CN103012273A - Neutralized crystallization system and method of preparing caprolactam through caprolactam rearrangement solution - Google Patents
Neutralized crystallization system and method of preparing caprolactam through caprolactam rearrangement solution Download PDFInfo
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- CN103012273A CN103012273A CN2012104891167A CN201210489116A CN103012273A CN 103012273 A CN103012273 A CN 103012273A CN 2012104891167 A CN2012104891167 A CN 2012104891167A CN 201210489116 A CN201210489116 A CN 201210489116A CN 103012273 A CN103012273 A CN 103012273A
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Abstract
The invention discloses neutralized crystallization system and method of preparing caprolactam through caprolactam rearrangement solution. The neutralized crystallization system is characterized in that a feeding mixer is connected with an inlet in the upper part of a neutralized crystallization reactor, an upper-layer organic phase outlet of the neutralized crystallization reactor is connected with an inlet of a caprolactam oil layer separator, a lower-layer heavy organic phase outlet of the neutralized crystallization reactor is connected with an inlet of an ammonium sulfate centrifugal machine, an outlet at one end of the caprolactam oil layer separator is connected with a caprolactam collecting tank, an outlet at the other end of the caprolactam oil layer separator is connected with an ammonium sulfate mother liquor collection tank, an outlet at the lower end of the ammonium sulfate centrifugal machine is connected with an ammonium sulfate washing dryer, an outlet at the upper end of the ammonium sulfate centrifugal machine is connected with the ammonium sulfate mother liquor collection tank which is connected with the neutralized crystallization reactor through a mother liquor circulating pump. The neutralized crystallization system and method have the advantages that the heating and cooling capacities are integrated in reaction process, the energy consumption is low, the process is simple, and the purity of the product is high.
Description
Technical field
The present invention relates to a kind of preparation method of hexanolactam, especially relate to a kind of hexanolactam reset liquid prepare hexanolactam in and crystal system and method thereof.
Background technology
Hexanolactam is one of important source material of synthon and synthetic materials, mainly for the manufacture of polyamide 6 fibers (nylon 6), resin and film, also be used as the raw material of medicine, coating, leatheroid, softening agent, and on a small quantity for chemosynthesis Methionin, in weaving, the numerous areas such as plastics, fine chemistry industry have widely purposes.The Beckmann rearrangement reaction of cyclohexanone-oxime is most important technological process in the caprolactam production process, and quality product is played the crux effect.
At present, the industrial production that hexanolactam is reset liquid (hexanolactam sulfuric ester) is as catalyzer take the vitriol oil or oleum, cyclohexanone-oxime is carried out rearrangement reaction under the effect of oleum obtain, then hexanolactam is reset liquid and sent into the ammonia neutralization reactor, use the ammonia neutralisation of sulphuric acid, to realize separating of follow-up hexanolactam and sulfuric acid, ammonia neutralization reaction process is thermopositive reaction, need to remove the part heat by adding cooling apparatus, reduce temperature of reaction, thereby guarantee normally carrying out of reaction.After the ammonia neutralization reaction is finished, obtain hexanolactam and ammonium sulfate product, just need to evaporate the water that adds and react generation in the system, because N-process and vaporize water process are carried out respectively, therefore, neutralization reaction process liberated heat need to be taken away by cooling way and lose, and the process need of follow-up vaporize water heats, consumed energy.The process of so carrying out respectively causes neutralization reaction heat release loss and the consumption of follow-up steaming water process heat energy, and this process has expended a large amount of colds and heat, and energy expenditure is high, and energy utilizes unreasonable.
Summary of the invention
Technical problem to be solved by this invention provides hexanolactam and resets in the liquid and crystallisation process carries out simultaneously that neutralization reaction heat and vaporize water institute heat requirement are integratedly carried out, organic liquor and inorganic-liquid ammonium layered effect are good, product purity is high, the hexanolactam that energy consumption is low reset liquid prepare hexanolactam in and crystal system and method thereof.
