CN209721832U - The separation and recovery system of NMP in a kind of saline solns - Google Patents
The separation and recovery system of NMP in a kind of saline solns Download PDFInfo
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- CN209721832U CN209721832U CN201920163492.4U CN201920163492U CN209721832U CN 209721832 U CN209721832 U CN 209721832U CN 201920163492 U CN201920163492 U CN 201920163492U CN 209721832 U CN209721832 U CN 209721832U
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Abstract
The utility model belongs to mixed solution recyclable device technical field, and in particular to the separation and recovery system of NMP in a kind of saline solns.The separation and recovery of the NMP and salt in solvent predominantly after washing neutralization is recycled, and includes extraction equipment, stripper, extractant removing means, NMP purifying plant and vaporising device.The recovery system uses dynamic extraction under normal temperature state, not only realizes the separation of solvent and water, but also the rate of recovery of the solvent greatly improved, the rate of recovery of solvent is made to reach 99.95% or more；The salinity in abraum salt solution is recycled by vaporising device, not only realizes that the recycling of salting liquid reduces cost, while also realizing the low emission of waste liquid, meets the requirement of national environmental protection.
Description
Technical field
The utility model belongs to mixed solution recyclable device technical field, and in particular in a kind of p-aramid fiber production process
The separation and recovery system of NMP in saline solns.
Background technique
During aramid fiber produces synthesis PPTA resin, need using NMP(N- methyl pyrrolidone) as molten
Agent, calcium chloride are as low temperature poly condensation is carried out in the organic solvent of cosolvent, meeting after the hydrochloric acid generated in reaction process neutralizes
A large amount of hydrochloride is generated, contained NMP, salt, water and micro oligomer can be removed to reaction solution washing after reaction
Obtain primary product PPTA resin, the water consumption in usual PPTA resin water-washing process is larger, and neutralize after solution be containing
If the aqueous solution of a large amount of organic solvents and salt not only can wherein containing a large amount of NMP and calcium chloride directly discarded to the solution
It causes largely to waste, causes the increase of production cost, while the discharge of untreated effluent will also result in problem of environmental pollution.
Chinese patent CN101457414 refers to desalination-steaming for separating and recovering processing NMP, salt, water mixed solvent system
Combined method is evaporated, it is specific that the salt for being dissolved in and neutralizing in recovered liquid is removed using electrodialysis or ion exchange resin, it then uses and steams
It evaporates method and separates water with NMP.This method needs film or ion exchange resin of good performance, the selection of film and ion exchange resin
It is the biggest problem of industrialized production, the stability being used for a long time is poor, and reliability is low, and operating cost is too high, practicability
It is poor.
N-Methyl pyrrolidone-calcium chloride solvent body is neutralized to neutrality with neutralizer by Chinese patent CN103087348, then
Add deionized water or recycling water washing PPTA, the slurry after distillation is carried out desalination by distillation under pressure dehydration in desalination kettle；Most
Rectification and purification recycling is carried out to the solvent of desalination afterwards.This method be the solvent after neutralizing first distill water outlet and it is micro-
The NMP of amount, then NMP is collected in redistillation, deviates from after moisture being not thorough for a large amount of salt removing in solvent, salt separating/enriching in distillation
Increase in the tar content that bottom causes NMP cracking to generate, while also resulting in abraum salt and can not recycle, causes short can not connect return period
Continuous metaplasia produces, and directly steams a large amount of water in solvent and also results in energy consumption increase, increases production cost.
Chinese patent CN101457414 proposes the method for recycling design NMP in p-aramid fiber production process a kind of: adopting
It uses aromatic alkyl halide as solvent NMP used in extractant extraction p-aramid fiber production process, extracts using being distilled to recover
Take the NMP in phase.It is directly distilled after this method extraction and separation, will cause extractant removing not exclusively, under high-temperature situation
The heavy corrosion that hydrolysis easily causes equipment occurs for extractant；And the impurity in the product and solution of extractant hydrolysis can accelerate
NMP cracking, causes NMP to lose, and is mingled with more impurity in NMP when recycling, influences polycondensation reaction and the PPTA of later period polymerization
Synthesis；Meanwhile unpurified extractant also will affect it in the effect of extracting of recycling.
