CN104844420B - The continuous treatment technique of neopentyl glycol condensation water cleaning mother liquor and device - Google Patents
The continuous treatment technique of neopentyl glycol condensation water cleaning mother liquor and device Download PDFInfo
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- CN104844420B CN104844420B CN201510028509.1A CN201510028509A CN104844420B CN 104844420 B CN104844420 B CN 104844420B CN 201510028509 A CN201510028509 A CN 201510028509A CN 104844420 B CN104844420 B CN 104844420B
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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Abstract
The present invention relates to the continuous treatment device of a kind of neopentyl glycol condensation water cleaning mother liquor, it is characterized in that: described device includes filter, one-level preheater, two grades of preheaters, rectifying column, chromatography device and cyclone hydraulic separators, described filter is in the front end of one-level preheater, described one-level preheater is connected with described two grades of preheaters by pipeline, described rectifying column is in the rear end of described two grades of preheaters, described rectifying column tower top is provided with return tank and chromatography device, is provided with cyclone hydraulic separators and reboiler at the bottom of described rectifying tower.The present invention relates to the continuous treatment technological process of a kind of neopentyl glycol condensation water cleaning mother liquor, the organic impurities in neopentyl glycol condensation water cleaning mother liquor can be removed and concentrate neopentyl glycol by continuous-stable.
Description
Technical field
The invention belongs to the separation field of pharmaceutical industry, be specifically related to the continuous treatment of neopentyl glycol condensation water cleaning mother liquor
Technique and device.
Background technology
Neopentyl glycol is called for short NPG, white crystalline solid, soluble in water, low-carbon alcohols, low-carbon (LC) ketone, ether and aromatic compound.Mesh
Before, the synthetic method of neopentyl glycol mainly has hydrogenation method and methyl alcohol method.Neopentyl glycol molecule has specific neopentyl structure, its
Containing two primary carbonyls in molecule, central carbon atom not having α-hydrogen atom, these features make neopentyl glycol have the highest heat
Stability and chemical stability, therefore, it is usually used in the production fields such as medicine, chemical industry, coating, agricultural chemicals, plastics and oil.Its
In, in pharmaceuticals industry, neopentyl glycol can as the important source material of the intermediate ketal of synthesis brufen, it be dissolved in oil
Chlorine ketone generation condensation reaction in ether generates ketal.The ketal product of unreacted neopentyl glycol and generation obtains after washing
Ketal solution and the neopentyl glycol solution containing petroleum ether.Neopentyl glycol containing organic impurities such as petroleum ethers is condensed washing mother
Liquid is concentrated into after neopentyl glycol mass fraction is 60%, is circularly used for the condensation reaction of chlorine ketone, reduces and produce unit consumption.
The treatment technology scheme of neopentyl glycol condensation water cleaning mother liquor is by existing water vapour equlibrium distillation technique: first by new penta
Glycol condensation water cleaning mother liquor is input in the distillation storage tank of 20 cubic metres, then passes to live steam and heats, along with in tank
Temperature raises, and organic impurities and water in neopentyl glycol condensation water cleaning mother liquor collect in tank deck the most in gaseous form.From tank
Top extraction contains the gas phase of organic impurities and water, then is cooled to form the waste water containing organic impurities, completes a collection of rear repetition
Carry out.Existing technique often processes one ton of neopentyl glycol condensation water cleaning mother liquor, produces waste water 900 liters, the chemical oxygen demand in this waste water
Amount (COD) is 2000～3000 mg/litre.After above-mentioned processing procedure continues 20～22 hours, stop being passed through fresh water steam, tank
Neopentyl glycol after interior concentration is recycled to be used in the condensation reaction of chlorine ketone.
