CN104707354A - Methylbenzene separation system in acrylic acid device and method - Google Patents

Methylbenzene separation system in acrylic acid device and method Download PDF

Info

Publication number
CN104707354A
CN104707354A CN201510154036.XA CN201510154036A CN104707354A CN 104707354 A CN104707354 A CN 104707354A CN 201510154036 A CN201510154036 A CN 201510154036A CN 104707354 A CN104707354 A CN 104707354A
Authority
CN
China
Prior art keywords
toluene
pipeline
return tank
output pipe
condenser
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201510154036.XA
Other languages
Chinese (zh)
Other versions
CN104707354B (en
Inventor
张乐功
杨光友
孙永伟
曹云飞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
SHANDONG KAITAI PETROCHEMICAL CO Ltd
Original Assignee
SHANDONG KAITAI PETROCHEMICAL CO Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by SHANDONG KAITAI PETROCHEMICAL CO Ltd filed Critical SHANDONG KAITAI PETROCHEMICAL CO Ltd
Priority to CN201510154036.XA priority Critical patent/CN104707354B/en
Publication of CN104707354A publication Critical patent/CN104707354A/en
Application granted granted Critical
Publication of CN104707354B publication Critical patent/CN104707354B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Landscapes

  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention relates to a methylbenzene separation system in an acrylic acid device and a method. A tower top gas phase pipeline of a fractionating tower (1) is connected with a condensing mechanism; the condensing mechanism is connected with a return tank (4) for separating methylbenzene through a pipeline; a wastewater output pipeline (12) and a methylbenzene output pipeline are arranged at the bottom of the return tank (4); a coalescer and a baffle (17) are sequentially arranged in the return tank (4) along the flow direction of liquid, the coalescer is used for separating oil and water, the baffle (17) is used for baffling methylbenzene and is located between the wastewater output pipeline (12) and the methylbenzene output pipeline, and the wastewater output pipeline (12) is located between the coalescer and the baffle (17); the condensing mechanism is connected with a pressure regulating device through a pipeline. According to the methylbenzene separation system, the consumption of methylbenzene can be obviously reduced, the working environment is improved, the energy is saved, and the emission amount is reduced; the method is flexible, simple and convenient, and the recovery efficiency of methylbenzene is improved.

