CN103768822A - Treatment method of unsaturated polyester steam - Google Patents
Treatment method of unsaturated polyester steam Download PDFInfo
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Abstract
The invention relates to a treatment method of unsaturated polyester steam. The method includes the following steps: (1) first stage condensation to transfer organic matters with boiling points higher than that of water from the gas phase into the liquid phase and reduce the concentration of organic matters in the steam; (2) second stage condensation to condense steam condensate from the first stage condensation into low-concentration polyester wastewater; (3) anaerobic treatment on the wastewater from the second stage condensation; (4) aerobic treatment on the wastewater subjected to aerobic treatment; and (5) precipitation and filtering by precipitating and filtering the water outlet from aerobic treatment and discharging. The method does not have to condensate polyester steam into high-concentration organic wastewater and has the advantages of high recovery rate, low energy consumption of subsequent treatment, short process, simple equipment, stable operation, and standard discharge of outlet water.
Description
Technical field
The present invention relates to a kind of processing method of polyester steam, particularly relate to the processing of the polyester steam that in a kind of unsaturated polyester resin (UPR) production process, the polycondensation reaction stage produces.
Background technology
Unsaturated polyester resin (UPR) is to be made through polycondensation reaction by binary acid, dihydroxylic alcohols, polycondensation reaction is a reversible reaction that generates condensation water, therefore in course of reaction, make to generate water and be constantly evaporated, thereby reaction is carried out to the direction that generates product.Its polyester steam mainly contains reaction mass and the intermediate products such as ethylene glycol, propane diols, diglycol, low molecular weight polycaprolactone ester monomer, phthalic acid, maleic acid, and concentration is at 50～150 g/m
3between.It is large that this class unsaturated polyester (UP) steam has vapour content, the feature that organic concentration is high, and directly condensation will form acid extremely strong high concentrated organic wastewater, and its biochemical treatment not only investment cost is high, and processing cost is also very expensive.
Production by Catalytic Combustion Process is to process a kind of effective ways of flammable organic exhaust gas, and CN02109675.9 and CN200610047791.9 all propose to adopt the method for catalytic combustion to process waste polyester gas.But these methods all need through complicated pretreatment, remove water vapour in waste gas, dust and some has corrosive organic matter, avoid affecting the service life of catalyst and device.CN200510015163.8 discloses a kind of purification method of waste polyester gas, and waste polyester gas is removed most of moisture through gas-liquid separator, then after preheating, carries out catalytic combustion, and partial reaction tail gas directly mixes to recover energy with waste polyester gas as carrier gas.Although the method can make waste polyester gas qualified discharge, but in unsaturated polyester (UP) steam, contain a large amount of moisture, after gas-liquid separation pretreatment, the organic pollution that is wherein soluble in shipwreck volatilization can be transferred in water and produce high concentrated organic wastewater as acetaldehyde, ethylene glycol, and subsequent treatment difficulty is large.In addition, in polyester steam, organic concentration fluctuates greatlyr with the variation of polycondensation reaction degree, and this makes catalytic combustion in the larger state of temperature fluctuation, and all there are adverse effect in the performance to catalyst and the life-span of equipment.Therefore, Production by Catalytic Combustion Process is not the method for optimal processing unsaturated polyester (UP) steam.
Early stage polyester enterprise adopts the method that hot Media Oven burns to process polyester steam more, but adopts the cost of this method processing polyester steam higher, and in steam, a large amount of useful resources can not be recycled, and causes the huge wasting of resources; Because system pressure is difficult for balance, have serious safety problem, the method does not re-use simultaneously.That domestic existing most of unsaturated polyester (UP) manufacturing enterprise all adopts is cooling, rectifying, biochemical processing route, the unsaturated polyester (UP) steam of high concentration is directly condensed into waste water, then it is carried out to rectifying, recovery section material, distillate carries out anaerobism, aerobic treatment.CN201010602167.7 discloses a kind of method that reclaims ethylene glycol and acetaldehyde in polyester waste water, esterification waste water enters stripping tower processing, overhead collection to organic gas and steam directly enter Ethanal distillation column, after Ethanal distillation column is processed, arrive high-purity acetaldehyde in overhead collection, at the bottom of tower, waste water enters after the processing of ethylene glycol destilling tower, collects high-purity ethylene glycol solution at the bottom of tower, and steam and steam that tower top produces enter stripping tower circular treatment again.In the method, every kind of organic matter need to be distinguished condensation recovery, need to after multiple condensation, just form low concentration wastewater, and recovery is not thorough, and energy consumption is large, and cost is high, does not meet the theory of cleaner production and recycling economy.
