CN110922370A - Process method and device for batch rectification of crude maleic anhydride - Google Patents
Process method and device for batch rectification of crude maleic anhydride Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 49
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 238000010992 reflux Methods 0.000 claims abstract description 68
- 150000008064 anhydrides Chemical class 0.000 claims abstract description 41
- 238000007670 refining Methods 0.000 claims abstract description 32
- 238000005086 pumping Methods 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 24
- 238000002360 preparation method Methods 0.000 claims description 15
- 238000000998 batch distillation Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 2
- KNEXRQWDSVGRMS-UHFFFAOYSA-N phthalic acid;hydrate Chemical group O.OC(=O)C1=CC=CC=C1C(O)=O KNEXRQWDSVGRMS-UHFFFAOYSA-N 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims 1
- 238000005194 fractionation Methods 0.000 claims 1
- 235000013547 stew Nutrition 0.000 claims 1
- 238000003795 desorption Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 230000000087 stabilizing effect Effects 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000002918 waste heat Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000007789 gas Substances 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- XMTOUDRCWLYEHL-UHFFFAOYSA-N (2-bromo-3-ethoxy-6-fluorophenyl)boronic acid Chemical compound CCOC1=CC=C(F)C(B(O)O)=C1Br XMTOUDRCWLYEHL-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 241001093575 Alma Species 0.000 description 2
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003883 substance clean up Methods 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
- C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
- C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D307/60—Two oxygen atoms, e.g. succinic anhydride
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/007—Energy recuperation; Heat pumps
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
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- 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
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- 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
- Y02P20/50—Improvements relating to the production of bulk chemicals
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- 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
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
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Abstract
The invention discloses a process for batch rectification of crude maleic anhydride, which comprises the steps of stabilizing the steam flow in the batch rectification process of the crude maleic anhydride, pumping the crude anhydride into a standing tank through a pump, immersing a reboiler in the standing tank, using medium-pressure steam as a heat source, condensing a gas phase of a refining tower through a tower top condenser, then entering a reflux tank, refluxing a part of materials in the reflux tank to the top, and collecting the other part of materials out of a desorption tower or a tank area. Pumping out the heavy component residual anhydride in the standing tank; the overhead condenser uses hot water or other heat-taking media to take heat; the heat medium is taken out and enters the condenser, the other part of the heat medium is taken out of a secondary line, two paths of the heat medium are converged and enter the heater, and medium-pressure steam is used as a heat source for the heater. The invention stabilizes the flow of the heat-taking medium by the secondary line regulating valve of the condenser, stabilizes the temperature by heating the heat-taking medium by the steam of the heater, achieves the effect of stabilizing the steam usage amount of the whole refining tower, stabilizes the flow and the temperature of the heat-taking medium, and is beneficial to the waste heat recovery of the heat-taking medium.
Description
Technical Field
The invention relates to the technical field of compound purification, in particular to a process method and a device for batch rectification of crude maleic anhydride.
Background
Maleic anhydride is short for maleic anhydride, also known as maleic anhydride, and is the third largest anhydride which is second only to phthalic anhydride and crude anhydride in the world at present. Benzene has been produced by catalytic oxidation, but due to the cost, the benzene process is now gradually replaced by the n-butane oxidation. At present, most of post-treatment of maleic anhydride by n-butane oxidation adopts a solvent absorption-desorption process, typically a Hunstman process, a connector process and an ALMA process, wherein except that ALMA adopts diisobutyl hexahydrophthalate (DIBE), both Hunstman and connector adopt dibutyl phthalate (DBP) as a solvent. There have been a lot of research efforts on maleic anhydride oxidation processes and solvent absorption desorption processes, and they are also relatively smooth from the industrial application point of view.
Maleic anhydride desorbed by solvent absorption is called crude anhydride, and also contains some impurities, such as acetic acid, acrylic acid, phthalic anhydride, tar, etc. At present, the crude anhydride is industrially refined in two major types, one is a batch refining process represented by Hunstman, and the other is a continuous rectification process. Continuous rectification is carried out to remove light components such as acetic acid and acrylic acid with boiling point lower than that of maleic anhydride in a light component removal tower, and then heavy components such as tar in a heavy component removal tower to obtain refined maleic anhydride. The batch rectification process is carried out in a refining tower, and comprises the steps of feeding, vacuumizing, establishing reflux, removing front fraction, center fraction, breaking vacuum and the like in sequence according to time. The batch rectification has the advantages of lower energy consumption and higher product purity, so that the batch rectification is more widely applied to two processes of continuous rectification and batch rectification. However, the fluctuation of the steam flow used in the intermittent rectification process is large, the interference on the steam system and the hot water flow of the tower top condenser is large, and the stability of the steam system and the hot water system in a plant is not facilitated.