Description

Toluene piece-rate system and method in a kind of acroleic acid device
Technical field
The invention belongs to toluene separation field, be specifically related to the toluene piece-rate system in a kind of acroleic acid device and method.
Background technology
General water and the acetic acid adopting the thick solution of method removing acrylic acid (the acrylic acid aqueous solution that acrylic acid oxidation unit produces) of azeotropic distillation in acroleic acid device, in acroleic acid device, multiplex toluene is as the entrainer of the thick solution of acrylic acid.Methylbenzene azeotropic agent and the thick solution of acrylic acid azeotropic distillation in Light ends fractionating column, tower bottom reboiler pump forced circulation, column bottom temperature raises as reboiler thermal source by low-pressure steam; Tower top tower reflux pump squeezes into entrainer solution, utilize that Azotropic distillation method makes most of water, acetic acid flows out from Light ends fractionation tower top after being separated with acrylic acid, after Light ends fractionator overhead condenser condenses, enter return tank, entrainer toluene and the waste water layering containing components such as acetic acid, in the overflow to return tank of entrainer toluene, the opposite side of baffle plate recycles; The gas be not condensed in return tank, in tank deck discharge gas condenser with the further condensing cooling of chilled water after, lime set flows into return tank, and solidifying gas is evacuated to by water-ring vacuum pump that vavuum pump separator carries out gas, water is separated.
In current production process the recovery of entrainer toluene be by Light ends fractionating column return tank with the waste water natural layering containing the component such as acetic acid, and carry out Recovery and recycle use by the opposite side of baffle plate in overflow to return tank, because chemical industry continuous seepage is in dynamic process, and the layering of toluene and waste water layered effect is poor in a dynamic state, cause part toluene and waste water mixing discharge system, cause the consumption of toluene, produce one ton of acrylic acid in acrylic acid industry and will consume 4.5 ~ 6 kilograms of toluene, this is the main cause causing toluene consumption higher.
Although, the static separation time extending toluene and waste water in theory can improve the separating effect of toluene and waste water greatly, but due to chemical industry continuous seepage, be difficult to provide long static layering, layered effect is poor in a dynamic state to cause the layering of toluene and waste water, produces one ton of acrylic acid and will consume 4.5 ~ 6 kilograms of toluene in acrylic acid industry.
Summary of the invention
The technical problem to be solved in the present invention is: for the above-mentioned deficiency of prior art, toluene piece-rate system in a kind of acroleic acid device and method are provided, this system obviously can reduce the consumption of toluene, realization improves working environment, energy-saving and emission-reduction, the method flexible and convenient, improves the organic efficiency of toluene.
The present invention is achieved by the following technical solutions: this is used for the toluene piece-rate system in acroleic acid device, comprise the fractionating column for separating of light component in acrylic acid crude product, fractionating column midsection is provided with fractionating column feed pipe, discharge nozzle at the bottom of tower is provided with at the bottom of fractionating column tower, it is characterized in that: fractionator overhead gas phase pipeline is connected with condensing mechanism, condensing mechanism is connected with the return tank for separating of toluene by pipeline, is provided with waste water output pipe and toluene output pipe bottom return tank; Return tank inside is provided with for the coalescer of water-oil separating and the baffle plate for the toluene that dams along liquid flow direction successively, baffle plate is between waste water output pipe and toluene output pipe, waste water output pipe is between coalescer and baffle plate, and condensing mechanism is connected with pressure-regulating device by pipeline.
Described toluene output pipe comprises refluxing toluene pipeline and toluene recovery pipeline, refluxing toluene pipeline is connected with fractionator overhead, toluene recovery pipeline is connected with toluene reservoir vessel, refluxing toluene pipeline and toluene recovery pipeline is equipped with the valve for control piper opening and closing.
Described condensing mechanism comprises the first condenser and the second condenser, first condenser is connected with fractionator overhead gaseous phase outlet pipeline, second condenser is connected with the first condenser gaseous phase outlet pipeline, and the first condenser is connected with return tank respectively with the condensed product output pipe of the second condenser.
Described pressure-regulating device comprises vavuum pump, water shutoff tank and water shutoff condenser, vavuum pump is connected with condensing mechanism by pipeline, the water of vavuum pump is connected with water shutoff tank with exhaust emission tube road, water shutoff pot bottom is connected with water shutoff condenser by pipeline, and water shutoff condenser is connected with vavuum pump by pipeline.
Described toluene output pipe is provided with reflux pump, and waste water output pipe is provided with distillation pump.
Described return tank is horizontal tank, return tank inside is provided with condensing mechanism interface, coalescer, waste water output pipe interface, baffle plate and toluene output pipe interface successively along liquid flow direction, coalescer and baffle plate are fixed on return tank bottom surface, there is the space of liquid flow between baffle plate and return tank roof, height of baffle plate is higher than coalescer height.
Described condensing mechanism interface is arranged on return tank top, and passes to bottom return tank by pipeline; Waste water output pipe interface is arranged on bottom return tank.
