CN104447480A - Continuous recycling method of NMP (N-methyl pyrrolidone) solvent for polyphenylene sulfide production device - Google Patents
Continuous recycling method of NMP (N-methyl pyrrolidone) solvent for polyphenylene sulfide production device Download PDFInfo
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- CN104447480A CN104447480A CN201410643648.0A CN201410643648A CN104447480A CN 104447480 A CN104447480 A CN 104447480A CN 201410643648 A CN201410643648 A CN 201410643648A CN 104447480 A CN104447480 A CN 104447480A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/18—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
- C07D207/22—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
- C07D207/267—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention discloses a novel continuous recycling method of an NMP (N-methyl pyrrolidone) solvent for a polyphenylene sulfide production device. The polyphenylene sulfide production device comprises three vacuum rectifying towers, a heat exchanger, a centrifuge machine, a storage tank, a pump and relevant pipelines. In an existing polyphenylene sulfide solvent recycling process, pipelines are easily blocked by salt crystals in a dehydration process, so that the halt maintenance needs to be frequently carried out, the rate of equipment utilization is low, and the solvent loss is high. According to the novel continuous recycling method of the NMP (N-methyl pyrrolidone) solvent for the polyphenylene sulfide production device, a novel technological process device is developed; by virtue of forced circulation of high-concentration salt fraction at the tower bottoms, solid salt formed after water and the solvent are removed can be adequately stirred and circulated, and the blockage, caused by the salt crystals, of valves of the pipelines is avoided, so that the heating efficiency of the column bottoms is increased, the yield of NMP is improved, the quality of an recycled NMP product can reach 99.5% or above, recycling requirements of a system are met, and meanwhile, the long-period, stable and efficient operation of the device are guaranteed.
Description
Technical field
The invention belongs to a kind of chemical engineering salvage material field, N-methyl pyrrole network alkane ketone (NMP) solvent just relating to a kind of polyphenylene sulfide production equipment specifically reclaims novel method continuously.
Background technology
Polyphenylene sulfide (being called for short PPS) is a kind of high-performance special engineering plastics.Be widely used in the fields such as aerospace, military affairs, electronics, electrical equipment, precision instrument, automobile, machinery, household electrical appliances, coating.Since 1978, domestic Duo Suo scientific research institutions all expand research and development tackling key problem to PPS, but due to polymerization technique, solvent recuperation, the Advances in Key Technology of the aspects such as engineering amplification is slow, PPS production of resins cost remains high, and causes domestic market exploitation to relatively lag behind, and is difficult to form suitability for industrialized production ability.By the unremitting effort of scientific and technical personnel and the continuous reinforcement of national supporting dynamics, the polymerization technique of PPS resin obtains important breakthrough nearly ten years.
In the process of producing PPS, the unit such as its synthesis, washing can produce a large amount of waste liquid, the solid compounds such as the sodium-chlor containing the water of 35%, the santochlor of 5%, the NMP (N-Methyl pyrrolidone) and 10% of 50% in waste liquid and lithium chloride.Along with the production-scale expansion of current PPS, the follow-up rate of recovery how improving solvent NMP, reduces production cost, has become and has improved PPS production of resins competitive power, strengthened enterprise's production economy benefit and reduce key subjects of environmental pollution.
Mostly what current domestic PPS manufacturer adopted is that after water washing polycondensation thing filter cake, discard mixed solvent to the NMP washed carries out the technique that batch fractionating reclaims NMP, this technique reclaims NMP technique have that extraction agent is cheap and easy to get compared with other organic solvent extraction, extraction phase nonflammable explosive, nontoxic, environmental pollution is little, water and solvent NMP is easily separated, extraction agent not short, the solvent recuperation low cost and other advantages of solvent slop, technical process.But in the application process of reality, its shortcoming is also more remarkable: mixing solutions is when vacuum batch distillation dewaters, owing to not dissolving NaCl in nmp solvent, in dehydration, along with a large amount of NaCl crystallization of minimizing of moisture in dehydration tower bottom of rectifying tower, when crystal salt generates, be easy to blocking tower reactor and pipeline.Therefore need timing out of service, the NaCl solid of cleaning tower reactor surface crystallization, cleaning process has taken away certain nmp solvent simultaneously, not only increase the time of maintenance of the equipment, too increase the loss of nmp solvent, simultaneously too much owing to discharging organic content in salt solution, the utilization of effluent brine is greatly limited.
How improvement of production process, reduce NaCl in tower reactor and ducted crystallization, crystal salt is discharged, to the cleaning interval extending tower reactor as early as possible completely with dehydration liquid, the service efficiency of raising equipment, the labour intensity reducing operator is all most important with the consumption reducing NMP solvent; How to realize heat energy to make full use of simultaneously, reduce the running cost of recovery process, improve heat utilization rate and be all significant.