There are the following problems for existing water vapour equlibrium distillation technique: first, and in processing procedure, neopentyl glycol loss amount is big, tank
In the waste water of top extraction, neopentyl glycol mass fraction is 2～3%, processes neopentyl glycol condensation water cleaning mother liquor per ton, neopentyl glycol
Loss amount is 20～30 kilograms；Second, the operation cycle is long, and the neopentyl glycol condensation water cleaning mother liquor often processing a collection of 20 tons needs 20
～22 hours, production efficiency is low；3rd, the neopentyl glycol solution colour after process is the most yellow, needs through activated carbon decolorizing ability
Recycling, existing technique uses batch (-type) to process, and in tank, solution is under the condition of high temperature for a long time, and cause in solution is organic
Thing is partially carbonized, and color is the most yellow；4th, neopentyl glycol alembic easily occurs fouling, causes heat-transfer effect deviation, neopentyl glycol
Containing trace calcium sulfate in condensation water cleaning mother liquor, after equlibrium distillation steams substantial amounts of water, in tank, calcium sulfate is gradually assembled and is caused
Fouling in distillation tank skin.
Summary of the invention
Instant invention overcomes the deficiencies in the prior art, develop the continuous treatment of a kind of neopentyl glycol condensation water cleaning mother liquor
Technique and device, can effectively remove the organic impurities in neopentyl glycol solution to concentrate neopentyl glycol, and provide realize above-mentioned
The device of technical process.
A kind of continuous treatment device of neopentyl glycol condensation water cleaning mother liquor, it is characterised in that: include that filter, one-level are pre-
Hot device, two grades of preheaters, rectifying column, chromatography device and cyclone hydraulic separators, described filter is provided with material inlet and material outlet, thing
Material outlet is connected with one-level preheater by pipeline, and the material outlet of described one-level preheater is connected by pipeline and two grades of preheaters
Connecing, described two grades of preheater material outlets are connected with rectifying column by pipeline, and described rectifying column is provided with material inlet, top gaseous phase
Outlet, reflux inlet and materials at bottom of tower outlet, top gaseous phase outlet is connected with one-level preheater by pipeline, at described rectifying column
Tower top be provided with a return tank, one-level preheater is connected with described return tank entrance by pipeline, and described return tank is provided with water
Phase materials outlet and organic phase material outlet, aqueous phase material outlet is connected with rectifier column reflux entrance by pipeline, described rectifying
Being provided with cyclone hydraulic separators and two grades of preheaters at the bottom of the tower of tower, described cyclone hydraulic separators passes through pipeline and rectifying column and reboiler phase
Even, described two grades of preheaters are connected with rectifying column and one-level preheater by pipeline.
Described one-level preheater is tubular heat exchanger, and its material is graphite；Two grades of described preheaters are board-like changing
Hot device.
A kind of continuous treatment technological process of neopentyl glycol condensation water cleaning mother liquor, it is characterised in that: described flow process is with water
It is primary raw material with neopentyl glycol, comprises the following steps:
The first step: filter solid particle in neopentyl glycol condensation water cleaning mother liquor
Containing petroleum ether, dichloromethane organic impurities and insoluble solid in described neopentyl glycol condensation water cleaning mother liquor
Grain, is transported to neopentyl glycol condensation water cleaning mother liquor in rectifying column by filter from storage tank with pump, intercepts the most insoluble
Solid particle, the filter residue in periodic cleaning filter, containing petroleum ether in the neopentyl glycol condensation water cleaning mother liquor obtained after filtration
And dichloromethane；
Second step: preheating neopentyl glycol condensation water cleaning mother liquor
With the neopentyl glycol solution after concentration at the bottom of the top gaseous phase and tower of rectifying column as thermal source, in described one-level and two
Neopentyl glycol condensation water cleaning mother liquor is heated to 85～95 DEG C from normal temperature by level preheater；
3rd step: organic impurities in removing neopentyl glycol condensation water cleaning mother liquor
Neopentyl glycol condensation water cleaning mother liquor after preheating is through being pumped in described rectifying column, and tower bottom reboiler is passed through
0.1～0.5MPa (gauge pressure) add vapours, make tower bottom pressure maintain 0.01～0.05MPa (gauge pressure), tower bottom separatory body
Being vaporized by reboiler, the gas of rising carries out multi-stage gas-liquid mass transfer, petroleum ether and two in described rectifying column with dropping liq
Chloromethanes organic impurities is enriched with the most in the gas phase, discharges from rectifying column gaseous phase outlet the most in gaseous form；
In rectifying column, tower top pressure maintains 0～0.01MPa (gauge pressure), containing the gas of petroleum ether, dichloromethane and water
Body forms upper, middle and lower three layers after condensation in return tank, and lower floor's dichloromethane organic phase extraction, as solvent reclaiming in former
Production technology；Intermediate layer is back in rectifying column by pipeline containing a small amount of organic aqueous phase, carries out heat with the gas phase risen
With mass exchange；The petroleum ether on upper strata enters chromatography device with water, is divided into two-phase in chromatography device, and organic phase petroleum ether is as solvent
It is back to original production process；
4th step: the neopentyl glycol solution after extraction concentration
In rectifying column, owing to neopentyl glycol boiling point is high, it is enriched with the most in the liquid phase and is down at the bottom of tower, tower bottom liquid body one
Dividing and vaporized by reboiler, another part is the neopentyl glycol after concentrating, extraction after pipeline flows through two grades of preheaters.
