CN104926609A - Method for processing neopentyl glycol mother liquor in ibuprofen synthesis process, and process flow thereof - Google Patents
Method for processing neopentyl glycol mother liquor in ibuprofen synthesis process, and process flow thereof Download PDFInfo
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- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 239000012452 mother liquor Substances 0.000 title claims abstract description 93
- 238000000034 method Methods 0.000 title claims abstract description 76
- 230000008569 process Effects 0.000 title claims abstract description 39
- HEFNNWSXXWATRW-UHFFFAOYSA-N Ibuprofen Chemical compound CC(C)CC1=CC=C(C(C)C(O)=O)C=C1 HEFNNWSXXWATRW-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229960001680 ibuprofen Drugs 0.000 title claims abstract description 17
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 16
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 16
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 97
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 claims abstract description 95
- 239000000463 material Substances 0.000 claims abstract description 3
- 238000000605 extraction Methods 0.000 claims description 54
- 239000007788 liquid Substances 0.000 claims description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 23
- 230000006835 compression Effects 0.000 claims description 20
- 238000007906 compression Methods 0.000 claims description 20
- 239000004744 fabric Substances 0.000 claims description 11
- 238000009833 condensation Methods 0.000 claims description 8
- 230000005494 condensation Effects 0.000 claims description 8
- 239000012141 concentrate Substances 0.000 claims description 7
- 230000000630 rising effect Effects 0.000 claims description 7
- 230000005540 biological transmission Effects 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 4
- 239000008346 aqueous phase Substances 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 2
- 239000003208 petroleum Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 description 17
- 239000002351 wastewater Substances 0.000 description 15
- 238000004821 distillation Methods 0.000 description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 239000007792 gaseous phase Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 230000008016 vaporization Effects 0.000 description 3
- 238000005917 acylation reaction Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 206010002556 Ankylosing Spondylitis Diseases 0.000 description 1
- 206010029240 Neuritis Diseases 0.000 description 1
- 230000036592 analgesia Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000013505 freshwater Substances 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 201000008482 osteoarthritis Diseases 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 201000003068 rheumatic fever Diseases 0.000 description 1
- 206010039073 rheumatoid arthritis Diseases 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention relates to a method for processing a neopentyl glycol mother liquor in an ibuprofen synthesis process. The method is characterized in the following steps: organics in the neopentyl glycol mother liquor are removed in a stripping tower; and the treated neopentyl glycol mother liquor is concentrated in a rectification tower. Reboilers are respectively arranged at the bottoms of the stripping tower and the rectification tower. A preheater is arranged at the bottom of the rectification tower, and two compressors and a condenser are arranged at the top of the rectification tower. A fresh material is heated by the preheater at the bottom of the rectification tower, and enters the stripping tower. The reboilers of the stripping tower and the rectification tower are first heated with driving steam, and then heated with the rectification tower top gas compressed by the compressor. With the process flow provided by the invention, monochloromethane, dichloromethane and petroleum ether in the neopentyl glycol mother liquor can be continuously removed, and neopentyl glycol can be concentrated.
Description
Technical field
The invention belongs to the separation field of pharmaceutical industry, be specifically related to method and the technical process thereof of neopentyl glycol mother liquor in a kind for the treatment of cloth ibuprofen synthesis procedure.
Background technology
Ibuprofen BP/EP, also known as ibuprofen, is white or off-white color crystalline powder.It has anti-inflammatory, analgesia, refrigeration function, is applicable to the diseases such as treatment rheumatic arthritis, rheumatoid arthritis, osteoarthritis, ankylosing spondylitis and neuritis.China generally adopts aryl 1; 2-position rotaring rearrangement method production technique synthesis Ibuprofen BP/EP, this technique take Isobuytel Benzene as starting raw material, first carries out Fu Ke acylation reaction with 2-chlorpromazine chloride; catalysis ketal reaction is carried out again, then through catalytically rearranging and hydrolysis reaction finally obtained finished product with neopentyl glycol.When Isobuytel Benzene and 2-chlorpromazine chloride carry out acylation reaction, need raw material to be dissolved in monochloro methane and methylene dichloride, the acidylate product be obtained by reacting is obtained by reacting condensed products with the neopentyl glycol be dissolved in sherwood oil again.After condensation reaction terminates in this technique, the neopentyl glycol mother liquor of a large amount of monochloro methanes, methylene dichloride and sherwood oil can be produced.Industrial needs process further to this mother liquor, removing monochloro methane, methylene dichloride and sherwood oil wherein be 60% to massfraction by neopentyl glycol mother liquor concentrations, are back to the condensation process of Ibuprofen BP/EP, reduction purchasing of raw materials expense.