Summary of the invention
The present invention, mainly for the recovery method of polyphenylene sulfide production equipment nmp solvent, develops a kind of brand-new continuous processing flow process.The application of this flow process, make the separation of product more efficient, the purity of separated portion is higher, realizes better effects if; By efficient centrifugal pump in tower bottom application row pump circulation, add the disturbance of salinity solution in tower reactor, avoid salinity solution and form small-particle crystallization in tower reactor and pipeline, decrease the adhesion effect of nmp solvent on salt grain, avoid NMP and to remove in a large number with salt grain and the loss that causes; Considered by the entirety of heat exchanging network, utilize overhead vapours heat to carry out preheating to charging, decrease the use of steam and cold consumption, improve the utilising efficiency of heat.The present invention, by innovative technology scheme and equipment use mode, makes operation continuous, effectively improves production efficiency, improve the organic efficiency of nmp solvent simultaneously, decrease the pollution of solvent to salt, have significant economic benefit and environmental benefit.
For solving the problem, the technical solution used in the present invention is:
First raw material enters rectifying tower C-101 through preheating, extraction moisture after overhead vapours condensation, saline solns at the bottom of tower enters reboiler through a forced circulation pump part, another part tower bottoms enters whizzer M-101 and carries out centrifugal treating, wet basis salt after centrifugal goes out outside battery limit (BL), liquid enters rectifying tower C-102, extraction santochlor component after overhead vapours condensation, component at the bottom of tower enters rectifying tower C-103, first the steam component of C-103 tower top returns feed heater and carries out preheating to raw material, return condenser after preliminary cooling again to carry out reducing temperature twice process and obtain nmp solvent and go out battery limit (BL) to reclaim and recycle, tower reactor is a small amount of NMP, the mixture of oligopolymer and chlorate, forced circulation pump is utilized to increase the disturbance of still liquid, prevent crystallization from blocking tower reactor and pipeline, a still liquid part enters tower reactor through reboiler, another part extraction is to outside battery limit (BL).
The continuous recovery method of polyphenylene sulfide production equipment nmp solvent of the present invention, comprises three rectifying tower systems.Consider that rectifying salt analyzes the impact on whole Tower System and pipeline, in rectifying tower C-101 system and rectifying tower C-103 system, tower reactor is provided with two forced circulation pumps, avoids because removing of liquid causes salinity constantly to be separated out, blocking tower reactor and pipeline; By the Optimum utilization of heat exchanger network, utilize rectifying tower C-103 overhead vapours first to carry out preheating to charging, carrying out cooling process, save steam consumption and cold consumption, reduce process cost, create good economic benefit and environmental benefit.Whole technical process, be provided with three tower continuous rectification modes, make the separation refinement more of component in raw material, product separation purity is higher, operability is better, fully demonstrate chemical process and eaten the clean Advanced Idea of dry squeezing, achieve further lifting and the optimization of polyphenylene sulfide nmp solvent recovery process flow process.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further described:
Accompanying drawing adopts the continuous remanufacture schematic flow sheet of polyphenylene sulfide nmp solvent of the present invention;
Embodiment
Below in conjunction with the device of accompanying drawing and embodiment, the present invention is further elaborated, but any restriction is not produced to the present invention.
Described polyphenylene sulfide production equipment solvent recovery process, is made up of three rectifying tower systems.Raw material enters rectifying tower C-101 after thermal pretreatment, at removed overhead moisture, along with removing of moisture, tower bottoms thickens gradually, a strong solution part for extraction at the bottom of tower is by forced circulation pump to strengthen the disturbance of salinity in still liquid, and avoid Crystallization Plugging tower reactor and pipeline, another part enters whizzer and is separated, wet basis salt is sent out-of-bounds, and liquid ingredient enters rectifying tower C-102.Rectifying tower C-102 distills out component santochlor at tower top and delivers to outside battery limit (BL), rectifying tower C-103 is sent in component extraction at the bottom of tower, the highly purified nmp solvent of C-103 overhead extraction is first that preheating is carried out in charging by feed exchanger, then returns after rectifying tower C-103 overhead condenser is condensed to room temperature further and sends out-of-bounds.For avoiding remaining chlorate solution crystallization at the bottom of tower, by forced circulation pump to strengthen disturbance, a part sends tower reactor back to after boiling again, and a part of extraction is delivered to and out-of-bounds done further process.
The invention has the beneficial effects as follows that polyphenylene sulfide production equipment solvent recovery process is by innovating again layout and improvement, reasonable in design, operate continuously, in product, various component can fine separation and purity improve greatly, disposable yield reaches more than 90%, and product purity reaches more than 99.5%; By adopting pump circulation pump technique to rectifying tower C-101 and C-103 tower reactor solution, add the disturbance of still fluid component, enhance the heat transfer efficiency between still liquid, avoid salinity crystallization and block tower reactor and pipeline, extend the operational cycle of equipment, alleviate the labour intensity of workman, effectively raise production efficiency, decrease owing to cleaning the NMP loss brought simultaneously.By Optimization of Heat Exchanger Networks, be that raw material does thermal pretreatment by overhead vapours heat, decrease the consumption to cold, improve the utilization ratio of heat.To sum up several process innovation, whole device solvent recuperation flow process can be in operation and obtain good economic benefit and environmental benefit.
