CN101190893B - System and method for purifying crude caprolactam water solution - Google Patents
System and method for purifying crude caprolactam water solution Download PDFInfo
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- CN101190893B CN101190893B CN2006101604235A CN200610160423A CN101190893B CN 101190893 B CN101190893 B CN 101190893B CN 2006101604235 A CN2006101604235 A CN 2006101604235A CN 200610160423 A CN200610160423 A CN 200610160423A CN 101190893 B CN101190893 B CN 101190893B
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Abstract
The invention relates to a system and a method of purifying crude caprolactam solution. The system comprises (A) a filtering area, in which resin is utilized to filter out ionic impurities, (B) a detecting unit used for judging whether the solution filtered by the resin conforms to preset detecting standard, (C) a purifying area used for concentrating the solution that is filtered and conforms topreset detecting standard and (D) a first temporary storage device used for receiving and storing the solution that is filtered and is unqualified for preset detecting standard and also used for mixingsolution therein with unfiltered crude caprolactam solution and leading the mixture to the filtering area once again. Continuous filtering is available to the system, thereby reducing operation chang ing frequency of the resin, having no final unqualified caprolactam and prolonging effective operation period of the resin device for filtering out ionic impurity; the system has the advantage of saving material and reducing waste.
Description
Technical field
The present invention relates to a kind of equipment of purifying crude caprolactam water solution, particularly utilize the equipment of Di purifying crude caprolactam water solution.
Background technology
At industrial manufacturing hexanolactam is under the oleum catalytic condition, make cyclohexanone-oxime carry out Beckmann rearrangement and generate hexanolactam, the mixed aqueous solution that will contain oleum and hexanolactam after the rearrangement reaction neutralizes with ammoniacal liquor, produce ammonium sulfate, separation and purification ammonium sulfate and crude amide again.Usually, carry out the extraction first time with organic solvent-benzene earlier, utilize water to carry out the extraction second time again, from organic solvent, disengage hexanolactam, and in reextraction, form the crude caprolactam water solution that contains 30 to 40% hexanolactams.
Because hexanolactam is the important source material of synthesizing polyamides, this kind crude caprolactam water solution need be further purified, and can reach the polyamide raw materials requirement of high purity.The purification process of multiple manufacturing high purity caprolactam has been proposed at present, for example recrystallize purifying, ion exchange resin, distillation etc., wherein, ion exchange resin has the effect that is quite showing for the salt impurity of removing in the crude caprolactam water solution.
Fig. 5 illustrates a kind of method of purifying crude caprolactam.At first, contain 30 to 40% hexanolactams, water, and the crude caprolactam water solution of impurity import the Di 110 that comprises resin anion(R.A) post and cationic resin column through pipeline 10, removal salt impurity.Then, import evaporation unit 210 formation concentration through pipeline 12 and be higher than 80% high density hexanolactam, and import snubber assemblys 220 through pipeline 14.Then, through pipeline 16 this high density caprolactam water solution is imported water distilling apparatus 230 and remove moisture formation high purity caprolactam finished product, derive by pipeline 18 again.
When utilizing ion exchange resin to filter crude caprolactam water solution, must be in resin device outlet carrying out aqueous solution quality examination, confirm that the aqueous solution behind the ion exchange resin filtration, purification has reached the certain quality requirement, can meet required purity rubric to guarantee the final hexanolactam finished product that forms.The 290nm absorption value (EXT.290) of general using basicity analytical value (ALK.) and industrial hexanolactam is as the aqueous assay standard behind the filtration, purification.When aqueous assay value EXT.290 after filtering purification and ALK. surpass examination criteria, can cause the hexanolactam final product quality rapid drawdown of back segment distillation output, can't meet EXT.290 less than 0.05 hexanolactam finished product standard, therefore must before detected value EXT.290 or ALK. surpass examination criteria, carry out resin and change operation.Usually, behind a certain amount of crude caprolactam water solution of purifying treatment, the aqueous solution quality examination value of this Di outlet can rise sharply near or surpass resin and change standard value, must suspend scavenging process, carry out resin and change operation.