At present, the industrial treatment process to neopentyl glycol mother liquor has: 1. equilibrium distillation method: first neopentyl glycol mother liquor is transported to a volume with pump and is 5 cubic metres and in the equilibrium distillation tank of jacketed, then in chuck, pass into live steam heating neopentyl glycol mother liquor, along with the rising of mother liquor temperature in retort, monochloro methane, methylene dichloride, sherwood oil and water are assembled at retort top gradually with gaseous phase, system is left with liquid form, the neopentyl glycol solution after pot liquid is mainly concentrated by after this portion gas condensation, 2. vaporizing extract process: neopentyl glycol mother liquor is transported in a stripping tower with pump, in the tower bottom reboiler of stripping tower, pass into live steam heat neopentyl glycol mother liquor, along with the rising of neopentyl glycol mother liquor temperature, monochloro methane, methylene dichloride, sherwood oil and water carry out the balanced exchange of multistage quality and heat with the neopentyl glycol mother liquor declined in gaseous phase and tower on column plate or filler, monochloro methane, methylene dichloride, sherwood oil and water are assembled at stripper top gradually with gaseous phase, stripping tower is discharged by after this portion gas condensation, neopentyl glycol after being concentrated is by extraction bottom stripping tower, 3. simple rectification method: neopentyl glycol mother liquor is transported in a rectifying tower with pump, in the tower bottom reboiler of rectifying tower, pass into live steam heat neopentyl glycol mother liquor, along with the rising of neopentyl glycol mother liquor temperature, monochloro methane, methylene dichloride, sherwood oil and water carry out the balanced exchange of multistage quality and heat with the neopentyl glycol mother liquor declined in gaseous phase and tower on column plate or filler, monochloro methane, methylene dichloride, sherwood oil and water are assembled at rectifying tower top gradually with gaseous phase, by this portion gas by flowing in return tank after condenser condenses, with pump, the liquid part in return tank is input to rectifying tower inside to reflux, another part is with liquid state extraction, neopentyl glycol after being concentrated is by rectifier bottoms extraction.
Mainly there is following problem in current three kinds of conventional treatment processs.The first, equilibrium distillation method: 1. neopentyl glycol loss amount is large, and neopentyl glycol massfraction average out to 3% in the waste water of equilibrium distillation tank top extraction, processes neopentyl glycol mother liquor per ton, loss neopentyl glycol quality is 20 ~ 30 kilograms; 2. the operational cycle is long, and equilibrium distillation method adopts intermittent operation process neopentyl glycol mother liquor, and the mother liquor processing 5 tons on average needs 8 hours; 3. in the waste water steamed, chemical oxygen demand (COD) (COD) is high, often processes one ton of neopentyl glycol mother liquor, on average steams the waste water of 0.8 cubic metre, COD average out to 2500 mg/litre in this waste water.Second, vaporizing extract process: the secondary waste water difficult treatment that stripper overhead steams, containing monochloro methane, methylene dichloride, sherwood oil, water and massfraction in the waste water that tower top steams is the neopentyl glycol of 1% ~ 2%, because the boiling point of neopentyl glycol is higher and to account for the ratio of total COD large than water, the further process of the neopentyl glycol therefore in waste water to waste water causes difficulty.3rd, simple rectification method: the waste water that tower top steams needs through secondary treatment, main containing monochloro methane, methylene dichloride, sherwood oil and water in the waste water of overhead extraction, need that secondary treatment is carried out to it and reclaim monochloro methane wherein, methylene dichloride, sherwood oil organism reduce COD to reaching emission standard.
Summary of the invention
Instant invention overcomes the deficiencies in the prior art, develop method and the technical process thereof of neopentyl glycol mother liquor in a kind for the treatment of cloth ibuprofen synthesis procedure, energy efficient recovery monochloro methane wherein, methylene dichloride, sherwood oil, concentrated neopentyl glycol solution makes the massfraction of neopentyl glycol be 60% ~ 90%.
Technical scheme of the present invention is: a kind of method of neopentyl glycol mother liquor in treatment cloth ibuprofen synthesis procedure, first described method utilizes stripping tower to remove organism in neopentyl glycol mother liquor, recycling rectifying tower concentrates the neopentyl glycol mother liquor after stripping tower process, reboiler is respectively equipped with at the bottom of described stripping tower and rectifying tower, separately preheater is provided with at the bottom of described rectifying tower, tower top is provided with two compressors and a condenser, fresh material enters stripping tower after the preheater preheats at the bottom of described rectifying tower, the reboiler of described stripping tower and the reboiler of described rectifying tower are first by driving steam heating, heated by the rectifying tower top gaseous body after compressor compresses again.