Described coalescer comprises the orifice plate and silk screen that set gradually along liquid flow direction, gap is there is between orifice plate and silk screen, the height of orifice plate is greater than or equal to the height of silk screen, orifice plate is distributed with multiple perforate, the thickness of silk screen is 300 ~ 500mm, and the height of silk screen is 60 ~ 80% of return tank height.
The above-described method for the toluene piece-rate system in acroleic acid device, step is as follows:
A) pressure in condensing mechanism and return tank is regulated to be 13.5 ~ 15.5kPa by pressure-regulating device; Gas-phase product fractionator overhead distillated, through condensing mechanism condensation, obtains the condensation mixed liquor of temperature 23 ~ 33 DEG C;
B) condensation mixed liquor enters return tank by pipeline, temperature 23 ~ 33 DEG C in return tank, condensation mixed liquor in return tank makes water and toluene layering obtain layering solution by coalescer, the layering interfaces of layering solution remains on 50 ~ 80% of coalescer height, and layering solution obtains toluene after baffle plate dams;
C) return tank bottom part from waste water be disposed to treatment unit for waste water through distillation pump, waste water output pipe discharge rate is 9000 ~ 11000kg/h, the toluene obtained in return tank by toluene output pipe flow out return tank.
Described toluene output pipe comprises refluxing toluene pipeline and toluene recovery pipeline, refluxing toluene pipeline is connected with fractionator overhead, toluene recovery pipeline is connected with toluene reservoir vessel, refluxing toluene pipeline and toluene recovery pipeline are equipped with the valve for control piper opening and closing, the ratio controlling refluxing toluene piping flow and waste water output pipe discharge rate is 7:1.
In the present invention, the technological process of applicant's design is as follows: acrylic acid crude product enters from fractionating column stage casing, described fractionator overhead is provided with toluene and adds pipeline, toluene is as entrainer, water in acrylic acid crude product and acetate in minute and the methylbenzene azeotropic added from fractionator overhead, gaseous component steams from tower top.The main component of gaseous component is water, toluene and acetate in minute, and acetate in minute content is less negligible.Gaseous component, after as the first condenser of condensing mechanism and the second condenser condenses, enters return tank with the condensation mixed liquor that water and toluene are main component, and in return tank, coalescent layering forms layering solution.Lower floor in layering solution is waste water, and the lower floor in layering solution is toluene.Lower floor's waste water directly discharges piece-rate system of the present invention through waste water output pipe, and upper toluene outputs to return tank outside through toluene output pipe.There is provided power by reflux pump, the toluene that toluene output pipe exports can be got in tower through refluxing toluene pipeline on the one hand and continue to utilize as entrainer, can be recycled in toluene reservoir vessel on the other hand preserve through toluene recovery pipeline.
Applicant finds under study for action: in the fractionation subtractive process of acrylic acid crude product, and the toluene as entrainer exists the larger problem of loss, although carried out recycling to toluene, finds still have a large amount of toluene to run off by calculating toluene input amount.The toluene of entrainer is made a big purchase in large quantities, and cost is refined in the fractionation adding acrylic acid crude product.
Applicant is by determining: a large amount of losses of entrainer toluene are main, comprises vapor phase stream liquid phase of becoming estranged and to run off two aspects.It is in condensing mechanism condensation process, have a large amount of toluene to volatilize in the form of a vapor loss at fractionator overhead gas phase light component that gas phase runs off, toluene has toxicity and penetrating odor, gas phase runs off also can cause that toluene concentration in air is too high, the problem of work under bad environment, there is harmful effect to the healthy of workman, also in a disguised form add cost of labor; It is because the toluene in condensation mixed liquor cannot comparatively fast be separated preferably with water that liquid phase runs off, and causes being separated still containing a large amount of toluene in the waste water of rear discharge, can pollute after a large amount of toluene discharges in waste water to surrounding environment.Applicant devises pressure-regulating device, and pressure-regulating device can regulate the pressure in whole system by the pipeline be connected, pressure-regulating device regulates the scope of pressure to comprise fractionating column, condensing mechanism and return tank.The pressure in condensing mechanism and return tank is regulated to be 13.5 ~ 15.5kPa by pressure-regulating device, the pressure in condensing mechanism and return tank is regulated to be 14 ~ 14.8kPa preferably through pressure-regulating device, the smell of toluene in the working environment outside this system is reduced to negligible, the gas phase also simultaneously decreasing toluene in system runs off.