Yet, find through test, the aqueous solution quality examination value of this Di outlet rise sharply near or surpass resin and change standard value after, can descend and return near the preceding numerical range that rises sharply, and change under the numerical range of standard surpassing resin, one period considerable time of this detections numerical value experience presents steadily slowly rising.In other words, when utilizing resin to carry out the purifying treatment of crude caprolactam water solution, the detected value of resin device outlet rise sharply near or surpass resin replacing standard after, still can operate one period considerable time effectively, form the caprolactam water solution that meets the certain mass requirement.And currently used ion exchange resin purifying treatment method for avoiding finally forming non-compliant hexanolactam product, promptly carries out resin usually and changes operation before detected value rises sharply.Frequent resin is changed reproducer, need expend a large amount of acid, alkali and water, and can produce a large amount of waste water with pending.
In view of this, how to prolong effective running time of Di group, finally can not generate underproof hexanolactam finished product, and reduce resin and change spent acid, alkali, the water and wastewater produced of reproducer, be a technical problem that needs to be resolved hurrily.
Summary of the invention
The purpose of this invention is to provide and a kind ofly can prolong the equipment that Di effectively operates the purifying crude caprolactam water solution of time.
Another purpose of the present invention provides a kind of equipment that can avoid generating the purifying crude caprolactam water solution of defective hexanolactam finished product.
A further object of the present invention provides a kind of equipment that can save the purifying crude caprolactam water solution of the employed material of resin regeneration.
Another purpose of the present invention provides a kind of equipment that can reduce the purifying crude caprolactam water solution of the waste material that resin regeneration produces.
For reaching above-mentioned and other purpose, the invention provides a kind of equipment of purifying crude caprolactam water solution, comprise (A) filtrating area, be provided with resin filter device group, in order to filter the ionic impurity of removing in this crude caprolactam water solution, form filtered caprolactam water solution; Whether (B) detecting unit meets the preset detection standard in order to judge filtered caprolactam water solution; (C) zone purification is in order to receive after filtration and to meet the caprolactam water solution of predetermined detection standard and carry out the concentrated and purified formation hexanolactam finished product of caprolactam water solution; And (D) first apparatus for temporary storage, store after filtration but do not reach the caprolactam water solution of predetermined detection standard yet in order to receive, this aqueous solution that is stored in first apparatus for temporary storage with import this filtrating area again after the crude caprolactam water solution of filtered mixes.This equipment can filter constantly, reduces the number of times that resin is changed operation, and finally can not generate underproof hexanolactam finished product, thereby can prolong effective running time of this Di, has the material of saving and subtracts useless advantage.
The present invention provides a kind of method of purifying crude caprolactam water solution again, comprise the following steps: that (a) imports filtrating area with pending crude caprolactam water solution, the resin filter device group that utilization is located in the filtrating area is filtered the ionic impurity of removing in this crude caprolactam water solution, forms filtered caprolactam water solution; (b) detect this filtered caprolactam water solution of judgement and whether meet the preset detection standard; (c1) will detect and judge that the caprolactam water solution meet the predetermined detection standard imports the concentrated and purified formation hexanolactam finished product that caprolactam water solution is carried out in the zone purification; And (c2) will detect and judge that the caprolactam water solution do not reach the predetermined detection standard imports and is stored in first apparatus for temporary storage, and carry out step (a) again after making this caprolactam water solution that is stored in first apparatus for temporary storage and the crude caprolactam water solution of filtered mixing.
Description of drawings
Figure 1A to 1C illustrates the embodiment of the invention 1;
Fig. 2 is the graphic representation of quality examination value of the resin device group operation of the embodiment of the invention 1;
Fig. 3 illustrates the embodiment of the invention 2;
Fig. 4 illustrates the embodiment of the invention 3; And
Fig. 5 explanation becomes known for the equipment flowsheet of purifying crude caprolactam water solution.
[primary clustering nomenclature]
100 filtrating areas
110 Di groups
100a, 100b Di
112,114,116 resin columns
130 detecting units
150 hydrogenation apparatuss
200 zone purifications
210 evaporation units
220 snubber assemblys
230 water distilling apparatus
300 first apparatus for temporary storage
400 second install temporarily
10,11,12,14,16,18,20,22,24,26,28 pipelines
Embodiment
Below be to describe purpose of the present invention and effect in detail by embodiment.
