CN103833537B - Absorption and refining method for high-purity methylacrolein - Google Patents
Absorption and refining method for high-purity methylacrolein Download PDFInfo
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- CN103833537B CN103833537B CN201410071066.XA CN201410071066A CN103833537B CN 103833537 B CN103833537 B CN 103833537B CN 201410071066 A CN201410071066 A CN 201410071066A CN 103833537 B CN103833537 B CN 103833537B
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- 238000010521 absorption reaction Methods 0.000 title claims abstract description 83
- 238000000034 method Methods 0.000 title claims abstract description 38
- FUSUHKVFWTUUBE-UHFFFAOYSA-N buten-2-one Chemical compound CC(=O)C=C FUSUHKVFWTUUBE-UHFFFAOYSA-N 0.000 title abstract 8
- 238000007670 refining Methods 0.000 title abstract 3
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 150000001335 aliphatic alkanes Chemical class 0.000 claims abstract description 7
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 4
- STNJBCKSHOAVAJ-UHFFFAOYSA-N Methacrolein Chemical compound CC(=C)C=O STNJBCKSHOAVAJ-UHFFFAOYSA-N 0.000 claims description 53
- 239000003795 chemical substances by application Substances 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 15
- MLUCVPSAIODCQM-NSCUHMNNSA-N crotonaldehyde Chemical compound C\C=C\C=O MLUCVPSAIODCQM-NSCUHMNNSA-N 0.000 claims description 13
- 238000000746 purification Methods 0.000 claims description 13
- GXDHCNNESPLIKD-UHFFFAOYSA-N 2-methylhexane Chemical compound CCCCC(C)C GXDHCNNESPLIKD-UHFFFAOYSA-N 0.000 claims description 8
- VLJXXKKOSFGPHI-UHFFFAOYSA-N 3-methylhexane Chemical compound CCCC(C)CC VLJXXKKOSFGPHI-UHFFFAOYSA-N 0.000 claims description 8
- IFTRQJLVEBNKJK-UHFFFAOYSA-N Ethylcyclopentane Chemical compound CCC1CCCC1 IFTRQJLVEBNKJK-UHFFFAOYSA-N 0.000 claims description 8
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 8
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000000470 constituent Substances 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 6
- 238000010992 reflux Methods 0.000 claims description 5
- JVSWJIKNEAIKJW-UHFFFAOYSA-N 2-Methylheptane Chemical compound CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 claims description 4
- LAIUFBWHERIJIH-UHFFFAOYSA-N 3-Methylheptane Chemical compound CCCCC(C)CC LAIUFBWHERIJIH-UHFFFAOYSA-N 0.000 claims description 4
- IIEWJVIFRVWJOD-UHFFFAOYSA-N ethylcyclohexane Chemical compound CCC1CCCCC1 IIEWJVIFRVWJOD-UHFFFAOYSA-N 0.000 claims description 4
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 claims description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 238000010791 quenching Methods 0.000 claims description 2
- FLTJDUOFAQWHDF-UHFFFAOYSA-N trimethyl pentane Natural products CCCCC(C)(C)C FLTJDUOFAQWHDF-UHFFFAOYSA-N 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 21
- 238000005265 energy consumption Methods 0.000 abstract description 11
- 239000000543 intermediate Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 230000018044 dehydration Effects 0.000 abstract description 2
- 238000006297 dehydration reaction Methods 0.000 abstract description 2
- 239000012535 impurity Substances 0.000 abstract description 2
- 230000002745 absorbent Effects 0.000 abstract 2
- 239000002250 absorbent Substances 0.000 abstract 2
- 239000012847 fine chemical Substances 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 27
- 239000000047 product Substances 0.000 description 14
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 12
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 150000001721 carbon Chemical group 0.000 description 4
- 239000002608 ionic liquid Substances 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 2
- AMIMRNSIRUDHCM-UHFFFAOYSA-N Isopropylaldehyde Chemical compound CC(C)C=O AMIMRNSIRUDHCM-UHFFFAOYSA-N 0.000 description 2
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 2
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 238000007600 charging Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000006709 oxidative esterification reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 235000013599 spices Nutrition 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000003808 methanol extraction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/79—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the field of fine chemicals and chemical intermediates, and particularly discloses an absorption and refining method for high-purity methylacrolein. The invention provides a methylacrolein product which is prepared through two-step rectification by taking alkane containing six to eight carbon atoms as an absorbent for absorbing MA, and the content of the methylacrolein product is 99.5wt%, and the moisture content of the methylacrolein product is less than 0.1wt%. The method utilizes the characteristics of weak polarity of six to eight carbon atoms and the mutual solubility of water, the high-purity methylacrolein has higher absorption efficiency as an absorbent, the moisture content in absorption liquid is only about 0.5wt%, the burden of dehydration in the follow-up rectification operation can be greatly lightened, and the energy consumption can be saved. The absorption and refining method is simple in technological process, low in cost, and the methylacrolein is high in purity, low in the content of water and other impurities, and low in energy consumption, and can meet the application situation having high requirement on the quality of the methylacrolein.