Utility model content
The utility model aim is that the rate of recovery can be improved in p-aramid fiber production process, reduce energy by providing one kind
Consumption recycles the n-methlpyrrolidone (NMP) in Organic Solvents Containing and hydrochloride in solvent and the two is recycled
System.
To achieve the goals above, the utility model devises the separation and recovery system of NMP in a kind of saline solns, packet
Containing extraction equipment, stripper, extractant removing means, thick NMP purifying plant and saline solution recyclable device；
Extraction equipment includes mother liquor tank, disc type extraction tower, extractant basin and extraction pans；The mother liquor tank
Output end extracts tower bottom with disc type by pipeline and is connected, and the output end of extractant basin extracts tower top by pipeline and disc type
Portion is connected, and the output end of disc type extraction tower bottom is connected by pipeline with extraction pans；Disc type extraction tower top passes through
Pipeline is connected with stripper top；
Extractant removing means includes that extractant removing feed heater, extractant removing tower, extractant removing tower are boiled again
Device, extractant condenser and extractant purify storage tank；The output end of the extraction pans by pipeline and extractant remove into
Material heater is connected；Extractant removing feed heater output end in the middle part of pipeline and extractant removing tower by being connected；Extraction
It takes agent removing tower bottom end to remove tower reboiler input terminal with extractant by pipeline to be connected, extractant removes tower reboiler output
End is connected by pipeline with extractant removing tower；The output end of extractant removing tower and stripper top passes through pipeline and extraction
Agent condenser is taken to be connected；Extractant condenser output end purifies storage tank with extractant by pipeline and is connected；Extractant purification
Storage tank output end is equipped with three branches, is wherein connected at the top of the first branch and extractant removing tower, second branch and extractant
Basin is connected, and third branch is connected with stripper；
Thick NMP purifying plant include NMP recovery tower, NMP recycling tower reboiler, NMP recycling condenser, NMP return tank,
NMP basin and waste residue heater；The extractant removing tower bottom output end in the middle part of pipeline and NMP recovery tower by being connected；
NMP recycles tower bottom output end and is equipped with two branches, and the first branch is connected with NMP recycling tower reboiler input terminal, and second
Road is connected with waste residue heater；NMP recycles tower reboiler output end and is connected with NMP recycling tower bottom；At the top of NMP recovery tower
Output end recycles condenser with NMP by pipeline and is connected；NMP recycles condenser output end and is equipped with two branches, the first branch
It is connected with NMP return tank, second branch is connected with vacuum system；NMP return tank output end is equipped with three branches, the first branch
It is connected with NMP basin, second branch is connected with NMP recovery tower, and third branch is connected in vacuum system；
Saline solution recyclable device includes abraum salt solution basin, level-one evaporator, level-one evaporator heating chamber, second level forced evaporation
Device, second level forcing vaporiser heating room, evaporative condenser, resin water washing tank, salting liquid basin and crystallization sheeting device；The stripping
Tower bottom output end is connected by pipeline with abraum salt solution basin；The abraum salt solution basin passes through pipeline and level-one evaporator
Middle part is connected, and level-one base of evaporator output end is equipped with two branches, and wherein the first branch is connected with level-one heating room, the
Two branches are connected with salting liquid basin；Level-one evaporator top output port is connected by pipeline with evaporative condenser, evaporation
Condenser output end is connected by pipeline with resin water washing tank；Second level forcing vaporiser bottom output end is equipped with two branches,
Wherein the first branch is connected with the input terminal of second level forcing vaporiser heating room, and second branch is connected with crystallization sheeting device；Salt
Solution basin output end is connected with second level forcing vaporiser heating room input terminal；Level-one evaporator heating chamber and second level force to steam
The bottom output end of hair device heating room passes through pipeline and is connected with evaporative condenser；Output at the top of level-one evaporator heating chamber
It is connected in the middle part of end and level-one evaporator；The output end in second level forcing vaporiser heating ceiling portion is connected with second level forcing vaporiser
It is logical.