Figure 1A illustrates embodiments of the invention 1.Equipment of the present invention comprises filtrating area 100, detecting unit 130, zone purification 200, reaches first apparatus for temporary storage 300, be provided with the resin filter device in the filtrating area, for example the Di group 110, filter the ionic impurity of removing in this crude caprolactam water solution by resin absorption, form filtered caprolactam water solution.Via Beckmann rearrangement generate contain 30 to 40% lactan, water, and the crude caprolactam water solution of impurity import filtrating areas 100 through pipeline 10, utilization is located at the Di group 110 of this filtrating area 100 and is carried out resin filter, remove the ionic impurity in this crude caprolactam water solution, form filtered caprolactam water solution.Shown in Figure 1B, this Di group 110 can comprise two covers in parallel and interchangeable Di 110a, 110b.When using Di 110a to carry out the resin filter purification, Di 110b is stand-by state, when carrying out filtration, purification, handles when reaching the replacing standard device 110a, then use device 110b instead and proceed the purifying treatment of resin filter, device 110a then uses the acid of dilution or alkali to carry out salinization regeneration, resin is restored to the original state, appended ionic impurity and the organic impurities of while deresinate, put with the demineralization water logging again, be stand-by state, use when changing operation next time, thereby can be continuously and interruptedly do not continue to carry out the resin filter purifying treatment.Shown in Fig. 1 C, in present embodiment, this Di 110a can comprise placed in-line resin anion(R.A) post 112, cationic resin column 114 and resin anion(R.A) post 116 in regular turn, forms a cover Di 110a.Sulfate ion in removable this crude caprolactam water solution of this resin anion(R.A), the ammonium radical ion in removable this crude caprolactam water solution of resin cation (R.C.), and reach the purpose of the ionic impurity in the preliminary removal aqueous solution.In addition, the partial organic substances impurity in this crude caprolactam water solution also can remove by the adsorption of Di.The resin absorption service temperature of this Di is preferably and is no more than 60 ℃, more preferably is no more than 50 ℃.Crude caprolactam water solution carries out the flow velocity of resin filter preferably between 3 to 6BV/hr (every cubic metre of resin of 1BV=contains 1 cubic metre of solution) by resin device.
The aqueous solution of distinguishing after filtration after 100 Di group 110 is filtered imports detecting units 130 through pipeline 11, carries out quality examination, judges whether this filtered caprolactam water solution meets the preset detection standard.In order to judge that test item that whether this filtered caprolactam water solution reaches the filtration, purification standard comprises the 290nm absorption value (EXT.290) and the basicity analysis (ALK.) of industrial hexanolactam.The 290nm absorption value (EXT.290) of industrial hexanolactam is to measure according to ISO 7059, and basicity analysis (ALK.) then is the caprolactam water solution that will obtain, and to the point of neutralization, (V) calculates according to its volume with the titration of 0.01N hydrochloric acid soln
V=adds standard hydrochloric acid volume (ml)
N=standard salt acid equivalent concentration (0.01)
A=sample heavy (g)
The per-cent of caprolactam content in the hexanolactam %=sample
In present embodiment, aqueous assay value EXT.290 behind resin filter less than 0.15, ALK. is less than 0.5 o'clock, the filtered aqueous solution sees through pipeline 12 and imports zone purifications 200, carries out the concentrated and purified of caprolactam water solution, remove remaining moisture and impurity, form the hexanolactam finished product.If the aqueous solution behind resin filter does not reach examination criteria yet, be EXT.290 greater than 0.15, ALK. sees through pipeline 14 greater than 0.5 and imports and be stored in this first apparatus for temporary storage 300, when treating that aqueous assay value behind this resin filter drops to criterion of acceptability, this aqueous solution that is stored in first apparatus for temporary storage 300 then sees through pipeline 16 again to be mixed with the crude caprolactam water solution of filtered, imports the ionic impurity that this filtrating area 100 is removed in the aqueous solution once more.The volumetric flow rate blending ratio of the hexanolactam of this first apparatus for temporary storage 300 and the crude caprolactam water solution of this filtered is preferably in 1: 0.05 to 1: 0.4 scope, more preferably in 1: 0.2 to 1: 0.4 scope.If blending ratio is low excessively, can prolong recovery time, may influence next time and change, if blending ratio is too high, each purification step possibly can't be loaded, and causes degradation.
