CN1083294C - Method for reducing influence on evaporation post of caprolactam during regeneration of ion exchange resin - Google Patents
Method for reducing influence on evaporation post of caprolactam during regeneration of ion exchange resin Download PDFInfo
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- CN1083294C CN1083294C CN99115316A CN99115316A CN1083294C CN 1083294 C CN1083294 C CN 1083294C CN 99115316 A CN99115316 A CN 99115316A CN 99115316 A CN99115316 A CN 99115316A CN 1083294 C CN1083294 C CN 1083294C
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- China
- Prior art keywords
- caprolactam
- ion exchange
- tower
- water solution
- nitrogen
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- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 50
- 238000001704 evaporation Methods 0.000 title claims abstract description 24
- 230000008020 evaporation Effects 0.000 title claims abstract description 23
- 230000008929 regeneration Effects 0.000 title claims abstract description 14
- 238000011069 regeneration method Methods 0.000 title claims abstract description 14
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 title claims abstract description 8
- 239000003456 ion exchange resin Substances 0.000 title claims abstract description 8
- 229920003303 ion-exchange polymer Polymers 0.000 title claims abstract description 8
- 238000005342 ion exchange Methods 0.000 claims abstract description 58
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- AWSFEOSAIZJXLG-UHFFFAOYSA-N azepan-2-one;hydrate Chemical compound O.O=C1CCCCCN1 AWSFEOSAIZJXLG-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 27
- 230000000694 effects Effects 0.000 claims abstract description 9
- 230000001172 regenerating effect Effects 0.000 abstract description 4
- 230000018044 dehydration Effects 0.000 abstract description 2
- 238000006297 dehydration reaction Methods 0.000 abstract description 2
- 238000004904 shortening Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 3
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000003643 water by type Substances 0.000 description 5
- 239000002699 waste material Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
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- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention relates to a method for reducing the influence on the triple effect evaporation post of caprolactam when regenerating ion exchange resin, which is used for the regeneration of the ion exchange resin for refining caprolactam, the caprolactam water solution in an ion exchange tower is ejected by process water, and the process water is ejected by the caprolactam water solution, and is characterized in that the caprolactam water solution and the process water in the ion exchange tower are ejected by nitrogen, the pressure of the nitrogen is 0.2-0.6Mpa, and the flow is 5-10 cubic meters per hour. The invention can effectively prevent the problems that the concentration of caprolactam becomes thin due to dehydration and caprolactam removal aqueous solution during regeneration of an ion exchange post, evaporation fluctuation is generated due to evaporation and flashing of a tower, and a large amount of caprolactam flows out along with the entrainment of top steam, thereby saving a large amount of process water and greatly shortening the regeneration operation time.
Description
The present invention relates to a kind of method to hexanolactam evaporation post influence when reducing ion exchange resin regeneration.
Refined caprolactam has a variety of methods, wherein has a kind of method to need ion exchange tower to do a post and comes refined caprolactam.As shown in Figure 1: Fig. 1 is the former process flow diagram in ion-exchange post, among the figure: 1-ion exchange tower, 2-ion exchange tower, 3-ion exchange tower, 4,5,6,7,11-quick-closing valve, 8-dashpot, 9-dashpot, 10-caprolactam water solution pipeline, 12-waste line, 13-pump, 14-caprolactam water solution pipeline, 15-caprolactam water solution pipeline, 16-wastewater disposal basin, 19,20-stopping valve, 22-process water pipeline.There are two cover ion exchange towers in this post, and tower 1, tower 2, tower 3 are formed first cover, form second cover by three towers in addition.Suppose that now the second cover ion exchange tower is in the operation running status, it is standby after the first cover ion exchange tower need be regenerated, the regenerated purpose is to clean up for the organic and inorganic impurity the resin absorption of ion-exchange, the first two step of regenerating is to be enclosed within after the operation in order to deviate from first, switches under the stand-by state caprolactam water solution in the retention tower.Open stopping valve 19 on the pipeline 22, with 15 cubic metres of/hour process waters from tower 1 overhead stream through tower 2, tower 3, open fast shut-off valve during 4,120 minutes in the ion exchange tower caprolactam water solution