CN107915641A - The method of extracting distillation separation C dimethyl phthalate and methanol - Google Patents
The method of extracting distillation separation C dimethyl phthalate and methanol Download PDFInfo
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- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/08—Purification; Separation; Stabilisation
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- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
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- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
- C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
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Abstract
The present invention relates to a kind of method of extracting distillation separation C dimethyl phthalate and methanol, mainly solve the problems, such as that prior art energy consumption is excessive and environmental pollution.Method of the invention by using extracting distillation separation C dimethyl phthalate and methanol, the extracting rectifying uses anion as technical solution of the ionic liquid of three (pentafluoroethyl group) trifluoro phosphate radicals as extractant, preferably solves the technical problem, available in the industrial production of separating dimethyl carbonate and methanol.
Description
Technical field
The present invention relates to a kind of method of extracting distillation separation C dimethyl phthalate and methanol.
Background technology
Dimethyl carbonate (DMC) is a kind of environmental-friendly chemical intermediate, be widely used in methylate, be carbonylated, carbonyl
Methylate and methoxylation etc. is reacted, be known as " the new foundation stone " of current organic synthesis.Industrial generally use ester-interchange method life
Dimethyl carbonate is produced, in process of production, dimethyl carbonate forms azeotropic mixture with methanol, it is difficult to is separated with conventional distillation method.
Have the technologies such as extracting rectifying, compression rectification, azeotropic distillation and UF membrane in recent years to be used to produce high-purity
Dimethyl carbonate.Compared with three kinds of techniques below, extracting rectifying has that energy consumption is low, technique is simple and solvent selection is extensively etc. excellent
Gesture, is the technological trend of energy-saving separating dimethyl carbonate and methanol azeotrope.
Patent CN103159586A discloses a kind of dimethyl carbonate-methanol azeotropic mixture continuous extraction rectifying separation
Method.Under normal pressure, spent glycol is 1~3 as extractant, solvent ratio, is existed by separated dimethyl carbonate-carbinol mixture
The middle part charging of tower, extractant is in its top feed of tower, reflux ratio 2, in the first of the overhead extraction high-purity of extractive distillation column
Alcohol, bottom of towe extraction dimethyl carbonate and extractant, tower bottom distillate enter extractant recovery tower, reflux ratio 3, overhead extraction carbonic acid
Dimethyl ester, the extractant of bottom of towe extraction can recycle.Extractant ethylene glycol and dimethyl carbonate and methanol there are phase-separating section,
Separative efficiency is caused to reduce, energy consumption increase.
Patent CN105037162A discloses a kind of continuous extraction rectifying point of dimethyl carbonate-methanol azeotropic mixture
From method.With N, N-dimethylformamide, N-N-formyl morpholine N or the two using the mixture that arbitrary proportion forms as extractant.Extraction
Rectifying column, solvent recovery tower operating condition under normal or reduced pressure, the ratio of extractive distillation column overhead and extractant
For 0.5:1—10:1, the charge ratio (quality) of extractant and mixture is 1:10—5:1, reach extraction using two rectifying columns
Take the recycling of agent.Using volatile N, N- dimethylformamides, N- N-formyl morpholine Ns or both mixture are as extractant, easily
Cause problem of environmental pollution.
Patent CN1367772A discloses a kind of side for separating methanol and dimethyl carbonate in distillation column by extractive distillation
Method, takes steam side run-off away from distillation column.Phenol is used as extractant, but phenol fusing point is higher, easily ties at normal temperatures
Crystalline substance causes line clogging problem.
In conclusion the prior art uses conventional organic solvents to separate carbonic acid two by extracting rectifying as extractant
Methyl esters and methanol, there are energy consumption is excessive and problem of environmental pollution.
Ionic liquid is made of zwitterion, there is non-volatile, good heat stability, structure can design low with fusing point etc. excellent
Benign matter, it is considered to be a kind of new green solvent, obtains in fields such as chemical reaction, chemical separating and gas treatments in recent years
To extensive use and research.
The content of the invention
The technical problems to be solved by the invention are that energy consumption existing in the prior art is excessive and problem of environmental pollution；There is provided
A kind of separation method of new dimethyl carbonate and methanol, this method have a good separating effect, low and environmentally protective excellent of energy consumption
Point.
