CN101190784B - Method for concentrating dilute nitric acid in adipic acid production - Google Patents
Method for concentrating dilute nitric acid in adipic acid production Download PDFInfo
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- CN101190784B CN101190784B CN200610114723XA CN200610114723A CN101190784B CN 101190784 B CN101190784 B CN 101190784B CN 200610114723X A CN200610114723X A CN 200610114723XA CN 200610114723 A CN200610114723 A CN 200610114723A CN 101190784 B CN101190784 B CN 101190784B
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- nitric acid
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- upgrading tower
- upgrading
- interchanger
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- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 title claims abstract description 144
- 229910017604 nitric acid Inorganic materials 0.000 title claims abstract description 144
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title abstract description 26
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 title abstract description 12
- 235000011037 adipic acid Nutrition 0.000 title abstract description 6
- 239000001361 adipic acid Substances 0.000 title abstract description 6
- 239000002253 acid Substances 0.000 claims description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000002351 wastewater Substances 0.000 claims description 14
- 239000012141 concentrate Substances 0.000 claims description 13
- 238000005516 engineering process Methods 0.000 claims description 13
- 239000007921 spray Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 5
- 238000011084 recovery Methods 0.000 claims description 5
- 238000009835 boiling Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000010865 sewage Substances 0.000 abstract description 8
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 abstract description 4
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000008020 evaporation Effects 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 150000007513 acids Chemical class 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 241000282326 Felis catus Species 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The invention is used for the concentration of nitric acid in the process of producing adipic acid by taking the mixture of nitric acid, cyclohexane and cyclohexanone as raw materials. Is characterized in that: a dilute nitric acid concentration device in adipic acid production is improved, a double concentration tower is adopted, and a dilute nitric acid concentration process in adipic acid production is improved, so that the concentration of concentrated nitric acid can meet the production requirement, and the improved dilute nitric acid concentration process is adapted. Through the improvement of the dilute nitric acid concentration process and device, the evaporation capacity of a concentration tower is improved, the steam consumption is saved, and the energy is saved in the dilute nitric acid concentration process in adipic acid production; reducing the sewage discharge.
Description
Technical field
The present invention relates to the petrochemical complex production technical field, the mixture that particularly is used for nitric acid and hexanaphthene, pimelinketone is the raw material production hexanodioic acid course of processing, makes spissated a kind of device of rare nitric acid and the spissated technology of rare nitric acid.
Background technology
Liaoyang petrochemical industry branch office introduced French Long Baili company hexanodioic acid production technology in 1974, be raw material with nitric acid, produced hexanodioic acid with the mixture reaction of hexanaphthene, pimelinketone, produced 5.7 ten thousand tons of hexanodioic acids per year.Because what reaction process was taked is the nitric acid excessive response, so the dilute nitric acid solution that produces in the production hexanodioic acid reaction process need concentrate and recycle.Nitric acid concentration tower in the production unit is that rare nitric acid that will be about 20-30% from the concentration of a plurality of operations generations such as enrichment device, whizzer and gas absorption, catalyst recovery concentrates, make concentration of nitric acid reach 43-50%, recycle so that turn back to reaction workshop section.
Existing nitric acid concentration tower adopts single effect distillation technology.Consult Fig. 2.Single effect distillation nitric acid concentration tower structure is: be made up of upgrading tower (2), interchanger (4) and tower bottom reboiler (3).Spray header (1) is arranged on the top of upgrading tower, and steam outlet is arranged at the top of upgrading tower, and the back of concentrating nitric acid outlet is arranged at the bottom of upgrading tower.The concentration that produces from a plurality of operations such as enrichment device, whizzer and gas absorption, catalyst recovery in the hexanodioic acid production is about rare nitric acid of 20-30%, at first enter interchanger (4), with the spissated nitric acid heat exchange of coming out in the upgrading tower bottom of process, improve the temperature of rare nitric acid.Rare nitric acid inlet enters upgrading tower to rare nitric acid from the upgrading tower middle part.Rare nitric acid distills out steam and directly enters the condensation flow process in tower, concentration of nitric acid can reach 43-50%.Nitric acid after concentrating flows out from the tower bottom outlet, flows out to the concentrated nitric acid storage tank for standby use through interchanger (4).Can satisfy the needs of producing 60000 tons of hexanodioic acid production equipments per year.Per hour handle rare nitric acid 30-40 ton, need vaporize water 14-20 ton, discharge contains nitre waste water 200-300 ton.Existing nitric acid is concentrated, and not only water loss is big, and steam consumption quantity is big, and a large amount of waste water that produce bring very big difficulty for further expanding production of hexanodioic acid production equipment.Nitric acid concentration tower is the core of hexanodioic acid production equipment, also is save energy and antipollution keypoint part.