A technical process for neopentyl glycol mother liquor in treatment cloth ibuprofen synthesis procedure, described flow process, comprises the following steps wherein containing monochloro methane, methylene dichloride, sherwood oil, water and neopentyl glycol for raw material with neopentyl glycol mother liquor:
The first step: preheating neopentyl glycol mother liquor
Pending neopentyl glycol mother liquor temperature is 25 ~ 35 DEG C, and with Produced Liquid at the bottom of described rectifying tower for thermal source, after preheater at the bottom of rectifying tower, neopentyl glycol mother liquor temperature reaches 70 ~ 90 DEG C;
Second step: remove the organism in neopentyl glycol mother liquor
Neopentyl glycol mother liquor after preheating enters in tower by pipeline by described stripping tower is middle, described stripper overhead pressure is 0.00 ~ 0.02Mpa (gauge pressure), first be that 0.1 ~ 0.3MPa drives steam after compressor compresses to gauge pressure is 0.5 ~ 0.6MPa to described stripping tower tower bottom reboiler heating by gauge pressure, along with the rising of fluid temperature at the bottom of tower, monochloro methane in neopentyl glycol mother liquor, methylene dichloride, sherwood oil, water and neopentyl glycol rise to tower top with gas form gradually, the gas risen and the interior liquid declined of tower carry out the transmission of multistage quality and heat, tower top monochloro methane, methylene dichloride, sherwood oil and water are drawn with gas form flow into stripper overhead return tank after condensation, three layers are divided in return tank, upper strata is the mixture of sherwood oil and monochloro methane, by the extraction of return tank top, lower floor is that methylene dichloride is by the extraction of return tank bottom, the aqueous phase in middle layer returns in stripping tower by return line, continue to realize multi-stage gas-liquid with the gas risen to balance, when described stripping tower column bottom temperature reaches 102 ~ 106 DEG C, neopentyl glycol mother liquor after extraction process at the bottom of tower, in neopentyl glycol mother liquor after described process, the massfraction of monochloro methane is 0 ~ 2ppm, methylene dichloride massfraction is 0 ~ 2ppm, sherwood oil content is 0 ~ 3ppm,
3rd step: concentrated neopentyl glycol mother liquor after stripping tower process
The neopentyl glycol mother liquor of extraction at the bottom of stripping tower tower by pump delivery in described rectifying tower, described rectifying tower pressure on top surface is 0.00 ~ 0.02Mpa (gauge pressure), first be that 0.1 ~ 0.3MPa drives steam after compressor compresses to gauge pressure is 0.5 ~ 0.6MPa to described rectifying tower tower bottom reboiler heating by gauge pressure, along with the rising of fluid temperature at the bottom of tower, water and neopentyl glycol rise to tower top with gas form gradually, the gas risen and the interior liquid declined of tower carry out the transmission of multistage quality and heat, when described rectifying tower tower top temperature reaches 100 ~ 105 DEG C, stop the driving steam for described stripping tower and the heating of rectifying tower tower bottom reboiler, rectifying tower top gaseous body is given after two compressor compresses to gauge pressure is 0.5 ~ 0.6MPa stripping tower tower bottom reboiler and the heating of rectifying tower tower bottom reboiler, by the residual gas after reboiler again through rectifying tower tower top condenser condenses, the liquid of cooling flow in return tank, liquid portion in return tank returns in rectifying tower by return line, another part liquid is by pipeline extraction, when described rectifying tower column bottom temperature reaches 106 ~ 128 DEG C, neopentyl glycol massfraction at the bottom of tower is 60% ~ 90%, at the bottom of tower extraction concentrate after neopentyl glycol mother liquor, described concentrated after neopentyl glycol mother liquor in the massfraction of monochloro methane be 0 ~ 100ppb, methylene dichloride massfraction is 0 ~ 100ppb, sherwood oil content is 0 ~ 200ppb, extraction at the bottom of tower concentrated after neopentyl glycol mother liquor temperature after preheater at the bottom of described rectifying tower drop to 95 ~ 102 DEG C.