by warp let-off dashpot 8.After 120 minutes, same 15 cubic metres of/hour process water Continuous Flow are through tower 1, tower 2 and tower 3, and caprolactam water solution is by in the warp let-off dashpot 9 in the ion exchange tower during 360 minutes, and ion exchange tower removes caprolactam water solution and finishes.Three steps are to stay process water in the tower when deviating to regenerate behind the ion exchange tower regenerated.The first step in three steps of back: quick-closing valve 11 on the 30wt% caprolactam water solution pipeline 10 that advances tower 1 is opened, simultaneously, also open leading on wastewater disposal basin 16 pipelines 12 quick-closing valve 7, by pump 13 the 30wt% caprolactam water solution is sent into tower 1 with 10 cubic metres/hour from hexanolactam dashpot 8, flow through tower 2, tower finishes after 3,30 minutes.Second step: close quick-closing valve 7, open 6,10 cubic metres of/hour caprolactam water solutions of quick-closing valve that lead on caprolactam water solution dashpot 9 discharge line 14 and send into tower 1, the tower 2 of flowing through, tower entered dashpot 9 to caprolactam water solution during 3,60 minutes.The 3rd step: close quick-closing valve 6, open the quick-closing valve 4 that leads on dashpot 8 pipelines 15, keep 10 cubic metres of/hour caprolactam water solutions to send into tower 1, the tower 2 of flowing through, tower 3,80-90 minute, stop into caprolactam water solution, remove the interior process water of tower and finish.Aforesaid method exists shortcoming to have: this method uses process water to eject, according to material properties, hexanolactam and water dissolve each other, feed like this process water in tower after, caprolactam water solution is at once thinning, after caprolactam water solution concentration was thinning, influence is operation triple effect evaporation post charging caprolactam concentration down.Because caprolactam concentration is thinning, the easy general tower in triple effect evaporation post and produce fluctuation, a large amount of hexanolactams have been carried secretly away with water vapour from the top.And last tower discharging caprolactam concentration does not reach processing requirement on the contrary from the triple effect evaporation post.Not only waste hexanolactam, and loss steam, a large amount of process waters also wasted.The ultimate analysis ion exchange tower includes hexanolactam or higher, can not thoroughly remove hexanolactam in the ion exchange tower.Dewater with aforesaid method, yet exist because of hexanolactam and dissolve each other with water, can not be with caprolactam water solution thoroughly difficulties such as process water in the ion exchange tower eject, a part of process water dissolves each other with the caprolactam water solution of coming in the ion exchange tower, and process water is stayed in the tower, make charging caprolactam concentration in triple effect evaporation post thinning, and then evaporation operation produce fluctuation.Also caprolactam water solution is discharged to wastewater disposal basin 16 with this method in addition, not only waste hexanolactam, and the required time is longer: also limited because of dashpot 9 reserves sometimes, the caprolactam water solution that enters dashpot 9 has to directly enter wastewater disposal basin 16, cause the COD (chemical oxygen demand) of wastewater disposal basin 16 higher, wastewater flow rate increases, and brings difficulty to environment-friendly processing unit.
When the objective of the invention is to prevent effectively the regeneration of ion-exchange post, it is thinning and cause the fluctuation of this post to advance triple effect evaporation post caprolactam water solution, prevent that effectively hexanolactam enters wastewater disposal basin 16 in the ion exchange tower, and save a large amount of process waters, shorten regeneration and produce required time.The wastewater disposal basin wastewater flow rate reduces in a large number, reduces waste water COD (chemical oxygen demand).
When the present invention is achieved in that ion exchange tower regeneration, the first two step ejects caprolactam water solution in the ion exchange tower, former used process water changes nitrogen into and ejects caprolactam water solution, 0.2-0.6Mpa nitrogen enters ion exchange tower 1 top, flow through tower 2, tower 3 by stopping valve 17 control nitrogen flows, rate of flow meter 18 be the 5-10 cubic meter/hour, caprolactam water solution in three towers of ion-exchange thoroughly removed in 60-80 minute.Remove the process water of retaining when regenerating in the ion exchange tower, also replace caprolactam water solution with nitrogen, 0.2-0.6Mpa nitrogen enters ion exchange tower 1 top, the tower 2 of flowing through, tower 3, process water in the ion exchange tower is ejected with nitrogen, process water in the ion exchange tower pushed up in 60-80 minute.
