cause cleaner liquid contaminated, therefore can consider to omit this step according to practical situation from blow-down pipe.
The 13 step: restart pre-filling step behind the discharge, different with the second step state is: circular flow control valve aperture becomes 14t/h by 10%.The effect of this step is to proceed pre-filling; Keep the stripping tower works better by bypass; The circular flow control valve is adjusted to flow set point.
Recovery system of the present invention provides two kinds of operating method: a kind of is fully manually control, and another is made up of manual control and automatic control two portions.
Manually red-tape operati be by manual operation finish preheating, fill in advance, slowly reach the standard grade, filtration and 5 steps of back flushing.Under manual manipulation mode, the operator can regulate the switch of valve site by the valve trip switch.Be that switch is in the ON state, respective valves is opened, and switch is in the OFF state, and respective valves is closed.Just for providing under technology trouble and the repair, the operator must be familiar with whole technology and equipment to manual mode of operation before carrying out manual mode of operation.Filtering system is operated under manual mode, only reports to the police, and is not chain, therefore may be owing to misoperation is damaged filter core.
Manually control and automatically red-tape operati be to finish pre-heating step by manual red-tape operati, (pre-heating step only go into operation first and stop work after go into operation carry out), all the other 4 steps are finished by automatic red-tape operati.Under automatic operation scheme, need not operator and operate.Control valve moves automatically by pre-set program.
Claims (9)
1. the recovering system of suspended substance in the p xylene oxidation mother liquor, it is characterized in that it comprises mother liquor tank, fresh feed pump, water cooler, strainer and by-pass valve control, oxidation mother liquor in the mother liquor tank is delivered to water cooler by fresh feed pump, cooled mother liquor reclaims strainer through suspended substance and filters, clear liquid after the filtration is delivered to solvent recovering system and is reclaimed acetic acid, suspended substance returns mother liquor tank with mother liquor, being pumped into the charging mixing tank by mother liquor then continues to use, be provided with by-pass valve control in the pipeline, the action of valve is by time variable control.
2. the recovering system of suspended substance in the p xylene oxidation mother liquor according to claim 1, it is characterized in that described water cooler is connected with cooling water circuit system, in cooling water circuit system, be provided with the valve and the temperature regulator of controlled chilling discharge and temperature.
3. the recovering system of suspended substance in the p xylene oxidation mother liquor according to claim 1 is characterized in that being provided with bypass conduit in the ingress of water cooler is connected with solvent recovering system with the charging mixing tank.
4. the recovering system of suspended substance in the p xylene oxidation mother liquor according to claim 1 is characterized in that being provided with the valve of Control Circulation flow on the pipeline between strainer and the mother liquor tank.
5. the recovering system of suspended substance in the p xylene oxidation mother liquor according to claim 1 is characterized in that being provided with the valve of controlling the clear liquid flow between strainer and solvent recovering system.
6. the recovering system of suspended substance in the p xylene oxidation mother liquor according to claim 1 is characterized in that being connected with on the strainer pipeline that strainer is cleaned.
7. the recovering system of suspended substance in the p xylene oxidation mother liquor according to claim 1 is characterized in that strainer is connected with the normal pressure absorption tower by pipeline respectively with mother liquor tank.
8. the recovering system of suspended substance in the p xylene oxidation mother liquor according to claim 1 is characterized in that being provided with flushing pipeline at the inlet of fresh feed pump.
9. the recovering system of suspended substance in the p xylene oxidation mother liquor according to claim 1 is characterized in that described strainer is a tube shell type structure, is furnished with micropore on its tubulation.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100391689A CN100368370C (en) | 2006-03-29 | 2006-03-29 | Recovery system of suspended substance in para dimethyl benzene oxidation mother liquor |
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| CNB2006100391689A CN100368370C (en) | 2006-03-29 | 2006-03-29 | Recovery system of suspended substance in para dimethyl benzene oxidation mother liquor |
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| CN100368370C true CN100368370C (en) | 2008-02-13 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101391952B (en) * | 2008-11-12 | 2012-02-22 | 中国石油化工股份有限公司 | Recovery method of terephthalic acid/isophthalic acid refinement mother liquor |
| CN111111312A (en) * | 2020-01-17 | 2020-05-08 | 郑国强 | Device for recovering suspended particles in PTA oxidation mother liquor and using method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5142097A (en) * | 1991-05-31 | 1992-08-25 | E. I. Du Pont De Nemours And Company | Recovery and recycle of acetic acid in an oxidation process |
| US5304676A (en) * | 1991-02-05 | 1994-04-19 | Imperial Chemical Industries Plc | Process for the production of terephthalic acid |
| US5563293A (en) * | 1991-03-07 | 1996-10-08 | Imperial Chemical Industries Plc | Process for the production of terephthalic acid |
| CN1277184A (en) * | 2000-05-09 | 2000-12-20 | 华东理工大学 | Production process of aromatic binary carboxylic acid |
| CN1293184A (en) * | 2000-10-24 | 2001-05-02 | 华东理工大学 | Process and equipment for preparing aromatic carboxylicacid |
| WO2004074231A1 (en) * | 2003-02-21 | 2004-09-02 | Mitsubishi Chemical Corporation | Process for producing aromatic carboxylic acid |
-
2006
- 2006-03-29 CN CNB2006100391689A patent/CN100368370C/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5304676A (en) * | 1991-02-05 | 1994-04-19 | Imperial Chemical Industries Plc | Process for the production of terephthalic acid |
| CN1150944A (en) * | 1991-02-05 | 1997-06-04 | 帝国化学工业公司 | Production of terephthalic acid |
| US5563293A (en) * | 1991-03-07 | 1996-10-08 | Imperial Chemical Industries Plc | Process for the production of terephthalic acid |
| US5142097A (en) * | 1991-05-31 | 1992-08-25 | E. I. Du Pont De Nemours And Company | Recovery and recycle of acetic acid in an oxidation process |
| CN1277184A (en) * | 2000-05-09 | 2000-12-20 | 华东理工大学 | Production process of aromatic binary carboxylic acid |
| CN1293184A (en) * | 2000-10-24 | 2001-05-02 | 华东理工大学 | Process and equipment for preparing aromatic carboxylicacid |
| WO2004074231A1 (en) * | 2003-02-21 | 2004-09-02 | Mitsubishi Chemical Corporation | Process for producing aromatic carboxylic acid |
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Effective date of registration: 20160810 Address after: 211900 Yizheng Changjiang Road, Jiangsu, China, No. 1, No. Patentee after: CHINA SINOPEC YIZHENG CHEMICAL FIBER CO., LTD. Address before: 211900 No. 1 Changjiang Road, Jiangsu, Yizheng Patentee before: Yizheng Chemical Fiber Co., Ltd., China Petrochemical Group Corp. |