Further, mother liquor tank is equipped with mother liquor pH meter, and mother liquor tank output end is equipped with mother liquor delivery pump, mother liquor tank
The pipeline being connected with disc type extraction tower is equipped with mother liquor stream meter；Extractant basin output end is equipped with extractant delivery pump, extraction
The pipeline that agent basin is connected with disc type extraction tower is equipped with extractant flowmeter；Disc type extraction tower is connected pipeline with extraction pans
It is equipped with extraction flowmeter.
Further, the output end for extracting pans, which is equipped with, extracts intermediate delivery pump, and extraction pans and extractant remove
The connected pipeline of feed heater is equipped with extraction multi-phase flowmeter.
Further, stripper bottom output end is equipped with saline solution delivery pump；The output end of extractant removing tower bottom is equipped with
Extractant removes column bottoms pump.
Further, the pipeline that extractant removing tower is connected with NMP recovery tower is equipped with NMP purifying column feed flow meter；
The second branch that extractant purifies storage tank output end is equipped with extractant delivery pump, and extractant purifies first of storage tank output end
Road is equipped with extractant and removes column bottoms pump.
Further, the output end of NMP recovery tower is equipped with NMP and recycles column bottoms pump, and the NMP return tank output end is equipped with
NMP reflux pump.
Further, the output end of abraum salt solution basin is equipped with abraum salt delivery pump；Second level forcing vaporiser heats room input
End is equipped with forced circulation pump；The output end of salting liquid basin is equipped with salting liquid delivery pump.
Compared with prior art, the utility model has the beneficial effects that
1, energy consumption greatly reduces in entire separation process.The utility model uses rotating disc type abstraction technique by NMP and water
Separation is changed into the separation of NMP and chloroform, is only needed to realize using electrical loss according to the characteristic of material in entire separation process
The separation of NMP and water.
2, salt content≤0.05% in NMP is made by the separation of abstraction technique, solve in recycling rectifying in tower reactor due to
The enrichment of salt causes system interval to carry out, the periodical of cleaning increases；The reduction of salt content solves salt under high-temperature situation and splits to NMP
The a series of problem such as the influence of solution increases the rate of recovery of NMP to reach system long-term operation.
3, disc type extraction tower can be such that the salt content in extraction phase is down within≤0.05%, make the content of NMP in raffinate phase
It is down to≤0.05%, NMP ult rec is made to reach 99.93% or more.
It 4, is salt in raffinate phase, the aqueous solution of NMP, extractant, wherein NMP≤0.05%, extractant≤0.12%, using vapour
The mode of mentioning removes extractant≤0.0001% in the salting liquid after extractant reaches separation；The salting liquid for removing extractant can be with
35% salting liquid is directly concentrated to give to salting liquid by level-one evaporation, 35% salting liquid returns to solvent and prepares progress essence
Solvent preparation is used as polyplant cosolvent before making, and 35% extra salting liquid, which enters second level forcing vaporiser, to carry out again
Primary concentration, reaches the salt solvent that salt content is 65%, and 65% salt solvent after concentration is directly entered sheeting crystallizer；Two effects are strong
The middle pressure steam that evaporimeter thermal source processed uses system itself to use, does not need to re-lay pipeline；What two effect forcing vaporiser generated
Raw steam can be back to level-one evaporator, the heat source as level-one evaporator carry out using, the condensed water of two groups of evaporators and
Level-one evaporator steam water by condenser condensation be back to resin wash basin storage carry out resin washing use；Two groups of steamings
Hair device is all made of vacuumizing, and existing vacuum pump can be used and carry out, without in addition purchasing vacuum equipment.
5, extraction phase enters rectifying column (i.e. extractant removing tower) and removes to the chloroform in solution, due to micro chlorine
Imitative removing is more difficult and has the characteristic of facile hydrolysis, remaining minim chloroform is removed by stripping mode in bottom, while making thick NMP
Chloroform content≤0.0001% in solvent, and can prevent chloroform from hydrolyzing the corrosion to equipment 5%~7% water content control, and
And reach the requirement that NMP is aqueous in polymerization proportion, without directly reaching requirement to deploying before nmp solution ingredient.
6, due to containing micro salt and other impurity in solution, thick nmp solution is carried out by the way of rectification under vacuum
Purification, is that nmp solvent reaches the requirement directly used.