In order to solve the above technical problems, technical scheme is as follows：A kind of extracting distillation separation C dimethyl phthalate and
The method of methanol, the extracting rectifying use the ionic liquid that anion is three (pentafluoroethyl group) trifluoro phosphate radicals to be used as extraction
Agent.
In above-mentioned technical proposal, it is preferable that the cation of the ionic liquid is selected from alkylimidazolium cation, alkyl pyridine
At least one of cation and quaternary ammonium cation.
In above-mentioned technical proposal, it is highly preferred that the cation of the ionic liquid is selected from the alkyl-substituted imidazoles sun of 1,3-
Ion [R1R3im]+, N- alkylpyridiniium cations [Rpy]+With alkyl-quaternaryammonium cations [NR1R2R3R4]+At least one of.
In above-mentioned technical proposal, it is further preferred that in the cation of the ionic liquid alkyl be selected from methyl, ethyl,
Propyl group, isopropyl, normal-butyl, sec-butyl, the tert-butyl group, hexyl, heptyl and octyl group.
In above-mentioned technical proposal, it is preferable that the molar ratio of the ionic liquid and dimethyl carbonate and carbinol mixture is
More than 0.2, it is preferably 0.4~1, more preferably 0.6~0.8.
In above-mentioned technical proposal, it is preferable that the quality of dimethyl carbonate is dense in the dimethyl carbonate and carbinol mixture
Spend for 1~60%, preferably 20~50%.
In above-mentioned technical proposal, it is preferable that the extractant is added from extractive distillation column top, dimethyl carbonate and methanol
Added by extractive distillation column lower part, overhead product is methanol, and tower kettle product is dimethyl carbonate and ionic liquid mixture.
In above-mentioned technical proposal, it is preferable that the tower kettle product is sent to solvent recovery flash column, and tower top obtains after flash distillation
Dimethyl carbonate, the ionic liquid that tower reactor obtains are recycled to extractive distillation column.
In above-mentioned technical proposal, it is preferable that the extractive distillation column operating pressure is normal pressure~0.5MPa, and reflux ratio is
0.5~5, bottom temperature is 60~150 DEG C, and theoretical cam curve is 20~50 pieces.
In above-mentioned technical proposal, it is preferable that the solvent recovery flash column operating pressure is 0.001~0.05MPa, operation
Temperature is 100~200 DEG C.
Ionic liquid of the present invention may be selected from three fluorophosphate of 1- ethyl-3-methylimidazoles three (pentafluoroethyl group)
([emim] [FEP]), three fluorophosphate of 1- hexyls pyridine three (pentafluoroethyl group) ([hpy] [FEP]) and tributyl-methyl phosphonium ammonium three (five
Fluoro ethyl) three fluorophosphate ([N1444] [FEP]) at least one of, preferably three-pentafluoroethyl group of 1- ethyl-3-methylimidazoles-
- three fluorophosphate of three fluorophosphates and three-pentafluoroethyl group of 1- hexyl pyridines.
Extractive distillation column of the present invention can be plate column or packed tower.Plate column includes bubble column, sieve-plate tower and floats
Valve tower, is preferably sieve-plate tower；Filler used in packed tower includes dumped packing and structured packing, filler be preferably Pall ring filler or
Woven wire structured packing.
Fig. 1 is-three fluorophosphate of three-pentafluoroethyl group of ionic liquid 1- ethyl-3-methylimidazoles ([emim] [FEP]) not
With the influence under the conditions of solvent ratio to dimethyl carbonate-methanol vapor liquid equilibrium curve；Fig. 2 be ionic liquid 1- hexyls pyridine three-
The fluorophosphate of pentafluoroethyl group-three ([hpy] [FEP]) is bent to dimethyl carbonate-methanol vapor liquid equilibrium under the conditions of different solvents ratio
The influence of line.When [emim] [FEP] and dimethyl carbonate-methanol admixture solvent ratio are 0.25, [hpy] [FEP] and carbonic acid two
When methyl esters-carbinol mixture solvent ratio is 0.25, ionic liquid will improve methanol concentration in gas-liquid, break dimethyl carbonate
Formed with the azeotropic of methanol, so that the dimethyl carbonate of high-purity can be obtained by rectification method.