Concrete processing step is as follows:
One, ejects caprolactam water solution concrete steps in the ion exchange tower: as shown in Figure 2, Fig. 2 is that the back process flow diagram is improved in ion-exchange of the present invention post, among the figure: 1-ion exchange tower, 2-ion exchange tower, 3-ion exchange tower, 4,5,6,7,11-quick-closing valve, 8-dashpot, 9-dashpot, 10-caprolactam water solution pipeline, 12-waste line, 13-pump, 14-caprolactam water solution pipeline, 15-caprolactam water solution pipeline, 16-wastewater disposal basin, 17,19,20-stopping valve, 18-under meter, 21-nitrogen pipeline, 22-process water pipeline.Close into ion exchange tower process water stopping valve 19, open stopping valve 17 on the nitrogen pipeline 21, open quick-closing valve 4,5-10 cubic meter/hour nitrogen from ion exchange tower 1 overhead stream through tower 2 and tower 3, caprolactam water solution in the ion exchange tower is entered dashpot 8,60-80 minute, just can thoroughly remove caprolactam water solution in three ion exchange towers.Close stopping valve 17 on the nitrogen pipeline 21, stop into nitrogen, eject caprolactam water solution with nitrogen and finish.
Two, ion exchange tower dehydration concrete steps: close quick-closing valve 11 preceding stopping valve 20, open quick-closing valve 7, stopping valve 17 on the nitrogen pipeline 21 is opened, process water in the ion exchange tower is entered wastewater disposal basin 16 by quick-closing valve 7, process water had been pushed up in 60-80 minute, close stopping valve 17 on the nitrogen pipeline 21, stop into nitrogen, remove with nitrogen that process water finishes in the tower.
Positively effect of the present invention is to prevent effectively ion-exchange post when regeneration removing process water, remove caprolactam water solution and cause that caprolactam concentration is thinning, causes the general tower in evaporation post, and produces the evaporation fluctuation.A large amount of hexanolactams is carried loss secretly with the upper water steam, can save a large amount of process waters.Each shortening of regenerative operation time 8 hours can reduce caprolactam water solution inflow wastewater disposal basin 16 in the ion exchange tower, reduces wastewater flow rate, reduces waste water COD (chemical oxygen demand), thereby alleviates the environmental protecting device operating load.
From 50,000 tons of production equipments,, obtain following data through repeatedly calculating from the production test data statistics:
Regeneration times was 5 times in every month, lost 4 cubic metres of hexanolactams at every turn.
Be 12 months every year, 12
*5
*4=240 cubic meter hexanolactam, per ton is 10,000 yuan, 2,400,000 yuan of annual saving.
Each process water of saving is: 8 hours
*15 cubic metres/hour=120 cubic metres
Every month be: 5
*The 120=600 cubic meter
The annual water rate of saving: 600 cubic metres/month
*December
*4 yuan/cubic metre=28800 yuan
Embodiment 1:1, by preceding mask body processing step: 5 cubic metres of/hour nitrogen (pressure is 0.3Mpa), enter ion exchange tower 1, flow through tower 2 and tower 3, just can thoroughly remove caprolactam water solution in the ion exchange tower in 80-90 minute, evaporating post hexanolactam input concentration by analysis is 29.3wt% (processing requirement is 30wt%).Ion exchange tower 1, tower 2 and tower 3 carry out removing process water by concrete processing step noted earlier, feed 5 cubic metres/hour of nitrogen (pressure is 0.3Mpa), just can thoroughly remove process water in the ion exchange tower, and discharge nitrogen then in 80-90 minute.After putting into operation, analyzing evaporation post caprolactam concentration is 29.2wt%.It is 0.02wt% that three overhead condensation liquid of analysis evaporation contain hexanolactam.Ion-exchange post wastewater disposal basin COD (chemical oxygen demand) is 2356mg/h, being drained into ion-exchange wastewater disposal basin 16 process waters, to contain hexanolactam be 0.2wt%, test data before the present invention is: get a monthly average value, evaporation post charging caprolactam concentration is 21.8wt%, it is 8.58wt% that analysis evaporation top, post phlegma contains hexanolactam, the COD of ion-exchange wastewater disposal basin 16 (chemical oxygen demand) is 8219mg/h, and the ion-exchange wastewater disposal basin contains hexanolactam 4.15wt%.
