CN101585755A - Method for recovering acetone from volatile mixed gas of solvent discharged from vacuum system - Google Patents

Method for recovering acetone from volatile mixed gas of solvent discharged from vacuum system Download PDF

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CN101585755A
CN101585755A CNA2008101121741A CN200810112174A CN101585755A CN 101585755 A CN101585755 A CN 101585755A CN A2008101121741 A CNA2008101121741 A CN A2008101121741A CN 200810112174 A CN200810112174 A CN 200810112174A CN 101585755 A CN101585755 A CN 101585755A
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gas
liquid
acetone
recovery
vacuum
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CN101585755B (en
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马杰
王军晖
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Abstract

The invention discloses a method for recovering acetone from volatile mixed gas of a solvent discharged from a vacuum system. An acetone recovery system consists of the vacuum system, an on-site gas recovery system, a gas collection system, a recovery system and a control system, the process comprises the steps of gas collection, first gas-liquid separation, secondary gas-liquid separation, gas-liquid heat exchange absorption, acetone recovery and the like, gas after the recovery is realized is directly discharged, and the acetone is recovered through a distillator after a recovered absorption liquid reaches certain concentration. The method has the advantages of simple and convenient operation, simple process, high recovery efficiency and recovery purity of an acetone solvent, high economical benefit, and suitable popularization and application, and ensures that the gas and liquid discharge after the recovery satisfies the environmental protection standard.