It is the ionic liquid of three (pentafluoroethyl group) trifluoro phosphate radicals as extractant that the present invention, which uses anion, improves carbon
Dimethyl phthalate and methanol relative volatility, have obtained the dimethyl carbonate of high-purity, achieve preferable technique effect, can be used for
In the industrial production of continuous separating dimethyl carbonate and methanol.Technical solution using the present invention, not only dimethyl carbonate and first
Alcohol good separating effect, and have the characteristics that energy consumption is low and environmentally protective.
Brief description of the drawings
Fig. 1 is isothermal (60 DEG C) vapor liquid equilibrium curve of [emim] [FEP]-dimethyl carbonate-methanol three-component system.
In Fig. 1, methanol concentration is represented in Methanol-Dimethyl Carbonate-ionic liquid ternary system after removing ionic liquid, will
The Methanol Molar fraction obtained after methanol and concentration of dimethyl carbonate solution normalization.[emim] [FEP] is mixed with dimethyl carbonate-methanol
Compound solvent is than being respectively 0.25,0.42 and 1.
Fig. 2 is isothermal (60 DEG C) vapor liquid equilibrium curve of [hpy] [FEP]-dimethyl carbonate-methanol three-component system.
In Fig. 2, methanol concentration is represented in Methanol-Dimethyl Carbonate-ionic liquid ternary system after removing ionic liquid, will
The Methanol Molar fraction obtained after methanol and concentration of dimethyl carbonate solution normalization.[hpy] [FEP] is mixed with dimethyl carbonate-methanol
Compound solvent is than being respectively 0.25,0.42 and 1.
Fig. 3 is separation of extractive distillation process flow chart.
In Fig. 3, T1 is extractive distillation column；T2 is flash column；1 is dimethyl carbonate and the mixture of methanol；2 be ionic liquid
Body；3 be methanol；4 be dimethyl carbonate.Extractant ionic liquid from extractive distillation column top add, oxide spinel dimethyl ester and
The mixture of methanol is added from extractive distillation column lower part, and after extract and separate, extracting rectifying tower overhead is methanol, and tower reactor is produced
Thing is dimethyl carbonate and ionic liquid mixture, and extractive distillation column tower kettle product is delivered to solvent recovery flash column through pump,
Flashed through high temperature, tower top obtains high purity carbon dimethyl phthalate, and the ionic liquid of tower reactor extraction, which is back to extractive distillation column circulation, to be made
With.
Further instruction is given to the present invention below by embodiment, but does not limit present disclosure.
Embodiment
【Embodiment 1】
Extracting rectifying flow as shown in Figure 3.Extractive distillation column has 25 pieces of theoretical trays (number of plates counts from top to bottom), extraction
Agent ionic liquid 1- ethyl-3-methylimidazoles three (pentafluoroethyl group) three fluorophosphate ([emim] [FEP]) is taken to add from the 2nd block of column plate
Enter, flow 9kg/h, the mixture of oxide spinel dimethyl ester and methanol is added from the 23rd block of column plate, and DMC addition is
30wt%, methanol content 70wt%, total flow 1kg/h, extractant and feed molar solvent ratio are 0.64 at this time.Extraction essence
Evaporate tower to operate under normal pressure, tower top condenses entirely, reflux ratio 1.2, and overhead extraction amount is 0.7kg/h, can obtain 99.85wt%'s
The dimethyl carbonate of methanol and 0.15wt%.Extracting rectifying column overhead temperatures are 40 DEG C, and bottom temperature is 99 DEG C.Extractive distillation column
Tower kettle product is to be delivered to solvent recovery flash column, operating pressure 1kPa through pump, and heating-up temperature is 120 DEG C, and tower top flow is
0.3kg/h, can obtain the dimethyl carbonate and 0.2wt% methanol of 99.8wt%.