Description
(1) technical field
The invention belongs to fine chemistry industry and chemical intermediate field, particularly a kind of absorption process for purification of high-purity methyl propenal.
(2) background technology
Methylacrylaldehyde (MA) is a kind of important chemical intermediate, can be oxidized further and produce methacrylic acid (MAA), can also directly and methyl alcohol and oxygen effect produce methyl methacrylate (MMA), MMA is the principal monomer raw material producing synthetic glass, has application widely in fields such as national defence, aviation, building, home decoration and coating; Methylacrylaldehyde still prepares the raw material of thermoplastics monomer, multiple spices and medicine intermediate.Produce Methylacrylaldehyde with the trimethyl carbinol (iso-butylene) oxidation is a desirable operational path in Technology, economy and environmental protection.
In order to meet the requirement of the further processing and utilization of MA, need MA is absorbed and refines, but the absorption of MA is difficult with being separated.Traditional Methylacrylaldehyde absorption process adopts water as absorption agent, because the polarity of water is stronger, the MA more weak to polarity is difficult to absorb, need a large amount of water cycles, energy consumption is caused to rise, and can azeotrope be formed due to water and MA, the MA product purity obtained is only about 90wt%, which includes the acetaldehyde of suitable content, acetone and water.
Patent GP2110031 proposes a kind of separation method absorbing and extract for this reason, namely utilizes methyl alcohol to be absorbed by MA as absorption agent, and as extraction agent by methanol extraction out, methyl alcohol is separated Posterior circle and utilizes recycling water with water.The subject matter that the method exists be needed for quantity of methyl alcohol very large, the extraction agent water consumption matched is also very large, causes that facility investment is large, supplies consumption is large; And all there is azeotropism due to methyl alcohol and MA, water and MA, next step thus inevitably affecting MA in MA product with a small amount of methyl alcohol uses.Patent US3957880 proposes the alcohols adopting low-carbon (LC), comprise methyl alcohol, ethanol, n-propyl alcohol or Virahol as absorption agent, MA is absorbed from mixed gas, then use water as extraction agent carries out extracting rectifying, but water and MA can form azeotrope to be caused containing moisture in MA product, cannot meet the service requirements of MA oxidative esterification catalyzer.Patent US5969178 report a kind of washing, methanol dehydration, MA absorb and and Methanol Recovery four towers associating absorption techniques, but the MA product that content is higher can not be obtained, only be suitable for oxidative esterification and produce MMA, but further the other products such as spices are processed into for MA and inapplicable.The disclosed alcohols of more than 4 carbon atoms that adopts of patent CN101844973 is as absorption agent, and adopt the method for two step rectifying, the MA product purity obtained is 98wt%, but still containing the water of about 1wt% and other light constituent impurity of 1wt%.
Patent US4618709 discloses a kind of method utilizing the aqueous solution containing MAA to absorb MA as absorption agent, although the method has good assimilated efficiency, the MA reclaimed contains the by products such as water, acetaldehyde and acetone, and next step uses to affect MA product.Research shows, in the method, assimilated efficiency improves along with the increase of MAA concentration, but the side effect that the increase of MAA concentration brings is the increase of polymerization tendency, thus limits the application of the method.
Patent CN101020625 also discloses and adopts ionic liquid as absorption agent to absorb the method for MA, although described assimilated efficiency is higher, but the high boiling substance produced in absorption process is not easy be separated with ionic liquid and cause ionic liquid quality to decline, and ionic liquid cost is higher, therefore the industrial application value of the method is limited.