The present invention solves the problems of the technologies described above the technical scheme that adopts: a kind of hexanolactam reset liquid prepare hexanolactam in and crystal system, comprise entry mixers, in and crystallization reactor, hexanolactam oil quantizer, sulphur ammonium whizzer, sulphur ammonium washing moisture eliminator, ammonium sulfate liquor holding tank and hexanolactam holding tank, described entry mixers with described in be connected upper inlet with crystallization reactor and be connected, the light organic phase outlet in upper strata of being connected with crystallization reactor in described is connected with the import of the oily quantizer of described hexanolactam, the heavy organic phase outlet of lower floor of being connected with crystallization reactor in described is connected with the import of described sulphur ammonium whizzer, one of described hexanolactam oil quantizer brings out mouth and is connected with described hexanolactam holding tank, the other end outlet is connected with described ammonium sulfate liquor holding tank, the lower end outlet of described sulphur ammonium whizzer is connected with described sulphur ammonium washing moisture eliminator, the outlet of the upper end of described sulphur ammonium whizzer is connected with described ammonium sulfate liquor holding tank, described ammonium sulfate liquor holding tank pass through the Recycling Mother Solution pump with described in be connected with crystallization reactor.
Be provided with feed liquid recycle pump and interchanger in described and on the connecting pipeline between the lower part outlet of crystallization reactor and the described entry mixers.In and the crystal solution circulation line be provided with heat exchange (cooling, heating) device, be used for guaranteeing the balance of cold and heat.
In the described and position of the lower part outlet of crystallization reactor be higher than described in and the position of the heavy organic phase outlet of lower floor of crystallization reactor.In and carry by the circulation of material between the lower part outlet of crystallization reactor and the upper inlet and carry out cold and heat recycle, heavy organic phase is discharged from the heavy organic phase outlet of the lower floor of crystallizer and is entered next step operation.
Also comprise condenser and condensate drum, be connected the upper end in described is connected with described condensate drum by described condenser with crystallization reactor, described condensate drum is connected with described entry mixers, is provided be used to the water inlet pipe that keeps the skin wet on the fluid pipeline of described condensate drum.The water vapour that steams is through condenser condenses, during lime set is returned and the crystallization reactor recycle.
Be provided with reactor heavy phase discharging pump in described and between crystallization reactor and the described sulphur ammonium whizzer, be provided with layering oil phase discharging pump between described hexanolactam oil quantizer and the described hexanolactam holding tank.
A kind of hexanolactam is reset the method that liquid prepares hexanolactam, specifically comprises the steps:
(1) hexanolactam is reset in mass ratio 1:(3～4 of liquid, ammonia and water): after (2.5～3) are sent into entry mixers and are mixed, in delivering to again and crystallization reactor generation neutralization reaction, the heat that reaction produces makes the moisture evaporation, reduced simultaneously temperature of reaction, after the neutralization reaction 5～20 minutes, in and the liquid in the crystallization reactor be divided into upper strata the first light organic phase and lower floor the first weight organic phase, wherein and the working pressure of crystallization reactor be-0.095 MPaG～-0.05MPaG, service temperature is 50～90 ℃;
(2) with the first light organic phase from extract out with crystallization reactor top and to send into hexanolactam oil quantizer and further separate, obtain the second light organic phase and the second heavy organic phase, the second heavy organic phase is sent into the mother liquor holding tank, the second light organic phase is sent into the hexanolactam holding tank make with extra care and obtain caprolactam product;
(3) with the first heavy organic phase by discharging pump from and the crystallization reactor bottom extract out and send into sulphur ammonium whizzer, separate and obtain the thick product of ammonium sulfate and ammonium sulfate centrifuge mother liquor, the thick product of ammonium sulfate is sent into sulphur ammonium washing moisture eliminator from the lower end outlet of sulphur ammonium whizzer, obtain ammonium sulfate products through washing impurity-removing and drying;
(4) the ammonium sulfate centrifuge mother liquor is sent into the mother liquor holding tank from the upper end outlet of sulphur ammonium whizzer, by in the Recycling Mother Solution pumped back and in the crystallization reactor, the hexanolactam preparation process is namely finished in recycling with the mixed solution in the mother liquor holding tank;
(5) repeat above-mentioned steps (1)-(4) and carry out cyclical operation.