Description

From the volatile mixed gas of solvent that vacuum system is discharged, reclaim the method for acetone
Affiliated technical field
The present invention relates to pharmaceutical chemistry technical field, specifically relate to a kind of method that from the volatile mixed gas of solvent that vacuum system is discharged, reclaims acetone.
Background technology
In the production process of medication chemistry production and other relevant industries, post-processed method for bulk drug and other products, generally be to adopt solvent washing, vacuum filtration, vacuum drying traditional technology method, solvent and moisture content are taken away to reach washing and drying purpose by vacuum during this period.What the solvent washings then adopted is acetone solvent, will vapor away a large amount of acetone solvents in the traditional processing technology method, not only causes the waste of acetone solvent and improves production cost, and the acetone solvent volatilization gas also pollutes production environment simultaneously.Now, the manufacturing enterprise that this area is relevant has recognized this problem, having adopted some recovery technology means that the acetone solvent volatilization gas is carried out reclaims, but, reasons such as amount of inert gas is bigger reclaim failure owing to having caused, yield is low or recovery value less than energy waste, thereby lost the value of solvent recuperation.One of recovery method commonly used now is a condensation method, selects spiral plate type or tubular heat exchange for use, makes heat-eliminating medium with icy salt solution, and acetone is reclaimed in condensation.This method of discovery can not be given full play to its usefulness between the actual usage period, is embodied in acetone gas and can not fully be condensed into liquid after cooling.Reason is the cooling area (cooling area in the unit volume) of interchanger and, makes in solution-air thermal exchange process that interchanger can not cause and reclaim failure the abundant heat exchange of gas much smaller than required amount of cooling water.If reach the ideal recovering effect, will enlarge the cooling area of several times interchanger, thereby increase huge investment, even but reached heat interchanging area because the cold of needs of production is very big, its huge cost of investment has also been offset the value of recovered solvent.Except condensation method, now also use a kind of carbon fiber absorption method to be used for the recovery of solvent, its action principle is to utilize the physical property of the easy desorption of the anti-absorption of activated carbon fiber to do medium, employing water vapour is desorbing agent, bring the organic solvent desorption that is adsorbed in the activated carbon fiber into drainer,, organic solvent and mixture of steam condensation are got off to enter the layering groove through condensation, by gravity settling separation, reach the purpose of solvent recuperation.This scheme is used for not the solvent recuperation system of dissolving each other with water mostly, if use in the system of dissolving each other with water then still need to carry out distillation procedure.Also there are a lot of potential potential safety hazards simultaneously in the energy consumption height that this method needs.So this difficult problem of acetone is reclaimed in rationally economic as early as possible solution from the acetone solvent volatile mixed gas, be the vital task that the present technique field faces.
Summary of the invention
The objective of the invention is to overcome the above-mentioned deficiency that from solvent mixture, reclaims on the acetone prior art, provide a kind of easy and simple to handle, technology simple and organic efficiency and reclaim the high a kind of method that reclaims acetone from the volatile mixed gas of solvent that vacuum system is discharged of purity.
In order to achieve the above object, the present invention adopts following technical scheme, a kind of method that from the volatile mixed gas of solvent that vacuum system is discharged, reclaims acetone, form the acetone recovery system by vacuum system, gas production on the throne system, gas gathering system, gas treating system and Controlling System, its concrete process flow steps is as follows:
A. gas collecting:
The gas of vacuum system discharging is introduced gas production on the throne system by the gas collecting pump in the gas production on the throne system, and the gravity flow of the circulating liquid in the vacuum system enters gas production on the throne system;
B. gas-liquid flash liberation
The gas that enters gas production on the throne system pumps into gas gathering system by the gas production pump in the gas gathering system, and liquid then pumps into gas gathering system by liquid; Thereby separate the first time that is implemented in gas liquid in the gas production on the throne system;
C. gas-liquid secondary separation
Gas in the gas gathering system enters recovery system from the bottom, and liquid pumps into the top of recovery system by liquor pump, realizes the gas-liquid secondary separation in gas gathering system;
D. gas-liquid heat exchange absorbs
The liquid that pumps into recovery system is by the mixed gases in the spray of the spray equipment on the rectifying column in recovery system back and the recovery system, the heat exchange of finishing gas and liquid absorbs, directly discharge through the gas after the liquid heat exchange absorption, after absorption liquid after the process liquid heat exchange absorbs then is back to the gas collecting system, enter vacuum system once more and realize recycling, the absorption liquid temperature is lower than 15 ℃;
E. carrying out acetone reclaims
Absorption liquid through after the cycle heat exchange absorption after its concentration reaches 10%---30%, both can be discharged on the distiller in the recovery system, carried out acetone and reclaimed.
PLC (programmable logic controller) Controlling System is adopted in the operation control of above-mentioned vacuum system, gas production on the throne system, gas gathering system, gas recovery system.
Vacuum system among the above-mentioned described step a is made up of Lodz vacuum pump, water ring vacuum pump, gas-liquid separator, pipeline and valve, and the operating mode of vacuum system is: rate of air sucked in required: 150-300L/s; Vacuum tightness is greater than 95%; Vacuum pump water ring flow be the 0.6-1 cubic meter per hour; The water ring temperature is less than 35 ℃;
Gas collecting on the throne system among the above-mentioned described step b is made up of with pipeline and valve the combined type surge tank that over-pass, liquid level control, gas collecting pump constitute; The pressure of its liquid is that 1-2kg pressure, temperature are less than 35 ℃;
Gas collector among the above-mentioned described step c is to have increased interchanger on gas collecting system-based on the throne.
Recovery system in the above-mentioned described steps d is made up of rectifying column and corresponding instrument piping and valve, and the structure of rectifying column is by Stainless Steel Helices and column plate is compound constitutes, and comprises packing section, column plate section and liquid spraying device, and the pressure in the recovery system is 3-5Kg.
