CN107935856A - Energy-saving methyl formate process units and its technique - Google Patents
Energy-saving methyl formate process units and its technique Download PDFInfo
- Publication number
- CN107935856A CN107935856A CN201711474419.0A CN201711474419A CN107935856A CN 107935856 A CN107935856 A CN 107935856A CN 201711474419 A CN201711474419 A CN 201711474419A CN 107935856 A CN107935856 A CN 107935856A
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- China
- Prior art keywords
- methyl formate
- methanol
- tower
- gas
- heater
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- TZIHFWKZFHZASV-UHFFFAOYSA-N Methyl formate Chemical compound COC=O TZIHFWKZFHZASV-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title claims abstract description 26
- OKKJLVBELUTLKV-UHFFFAOYSA-N methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 76
- 238000006356 dehydrogenation reaction Methods 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000009834 vaporization Methods 0.000 claims abstract description 16
- 238000005201 scrubbing Methods 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 24
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000007791 liquid phase Substances 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 229910000423 chromium oxide Inorganic materials 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 229910000460 iron oxide Inorganic materials 0.000 claims description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- WGLPBDUCMAPZCE-UHFFFAOYSA-N trioxochromium Chemical group O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract 1
- BDAGIHXWWSANSR-UHFFFAOYSA-N formic acid Chemical compound OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 6
- 239000002699 waste material Substances 0.000 description 4
- 239000012267 brine Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- WBJINCZRORDGAQ-UHFFFAOYSA-N Ethyl formate Chemical group CCOC=O WBJINCZRORDGAQ-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 125000004435 hydrogen atoms Chemical group [H]* 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000004702 methyl esters Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006011 modification reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/39—Preparation of carboxylic acid esters by oxidation of groups which are precursors for the acid moiety of the ester
- C07C67/40—Preparation of carboxylic acid esters by oxidation of groups which are precursors for the acid moiety of the ester by oxidation of primary alcohols
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention discloses a kind of energy-saving methyl formate process units and its technique.The device includes the methanol reaction zone and methyl formate rectification zone being connected；Methanol reaction zone includes methanol basin, methanol pump, heater, vaporization tower, heat exchanger, superheater and the dehydrogenation reactor being sequentially communicated；Heat exchanger is connected with dehydrogenation reactor and heater respectively；Methyl formate rectification zone includes rectifying column, condenser, gas-liquid separator and the scrubbing tower being sequentially communicated；Rectifying column is connected with scrubbing tower, heater and vaporization tower respectively；The technique comprises the following steps：(1) methanol carries out dehydrogenation reaction, prepares mixed gas；(2) mixed gas heat recovery, and enter rectifying column；(3) mixed gas isolated product methyl formate in rectifying column；(4) washing gas by the way of low-temp methanol is washed.The present apparatus is during methyl formate is prepared, and consume energy low, high income.
Description
Technical field
The invention belongs to methyl formate preparing technical field, and in particular to a kind of energy-saving methyl formate process units and its
Technique.
Background technology
Methyl formate is typically all to be prepared by methanol dehydrogenation, is usually to pass through methyl formate gas in traditional handicraft
Cross condenser and be cooled to room temperature, into scrubbing tower, then with the methanol after chilled brine freezing to the methyl formate in gas
Absorbed, enter methyl esters rectifying column after the mixed liquor after absorption is preheated, this technique is first by gas cooling, and absorbing liquid is with cold
Freeze brine-cooled, reabsorb, absorption is over and heats, this part energy causes great waste.
The content of the invention
For above-mentioned deficiency of the prior art, the present invention provides a kind of energy-saving methyl formate process units and its work
Skill, can effectively solve the problem of existing apparatus energy consumption is high, and efficiency is low.
To solve above-mentioned technical problem, the technical solution adopted by the present invention is：
A kind of energy-saving methyl formate process units, including the methanol reaction zone being connected and methyl formate rectifying are provided
Area；
Methanol reaction zone include be sequentially communicated methanol basin, methanol pump, heater, vaporization tower, heat exchanger, superheater with
And dehydrogenation reactor；Heat exchanger is connected with dehydrogenation reactor and heater respectively；
Methyl formate rectification zone includes rectifying column, condenser, gas-liquid separator and the scrubbing tower being sequentially communicated；Rectifying column
Connected respectively with scrubbing tower, heater and vaporization tower.
Further, condenser includes the first condenser and the second condenser being connected；First condenser and second cold
Condenser is connected with rectifying column and gas-liquid separator respectively.
Further, scrubbing tower is also connected with methanol subcooler.
