CN103833537A - Absorption and refining method for high-purity methylacrolein - Google Patents
Absorption and refining method for high-purity methylacrolein Download PDFInfo
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- CN103833537A CN103833537A CN201410071066.XA CN201410071066A CN103833537A CN 103833537 A CN103833537 A CN 103833537A CN 201410071066 A CN201410071066 A CN 201410071066A CN 103833537 A CN103833537 A CN 103833537A
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- 238000010521 absorption reaction Methods 0.000 title claims abstract description 81
- 238000000034 method Methods 0.000 title claims abstract description 37
- 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 3
- 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
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 8
- 239000000470 constituent Substances 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 6
- 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
- 238000000926 separation method Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 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 13
- 239000007789 gas Substances 0.000 description 8
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 6
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 6
- 150000001721 carbon Chemical group 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 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
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-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
- 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
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- 238000000576 coating method Methods 0.000 description 1
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- 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
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- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- 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
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- 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 further be oxidized and produce methacrylic acid (MAA), all right direct and methyl alcohol and oxygen effect production methyl methacrylate (MMA), MMA is the principal monomer raw material of producing synthetic glass, has application very widely in fields such as national defence, aviation, building, home decoration and coating; Methylacrylaldehyde is still prepared the raw material of thermoplastics monomer, multiple spices and medicine intermediate.Produce Methylacrylaldehyde with the trimethyl carbinol (iso-butylene) oxidation and aspect Technology, economy and environmental protection, be a desirable operational path.
In order to meet the requirement of the further processing and utilization of MA, MA need to be absorbed and refine, but the absorption of MA is difficult with separating.Traditional Methylacrylaldehyde absorption process is to adopt water as absorption agent, because the polarity of water is stronger, to polarity, weak MA is difficult to absorb, need a large amount of water cycles, cause energy consumption to rise, and because water and MA can form azeotrope, the MA product purity obtaining is only for 90wt% left and right, comprising the acetaldehyde of suitable content, acetone and water.
Patent GP2110031 has proposed a kind of separation method that absorbs and extract for this reason, utilizes methyl alcohol as absorption agent, MA to be absorbed, and recycles water as extraction agent by methanol extraction out, recycle after methyl alcohol separates with water.The subject matter that the method exists is that the quantity of methyl alcohol of required use is very large, and the extraction agent water consumption matching is also very large, causes that facility investment is large, supplies consumption is large; And because methyl alcohol and MA, water and MA all exist azeotropism, thereby in MA product, inevitably affect next step use of MA with a small amount of methyl alcohol.Patent US3957880 proposes to adopt the alcohols of low-carbon (LC), comprise that methyl alcohol, ethanol, n-propyl alcohol or Virahol are as absorption agent, MA is absorbed from mixed gas, then water carries out extracting rectifying as extraction agent, 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 reported that a kind of washing, methanol dehydration, MA absorb and and four towers associating absorption techniques of Methanol Recovery, but can not obtain the MA product that content is higher, only be suitable for oxidative esterification and produce MMA, but be further processed into the other products such as spices inapplicable for MA.4 of disclosed employings of patent CN101844973 alcohols more than carbon atom, as absorption agent, adopts the method for two step rectifying, and the MA product purity obtaining is 98wt%, but still the water that contains 1wt% left and right and other light constituent impurity of 1wt%.
Patent US4618709 discloses the aqueous solution that a kind of utilization contains MAA and has absorbed as absorption agent the method for MA, although the method has good assimilated efficiency, the MA reclaiming contains the by products such as water, acetaldehyde and acetone, can affect next step use of MA product.Research shows, in the method, assimilated efficiency improves along with the increase of MAA concentration, increases, thereby limited the application of the method but the side effect that the increase of MAA concentration brings is polymerization tendency.
Patent CN101020625 also discloses and has adopted ionic liquid to absorb the method for MA as absorption agent, although described assimilated efficiency is higher, but being not easy to separate with ionic liquid, the high boiling substance producing in absorption process 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 to use the occasion of high-purity methyl propenal, for example, apply Methylacrylaldehyde and produce isobutyric aldehyde etc. as monomer, the hydrogenation of thermoplastic polymer, and 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, under in absorption tower, the Methylacrylaldehyde in quench tower overhead gas being absorbed;
(2) by the process of the mixed solution containing the Methylacrylaldehyde water-and-oil separator after absorbing, occur that, after layering, upper oil phase enters lightness-removing column, 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) material that enters weight-removing column is through rectifying separation, and a tower top material part refluxes, and 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 the alkane that a kind of use contains 6-8 carbon atom and absorb MA as absorption agent, and obtain content by two step rectifying and be greater than the Methylacrylaldehyde product that 99.5wt%, water-content are less than 0.1wt%.The method has been utilized the low-pole of 6-8 carbon atom and the feature little with water mutual solubility, use it to have higher assimilated efficiency as absorption agent, water-content in absorption liquid is only 0.5wt% left and right, has greatly alleviated the burden of dewatering in follow-up distillation operation, has saved 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 one or more in 2-methyl hexane, 3-methyl hexane, normal heptane, methylcyclohexane and ethyl cyclopentane.