Summary of the invention
The purpose of this invention is to provide a kind of hexanodioic acid produce in rare nitric acid concentration method, adopt two concentration method, improve hexanodioic acid produce in rare nitric acid concentration technology, make the concentration of nitric acid after concentrating can reach production requirement; Another object of the present invention be improve hexanodioic acid produce in rare nitric acid concentrating unit, to adapt to the spissated technology of rare nitric acid after the improvement.By the improvement of rare nitric acid concentration technology and device, finally reach in rare nitric acid concentration process that hexanodioic acid is produced, improve the upgrading tower steam capability, save steam consumption, save energy; Reduce quantity of wastewater effluent.
The technical solution used in the present invention is:
1, rare nitric acid concentrating unit during hexanodioic acid is produced, by upgrading tower A, upgrading tower B, and interchanger, pump and pipeline are formed.Upgrading tower A and upgrading tower B have rare nitric acid inlet.Spray header 1 is arranged at upgrading tower A and upgrading tower B top.Vapour outlet is arranged at upgrading tower A and upgrading tower B top.The back of concentrating nitric acid outlet is arranged at upgrading tower A and upgrading tower B bottom, and the concentrated back nitric acid outlet of upgrading tower A connects interchanger A, and interchanger A has pipeline to connect pump (5).Pump (5) connects rare nitric acid inlet of upgrading tower B.Upgrading tower B outlet at bottom is connected with the concentrated nitric acid jar, and the nitric acid that come out in upgrading tower B bottom after concentrating is collected in the concentrated nitric acid jar.The vapour outlet of upgrading tower A connects the tower bottom reboiler of upgrading tower B, and the tower bottom reboiler of upgrading tower B (8) outlet connects the inlet of interchanger B.The outlet of interchanger B connects wastewater collection jar (6).The vapour outlet of upgrading tower B connects water cooler (10) inlet, and water cooler (10) outlet connects wastewater collection jar (6).Rare nitric acid outlet of interchanger A connects rare nitric acid inlet of interchanger B.Rare nitric acid outlet of interchanger B connects rare nitric acid inlet of upgrading tower A.
2, since improved hexanodioic acid produce in rare nitric acid concentrating unit, its technical process is also corresponding to obtain corresponding change.Rare nitric acid concentration technology flow process was as follows during hexanodioic acid after the improvement was produced:
The concentration that produces from a plurality of operations such as enrichment device, whizzer and gas absorption, catalyst recovery in the hexanodioic acid production is about rare nitric acid of 20-30%, at first enters interchanger A (4).Concentration is about the rare nitric acid of 20-30% and the spissated nitric acid heat exchange of coming out in upgrading tower A bottom of process, improves the temperature of rare nitric acid for the first time; Rare nitric acid passes through interchanger B (7) again, steams wastewater heat exchange with upgrading tower B tower bottom reboiler (8) comes out, enters the nitric acid inlet that tower concentrates A after improving the temperature of rare nitric acid for the second time.After the concentrated A of tower concentrated, what the concentrated A of tower came out the bottom was concentrated into 35-40% through spissated nitric acid.The nitric acid that is concentrated into 35-40% is after rare nitric acid heats through interchanger 4, squeezes into the nitric acid inlet of upgrading tower B with pump (5).In upgrading tower B, rare nitric acid of 35-40% enters into upgrading tower B to be continued to concentrate, and, collects in the concentrated nitric acid storage tank at upgrading tower B bottom discharge through spissated nitric acid.
The steam that upgrading tower A evaporated on top is come out enters the interior tower bottom reboiler inlet of tower of upgrading tower B bottom.The steam that upgrading tower A evaporated on top is come out provides boiling hot energy for upgrading tower B again.After the steam that upgrading tower B evaporated on top is come out enters water cooler (10), collect in the wastewater collection jar (6).
The steam condensate of last upgrading tower A and upgrading tower B is collected in the storage tank, feeder Sewage treatment systems or carried out depickling and handle before entering sewage disposal.