Therefore, aforesaid method has certain limitation, especially needs the occasion using high-purity methyl propenal, and such as apply the monomer, hydrogenation production isobutyric aldehyde etc. of Methylacrylaldehyde as thermoplastic polymer, aforesaid method is all inapplicable.
(3) summary of the invention
The present invention, in order to make up the deficiencies in the prior art, provides the absorption process for purification of the high-purity methyl propenal that a kind of production energy consumption is low, product purity is high.
The present invention is achieved through the following technical solutions:
An absorption process for purification for high-purity methyl propenal, comprises the steps:
(1) adopt the alkane of one or more 6-8 carbon atom as absorption agent, in absorption tower, the Methylacrylaldehyde in quench tower overhead gas is absorbed;
(2) by after absorbing containing the mixed solution of Methylacrylaldehyde through water-and-oil separator, after there is layering, upper oil phase enters lightness-removing column, and lightness-removing column tower top part material is as backflow, and a part is as light constituent extraction, and materials at bottom of tower enters weight-removing column;
(3) enter the material of weight-removing column through rectifying separation, the backflow of a tower top material part, a part is as Methylacrylaldehyde product, and materials at bottom of tower returns to top, absorption tower and recycles as absorption agent.
The invention provides a kind of alkane containing 6-8 carbon atom that uses and absorb MA as absorption agent, and obtain by two step rectifying the Methylacrylaldehyde product that content is greater than 99.5wt%, water-content is less than 0.1wt%.This process employs the low-pole of 6-8 carbon atom and the feature little with water mutual solubility, it is used to have higher assimilated efficiency as absorption agent, water-content in absorption liquid is only about 0.5wt%, significantly reduces the burden of dewatering in follow-up distillation operation, saves energy consumption.
The classical group that the reactant gases of Methylacrylaldehyde is produced in the trimethyl carbinol or selective isobutene oxidation becomes MA15wt%-18wt%, H
2o13wt%-15wt%, N
260wt%-65wt%, O
26wt%-8wt% and carbonic acid gas, carbon monoxide and a small amount of acetaldehyde, methacrylic acid, acetone etc.
More excellent scheme of the present invention is:
In step (1), absorption agent is one or more in hexanaphthene, 2-methyl hexane, 3-methyl hexane, normal heptane, methylcyclohexane, ethyl cyclopentane, ethylcyclohexane, 2-methylheptane, 3-methylheptane, trimethylpentane and octane; Be preferably in 2-methyl hexane, 3-methyl hexane, normal heptane, methylcyclohexane and ethyl cyclopentane one or more.
In step (1), the absorption agent temperature on absorption tower is 0-30 DEG C, and working pressure is 20-100KPa, and column bottom temperature is 5-35 DEG C, and absorption liquid gas mass ratio is 0.5-10.
The process conditions assimilated efficiency absorbed.After above-mentioned absorption agent is determined, assimilated efficiency depends primarily on the consumption of temperature, pressure and absorption agent.Temperature is higher, more unfavorable to absorption, but reduces absorption temperature to sacrifice energy consumption for cost.Consider assimilation effect and energy consumption, the service temperature on absorption tower at 0-30 DEG C, preferred 5-15 DEG C.The working pressure on absorption tower also affects assimilated efficiency, and working pressure is high, favourable to absorption, but increases the energy consumption of front system compressors, considers assimilated efficiency and energy consumption, and the working pressure on absorption tower is in 20-100kPa(gauge pressure, lower same), preferred 30-70kPa.The consumption of absorption agent is also very large on assimilation effect impact, and absorption agent consumption is larger, and assimilated efficiency is higher, but energy consumption required for desorb and solvent loss also larger.The consumption of the absorption agent ratio of the mass rate of gas phase (absorption agent with) is generally 0.5-10, preferred 2-5.
In step (2), service temperature at the bottom of the tower of lightness-removing column is 70-120 DEG C, and operating reflux ratio is 1-10, atmospheric operation.
In step (3), service temperature at the bottom of the tower of weight-removing column is 80-130 DEG C, and operating reflux ratio is 0.5-5, negative-pressure operation, and tower top pressure controls the absolute pressure at 60-90KPa.
The structure type of described absorption tower, lightness-removing column and weight-removing column to adopt in sieve-tray tower, packing tower, bubble-plate column and valve tray column one or more.