The principle that the present invention realizes is:
Containing monochloro methane, methylene dichloride, sherwood oil, water and neopentyl glycol in pending neopentyl glycol mother liquor.The present invention first removes the organism in neopentyl glycol mother liquor by stripping tower, organism is capable of circulation for former synthesis procedure after stripper overhead extraction, the neopentyl glycol mother liquor of extraction at the bottom of stripping tower tower is input to rectifying tower by pump again and concentrates neopentyl glycol mother liquor, and the neopentyl glycol massfraction after concentrated is 60% ~ 90%.First will be the reboiler heating of stripping tower and rectifying tower after driving vapour compression, the gas formed in two towers rises along body, reach multi-stage gas-liquid with the liquid declined to balance and carry out quality and heat transmission, finally, light constituent in tower in tower top enrichment after condenser condenses, partial reflux, another part is from return tank extraction.When rectifying tower tower top temperature reaches 100 ~ 105 DEG C, stop driving steam, the tower bottom reboiler heat supply of stripping tower and rectifying tower is given respectively after the gas compression utilizing compressor to be risen by tower top, realize effective utilization of matter and energy, by the gas of stripping tower and rectifying tower tower bottom reboiler, then after rectifying tower tower top condenser condenses, enter backflow and the extraction that return tank realizes tower top.
The present invention has following beneficial effect:
(1) the present invention decreases the loss amount of neopentyl glycol in process neopentyl glycol mother liquor process.The equilibrium distillation method of current employing, the massfraction average out to 3% of neopentyl glycol in the waste water steamed, processes the neopentyl glycol of neopentyl glycol mother liquor per ton loss 20 ~ 30 kilograms.The present invention adopts the method for first stripping rectifying again, and first remove the monochloro methane in neopentyl glycol mother liquor, methylene dichloride, sherwood oil organism, in the organism removed, the content of neopentyl glycol is 200 ~ 300ppb; Neopentyl glycol mother liquor after removing enters rectifying tower again and concentrates, by moisture wherein from the extraction of rectifying tower top, in the water of extraction, neopentyl glycol content is 1 ~ 3ppm, and relative to equilibrium distillation method, process of the present invention neopentyl glycol mother liquor per ton can reclaim neopentyl glycol 18 ~ 29 kilograms more.
(2) present invention saves the treatment time of neopentyl glycol mother liquor.Equilibrium distillation method batch process neopentyl glycol mother liquor, the neopentyl glycol mother liquor processing 5 tons needs 8 hours.The present invention adopts continuous treatment technology, per hourly processes 3 ~ 5 kilograms, neopentyl glycol mother liquor, and the neopentyl glycol mother liquor processing 5 tons only needs 1.0 ~ 1.7 hours.
(3) present invention saves amount of steam, reduce production run cost.Present invention employs height heat integrated technology, utilize the neopentyl glycol mother liquor that at the bottom of rectifying tower, hot logistics preheating is fresh on the one hand, utilize compressor compresses rectifying tower top gaseous body on the other hand, provide heat to stripping tower and rectifying tower tower bottom reboiler.When utilizing driving steam heating, processing neopentyl glycol mother liquor live steam consumption per ton is 600 ~ 800 kilograms, and when utilizing the overhead gas after compression to provide heat, do not need fresh water steam, quantity of steam and the plant running time of saving are proportionate.
(4) present invention reduces the COD value steamed in waste water.Existing equilibrium distillation method, vaporizing extract process and simple rectification method are when processing neopentyl glycol mother liquor, and containing monochloro methane, methylene dichloride, sherwood oil and neopentyl glycol organism in the waste water steamed, the COD value of this waste water is 200000 ~ 300000 mg/litre.Continuous treatment neopentyl glycol mother liquor of the present invention, the organism first removed wherein concentrates neopentyl glycol mother liquor again, the organism removed is capable of circulation for former synthesis technique, in the neopentyl glycol mother liquor removed, the massfraction of monochloro methane is 0 ~ 2ppm, methylene dichloride massfraction is 0 ~ 2ppm, and sherwood oil content is 0 ~ 3ppm, after this mother liquor concentrations, in the waste water steamed, neopentyl glycol content is 1 ~ 3ppm, and its COD is 500 ~ 800 mg/litre.
Accompanying drawing explanation
Accompanying drawing is structural representation of the present invention.
In figure, 1. stripping tower; 2. condenser; 3. return tank; 4. reboiler; 5. rectifying tower; 6. compressor; 7. preheater.
Embodiment
Further illustrate below in conjunction with accompanying drawing, and unrestricted scope involved in the present invention.