The operating pressure of upgrading tower A is 0.01～0.06Mpa; Working temperature is 100-140 ℃; Inner liquid level is 20%-80%; It is 70-100 ℃ that rare nitric acid enters temperature; Cat head spray water flow is 1-10m
3/ h.
The operating pressure of upgrading tower B is little negative pressure ,-0.2--0.1Mpa; Working temperature is 30～140 ℃; Inner liquid level is 20%～80%; Cat head spray water flow is 1-10m
3/ h.
The rare nitric acid inlet of upgrading tower A is located at upgrading tower A the 3rd or 5 layers of tower tray place, and the rare nitric acid through improving temperature for twice enters upgrading tower A from rare nitric acid inlet of upgrading tower A the 3rd or 5 layers of tower tray.
Concentrating the cat head spray water is the hot mother liquor water of device, is the sour water of separating in the hexanodioic acid aqueous solution inspissation process.
Beneficial effect of the present invention: rare nitric acid concentration technique has not only been improved rare nitric acid concentrating unit in the hexanodioic acid production in the hexanodioic acid production of the present invention, but also changed the spissated technology of rare nitric acid in the hexanodioic acid production, adopt two concentration techniques to improve the water yield steam capability of rare nitric acid in concentrating effectively, the product that adopts interchanger that upgrading tower is discharged, thermal source as rare nitric acid, save steam consumption and reduce quantity of wastewater effluent, saved energy-output ratio in the production.
Rare nitric acid concentrating unit and technology have bigger improvement in the above-mentioned hexanodioic acid production of the present invention, rare nitric acid in the hexanodioic acid production are concentrated meet the needs of hexanodioic acid production and have produced energy-saving and cost-reducing and reduce the effect of sewage discharge.It is a new and innovative, progressive, practical new design.
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
Description of drawings
Fig. 1 is rare nitric acid concentrating unit and a process route view during hexanodioic acid of the present invention is produced.
Fig. 2 is rare nitric acid concentrating unit and a process route view during former hexanodioic acid is produced.
Among the figure, 1. spray header, 2. upgrading tower A, 3. tower bottom reboiler, 4. interchanger A, 5. pump, 6. storage tank, 7. interchanger B, 8. tower bottom reboiler, 9. upgrading tower B, 10. water cooler.
Embodiment
Embodiment: consult accompanying drawing 1.Rare nitric acid concentrating unit during hexanodioic acid of the present invention is produced, the diameter of upgrading tower A and upgrading tower B is 4 meters, highly is 22 meters.There are 25 layers of tower tray inside.Upgrading tower A and upgrading tower B have rare nitric acid inlet.Spray header 1 is arranged at upgrading tower A and upgrading tower B top.Vapour outlet is arranged at upgrading tower A and upgrading tower B top.The back of concentrating nitric acid outlet is arranged at upgrading tower A and upgrading tower B bottom, concentrates back nitric acid outlet and connects interchanger A, and interchanger A has pipeline to connect pump (5).Pump (5) is an impeller pump.Interchanger A and interchanger B are shell and tube.Pump (5) connects rare nitric acid inlet of upgrading tower B.The vapour outlet of upgrading tower A connects the tower bottom reboiler of upgrading tower B, and the tower bottom reboiler of upgrading tower B (8) outlet connects the inlet of interchanger B.The outlet of interchanger B connects wastewater collection jar (6).The vapour outlet of upgrading tower B connects water cooler (10) inlet, and water cooler (10) outlet connects wastewater collection jar (6).Come out at the bottom of the upgrading tower B tower concentrate after nitric acid collect in the concentrated nitric acid jar.Rare nitric acid outlet of interchanger A connects rare nitric acid inlet of interchanger B.Rare nitric acid outlet of interchanger B connects rare nitric acid inlet of upgrading tower A.
The processing method that is adopted is as follows: rare nitric acid of the concentration 15%～30% that produces from a plurality of operations such as enrichment device, whizzer and gas absorption, catalyst recovery during hexanodioic acid is produced at first enters interchanger A (4).Concentration is about the spissated nitric acid heat exchange of coming out in rare nitric acid of 15%～30% and upgrading tower A bottom of process, improves the temperature of rare nitric acid for the first time; Rare nitric acid passes through interchanger B (7) again, and the concentrated nitric acid heat exchange of coming out with upgrading tower B tower bottom reboiler (8) improves the nitric acid inlet that enters upgrading tower A after the temperature of rare nitric acid for the second time.After upgrading tower A concentrated, what upgrading tower A came out the bottom was concentrated into 30%～40% through spissated nitric acid.Be concentrated into 30%～40% nitric acid through interchanger 4 for rare nitric acid heating after, the nitric acid of squeezing into upgrading tower B with pump (5) enters the mouth.In upgrading tower B, rare nitric acid of 30%～40% enters into upgrading tower B and continue to concentrate, from upgrading tower B come out concentrate after nitric acid collect the concentrated nitric acid storage tank.