In present embodiment, when utilizing ion exchange resin to carry out the filtration, purification of crude caprolactam water solution, after handling about 2100 to 2500 tonnes pure hexanolactam (becoming pure hexanolactam with its concentration conversion) with crude caprolactam water solution, detected value such as EXT.290 and ALK. can experience one and rise sharply the stage, be increased near or surpass the detected value that resin is changed.As shown in Figure 2, detected value EXT.290 will surpass 0.15 by rising sharply less than 0.1, even near 0.2, descending then returns to below 0.15, is stable and slowly rises.Detected value ALK. is then by rising sharply to more than 0.5 decline gradually then less than 0.3.Since the caprolactam water solution detected value EXT.290 after resin filter purifies greater than 0.15, ALK. is greater than 0.5, can cause the formed hexanolactam finished product of follow-up concentrated and purified step can't meet hexanolactam finished product acceptance value (that is, EXT.290 is less than 0.05).Therefore must before detected value rises sharply above examination criteria, carry out resin and change operation, avoid forming the aqueous solution that does not reach examination criteria, cause the final qualified hexanolactam finished product that generates.Yet, if the replacing operation frequency of Di is too high, not only can reduce production efficiency, also need to expend a large amount of materials and produce a large amount of waste materials simultaneously, increase production cost.On the other hand, if desire reduces the purifying treatment that the replacing frequency of resin device continues to carry out resin filter, though can increase the output of hexanolactam, but during detected value rises sharply (promptly, EXT.290 greater than 0.15, ALK. is greater than 0.5) the formed aqueous solution, finally can cause the hexanolactam finished product can't meet acceptance value.
Because in the resin filter scavenging process of crude caprolactam water solution, can the experience one section detected value rise sharply during and cause final formed hexanolactam finished product can't meet the finished product acceptance value, but still have afterwards one section quite long during can effectively operate, form the caprolactam water solution of coincidence detection standard.Therefore, equipment of the present invention, during detected value rises sharply, with this after filtration but the aqueous solution that does not reach examination criteria yet imports first apparatus for temporary storage stores, carry out simultaneously resin filter constantly, do not need to suspend immediately processing procedure and carry out resin replacing operation, and can not cause finally forming underproof hexanolactam finished product because of carrying out resin filter constantly.Therefore, equipment of the present invention can prolong effective running time of Di, and has the material of saving and subtract useless advantage.
The method that the present invention is used for purifying crude caprolactam water solution comprises the following steps: that (a) imports filtrating area with pending crude caprolactam water solution, the resin filter device group that utilization is located in the filtrating area is filtered the ionic impurity of removing in this crude caprolactam water solution, forms filtered caprolactam water solution; (b) detect this filtered caprolactam water solution of judgement and whether meet the preset detection standard; (c1) will detect and judge that the caprolactam water solution meet the predetermined detection standard imports the concentrated and purified formation hexanolactam finished product that caprolactam water solution is carried out in the zone purification; And (c2) will detect and judge that the caprolactam water solution do not reach the predetermined detection standard imports and is stored in first apparatus for temporary storage, and carry out step (a) again after making this caprolactam water solution that is stored in first apparatus for temporary storage and the crude caprolactam water solution of filtered mixing.As described above, can utilize the 290nm absorption value (EXT.290) of industrial hexanolactam and basicity analysis (ALK.) to judge whether this filtered caprolactam water solution reaches predetermined filtration, purification standard.This method also can be in the preceding step of hydrogenation of carrying out of step (c1), promptly, judge after testing at this filtered caprolactam water solution and to meet the predetermined detection standard but do not import as yet before the zone purification carries out the concentrated and purified formation hexanolactam finished product of caprolactam water solution, carry out the hydrogenation of caprolactam water solution, to convert the unsaturation organic impurity in the caprolactam water solution to saturated organic step of hydrogenation, remove in order to the purifying of back segment.