As shown in drawings, first the present invention adopts and drives steam after compressor 6 compresses for the reboiler 4 of stripping tower and rectifying tower provides heat.Fresh neopentyl glycol mother liquor enters stripping tower 1 after preheater at the bottom of rectifying tower 7 preheating, neopentyl glycol mother liquor reaches multi-stage gas-liquid balance in stripping tower 1, monochloro methane, methylene dichloride, sherwood oil and water flow into return tank 3 from tower top extraction with gas form after condenser 2 condensation, the liquid of condensation is divided into three layers in return tank, monochloro methane and sherwood oil are from upper strata extraction, methylene dichloride is from lower floor's extraction, and middle layer aqueous phase returns stripping tower 1 through return line.Neopentyl glycol mother liquor after stripping tower process enters rectifying tower 5 after extraction at the bottom of tower, when rectifying tower 5 tower top temperature reaches 100 ~ 105 DEG C, stop driving steam, the gas of compressor compresses rectifying tower 5 tower top is utilized to heat to stripping tower and rectifying tower tower bottom reboiler 4, after condenser 2 condensation, return tank 3 is being entered by the gas of reboiler 4, in return tank, partially liq returns rectifying tower 5 by return line, all the other liquid are plucked out of, neopentyl glycol mother liquor after concentrated, from extraction at the bottom of rectifying tower 5 tower, enters finished product storage tank after flowing through preheater 7.
Below specific embodiment of the invention example:
Embodiment 1: neopentyl glycol mother liquid flow rate is 3500 kgs/hr, after preheater preheats, temperature is elevated to 76.4 DEG C from 25.5 DEG C, and rectifying tower column bottom temperature is reduced to 97.3 DEG C from 121.6 DEG C.Driving vapor pressure is 0.12Mpa, and flow is 2100 kgs/hr, and after compression, the pressure of live steam is 0.51Mpa, and temperature is 151.9 DEG C.The monochloro methane quality of stripper overhead extraction is 120.2 kilograms, and methylene dichloride quality is 119.1 kilograms, and sherwood oil quality is 90.0 kilograms.When rectifying tower tower top temperature reaches 103.7 DEG C, stop driving steam, compression rectifying tower top gaseous body makes that its pressure is 0.55Mpa, temperature is to stripping tower and the heating of rectifying tower tower bottom reboiler after 155.5 DEG C, in the water of rectifying tower overhead extraction, neopentyl glycol mass content is 1.1ppm, its COD value is 765 mg/litre, the neopentyl glycol massfraction of extraction at the bottom of tower is 86.2%, and wherein monochloro methane, methylene dichloride and sherwood oil content do not detect.
Embodiment 2: neopentyl glycol mother liquid flow rate is 3700 kgs/hr, after preheater preheats, temperature is elevated to 72.2 DEG C from 27.4 DEG C, and rectifying tower column bottom temperature is reduced to 95.2 DEG C from 108.1 DEG C.Driving vapor pressure is 0.14Mpa, and flow is 2220 kgs/hr, and after compression, the pressure of live steam is 0.52Mpa, and temperature is 153.4 DEG C.The monochloro methane quality of stripper overhead extraction is 110.5 kilograms, and methylene dichloride quality is 124.5 kilograms, and sherwood oil quality is 94.1 kilograms.When rectifying tower tower top temperature reaches 104.8 DEG C, stop driving steam, compression rectifying tower top gaseous body makes that its pressure is 0.54Mpa, temperature is to stripping tower and the heating of rectifying tower tower bottom reboiler after 154.8 DEG C, in the water of rectifying tower overhead extraction, neopentyl glycol mass content is 1.3ppm, its COD value is 558 mg/litre, the neopentyl glycol massfraction of extraction at the bottom of tower is 66.5%, and wherein monochloro methane content is 92ppb, methylene dichloride content is 84ppb, sherwood oil content is 165ppb.
Embodiment 3: neopentyl glycol mother liquid flow rate is 5000 kgs/hr, after preheater preheats, temperature is elevated to 75.1 DEG C from 35.2 DEG C, and rectifying tower column bottom temperature is reduced to 99.6 DEG C from 126.2 DEG C.Driving vapor pressure is 0.15Mpa, and flow is 3100 kgs/hr, and after compression, the pressure of live steam is 0.58Mpa, and temperature is 157.6 DEG C.The monochloro methane quality of stripper overhead extraction is 110.5 kilograms, and methylene dichloride quality is 124.5 kilograms, and sherwood oil quality is 94.1 kilograms.When rectifying tower tower top temperature reaches 104.1 DEG C, stop driving steam, compression rectifying tower top gaseous body makes that its pressure is 0.60Mpa, temperature is to stripping tower and the heating of rectifying tower tower bottom reboiler after 158.9 DEG C, in the water of rectifying tower overhead extraction, neopentyl glycol mass content is 1.5ppm, its COD value is 553 mg/litre, the neopentyl glycol massfraction of extraction at the bottom of tower is 89.2%, and wherein monochloro methane, methylene dichloride and sherwood oil content do not detect.