Detailed description of the invention
Fig. 1 is the schematic diagram of the separation of NMP and recovery system in saline solns described in the utility model.
Specific embodiment
The embodiments of the present invention is illustrated by particular specific embodiment below, those skilled in the art can be by this
Content disclosed by specification understands other advantages and effect of the utility model easily.
Embodiment 1
As shown in Figure 1, in a kind of saline solns NMP separation and recovery system, comprising extraction equipment, stripper 9, extraction
Agent removing means, thick NMP purifying plant and saline solution recyclable device；
Extraction equipment includes mother liquor tank 1, disc type extraction tower 6, extractant basin 3 and extraction pans 7；The mother liquor storage
The output end of tank 1 is connected by pipeline with 6 bottom of disc type extraction tower, and the output end of extractant basin 3 passes through pipeline and disc type
It is connected at the top of extraction tower 6, the output end of 6 bottom of disc type extraction tower is connected by pipeline with extraction pans 7；Disc type extraction
6 top of tower is connected by pipeline with 9 top of stripper；9 bottom output end of stripper is equipped with saline solution delivery pump 10；
Mother liquor tank 1 is equipped with mother liquor pH meter 2, and 1 output end of mother liquor tank is equipped with mother liquor delivery pump 4, mother liquor tank 1 and disk
The connected pipeline of formula extraction tower 6 is equipped with mother liquor stream meter 26；3 output end of extractant basin is equipped with extractant delivery pump 5, extraction
The pipeline that agent basin 3 is connected with disc type extraction tower 6 is equipped with extractant flowmeter 27；Disc type extraction tower 6 and extraction 7 phase of pans
Connecting leg road is equipped with extraction flowmeter 28；
Extractant removing means includes extractant removing feed heater 11, extractant removing tower 12, extractant removing tower
Reboiler 14, extractant condenser 15 and extractant purify storage tank 16；The output end of the extraction pans 7 passes through pipeline and extraction
Agent removing feed heater 11 is taken to be connected, the output end of extraction pans 7, which is equipped with, extracts intermediate delivery pump 8, extracts pans 7
The pipeline being connected with extractant removing feed heater 11 is equipped with extraction multi-phase flowmeter 29；Extractant removes feed heater 11
Output end in the middle part of pipeline and extractant removing tower 12 by being connected；12 bottom end of extractant removing tower is de- by pipeline and extractant
Except 14 input terminal of tower reboiler is connected, extractant removes 14 output end of tower reboiler and passes through pipeline and 12 phase of extractant removing tower
Connection；The output end at 9 top of extractant removing tower 12 and stripper passes through pipeline and is connected with extractant condenser 15；Extraction
15 output end of agent condenser purifies storage tank 16 with extractant by pipeline and is connected；Extractant purifies 16 output end of storage tank and is equipped with three
Branch, is wherein connected at the top of the first branch and extractant removing tower 12, and second branch is connected with extractant basin 3, and
Three branches are connected with stripper 9；
The second branch that extractant purifies 16 output end of storage tank is equipped with extractant delivery pump 17, and extractant purifies storage tank 16
The first branch of output end is equipped with extractant and removes column bottoms pump 18；Thick NMP purifying plant includes NMP recovery tower 19, NMP recycling
Tower reboiler 21, NMP recycling condenser 22, NMP return tank 23, NMP basin 45 and waste residue heater 25；The extractant removing
By being connected in the middle part of pipeline and NMP recovery tower 19, the output end of 12 bottom of extractant removing tower is equipped with 12 bottom output end of tower
Extractant removes column bottoms pump 13；The pipeline that extractant removing tower 12 is connected with NMP recovery tower 19 is equipped with NMP purifying column feeding flow
Meter 30；19 bottom output end of NMP recovery tower is equipped with two branches, and the first branch recycles 21 input terminal phase of tower reboiler with NMP
Connection, second branch are connected with waste residue heater 25；NMP recycles 21 output end of tower reboiler and 19 bottom phase of NMP recovery tower
Connection；19 top output port of NMP recovery tower recycles condenser 22 with NMP by pipeline and is connected；NMP recycles condenser 22 and exports
End is equipped with two branches, and the first branch is connected with NMP return tank 23, and second branch is connected with vacuum system 46；NMP return tank