Fig. 3 illustrates embodiments of the invention 2.Embodiment 1 as described above, and the crude caprolactam water solution that contains 30 to 40% hexanolactams carries out resin filter through the Di group 110 that pipeline 10 imports filtrating area 100.Through resin filter and after testing unit 130 judge that the aqueous solution that meets the predetermined detection standard imports hydrogenation apparatuss 150 through pipeline 12, to have two keys in the aqueous solution or triple-linked unsaturation organic impurity changes into single bonded saturated organism, remove in order to the purifying of back segment.Then, through pipeline 18 caprolactam water solution after the hydrogenation is imported zone purification 200 and remove remaining moisture and impurity formation hexanolactam finished product.Resin filter is after detecting unit 130 is judged the caprolactam water solution that does not meet the predetermined detection standard yet, then see through pipeline 14 and import and be stored in this first apparatus for temporary storage 300, when treating that aqueous assay value behind this resin filter drops to criterion of acceptability, this aqueous solution that is stored in first apparatus for temporary storage 300 then sees through pipeline 16 again to be mixed with the crude caprolactam water solution of filtered, imports the ionic impurity that this filtrating area 100 is removed in the aqueous solution once more.
Fig. 4 illustrates the embodiment of the invention 3.Crude caprolactam water solution carries out resin filter through the Di group 110 that pipeline 10 imports filtrating area 100.Through resin filter and after testing unit 130 judge that the aqueous solution that meets the predetermined detection standard imports hydrogenation apparatuss 150 through pipeline 12, to have two keys in the aqueous solution or triple-linked unsaturation organic impurity changes into single bonded saturated organism, remove in order to the purifying of back segment.Then, through pipeline 18 caprolactam water solution after the hydrogenation is imported zone purification 200 and remove remaining moisture and impurity formation hexanolactam finished product.Zone purification 200 comprises in order to the evaporation unit 210 that forms the high density hexanolactam, in order to the snubber assembly 220 that receives this high density hexanolactam, and in order to form the water distilling apparatus 230 of hexanolactam finished product.This evaporation unit 210 in order to concentrate through resin filter and after testing unit 130 judge the caprolactam water solution that meets the predetermined detection standard, remove the most of moisture in this aqueous solution, form concentration and be higher than 80%, preferably be higher than 90%, more preferably be higher than 99% high density hexanolactam.These evaporation unit 210 formed high density hexanolactams import snubber assembly 220 through pipeline 20, import water distilling apparatus 230 via pipeline 22 again and remove remaining moisture and organic impurity, form the hexanolactam finished product.In equipment of the present invention, when this caprolactam water solution is distinguished 100 resin filter after filtration after detecting unit 130 judgements do not meet the predetermined detection standard yet, and see through that pipeline 14 imports and when being stored in this first apparatus for temporary storage 300, hydrogenation apparatus 150 temporarily falls product 40 to 60% with 210 of the evaporation units of zone purification 200, after the detected value for the treatment of resin filter dropped to standard value, the evaporation unit 210 that the aqueous solution that meets the predetermined detection standard then imports hydrogenation apparatus 150 and zone purification 200 again formed the high density hexanolactams.
In this embodiment, can further be provided with second apparatus for temporary storage 400, formed high density hexanolactam between term falls in order to store this hydrogenation apparatus 150 and evaporation unit 210.This hydrogenation apparatus 150 and evaporation unit 210 fall between term formed high density hexanolactam and import second apparatus for temporary storage 400 through pipeline 26, after the resin filter detected value in district 100 to be filtered drops to predetermined standard value, mix with the high density caprolactam water solution of snubber assembly 220 through pipeline 28 again, utilize pumping to import water distilling apparatus 230, reclaim fully up to the high density hexanolactam of second apparatus for temporary storage 400.This volumetric flow rate blending ratio of high density hexanolactam that is stored in the high density hexanolactam of second apparatus for temporary storage 400 and this snubber assembly 220 is preferably in 1: 0.05 to 1: 0.4 scope, more preferably in 1: 0.2 to 1: 0.4 scope.If blending ratio is too high, each purification step possibly can't be loaded, and causes degradation.
Claims (14)
1. the equipment of a purifying crude caprolactam water solution comprises:
(A) filtrating area is provided with resin filter device group, in order to filter the ionic impurity of removing in this crude caprolactam water solution, forms filtered caprolactam water solution;
(B) detecting unit, in order to judge whether filtered caprolactam water solution meets the preset detection standard, wherein, this preset detection standard 290nm absorption value of being meant the caprolactam water solution behind resin filter less than 0.15 and the basicity analytical value less than 0.5;
(C) zone purification is in order to receive after filtration and to meet the caprolactam water solution of predetermined detection standard and carry out the concentrated and purified formation hexanolactam finished product of caprolactam water solution; And
(D) first apparatus for temporary storage, in order to receive to store after filtration but do not reach the caprolactam water solution of predetermined detection standard yet, this water solution system that is stored in first apparatus for temporary storage with import this filtrating area again after the crude caprolactam water solution of filtered mixes.