The described first light organic phase and the second light organic phase are the aqueous solution that contains hexanolactam oil, and the described first heavy organic phase and the described second heavy organic phase are sulphur ammonium crystal slurry.
In described and crystallization reactor under condition of negative pressure, operate, the water vapour that steams is through condenser condenses, during the phlegma that obtains returns and the crystallization reactor recycle.Can be implemented in evaporation of water under the relative low temperature.
Be provided with the interchanger that feed liquid recycle pump and being used for guarantees the balance of cold and heat in described and on the connecting pipeline between the lower part outlet of crystallization reactor and the described entry mixers.
Compared with prior art, the invention has the advantages that:
(1) compares with common neutralization reaction, sulphur crystalline ammonium technique, the heat of process and cold are carried out integrated, effectively utilize neutralization reaction heat to carry out vaporize water, saved simultaneously heat and cold, do not need to take away reaction heat with other heat-eliminating mediums (water coolant).Produce 1 ton of hexanolactam and can save 2.4 tons of steam;
(2) be coupled in and crystallization operation, shortened technical process and facility investment.
Description of drawings
Fig. 1 be of the present invention in and the equipment flowsheet of crystal system.
Embodiment
Embodiment is described in further detail the present invention below in conjunction with accompanying drawing.
Embodiment one
A kind of hexanolactam of the present invention reset liquid prepare hexanolactam in and crystal system, as shown in Figure 1, comprise entry mixers 1, in and crystallization reactor 2, hexanolactam oil quantizer 3, sulphur ammonium whizzer 4, sulphur ammonium washing moisture eliminator 5, ammonium sulfate liquor holding tank 6 and hexanolactam holding tank 7, entry mixers 1 with in the upper inlet of being connected with crystallization reactor be connected, in the light organic phase outlet in the upper strata of being connected with crystallization reactor be connected with the import of the oily quantizer 3 of hexanolactam, in the heavy organic phase outlet of the lower floor of being connected with crystallization reactor 14 be connected with the import of sulphur ammonium whizzer 4, one of hexanolactam oil quantizer 3 brings out mouth and is connected with hexanolactam holding tank 7, the other end outlet is connected with ammonium sulfate liquor holding tank 6, the lower end outlet of sulphur ammonium whizzer 4 is connected with sulphur ammonium washing moisture eliminator 5, the outlet of the upper end of sulphur ammonium whizzer 4 is connected with ammonium sulfate liquor holding tank 6, ammonium sulfate liquor holding tank 6 pass through Recycling Mother Solution pump 17 with in are connected with crystallization reactor and are connected.
In this specific embodiment, in and be provided with feed liquid recycle pump 8 on the lower part outlet 13 of crystallization reactor 2 and the connecting pipeline between the entry mixers 1 and be used for guaranteeing the interchanger 9 of the balance of cold and heat.In and the crystal solution circulation line be provided with heat exchange (cooling, heating) device 9, be used for guaranteeing the balance of cold and heat; In and the position of the lower part outlet 13 of crystallization reactor 2 be higher than in and the position of the heavy organic phase outlet 14 of lower floor of crystallization reactor 2.
In this specific embodiment, this system also comprises condenser 10 and condensate drum 11, in the upper end of being connected with crystallization reactor be connected with condensate drum 11 by condenser 10, condensate drum 11 is connected with entry mixers 1, is provided be used to the water inlet pipe 12 that keeps the skin wet on the fluid pipeline of condensate drum 11.The water vapour that steams is through condenser 10 condensations, during lime set is returned and crystallization reactor 2 recycles; In and be provided with reactor heavy phase discharging pump 15(between crystallization reactor 2 and the sulphur ammonium whizzer 4 and adopt common recycle pump to get final product); Be provided with layering oil phase discharging pump 16 between hexanolactam oil quantizer 3 and the hexanolactam holding tank 6.