The present invention adopts the coalescer in return tank to accelerate coalescent in condensation mixed liquor of aqueous phase toluene, coalescer is vertically fixed in return tank, coalescer lower limb connects with at the bottom of tank, top edge is positioned at more than water and toluene interface, in conjunction with high and low surface free energy, the water in condensation mixed liquor and toluene through coalescer, when drop be captured, and in orifice plate and silk screen, assemble between orifice plate and silk screen, so just greatly increase the speed of gathering.The thickness that applicant designs silk screen is 300 ~ 500mm, and preferably, the thickness of silk screen is 350 ~ 400mm.Because applicant finds under study for action: condensation mixed liquor is when passing along screen thickness direction, as screen thickness, to be less than 300mm then undesirable through the condensation mixed liquor layered effect of silk screen, to cause in discharged waste water containing a large amount of toluene, cause the serious and liquid phase toluene loss of blowdown; When screen thickness is greater than 500mm, coalescence time can be caused long, reduce the separative efficiency of toluene.Study the design of discovery 300 ~ 500mm through applicant, both can ensure that in return tank, toluene has higher separative efficiency, can ensure that again toluene is effectively coalescent, avoid a large amount of losses of liquid toluene in waste water.
Applicant is found by research: not only may be used for separation and azeotropic agent toluene, the toluene piece-rate system in a kind of acroleic acid device of the present invention, is applicable to the acrylic acid crude product fractionation entrainer that separation proportion is less than 1.Such as entrainer methylisobutylketone is also applicable to this system and is separated, and can obtain good separating effect equally.
Compared with prior art, the beneficial effect that the toluene piece-rate system in a kind of acroleic acid device of the present invention and method have is:
1, this toluene piece-rate system be used in acroleic acid device significantly improves the separative efficiency of aqueous phase toluene, and the volatilization reducing vapor phase toluene is run off, and improves the working environment of this system.Return tank coalesce inside device can be separated the upper toluene in layering solution fast and effectively with the design of baffle plate, the liquid level of layering solution regulates by the discharge rate of waste water output pipe, while improve the treating capacity of water and toluene, make the separative efficiency held stationary in return tank.Due to the raising of separative efficiency in return tank, also in a disguised form improve the load of fractionating column, add acrylic acid output.The design of pressure-regulating device can reduce the volatilization loss of vapor phase toluene, improves the working environment of this system, avoids workman to work in the air ambient that toluene concentration is higher.
2, this toluene piece-rate system be used in acroleic acid device significantly improves the yield of aqueous phase toluene in return tank, solves the problem that Toluene in Wastewater residual quantity is high, has the effect of energy-saving and emission-reduction.The content of Toluene in Wastewater obviously reduces, and reduces the consumption of entrainer toluene.Produce the consumption that one ton of acrylic acid will consume 4.5 ~ 6 kilograms of toluene toluene in acrylic acid industry compared to existing technology, in system of the present invention, every fractionation obtains one ton of (being abbreviated as unit t) acrylic acid and only need consume 2 ~ 2.8kg toluene, consumption reduction Be very effective.In the art, in annual output ten thousand tons to 100,000 tons acrylic acid suitability for industrialized production, technical scheme of the present invention can save substantial contribution for enterprise, has outstanding technique effect.
Accompanying drawing explanation
A kind of schematic diagram for the toluene piece-rate system in acroleic acid device of Fig. 1.
Fig. 2 is a kind of internal structure schematic diagram for return tank in the toluene piece-rate system in acroleic acid device.
Fig. 3 is the A-A face sectional view of return tank in Fig. 2.
Wherein: 1, fractionating column 2, first condenser 3, second condenser 4, return tank 5, reflux pump 6, distillation pump; 7, discharge nozzle 12, waste water output pipe 13, refluxing toluene pipeline 14, toluene recovery pipeline 15, orifice plate 16, silk screen 17, baffle plate 18, framework 19, first condenser interface 20, second condenser interface 21, waste water output pipe interface 22, toluene output pipe interface at the bottom of vavuum pump 8, water shutoff tank 9, water shutoff condenser 10, fractionating column feed pipe 11, tower.
Detailed description of the invention
Fig. 1 ~ 3 are a kind of most preferred embodiments for the toluene piece-rate system in acroleic acid device of the present invention, and below in conjunction with accompanying drawing 1 ~ 3, the present invention will be further described.
With reference to Fig. 1 ~ 3, of the present invention a kind of for the toluene piece-rate system in acroleic acid device, comprise the fractionating column 1 for separating of light component in acrylic acid crude product, fractionating column 1 midsection is provided with fractionating column feed pipe 10, discharge nozzle 11 at the bottom of tower is provided with at the bottom of fractionating column 1 tower, it is characterized in that: fractionating column 1 top gaseous phase pipeline is connected with condensing mechanism, condensing mechanism is connected with the return tank 4 for separating of toluene by pipeline, waste water output pipe 12 and toluene output pipe is provided with bottom return tank 4, waste water output pipe 12 is provided with distillation pump 6, toluene output pipe is provided with reflux pump 5, condensing mechanism connects the pressure-regulating device for regulating condensing mechanism and return tank 4 air pressure by pipeline, return tank 4 inside is provided with the coalescer for water-oil separating and the baffle plate 17 for the toluene that dams successively along liquid flow direction.Baffle plate 17 is between waste water output pipe 12 and toluene output pipe, and waste water output pipe 12 is between coalescer and baffle plate 17.In Fig. 1, return tank 4 is sketch, simply illustrates the coalescer of its inside and the position of baffle plate 17 in Fig. 1 in return tank 4.In Fig. 2, return tank 4 is internal structure schematic diagram, has carried out detailed expression to return tank 4 internal structure.