The steam that upgrading tower A evaporated on top is come out enters the interior tower bottom reboiler inlet of tower of upgrading tower B bottom.The steam that upgrading tower A evaporated on top is come out provides boiling hot energy for upgrading tower B again.After the steam that upgrading tower B evaporated on top is come out enters water cooler (10), collect in the wastewater collection jar (6).
Sewage treatment systems or before entering sewage disposal, carry out depickling and handle.
The rare nitric acid concentration technology parameter that adopts is:
The operating pressure of upgrading tower A is 0.15Mpa; Working temperature is 130 ℃; Inner liquid level is 40%; It is 85 ℃ that rare nitric acid enters temperature; Cat head spray water flow is 5m
3/ h.
The operating pressure of upgrading tower B is negative 0.05Mpa; Working temperature is 50 ℃; Inner liquid level is 40%; Cat head spray water flow is 5m
3/ h.
Rare nitric acid inlet of upgrading tower A is located at upgrading tower A the 3rd or 5 layers of tower tray place, and rare nitric acid of twice raising temperature enters upgrading tower A from rare nitric acid inlet of upgrading tower A the 3rd tower tray.
Adipic acid plant, adopt above-mentioned measure to improve technical process after, realize producing 140000 tons per year, increased the target of production capacity, save energy, minimizing sewage.
About 15 tons/hour of spray water.
The production equipment of producing 140000 tons of hexanodioic acids per year adopt this technology can save steam 8-15 ton/hour, reduce 200 tons/hour of sewage discharges.
Claims (1)
1. rare nitric acid concentration method during a hexanodioic acid is produced, it is characterized in that: the equipment of employing is by upgrading tower A (2), upgrading tower B (9), and interchanger, pump and pipeline are formed, the diameter of upgrading tower A (2) and upgrading tower B (9) is 4 meters, highly be 22 meters, there are 25 layers of tower tray inside, upgrading tower A (2) and upgrading tower B (9) have rare nitric acid inlet, spray header (1) is arranged at upgrading tower A (2) and upgrading tower B (9) top, vapour outlet is arranged at upgrading tower A (2) and upgrading tower B (9) top, the back of concentrating nitric acid outlet is arranged at upgrading tower A (2) and upgrading tower B (9) bottom, concentrate back nitric acid outlet and connect interchanger A (4), interchanger A (4) has pipeline to connect pump (5), pump (5) is an impeller pump, interchanger A (4) and interchanger B are shell and tube, pump (5) connects rare nitric acid inlet of upgrading tower B (9), the vapour outlet of upgrading tower A (2) connects the tower bottom reboiler (8) of upgrading tower B (9), tower bottom reboiler (8) outlet of upgrading tower B (9) connects the inlet of interchanger B (7), the outlet of interchanger B (7) connects wastewater collection jar (6), the vapour outlet of upgrading tower B (9) connects water cooler (10) inlet, water cooler (10) outlet connects wastewater collection jar (6), come out at the bottom of upgrading tower B (9) tower concentrate after nitric acid collect in the concentrated nitric acid jar, rare nitric acid outlet of interchanger A (4) connects rare nitric acid inlet of interchanger B (7), and rare nitric acid outlet of interchanger B (7) connects rare nitric acid inlet of upgrading tower A (2);
The concentration method that adopts is: rare nitric acid of the concentration 15%～30% that produces from enrichment device, whizzer and gas absorption, catalyst recovery operation during hexanodioic acid is produced, at first enter interchanger A (4), concentration is the spissated nitric acid heat exchange of coming out in 15%～30% rare nitric acid and upgrading tower A (2) bottom of process, improves the temperature of rare nitric acid for the first time; Rare nitric acid passes through interchanger B (7) again, the concentrated nitric acid heat exchange of coming out with upgrading tower B (9) tower bottom reboiler (8), improve for the second time the nitric acid inlet that enters upgrading tower A (2) after the temperature of rare nitric acid, after upgrading tower A (2) concentrates, what upgrading tower A (2) came out the bottom is concentrated into 30%～40% through spissated nitric acid, be concentrated into 30%～40% nitric acid through interchanger A (4) for rare nitric acid heating after, squeeze into the nitric acid inlet of upgrading tower B (9) with pump (5), in upgrading tower B (9), rare nitric acid of 30%～40% enters into upgrading tower B (9) and continue to concentrate, from upgrading tower B (9) come out concentrate after nitric acid collect the concentrated nitric acid storage tank;
