CN204543614U - Purifying ethylene glycol piece-rate system - Google Patents
Purifying ethylene glycol piece-rate system Download PDFInfo
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- CN204543614U CN204543614U CN201520169888.1U CN201520169888U CN204543614U CN 204543614 U CN204543614 U CN 204543614U CN 201520169888 U CN201520169888 U CN 201520169888U CN 204543614 U CN204543614 U CN 204543614U
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Abstract
The utility model discloses a kind of purifying ethylene glycol piece-rate system, solve the problem that the complex process of prior art existence, separation difficulty, equipment investment and energy consumption are high.Comprise the ethylene glycol synthesis system connected successively, methanol distillation column, degreasing tower, lightness-removing column and treating column, wherein, ethylene glycol synthesis system is first connected with the second gas-liquid separator through the reboiler of degreasing tower, the gaseous phase outlet of described second gas-liquid separator is connected with the first gas-liquid separator through the reboiler of methanol distillation column, the gaseous phase outlet of described first gas-liquid separator is connected with ethylene glycol synthesis system, liquid-phase outlet is connected with the charging aperture of methanol distillation column, the tower bottoms outlet of described methanol distillation column is connected with the charging aperture of degreasing tower with the liquid-phase outlet of the second separator.The utility model flow process is simple, easy and simple to handle, equipment investment and operating cost is low, magazins' layout is effective, yield is high.
Description
Technical field
The utility model relates to a kind of ethylene glycol piece-rate system, specifically a kind of purifying ethylene glycol piece-rate system.
Background technology
What be most widely used in the preparation technology of ethylene glycol is that epoxyethane water is legal, due to the impact of oil crisis in recent years, prepares the research of ethylene glycol both at home and abroad increasing for Non oil-based route.And the CO gaseous oxidation coupling method of Non oil-based route prepares the advantages such as technique has abundant raw material source, cost is low, pollution-free, reaction condition is gentle, product purity is high, the production serialization of ethylene glycol, it is the green chemistry process of clear production, eco-friendly advanced person.Its development success, has important function and significance to changing existing oxalate, ethylene glycol and some conventional processing routes that is medical, dyestuff intermediate.
CO gaseous oxidation coupling method prepares the technique of ethylene glycol while saving petroleum resources, have also been introduced the impurity that oil synthesis technique does not have, wherein low-grade carboxylic acid and other alkoxides are mixed showed increased, particularly 1, the introducing of 2-butanediol, due to 1,2-butanediol and ethylene glycol boiling point relatively, easy formation azeotropic, the difficulty and the energy consumption that realize separation have increase.Impurity how in separating ethylene glycol product particularly 1,2-butanediol finally obtains qualified ethylene glycol product, and meanwhile ensure the simple validity of separation process and energy consumption reasonability again, this becomes the emphasis of purifying ethylene glycol Separation Research.
On the other hand, past is when carrying out first step Methanol Recovery for the reacting synthesis gas come by ethylene glycol synthesis system, need to carry out gas-liquid separation, the liquid phase containing methyl alcohol is made to enter methanol distillation column separation of methanol, this part liquid measure is large, often need bulky methanol distillation column process, have that equipment volume is large, cost of investment and operating cost is high, energy consumption is large problem.
Summary of the invention
The purpose of this utility model is to solve the problems of the technologies described above, and provides that a kind of flow process is simple, easy and simple to handle, equipment investment and operating cost is low, magazins' layout is effective, yield is high purifying ethylene glycol piece-rate system.
The utility model system, comprise the ethylene glycol synthesis system connected successively, methanol distillation column, degreasing tower, lightness-removing column and treating column, wherein, ethylene glycol synthesis system is first connected with the second gas-liquid separator through the reboiler of degreasing tower, the gaseous phase outlet of described second gas-liquid separator is connected with the first gas-liquid separator through the reboiler of methanol distillation column, the gaseous phase outlet of described first gas-liquid separator is connected with ethylene glycol synthesis system, liquid-phase outlet is connected with the charging aperture of methanol distillation column, the tower bottoms outlet of described methanol distillation column is connected with the charging aperture of degreasing tower with the liquid-phase outlet of the second separator.