The principle that the present invention realizes is:
Impurity in neopentyl glycol condensation water cleaning mother liquor includes insoluble solid particle, trace calcium sulfate, petroleum ether, dichloro
Methane etc..Neopentyl glycol condensation water cleaning mother liquor by a filter, is first filtered out the solid particle in solution by the present invention,
After again mother liquor being preheating to 85～95 DEG C by firsts and seconds preheater, send in tower in the middle part of rectifying column.Enter in tower
Neopentyl glycol condensation water cleaning mother liquor carries out heat and quality transmission with the gas phase of rising in tower.Light component organic impurities and part water
Constantly it is enriched with in the gas phase, rises to tower top extraction organic phase and some aqueous phase after condenser and chromatography device；Heavy constituent is new
Pentanediol is enriched with the most in the liquid phase, is plucked out of after dropping at the bottom of tower.In the aqueous phase of overhead extraction, neopentyl glycol content is at 10ppm
Hereinafter, in the neopentyl glycol concentrated product of extraction at the bottom of tower content of organics at below 2ppm.Due to neopentyl glycol condensation washing mother
Trace calcium sulfate in liquid is non-volatile, gradually can assemble at the bottom of tower, separate and extraction through cyclone hydraulic separators in processing procedure, from
The heated vaporization of cyclone hydraulic separators liquid out, the liquid declined in entering tower and in tower carries out heat and quality transmission.
There is advantages that
(1) The present invention reduces the loss amount of neopentyl glycol in neopentyl glycol condensation water cleaning mother liquor processing procedure.Existing water
Steam distillation technique is when concentrating neopentyl glycol condensation water cleaning mother liquor, along with organic impurities is distilled out of, and equlibrium distillation tank top
In the liquid of condensation, the mass fraction of neopentyl glycol is 2～3%, causes the waste of raw material.Technique of the present invention and
Device is during processing neopentyl glycol condensation water cleaning mother liquor, and in the water that tower top steams, neopentyl glycol content is at below 10ppm, place
Manage every batch of mother liquor many recovery neopentyl glycol 35～55 kilograms.
(2) invention increases the treatment effeciency of neopentyl glycol condensation water cleaning mother liquor.Existing steam distillation technique is dense
During contracting neopentyl glycol solution, every batch materials is about 20 tons, needs to process 20 hours.The present invention uses continuous treatment technique, place
Manage 20 tons of neopentyl glycol solution and only need 6 hours.
(3) The present invention reduces water vapour and recirculated water consumption, reduce production cost.Present invention employs heat integrated
Method, neopentyl glycol condensation water cleaning mother liquor preheats through rectifying tower top gaseous phase and tower bottom liquid phase two-stage, and after preheating, solution temperature reaches
To 85～95 DEG C, on the one hand decrease live steam consumption, on the other hand decrease the recirculated water consumption of overhead condenser.Process
Neopentyl glycol condensation water cleaning mother liquor per ton saves fresh water steam 110～130 kilograms, saves recirculated water 6000～7000 kilograms.