Principle of work of the present invention is, the exhaust of several vacuum systems and waste water are introduced gas collecting on the throne system, gas is pumped into gas collecting on the throne system from vaccum exhaust outlet under the suction function of gas collecting pump, and liquid gravity flow enters gas production also on the throne system, because the different specific weight of gas and liquid, realize gas-liquid separation by the combined type surge tank in the gas production on the throne system, sent into gas gathering system by gas pump and liquor pump respectively through gas-liquid after the flash liberation, carry out the cycling hot exchange by the interchanger in the gas gathering system, then gas be pumped to rectifying column in the recovery system the bottom, liquid is pumped into the top of rectifying column in the recovery system by liquor pump, realized in gas gathering system, realizing the gas-liquid secondary separation, the liquid that enters the top of recovery system rectifying column is sprayed the mixed gases of back and bottom by spray equipment, acetone gas in the adsorbed gas, through the gas after the liquid adsorption, directly from rectifying column outlet discharging, and the absorption liquid after the absorption is back to the gas collecting system, circulation fluid as vacuum system enters vacuum system by the pump pressurization again, carrying out cycle heat exchange once more handles, through the absorption liquid after the cycle heat exchange absorption, after its concentration reaches 10%---30%, both can be discharged on the distiller in the recovery system, and carry out acetone by the distillatory method and reclaim.The whole recovery system control sytsem adopts PLC (programmable logic controller) Controlling System, under the management of computer software each technology controlling and process point in the recovery system is carried out in good time monitoring, and all parameter reference mark all adopt the mode of transmitter to conduct data.
Because the present invention adopts above-mentioned exhaust and waste water with vacuum system to introduce treatment system, utilize waste liquid that gas is adsorbed, reduce the loss of the acetone of vacuum operating process, reduced production cost, reduced the loss of acetone solvent effectively, make gaseous emission reach national standard, waste liquid has been recovered to this useful component of acetone through handling simultaneously, and treatment liq has also obtained utilization to a certain extent.The acetone gas rate of recovery of present method is greater than 95%, acetone content in the emission gases is lower than 100PPm, be lower than national proposed standard, the energy consumption of itself is lower than 20% of recovery value, absorption liquid acetone concentration 10%---30%, the energy consumption that the has effectively reduced subsequent disposal waste water that vacuum system produces of forgoing fully, basically eliminate the solvent odor of production environment.Present method is easy and simple to handle, technology is simple and acetone solvent organic efficiency and recovery purity height, has reached goal of the invention.
Description of drawings:
Fig. 1 is a technical process schematic block diagram of the present invention
Fig. 2 is the principle schematic of rectifying column among the present invention
Embodiment:
Below in conjunction with accompanying drawing 1-Fig. 2 and embodiment in detail the present invention is described in detail, Fig. 1 clearly demonstrates technical process of the present invention: a kind of method that reclaims acetone from the volatile mixed gas of solvent that vacuum system is discharged, form the acetone recovery system by two cover vacuum systems, two covers gas collecting system on the throne, a cover gas gathering system, a cover gas treating system and Controlling System, its concrete process flow steps is as follows:
A. gas collecting
The gas of vacuum system discharging is introduced gas production on the throne system by the gas collecting pump in the gas production on the throne system, and the pumping speed of a cover vacuum system is 300m3/hr, 2; Flow 0.4-0.8 cubic meters/hour, work in 24 hours; The pumping speed of another set of vacuum system is 500m3/hr,, 2; Flow 0.6-1.0 cubic meters/hour, work in 18 hours; And the circulating liquid in vacuum system gravity flow enters gas production on the throne system;
B. gas-liquid flash liberation
The gas that enters gas production on the throne system pumps into gas gathering system by the gas production pump in the gas gathering system, and liquid then pumps into gas gathering system by liquid; Thereby separate the first time that is implemented in gas liquid in the gas production on the throne system;
C. gas-liquid secondary separation
Gas in the gas gathering system enters recovery system from the bottom, and liquid pumps into the top of recovery system by liquor pump, realizes the gas-liquid secondary separation in gas gathering system;
D. gas-liquid heat exchange absorbs
The liquid that pumps into recovery system is by the mixed gases in the spray of the spray equipment on the rectifying column in recovery system back and the recovery system, the heat exchange of finishing gas and liquid absorbs, directly discharge through the gas after the liquid heat exchange absorption, after absorption liquid after the process liquid heat exchange absorbs then is back to the gas collecting system, enter vacuum system once more and realize recycling, the absorption liquid temperature is lower than 15 ℃;
E. carrying out acetone reclaims
Absorption liquid through after the cycle heat exchange absorption after its concentration reaches 20%, is discharged on the distiller in the recovery system, carries out acetone and reclaims.
What Fig. 2 then showed is the structure of rectifying column in the recovery system, be made up of parts such as gas and liquid entrance, a plurality of packing section and column plate section, liquid distributor, secondary liquid distributors, gas enters rectifying column by inlet mouth 1 and is discharged by venting port 13 by column plate section 3, packing section 4, column plate section 5, packing section 8, transition zone 9, column plate section 10 backs; Liquid enters rectifying column by liquid-inlet 12 and carries out liquid distribution by liquid distributor 11; Discharge by leakage fluid dram 2 by column plate section 10, transition zone 9, packing section 8, column plate section 5, packing section 4, column plate section 3 backs.Another road liquid enters rectifying column by liquid-inlet 7 and enters secondary liquid distributor 6 and carry out liquid distribution; Discharge by leakage fluid dram 2 by column plate section 5, packing section 4, column plate section 3 backs
The gross exhaust gas of total system is 1600m3/hr; The global cycle water yield is<5.0 cubic meters/hours.
The technical indicator that present embodiment reaches is as follows:
1) the acetone rate of recovery 〉=90%);
2) cat head acetone emission concentration≤100PPM;
3) absorption liquid is discharged acetone concentration 〉=10%;
4) 7 of demand cold≤20T/hr degree water.
5) acetone content is reduced to 0.07% by 1.4% before reclaiming in the vacuum pump exhaust;
6) the COD value meets environmental emission standard owing to descending with the recovery system coupling in the vacuum pump draining.