【Embodiment 2】
Extracting rectifying flow as shown in Figure 3.Extractive distillation column has 25 pieces of theoretical trays (number of plates counts from top to bottom), extraction
Agent ionic liquid 1- ethyl-3-methylimidazoles three (pentafluoroethyl group) three fluorophosphate ([emim] [FEP]) is taken to add from the 2nd block of column plate
Enter, flow 10kg/h, the mixture of oxide spinel dimethyl ester and methanol is added from the 23rd block of column plate, and DMC addition is
40wt%, methanol content 60wt%, total flow 1kg/h, extractant and feed molar solvent ratio are 0.78 at this time.Extraction essence
Evaporate tower to operate under normal pressure, tower top condenses entirely, reflux ratio 0.9, and overhead extraction amount is 0.6kg/h, can obtain 99.9wt%'s
The dimethyl carbonate of methanol and 0.1wt%.Extracting rectifying column overhead temperatures are 40 DEG C, and bottom temperature is 96 DEG C.Extractive distillation column
Tower kettle product is to be delivered to solvent recovery flash column, operating pressure 1kPa through pump, and heating-up temperature is 120 DEG C, and tower top flow is
0.4kg/h, can obtain the dimethyl carbonate and 0.11wt% methanol of 99.89wt%.
【Embodiment 3】
Extracting rectifying flow as shown in Figure 3.Extractive distillation column has 25 pieces of theoretical trays (number of plates counts from top to bottom), extraction
Agent ionic liquid 1- ethyl-3-methylimidazoles three (pentafluoroethyl group) three fluorophosphate ([emim] [FEP]) is taken to add from the 2nd block of column plate
Enter, flow 9.5kg/h, the mixture of oxide spinel dimethyl ester and methanol is added from the 23rd block of column plate, DMC addition
For 50wt%, methanol content 50wt%, total flow 1kg/h, extractant and feed molar solvent ratio are 0.81 at this time.Extraction
Rectifying column operates under normal pressure, and tower top condenses entirely, reflux ratio 0.7, and overhead extraction amount is 0.5kg/h, can obtain 99.93wt%
Methanol and 0.07wt% dimethyl carbonate.Extracting rectifying column overhead temperatures are 40 DEG C, and bottom temperature is 89 DEG C.Extracting rectifying
Tower tower kettle product is to be delivered to solvent recovery flash column, operating pressure 1kPa through pump, and heating-up temperature is 120 DEG C, tower top flow
For 0.5kg/h, the dimethyl carbonate and 0.10wt% methanol of 99.90wt% can obtain.
【Embodiment 4】
Extracting rectifying flow as shown in Figure 3.Extractive distillation column has 25 pieces of theoretical trays (number of plates counts from top to bottom), extraction
Agent ionic liquid 1- ethyl-3-methylimidazoles three (pentafluoroethyl group) three fluorophosphate ([emim] [FEP]) is taken to add from the 2nd block of column plate
Enter, flow 6.5kg/h, the mixture of oxide spinel dimethyl ester and methanol is added from the 23rd block of column plate, DMC addition
For 40wt%, methanol content 60wt%, total flow 1kg/h, extractant and feed molar solvent ratio are 0.47 at this time.Extraction
Rectifying column operates under normal pressure, and tower top condenses entirely, reflux ratio 1.2, and overhead extraction amount is 0.6kg/h, can obtain 99.50wt%
Methanol and 0.50wt% dimethyl carbonate.Extracting rectifying column overhead temperatures are 40 DEG C, and bottom temperature is 96 DEG C.Extracting rectifying
Tower tower kettle product is to be delivered to solvent recovery flash column, operating pressure 1kPa through pump, and heating-up temperature is 120 DEG C, tower top flow
For 0.4kg/h, the dimethyl carbonate and 0.9wt% methanol of 99.1wt% can obtain.
【Embodiment 5】
Extracting rectifying flow as shown in Figure 3.Extractive distillation column has 30 pieces of theoretical trays (number of plates counts from top to bottom), extraction
Three (pentafluoroethyl group) three fluorophosphate ([hpy] [FEP]) of agent ionic liquid 1- hexyls pyridine is taken to be added from the 2nd block of column plate, flow
For 9kg/h, the mixture of oxide spinel dimethyl ester and methanol is added from the 27th block of column plate, DMC addition 30wt%,
Methanol content is 70wt%, total flow 1kg/h, and extractant and feed molar solvent ratio are 0.64 at this time.Extractive distillation column exists
Operated under 1bar, tower top condenses entirely, reflux ratio 1.4, and overhead extraction amount is 0.7kg/h, can obtain 99.9wt% methanol and
The dimethyl carbonate of 0.1wt%.Extracting rectifying column overhead temperatures are 40 DEG C, and bottom temperature is 105 DEG C.Extractive distillation column tower reactor is produced
Thing is to be delivered to solvent recovery flash column, operating pressure 2kPa through pump, and heating-up temperature is 160 DEG C, and tower top flow is 0.3kg/
H, can obtain the dimethyl carbonate and 0.18wt% methanol of 99.82wt%.