Absorption tower tower reactor is absorbed the mixed solution of agent and Methylacrylaldehyde.Due to (ring) alkane solvents that selected absorption agent is 6-8 carbon atom, therefore, the water in absorption liquid separates the overwhelming majority by water-and-oil separator.The phase-splitting time between water and many carbon (ring) alkane is very short, and the general residence time is at 10-20 minute.
The oil phase of water-and-oil separator enters Methylacrylaldehyde lightness-removing column.The lightness-removing column effect of Methylacrylaldehyde is the acetaldehyde removed in absorption liquid, acetone, propenal and water.Tower top discharging is light constituent, mainly acetaldehyde, acetone and Methylacrylaldehyde, and water is removed by the separatory bag of return tank of top of the tower; Be Methylacrylaldehyde at the bottom of tower and the mixture of (ring) alkane, enter weight-removing column and carry out de-ly heavily being separated.
In the operation of above-mentioned de-light and weight-removing column, adding of stopper is very necessary.
Adopt above-mentioned absorption and process for purification and suitable processing condition, obtain Methylacrylaldehyde product purity is greater than 99.5wt%, water-content is less than 0.1wt%.
Present invention process flow process is simple, and with low cost, the Methylacrylaldehyde purity obtained is high, and the foreign matter contents such as water are low, and energy consumption is low, meets the application scenario high to Methylacrylaldehyde specification of quality.
(4) accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention is further illustrated.
Fig. 1 is absorption rectification flow schematic diagram of the present invention.
In figure, 1 containing the reaction mixer of Methylacrylaldehyde, 2 absorption towers, 3 water-and-oil separators, 4 waste gas, 5 oil phases, 6 waste water, 7 lightness-removing columns, 8 light constituents, 9 weight-removing column chargings, 10 weight-removing columns, 11 products pots, 12 heat exchangers.
(5) embodiment
Accompanying drawing is a kind of process flow diagram of the present invention, and its concrete technology process description is as follows:
Reaction mixture gas 1 containing Methylacrylaldehyde enters bottom Methylacrylaldehyde absorption tower 2, and the solvent from weight-removing column 9 tower reactor enters top, absorption tower 2 after heat exchanger cooling, counter-current absorption.Top, absorption tower waste gas 4 emptying after the process of removing organism; Bottom absorption tower, absorption liquid enters water-and-oil separator 3.
The oil phase 5 on water-and-oil separator upper strata enters in the middle part of lightness-removing column 7.Lightness-removing column 7 tower top is light constituent 8, is the mixture 9 of Methylacrylaldehyde and absorption agent, enters weight-removing column 10 at the bottom of tower.
The tower top material part backflow of weight-removing column 10, a part directly enters products pot 11 as product extraction, and materials at bottom of tower recycles as absorption agent after overcooling.
The embodiment of this invention is described below by concrete case study on implementation, but protection domain is not by the restriction of case study on implementation.
Methylacrylaldehyde mixed gas (composition is in sequence number in table 1 1) to be absorbed relies on pressure to send into Methylacrylaldehyde absorption tower with the flow of 2000kg/h, and absorption agent is heptane.Tower top temperature is 7 DEG C, and column bottom temperature is 15 DEG C.Absorbing liquid-gas ratio (mass ratio) is 1.0, and tower top waste gas is direct emptying after heating power burning disposal, and absorption liquid at the bottom of tower enters water-and-oil separator and carries out layering, and upper strata is oil phase (composition is in table 1 sequence number 2), and as the charging of lightness-removing column, flow is 1980kg/h.
The major function of lightness-removing column utilizes azeotropic distillation to remove moisture, utilizes conventional distillation to remove the light constituent such as acetaldehyde and acetone.Lightness-removing column atmospheric operation, tower top temperature 64 DEG C, bottom temperature 95 DEG C, reflux ratio 4, tower top discharging is 206kg/h, and tower top material composition is in sequence number in table 13.Materials at bottom of tower sends into weight-removing column 10 by pump.
The major function of weight-removing column removes absorption agent heptane, obtains highly purified Methylacrylaldehyde.