Embodiment 4: neopentyl glycol mother liquid flow rate is 3350 kgs/hr, after preheater preheats, temperature is elevated to 82.5 DEG C from 25.2 DEG C, and rectifying tower column bottom temperature is reduced to 95.8 DEG C from 114.8 DEG C.Driving vapor pressure is 0.17Mpa, and flow is 2640 kgs/hr, and after compression, the pressure of live steam is 0.53Mpa, and temperature is 154.1 DEG C.The monochloro methane quality of stripper overhead extraction is 113.5 kilograms, and methylene dichloride quality is 95.9 kilograms, and sherwood oil quality is 79.6 kilograms.When rectifying tower tower top temperature reaches 102.3 DEG C, stop driving steam, compression rectifying tower top gaseous body makes that its pressure is 0.58Mpa, temperature is to stripping tower and the heating of rectifying tower tower bottom reboiler after 157.6 DEG C, in the water of rectifying tower overhead extraction, neopentyl glycol mass content is 1.8ppm, its COD value is 694 mg/litre, the neopentyl glycol massfraction of extraction at the bottom of tower is 79.8%, and wherein monochloro methane content is 15ppb, methylene dichloride content is 76ppb, sherwood oil content is 146ppb.
Embodiment 5: neopentyl glycol mother liquid flow rate is 3260 kgs/hr, after preheater preheats, temperature is elevated to 79.2 DEG C from 27.1 DEG C, and rectifying tower column bottom temperature is reduced to 97.2 DEG C from 113.4 DEG C.Driving vapor pressure is 0.16Mpa, and flow is 2530 kgs/hr, and after compression, the pressure of live steam is 0.53Mpa, and temperature is 154.1 DEG C.The monochloro methane quality of stripper overhead extraction is 107.8 kilograms, and methylene dichloride quality is 119.7 kilograms, and sherwood oil quality is 76.6 kilograms.When rectifying tower tower top temperature reaches 101.9 DEG C, stop driving steam, compression rectifying tower top gaseous body makes that its pressure is 0.57Mpa, temperature is to stripping tower and the heating of rectifying tower tower bottom reboiler after 156.9 DEG C, in the water of rectifying tower overhead extraction, neopentyl glycol mass content is 1.9ppm, its COD value is 594 mg/litre, the neopentyl glycol massfraction of extraction at the bottom of tower is 77.8%, and wherein monochloro methane and methylene dichloride content do not detect, and sherwood oil content is 108ppb.
Embodiment 6: neopentyl glycol mother liquid flow rate is 4390 kgs/hr, after preheater preheats, temperature is elevated to 74.7 DEG C from 32.8 DEG C, and rectifying tower column bottom temperature is reduced to 98.1 DEG C from 117.1 DEG C.Driving vapor pressure is 0.14Mpa, and flow is 3280 kgs/hr, and after compression, the pressure of live steam is 0.55Mpa, and temperature is 155.5 DEG C.The monochloro methane quality of stripper overhead extraction is 113.9 kilograms, and methylene dichloride quality is 93.5 kilograms, and sherwood oil quality is 94.0 kilograms.When rectifying tower tower top temperature reaches 102.7 DEG C, stop driving steam, compression rectifying tower top gaseous body makes that its pressure is 0.56Mpa, temperature is to stripping tower and the heating of rectifying tower tower bottom reboiler after 156.2 DEG C, in the water of rectifying tower overhead extraction, neopentyl glycol mass content is 1.1ppm, its COD value is 635 mg/litre, the neopentyl glycol massfraction of extraction at the bottom of tower is 79.2%, and wherein monochloro methane content is 45ppb, methylene dichloride content is 20ppb, sherwood oil content is 180ppb.