(4) present invention improves over the neopentyl glycol external appearance characteristic after concentration.Existing steam distillation technique uses batch (-type)
Operation, processing a collection of neopentyl glycol condensation water cleaning mother liquor used time is 20～22 hours, owing in tank, solution is in high temperature for a long time
Under state, causing part solution carbonization, color is the most yellow.The present invention uses continuous treatment technique, process qualified after new penta 2
Alcoholic solution is plucked out of from the bottom of tower in time, it is ensured that the purity of neopentyl glycol product and colourity.
(5) present invention has the ability of trace calcium sulfate in neopentyl glycol condensation water cleaning mother liquor that processes.Existing water vapour steams
Evaporate technology utilization alembic batch process neopentyl glycol condensation water cleaning mother liquor, along with the water in mother liquor is constantly distilled out of, molten in tank
Calcium sulfate in liquid is gradually assembled, and causes distilling fouling in tank skin.The present invention utilizes cyclone hydraulic separators in time by gathering at the bottom of tower
Calcium sulfate removes, and adds the neopentyl glycol condensation water cleaning mother liquor continuous treatment device disposal ability to calcium sulfate, prevents sulphur
Acid calcium fouling in rectifying column wall.
Accompanying drawing explanation
Accompanying drawing is the structural representation of the present invention.
In figure, 1. filter；2. one-level preheater；3. two grades of preheaters；4. rectifying column；5. return tank；6. reboiler；7.
Chromatography device；8. cyclone hydraulic separators.
Detailed description of the invention
Further illustrate below in conjunction with accompanying drawing, and unrestricted scope involved in the present invention.
As shown in drawings, first neopentyl glycol condensation water cleaning mother liquor is passed through filter 1 by the present invention, filters out the most insoluble
Property solid particle.Solution after filtration enters rectifying column after being preheating to uniform temperature by one-level preheater 2 and two grades of preheaters 3
In 4.Rectifying column is heated by reboiler 6, the gas risen in tower through supercooling laggard enter return tank 5.Dichloromethane is from return tank 5
Bottom extraction, petroleum ether and water enter chromatography device 7 from the extraction of return tank top, and water extraction bottom chromatography device 7, petroleum ether is from layer
Parser 7 top extraction.Neopentyl glycol condensation water cleaning mother liquor contains the calcium sulfate of trace, can be the denseest in heating process
Contracting, discharges from bottom after cyclone hydraulic separators 8, and liquid enters reboiler and carries out heating vaporization.
The following is the example that is embodied as of the present invention:
Embodiment 1: neopentyl glycol condensation water cleaning mother liquor inlet amount is 4000 kgs/hr, after one-level preheater
Temperature is increased to 70 DEG C from 20 DEG C, and after two grades of preheaters, temperature is increased to 90 DEG C, and temperature of charge at the bottom of rectifying tower is from 109 DEG C
Dropping to 75 DEG C, steam consumption is 450 kgs/hr.20 tons of neopentyl glycol solution process about 5 hours time, overhead extraction dichloro
The volume of methane is 800 liters, and the volume of petroleum ether is 500 liters.The water of overhead extraction is after water knockout drum, and wherein neopentyl glycol contains
Amount is 236 mg/litre for 8ppm and COD, and the neopentyl glycol mass fraction of extraction at the bottom of tower is 70%, wherein dichloromethane and oil
Ether does not detects.
Embodiment 2: neopentyl glycol condensation water cleaning mother liquor inlet amount is 4000 kgs/hr, after one-level preheater
Temperature is increased to 75 DEG C from 20 DEG C, and after two grades of preheaters, temperature is increased to 95 DEG C, and temperature of charge at the bottom of rectifying tower is from 108 DEG C
Dropping to 70 DEG C, steam consumption is 400 kgs/hr.20 tons of neopentyl glycol solution process about 5 hours time, overhead extraction dichloro
The volume of methane is 830 liters, and the volume of petroleum ether is 550 liters.The water of overhead extraction is after water knockout drum, and wherein neopentyl glycol contains
Amount is 156 mg/litre for 9ppm and COD, and the neopentyl glycol mass fraction of extraction at the bottom of tower is 68%, wherein dichloromethane and oil
Ether concentration is 1ppm.