Disclosure of Invention
The invention aims to provide a process method and a device for batch rectification of crude maleic anhydride, which can stabilize the steam usage amount of a refining tower.
In order to solve the technical problems, the invention adopts the technical scheme that:
a process method for batch rectification of crude maleic anhydride comprises the following steps:
i) feeding: pumping the crude anhydride into a static tank V-1607;
j) vacuumizing: the refining process of the crude anhydride is negative pressure operation, and a vacuum pump is used for vacuumizing;
k) establishing tower internal reflux: introducing steam into an E-1606 reboiler, introducing a heat-taking medium into an E-1609 condenser for cooling, introducing steam into an E-1807 heater for heating the heat-taking medium, and establishing total reflux in a refining tower, wherein except for one part of the heat-taking medium entering the condenser, the other part of the heat-taking medium enters a heater after passing through a secondary line and being converged with the condensed heat-taking medium;
l) removing front cut fraction: introducing steam into an E-1606 reboiler, introducing a heat-taking medium into an E-1609 condenser for cooling, introducing steam into an E-18077 heater for heating the heat-taking medium, and removing front cut (light boiling point substances), wherein one part of the heat-taking medium enters the condenser, and the other part of the heat-taking medium enters the heater after being converged by the condensed heat-taking medium after passing through a secondary line;
m) center fraction: introducing steam into an E-1606 reboiler, introducing a heat medium into an E-1609 condenser for cooling, introducing steam into an E-1807 heater for heating the heat medium, and evaporating out central fraction, namely refined maleic anhydride, wherein except for one part of the heat medium entering the condenser, the other part of the heat medium enters the heater after passing through a secondary line and being converged with the condensed heat medium;
n) breaking vacuum: introducing nitrogen into the refining tower;
o) preparation state: the refining tower enters a preparation state and waits for the step of feeding or pumping out residual anhydride;
p) residual anhydride pump out: after a certain batch is carried out, residual anhydride in the standing tank can be accumulated and needs to be pumped out by a pump.
Preferably, the heat-taking medium is selected from water or dibutyl phthalate.
Preferably, the temperature of the heated medium is stabilized at 80 to 90 ℃, more preferably 84 to 86 ℃.
Preferably, the evacuation stage has an overhead pressure in the range of from 20 to 50kPaA, more preferably from 30 to 40 kPaA.
Preferably, said establishing of the reflux phase in the column is carried out at a reflux ratio of 1 to 15, more preferably 5 to 9.
Preferably, the prefractionation stage is operated at a pressure of from 20 to 50kPaA, more preferably from 30 to 40 kPaA; the reflux ratio is 1 to 10, more preferably 5 to 9.
Preferably, said heart cut stage operating pressure is in the range of from 1 to 20kPaA, more preferably from 1 to 10 kPaA; the reflux ratio is preferably from 0.3 to 2, more preferably from 0.3 to 1.
Preferably, the residual anhydride is pumped out in cumulative batches of 1 to 100, more preferably 30 to 50.
The invention also aims to provide a crude maleic anhydride batch rectification device which comprises a standing tank, a refining tower connected with the standing tank, a condenser arranged at the top of the refining tower, and a reflux tank connected with the condenser, wherein a heat taking medium inlet pipeline is connected to the condenser, a secondary line for regulating the flow of the heat taking medium is also arranged on the pipeline, one part of the heat taking medium enters the condenser, the other part of the heat taking medium enters the secondary line, and the two parts of the heat taking medium are converged and then enter a heater.
Further, the heater uses medium pressure steam as a heat source.
In summary, the technical scheme of the invention has the following beneficial effects:
1. the batch rectification method is adopted, the process flow is short, the equipment investment is low, the energy consumption is low, and the purity of the processed refined maleic anhydride product is high.
2. The steam quantity used in each stage of the batch distillation in the prior art is fluctuant, and the flow of the heat-taking medium entering the overhead condenser E-1609 is also fluctuant. The invention stabilizes the flow of the heat-taking medium by the E-1609 secondary line regulating valve, stabilizes the temperature by heating the heat-taking medium by E-1807 steam, achieves the effect of stabilizing the steam usage of the whole refining tower, stabilizes the flow and the temperature of the heat-taking medium, and is beneficial to the waste heat recovery of the heat-taking medium.