Embodiment 7: neopentyl glycol mother liquid flow rate is 4120 kgs/hr, after preheater preheats, temperature is elevated to 78.6 DEG C from 33.9 DEG C, and rectifying tower column bottom temperature is reduced to 97.8 DEG C from 114.6 DEG C.Driving vapor pressure is 0.16Mpa, and flow is 3260 kgs/hr, and after compression, the pressure of live steam is 0.52Mpa, and temperature is 153.4 DEG C.The monochloro methane quality of stripper overhead extraction is 113.3 kilograms, and methylene dichloride quality is 114.4 kilograms, and sherwood oil quality is 79.9 kilograms.When rectifying tower tower top temperature reaches 102.1 DEG C, stop driving steam, compression rectifying tower top gaseous body makes that its pressure is 0.55Mpa, temperature is to stripping tower and the heating of rectifying tower tower bottom reboiler after 155.5 DEG C, in the water of rectifying tower overhead extraction, neopentyl glycol mass content is 2.9ppm, its COD value is 598 mg/litre, the neopentyl glycol massfraction of extraction at the bottom of tower is 79.5%, and wherein monochloro methane content is 66ppb, methylene dichloride content is 41ppb, sherwood oil content is 114ppb.
Embodiment 8: neopentyl glycol mother liquid flow rate is 4830 kgs/hr, after preheater preheats, temperature is elevated to 76.3 DEG C from 34.6 DEG C, and rectifying tower column bottom temperature is reduced to 96.3 DEG C from 112.3 DEG C.Driving vapor pressure is 0.19Mpa, and flow is 3020 kgs/hr, and after compression, the pressure of live steam is 0.50Mpa, and temperature is 151.9 DEG C.The monochloro methane quality of stripper overhead extraction is 105.4 kilograms, and methylene dichloride quality is 112.6 kilograms, and sherwood oil quality is 77.6 kilograms.When rectifying tower tower top temperature reaches 104.2 DEG C, stop driving steam, compression rectifying tower top gaseous body makes that its pressure is 0.53Mpa, temperature is to stripping tower and the heating of rectifying tower tower bottom reboiler after 154.1 DEG C, in the water of rectifying tower overhead extraction, neopentyl glycol mass content is 2.7ppm, its COD value is 598 mg/litre, the neopentyl glycol massfraction of extraction at the bottom of tower is 76.1%, and wherein monochloro methane content is 60ppb, methylene dichloride content is 55ppb, sherwood oil content is 171ppb.
Claims (6)
1. the method for neopentyl glycol mother liquor in a treatment cloth ibuprofen synthesis procedure, it is characterized in that: first utilize stripping tower to remove organism in neopentyl glycol mother liquor, recycling rectifying tower concentrates the neopentyl glycol mother liquor after stripping tower process, reboiler is respectively equipped with at the bottom of described stripping tower and rectifying tower, preheater is provided with at the bottom of described rectifying tower, tower top is provided with two compressors and a condenser, fresh material enters stripping tower after the preheater preheats at the bottom of described rectifying tower, the reboiler of described stripping tower and the reboiler of described rectifying tower are first by driving steam heating, heated by the rectifying tower top gaseous body after compressor compresses again.
2. the technical process of neopentyl glycol mother liquor in treatment cloth ibuprofen synthesis procedure, described flow process, comprises the following steps wherein containing monochloro methane, methylene dichloride, sherwood oil, water and neopentyl glycol for raw material with neopentyl glycol mother liquor:
The first step: preheating neopentyl glycol mother liquor
Pending neopentyl glycol mother liquor temperature is 25 ~ 35 DEG C, and with Produced Liquid at the bottom of described rectifying tower for thermal source, after preheater at the bottom of rectifying tower, neopentyl glycol mother liquor temperature reaches 70 ~ 90 DEG C;
Second step: remove the organism in neopentyl glycol mother liquor
Neopentyl glycol mother liquor after preheating enters in tower by pipeline by described stripping tower is middle, described stripper overhead pressure is 0.00 ~ 0.02Mpa (gauge pressure), first be that 0.1 ~ 0.3MPa drives steam after compressor compresses to gauge pressure is 0.5 ~ 0.6MPa to described stripping tower tower bottom reboiler heating by gauge pressure, along with the rising of fluid temperature at the bottom of tower, monochloro methane in neopentyl glycol mother liquor, methylene dichloride, sherwood oil, water and neopentyl glycol rise to tower top with gas form gradually, the gas risen and the interior liquid declined of tower carry out the transmission of multistage quality and heat, tower top monochloro methane, methylene dichloride, sherwood oil and water are drawn with gas form and after condensation, are flow into stripper overhead return tank, three layers are divided in return tank, upper strata is the mixture of sherwood oil and monochloro methane, by the extraction of return tank top, lower floor is methylene dichloride, by the extraction of return tank bottom, the aqueous phase in middle layer returns in stripping tower by return line, continue to realize multi-stage gas-liquid with the gas risen to balance, when described stripping tower column bottom temperature reaches 102 ~ 106 DEG C, neopentyl glycol mother liquor after extraction process at the bottom of tower, in neopentyl glycol mother liquor after described process, the massfraction of monochloro methane is 0 ~ 2ppm, methylene dichloride massfraction is 0 ~ 2ppm, sherwood oil content is 0 ~ 3ppm,