Embodiment two
A kind of hexanolactam of the present invention is reset the method that liquid prepares hexanolactam, as shown in Figure 1, specifically comprises the steps:
(1) hexanolactam is reset liquid, ammonia and water 1:3:2.5 is sent into entry mixers 1 and mixes in mass ratio after, in delivering to crystallization reactor 2 neutralization reactions occur again, the heat that reaction produces makes the moisture evaporation, reduced simultaneously temperature of reaction, after the neutralization reaction 5 minutes, in and the liquid in the crystallization reactor 2 be divided into upper strata the first light organic phase and lower floor's the first heavy organic phase, wherein in the working pressure of crystallization reactor 2 be-0.095MPaG that service temperature is 50 ℃;
(2) with the first light organic phase from extract out with crystallization reactor 2 tops and to send into hexanolactam oil quantizer 3 and further separate, obtain the second light organic phase and the second heavy organic phase, the second heavy organic phase is sent into mother liquor holding tank 6, the second light organic phase is sent into hexanolactam holding tank 7 make with extra care and obtain caprolactam product;
(3) with the first heavy organic phase by reactor heavy phase discharging pump 15 from and crystallization reactor 2 bottoms extract out and to send into sulphur ammonium whizzer 4, separate and obtain the thick product of ammonium sulfate and ammonium sulfate centrifuge mother liquor, the thick product of ammonium sulfate is sent into sulphur ammonium washing moisture eliminator 5 from the outlet of sulphur ammonium whizzer 4 lower ends, obtain ammonium sulfate products through washing impurity-removing and drying;
(4) the ammonium sulfate centrifuge mother liquor is sent into mother liquor holding tank 6 from the upper end outlet of sulphur ammonium whizzer 4, during the mixed solution in the mother liquor holding tank 6 is sent back to by Recycling Mother Solution pump 17 and in the crystallization reactor 2, the hexanolactam preparation process is namely finished in recycling;
(5) repeat above-mentioned steps (1)-(4) and carry out cyclical operation.
In this specific embodiment, the first light organic phase and the second light organic phase are the aqueous solution that contains hexanolactam oil, and the first heavy organic phase and the second heavy organic phase are sulphur ammonium crystal slurry; In and crystallization reactor 2 under condition of negative pressure, operate, the water vapour that steams is through condenser condenses, during phlegma returns and crystallization reactor 2 recycles.Can be implemented in evaporation of water under the relative low temperature.In and be provided with feed liquid recycle pump 8 on the lower part outlet 13 of crystallization reactor 2 and the connecting pipeline between the entry mixers 1 and be used for guaranteeing the interchanger 9 of the balance of cold and heat.
Embodiment three
With embodiment two, its difference is: after in the step (1) hexanolactam being reset liquid, ammonia and water 1:3.5:2.75 sending into entry mixers 1 and mixes in mass ratio, in delivering to crystallization reactor 2 neutralization reactions occur again, after the neutralization reaction 10 minutes, in and the working pressure of crystallization reactor 2 be-0.07MPaG that service temperature is 70 ℃.
Embodiment four
With embodiment two, its difference is: after in the step (1) hexanolactam being reset liquid, ammonia and water 1:4:3 sending into entry mixers 1 and mixes in mass ratio, in delivering to crystallization reactor 2 neutralization reactions occur again, after the neutralization reaction 20 minutes, in and the working pressure of crystallization reactor 2 be-0.05MPaG that service temperature is 90 ℃.
Certainly, above-mentioned explanation is not limitation of the present invention, and the present invention also is not limited to above-mentioned giving an example.Those skilled in the art are in essential scope of the present invention, and the variation of making, remodeling, interpolation or replacement also should belong to protection scope of the present invention.
Claims (9)
- A hexanolactam reset liquid prepare hexanolactam in and crystal system, it is characterized in that: comprise entry mixers, in and crystallization reactor, hexanolactam oil quantizer, sulphur ammonium whizzer, sulphur ammonium washing moisture eliminator, ammonium sulfate liquor holding tank and hexanolactam holding tank, described entry mixers with described in be connected upper inlet with crystallization reactor and be connected, the light organic phase outlet in upper strata of being connected with crystallization reactor in described is connected with the import of the oily quantizer of described hexanolactam, the heavy organic phase outlet of lower floor of being connected with crystallization reactor in described is connected with the import of described sulphur ammonium whizzer, one of described hexanolactam oil quantizer brings out mouth and is connected with described hexanolactam holding tank, the other end outlet is connected with described ammonium sulfate liquor holding tank, the lower end outlet of described sulphur ammonium whizzer is connected with described sulphur ammonium washing moisture eliminator, the outlet of the upper end of described sulphur ammonium whizzer is connected with described ammonium sulfate liquor holding tank, described ammonium sulfate liquor holding tank pass through the Recycling Mother Solution pump with described in be connected with crystallization reactor.