Embodiment 3: neopentyl glycol condensation water cleaning mother liquor inlet amount is 5000 kgs/hr, after one-level preheater
Temperature is increased to 65 DEG C from 20 DEG C, and after two grades of preheaters, temperature is increased to 92 DEG C, and temperature of charge at the bottom of rectifying tower is from 108 DEG C
Dropping to 72 DEG C, steam consumption is 550 kgs/hr.20 tons of neopentyl glycol solution process about 4 hours time, overhead extraction dichloro
The volume of methane is 850 liters, and the volume of petroleum ether is 520 liters.The water of overhead extraction is after water knockout drum, and wherein neopentyl glycol contains
Amount is 221 mg/litre for 5ppm and COD, and the dense mass fraction of neopentyl glycol of extraction at the bottom of tower is 67%, wherein dichloromethane and stone
Oil ether concentration is 1ppm.
Embodiment 4: neopentyl glycol condensation water cleaning mother liquor inlet amount is 5000 kgs/hr, after one-level preheater
Temperature is increased to 63 DEG C from 20 DEG C, and after two grades of preheaters, temperature is increased to 95 DEG C, and temperature of charge at the bottom of rectifying tower is from 110 DEG C
Dropping to 68 DEG C, steam consumption is 580 kgs/hr.20 tons of neopentyl glycol solution process about 4 hours time, overhead extraction dichloro
The volume of methane is 900 liters, and the volume of petroleum ether is 550 liters.The water of overhead extraction is after water knockout drum, and wherein neopentyl glycol contains
Amount is 250 mg/litre for 2ppm and COD, and the neopentyl glycol mass fraction of extraction at the bottom of tower is 72%, wherein dichloromethane and oil
Ether does not detects.
Embodiment 5: neopentyl glycol condensation water cleaning mother liquor inlet amount is 3000 kgs/hr, after one-level preheater
Temperature is increased to 78 DEG C from 20 DEG C, and after two grades of preheaters, temperature is increased to 95 DEG C, and temperature of charge at the bottom of rectifying tower is from 112 DEG C
Dropping to 73 DEG C, steam consumption is 350 kgs/hr.18 tons of neopentyl glycol solution process about 6 hours time, overhead extraction dichloro
The volume of methane is 700 liters, and the volume of petroleum ether is 450 liters.The water of overhead extraction is after water knockout drum, and wherein neopentyl glycol contains
Amount is 153 mg/litre for 8ppm and COD, and the neopentyl glycol mass fraction of extraction at the bottom of tower is 73%, wherein dichloromethane and oil
Ether does not detects.
Embodiment 6: neopentyl glycol condensation water cleaning mother liquor inlet amount is 3000 kgs/hr, after one-level preheater
Temperature is increased to 74 DEG C from 20 DEG C, and after two grades of preheaters, temperature is increased to 93 DEG C, and temperature of charge at the bottom of rectifying tower is from 109 DEG C
Dropping to 67 DEG C, steam consumption is 380 kgs/hr.18 tons of neopentyl glycol solution process about 6 hours time, overhead extraction dichloro
The volume of methane is 720 liters, and the volume of petroleum ether is 440 liters.The water of overhead extraction is after water knockout drum, and wherein neopentyl glycol contains
Amount is 142 mg/litre for 5ppm and COD, and the neopentyl glycol mass fraction of extraction at the bottom of tower is 70%, wherein dichloromethane and oil
Ether concentration is 1ppm.