The technique that methyl formate is prepared using above device, is comprised the following steps：
(1) methanol is pumped into heater, and the mixed gas heat exchange in system, and 50~60 DEG C are warming up to, Ran Houjin
Enter vaporization tower, vaporized at 60~80 DEG C, then enter 200~230 DEG C of dehydrogenation reactor through heat exchanger, dehydrogenation prepares gaseous mixture
Body；
(2) mixed gas is entered heat exchanger, then heater is entered by heat exchanger, rectifying column is then entered by heater
Rectifying；
(3) methyl formate and hydrogen in mixed gas, is entered in condenser by rectifying column tower top and condensed, then passes through gas-liquid
Separator separates, and rectifying tower bottom component directly returned in vaporization tower, vaporizes, subsequently into dehydrogenation reactor dehydrogenation, continue by
Step (2) and step (3) process carry out；
(4) gas phase that gas-liquid separator separates obtain is washed into scrubbing tower, is collected the methyl formate that washing obtains, is made it
Return to rectifying column and continue to separate by step (3) process；The liquid phase that gas-liquid separator separates obtain is collected, obtains formic acid first
Ester.
Further, the catalyst in step (1) in dehydrogenation reactor for chromium oxide, iron oxide, magnesia, copper, nickel or
Platinum.
Beneficial effects of the present invention are：
1st, enter from the methyl formate gas that dehydrogenation reactor comes out in heat exchanger, heat is carried out with the methanol steam newly entered
After exchange, enter back into heater and continue to carry out heat exchange with the methanol newly entered, reaching makes the formic acid first with amount of heat
Ester gas heat reduces, and reduces condenser negative pressure, reduces the purpose of heat waste in preparation process.
2nd, heat exchange is carried out by methanol and methyl formate gas, absorbs methyl formate gas heat, and rectifying column with
Vaporization tower directly connects so that tower bottom liquid is returned directly to vaporization tower, can effectively reduce and prepare energy during methyl formate
Waste, lifted preparation efficiency.
3rd, it under the cooperation of each component of the present apparatus, can effectively realize during methyl formate is prepared, reduce energy
Consumption and waste, save energy, reduce the purpose of production cost.
Brief description of the drawings
Fig. 1 is the structure diagram of the present apparatus.
Wherein, 1, methanol basin；2nd, methanol pump；3rd, heater；4th, vaporization tower；5th, heat exchanger；6th, superheater；7th, dehydrogenation is anti-
Answer device；8th, rectifying column；9th, the first condenser；10th, the second condenser；11st, gas-liquid separator；12nd, scrubbing tower；13rd, methanol is subcooled
Device.
Embodiment
The embodiment of the present invention is described below, in order to facilitate understanding by those skilled in the art this hair
It is bright, it should be apparent that the invention is not restricted to the scope of embodiment, for those skilled in the art,
As long as various change in the spirit and scope of the present invention that appended claim limits and determines, these changes are aobvious and easy
See, all are using the innovation and creation of present inventive concept in the row of protection.
As shown in Figure 1, the energy-saving methyl formate process units, including the methanol reaction zone being connected and methyl formate essence
Evaporate area, wherein, methanol reaction zone include be sequentially communicated methanol basin 1, methanol pump 2, heater 3, vaporization tower 4, heat exchanger 5,
Superheater 6 and dehydrogenation reactor 7.
As shown in Figure 1, heat exchanger 5 is connected with dehydrogenation reactor 7 and heater 3 respectively.
As shown in Figure 1, methyl formate rectification zone include be sequentially communicated rectifying column 8, condenser, gas-liquid separator 11 and
Scrubbing tower 12；Wherein, rectifying column 8 is connected with scrubbing tower 12, heater 3 and vaporization tower 4 respectively.
As shown in Figure 1, condenser includes the first condenser 9 and the second condenser 10 that are connected, the first condenser 9 and the
Two condensers 10 are separately provided for the chilled brine condensed；And first condenser 9 and the second condenser 10 respectively with
Rectifying column 8 is connected with gas-liquid separator 11.
As shown in Figure 1, scrubbing tower 12 is also connected with methanol subcooler 13.
The technique that methyl formate is prepared using above device, is comprised the following steps：
By the methanol from methanol basin 1 after methanol pump 2 is pressurizeed through existing mixed gas in heater 3 and device into
Row heat exchange, the methanol for making newly to enter are warming up to 60 DEG C, subsequently into vaporization tower 4, are vaporized at 60 DEG C, then respectively through heat exchanger
5th, cross dehydrogenation reactor 7 after superheater 6, dehydrogenation reaction occur under the action of the catalyst magnesia in dehydrogenation reactor 7,
Reaction temperature is 230 DEG C, obtains mixed gas, from the mixed gas that dehydrogenation reactor 7 comes out through heat exchanger 5 and the first newly entered
After alcohol carries out heat exchange, enter back into heater 3 and continue to carry out heat exchange with methanol, recycle the heat in mixed gas；
Then mixed gas is directly entered rectifying column 8 by heater 3 and carries out rectifying, and methyl formate gas and reaction produce
Hydrogen from 8 tower top of rectifying column through the first condenser 9 and the second condenser 10, condensed with chilled brine, gas-liquid entered after cooling
Separator 11 is separated, and liquid phase is formic ether product, and gas phase is hydrogen and a small amount of methyl formate, and then gas, which enters, washs
Tower 12 washs, and collects methyl formate therein, returns it in rectifying column 8, is separated again, and then gas-liquid separator 11 divides
It is 98.6% up to purity, yield reaches 98.3% methyl formate from obtained liquid phase.