23 output ends are equipped with three branches, and the first branch is connected with NMP basin 45, and second branch is connected with NMP recovery tower 19, the
Three branches are connected in vacuum system 46；
The output end of NMP recovery tower 19 is equipped with NMP and recycles column bottoms pump 20, and 23 output end of NMP return tank is returned equipped with NMP
Stream pump 24；
Saline solution recyclable device includes that abraum salt solution basin 31, level-one evaporator 33, level-one evaporator heating chamber 34, second level are strong
Evaporator 36, second level forcing vaporiser heating room 37, evaporative condenser 35, resin water washing tank 42, salting liquid basin 40 and knot processed
Brilliant sheeting device 39；The 9 bottom output end of stripper is connected by pipeline with abraum salt solution basin 31；The abraum salt solution storage
For tank 31 by being connected in the middle part of pipeline and level-one evaporator 33,33 bottom output end of level-one evaporator is equipped with two branches, wherein
The first branch is connected with level-one heating room 34, and second branch is connected with salting liquid basin 40；33 top of level-one evaporator is defeated
Outlet is connected by pipeline with evaporative condenser 35, and 35 output end of evaporative condenser is equipped with two branches, the first branch and tree
Rouge water washing tank 42 is connected, and second branch is connected with condenser vacuum system 47；36 bottom output end of second level forcing vaporiser
Equipped with two branches, wherein the first branch is connected with the input terminal of second level forcing vaporiser heating room 37, second branch and knot
Brilliant sheeting device 39 is connected；40 output end of salting liquid basin is connected with second level forcing vaporiser heating 37 input terminal of room (in order to just
It is refined in the salting liquid that salting liquid basin 40 is discharged, second branch can also be arranged with after in 40 output end of salting liquid basin
Continuous refining solvent prepares unit and is connected)；The bottom of level-one evaporator heating chamber 34 and second level forcing vaporiser heating room 37 is defeated
Outlet passes through pipeline and is connected with evaporative condenser 35；The output end and level-one evaporator at 34 top of level-one evaporator heating chamber
33 middle parts are connected；The output end at 37 top of second level forcing vaporiser heating room is connected with second level forcing vaporiser 36；
The output end of abraum salt solution basin 31 is equipped with abraum salt delivery pump 32；Second level forcing vaporiser heating 37 input terminal of room is set
There is forced circulation pump 38；The output end of salting liquid basin 40 is equipped with salting liquid delivery pump 41.
Utilize the separation of NMP in above-mentioned saline solns and the process of recovery system: using chloroform as extractant, In
The NMP in salting liquid is extracted in production process, NMP is located at extraction phase, is returned by the extractant in rectifying recycling extraction phase
It receives and uses, NMP is purified, directly reaches in polymerization and uses.Specific steps are as follows:
1, PPTA resin will be synthesized to be washed, obtain aqueous 52%, containing NMP 42%, saliferous 6% and micro oligomer composition
Solvent, is stored in mother liquor tank 1 as mother liquor, mother liquor mother liquor pH meter 2 is adjusted pH to 7-8, and low in filter solvents
After polymers and impurity, it is delivered to the bottom of disc type extraction tower 6 by the adjusting of mother liquor delivery pump 4 and mother liquor stream meter 26, extracts
Extractant in agent basin 3 is delivered to 6 top of disc type extraction tower by the adjusting of extractant delivery pump 5 and extractant flowmeter 27
Extraction and separation are carried out, the extraction phase of 6 bottom of disc type extraction tower is delivered to extraction pans 7 after being extracted the metering of flowmeter 28,
Then the extraction phase in pans 7 is extracted using delivery pump 8 among extracting and by defeated after the metering of extraction multi-phase flowmeter 29
It send to extractant and removes feed heater 11；
2, the step of stripping is: using the micro chloroform in stripping mode condensing recovery raffinate phase, preventing hazardous
The outlet of product, extractant chloroform and mother liquor tank 1 in extractant basin 3 neutralize after solvent 4:1 in mass ratio into
Enter disc type extraction tower 6, the NMP in disc type extraction tower 6 in solvent, which is transferred in chloroform, forms extraction phase；It is saline solution, micro
Chloroform forms raffinate phase, and the raffinate phase at 6 top of disc type extraction tower is delivered to stripper 9 and removes chloroform remaining in raffinate phase, vapour