Drawings
FIG. 1 is a schematic process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, but the technical solutions do not limit the scope of the present invention.
A method for batch distillation of crude maleic anhydride is provided, which is used for stabilizing steam flow in batch distillation process of crude maleic anhydride, and the process flow diagram is shown in figure 1;
pumping the crude anhydride into a standing tank V-1607 by a pump, immersing a reboiler E-1606 in the standing tank, using medium-pressure steam as a heat source, condensing the gas phase of a refining tower T-1608 by a tower top condenser E-1609, then entering a reflux tank V-1610, refluxing a part of materials in the reflux tank to T-1608, and extracting the other part of materials out of a desorption tower or a tank area. And pumping out the heavy component residual anhydride in the standing tank. The overhead condenser E-1609 uses hot water or other heat-extracting medium to extract heat. Taking the heat medium, except the condenser E-1609, the other part of the heat medium is taken as a secondary line, the two paths are converged and then enter the heater E-1807, and the heater E-1807 uses medium-pressure steam as a heat source.
The batch rectification step of the crude anhydride comprises the following steps:
a) feeding: pumping the crude anhydride into a static tank V-1607;
b) vacuumizing: the refining process of the crude anhydride is negative pressure operation, and the crude anhydride is pumped by a vacuum pump until the pressure at the top of the tower is 20-50kPaA, preferably 30-40 kPaA;
c) establishing tower internal reflux: introducing steam into an E-1606 reboiler, introducing a heat-taking medium into an E-1609 condenser for cooling, introducing steam into an E-1807 heater for heating the heat-taking medium, and establishing total reflux in a refining tower, wherein except for one part of the heat-taking medium entering the condenser, the other part of the heat-taking medium enters a heater after passing through a secondary line and being converged with the condensed heat-taking medium; reflux ratio of 1-15, preferably 5-9;
d) removing front cut fraction: : e-1606 is filled with steam, E-1609 is filled with a heat-taking medium for cooling, E-1807 is filled with steam for heating the heat-taking medium, and front cut (light boiling point substances) is removed, wherein except that one part of the heat-taking medium enters a condenser, the other part of the heat-taking medium enters a heater after being converged by a sub-line and then enters the condenser; operating pressures of from 20 to 50kPaA, preferably from 30 to 40 kPaA; reflux ratio of 1-10, preferably 5-9;
e) center fraction: e-1606 is filled with steam, E-1609 is filled with a heat-taking medium for cooling, E-1807 is filled with steam for heating the heat-taking medium, and the central fraction, namely the refined maleic anhydride, is evaporated, wherein except that one part of the heat-taking medium enters a condenser, the other part of the heat-taking medium enters a heater after being converged by a sub-line and the condensed heat-taking medium; operating pressures of from 1 to 20kPaA, preferably from 1 to 10 kPaA; a reflux ratio of 0.3 to 2, preferably 0.3 to 1;
f) breaking vacuum: introducing nitrogen into the refining tower until the pressure is-3-3 KPaG, preferably-1-1 KPaG;
g) a preparation state: the refining tower enters a preparation state and waits for the step of feeding or pumping out residual anhydride;
h) pumping out residual anhydride: after a certain batch is carried out, residual anhydride in the standing tank can be accumulated and needs to be pumped out by a pump. The number of batches is from 1 to 100, preferably from 30 to 50;
the overhead condenser E-1609 uses a heat-removing medium, which may be water, dibutyl phthalate (DBP) or other medium. E-1609 is cooled at a temperature of 55-70 deg.C, preferably 57-65 deg.C. The total flow of the heat-taking medium is kept stable by an E-1609 auxiliary line regulating valve. The medium after heat removal is heated with medium pressure steam to stabilize the temperature of the medium after heat removal at 80-90 deg.C, preferably 84-86 deg.C. Because the heat-taking medium has stable flow and temperature, the waste heat of the heat-taking medium can be recovered, and the aims of saving energy and reducing consumption are fulfilled.
As shown in the attached figure 1, the invention also provides another purpose of the invention, and the invention provides a crude maleic anhydride batch distillation device which comprises a standing tank, a refining tower connected with the standing tank, a condenser arranged at the top of the refining tower, and a reflux tank connected with the condenser, wherein the condenser is connected with a heat-taking medium inlet pipeline, the pipeline is also provided with a secondary line for adjusting the flow of the heat-taking medium, one part of the heat-taking medium enters the condenser, the other part of the heat-taking medium leaves the secondary line, and the two parts of the heat-taking medium are converged and then enter a heater; the heater uses medium pressure steam as a heat source.