【Embodiment 6】
Extracting rectifying flow as shown in Figure 3.Extractive distillation column has 25 pieces of theoretical trays (number of plates counts from top to bottom), extraction
Take agent ionic liquid 1- ethyl-3-methylimidazoles three (pentafluoroethyl group) three fluorophosphate ([emim] [FEP]) and 1- hexyl pyridines
Three (pentafluoroethyl group) three fluorophosphate ([hpy] [FEP]) mixed solvent is added from the 2nd block of column plate, flow be respectively 4kg/h and
The mixture of 4kg/h, oxide spinel dimethyl ester and methanol is added from the 23rd block of column plate, DMC addition 30wt%, first
Alcohol content is 70wt%, total flow 1kg/h, and extractant and feed molar solvent ratio are 0.57 at this time.Extractive distillation column exists
Operated under 1bar, tower top condenses entirely, reflux ratio 0.9, and overhead extraction amount is 0.7kg/h, can obtain 99.9wt% methanol and
The dimethyl carbonate of 0.1wt%.Extracting rectifying column overhead temperatures are 40 DEG C, and bottom temperature is 95 DEG C.Extractive distillation column tower reactor is produced
Thing is to be delivered to solvent recovery flash column, operating pressure 2kPa through pump, and heating-up temperature is 160 DEG C, and tower top flow is 0.3kg/
H, can obtain the dimethyl carbonate and 0.14wt% methanol of 99.86wt%.
【Embodiment 7】
Extracting rectifying flow as shown in Figure 3.Extractive distillation column has 25 pieces of theoretical trays (number of plates counts from top to bottom), extraction
Take agent ionic liquid tributyl-methyl phosphonium ammonium three (pentafluoroethyl group) three fluorophosphate ([N1444] [FEP]) added from the 2nd block of column plate, stream
Measure as 8kg/h, the mixture of oxide spinel dimethyl ester and methanol is added from the 23rd block of column plate, and DMC addition is
30wt%, methanol content 70wt%, total flow 1kg/h, extractant and feed molar solvent ratio are 0.66 at this time.Extraction essence
Evaporate tower to operate under normal pressure, tower top condenses entirely, reflux ratio 1.6, and overhead extraction amount is 0.7kg/h, can obtain 99.79wt%'s
The dimethyl carbonate of methanol and 0.31wt%.Extracting rectifying column overhead temperatures are 40 DEG C, and bottom temperature is 93 DEG C.Extractive distillation column
Tower kettle product is to be delivered to solvent recovery flash column, operating pressure 1kPa through pump, and heating-up temperature is 120 DEG C, and tower top flow is
0.4kg/h, can obtain the dimethyl carbonate and 0.49wt% methanol of 99.51wt%.
【Comparative example 1】
Using anion as tetrafluoroborate ion liquid [BF4] exemplified by, [omim] BF4With dimethyl carbonate-methanol mixture
When solvent ratio is 0.42, the relative volatility under certain concentration is 1.668 to dimethyl carbonate with methanol.Under the same conditions, originally
Example used in ionic liquid [hmim] [FEP], [bmmim] [FEP] and [EOEmim] [FEP] dimethyl carbonate and methanol it is opposite
Volatility is 2,2.2 and 1.8, better than [omim] BF4。
【Comparative example 2】
Extracting rectifying flow as shown in Figure 3.Extractive distillation column has 25 pieces of theoretical trays (number of plates counts from top to bottom), extraction
Take agent ionic liquid 1- decyl -3- methyl imidazolium tetrafluoroborates ([omim] [BF4]) added from the 2nd block of column plate, flow is
The mixture of 6.4kg/h, oxide spinel dimethyl ester and methanol is added from the 23rd block of column plate, DMC addition 30wt%,
Methanol content is 70wt%, total flow 1kg/h, and extractant and feed molar solvent ratio are 0.92 at this time.Extractive distillation column exists
Normal pressing operation, tower top condense entirely, reflux ratio 1.5, and overhead extraction amount is 0.7kg/h, can obtain 99.3wt% methanol and
The dimethyl carbonate of 0.7wt%.Extracting rectifying column overhead temperatures are 40 DEG C, and bottom temperature is 99 DEG C.Extractive distillation column tower reactor is produced
Thing is to be delivered to solvent recovery flash column, operating pressure 1kPa through pump, and heating-up temperature is 120 DEG C, and tower top flow is 0.3kg/
H, can obtain the dimethyl carbonate and 1.50wt% methanol of 98.50wt%.