Claims (6)

1. method that reclaims acetone from the volatile mixed gas of solvent that vacuum system is discharged is formed the acetone recovery system by vacuum system, gas production on the throne system, gas gathering system, gas treating system and Controlling System, and its concrete process flow steps is as follows:
A. gas collecting
The gas of vacuum system discharging is introduced gas production on the throne system by the gas collecting pump in the gas production on the throne system, and the gravity flow of the circulating liquid in the vacuum system enters gas production on the throne system;
B. gas-liquid flash liberation
The gas that enters gas production on the throne system pumps into gas gathering system by the gas production pump in the gas gathering system, and liquid then pumps into gas gathering system by liquid; Thereby separate the first time that is implemented in gas liquid in the gas production on the throne system;
C. gas-liquid secondary separation
Gas in the gas gathering system enters recovery system from the bottom, and liquid pumps into the top of recovery system by liquor pump, realizes the gas-liquid secondary separation in gas gathering system;
D. gas-liquid heat exchange absorbs
The liquid that pumps into recovery system is by the mixed gases in the spray of the spray equipment on the rectifying column in recovery system back and the recovery system, the heat exchange of finishing gas and liquid absorbs, directly discharge through the gas after the liquid heat exchange absorption, after absorption liquid after the process liquid heat exchange absorbs then is back to the gas collecting system, enter vacuum system once more and realize recycling, the absorption liquid temperature is lower than 15 ℃;
E. carrying out acetone reclaims
Absorption liquid through after the cycle heat exchange absorption after its concentration reaches 10%---30%, both can be discharged on the distiller in the recovery system, carried out acetone and reclaimed.
2. the method that reclaims acetone from the volatile mixed gas of solvent that vacuum system is discharged according to claim 1, it is characterized in that: the vacuum system among the above-mentioned described step a is made up of Lodz vacuum pump, water ring vacuum pump, gas-liquid separator, pipeline and valve.
3. the method that from the volatile mixed gas of solvent that vacuum system is discharged, reclaims acetone according to claim 1, it is characterized in that: the gas collecting on the throne system among the above-mentioned described step b is made up of with pipeline and valve the combined type surge tank that over-pass, liquid level control, gas collecting pump constitute, and the pressure of its liquid is that 1-2kg pressure, temperature are less than 35 ℃.
4. the method that reclaims acetone from the volatile mixed gas of solvent that vacuum system is discharged according to claim 1, it is characterized in that: the gas collector among the above-mentioned described step c is to have increased interchanger on gas collecting system-based on the throne.
5. the method that from the volatile mixed gas of solvent that vacuum system is discharged, reclaims acetone according to claim 1, it is characterized in that: the recovery system in the above-mentioned described steps d is made up of rectifying column and corresponding instrument piping and valve, the structure of rectifying column is by Stainless Steel Helices and column plate is compound constitutes, comprise packing section, column plate section and liquid spraying device, the pressure in the recovery system is 3-5Kg.
6. the method that from the volatile mixed gas of solvent that vacuum system is discharged, reclaims acetone according to claim 1, it is characterized in that: the above-mentioned operation control that comprises the total system of vacuum system, gas production on the throne system, gas gathering system and gas recovery system, adopt the Controlled by Programmable Controller system.
CN 200810112174 2008-05-22 2008-05-22 Method for recovering acetone from volatile mixed gas of solvent discharged from vacuum system Expired - Fee Related CN101585755B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103084042A (en) * 2011-11-02 2013-05-08 韶关市曲江天瑞德化工有限公司 Device and process used for recovering acetone exhaust gas
CN103570516A (en) * 2013-10-31 2014-02-12 广西科伦制药有限公司 Technology for recovering acetone in production of cefotaxime sodium
CN106310877A (en) * 2016-08-23 2017-01-11 孙桂菊 High-efficiency energy-saving volatile-organic-solvent-containing tail gas recovery technique

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5152812A (en) * 1991-05-10 1992-10-06 Kovach J Louis Recovery of condensable organic compounds from inert gas streams laden
CN2912776Y (en) * 2006-01-22 2007-06-20 石建平 Recovering device with spraying function

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103084042A (en) * 2011-11-02 2013-05-08 韶关市曲江天瑞德化工有限公司 Device and process used for recovering acetone exhaust gas
CN103084042B (en) * 2011-11-02 2016-06-22 韶关市曲江天瑞德化工有限公司 A kind of device for reclaiming acetone waste gas and technique
CN103570516A (en) * 2013-10-31 2014-02-12 广西科伦制药有限公司 Technology for recovering acetone in production of cefotaxime sodium
CN103570516B (en) * 2013-10-31 2015-03-11 广西科伦制药有限公司 Technology for recovering acetone in production of cefotaxime sodium
CN106310877A (en) * 2016-08-23 2017-01-11 孙桂菊 High-efficiency energy-saving volatile-organic-solvent-containing tail gas recovery technique

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