Example 1
122670kg of crude anhydride was added to V-1607 to establish a total reflux ratio of 8, a prefractionation reflux ratio of 7 and a heart cut stage reflux ratio of 0.33. Hot water is used as a heat-taking medium, the total flow of the heat-taking medium is 155556kg/h, the inlet temperature of the heat-taking medium is 60 ℃, the heat-taking medium is heated by E-1807 after being converged, and the temperature is 85 ℃. The steam usage amount of each stage of E-1606 is as follows: feeding 0kg/h, vacuumizing 667kg/h, establishing column internal reflux 5500kg/h, removing front fraction 5504kg/h, center fraction 7808kg/h, breaking vacuum 0kg/h, and preparing state 0 kg/h. The steam usage amount of each stage of E-1807 is as follows: 7900kg/h of feeding, 7200kg/h of vacuumizing, 2410kg/h of tower internal reflux, 2398kg/h of pre-removing fraction, 95kg/h of center fraction, 7850kg/h of vacuum breaking and 7850kg/h of preparation state. The total steam usage amount of each stage of the whole refining tower is as follows: 7900kg/h of feed, 7867kg/h of vacuum, 7910kg/h of internal reflux of the column, 7902kg/h of pre-stripping fraction, 7903kg/h of center fraction, 7850kg/h of vacuum breaking and 7850kg/h of preparation state. The steam usage amount in the whole rectification process is stabilized between 7850 and 7950 kg/h.
Example 2
147204kg of crude anhydride was added to V-1607 to establish a total reflux ratio of 15, a prefractionation reflux ratio of 10 and a heart cut stage reflux ratio of 1. Dibutyl phthalate (DBP) is used as a heat-taking medium, the total flow of the heat-taking medium is 1298182kg/h, the inlet temperature of the heat-taking medium is 60 ℃, the heat-taking medium is converged and then heated by E-1807, and the temperature is 85 ℃. The steam usage amount of each stage of E-1606 is as follows: feeding 0kg/h, vacuumizing 800kg/h, establishing tower internal reflux 12385kg/h, pre-stripping fraction 9436kg/h, center fraction 28394kg/h, breaking vacuum 0kg/h, and preparing state 0 kg/h. The steam usage amount of each stage of E-1807 is as follows: 28730kg/h of feed, 27940kg/h of vacuum pumping, 16330kg/h of tower internal reflux, 19280kg/h of pre-stripping fraction, 320kg/h of center fraction, 28610kg/h of vacuum breaking and 28733kg/h of preparation state. The total steam usage amount of each stage of the whole refining tower is as follows: 28730kg/h of feeding, 28740kg/h of vacuumizing, 28715kg/h of establishing tower internal reflux, 28716kg/h of removing front fraction, 28714kg/h of center fraction, 28610kg/h of vacuum breaking and 28733kg/h of preparing state. The steam usage amount in the whole rectification process is stabilized between 28600 and 28750 kg/h.
Example 3
200733kg of crude anhydride was added to V-1607 to establish a total reflux ratio of 8, a prefractionation reflux ratio of 7, and a center distillate stage reflux ratio of 0.33. Dibutyl phthalate (DBP) is used as a heat-taking medium, the total flow of the heat-taking medium is 584182kg/h, the inlet temperature of the heat-taking medium is 60 ℃, the heat-taking medium is converged and then heated by E-1807, and the temperature is 85 ℃. The steam usage amount of each stage of E-1606 is as follows: feeding 0kg/h, vacuumizing 1091kg/h, establishing 9000kg/h of tower internal reflux, removing 9007kg/h of front fraction, 12777kg/h of center fraction, breaking vacuum 0kg/h and preparing state 0 kg/h. The steam usage amount of each stage of E-1807 is as follows: 12910kg/h of feeding, 11832kg/h of vacuumizing, 3911kg/h of establishing tower internal reflux, 3990kg/h of pre-stripping fraction, 162kg/h of center fraction, 12944kg/h of vacuum breaking and 12912kg/h of preparation state. The total steam usage amount of each stage of the whole refining tower is as follows: feed 12910kg/h, evacuation 12923kg/h, establishing column reflux 12911kg/h, depletions 12997kg/h, core 12939kg/h, break vacuum 12944kg/h, readiness 12912 kg/h. The steam usage amount in the whole rectification process is stabilized between 12900-13000 kg/h.