Claims (10)
1. a kind of method of extracting distillation separation C dimethyl phthalate and methanol, the extracting rectifying uses anion as three (five fluorine
Ethyl) trifluoro phosphate radical ionic liquid as extractant.
2. the method for extracting distillation separation C dimethyl phthalate and methanol according to claim 1, it is characterised in that the ion
The cation of liquid is selected from least one of alkylimidazolium cation, alkylpyridiniium cation and quaternary ammonium cation.
3. the method for extracting distillation separation C dimethyl phthalate and methanol according to claim 2, it is characterised in that the ion
The cation of liquid is selected from the alkyl-substituted glyoxaline cation [R of 1,3-1R3im]+, N- alkylpyridiniium cations [Rpy]+, alkyl
Quaternary ammonium cation [NR1R2R3R4]+At least one of.
4. the method for extracting distillation separation C dimethyl phthalate and methanol according to claim 3, it is characterised in that the ion
In the cation of liquid alkyl be selected from methyl, ethyl, propyl group, isopropyl, normal-butyl, sec-butyl, the tert-butyl group, hexyl, heptyl and
Octyl group.
5. the method for extracting distillation separation C dimethyl phthalate and methanol according to claim 1, it is characterised in that the ion
Liquid is more than 0.2 with the molar ratio of dimethyl carbonate and carbinol mixture, is preferably 0.4~1, more preferably 0.6~0.8.
6. the method for extracting distillation separation C dimethyl phthalate and methanol according to claim 1, it is characterised in that the carbonic acid
The mass concentration of dimethyl carbonate is 1~60% in dimethyl ester and carbinol mixture, is preferably 20~50%.
7. according to the method for any one of claim 1 to the 6 extracting distillation separation C dimethyl phthalate and methanol, it is characterised in that
The extractant is added from extractive distillation column top, and dimethyl carbonate and methanol are added by extractive distillation column lower part, overhead product
For methanol, tower kettle product is dimethyl carbonate and ionic liquid mixture.
8. the method for extracting distillation separation C dimethyl phthalate and methanol according to claim 7, it is characterised in that the tower reactor
Product is sent to solvent recovery flash column, and tower top obtains dimethyl carbonate after flash distillation, and the ionic liquid that tower reactor obtains is recycled to extraction
Take rectifying column.
9. the method for extracting distillation separation C dimethyl phthalate and methanol according to claim 7, it is characterised in that the extraction
Rectifying column operating pressure is normal pressure~0.5MPa, and reflux ratio is 0.5~5, and bottom temperature is 60~150 DEG C, and theoretical cam curve is
20~50 pieces.
10. the method for extracting distillation separation C dimethyl phthalate and methanol according to claim 8, it is characterised in that the solvent
Recycling flash column operating pressure is 0.001~0.05MPa, and operation temperature is 100~200 DEG C.
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| CN111004092A (en) * | 2019-12-26 | 2020-04-14 | 岳阳昌德环境科技有限公司 | Method for separating dimethyl carbonate and methanol |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111004092A (en) * | 2019-12-26 | 2020-04-14 | 岳阳昌德环境科技有限公司 | Method for separating dimethyl carbonate and methanol |
| CN111004092B (en) * | 2019-12-26 | 2022-04-29 | 昌德新材科技股份有限公司 | Method for separating dimethyl carbonate and methanol |
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