The steam that upgrading tower A (2) evaporated on top is come out enters interior tower bottom reboiler (8) inlet of tower of upgrading tower B (9) bottom, the steam that upgrading tower A (2) evaporated on top is come out is that upgrading tower B (9) provides boiling hot energy again, after the steam that upgrading tower B (9) evaporated on top is come out enters water cooler (10), collect in the wastewater collection jar (6);
The rare nitric acid concentration technology parameter that adopts is:
The operating pressure of upgrading tower A (2) is 0.15MPa; Working temperature is 130 ℃; Inner liquid level is 40%; It is 85 ℃ that rare nitric acid enters temperature; Cat head spray water flow is 5m
3/ h;
The operating pressure of upgrading tower B (9) is negative 0.05MPa; Working temperature is 50 ℃; Inner liquid level is 40%; Cat head spray water flow is 5m
3/ h;
Rare nitric acid inlet of upgrading tower A (2) is located at the 3rd layer of tower tray place of upgrading tower A (2), and rare nitric acid of twice raising temperature enters upgrading tower A (2) from rare nitric acid inlet of upgrading tower A (2) the 3rd tower tray.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610114723XA CN101190784B (en) | 2006-11-22 | 2006-11-22 | Method for concentrating dilute nitric acid in adipic acid production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610114723XA CN101190784B (en) | 2006-11-22 | 2006-11-22 | Method for concentrating dilute nitric acid in adipic acid production |
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| Publication Number | Publication Date |
|---|---|
| CN101190784A CN101190784A (en) | 2008-06-04 |
| CN101190784B true CN101190784B (en) | 2010-08-11 |
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ID=39486008
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200610114723XA Active CN101190784B (en) | 2006-11-22 | 2006-11-22 | Method for concentrating dilute nitric acid in adipic acid production |
Country Status (1)
| Country | Link |
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| CN (1) | CN101190784B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1076025A (en) * | 1964-07-09 | 1967-07-19 | Gnii Pi Azotnoj | Mehtod for purifying nitric acid |
| CN1119624A (en) * | 1994-12-09 | 1996-04-03 | 门伟 | Method for producing concentrated nitric acid |
| CN1454181A (en) * | 2000-05-22 | 2003-11-05 | Qvf工程有限公司 | Method for producing concentrated nitric acid and installation for carrying out a method of this type |
| CN1487914A (en) * | 2001-01-25 | 2004-04-07 | ������������ʽ���� | Process for producing alkanedicarboxylic acid |
-
2006
- 2006-11-22 CN CN200610114723XA patent/CN101190784B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1076025A (en) * | 1964-07-09 | 1967-07-19 | Gnii Pi Azotnoj | Mehtod for purifying nitric acid |
| CN1119624A (en) * | 1994-12-09 | 1996-04-03 | 门伟 | Method for producing concentrated nitric acid |
| CN1454181A (en) * | 2000-05-22 | 2003-11-05 | Qvf工程有限公司 | Method for producing concentrated nitric acid and installation for carrying out a method of this type |
| CN1487914A (en) * | 2001-01-25 | 2004-04-07 | ������������ʽ���� | Process for producing alkanedicarboxylic acid |
Non-Patent Citations (6)
| Title |
|---|
| JP平2-59409A 1990.02.28 |
| JP特开2004-250294A 2004.09.09 |
| 赵铎等.硝酸浓缩塔节能工艺.河南化工 3.2003,(3),第27页左栏第1行至右栏第23行. |
| 赵铎等.硝酸浓缩塔节能工艺.河南化工 3.2003,(3),第27页左栏第1行至右栏第23行. * |
| 郝翠冉等.浅谈硝酸浓缩塔的设计、安装及维护.化工设备与管道40 4.2004,40(4),15-18. |
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