Example 4
184005kg of crude anhydride was added to V-1607 to establish a total reflux ratio of 10, a prefractionation reflux ratio of 9 and a heart cut stage reflux ratio of 0.41. Dibutyl phthalate (DBP) is used as a heat-taking medium, the total flow of the heat-taking medium is 841560kg/h, the inlet temperature of the heat-taking medium is 60 ℃, the heat-taking medium is converged and then heated by E-1807, and the temperature is 80 ℃. The steam usage amount of each stage of E-1606 is as follows: feeding 0kg/h, vacuumizing 1000kg/h, establishing tower internal reflux 10313kg/h, pre-stripping fraction 10616kg/h, center fraction 14552kg/h, breaking vacuum 0kg/h, and preparing state 0 kg/h. The steam usage amount of each stage of E-1807 is as follows: 14573kg/h of feed, 13925kg/h of vacuum pumping, 4514kg/h of tower internal reflux establishment, 4612kg/h of pre-stripping fraction, 169kg/h of center fraction, 14535kg/h of vacuum breaking and 14783kg/h of preparation state. The total steam usage amount of each stage of the whole refining tower is as follows: 14573kg/h of feed, 14925kg/h of vacuum pumping, 14826kg/h of column internal reflux establishing, 15228kg/h of pre-stripping fraction, 14721kg/h of center fraction, 14535kg/h of vacuum breaking and 14783kg/h of preparation state. The steam usage amount in the whole rectification process is stabilized between 14530-14930 kg/h.
Example 5
220806kg of crude anhydride was added to V-1607 to establish a total reflux ratio of 5, a prefractionation reflux ratio of 4 and a heart cut stage reflux ratio of 0.3. Hot water is used as a heat-taking medium, the total flow of the heat-taking medium is 254545kg/h, the inlet temperature of the heat-taking medium is 60 ℃, the heat-taking medium is heated by E-1807 after being converged, and the temperature is 83 ℃. The steam usage amount of each stage of E-1606 is as follows: feeding 0kg/h, vacuumizing 1200kg/h, establishing column internal reflux 6193kg/h, removing front fraction 5662kg/h, center fraction 12777kg/h, breaking vacuum 0kg/h, and preparing state 0 kg/h. The steam usage amount of each stage of E-1807 is as follows: 12856kg/h of feed, 11598kg/h of vacuum pumping, 6651kg/h of tower internal reflux establishment, 7249kg/h of pre-stripping fraction, 155kg/h of center fraction, 12666kg/h of vacuum breaking and 12573kg/h of preparation state. The total steam usage amount of each stage of the whole refining tower is as follows: 12856kg/h of feeding, 12798kg/h of vacuumizing, 12843kg/h of establishing tower internal reflux, 12911kg/h of pre-stripping fraction, 12932kg/h of center fraction, 12666kg/h of vacuum breaking and 12573kg/h of preparation state. The steam usage amount in the whole rectification process is stabilized between 12570-12940 kg/h.
Example 6
220806kg of crude anhydride was added to V-1607 to establish a total reflux ratio of 8, a prefractionation reflux ratio of 7 and a heart cut stage reflux ratio of 0.33. Hot water is used as a heat-taking medium, the total flow of the heat-taking medium is 280000kg/h, the inlet temperature of the heat-taking medium is 60 ℃, the heat-taking medium is heated by E-1807 after being converged, and the temperature is 83 ℃. The steam usage amount of each stage of E-1606 is as follows: feeding 0kg/h, vacuumizing 1200kg/h, establishing column internal reflux 9908kg/h, pre-stripping fraction 9908kg/h, center fraction 14055kg/h, breaking vacuum 0kg/h and preparing state 0 kg/h. The steam usage amount of each stage of E-1807 is as follows: 14200kg/h of feed, 13010kg/h of vacuum pumping, 4316kg/h of tower internal reflux, 4310kg/h of pre-stripping fraction, 170kg/h of center fraction, 14220kg/h of vacuum breaking and 14224kg/h of preparation state. The total steam usage amount of each stage of the whole refining tower is as follows: 14200kg/h of feed, 14210kg/h of evacuation, 14224kg/h of column reflux, 14218kg/h of pre-void fraction, 14225kg/h of center fraction, 14220kg/h of vacuum break, and 14224kg/h of readiness. The steam usage amount in the whole rectification process is stabilized between 14200-14300 kg/h.