With reference to Fig. 2, return tank 4 is horizontal tank, return tank 4 inside is provided with condensing mechanism interface, coalescer, waste water output pipe interface 21, baffle plate 17 and toluene output pipe interface 22 successively along liquid flow direction, coalescer and baffle plate 17 are fixed on return tank 4 bottom surface, there is the space of liquid flow between baffle plate 17 and return tank 4 roof, baffle plate 17 height is higher than coalescer height.Condensing mechanism interface is arranged on return tank 4 top, and passes to bottom return tank 4 by pipeline; Waste water output pipe interface 21 is arranged on bottom return tank 4.Return tank 4 is level installation, and coalescer and baffle plate 17 are all vertically fixed on return tank 4 bottom surface, there is interval between coalescer and baffle plate 17.End face and the horizontal plane of baffle plate 17 maintain an equal level, so that the upper toluene of effectively damming in layering solution.In the present embodiment, condensing mechanism interface comprises the first condenser interface 19, second condenser interface 20, first condenser interface 19 and the second condenser interface 20 is all passed to bottom return tank 4 by pipeline.
With reference to Fig. 2 ~ 3, coalescer comprises the orifice plate 15 and silk screen 16 that set gradually along liquid flow direction, there is gap between orifice plate 15 and silk screen 16, and the height of orifice plate 15 is greater than or equal to the height of silk screen 16, and the height of orifice plate 15 is lower than the height of baffle plate 17; Orifice plate 15 is distributed with multiple perforate, and the aperture of the perforate on orifice plate 15 is greater than screen diameter, and the effect of orifice plate 15 dredges liquid flow direction by perforate, so that improve the coalescence efficiency of silk screen.Silk screen 16 is connected with return tank 4 bottom surface by the framework 18 being arranged on silk screen 16 periphery, silk screen 16 is arranged in framework 18, framework 18 shape is agreed with mutually with silk screen 16 shape, be bolted between framework 18 and return tank 4, so that change silk screen 16 by the mode dismantling framework 18, be 300 ~ 500mm at the thickness of silk screen 16, the height of silk screen 16 is 60 ~ 80% of return tank 4 height, in the present embodiment, silk screen 16 is highly 1700 ~ 1750mm, and silk screen 16 end face and horizontal plane maintain an equal level.
With reference to Fig. 1, toluene output pipe comprises refluxing toluene pipeline 13 and toluene recovery pipeline 14, refluxing toluene pipeline 13 is connected with fractionating column 1 tower top, toluene recovery pipeline 14 is connected with toluene reservoir vessel, refluxing toluene pipeline 13 and toluene recovery pipeline 14 is equipped with the valve for control piper opening and closing.
With reference to Fig. 1, condensing mechanism comprises the first condenser 2 and the second condenser 3, first condenser 2 is connected with fractionating column 1 top gaseous phase export pipeline, second condenser 3 is connected with the first condenser 2 gaseous phase outlet pipeline, and the first condenser 2 is connected with return tank 4 respectively with the condensed product output pipe of the second condenser 3.
With reference to Fig. 1, pressure-regulating device comprises vavuum pump 7, water shutoff tank 8 and water shutoff condenser 9, vavuum pump 7 is connected with condensing mechanism by pipeline, the water of vavuum pump 7 is connected with water shutoff tank 8 with exhaust emission tube road, be connected with water shutoff condenser 9 by pipeline bottom water shutoff tank 8, water shutoff condenser 9 is connected with vavuum pump 7 by pipeline.Pressure-regulating device carrys out controlled pressure by regulating the reflux airflow amount of vavuum pump 7.
Embodiment 1 ~ 3 is the detailed description of the invention of the method for the toluene piece-rate system in acroleic acid device of the present invention.
embodiment 1
A) condensation: regulate pressure in condensing mechanism and return tank 4 to be 14 ~ 14.8kPa by pressure-regulating device; The gas-phase product distillated by fractionating column 1 tower top, through condensing mechanism condensation, obtains the condensation mixed liquor of temperature 23 ~ 33 DEG C; Condensing mechanism comprises the first condenser 2 and the second condenser 3, first condenser 2 is connected with fractionating column 1 top gaseous phase export pipeline, second condenser 3 is connected with the first condenser 2 gaseous phase outlet pipeline, and the first condenser 2 is connected with return tank 4 respectively with the condensed product output pipe of the second condenser 3; Be condensed to temperature 25 ~ 35 DEG C through the first condenser 2, the second condenser 3 is condensed to temperature 15 ~ 25 DEG C; In second condenser 3, the vavuum pump 7 of uncooled gas in pressure-regulating device is extracted out outside system, and by regulating the reflux airflow amount of vavuum pump 7 to realize controlled pressure;
B) be separated: condensation mixed liquor enters return tank 4 by pipeline, temperature 23 ~ 33 DEG C in return tank 4, condensation mixed liquor in return tank 4 makes water and toluene layering obtain layering solution by coalescer, the layering interfaces of layering solution remains on 50 ~ 80% of coalescer height, layering solution is after baffle plate 17 dams, lower floor's waste water is trapped within baffle plate 17 side, and upper toluene flows through from baffle plate 17 top, obtains toluene at baffle plate 17 opposite side;
C) return tank 4 bottom part from waste water be disposed to treatment unit for waste water through distillation pump 6, waste water output pipe 12 discharge rate is 10000kg/h, in return tank 4 obtain toluene by toluene output pipe flow out return tank 4; Toluene output pipe comprises refluxing toluene pipeline 13 and toluene recovery pipeline 14, refluxing toluene pipeline 13 is connected with fractionating column 1 tower top, toluene recovery pipeline 14 is connected with toluene reservoir vessel, and the ratio controlling refluxing toluene pipeline 13 flow and waste water output pipe 12 discharge rate is 7:1.