Described methanol distillation column arranges number of plates 45-60 block, and at the bottom of charging aperture and tower, distance is 5-8 block column plate; Described degreasing tower arranges number of plates 15-40 block, and at the bottom of charging aperture and tower, distance is 4-8 block column plate; Described lightness-removing column arranges number of plates 90-120 block, 10-15 block at the bottom of charging aperture distance tower; Described treating column arranges number of plates 50-70 block, and at the bottom of charging aperture and tower, distance be 5-8 block column plate, and side line discharge and tower top are apart from being 4-8 tower block.
Adopt the method for said system, through the first gas-liquid separator gas-liquid separation after the reaction mixture gas comprised from ethylene glycol synthesis system is cooled to 40-60 DEG C, gas phase enters ethylene glycol synthesis system as hydrogeneous circulating air loopback, liquid phase sends into methanol distillation column, tower top produces methyl alcohol, described reaction mixture gas first sends into the second gas-liquid separator gas-liquid separation after being first cooled to 120-140 DEG C, gas phase sends into the first gas-liquid separator after being cooled to 40-60 DEG C further, degreasing tower is sent into after liquid phase mixes with the tower bottoms from methanol distillation column, degreasing column overhead produces mixed alcohol ester, lightness-removing column sent into by tower bottoms, lightness-removing column tower top produces light alcohols, treating column sent into by tower bottoms, treating column tower top produces the ethylene glycol of certified products, side line produces high-class product ethylene glycol, tower bottoms is heavy alcohol.
Send into the second gas-liquid separator gas-liquid separation after the reboiler that described reaction mixture gas is introduced into degreasing tower is cooled to 120-140 DEG C as thermal source, gas phase sends into the first gas-liquid separator after sending into and being cooled to 40-60 DEG C as thermal source in the reboiler of methanol distillation column.
The tower top temperature of described methanol distillation column controls at 50-65 DEG C, and column bottom temperature controls at 85-95 DEG C; Described degreasing column overhead temperatures controls at 40-55 DEG C, and column bottom temperature controls at 140-160 DEG C; Described lightness-removing column tower top temperature controls at 130-150 DEG C, and column bottom temperature controls at 143-145 DEG C; Described treating column tower top temperature controls at 130-149 DEG C, and column bottom temperature controls at 145-165 DEG C.
Described methanol distillation column arranges number of plates 45-60 block, and at the bottom of charging aperture and tower, distance is 5-8 block column plate; Described degreasing tower arranges number of plates 15-40 block, and at the bottom of charging aperture and tower, distance is 4-8 block column plate; Described lightness-removing column arranges number of plates 90-120 block, 10-15 block at the bottom of charging aperture distance tower; Described treating column arranges number of plates 50-70 block, and at the bottom of charging aperture and tower, distance be 5-8 block column plate, and side line discharge and tower top are apart from being 4-8 tower block.
Beneficial effect:
(1) at different temperatures twice gas-liquid separation is carried out for reaction mixture gas, the second gas-liquid separator gas-liquid separation is first sent into after first reaction mixture gas being first cooled to 120-140 DEG C, this temperature is more than the boiling point of methyl alcohol, therefore most methyl alcohol can be deposited in the gas phase in a gaseous form, now carry out gas-liquid separation, the liquid phase of separation is not sent into methanol distillation column, but degreasing tower is sent into together with the tower bottoms of methanol distillation column, pass through pre-separation, reduce the tolerance entering the first gas-liquid separator, again by cooling further, the first gas-liquid separator is sent into after the gas phase temperature of using the second gas-liquid separator is down to 40-60 DEG C, because temperature is below the boiling point of methyl alcohol, therefore most methyl alcohol can exist in liquid form, liquid phase containing methyl alcohol enters methanol distillation column, owing to carrying out the gas-liquid separation under twice different temperatures, while guarantee Methanol Recovery rate, the liquid measure finally entering methanol distillation column is declined to a great extent, and then volume and the height of methanol distillation column can be reduced, reduce manufacturing cost and control difficulty, also there is the advantage that reboiler energy consumption is low.
(2) problem of showed increased of mixing for low-grade carboxylic acid in reaction mixture gas and other alkoxides, be provided with methanol distillation column, degreasing tower, lightness-removing column and treating column and reclaim methyl alcohol, mixed alcohol ester, light alcohols, ethylene glycol and heavy alcohol respectively, adopt four tower rectification systems, more simpler than traditional ethylene glycol rectificating method, reduce cost of equipment, control by the strict of the entry level to each tower, column plate quantity, tower top and column bottom temperature the organic efficiency improving high-quality ethylene glycol, the rate of recovery of high-class product ethylene glycol can reach 95%.
(3) reboiler that the pyroreaction gaseous mixture of synthesis reactor is followed successively by de-ester tower and methanol distillation column provides heat, and Appropriate application used heat reaches energy-conservation object.
(4) the utility model technique has that flow process is simple and reliable, good separating effect, high-class product yield are high, decrease the volume of equipment thus reduce equipment investment and operating cost, energy consumption is low, environmentally friendly.
Accompanying drawing explanation
Fig. 1 is the utility model process chart and system diagram.
Wherein, 1-ethylene glycol synthesis system, 2-second gas-liquid separator, 3-first gas-liquid separator, 4-methanol distillation column, 4.1-reboiler, 5-degreasing tower, 5.1-reboiler, 6-lightness-removing column, 6.1-reboiler, 7-treating column, 7.1-reboiler, 7.2-side line discharge, 8-condenser, 9-separator, 10-vacuum equipment.
Detailed description of the invention
Below in conjunction with accompanying drawing, explanation is further explained to the utility model system:
Ethylene glycol synthesis system 1, methanol distillation column 4, degreasing tower 5, lightness-removing column 6 is connected successively with treating column 7, wherein, ethylene glycol synthesis system 1 is first connected with the second gas-liquid separator 2 through the reboiler 5.1 of degreasing tower 5, the gaseous phase outlet of described second gas-liquid separator 2 is connected with the first gas-liquid separator 3 through the reboiler 4.1 of methanol distillation column 4, the gaseous phase outlet of described first gas-liquid separator 3 is connected with ethylene glycol synthesis system 1, liquid-phase outlet is connected with the charging aperture of methanol distillation column 4, the tower bottoms outlet of described methanol distillation column 4 is connected with the charging aperture of degreasing tower 5 with the liquid-phase outlet of the second separator 2.Described methanol distillation column 4 arranges number of plates 45-60 block, and at the bottom of charging aperture and tower, distance is 5-8 block column plate; Described degreasing tower 5 arranges number of plates 15-40 block, and at the bottom of charging aperture and tower, distance is 4-8 block column plate; Described lightness-removing column 6 arranges number of plates 90-120 block, 10-15 block at the bottom of charging aperture distance tower; Described treating column 7 arranges number of plates 50-70 block, and at the bottom of charging aperture and tower, distance be 5-8 block column plate, and side line discharge and tower top are apart from being 4-8 block column plate.
Each column overhead establishes condenser 8, and described condenser 8 connects separator 9, and the gas vent of described separator is connected with air or vacuum equipment 10, and liquid outlet is communicated with corresponding each tower through pump.Namely top gaseous phase is sent into separator 9 gas-liquid separation and is obtained fixed gas and condensate liquid after condenser 8 condensation, except the fixed gas discharge of the separator 9 of methanol distillation column 4, the fixed gas access vacuum equipment 10 of other each column separators 9 is to produce the vacuum condition needed for this tower, the condensate liquid of separator 9 is through pump pressurization rear section backflow, and remainder is as product extraction.
Process chart as shown in Figure 1, raw material is the reaction mixture gas from ethylene glycol synthesis reactor 1, primarily of hydrogen, dimethyl oxalate, ethylene glycol, methyl alcohol, 1, 2-butanediol, methyl glycollate, nitrogen, ethanol, the composition such as methane and carbon monoxide, wherein hydrogen quality mark is 30-40%, quality of glycol mark is 15-20%, 1, 2-butanediol mass fraction is 0.05-0.08%, methanol quality mark is 24-30%, methyl glycollate mass fraction is 0.1-0.3%, ethanol mass fraction is 0.2-0.5%, nitrogen, the content of methane and carbon monoxide is at 15-25%, other are the heavy alcohol of complicated component.
To produce 12.7 ten thousand tons of ethylene glycol high-class products per year, assuming that the working time in device year is 8000 hours, methanol distillation column volume is 180m
3, wherein the volume of methanol distillation column can reduce 18%.
Process example: reaction mixture gas (the thick glycol reaction gas come by ethylene glycol synthesis reactor 1, mass flow is 82340Kg/h, ) enter the reboiler 5.1 of de-ester tower 5 as its thermal source, its temperature is 190-210 DEG C, pressure is 1.8-2.1MPa, after heat exchange, the temperature of reaction mixture gas is reduced to 120-140 DEG C, then deliver to the second gas-liquid separator 2 and carry out gas-liquid separation, the reboiler 4.1 that wherein gas phase (mass flow is 70669.5Kg/h) delivers to methanol distillation column 4 provides heat for it, described gas phase is reduced to 40-60 DEG C through reboiler 4.1 temperature and enters the first gas-liquid separator 3 gas-liquid separation again, its liquid phase (mass flow is 25004Kg/h) enters methanol distillation column 4 by charging aperture, gas phase recycles as hydrogeneous circulating air loopback ethylene glycol synthesis reactor 1, methanol distillation column 4 arranges number of plates 45-60 block, at the bottom of charging aperture and tower, distance is 5-8 block column plate, tower top pressure is 90-110KPa, tower bottom pressure is 100-120KPa, tower top temperature controls at 40-65 DEG C, separator 9 gas-liquid separation is sent into after overhead condenser 8 condensation, fixed gas emptying, condensate liquid is through pump pressurization rear section backflow, reflux ratio is set to 35-40, all the other condensate liquids are as methanol product extraction, column bottom temperature controls at 85-95 DEG C, tower bottoms sends into de-ester tower 5 after being pressurizeed by pump, de-ester tower 5 theoretical cam curve 15-40 block, at the bottom of charging aperture and tower, distance is 4-8 tower block, tower top pressure is 70-90KPa, tower bottom pressure is 80-100KPa, tower top temperature controls at 40-55 DEG C, separator 9 gas-liquid separation is sent into after overhead condenser 8 condensation, fixed gas access vacuum equipment 10 is to produce vacuum, condensate liquid is through pump pressurization rear section backflow, reflux ratio is set to 2-5, all the other condensate liquids are as the extraction of mixed alcohol ester product, and column bottom temperature controls at 140-160 DEG C, and tower bottoms is sent into and entered lightness-removing column after pump pressurization.Lightness-removing column 6 theoretical cam curve 90-120 block, 10-15 block at the bottom of feed entrance point distance tower, tower top pressure is 10-20KPa, tower bottom pressure is 15-25KPa, tower top temperature controls at 130-150 DEG C, separator 9 is sent into after overhead condenser 8 condensation, fixed gas access vacuum equipment 10 is to produce vacuum, condensate liquid is through pump pressurization rear section backflow, reflux ratio is set to 80-120, all the other condensate liquids are as the extraction of light alcohols product, and column bottom temperature controls at 143-155 DEG C, and tower bottoms is sent into and entered treating column after pump pressurization.Treating column 7 adopts side take-off form, theoretical cam curve 50-70 block, at the bottom of charging aperture and tower, distance is 5-8 tower block, side line discharge 7.2 is 4-8 tower block with tower top distance, tower top pressure is 10-15KPa, tower bottom pressure is 15-20KPa, tower top temperature controls at 130-149 DEG C, separator 9 gas-liquid separation is sent into after overhead condenser 8 condensation, fixed gas access vacuum equipment 10 is to produce vacuum, condensate liquid is through pump pressurization rear section backflow, reflux ratio is set to 30-50, all the other condensate liquids are as the extraction of ethylene glycol certified products, side line discharge 7.2 extraction product is ethylene glycol high-class product, column bottom temperature controls at 145-165 DEG C, tower bottoms is heavy alcohol.
In the present embodiment, the mass flow of methyl alcohol is 17259Kg/h, methanol content >99%; Mixed alcohol ester quality adopts flow to be 1332Kg/h, and quality group becomes ethylene glycol 0.08, methyl alcohol 0.462,1,2-butanediol 0.001, methyl glycollate 0.208, ethanol 0.244; Described light alcohols adopts mass flow to be 1242.5Kg/h, and quality group becomes ethylene glycol 0.885,1,2-butanediol 0.006, dimethyl oxalate 0.005, and other are the light alcohols (as 2,3-butanediol) of boiling point lower than ethylene glycol; Ethylene glycol certified products extraction mass flow is 600Kg/h, the mass fraction >0.994 of ethylene glycol, and the mass flow of ethylene glycol certified products is 15864.7Kg/h, and heavy alcohols adopts mass flow to be 100.3Kg/h; The mass flow of ethylene glycol high-class product is 15864.7Kg/h, and annual production is 12.7 ten thousand tons.
Claims (2)
1. a purifying ethylene glycol piece-rate system, it is characterized in that, comprise the ethylene glycol synthesis system connected successively, methanol distillation column, degreasing tower, lightness-removing column and treating column, wherein, ethylene glycol synthesis system is first connected with the second gas-liquid separator through the reboiler of degreasing tower, the gaseous phase outlet of described second gas-liquid separator is connected with the first gas-liquid separator through the reboiler of methanol distillation column, the gaseous phase outlet of described first gas-liquid separator is connected with ethylene glycol synthesis system, liquid-phase outlet is connected with the charging aperture of methanol distillation column, the tower bottoms outlet of described methanol distillation column is connected with the charging aperture of degreasing tower with the liquid-phase outlet of the second separator.
2. purifying ethylene glycol piece-rate system as claimed in claim 1, it is characterized in that, described methanol distillation column arranges number of plates 45-60 block, charging aperture with at the bottom of tower apart from being 5-8 block column plate; Described degreasing tower arranges number of plates 15-40 block, and at the bottom of charging aperture and tower, distance is 4-8 block column plate; Described lightness-removing column arranges number of plates 90-120 block, 10-15 block column plate at the bottom of charging aperture distance tower; Described treating column arranges number of plates 50-70 block, and at the bottom of charging aperture and tower, distance be 5-8 block column plate, and side line discharge and tower top are apart from being 4-8 block column plate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104725191A (en) * | 2015-03-24 | 2015-06-24 | 中国五环工程有限公司 | Ethylene glycol refining and separating method and system |
| CN112062654A (en) * | 2020-08-21 | 2020-12-11 | 陕西聚能新创煤化科技有限公司 | Ethylene glycol rectification system and rectification process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104725191A (en) * | 2015-03-24 | 2015-06-24 | 中国五环工程有限公司 | Ethylene glycol refining and separating method and system |
| CN112062654A (en) * | 2020-08-21 | 2020-12-11 | 陕西聚能新创煤化科技有限公司 | Ethylene glycol rectification system and rectification process |
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