Embodiment 2: the same with embodiment 1, nitrogen flow is controlled to be 10 cubic metres/hour (pressure is 0.6Mpa), and after 30-40 minute, caprolactam water solution thoroughly removes in three towers of ion exchange tower, and analyzing evaporation post input concentration is 29.1wt%.Ion exchange tower 1, tower 2 and tower 3 be by embodiment 1 removing process water noted earlier, feeds after the nitrogen (pressure is 0.6Mpa) 30-40 minute, and the ion exchange tower process water thoroughly removes.Discharge after the nitrogen, put into operation, analyzing evaporation post caprolactam concentration is 29.2wt%, and analyzing evaporation top, post phlegma, to contain hexanolactam be 0.02wt%, and being drained into ion-exchange post wastewater disposal basin process water, to contain hexanolactam be 0.58wt%.Ion-exchange wastewater disposal basin waste water COD (chemical oxygen demand) is 2570mg/l.
Claims (2)
- One kind when reducing ion exchange resin regeneration to the method for hexanolactam triple effect evaporation post influence, when being used for the ion exchange resin regeneration of refined caprolactam, it is characterized in that replacing the process water of original use to eject caprolactam water solution in the ion exchange tower, replace the original caprolactam water solution that uses to eject process water in the ion exchange tower with nitrogen with nitrogen.
- 2. according to claim 1 a kind of when reducing ion exchange resin regeneration to the method for hexanolactam triple effect evaporation post influence, it is characterized in that used nitrogen pressure is 0.2MPa-0.6MPa, flow be the 5-10 cubic meter/hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99115316A CN1083294C (en) | 1999-04-02 | 1999-04-02 | Method for reducing influence on evaporation post of caprolactam during regeneration of ion exchange resin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN99115316A CN1083294C (en) | 1999-04-02 | 1999-04-02 | Method for reducing influence on evaporation post of caprolactam during regeneration of ion exchange resin |
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| Publication Number | Publication Date |
|---|---|
| CN1247774A CN1247774A (en) | 2000-03-22 |
| CN1083294C true CN1083294C (en) | 2002-04-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN99115316A Expired - Fee Related CN1083294C (en) | 1999-04-02 | 1999-04-02 | Method for reducing influence on evaporation post of caprolactam during regeneration of ion exchange resin |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111068361B (en) * | 2018-10-22 | 2022-02-11 | 中国石油化工股份有限公司 | Caprolactam ion exchange device and regeneration method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02222769A (en) * | 1989-02-27 | 1990-09-05 | Hitachi Plant Eng & Constr Co Ltd | Method and apparatus for two stage reverse osmosis treatment of water |
| JPH05188184A (en) * | 1992-01-13 | 1993-07-30 | Toshiba Corp | Resin regenerating device of condensing and desalting apparatus |
| JPH06106165A (en) * | 1992-09-30 | 1994-04-19 | Toshiba Corp | Condensed water desalting device |
-
1999
- 1999-04-02 CN CN99115316A patent/CN1083294C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02222769A (en) * | 1989-02-27 | 1990-09-05 | Hitachi Plant Eng & Constr Co Ltd | Method and apparatus for two stage reverse osmosis treatment of water |
| JPH05188184A (en) * | 1992-01-13 | 1993-07-30 | Toshiba Corp | Resin regenerating device of condensing and desalting apparatus |
| JPH06106165A (en) * | 1992-09-30 | 1994-04-19 | Toshiba Corp | Condensed water desalting device |
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| Publication number | Publication date |
|---|---|
| CN1247774A (en) | 2000-03-22 |
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Granted publication date: 20020424 Termination date: 20170402 |