embodiment 2
A) condensation: regulate pressure in condensing mechanism and return tank 4 to be 13.5 ~ 14kPa by pressure-regulating device; The gas-phase product distillated by fractionating column 1 tower top, through condensing mechanism condensation, obtains the condensation mixed liquor of temperature 23 ~ 33 DEG C; Condensing mechanism comprises the first condenser 2 and the second condenser 3, first condenser 2 is connected with fractionating column 1 top gaseous phase export pipeline, second condenser 3 is connected with the first condenser 2 gaseous phase outlet pipeline, and the first condenser 2 is connected with return tank 4 respectively with the condensed product output pipe of the second condenser 3; Be condensed to temperature 25 ~ 35 DEG C through the first condenser 2, the second condenser 3 is condensed to temperature 15 ~ 25 DEG C; In second condenser 3, the vavuum pump 7 of uncooled gas in pressure-regulating device is extracted out outside system, and by regulating the reflux airflow amount of vavuum pump 7 to realize controlled pressure;
B) be separated: condensation mixed liquor enters return tank 4 by pipeline, temperature 23 ~ 33 DEG C in return tank 4, condensation mixed liquor in return tank 4 makes water and toluene layering obtain layering solution by coalescer, the layering interfaces of layering solution remains on 50 ~ 80% of coalescer height, layering solution is after baffle plate 17 dams, lower floor's waste water is trapped within baffle plate 17 side, and upper toluene flows through from baffle plate 17 top, obtains toluene at baffle plate 17 opposite side;
C) return tank 4 bottom part from waste water be disposed to treatment unit for waste water through distillation pump 6, waste water output pipe 12 discharge rate is 9000kg/h, in return tank 4 obtain toluene by toluene output pipe flow out return tank 4; Toluene output pipe comprises refluxing toluene pipeline 13 and toluene recovery pipeline 14, refluxing toluene pipeline 13 is connected with fractionating column 1 tower top, toluene recovery pipeline 14 is connected with toluene reservoir vessel, and the ratio controlling refluxing toluene pipeline 13 flow and waste water output pipe 12 discharge rate is 7:1.
embodiment 3
A) condensation: regulate pressure in condensing mechanism and return tank 4 to be 14.8 ~ 15.5kPa by pressure-regulating device; The gas-phase product distillated by fractionating column 1 tower top, through condensing mechanism condensation, obtains the condensation mixed liquor of temperature 23 ~ 33 DEG C; Condensing mechanism comprises the first condenser 2 and the second condenser 3, first condenser 2 is connected with fractionating column 1 top gaseous phase export pipeline, second condenser 3 is connected with the first condenser 2 gaseous phase outlet pipeline, and the first condenser 2 is connected with return tank 4 respectively with the condensed product output pipe of the second condenser 3; Be condensed to temperature 25 ~ 35 DEG C through the first condenser 2, the second condenser 3 is condensed to temperature 15 ~ 25 DEG C; In second condenser 3, the vavuum pump 7 of uncooled gas in pressure-regulating device is extracted out outside system, and by regulating the reflux airflow amount of vavuum pump 7 to realize controlled pressure;
B) be separated: condensation mixed liquor enters return tank 4 by pipeline, temperature 23 ~ 33 DEG C in return tank 4, condensation mixed liquor in return tank 4 makes water and toluene layering obtain layering solution by coalescer, the layering interfaces of layering solution remains on 50 ~ 80% of coalescer height, layering solution is after baffle plate 17 dams, lower floor's waste water is trapped within baffle plate 17 side, and upper toluene flows through from baffle plate 17 top, obtains toluene at baffle plate 17 opposite side;
C) return tank 4 bottom part from waste water be disposed to treatment unit for waste water through distillation pump 6, waste water output pipe 12 discharge rate is 11000kg/h, in return tank 4 obtain toluene by toluene output pipe flow out return tank 4; Toluene output pipe comprises refluxing toluene pipeline 13 and toluene recovery pipeline 14, refluxing toluene pipeline 13 is connected with fractionating column 1 tower top, toluene recovery pipeline 14 is connected with toluene reservoir vessel, and the ratio controlling refluxing toluene pipeline 13 flow and waste water output pipe 12 discharge rate is 7:1.
performance test is tested
In Statistics Implementation example 1 ~ 3: the acrylic acid gross mass of adding up monthly discharge nozzle 11 output at the bottom of tower in units of ton, in units of kg, add up monthly toluene consumption, monthly toluene consumption.Per month calculate this moon " toluene consumption/acrylic acid per ton " value by " the acrylic acid gross mass of discharge nozzle 11 output at the bottom of tower of monthly toluene consumption/monthly ".Each embodiment records 6 months continuously, and each embodiment all obtains " toluene consumption/acrylic acid per ton " value of 6 each moons in the middle of the month, calculates the mean value of each embodiment " toluene consumption/acrylic acid per ton ".
Table 1 embodiment 1 ~ 3 the performance test results
By above data can find out produce acrylic acid toluene consumption per ton have obvious minimizing compared to existing technology, and in embodiment 1 ~ 3 production process in its exterior working environment without obvious toluene smell, working environment be improved significantly.
The above is only preferred embodiment of the present invention, and be not restriction invention being made to other form, any those skilled in the art may utilize the technology contents of above-mentioned announcement to be changed or be modified as the Equivalent embodiments of equivalent variations.But everyly do not depart from technical solution of the present invention content, any simple modification, equivalent variations and the remodeling done above embodiment according to technical spirit of the present invention, still belong to the protection domain of technical solution of the present invention.