In step (1), the absorption agent temperature on absorption tower is 0-30 ℃, and working pressure is 20-100KPa, and column bottom temperature is 5-35 ℃, and absorption liquid gas mass ratio is 0.5-10.
The processing condition that absorb affect assimilated efficiency.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 absorbing, but reduces absorption temperature to sacrifice energy consumption as cost.Consider assimilation effect and energy consumption, the service temperature on absorption tower is at 0-30 ℃, preferably 5-15 ℃.The working pressure on absorption tower also affects assimilated efficiency, and working pressure is high, favourable to absorbing, but the energy consumption of system compresses machine before increasing considers assimilated efficiency and energy consumption, and the working pressure on absorption tower is in 20-100kPa(gauge pressure, lower same), preferably 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 the needed energy consumption of desorb and solvent loss are also larger.The consumption of the absorption agent ratio of the mass rate of gas phase (absorption agent with) is generally 0.5-10, preferably 2-5.
In step (2), at the bottom of the tower of lightness-removing column, service temperature is 70-120 ℃, and operating reflux ratio is 1-10, atmospheric operation.
In step (3), at the bottom of the tower of weight-removing column, service temperature is 80-130 ℃, and operating reflux ratio is 0.5-5, negative-pressure operation, and tower top pressure is controlled at the absolute pressure of 60-90KPa.
The structure type of described absorption tower, lightness-removing column and weight-removing column adopts in sieve-tray tower, packing tower, bubble-plate column and valve tray column one or more.
The be absorbed mixed solution of agent and Methylacrylaldehyde of absorption tower tower reactor.Because selected absorption agent is (ring) alkane solvents of 6-8 carbon atom, therefore, the water in absorption liquid can be separated 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 acetaldehyde, acetone, propenal and the water removing in absorption liquid.Tower top discharging is light constituent, is mainly acetaldehyde, acetone and Methylacrylaldehyde, and water is removed by the separatory bag of return tank of top of the tower; At the bottom of tower, be the mixture of Methylacrylaldehyde and (ring) alkane, enter weight-removing column and take off heavily separation.
In the above-mentioned operation that takes off light and weight-removing column, adding of stopper is very necessary.
Adopt above-mentioned absorption and process for purification and suitable processing condition, the Methylacrylaldehyde product purity obtaining is greater than 99.5wt%, water-content is less than 0.1wt%.
Technical process of the present invention is simple, with low cost, and the Methylacrylaldehyde purity obtaining 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 reaction mixer that contains 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:
The reaction mixture gas 1 that contains Methylacrylaldehyde enters 2 bottoms, Methylacrylaldehyde absorption tower, enters 2 tops, absorption tower, counter-current absorption from the solvent of weight-removing column 9 tower reactors after heat exchanger cooling.Top, absorption tower waste gas 4 emptying after removing organism processing; Bottom, absorption tower absorption liquid enters water-and-oil separator 3.
The oil phase 5 on water-and-oil separator upper strata enters lightness-removing column 7 middle parts.Lightness-removing column 7 tower tops are light constituent 8, are the mixture 9 of Methylacrylaldehyde and absorption agent at the bottom of tower, enter weight-removing column 10.
A tower top material part for weight-removing column 10 refluxes, and 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 subject to 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 ℃, and column bottom temperature is 15 ℃.Absorbing liquid-gas ratio (mass ratio) is 1.0, and tower top waste gas is directly emptying after heating power burning disposal, and at the bottom of tower, absorption liquid 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 is to utilize azeotropic distillation to remove moisture, utilizes conventional distillation to remove the light constituent such as acetaldehyde and acetone.Lightness-removing column atmospheric operation, 64 ℃ of tower top temperatures, 95 ℃ of tower reactor temperature, reflux ratio 4, tower top discharging is 206kg/h, tower top material forms in sequence number in table 13.Materials at bottom of tower is sent into weight-removing column 10 by pump.
The major function of weight-removing column is to remove 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, under in absorption tower, the Methylacrylaldehyde in quench tower overhead gas being absorbed; (2) by the process of the mixed solution containing the Methylacrylaldehyde water-and-oil separator after absorbing, occur that, after layering, upper oil phase enters lightness-removing column, 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) material that enters weight-removing column is through rectifying separation, and a tower top material part refluxes, and 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 ℃, and working pressure is 20-100KPa, column bottom temperature is 5-35 ℃, 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), at the bottom of the tower of lightness-removing column, service temperature is 70-120 ℃, 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), at the bottom of the tower of weight-removing column, service temperature is 80-130 ℃, and operating reflux ratio is 0.5-5, negative-pressure operation, tower top pressure is controlled at the absolute pressure of 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 adopts 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), the absorption agent temperature on absorption tower is 5-15 ℃, and working pressure is 30-70KPa, and absorption liquid gas mass ratio is 2-5.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113845409A (en) * | 2021-10-18 | 2021-12-28 | 浙江皇马科技股份有限公司 | Absorption and refining method of high-purity methacrolein |
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| 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 |
| CN113845409A (en) * | 2021-10-18 | 2021-12-28 | 浙江皇马科技股份有限公司 | Absorption and refining method of high-purity methacrolein |
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| CN103833537B (en) | 2015-04-01 |
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