- A kind of hexanolactam according to claim 1 reset liquid prepare hexanolactam in and crystal system, it is characterized in that: be provided with feed liquid recycle pump and interchanger in described and on the connecting pipeline between the lower part outlet of crystallization reactor and the described entry mixers.
- A kind of hexanolactam according to claim 2 reset liquid prepare hexanolactam in and crystal system, it is characterized in that: in the described and position of the lower part outlet of crystallization reactor be higher than described in and the position of the heavy organic phase outlet of lower floor of crystallization reactor.
- A kind of hexanolactam according to claim 1 reset liquid prepare hexanolactam in and crystal system, it is characterized in that: also comprise condenser and condensate drum, be connected the upper end in described is connected with described condensate drum by described condenser with crystallization reactor, described condensate drum is connected with described entry mixers, is provided be used to the water inlet pipe that keeps the skin wet on the fluid pipeline of described condensate drum.
- A kind of hexanolactam according to claim 1 reset liquid prepare hexanolactam in and crystal system, it is characterized in that: be provided with reactor heavy phase discharging pump in described and between crystallization reactor and the described sulphur ammonium whizzer, be provided with layering oil phase discharging pump between described hexanolactam oil quantizer and the described hexanolactam holding tank.
- One kind utilize hexanolactam claimed in claim 1 reset liquid prepare hexanolactam in and the method for crystal system, it is characterized in that specifically comprising the steps:(1) hexanolactam is reset in mass ratio 1:(3～4 of liquid, ammonia and water): after (2.5～3) are sent into entry mixers and are mixed, in delivering to again and crystallization reactor generation neutralization reaction, after the neutralization reaction 5～20 minutes, in and the liquid in the crystallization reactor be divided into upper strata the first light organic phase and lower floor the first weight organic phase, wherein and the working pressure of crystallization reactor be-0.095 MPaG～-0.05MPaG, service temperature is 50～90 ℃;(2) with the first light organic phase from extract out with crystallization reactor top and to send into hexanolactam oil quantizer and further separate, obtain the second light organic phase and the second heavy organic phase, the second heavy organic phase is sent into the mother liquor holding tank, the second light organic phase is sent into the hexanolactam holding tank make with extra care and obtain caprolactam product;(3) with the first heavy organic phase by discharging pump from and the crystallization reactor bottom extract out and send into sulphur ammonium whizzer, separate and obtain the thick product of ammonium sulfate and ammonium sulfate centrifuge mother liquor, the thick product of ammonium sulfate is sent into sulphur ammonium washing moisture eliminator from the lower end outlet of sulphur ammonium whizzer, obtain ammonium sulfate products through washing impurity-removing and drying;(4) the ammonium sulfate centrifuge mother liquor is sent into the mother liquor holding tank from the upper end outlet of sulphur ammonium whizzer, by in the Recycling Mother Solution pumped back and in the crystallization reactor, the hexanolactam preparation process is namely finished in recycling with the mixed solution in the mother liquor holding tank;(5) repeat above-mentioned steps (1)-(4) and carry out cyclical operation.
- 7. a kind of hexanolactam according to claim 6 is reset the method that liquid prepares hexanolactam, it is characterized in that: the described first light organic phase and the second light organic phase are the aqueous solution that contains hexanolactam oil, and the described first heavy organic phase and the described second heavy organic phase are sulphur ammonium crystal slurry.
- 8. a kind of hexanolactam according to claim 6 is reset the method that liquid prepares hexanolactam, it is characterized in that: operate under condition of negative pressure with crystallization reactor in described, the water vapour that steams is through condenser condenses, during the phlegma that obtains returns and the crystallization reactor recycle.