Claims (10)

1. one kind for the toluene piece-rate system in acroleic acid device, comprise the fractionating column (1) for separating of light component in acrylic acid crude product, fractionating column (1) midsection is provided with fractionating column feed pipe (10), discharge nozzle at the bottom of tower (11) is provided with at the bottom of fractionating column (1) tower, it is characterized in that: fractionating column (1) top gaseous phase pipeline is connected with condensing mechanism, condensing mechanism is connected with the return tank (4) for separating of toluene by pipeline, and return tank (4) bottom is provided with waste water output pipe (12) and toluene output pipe; Return tank (4) inside is provided with the coalescer for water-oil separating and the baffle plate (17) for the toluene that dams successively along liquid flow direction, baffle plate (17) is positioned between waste water output pipe (12) and toluene output pipe, waste water output pipe (12) is positioned between coalescer and baffle plate (17), and condensing mechanism is connected with pressure-regulating device by pipeline.
2. according to claim 1 a kind of for the toluene piece-rate system in acroleic acid device, it is characterized in that: described toluene output pipe comprises refluxing toluene pipeline (13) and toluene recovery pipeline (14), refluxing toluene pipeline (13) is connected with fractionating column (1) tower top, toluene recovery pipeline (14) is connected with toluene reservoir vessel, refluxing toluene pipeline (13) and toluene recovery pipeline (14) is equipped with the valve for control piper opening and closing.
3. according to claim 1 a kind of for the toluene piece-rate system in acroleic acid device, it is characterized in that: described condensing mechanism comprises the first condenser (2) and the second condenser (3), first condenser (2) is connected with fractionating column (1) top gaseous phase export pipeline, second condenser (3) is connected with the first condenser (2) gaseous phase outlet pipeline, and the first condenser (2) is connected with return tank (4) respectively with the condensed product output pipe of the second condenser (3).
4. according to claim 1 a kind of for the toluene piece-rate system in acroleic acid device, it is characterized in that: described pressure-regulating device comprises vavuum pump (7), water shutoff tank (8) and water shutoff condenser (9), vavuum pump (7) is connected with condensing mechanism by pipeline, the water of vavuum pump (7) is connected with water shutoff tank (8) with exhaust emission tube road, water shutoff tank (8) bottom is connected with water shutoff condenser (9) by pipeline, and water shutoff condenser (9) is connected with vavuum pump (7) by pipeline.
5. according to claim 1 a kind of for the toluene piece-rate system in acroleic acid device, it is characterized in that: described toluene output pipe is provided with reflux pump (5), waste water output pipe (12) is provided with distillation pump (6).
6. according to claim 1 a kind of for the toluene piece-rate system in acroleic acid device, it is characterized in that: described return tank (4) is horizontal tank, return tank (4) inside is provided with condensing mechanism interface, coalescer, waste water output pipe interface (21), baffle plate (17) and toluene output pipe interface (22) successively along liquid flow direction, coalescer and baffle plate (17) are fixed on return tank (4) bottom surface, there is the space of liquid flow between baffle plate (17) and return tank (4) roof, baffle plate (17) height is higher than coalescer height.
7. according to claim 6 a kind of for the toluene piece-rate system in acroleic acid device, it is characterized in that: described condensing mechanism interface is arranged on return tank (4) top, and pass to return tank (4) bottom by pipeline; Waste water output pipe interface (21) is arranged on return tank (4) bottom.
8. according to claim 1 a kind of for the toluene piece-rate system in acroleic acid device, it is characterized in that: described coalescer comprises the orifice plate (15) and silk screen (16) that set gradually along liquid flow direction, gap is there is between orifice plate (15) and silk screen (16), the height of orifice plate (15) is greater than or equal to the height of silk screen (16), (15) are distributed with multiple perforate to orifice plate, the thickness of silk screen (16) is 300 ~ 500mm, and the height of silk screen (16) is 60 ~ 80% of return tank (4) height.
9. the method for the toluene piece-rate system in acroleic acid device described in any one of claim 1 ~ 8, it is characterized in that, step is as follows:
A) pressure in condensing mechanism and return tank (4) is regulated to be 13.5 ~ 15.5kPa by pressure-regulating device; The gas-phase product distillated by fractionating column (1) tower top, through condensing mechanism condensation, obtains the condensation mixed liquor of temperature 23 ~ 33 DEG C;
B) condensation mixed liquor enters return tank (4) by pipeline, temperature 23 ~ 33 DEG C in return tank (4), condensation mixed liquor in return tank (4) makes water and toluene layering obtain layering solution by coalescer, the layering interfaces of layering solution remains on 50 ~ 80% of coalescer height, and layering solution obtains toluene after baffle plate (17) dams;
C) return tank (4) bottom part from waste water be disposed to treatment unit for waste water through distillation pump (6), waste water output pipe (12) discharge rate is 9000 ~ 11000kg/h, and the toluene obtained in return tank (4) flows out return tank (4) by toluene output pipe.
10. the method for the toluene piece-rate system in acroleic acid device according to claim 9, it is characterized in that: described toluene output pipe comprises refluxing toluene pipeline (13) and toluene recovery pipeline (14), refluxing toluene pipeline (13) is connected with fractionating column (1) tower top, toluene recovery pipeline (14) is connected with toluene reservoir vessel, refluxing toluene pipeline (13) and toluene recovery pipeline (14) are equipped with the valve for control piper opening and closing, the ratio controlling refluxing toluene pipeline (13) flow and waste water output pipe (12) discharge rate is 7:1.
CN201510154036.XA 2015-04-02 2015-04-02 Toluene piece-rate system and method in a kind of acroleic acid device Active CN104707354B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510154036.XA CN104707354B (en) 2015-04-02 2015-04-02 Toluene piece-rate system and method in a kind of acroleic acid device