Embodiment 7: neopentyl glycol condensation water cleaning mother liquor inlet amount is 4500 kgs/hr, after one-level preheater
Temperature is increased to 69 DEG C from 20 DEG C, and after two grades of preheaters, temperature is increased to 91 DEG C, and temperature of charge at the bottom of rectifying tower is from 110 DEG C
Dropping to 70 DEG C, steam consumption is 500 kgs/hr.18 tons of neopentyl glycol solution process about 4 hours time, overhead extraction dichloro
The volume of methane is 710 liters, and the volume of petroleum ether is 450 liters.The water of overhead extraction is after water knockout drum, and wherein neopentyl glycol contains
Amount is 285 mg/litre for 5ppm and COD, and the neopentyl glycol mass fraction of extraction at the bottom of tower is 71%, wherein dichloromethane and oil
Ether does not detects.
Embodiment 8: neopentyl glycol condensation water cleaning mother liquor inlet amount is 4500 kgs/hr, after one-level preheater
Temperature is increased to 70 DEG C from 20 DEG C, and after two grades of preheaters, temperature is increased to 88 DEG C, and temperature of charge at the bottom of rectifying tower is from 107 DEG C
Dropping to 69 DEG C, steam consumption is 520 kgs/hr.18 tons of neopentyl glycol solution process about 4 hours time, overhead extraction dichloro
The volume of methane is 730 liters, and the volume of petroleum ether is 400 liters.The water of overhead extraction is after water knockout drum, and wherein neopentyl glycol contains
Amount is 213 mg/litre for 3ppm and COD, and the neopentyl glycol mass fraction of extraction at the bottom of tower is 66%, wherein dichloromethane and oil
Ether concentration is 2ppm.
Embodiment 9: neopentyl glycol condensation water cleaning mother liquor inlet amount is 6000 kgs/hr, after one-level preheater
Temperature is increased to 72 DEG C from 20 DEG C, and after two grades of preheaters, temperature is increased to 95 DEG C, and temperature of charge at the bottom of rectifying tower is from 111 DEG C
Dropping to 72 DEG C, steam consumption is 850 kgs/hr.22 tons of neopentyl glycol solution process about 4 hours time, overhead extraction dichloro
The volume of methane is 880 liters, and the volume of petroleum ether is 530 liters.The water of overhead extraction is after water knockout drum, and wherein neopentyl glycol contains
Amount is 157 mg/litre for 4ppm and COD, and the neopentyl glycol mass fraction of extraction at the bottom of tower is 72%, wherein dichloromethane and oil
Ether does not detects.
Embodiment 10: neopentyl glycol condensation water cleaning mother liquor inlet amount is 6000 kgs/hr, after one-level preheater
Temperature is increased to 70 DEG C from 20 DEG C, and after two grades of preheaters, temperature is increased to 86 DEG C, and temperature of charge at the bottom of rectifying tower is from 115 DEG C
Dropping to 76 DEG C, steam consumption is 800 kgs/hr.22 tons of neopentyl glycol solution process about 4 hours time, overhead extraction dichloro
The volume of methane is 800 liters, and the volume of petroleum ether is 580 liters.The water of overhead extraction is after water knockout drum, and wherein neopentyl glycol contains
Amount is 108 mg/litre for 6ppm and COD, and the neopentyl glycol mass fraction of extraction at the bottom of tower is 76%, wherein dichloromethane and oil
Ether does not detects.