- 9. a kind of hexanolactam according to claim 8 is reset the method that liquid prepares hexanolactam, it is characterized in that: the interchanger that is provided with feed liquid recycle pump and the balance that is used for guaranteeing cold and heat in described and on the connecting pipeline between the lower part outlet of crystallization reactor and the described entry mixers.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105408313A (en) * | 2013-07-26 | 2016-03-16 | Capiii有限公司 | Continuous process for recovery of caprolactam and crystalline ammonium sulfate |
| CN108341763A (en) * | 2018-04-24 | 2018-07-31 | 河北美邦工程科技股份有限公司 | A kind of caprolactam crystallization purifications |
| CN108409658A (en) * | 2018-04-24 | 2018-08-17 | 河北美邦工程科技股份有限公司 | A kind of effectively refining method of caprolactam |
| CN108530358A (en) * | 2018-04-24 | 2018-09-14 | 河北美邦工程科技股份有限公司 | A kind of method of caprolactam crystallization purifying |
| CN111408157A (en) * | 2020-04-14 | 2020-07-14 | 中石化南京工程有限公司 | Ammonium sulfate crystallization method and device thereof |
| CN111530119A (en) * | 2020-04-14 | 2020-08-14 | 中石化南京工程有限公司 | Tandem ammonium sulfate crystallization method and device thereof |
| CN112543803A (en) * | 2018-08-24 | 2021-03-23 | 南沼气技术有限责任公司 | Apparatus and method for neutralizing ammonium sulfate solution |
| CN115138326A (en) * | 2022-07-04 | 2022-10-04 | 山东安诺其化工技术研究有限公司 | Device and process for continuously producing monopersulfate composite salt |
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| US3907781A (en) * | 1973-06-26 | 1975-09-23 | Stamicarbon | Process for recovery of {68 -caprolactam from a reaction mixture of {68 -caprolactam and sulphuric acid |
| US3937789A (en) * | 1965-01-21 | 1976-02-10 | Snia Viscosa Societa' Nazionale Industria Applicazioni Viscosa S.P.A. | Process for the neutralization of acid solutions of caprolactam |
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| US3937789A (en) * | 1965-01-21 | 1976-02-10 | Snia Viscosa Societa' Nazionale Industria Applicazioni Viscosa S.P.A. | Process for the neutralization of acid solutions of caprolactam |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105408313A (en) * | 2013-07-26 | 2016-03-16 | Capiii有限公司 | Continuous process for recovery of caprolactam and crystalline ammonium sulfate |
| CN108341763A (en) * | 2018-04-24 | 2018-07-31 | 河北美邦工程科技股份有限公司 | A kind of caprolactam crystallization purifications |
| CN108409658A (en) * | 2018-04-24 | 2018-08-17 | 河北美邦工程科技股份有限公司 | A kind of effectively refining method of caprolactam |
| CN108530358A (en) * | 2018-04-24 | 2018-09-14 | 河北美邦工程科技股份有限公司 | A kind of method of caprolactam crystallization purifying |
| CN108341763B (en) * | 2018-04-24 | 2020-12-01 | 河北美邦工程科技股份有限公司 | Caprolactam crystallization and purification method |
| CN108530358B (en) * | 2018-04-24 | 2021-12-24 | 河北美邦工程科技股份有限公司 | Method for crystallizing and purifying caprolactam |
| CN112543803A (en) * | 2018-08-24 | 2021-03-23 | 南沼气技术有限责任公司 | Apparatus and method for neutralizing ammonium sulfate solution |
| CN111408157A (en) * | 2020-04-14 | 2020-07-14 | 中石化南京工程有限公司 | Ammonium sulfate crystallization method and device thereof |
| CN111530119A (en) * | 2020-04-14 | 2020-08-14 | 中石化南京工程有限公司 | Tandem ammonium sulfate crystallization method and device thereof |
| CN111530119B (en) * | 2020-04-14 | 2021-09-14 | 中石化南京工程有限公司 | Tandem ammonium sulfate crystallization method and device thereof |
| CN115138326A (en) * | 2022-07-04 | 2022-10-04 | 山东安诺其化工技术研究有限公司 | Device and process for continuously producing monopersulfate composite salt |
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Application publication date: 20130403 |