Comparative example
The difference from example 6 is that the medium pressure steam heating of E-1807 is not used, and the heat medium taking secondary line of E-1609 is not adjusted. 122670kg of crude anhydride was added to V-1607 to establish a total reflux ratio of 8, a prefractionation reflux ratio of 7 and a heart cut stage reflux ratio of 0.33. Hot water is used as a heat-taking medium, the inlet temperature of the heat-taking medium is 60 ℃, the temperature is 83 ℃ after the heat-taking medium is converged and heated by E-1807. The steam usage amount of each stage of E-1606 is as follows: feeding 0kg/h, vacuumizing 1200kg/h, establishing column internal reflux 9900kg/h, pre-stripping fraction 9918kg/h, center fraction 14055kg/h, breaking vacuum 0kg/h and preparing state 0 kg/h. The steam usage amount of the whole refining tower is the steam usage amount of each stage of E-1606. The flow of the heat-conducting medium in each stage is as follows: feeding 0kg/h, vacuumizing 24261kg/h, establishing column internal reflux 200314kg/h, pre-stripping fraction 200314kg/h, center fraction 284155kg/h, breaking vacuum 0kg/h and preparing state 0 kg/h. The steam consumption in the whole rectification process is stabilized between 0 and 14055kg/h and fluctuates greatly.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A process method for batch rectification of crude maleic anhydride is characterized by comprising the following steps:
a) feeding: pumping the crude anhydride into a standing tank;
b) vacuumizing: the refining process of the crude anhydride is negative pressure operation, and a vacuum pump is used for vacuumizing;
c) establishing tower internal reflux: introducing steam into a reboiler, introducing steam into a condenser for cooling by using a heat-taking medium, introducing steam into a heater for heating the heat-taking medium, and establishing total reflux in a refining tower, wherein one part of the heat-taking medium enters the condenser, and the other part of the heat-taking medium enters the heater after being converged by a secondary line;
d) removing front cut fraction: introducing steam into the reboiler, introducing a heat medium into the condenser for cooling, introducing steam into the heater for heating the heat medium to remove front distillate, wherein one part of the heat medium enters the condenser, and the other part of the heat medium enters the heater after passing through a secondary line and being converged with the condensed heat medium;
e) center fraction: introducing steam into a reboiler, introducing a heat medium into a condenser for cooling, introducing steam into a heater for heating the heat medium, and evaporating out central fraction, namely refined maleic anhydride, wherein except for one part of the heat medium entering the condenser, the other part of the heat medium enters a secondary line and is converged with the condensed heat medium and then enters the heater;
f) breaking vacuum: introducing nitrogen into the refining tower;
g) a preparation state: the refining tower enters a preparation state and waits for the step of feeding or pumping out residual anhydride;
h) pumping out residual anhydride: after a certain batch is carried out, residual anhydride in the standing tank can be accumulated and needs to be pumped out by a pump.
2. The process for the batch distillation of crude anhydride according to claim 1, wherein: the heat-taking medium is selected from water or dibutyl phthalate.
3. The process for the batch distillation of crude anhydride according to claim 1, wherein: the temperature of the medium after heat extraction is stabilized at 80-90 ℃.
4. The process for the batch distillation of crude anhydride according to claim 1, wherein: in the vacuumizing stage, the pressure at the top of the tower is 20-50 kPaA.
5. The process for the batch distillation of crude anhydride according to claim 1, wherein: and in the stage of establishing the reflux in the tower, the reflux ratio is 1-15.
6. The process for the batch distillation of crude anhydride according to claim 1, wherein: the operation pressure of the pre-fractionation stage is 20-50 kPaA; the reflux ratio is 1-10.
7. The process for the batch distillation of crude anhydride according to claim 1, wherein: the operating pressure of the center fraction stage is 1-20 kPaA; the reflux ratio is 0.3-2.
8. The process for the batch distillation of crude anhydride according to claim 1, wherein: the accumulated batch quantity pumped out by the residual anhydride is 1-100.
9. The utility model provides a crude maleic anhydride batch distillation device, including a rest groove, with the refining column that the groove is connected that stews, locate the condenser on the refining column top of the tower, with the reflux drum that the condenser is connected which characterized in that: the condenser is connected with a heat taking medium inlet pipeline, the pipeline is also provided with a secondary line for adjusting the flow of the heat taking medium, one part of the heat taking medium enters the condenser, the other part of the heat taking medium goes through the secondary line, and the two parts of the heat taking medium are converged and then enter the heater.
10. The crude maleic anhydride batch rectification apparatus of claim 9 wherein: the heater uses medium pressure steam as a heat source.
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