Claims (7)
1. the continuous treatment technological process of a neopentyl glycol condensation water cleaning mother liquor, it is characterised in that: described flow process with water and
Neopentyl glycol is primary raw material, comprises the following steps:
The first step: filter solid particle in neopentyl glycol condensation water cleaning mother liquor
Containing petroleum ether, dichloromethane organic impurities and insoluble solid particle in described neopentyl glycol condensation water cleaning mother liquor, use
Neopentyl glycol condensation water cleaning mother liquor is transported in rectifying column from storage tank by pump by filter, intercepts wherein insoluble solid
Grain, the filter residue in periodic cleaning filter, containing petroleum ether and dichloro in the neopentyl glycol condensation water cleaning mother liquor obtained after filtration
Methane；
Second step: preheating neopentyl glycol condensation water cleaning mother liquor
With the neopentyl glycol solution after concentration at the bottom of the top gaseous phase and tower of rectifying column as thermal source, pre-at described firsts and seconds
Neopentyl glycol condensation water cleaning mother liquor is heated to 85～95 DEG C from normal temperature by hot device；
3rd step: organic impurities in removing neopentyl glycol condensation water cleaning mother liquor
Neopentyl glycol condensation water cleaning mother liquor after preheating through being pumped in described rectifying column, tower bottom reboiler be passed through 0.1～
0.5MPa gauge pressure add vapours, make tower bottom pressure maintain 0.01～0.05MPa gauge pressure, tower bottom separatory body passes through reboiler
Vaporization, it is organic that the gas of rising carries out multi-stage gas-liquid mass transfer, petroleum ether and dichloromethane with dropping liq in described rectifying column
Impurity is enriched with the most in the gas phase, discharges from rectifying column gaseous phase outlet the most in gaseous form；
In rectifying column, tower top pressure maintains 0～0.01MPa gauge pressure, and the gas containing petroleum ether, dichloromethane and water passes through
Forming upper, middle and lower three layers after condensation in return tank, lower floor's dichloromethane organic phase extraction, as solvent reclaiming in original production work
Skill；Intermediate layer is back in rectifying column by pipeline containing a small amount of organic aqueous phase, carries out heat and quality with the gas phase risen
Exchange；The petroleum ether on upper strata with water enter chromatography device, chromatography device in be divided into two-phase, organic phase petroleum ether as solvent reclaiming in
Original production process；
4th step: the neopentyl glycol solution after extraction concentration
In rectifying column, owing to neopentyl glycol boiling point is high, being enriched with the most in the liquid phase and be down at the bottom of tower, a tower bottom liquid body part is led to
Crossing reboiler vaporization, another part is the neopentyl glycol after concentrating, extraction after pipeline flows through two grades of preheaters.
The continuous treatment technological process of neopentyl glycol condensation water cleaning mother liquor the most according to claim 1, it is characterised in that:
In handled neopentyl glycol condensation water cleaning mother liquor, the mass fraction of petroleum ether is 0.02～8%, the mass fraction of dichloromethane
Being 0.02～2%, the mass fraction of neopentyl glycol is 10～50%.
The continuous treatment technological process of neopentyl glycol condensation water cleaning mother liquor the most according to claim 1, it is characterised in that:
Can be with continuous treatment neopentyl glycol condensation water cleaning mother liquor.
The continuous treatment technological process of neopentyl glycol condensation water cleaning mother liquor the most according to claim 3, it is characterised in that:
Using continuous treatment technological process, processing neopentyl glycol solution required time per ton is 2～3 hours.
The continuous treatment technological process of neopentyl glycol condensation water cleaning mother liquor the most according to claim 1, it is characterised in that:
In the water steamed, neopentyl glycol mass fraction is at below 10ppm, and the rate of recovery of neopentyl glycol is more than 99.9%.
The continuous treatment technological process of neopentyl glycol condensation water cleaning mother liquor the most according to claim 1, it is characterised in that:
Using heat integrated technique, process neopentyl glycol condensation water cleaning mother liquor per ton, the steam required for rectifying column is 100～500kg.
The continuous treatment technological process of neopentyl glycol condensation water cleaning mother liquor the most according to claim 1, it is characterised in that:
The solid of calcium sulfate in neopentyl glycol condensation water cleaning mother liquor can be processed.
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| CN102336650A (en) * | 2011-07-19 | 2012-02-01 | 青岛科技大学 | Stripping process and device for removing organic impurities in brufen sodium salt |
| CN103524478A (en) * | 2013-10-24 | 2014-01-22 | 青岛科技大学 | Device and method for shortening ketalation time in ibuprofen synthesis process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107488094A (en) * | 2017-07-18 | 2017-12-19 | 青岛三瑞节能环保技术有限公司 | A kind of ibuprofen sodium salt centrifuge mother liquor petrochina ether recovery process and device |
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| CN104844420A (en) | 2015-08-19 |
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