The composition table look-up of each material in table 1 case study on implementation
Claims (8)
1. an absorption process for purification for high-purity methyl propenal, is characterized by, and comprises the steps: that (1) adopts the alkane of one or more 6-8 carbon atom as absorption agent, is absorbed by the Methylacrylaldehyde in quench tower overhead gas in absorption tower; (2) by after absorbing containing the mixed solution of Methylacrylaldehyde through water-and-oil separator, after there is layering, upper oil phase enters lightness-removing column, and lightness-removing column tower top part material is as backflow, and a part is as light constituent extraction, and materials at bottom of tower enters weight-removing column; (3) enter the material of weight-removing column through rectifying separation, the backflow of a tower top material part, a part is as Methylacrylaldehyde product, and materials at bottom of tower returns to top, absorption tower and recycles as absorption agent.
2. the absorption process for purification of high-purity methyl propenal according to claim 1, it is characterized in that: in step (1), absorption agent is one or more in hexanaphthene, 2-methyl hexane, 3-methyl hexane, normal heptane, methylcyclohexane, ethyl cyclopentane, ethylcyclohexane, 2-methylheptane, 3-methylheptane, trimethylpentane and octane.
3. the absorption process for purification of high-purity methyl propenal according to claim 1, it is characterized in that: in step (1), the absorption agent temperature on absorption tower is 0-30 DEG C, and working pressure is 20-100KPa, column bottom temperature is 5-35 DEG C, and absorption liquid gas mass ratio is 0.5-10.
4. the absorption process for purification of high-purity methyl propenal according to claim 1, is characterized in that: in step (2), and service temperature at the bottom of the tower of lightness-removing column is 70-120 DEG C, and operating reflux ratio is 1-10, atmospheric operation.
5. the absorption process for purification of high-purity methyl propenal according to claim 1, it is characterized in that: in step (3), service temperature at the bottom of the tower of weight-removing column is 80-130 DEG C, and operating reflux ratio is 0.5-5, negative-pressure operation, tower top pressure controls the absolute pressure at 60-90KPa.
6. the absorption process for purification of high-purity methyl propenal according to claim 1, is characterized in that: the structure type of described absorption tower, lightness-removing column and weight-removing column to adopt in sieve-tray tower, packing tower, bubble-plate column and valve tray column one or more.
7. the absorption process for purification of high-purity methyl propenal according to claim 2, is characterized in that: described absorption agent is one or more in 2-methyl hexane, 3-methyl hexane, normal heptane, methylcyclohexane and ethyl cyclopentane.
8. the absorption process for purification of high-purity methyl propenal according to claim 3, is characterized in that: in step (1), and the absorption agent temperature on absorption tower is 5-15 DEG C, and working pressure is 30-70KPa, and absorption liquid gas mass ratio is 2-5.
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| CN201410071066.XA CN103833537B (en) | 2014-02-28 | 2014-02-28 | Absorption and refining method for high-purity methylacrolein |
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| CN109467610A (en) * | 2018-11-27 | 2019-03-15 | 华南理工大学 | A kind of method that acetate starch production process and row prepare high substituted degree crosslinked starch |
| CN110256395A (en) * | 2019-07-02 | 2019-09-20 | 菏泽学院 | A kind of synthetic method of 4,4- dimethyl-2-isopropyl -1,3- dioxolane |
| CN113845409B (en) * | 2021-10-18 | 2023-06-13 | 浙江皇马科技股份有限公司 | Method for absorbing and refining methacrolein |
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| CN101020625A (en) * | 2007-03-12 | 2007-08-22 | 中国科学院过程工程研究所 | Process of absorbing methyl acraldehyde with ionic liquid |
| CN101844973A (en) * | 2010-06-01 | 2010-09-29 | 上海华谊丙烯酸有限公司 | Method for absorbing and separating methacrolein |
| US8273313B2 (en) * | 2007-02-14 | 2012-09-25 | Saudi Basic Industries Corporation | System for producing methacrylic acid |
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| JP4091766B2 (en) * | 2001-12-27 | 2008-05-28 | 三菱レイヨン株式会社 | Method for producing methacrolein |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US8273313B2 (en) * | 2007-02-14 | 2012-09-25 | Saudi Basic Industries Corporation | System for producing methacrylic acid |
| CN101020625A (en) * | 2007-03-12 | 2007-08-22 | 中国科学院过程工程研究所 | Process of absorbing methyl acraldehyde with ionic liquid |
| CN101844973A (en) * | 2010-06-01 | 2010-09-29 | 上海华谊丙烯酸有限公司 | Method for absorbing and separating methacrolein |
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