2. equipment according to claim 1, wherein, this caprolactam water solution that is stored in first apparatus for temporary storage mixes with the crude caprolactam water solution of filtered with 1: 0.05 to 1: 0.4 volumetric flow rate ratio.
3. equipment according to claim 1, wherein, this resin filter device group comprises the in parallel and interchangeable Di of at least two covers.
4. equipment according to claim 3, wherein, this Di comprises placed in-line resin anion(R.A) post, cationic resin column and resin anion(R.A) post in regular turn.
5. equipment according to claim 1, wherein, this crude caprolactam water solution comprises 30 to 40% hexanolactam, water and impurity.
6. equipment according to claim 1 also comprises in order to the unsaturation organic impurity in the caprolactam water solution is changed into saturated organic hydrogenation apparatus.
7. equipment according to claim 1, wherein, this zone purification comprises:
(C1) evaporation unit in order to concentrate after filtration and to meet the caprolactam water solution of predetermined detection standard, forms concentration and is higher than 80% hexanolactam;
(C2) snubber assembly is higher than 80% hexanolactam in order to receive the formed concentration of this evaporation unit; And
(C3) water distilling apparatus is higher than 80% hexanolactam in order to this concentration of purifying and forms the hexanolactam finished product.
8. equipment according to claim 7, wherein, this concentration is higher than 80% hexanolactam and is meant that concentration is higher than 90% hexanolactam.
9. equipment according to claim 8, wherein, this concentration is higher than 80% hexanolactam and is meant that concentration is higher than 99% hexanolactam.
10. equipment according to claim 7, wherein, this filtered caprolactam water solution does not reach the predetermined detection standard and when importing this first apparatus for temporary storage, product then temporarily falls in the evaporation unit of this zone purification.
11. equipment according to claim 10 also comprises second apparatus for temporary storage.
12. the method for a purifying crude caprolactam water solution comprises the following steps:
(a) pending crude caprolactam water solution is imported filtrating area, utilize the resin filter device group of being located in the filtrating area to filter the ionic impurity of removing in this crude caprolactam water solution, form filtered caprolactam water solution;
(b) detect to judge whether this filtered caprolactam water solution meets the preset detection standard, wherein, the 290nm absorption value that this preset detection standard is meant the caprolactam water solution behind resin filter less than 0.15 and the basicity analytical value less than 0.5;
(c1) will detect and judge that the caprolactam water solution meet the predetermined detection standard imports the concentrated and purified formation hexanolactam finished product that caprolactam water solution is carried out in the zone purification; And
(c2) will detect judgement and not reach the caprolactam water solution importing of predetermined detection standard and be stored in first apparatus for temporary storage, and carry out step (a) again after making this caprolactam water solution that is stored in first apparatus for temporary storage and the crude caprolactam water solution of filtered mixing.
13. method according to claim 12 also comprises in order to the unsaturation organic impurity in the caprolactam water solution is changed into saturated organic step of hydrogenation.
14. method according to claim 13, wherein, this step of hydrogenation is carried out in step (c1) is preceding.
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| CN101570503B (en) * | 2008-11-11 | 2011-04-27 | 广东新会美达锦纶股份有限公司 | Method for concentrating low-concentration caprolactam water solution |
| CN104059019B (en) * | 2013-10-28 | 2017-01-25 | 中国石油化工股份有限公司 | Caprolactam purification method and device |
| CN103965090B (en) * | 2014-05-31 | 2015-11-18 | 江苏诚信药业有限公司 | A kind of process for purification of oxiracetam |
| CN104098495A (en) * | 2014-07-28 | 2014-10-15 | 湘潭大学 | Method for improving caprolactam refining process |
| WO2017212605A1 (en) | 2016-06-09 | 2017-12-14 | 積水化学工業株式会社 | Apparatus for producing organic substance from waste, and method for producing organic substance from waste |
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