And 8 tower bottom liquid main matter of rectifying column is methanol, temperature is 65 DEG C, is returned directly to vaporization tower 4 and vaporizes, Ran Houjin
Enter in dehydrogenation reactor 7, continue to carry out the preparation of methyl formate by the above process, to lift the utilization rate of methanol.
Embodiment is described in detail, but should not be construed as the restriction to the protection domain of this patent.
In the described scope of claims, various modifications and deformation that those skilled in the art can make without creative work
Still belong to the protection domain of this patent.
Claims (5)
1. a kind of energy-saving methyl formate process units, it is characterised in that including the methanol reaction zone being connected and methyl formate
Rectification zone；
Methanol basin (1) that the methanol reaction zone includes being sequentially communicated, methanol pump (2), heater (3), vaporization tower (4), change
Hot device (5), superheater (6) and dehydrogenation reactor (7)；The heat exchanger (5) respectively with dehydrogenation reactor (7) and heater
(3) connect；
The methyl formate rectification zone includes rectifying column (8), condenser, gas-liquid separator (11) and the scrubbing tower being sequentially communicated
(12)；The rectifying column (8) connects with scrubbing tower (12), heater (3) and vaporization tower (4) respectively.
2. energy-saving methyl formate process units according to claim 1, it is characterised in that the condenser includes being connected
Logical the first condenser (9) and the second condenser (10)；First condenser (9) and the second condenser (10) respectively with rectifying
Tower (8) is connected with gas-liquid separator (11).
3. energy-saving methyl formate process units according to claim 1, it is characterised in that the scrubbing tower (12) also with
Methanol subcooler (13) connects.
4. the technique that methyl formate is prepared using claims 1 to 3 any one of them device, it is characterised in that including following
Step：
(1) methanol is pumped into heater, and the mixed gas heat exchange in system, and 50~60 DEG C are warming up to, subsequently into vapour
Change tower, vaporized at 60~80 DEG C, then enter 200~230 DEG C of dehydrogenation reactor through heat exchanger, dehydrogenation prepares mixed gas；
(2) mixed gas is entered heat exchanger, then heater is entered by heat exchanger, rectifying column essence is then entered by heater
Evaporate；
(3) methyl formate and hydrogen in mixed gas, is entered in condenser by rectifying column tower top and condensed, then passes through gas-liquid separation
Device separates, and rectifying tower bottom component is directly returned in vaporization tower, vaporizes, subsequently into dehydrogenation reactor dehydrogenation, continues by step
(2) carried out with step (3) process；
(4) gas phase that gas-liquid separator separates obtain is washed into scrubbing tower, is collected the methyl formate that washing obtains, is returned it to
Rectifying column simultaneously is continued to separate by step (3) process；The liquid phase that gas-liquid separator separates obtain is collected, obtains methyl formate.
5. the technique according to claim 4 for preparing methyl formate, it is characterised in that dehydrogenation reaction described in step (1)
Catalyst in device is chromium oxide, iron oxide, magnesia, copper, nickel or platinum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711474419.0A CN107935856A (en) | 2017-12-29 | 2017-12-29 | Energy-saving methyl formate process units and its technique |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711474419.0A CN107935856A (en) | 2017-12-29 | 2017-12-29 | Energy-saving methyl formate process units and its technique |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107935856A true CN107935856A (en) | 2018-04-20 |
Family
ID=61936971
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711474419.0A Pending CN107935856A (en) | 2017-12-29 | 2017-12-29 | Energy-saving methyl formate process units and its technique |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107935856A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108484400A (en) * | 2018-04-02 | 2018-09-04 | 中国科学院福建物质结构研究所 | A kind of methyl formate production equipment |
| CN114539060A (en) * | 2022-04-27 | 2022-05-27 | 太原理工大学 | Method for preparing methyl formate by dehydrogenation of methanol without emission |
-
2017
- 2017-12-29 CN CN201711474419.0A patent/CN107935856A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108484400A (en) * | 2018-04-02 | 2018-09-04 | 中国科学院福建物质结构研究所 | A kind of methyl formate production equipment |
| CN114539060A (en) * | 2022-04-27 | 2022-05-27 | 太原理工大学 | Method for preparing methyl formate by dehydrogenation of methanol without emission |
| CN114539060B (en) * | 2022-04-27 | 2022-07-05 | 太原理工大学 | Method for preparing methyl formate by dehydrogenation of methanol without emission |
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