3rd step: concentrated neopentyl glycol mother liquor after stripping tower process
The neopentyl glycol mother liquor of extraction at the bottom of stripping tower tower by pump delivery in described rectifying tower, described rectifying tower pressure on top surface is 0.00 ~ 0.02Mpa (gauge pressure), first be that 0.1 ~ 0.3MPa drives steam after compressor compresses to 0.5 ~ 0.6MPa to described rectifying tower tower bottom reboiler heating by gauge pressure, along with the rising of fluid temperature at the bottom of tower, water and neopentyl glycol rise to tower top with gas form gradually, the gas risen and the interior liquid declined of tower carry out the transmission of multistage quality and heat, when described rectifying tower tower top temperature reaches 100 ~ 105 DEG C, stop the driving steam for described stripping tower and the heating of rectifying tower tower bottom reboiler, rectifying tower top gaseous body is given after two compressor compresses to gauge pressure is 0.5 ~ 0.6MPa stripping tower tower bottom reboiler and the heating of rectifying tower tower bottom reboiler, by the residual gas after reboiler again through rectifying tower tower top condenser condenses, the liquid of cold one-tenth flow in return tank, liquid portion in return tank returns in rectifying tower by return line, another part liquid is by pipeline extraction, when described rectifying tower column bottom temperature reaches 106 ~ 128 DEG C, neopentyl glycol massfraction at the bottom of tower is 60% ~ 90%, at the bottom of tower extraction concentrate after neopentyl glycol mother liquor, described concentrated after neopentyl glycol mother liquor in the massfraction of monochloro methane be 0 ~ 100ppb, methylene dichloride massfraction is 0 ~ 100ppb, sherwood oil content is 0 ~ 200ppb, extraction at the bottom of tower concentrated after neopentyl glycol mother liquor temperature after preheater at the bottom of described rectifying tower drop to 95 ~ 102 DEG C.
3. the technical process of neopentyl glycol mother liquor in a kind for the treatment of cloth ibuprofen synthesis procedure according to claim 2, it is characterized in that: in handled neopentyl glycol mother liquor, monochloro methane massfraction is 0.02% ~ 4.50%, methylene dichloride massfraction is 0.02% ~ 4.50%, sherwood oil massfraction is 0.02% ~ 3.50%, and the massfraction of neopentyl glycol is 10% ~ 55%.
4. the technical process of neopentyl glycol mother liquor in a kind for the treatment of cloth ibuprofen synthesis procedure according to claim 2, is characterized in that: adopt continuous treatment technical process, treatment capacity is 500 ~ 5000 kgs/hr.
5. the technical process of neopentyl glycol mother liquor in a kind for the treatment of cloth ibuprofen synthesis procedure according to claim 2, it is characterized in that: first utilize and drive steam to described stripping tower and the heating of rectifying tower tower bottom reboiler, the rectifying tower top gaseous body after recycling compression gives described stripping tower and the heating of rectifying tower tower bottom reboiler.
6. the technical process of neopentyl glycol mother liquor in a kind for the treatment of cloth ibuprofen synthesis procedure according to claim 5, is characterized in that: the reboiler of adopt two compressors to compress respectively reboiler that described rectifying tower top gaseous body is described stripping tower and described rectifying tower provides heat.
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| CN108285403A (en) * | 2018-03-24 | 2018-07-17 | 青岛科技大学 | Recycling petroleum ether and chlorhydrin energy saving technique in a kind of ibuprofen sodium salt centrifuge mother liquor |
| CN110615494A (en) * | 2019-10-31 | 2019-12-27 | 吴嘉 | Post-treatment device and method for complex DMF wastewater after DMF recovery |
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| CN110615494B (en) * | 2019-10-31 | 2023-11-10 | 格琳嘉(杭州)科技发展有限公司 | Post-treatment device and method for complex DMF wastewater after DMF recovery |
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