Summary of the invention
For the feature of the deficiencies in the prior art and unsaturated polyester (UP) steam, the invention provides a kind of processing method of unsaturated polyester (UP) steam.The method is without becoming high concentrated organic wastewater by polyester steam-condensation, and the organic matter rate of recovery is high, and subsequent treatment energy consumption is low, flow process is short, equipment is simple, stable operation, and processing water outlet can qualified discharge.
The processing method of unsaturated polyester (UP) steam of the present invention, comprises following content:
(1) one-level condensation, makes polyester steam mid-boiling point transfer to liquid phase higher than the organic matter of water from gas phase, reduces organic concentration in steam;
(2) B-grade condensation, becomes low concentration polyester waste water by condensed one-level steam-condensation;
(3) Anaerobic Treatment, after B-grade condensation, waste water carries out Anaerobic Treatment;
(4) Aerobic Process for Treatment, the waste water after Anaerobic Treatment carries out Aerobic Process for Treatment;
(5) sedimentation and filtration, the discharge after precipitation, filtration of the water outlet after Aerobic Process for Treatment.
In the inventive method, described unsaturated polyester (UP) steam is from the polycondensation reaction stage in unsaturated polyester resin production process, organic concentration is high and fluctuation is large, mainly contains the organic pollution of the difficult volatilization such as ethylene glycol, propane diols, diglycol, low molecular weight polycaprolactone ester monomer, phthalic acid, maleic acid.
In the inventive method, the described one-level condensation of step (1) adopts condensing tower, and tower top arranges condensate pans, and tower body adopts the form of column plate and filler combination, and polyester steam inlet is combined column plate above, and theoretical cam curve is 3～15; Polyester steam inlet is packing section below, and filler is stainless steel helices, ceramic ring filler or plastic filler etc.Condensing tower entrance polyester vapor (steam) temperature is 190～220 ℃, and tower top temperature is 105～120 ℃, to guarantee that steam steams from tower top; Column bottom temperature is 140～170 ℃, can reduce condensed liquid phase and again evaporate, and be 5:1～50:1 by its gas/liquid weight ratio of steam inlet flow-control.In the present invention, condensed liquid phase organic matter is back to tower top through packing section, and liquid-phase reflux ratio is 1～50.Polyester steam mid-boiling point is transferred to liquid phase through condensation layer by layer from gas phase higher than the organic matter such as ethylene glycol, propane diols of water, and at the bottom of the tower forming by above-mentioned processing, in liquid phase, organic content is 90wt%～100wt%, and better value is 95wt%～100wt%.
In the inventive method, the described B-grade condensation of step (2) adopts common condenser, and inlet temperature is 105～120 ℃, and outlet temperature is 40～60 ℃, and heat exchange area is 15～25dm
2.Condensed waste water COD is 10000～20000mg/L, BOD
5be 4000～5600mg/L, subsequent treatment can adopt biochemical treatment.
In the inventive method, the described Anaerobic Treatment of step (3) adopts anaerobic UASB reactor, and the water inlet volumetric loading of reactor is 4～10kgCOD/ (m
3d), retention time of sewage is 20～60h, and inflow temperature is 30～40 ℃, and the methane gas content of collection is 55v%～70v%.
In the inventive method, the described Aerobic Process for Treatment of step (4) adopts contact-oxidation pool, and water inlet volumetric loading is 0.3～1.2 kgCOD/ (m
3d), retention time of sewage is 6～12 h, and gas-water ratio is 3:1～7:1.
Compared with the prior art, the polyester steam treatment method that the inventive method provides is without polyester steam-condensation is become to high-concentration waste water, but by the difficult volatile organic compounds of the higher boilings such as the ethylene glycol in one-level condensation high efficiente callback polyester steam, propane diols, phthalic acid, maleic acid, there is not second-order phase transition in this process, the rate of recovery is high, energy consumes low, and has reduced subsequent treatment energy consumption.Remaining steam forms low concentration wastewater by B-grade condensation and carries out anaerobism, Aerobic Process for Treatment, and flow process is short, equipment is simple, stable operation, and after processing, water outlet can qualified discharge.The method can reclaim a large amount of useful resources from polyester steam, turns waste into wealth, and can realize again the qualified discharge of polyester steam, and the rate of recovery is high, energy consumption is low, has good economic benefit and environmental benefit.
Accompanying drawing explanation
Fig. 1 is a kind of concrete unsaturated polyester (UP) steam treatment technique schematic flow sheet of the present invention.
Wherein: 10, first-stage condenser, 11, material storage tank, 12, secondary condenser, 13, effluent storage tank, 14, regulating reservoir, 15, anaerobic UASB, 16, air accumulator, 17, contact-oxidation pool, 18, sedimentation basin, 19, filter.
Fig. 2 is the concrete structure schematic diagram of first-stage condenser in the present invention.
Wherein: 1, steam inlet, 2, condensate pans, 3, steam (vapor) outlet, 4, refluxing opening, 5, liquid re-distributor, 6, column plate, 7, packing layer, 8, seal pot, 9, discharging opening.
The specific embodiment
Fig. 1 is a kind of concrete technological process of the present invention: the unsaturated polyester (UP) steam that polycondensation phase produces is introduced into first-stage condenser 10, organic matter in steam is mainly the reaction masses such as ethylene glycol, propane diols, diethylene glycol, phthalic acid, maleic acid, these organic boiling points are all high than the boiling point of water, form liquid phase oily organic matter in the bottom of first-stage condenser, recycling after material storage tank 11 is collected.All the other uncondensed vapor form low concentration polyester waste water by secondary condenser 12 and enter effluent storage tank 13, after mixing, enter anaerobic UASB reactor 15 in regulating reservoir 14 with the processing water outlet of sedimentation basin, and the biogas of generation enters air accumulator 16.Anaerobic Treatment water outlet enters in contact-oxidation pool 17 carries out Aerobic Process for Treatment, and the degree of depth is removed the organic matter in waste water.Water outlet after aerobic treatment can qualified discharge after processing through sedimentation basin 18, filter 19.
Fig. 2 is the concrete structure schematic diagram of condenser of the present invention, detailed process is as follows: unsaturated polyester (UP) steam enters from condenser import department, the temperature of steam inlet 1 is about between 190～220 ℃, top is provided with condensate pans 2, control its temperature between 105～120 ℃, making to have the thermograde of 70～115 ℃ between the bottom of condenser and top, is 5:1～50:1 by its gas/liquid weight ratio of steam inlet flow-control.In the time that polyester steam enters condenser, its steam rises to tower top at the bottom of tower, and through column plate 6 condensation layer by layer, the organic matter that makes gas phase mid-boiling point be greater than water is transferred to liquid phase from gas phase gradually, and uncooled steam is from exporting 3 discharges.Condensed liquid flows downward after by liquid re-distributor 5, after the column plate 6 of flowing through, packing layer 7, enters seal pot 8, and a part of condensed liquid is back to condenser by refluxing opening 4 and circulates, and liquid-phase reflux ratio is 1～50.In the liquid phase generating by 9 places of discharging opening at the bottom of above-mentioned treating column, content of organics scope is 90wt%～100wt%, and better value is 95wt%～100wt%.
Further illustrate the inventive method and effect below by embodiment, wherein wt% is mass fraction, and v% is volume fraction.
Embodiment 1
The unsaturated polyester resin steam that adopts the technological process of Fig. 1 and the condenser of Fig. 2 to produce polycondensation phase is processed.Unsaturated polyester resin is take diethylene glycol, ethylene glycol, propane diols, phthalic acid, maleic acid as main material production, and the discharge capacity of polyester steam is 500～3000Nm
3/ h, in polyester steam, organic content is about 15wt%, and wherein the content of dihydroxylic alcohols is about 12wt%, and the content of phthalic acid and maleic acid is 3wt%.Concrete operating condition and treatment effect are in table 1.
The main processing unit of table 1 embodiment 1 and treatment effect
| processing unit title | treating apparatus scale and chief component | main service condition and control parameter | treatment effect |
| one-level condensation | first-stage condenser adopts the condensing tower of stainless steel, 16L, treating capacity 200Nm 3/ h, with condensate pans and return-flow system, the number of plates is 6, adopts ceramic ring filler. | 200 ℃ of inlet temperatures, 120 ℃ of condensate pans temperature, 160 ℃ of left and right of column bottom temperature, gas/liquid weight ratio is 20:1, liquid-phase reflux ratio is 10. | in outlet steam, dihydroxylic alcohols content is 0.8wt%, and the content of phthalic acid and maleic acid is 0.1wt%, and at the bottom of tower, in liquid phase, content of organics is 95wt%. |
| b-grade condensation | b-grade condensation is common condenser, the outside cooling water circulation that adopts. | 120 ℃ of inlet temperatures, 60 ℃ of outlet temperatures, heat exchange area is 17.6 dm 2. | the waste water COD that condensation forms is 12100 mg/L, BOD 5be 5200 mg/L. |
| anaerobic Treatment | adopt UASB reactor, material is lucite, and reactor volume 40L mainly comprises the formations such as water distributing plate, granule sludge bed, mud cushion, three phase separator, blast pipe, drainpipe, screen cloth. | inflow temperature is 38 ℃, and volumetric loading is 8 kg COD/ (m 3.d), hydraulic detention time is 40 h, and collecting gases methane content is 60v%. | water outlet COD is less than 1200 mg/L, BOD 5be less than 200 mg/L. |
| aerobic Process for Treatment | adopt contact-oxidation pool, volume is 40L, hangs inside semi soft packing.Mainly comprise water-distributing device, packing area, aerator and drainage system. | water inlet volumetric loading is 0.8 kg COD/ (m 3.d), the time of staying is 9h, and gas-water ratio is 5:1. | water outlet COD is less than 100 mg/L, BOD 5be less than 20 mg/L. |
| sedimentation and filtration | adopt quartz sand filtration post, diameter 20 mm, high 50 mm. | the rate of filtration is 20mL/min | water outlet COD is less than 60 mg/L, BOD 5be less than 20 mg/L. |
Adopt processing method of the present invention, water outlet COD is less than 60mg/L, BOD
5be less than 20mg/L, can make the organic matter directly condensation recovery under the condition of gas phase in unsaturated polyester (UP) steam, the rate of recovery is high.
Adopt the technological process of Fig. 1 and the condenser of Fig. 2, under different condition, the polyester steam identical with embodiment 1 is processed, concrete operating condition and treatment effect are in table 2.
The main processing unit of table 2 embodiment 2 and treatment effect
| processing unit title | treating apparatus scale and chief component | main service condition and control parameter | treatment effect |
| one-level condensation | first-stage condenser adopts stainless steel, 16L, treating capacity 200 Nm 3/ h, with condensate pans and return-flow system, the number of plates is 6, adopts ceramic ring filler. | 220 ℃ of left and right of inlet temperature, 105 ℃ of condensate pans temperature, 140 ℃ of column bottom temperatures, gas/liquid weight ratio is 40:1 left and right, reflux ratio is 50. | in outlet steam, dihydroxylic alcohols content is 0.6wt%, and the content of phthalic acid and maleic acid is 0.08wt%, and at the bottom of tower, in liquid phase, content of organics is 97.5wt%. |
| b-grade condensation | secondary condenser is common condenser, the outside cooling water circulation that adopts. | 105 ℃ of inlet temperatures, 40 ℃ of outlet temperatures, heat exchange area is 17.6 dm 2. | the waste water COD that condensation forms is 10500 mg/L, BOD 5be 5000 mg/L. |
| anaerobic Treatment | adopt UASB anaerobic reactor, material is lucite, reactor volume 40L.Mainly comprise the formations such as water distributing plate, granule sludge bed, mud cushion, three phase separator, blast pipe, drainpipe, screen cloth. | inflow temperature is between 38 ℃, and volumetric loading is 6 kg COD/ (m 3.d), hydraulic detention time is 53h, and collecting gases methane content is 68v%. | water outlet COD is less than 900 mg/L, BOD 5be less than 180 mg/L. |
| aerobic Process for Treatment | adopt contact-oxidation pool, volume is 40L, hangs inside semi soft packing.Mainly comprise water-distributing device, packing area, aerator and drainage system. | water inlet volumetric loading is 0.6 kg COD/ (m 3.d), the time of staying is 12h, and gas-water ratio is 4:1. | water outlet COD is less than 80 mg/L, BOD 5be less than 20 mg/L. |
| sedimentation and filtration | quartz sand filtration post, diameter 20 mm, high 50 mm. | the rate of filtration is 20mL/min. | water outlet COD is less than 60 mg/L, BOD 5be less than 20 mg/L. |
Adopt processing method of the present invention, can make the organic matter directly condensation recovery under the condition of gas phase in unsaturated polyester (UP) steam, the rate of recovery is high, greatly reduces the energy consumption of subsequent treatment.Uncooled steam forms the polyester waste water of low concentration under the condition of time condensation, after anaerobism, aerobic and filtration treatment, can reach first discharge standard.
Claims (10)
1. a processing method for unsaturated polyester (UP) steam, comprises following content:
(1) one-level condensation, makes polyester steam mid-boiling point transfer to liquid phase higher than the organic matter of water from gas phase, reduces organic concentration in steam;
(2) B-grade condensation, becomes low concentration polyester waste water by condensed one-level steam-condensation;
(3) Anaerobic Treatment, after B-grade condensation, waste water carries out Anaerobic Treatment;
(4) Aerobic Process for Treatment, the waste water after Anaerobic Treatment carries out Aerobic Process for Treatment;
(5) sedimentation and filtration, the discharge after precipitation, filtration of the water outlet after Aerobic Process for Treatment.
2. in accordance with the method for claim 1, it is characterized in that: described unsaturated polyester (UP) steam, from the polycondensation reaction stage in unsaturated polyester resin production process, mainly contains ethylene glycol, propane diols, diglycol, low molecular weight polycaprolactone ester monomer, phthalic acid and maleic acid.
3. in accordance with the method for claim 1, it is characterized in that: the described one-level condensation of step (1) adopts condensing tower, and tower top arranges condensate pans, and tower body adopts the form of column plate and filler combination, polyester steam inlet is combined column plate above, and theoretical cam curve is 3～15; Polyester steam inlet is packing section below.
4. it is characterized in that in accordance with the method for claim 3: the filler of packing section is stainless steel helices, ceramic ring filler or plastic filler.
5. in accordance with the method for claim 3, it is characterized in that: condensing tower entrance polyester vapor (steam) temperature is 190～220 ℃, tower top temperature is 105～120 ℃, and column bottom temperature is 140～170 ℃, is 5:1～50:1 by its gas/liquid weight ratio of steam inlet flow-control.
6. according to the method described in claim 3 or 5, it is characterized in that: the condensed liquid phase organic matter of one-level is back to tower top through packing section, and liquid-phase reflux ratio is 1～50.
7. in accordance with the method for claim 1, it is characterized in that: the described B-grade condensation of step (2) adopts common condenser, and inlet temperature is 105～120 ℃, and outlet temperature is 40～60 ℃, and heat exchange area is 15～25dm
2.
8. according to the method described in claim 1 or 7, it is characterized in that: the waste water COD after B-grade condensation is 10000～20000mg/L, BOD
5be 4000～5600mg/L.
9. in accordance with the method for claim 1, it is characterized in that: the described Anaerobic Treatment of step (3) adopts anaerobic UASB reactor, and the water inlet volumetric loading of reactor is 4～10kgCOD/ (m
3d), retention time of sewage is 20～60h, and inflow temperature is 30～40 ℃, and the methane gas content of collection is 55v%～70v%.
10. in accordance with the method for claim 1, it is characterized in that: the described Aerobic Process for Treatment of step (4) adopts contact-oxidation pool, and water inlet volumetric loading is 0.3～1.2kgCOD/ (m
3d), retention time of sewage is 6～12h, and gas-water ratio is 3:1～7:1.
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| CN104150679A (en) * | 2014-06-04 | 2014-11-19 | 广州擎天材料科技有限公司 | Esterification wastewater treatment system and method capable of saving land and energy sources |
| CN115353262A (en) * | 2022-10-20 | 2022-11-18 | 威海蓝创环保设备有限公司 | Esterification wastewater treatment process |
| CN115353261A (en) * | 2022-10-19 | 2022-11-18 | 威海蓝创环保设备有限公司 | Polyester waste water treatment system |
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