A kind of polyphenylene sulfide production equipment method for recovering solvents that the present invention proposes, be described by preferred embodiment, the part wherein do not addressed in detail is the common practise of those skilled in the art.Protection scope of the present invention is as the criterion with the content of claim, and all similar replacements of enlightening based on technology of the present invention and change, be all deemed to be included in spirit of the present invention, scope and content.
Claims (4)
1. the continuous recovery method of the nmp solvent of a polyphenylene sulfide production equipment, step comprises and will enter rectifying tower C-101 after raw material preheating, waste water is from overhead extraction, at the bottom of tower, concentration kettle liquid carries out pump circulation by impeller pump, fraction solids product is discharged outside battery limit (BL) after centrifuge dewatering, supernatant mother liquor is squeezed into rectifying tower C-102 tower top and is isolated santochlor, tower bottoms enters rectifying tower C-103, after the nmp solvent that tower top steams and feeding liquid heat exchange, further cooling extraction, by the chlorate solution of forced circulation pump extraction nmp solvent at the bottom of tower.
2. the continuous recovery method of polyphenylene sulfide production equipment nmp solvent as claimed in claim 1, it is characterized in that have employed solution salinity removing process and the full technical process of solvent recuperation, it is high that this process solvent reclaims quality, and purity is greater than 99.5wt%, and the disposable rate of recovery of yield can reach more than 90%.
3. the continuous recovery method of polyphenylene sulfide production equipment nmp solvent as claimed in claim 1, it is characterized in that rectifying tower C-101 and C-103 tower reactor pass through forced circulation pump, crystal salt in solution is fully stirred, avoid the blocking of saline crystallization to pipeline valve, ensure that the steady Effec-tive Function of device long period, improve production efficiency, decrease the loss of the nmp solvent caused due to equipment washing simultaneously, improve the yield of NMP.
4. polyphenylene sulfide production equipment nmp solvent as claimed in claim 1 reclaims novel method continuously, it is characterized in that the nmp solvent of rectifying tower C-103 tower top and charging are cooled by heat exchange, reduce further the operation energy consumption of technique.
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| CN201410643648.0A CN104447480B (en) | 2014-11-06 | 2014-11-06 | A kind of nmp solvent continuous recovery method of polyphenylene sulfide process units |
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| CN201410643648.0A CN104447480B (en) | 2014-11-06 | 2014-11-06 | A kind of nmp solvent continuous recovery method of polyphenylene sulfide process units |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106366030A (en) * | 2016-10-12 | 2017-02-01 | 南京大学 | High-purity recycling process system of complex chemical waste liquid |
| CN106519231A (en) * | 2015-09-09 | 2017-03-22 | 中国科学院过程工程研究所 | Polyphenylene sulfide waste liquid recovery and separation process |
| CN108779253A (en) * | 2016-04-13 | 2018-11-09 | 株式会社吴羽 | The apparatus for continuously production of poly (arylene sulfide) and the method for continuous production of poly (arylene sulfide) |
| CN110563228A (en) * | 2018-06-05 | 2019-12-13 | 青岛海湾集团有限公司 | Styrene process condensate and heat energy recovery system and control method |
| CN111620803A (en) * | 2020-05-11 | 2020-09-04 | 山东滨化滨阳燃化有限公司 | System and method for separating and recovering solvent and raw materials in polyphenylene sulfide production |
| US10807062B2 (en) | 2017-10-12 | 2020-10-20 | Kureha Corporation | Continuous production apparatus and continuous production method for polymer |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106519231A (en) * | 2015-09-09 | 2017-03-22 | 中国科学院过程工程研究所 | Polyphenylene sulfide waste liquid recovery and separation process |
| CN106519231B (en) * | 2015-09-09 | 2019-03-19 | 中国科学院过程工程研究所 | A kind of polyphenylene sulfide devil liquor recovery separating technology |
| CN108779253A (en) * | 2016-04-13 | 2018-11-09 | 株式会社吴羽 | The apparatus for continuously production of poly (arylene sulfide) and the method for continuous production of poly (arylene sulfide) |
| US10538629B2 (en) | 2016-04-13 | 2020-01-21 | Kureha Corporation | Device for continuously producing poly(arylene sulfide) and method for continuously producing poly(arylene sulfide) |
| CN108779253B (en) * | 2016-04-13 | 2020-06-09 | 株式会社吴羽 | Apparatus for continuously producing polyarylene sulfide and method for continuously producing polyarylene sulfide |
| CN106366030A (en) * | 2016-10-12 | 2017-02-01 | 南京大学 | High-purity recycling process system of complex chemical waste liquid |
| US10807062B2 (en) | 2017-10-12 | 2020-10-20 | Kureha Corporation | Continuous production apparatus and continuous production method for polymer |
| CN110563228A (en) * | 2018-06-05 | 2019-12-13 | 青岛海湾集团有限公司 | Styrene process condensate and heat energy recovery system and control method |
| CN111620803A (en) * | 2020-05-11 | 2020-09-04 | 山东滨化滨阳燃化有限公司 | System and method for separating and recovering solvent and raw materials in polyphenylene sulfide production |
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