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510154036.XA CN104707354B (en) 2015-04-02 2015-04-02 Toluene piece-rate system and method in a kind of acroleic acid device

Publications (2)

Publication Number Publication Date
CN104707354A true CN104707354A (en) 2015-06-17
CN104707354B CN104707354B (en) 2016-01-27

Family

ID=53407388

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510154036.XA Active CN104707354B (en) 2015-04-02 2015-04-02 Toluene piece-rate system and method in a kind of acroleic acid device

Country Status (1)

Country Link
CN (1) CN104707354B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106699502A (en) * 2016-12-20 2017-05-24 广西壮族自治区林业科学研究院 Turpentine rectification tower vacuum system
CN108547666A (en) * 2018-03-16 2018-09-18 北京华清微拓节能技术股份公司 A method of making full use of low-pressure steam sensible heat latent heat
CN109678711A (en) * 2017-10-19 2019-04-26 山东开泰石化股份有限公司 A kind of system and method for extracting methoxy methyl propionate from methyl acrylate waste oil

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030092937A1 (en) * 2001-11-13 2003-05-15 Wagner David R. Extraction process for recovery of acrylic acid
US20030150705A1 (en) * 2002-01-08 2003-08-14 Deshpande Sanjeev D. Acrylic acid recovery utilizing ethyl acrylate and selected co-solvents
CN1535948A (en) * 2003-04-09 2004-10-13 上海高桥石化丙烯酸厂 Method for purifying acrylic acid b utilizing azeotropic rectification
CN101367720A (en) * 2008-09-18 2009-02-18 中国石油大学(华东) Acrylic purification process and apparatus of bulkhead azeotropy rectification column

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030092937A1 (en) * 2001-11-13 2003-05-15 Wagner David R. Extraction process for recovery of acrylic acid
US20030150705A1 (en) * 2002-01-08 2003-08-14 Deshpande Sanjeev D. Acrylic acid recovery utilizing ethyl acrylate and selected co-solvents
CN1535948A (en) * 2003-04-09 2004-10-13 上海高桥石化丙烯酸厂 Method for purifying acrylic acid b utilizing azeotropic rectification
CN101367720A (en) * 2008-09-18 2009-02-18 中国石油大学(华东) Acrylic purification process and apparatus of bulkhead azeotropy rectification column

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
侯海瑞: "液-液两相聚结分离原理及实际应用", 《过滤与分离》 *
刘志刚,崔嘉敏: "降低丙烯酸精制单元废水中丙烯酸含量", 《石化技术与应用》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106699502A (en) * 2016-12-20 2017-05-24 广西壮族自治区林业科学研究院 Turpentine rectification tower vacuum system
CN109678711A (en) * 2017-10-19 2019-04-26 山东开泰石化股份有限公司 A kind of system and method for extracting methoxy methyl propionate from methyl acrylate waste oil
CN109678711B (en) * 2017-10-19 2021-08-27 山东开泰石化股份有限公司 System and method for extracting methyl methoxypropionate from methyl acrylate waste oil
CN108547666A (en) * 2018-03-16 2018-09-18 北京华清微拓节能技术股份公司 A method of making full use of low-pressure steam sensible heat latent heat

Also Published As

Publication number Publication date
CN104707354B (en) 2016-01-27

Similar Documents

Publication Publication Date Title
CN104973638B (en) Processing technology of high-salt high-concentration organic waste liquid
CN108568131B (en) Stripping liquid regeneration device and stripping liquid regeneration process
CN104419444B (en) A kind of method utilizing the moisture sump oil of delayed coking unit freshening
CN104707354B (en) Toluene piece-rate system and method in a kind of acroleic acid device
CN103785191B (en) The method that vinyl chloride high-boiling components rectifier unit and the rectifying of vinyl chloride high-boiling components are separated
CN103215073B (en) Production method for extracting lignite wax from brown coal
CN111040805A (en) Crude oil pre-dehydration, deep dehydration and sewage oil removal integrated device and method
CN107638709A (en) The separator and its operating method of acetic acid and water
CN206553370U (en) A kind of sludge combined treatment device
CN211798889U (en) Refining system for by-product hydrochloric acid in methane chloride process
CN110015707B (en) Useless stripper recovery unit of photoresist
CN106914068A (en) A kind of delayed coking exhaust gas treating method
CN201526306U (en) Energy-saving type separating, heating, precipitating and buffering integrated device
CN207958183U (en) A kind of novel carbinol distillation system
CN106582053B (en) The process and device of the tower methanol distillation column by-product ethyl alcohol of partition
CN105062575A (en) Process and apparatus for controlling continuous and stable discharge of non-condensable gas in benzene recovery system
CN205346877U (en) Vertical multistage strip tower
CN206027129U (en) High yield distillation system of propane diamine production line
CN111333480A (en) Butadiene refining method and device
CN205925180U (en) Water oil separating processing apparatus
CN104310680B (en) A kind of acid alcohol polycondensation Wastewater Pretreatment Apparatus and method for
CN107837555A (en) The method of quality control of rectifying tower with bulkhead
CN106966875B (en) Anti-blocking device of polymethoxy dibutyl ether rectification system and refining method
CN205821023U (en) Oil recovery system in a kind of raising oily sludge waste water
CN206404352U (en) The device of the tower methanol distillation column by-product ethanol of dividing plate

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant