CN102060664B - High-efficiency and energy-saving reaction process for preparing ethylene glycol through hydrogenation of oxalate - Google Patents
High-efficiency and energy-saving reaction process for preparing ethylene glycol through hydrogenation of oxalate Download PDFInfo
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- CN102060664B CN102060664B CN2010106012593A CN201010601259A CN102060664B CN 102060664 B CN102060664 B CN 102060664B CN 2010106012593 A CN2010106012593 A CN 2010106012593A CN 201010601259 A CN201010601259 A CN 201010601259A CN 102060664 B CN102060664 B CN 102060664B
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 35
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000005984 hydrogenation reaction Methods 0.000 title abstract description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 title abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 57
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- 125000005233 alkylalcohol group Chemical group 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 230000004087 circulation Effects 0.000 claims description 7
- 230000002411 adverse Effects 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 238000012546 transfer Methods 0.000 claims description 4
- -1 alkyl carbon Chemical compound 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims description 2
- 239000012071 phase Substances 0.000 claims 2
- 239000007792 gaseous phase Substances 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 238000004904 shortening Methods 0.000 claims 1
- 230000008569 process Effects 0.000 abstract description 9
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 8
- 238000010438 heat treatment Methods 0.000 abstract description 7
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 30
- WYACBZDAHNBPPB-UHFFFAOYSA-N diethyl oxalate Chemical compound CCOC(=O)C(=O)OCC WYACBZDAHNBPPB-UHFFFAOYSA-N 0.000 description 15
- 238000004519 manufacturing process Methods 0.000 description 12
- 230000008016 vaporization Effects 0.000 description 12
- 239000000203 mixture Substances 0.000 description 11
- 235000019441 ethanol Nutrition 0.000 description 10
- 239000000047 product Substances 0.000 description 10
- 230000011218 segmentation Effects 0.000 description 10
- 238000009834 vaporization Methods 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 150000002431 hydrogen Chemical class 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 5
- 239000006227 byproduct Substances 0.000 description 5
- 239000000498 cooling water Substances 0.000 description 4
- 230000009466 transformation Effects 0.000 description 4
- 239000003245 coal Substances 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 239000003208 petroleum Substances 0.000 description 3
- 239000006200 vaporizer Substances 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- LOMVENUNSWAXEN-UHFFFAOYSA-N Methyl oxalate Chemical compound COC(=O)C(=O)OC LOMVENUNSWAXEN-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
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- 230000002194 synthesizing effect Effects 0.000 description 2
- 229910017813 Cu—Cr Inorganic materials 0.000 description 1
- 241000282326 Felis catus Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000004902 Softening Agent Substances 0.000 description 1
- 229920004935 Trevira® Polymers 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
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- 238000004364 calculation method Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
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- 230000008676 import Effects 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000005120 petroleum cracking Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000011020 pilot scale process Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
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Abstract
The invention discloses a reaction process for preparing ethylene glycol from oxalate serving as a raw material through hydrogenation in the presence of a catalyst. In the process, only a reaction product and unreacted oxalate in a reaction recycle loop are liquefied and separated by controlling each exit temperature in the reaction process, and fed into a rectification process; and hydrogen and alkyl alcohol required by a reaction cycle are always kept in a gas state and remained in recycle gas, boosted by a recycle blower and returned to a reactor. By the process, reaction heat is fully utilized, so that the temperature of the recycle gas can be increased, and heating energy consumption is reduced.
Description
Technical field
The present invention relates to the production of terepthaloyl moietie, further relate to a kind of technical process, belong to chemical technology field by barkite gas phase hydrogenation synthesizing glycol.
Background technology
China is terepthaloyl moietie (EG) consumption first big country, by the end of 2009 the end of the year China's terepthaloyl moietie manufacturer be 13 families, overall throughput is 243.8 ten thousand tons/year, and import volume in 2009 has reached 582.8 ten thousand tons, degree of self-sufficiency less than 30%.Terepthaloyl moietie can be used for producing trevira, frostproofer, softening agent, nonionogenic tenside etc., and China's terepthaloyl moietie is mainly used in producd fibers and uses polyester, accounts for aggregate consumption 93.7%.In the domestic manufacturer except that Tongliao Jinmei Chemical Co., Ltd adopts Coal Chemical Industry route technology; Other producer all adopts external oil ethene route technology; Be that the ethene that petroleum cracking produces obtains oxyethane through peroxo-; Then oxyethane and water are made into mixed aqueous solution by a certain percentage, under certain temperature and pressure condition, are converted into terepthaloyl moietie.The production cost of this route depends critically upon the price of oil and derived product thereof, and the reaction product water cut that obtains of this method is high simultaneously, the subsequent processing device complex process, and long flow path, energy consumption is high, directly influences the production cost of terepthaloyl moietie.
China is the country of few oily many coals; The national conditions that petroleum resources are deficient have relatively limited with petroleum synthesizing glycol operational path; Therefore development is a raw material with coal; Can give full play to the advantage of rich coal resources in China by CO through barkite intermediate product hydrogenation preparing terepthaloyl moietie, can possess the advantage of competing mutually with traditional petroleum path.Simultaneously China is the first phosphorus production big country in the world, contains abundant CO (90.7%) in the yellow phosphoric tail gas, therefore rationally utilizes yellow phosphoric tail gas can effectively reduce the terepthaloyl moietie production cost, and helps environment protection.
See from the achievement in research of public reported, more at present on the hydrogenation of oxalate for preparing ethylene glycol technology tend to adopt Cu-SiO more
2Catalyzer replaces early stage Cu-Cr catalyzer, because the Cr element all has greatly harm to human body and environment.Reaction mesoxalic acid ester conversion rate can reach 100%, and glycol selectivity can reach more than 90%.And take place in order effectively to suppress side reaction; It is excessive greatly that hydrogen in reaction needs; Add corresponding alkyl alcohol dilution barkite simultaneously (as being that raw material dilutes with methyl alcohol with the dimethyl oxalate; Oxalic acid diethyl ester is that raw material is used alcohol dilution), the mol ratio of hydrogen and barkite is generally 10～300, and the mol ratio of alkyl alcohol and barkite is 2～20.In the production technique of routine; Because a large amount of nonreactive materials (like alkyl alcohol) circulate in the reactive system circulation loop; Need reaction end gas be cooled to normal temperature at least makes just now and can coagulate components condense; Utilize the separation of by-products of rectificating method again with alkyl alcohol and barkite, terepthaloyl moietie and reaction; And then will need round-robin alkyl alcohol ratio on request to allocate into to carry out carburation by evaporation in the raw material barkite, round-robin hydrogen also reheats the entering reactor drum, does like this certainly will consume a large amount of heats and cause the tremendous economic loss.
Summary of the invention
Goal of the invention of the present invention provides a kind of production technique of new hydrogenation of oxalate for preparing ethylene glycol, reduces reaction process, and practices thrift water coolant and use steam with heating, thereby conserve energy reduces cost.
This reaction solves the technical scheme that its technical problem adopted: mainly be included in the reaction process; Temperature through the outlet of control rough segmentation tower; Only the liquefaction of reaction product in the reaction cycle loop and unreacted barkite is separated, send into rectification working process then, and required hydrogen of reaction cycle and alkyl alcohol all remain gaseous state and be retained in the circulation gas; And, make its Returning reactor through the recycle blower supercharging.In addition, the temperature out through control barkite vaporising device realizes the control to the barkite concentration in the mixed gas, simplifies production technique.Recycle stock among the present invention is mainly the permanent gases that adds in the reaction, mainly comprises hydrogen, rare gas element, like nitrogen, argon gas etc. and the alkyl alcohol that before reaction, adds; Wherein alkyl substituent is identical with alkyl carbon containing quantity in the barkite in the alkyl alcohol, for example is raw material with the dimethyl oxalate, adopts methyl alcohol; With the oxalic acid diethyl ester is raw material, adopts ethanol.
The barkite vaporising device that is adopted among the present invention is to guarantee that gas-liquid fully contacts and the little gas-liquid mass transfer (contact) equipment of gas phase drag mutually.Circulation loop mainly is made up of tower, pump, preheater, gas-liquid flow to be adverse current or and stream, thereby control the purpose that reaches the control Outlet Gas Temperature into the temperature of tower liquid through the heat that adds preheater.During reaction product is separated, realize only will react the material that generates through control condensator outlet gas temperature and from recycle gas, separate with unreacted barkite, and the constant rate of permanent gases and alkyl alcohol in the maintenance circulation gas.
Find that through test of many times condensing equipment can adopt two kinds of forms in the technology of the present invention, a kind of is the combination of rectifying tower and horizontal condenser, and another kind is the vertical (type) condenser of gas and phlegma adverse current.When adopting the combination of rectifying tower and horizontal condenser, only need rectifying section, do not need stripping section and reboiler.And in order to reduce resistance, rectifying section preferably adopts corrugated-plate packed tower.At this moment, condensing surface is preferably selected fractional distillating tube for use, and material gets into shell side, and dispersed phase holdup reaches the purpose of controlling Outlet Gas Temperature to regulate heat transfer area in the shell side through changing.If adopt vertical (type) condenser, two kinds of functions of rectifying and partial condensation are combined in the equipment, and material steam gets into tube side by the bottom, and phlegma is drawn by the bottom, and the tail gas that does not coagulate is drawn at the top, and the type of cooling is the most handy air-cooled, through air quantity control Outlet Gas Temperature.
Compared with prior art, the invention has the beneficial effects as follows: reduced separation rectification step, simplified production technique, improved production efficiency, saved energy expenditure and reduced cost most of components in the reaction system.
Description of drawings
Below in conjunction with accompanying drawing and specific embodiment the present invention is done further description.
Fig. 1 is a process flow diagram of the present invention, and wherein 1 is interchanger, and 2～4 is preheater, and 5 is partial condenser; 6 is vaporizer, and 7 is hydrogenator, and 8 are the rough segmentation tower; 9 is the barkite raw material storage tank, and 10～11 is the highly pressurised liquid fresh feed pump, and 12 is temperature-sensing valve; 13 is TP, and 14～34 is pipeline, and 35 is recycle blower.
Embodiment
Below in conjunction with embodiment foregoing invention content of the present invention is done further to describe in detail.But should this be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following embodiment.Not breaking away under the above-mentioned technological thought situation of the present invention, according to ordinary skill knowledge and customary means, make various replacements and change, all should comprise within the scope of the invention.
Embodiment 1:
Below in conjunction with Fig. 1 embodiment is described.The Cu/SiO of 4L packs at hydrogenator middle part
2Catalyzer, reactor drum two ends are equipped with and the equigranular porcelain ring of catalyzer, are raw material with the oxalic acid diethyl ester, and the reaction pressure of hydrogenation reaction is 1.5MPa (gauge pressure).
Oxalic acid diethyl ester pumps into preheater 2 through highly pressurised liquid fresh feed pump 10, and wherein the inlet amount of oxalic acid diethyl ester is 3.65kg/h, and the thermal response product generation heat exchange preheating with from pipeline 34 is heated to 108 ℃ at preheater 2 mesoxalic acid diethyl esters.Get into the bottom of vaporizer 6 through pipeline 30 through the barkite after the preheating.(mol ratio of hydrogen and nitrogen was 4 in the gas mixture after required additional hydrogen mixed with recycled offgas in the reaction; Nitrogen is carrier gas) get into interchanger 1 through pipeline 14; With the reaction end gas generation heat exchange from pipeline 19, gas mixture is heated to 166 ℃ in interchanger 1, gets into vaporizer 6 through pipeline 15; And mix with barkite from pipeline 30, mixed gas flow is 38m
3/ h.Absolute ethyl alcohol adds in initial reaction stage, treats that systemic circulation stops charging after stable, and keeping the mol ratio of absolute ethyl alcohol and oxalic acid diethyl ester in the reaction process is between 7.0～7.3.
In vaporization tower 6, the temperature in of gas mixture is 166 ℃.After heat exchange, the vaporization of part oxalic acid diethyl ester is discharged by cat head with hydrogen, and the mixture after the oxalic acid diethyl ester that bottom temp is lower is vaporized 16 gets into preheaters 4 by the road.The oxalic acid diethyl ester of not vaporizing fully in the vaporization tower is flowed out by vaporization tower 6 bottoms; Pump into preheater 3 through pipeline 31 through highly pressurised liquid fresh feed pump 11, after the steam heating vaporization, get into vaporization tower 6 tops and get into preheater 4 with the oxalic acid diethyl ester mixed gas of having vaporized.Tower 6 temperature outs of wherein vaporizing are controlled at 143 ℃, because reaction pressure is certain, so temperature out has just determined the composition of each material; Hydrogen (massfraction) 10.2% wherein, nitrogen 35.9%, ETHYLE ACETATE 2.8%; Ethanol 34.9%, oxalic acid diethyl ester 15.4%, other component 0.8% such as water.Get into preheater 4 again after reaction mixture gas is come out by vaporization tower 6 and further be heated to 182 ℃.Heating back gas mixture gets into reactor drum 7 and catalyzer contact reacts; Transformation efficiency through analyzing oxalic acid diethyl ester reaches 100%, and each component of reactor outlet consists of (massfraction): hydrogen 9.3%, nitrogen 35.9%; ETHYLE ACETATE 3.0%; Ethanol 44.5%, terepthaloyl moietie 6.1%, other component 1.2% such as water.Because reaction is thermopositive reaction, the reactor outlet exhaust temperature is increased to 210 ℃.The reaction end gas temperature is reduced to 129 ℃ and is got into rough segmentation towers 8 and separate, and will be heated to 166 ℃ by 99 ℃ from the material mixed gas of pipeline 14, is heated to 182 ℃ from the reaction raw materials gas mixture of pipeline 16 by 143 ℃.
After reaction end gas got into rough segmentation tower 8, control rough segmentation tower 8 top gas temperature outs are at 106 ℃, and were same because system pressure is constant; The saturated vapor pressure of each material of temperature decision has also determined the material composition, wherein contains (massfraction) hydrogen 8.7%; Nitrogen 33.5%, ETHYLE ACETATE 3.3%, ethanol 53.2%; Terepthaloyl moietie 0.02%, other material 1.3% such as water is because top exit gas still also has the terepthaloyl moietie of minute quantity; A spot of terepthaloyl moietie is present in the gas phase can influence catalyst life, and therefore necessary further condensing reflux gets off a spot of terepthaloyl moietie total condensation.In rough segmentation tower 8, terepthaloyl moietie and by product that reaction generates, and unreacted barkite raw material is condensate in the bottom, and take out through preheater 2 through pipeline 34.The gas that is come out by rough segmentation tower 8 tops gets into partial condenser 5, and the liquid that condensation is got off is back to the rough segmentation tower, and gas is discharged by the partial condenser top; Simultaneously the key of this technology is the temperature of control partial condenser outlet, thereby keeps constant ratio and temperature through aperture control partial condenser 5 Outlet Gas Temperatures that TP 13 temperature sensors are controlled temperature-sensing valve 12, and partial condenser 5 Outlet Gas Temperatures are controlled at 93 ℃; Wherein contain (massfraction) hydrogen 11.1%; Nitrogen 42.7%, ETHYLE ACETATE 3.3%, ethanol 41.8%; Water 0.5%, other component 0.6%.This gas mixture is being back to system response after recycle blower 34 boosts.And in rough segmentation tower 8 bottom liquids, contain (massfraction) ETHYLE ACETATE 1.5%, ethanol 59.0%, water 0.7%; Terepthaloyl moietie 38.0%; Other by product 0.8%, bottom expel liquid temperature is 116 ℃, this part heat can be used for the heating raw oxalic acid diethyl ester; Rough segmentation tower bottom liquid effluent temperature is reduced to 62 ℃ of taking-ups after preheater 2 heat exchange, and the raw material oxalic acid diethyl ester is heated to 108 ℃ and sends into vaporization tower 6 simultaneously.Hydrogen and gaseous state alkyl alcohol return interchanger 1 preheating after being boosted by recycle blower 35 through pipeline 23 again, are back to the reactive system reaction then.
Transformation efficiency according to the analytical results oxalic acid diethyl ester is 100%, and the average selectivity of terepthaloyl moietie is 93.8%.
In the prior art, reclaim ethanol and need rectifying.Ethanol rectifying tower overhead condenser load Q=m * C
p* (T
2-T
1)+m * r, wherein m is the overhead product mass rate, kg h
-1C
pBe the overhead product specific heat capacity, kJ K
-1Kg
-1(looking into the related tool handbook); T
1The condenser inlet temperature, K; T
2Be condensator outlet temperature, K; R is product latent heat of vaporization kJ kg
-1(looking into the related tool handbook).The substitution related data gets Q=10092.0kJ h
-1, required cooling water inflow W
Water=Q/ [C
p* (T
2-T
1)]=96kg h
-1(T
2Cooling water outlet temperature 313K; T
1Cooling water inlet temperature 298K; C
pBe that specific heat of water holds), by product, need cooling water inflow to be about the 61kg/kg product.
Same, need the material that rectifying is come out be heated once more with prior art production.In this process, be used for the reboiler Q=m that heats at the bottom of the rectifying tower
1* C
p* (T
2-T
1)+m
2* r, wherein m
1There are not phase transformation quality product flow, kg h for getting into reboiler
-1m
2For getting into reboiler phase transformation quality product flow, kg h are arranged
-1C
pBe the mix product mean specific heat, kJ K
-1Kg
-1T
1The reboiler inlet temperature, K; T
2Be reboiler temperature out, K; R is mixing prod latent heat of vaporization kJ kg
-1The substitution related data gets Q=9902.5kJ h
-1, required 180kPa (absolute pressure) steam 4.48kg h
-1,, need quantity of steam to be about the 3kg/kg product by product.Distillation ethanol selects for use 116 ℃ steam (corresponding vp 180kPa) to heat.
The calculating here is by 3.65kg h among the embodiment 1
-1The production capacity of raw material inlet amount (being equivalent to produce per year the pilot scale of 11 tons of terepthaloyl moietie) calculate.
Because do not need in the flow process of the present invention in the aforementioned calculation rectifying and with the step of reboiler heating, so the energy that can practice thrift of the present invention equal with quantity of steam above calculating rectifying and with reboiler heating heat and quantity of steam.
Claims (11)
1. working method by the continuous preparing ethylene glycol of barkite shortening; It is characterized in that: through controlled temperature; Make the recycle stock in the circulation loop keep gaseous phase, only reaction product and unreacted raw material condensation separation are come out, during reaction product is separated; Realize only will react the material that generates through control condensator outlet gas temperature and from recycle gas, separate with unreacted barkite, and the constant rate of permanent gases and alkyl alcohol in the maintenance circulation gas.
2. method according to claim 1 is characterized in that: recycle stock is mainly the permanent gases that adds in the reaction, mainly comprises hydrogen, rare gas element and the alkyl alcohol that before reaction, adds; Wherein alkyl substituent is identical with alkyl carbon containing quantity in the barkite in the alkyl alcohol.
3. method as claimed in claim 2 is characterized in that: rare gas element comprises at least a in nitrogen and the argon gas.
4. method according to claim 1 is characterized in that: the concentration of controlling the barkite in the mixed gas through the temperature of control barkite vaporising device outlet.
5. method according to claim 4 is characterized in that: the barkite vaporising device that is adopted is to guarantee that gas-liquid fully contacts and the little gas-liquid mass transfer (contact) equipment of gas phase drag mutually.
6. method according to claim 1; It is characterized in that: circulation loop mainly is made up of tower, pump, preheater; Gas-liquid flow to be adverse current or and stream, thereby control the purpose that reaches the control Outlet Gas Temperature into the temperature of tower liquid through the heat that adds preheater.
7. method according to claim 1 is characterized in that: condensing equipment can adopt two kinds of forms, and a kind of is the combination of rectifying tower and horizontal condenser, and another kind is the vertical (type) condenser of gas and phlegma adverse current.
8. method according to claim 7 is characterized in that: the characteristic of rectifying tower is rectifying section only to be arranged, no stripping section and reboiler in rectifying tower and the horizontal condenser combination; Condensing surface is a fractional distillating tube, it is characterized in that material gets into shell side, and dispersed phase holdup reaches the purpose of controlling Outlet Gas Temperature to regulate heat transfer area in the shell side through changing.
9. method as claimed in claim 8 is characterized in that: rectifying tower is for adopting corrugated-plate packed tower.
10. method according to claim 7 is characterized in that: two kinds of functions of rectifying in the adverse current vertical (type) condenser and partial condensation are combined in the equipment, and material steam gets into tube side by the bottom, and phlegma is drawn by the bottom, and the tail gas that does not coagulate is drawn at the top.
11. method according to claim 10 is characterized in that: the type of cooling is air-cooled, through air quantity control Outlet Gas Temperature.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102863316B (en) * | 2012-09-27 | 2015-04-08 | 安徽淮化股份有限公司 | Ethylene glycol production device |
| CN103804142B (en) * | 2012-11-07 | 2016-05-11 | 中国石油化工集团公司 | A kind of system and method for hydrogenation of oxalate for preparing ethylene glycol |
| CN103467248B (en) * | 2013-09-02 | 2016-05-04 | 东华工程科技股份有限公司 | A kind of energy-saving ester through hydrogenation technique |
| CN104355966A (en) * | 2014-11-06 | 2015-02-18 | 西南化工研究设计院有限公司 | Optimized reaction technology producing ethylene-glycol by adding hydrogen in oxalate |
| CN105418365A (en) * | 2015-12-27 | 2016-03-23 | 安徽淮化股份有限公司 | Novel synthetic-gas-to-ethylene-glycol hydrogenation unit |
| CN109482107B (en) * | 2018-11-30 | 2021-06-25 | 华东理工大学 | Method and apparatus for vaporizing dimethyl oxalate |
| CN112479814A (en) * | 2019-09-12 | 2021-03-12 | 南京延长反应技术研究院有限公司 | Reaction system and process for strengthening hydrogenation of dimethyl oxalate in coal-to-ethylene glycol |
| CN111454151B (en) * | 2020-04-26 | 2023-04-14 | 宁波中科远东催化工程技术有限公司 | Method for vaporizing dimethyl oxalate |
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| CN101475443A (en) * | 2008-12-18 | 2009-07-08 | 中国石油化工股份有限公司 | Method for preparing ethylene glycol |
| CN101475441A (en) * | 2008-12-18 | 2009-07-08 | 中国石油化工股份有限公司 | Method for preparing ethylene glycol from oxalic ester |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101342489A (en) * | 2007-07-12 | 2009-01-14 | 上海焦化有限公司 | Hydrogenation reaction catalyst, preparation and application thereof |
| CN101462961A (en) * | 2008-01-28 | 2009-06-24 | 上海戊正工程技术有限公司 | Process flow for producing ethylene glycol with coproduction product dimethyl carbonate |
| CN101475443A (en) * | 2008-12-18 | 2009-07-08 | 中国石油化工股份有限公司 | Method for preparing ethylene glycol |
| CN101475441A (en) * | 2008-12-18 | 2009-07-08 | 中国石油化工股份有限公司 | Method for preparing ethylene glycol from oxalic ester |
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