The gas-phase transport steamed at the top of stripper 9 to extractant condenser 15 carries out condensation subitem, and the salting liquid of 9 bottom of stripper is through saline solution
Delivery pump 10 is delivered to abraum salt solution basin 31；
3, the step of extractant removes is: extraction phase is heated to bubble point temperature in extractant removing feed heater 11
Afterwards, into extractant removing tower 12, the separation of extractant is carried out by way of atmospheric distillation；12 bottom of extractant removing tower
Material removes column bottoms pump 13 by extractant and is delivered to heat source of the extractant removing tower reboiler 14 as extractant removing tower 12,
12 bottom of extractant removing tower be equipped with steam input terminal, by the bottom input preventing trace amount of steam in extractant removing tower 12 into
Row stripping removes remaining extractant；It is residual that 12 bottom of extractant removing tower uses a small amount of steam stripped mode to remove denier in solution
The extractant deposited prevents extractant cracking harm caused by equipment and the loss of increase NMP under high temperature；Extractant removing tower 12
The extractant on top enters extractant condenser 15 with the gas phase of gas phase and the output of 9 top of stripper jointly and carries out condensation point
；After condensation subitem, remaining extractant is delivered to after extractant purification storage tank 16 purifies by extractant delivery pump 17
Extractant basin 3 is recycled, and water phase is delivered to extractant removing tower 12 through 18 reflux of water conveying pump, it is ensured that it stablizes fortune
Row, extra moisture enter stripper 9, and carrying out recycling again to extractant remaining in water phase prevents outlet, extractant removing
The thick nmp solvent in 12 bottom of tower is delivered to NMP recovery tower by extractant removing column bottoms pump 13 and NMP purifying column feed flow meter 30
19；
4, the step of thick NMP is purified is: the NMP by removing extractant is thick nmp solvent, and thick NMP passes through NMP recovery tower
It is that NMP recovery tower 19 provides heat source that bottom pump 20, which is delivered to NMP recycling tower reboiler 21, passes through rectification under vacuum in NMP recovery tower 19
Mode remove the impurity in thick nmp solvent, it is cold that the pure NMP that NMP recovery tower 19 steams by NMP recycles overhead condenser 22
Enter NMP recovery tower return tank 23 after solidifying, a part of NMP is back to NMP recovery tower in the output end of NMP recovery tower return tank 23
19, ensure the stable operation of NMP recovery tower 19, another part is delivered to NMP basin 45；The heavy constituents material such as remaining tar warp
Cross NMP recovery tower column bottoms pump 20 be delivered to waste residue heater 25 heat after, remaining tar pass through subsequent coke tar recovery system
It is timed quantitative discharge recycling, prevents the heavy constituent in abraum salt solution from influencing the quality of later period recycling salt, is mentioned by thick NMP
The nmp solution that pure device is purified；
5, the step of saline solution recycles is: the salting liquid of 9 bottom of stripper is delivered to abraum salt solution through saline solution delivery pump 10 and stores
Tank 31 carries out pre-concentration using single effect evaporator to remaining salting liquid, and the abraum salt in abraum salt solution basin 31 is defeated by abraum salt
It send pump 32 to send and the salting liquid for being 35% is concentrated by level-one evaporator heating chamber 34 to level-one evaporator 33, level-one evaporator 33 pushes up
Portion's steam is washed for resin by 35 condensing recovery of evaporative condenser to resin water washing tank 42 and is used, level-one evaporator heating chamber 34
In 35% salting liquid be sent into salting liquid basin 40, then by 41 a part of salting liquid delivery pump be delivered to refining solvent preparation singly
Member carry out ingredient use, another part by forced circulation pump 38 send to two effect forcing vaporiser heat rooms 37 be evaporated it is dense
Contracting, is made the salting liquid that concentration is 65%, and the heat source of second level forcing vaporiser heating room 37 is the middle pressure steam that uses of system, and two
The steam that grade forcing vaporiser heating room 37 generates enters level-one evaporator heating chamber 34 and uses as heat source, two effect forced evaporations
Salting liquid after device 36 is concentrated enters crystallization sheeting device 39 and carries out after crystallization sheeting that dress packet is outer to be sold, level-one evaporator heating chamber 34 and
The condensate liquid of two effect forcing vaporiser heating rooms 37 enters 35 condensing recovery of evaporative condenser to resin water washing tank 42 for resin water
Wash use.
Recovery system described in the utility model makes salt content≤0.05% in NMP, solves in recycling rectifying in tower reactor
Since the enrichment of salt causes system interval to carry out, the periodical of cleaning increases；The reduction of salt content solves salt pair under high-temperature situation
The a series of problems such as the influence of NMP cracking increase the rate of recovery of NMP to reach system long-term operation；Disc type extraction tower
The salt content in extraction phase can be made to be down within≤0.05%, the content of NMP in raffinate phase is made to be down to≤0.05%, make NMP most
The whole rate of recovery reaches 99.93% or more；It is salt in raffinate phase, the aqueous solution of NMP, extractant, wherein NMP≤0.05%, extractant
≤ 0.12%, extractant≤0.0001% in the salting liquid after extractant reaches separation is removed using stripping mode；Rectifying column is (i.e.
Extractant removing tower 12) minim chloroform of remnants is removed by stripping mode in bottom, while making chloroform content in thick nmp solvent
≤ 0.0001%, and can prevent chloroform from hydrolyzing the corrosion to equipment 5%~7% water content control.
The above embodiments are only illustrative of the principle and efficacy of the utility model, and not for limitation, this is practical new
Type.Any person skilled in the art can all carry out above-described embodiment under the spirit and scope without prejudice to the utility model
Modifications and changes.Therefore, such as those of ordinary skill in the art without departing from the revealed essence of the utility model
All equivalent modifications or change completed under mind and technical idea, should be covered by the claim of the utility model.
Claims (7)
1. the separation and recovery system of NMP in a kind of saline solns, which is characterized in that including extraction equipment, stripper, extractant
Removing means, thick NMP purifying plant and saline solution recyclable device；
Extraction equipment includes mother liquor tank, disc type extraction tower, extractant basin and extraction pans；The output of the mother liquor tank
End is connected by pipeline with disc type extraction tower, and the output end of extractant basin is connected by pipeline with disc type extraction tower, disk
The output end of formula extraction tower bottom is connected by pipeline with extraction pans；Disc type extraction tower top passes through pipeline and stripper
Top is connected；
Extractant removing means includes extractant removing feed heater, extractant removing tower, extractant removing tower reboiler, extraction
Agent condenser and extractant is taken to purify storage tank；The output end of the extraction pans passes through pipeline and extractant removing charging heating
Device is connected；Extractant removing feed heater output end is connected by pipeline with extractant removing tower；Extractant removing tower
Bottom end removes tower reboiler input terminal with extractant by pipeline and is connected, and extractant removing tower reboiler output end passes through pipeline
It is connected with extractant removing tower；It is cold with extractant that the output end of extractant removing tower top and stripper top passes through pipeline
Condenser is connected；Extractant condenser output end purifies storage tank with extractant by pipeline and is connected；It is defeated that extractant purifies storage tank
Outlet is equipped with three branches, is wherein connected at the top of the first branch and extractant removing tower, second branch and extractant basin phase
Connection, third branch are connected with stripper；
Thick NMP purifying plant includes NMP recovery tower, NMP recycling tower reboiler, NMP recycling condenser, NMP return tank, NMP storage
Tank and waste residue heater；The extractant removing tower bottom output end is connected by pipeline with NMP recovery tower；NMP recovery tower
Bottom output end is equipped with two branches, and the first branch is connected with NMP recycling tower reboiler input terminal, and second branch adds with waste residue
Hot device is connected；NMP recycling tower reboiler output end is connected with NMP recovery tower；NMP recovery tower top output port passes through pipeline
It is connected with NMP recycling condenser；NMP recycles condenser output end and is equipped with two branches, and the first branch is connected with NMP return tank
Logical, second branch is connected with vacuum system；NMP return tank output end is equipped with three branches, and the first branch is connected with NMP basin
Logical, second branch is connected with NMP recovery tower, and third branch is connected with vacuum system；
Saline solution recyclable device include abraum salt solution basin, level-one evaporator, level-one evaporator heating chamber, second level forcing vaporiser,
Second level forcing vaporiser heats room, evaporative condenser, resin water washing tank, salting liquid basin and crystallization sheeting device；The stripper
Bottom output end is connected by pipeline with abraum salt solution basin；The abraum salt solution basin passes through pipeline and level-one evaporator phase
Connection, level-one base of evaporator output end are equipped with two branches, and wherein the first branch is connected with level-one heating room, second branch
It is connected with salting liquid basin；Level-one evaporator top output port is connected by pipeline with evaporative condenser, evaporative condenser
Output end is connected by pipeline with resin water washing tank；Second level forcing vaporiser bottom output end is equipped with two branches, wherein the
One branch is connected with the input terminal of second level forcing vaporiser heating room, and second branch is connected with crystallization sheeting device；Salting liquid storage
Tank output end is connected with second level forcing vaporiser heating room input terminal；Level-one evaporator heating chamber and second level forcing vaporiser add
The bottom output end in hot cell passes through pipeline and is connected with evaporative condenser；Output end at the top of level-one evaporator heating chamber and one
Grade evaporator is connected；The output end in second level forcing vaporiser heating ceiling portion is connected with second level forcing vaporiser.
2. the separation and recovery system of NMP in saline solns according to claim 1, which is characterized in that on mother liquor tank
Equipped with mother liquor pH meter, mother liquor tank output end is equipped with mother liquor delivery pump, sets on the pipeline that mother liquor tank is connected with disc type extraction tower
There is mother liquor stream meter；Extractant basin output end is equipped with extractant delivery pump, the pipe that extractant basin is connected with disc type extraction tower
Road is equipped with extractant flowmeter；Disc type extraction tower is connected pipeline with extraction pans equipped with extraction flowmeter.
3. the separation and recovery system of NMP in saline solns according to claim 1, which is characterized in that extraction pans
Output end be equipped with and extract intermediate delivery pump, the pipeline that extraction pans are connected with extractant removing feed heater is equipped with extracting
Take multi-phase flowmeter.
4. the separation and recovery system of NMP in saline solns according to claim 1, which is characterized in that stripper bottom
Output end is equipped with saline solution delivery pump；The output end that extractant removes tower bottom is equipped with extractant and removes column bottoms pump.
5. the separation and recovery system of NMP in saline solns according to claim 1, which is characterized in that extractant removing
The pipeline that tower is connected with NMP recovery tower is equipped with NMP purifying column feed flow meter；Extractant purifies second of storage tank output end
Road is equipped with extractant delivery pump, and the first branch that extractant purifies storage tank output end is equipped with extractant and removes column bottoms pump.
6. the separation and recovery system of NMP in saline solns according to claim 1, which is characterized in that NMP recovery tower
Output end is equipped with NMP and recycles column bottoms pump, and the NMP return tank output end is equipped with NMP reflux pump.
7. the separation and recovery system of NMP in saline solns according to claim 1, which is characterized in that the storage of abraum salt solution
The output end of tank is equipped with abraum salt delivery pump；Second level forcing vaporiser heats room input terminal and is equipped with forced circulation pump；Salting liquid basin
Output end be equipped with salting liquid delivery pump.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761425A (en) * | 2019-01-24 | 2019-05-17 | 河南神马尼龙化工有限责任公司 | The separation and recovery system of NMP in a kind of saline solns |
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2019
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109761425A (en) * | 2019-01-24 | 2019-05-17 | 河南神马尼龙化工有限责任公司 | The separation and recovery system of NMP in a kind of saline solns |
| CN109761425B (en) * | 2019-01-24 | 2024-01-19 | 河南神马芳纶技术开发有限公司 | Separation and recovery system for NMP in salt-containing solution |
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