CN101367720A - Acrylic purification process and apparatus of bulkhead azeotropy rectification column - Google Patents
Acrylic purification process and apparatus of bulkhead azeotropy rectification column Download PDFInfo
- Publication number
- CN101367720A CN101367720A CNA2008101400580A CN200810140058A CN101367720A CN 101367720 A CN101367720 A CN 101367720A CN A2008101400580 A CNA2008101400580 A CN A2008101400580A CN 200810140058 A CN200810140058 A CN 200810140058A CN 101367720 A CN101367720 A CN 101367720A
- Authority
- CN
- China
- Prior art keywords
- tower
- acrylic acid
- acetic acid
- column
- iii
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention relates to a novel azeotropic distillation process method and a device thereof, in particular to a process method which use a septal azeotropic distillation column to produce acrylic acid, and a device thereof. The septal azeotropic distillation column is achieved by arranging a septal wall in the azeotropic distillation column in the vertical direction from the upper part to the bottom of the column, and the right side of the septal wall is sealed, and the azeotropic distillation column is divided into four areas. The acrylic acid solution containing the impurity of acetic acid enters into the column from the bottom of the rectification part (I); wherein, light components (water and acetic acid) and entrainer form azeotrope to be steamed out of the top of the column, and then the steam on the top of the column is condensed and treated by the phase separation; wherein, the organic phase (entrainer) reflows; the water phase (containing water and acetic acid) is exhaused out of the system; the material flow on the side rectification part (III) reflows to the feeding pipeline to be recycled; the acrylic acid product with the mass fraction of more than 99 percent can be obtained at the bottom of the public stripping part. With the invention, the dehydration of acrylic acid, the remove of acetic acid and the recycle of entrainer can be finished in the same column, thus the cost of the equipment and energy consumption are reduced.
Description
Technical field
The present invention relates to a kind of azeotropic distillation processing method and device, specifically be meant a kind of bulkhead azeotropy rectification column purify acrylic acid novel process method and device of utilizing, the present invention can realize the vinylformic acid dehydration, take off acetic acid and entrainment agent reclaims to be integrated in the same tower and carries out.
Background technology
Vinylformic acid is mainly used in to be produced comonomer butyl acrylate and the ethyl ester that water soluble paint and tackiness agent use and is used to produce super absorbent resin.Slightly (refining) vinylformic acid nearly all is used to produce acrylate (most important have butyl ester, methyl esters, ethyl ester and 2-(ethyl hexyl) ester) and industrial other derivatives of coating, papermaking, spinning, binding agent and printing ink.Glacial acrylic acid is mainly used in to be produced the super efficient water absorbent polymkeric substance (super absorbent resin SPA) and the washing composition polymkeric substance, is used to produce polyacrylic ester, on a small quantity as thickening material, dispersion agent and rheology control agent.
The acrylic acid aqueous solution (massfraction 35～60%) that industrial employing propylene or propenal vapor phase catalytic oxidation method make, mainly contain acetic acid impurity, contain by products such as a spot of formaldehyde, propenal, propionic acid and acrylic acid dimer in addition, this class material polarity is strong, contain hydrogen bond again, association very easily takes place, and therefore causes difficulty of acrylic acid purification.The separation and purification of acrylic acid aqueous solution mainly contains two kinds of technical process: solvent extration and azeotropic dehydration.
Chinese patent CN1683309A discloses a kind of azeotropic purification (methyl) acrylic acid that combines with extracting rectifying.Select for use a kind of hydrophobic, and the compound that can form azeotrope with water as solvent, comprise four towers such as extraction tower, cut light tower, topping still and treating tower in the whole process flow at least.Dense, dehydration (taking off acetic acid) is proposed in (methyl) vinylformic acid extraction organically to combine with (methyl) vinylformic acid azeotropic distillation dehydration (taking off acetic acid), purifying, (methyl) vinylformic acid extraction agent and azeotropic dehydration (taking off acetic acid) agent are united two into one, and (methyl) vinylformic acid azeotropic distillation dehydration (taking off acetic acid) part becomes the part that dense partial solvent regenerative process is put forward in extraction.This technical process is compared with conventional azeotropic distillation technical process, and the production cycle is long, the vinylformic acid purity height of production, but its energy consumption and facility investment expense are bigger.
Chinese patent CN1535948A discloses a kind of novel method for purifying acrylic acid, use single entrainer of zellon or zellon, the composite entrainer of aromatic hydrocarbon, adopting and flowing in the lightness-removing column of jet tray, azeotropic distillation removes water, the acetic acid in the acrylic acid aqueous solution.This processing method has higher dehydration rate, take off the acetic acid rate and lower vinylformic acid is taken rate out of, and return the method control tower still entrainer content of tower still by entrainer, to keep tower still service temperature within low scope, thereby reduce the polymerizing acrylic acid tendency, reduce acrylic acid loss, extend manufacture cycle.
Chinese patent CN1546453A discloses a kind of method of purifying propenoic acid, use novel organic extractant that vinylformic acid is separated from its aqueous solution, remove light component such as water and acetic acid by the azeotropic distillation method then, organic extractant comprises: toluene, vinyl acetic monomer, N-BUTYL ACETATE, isobutyl acetate, ethyl propionate, diisobutyl ketone, isophorone, methyl phenyl ether or their mixture, the composite mixture of preferred toluene and isobutyl acetate, wherein the quality of toluene and isobutyl acetate is 1:1～1:50 than scope, is preferably 1:2～1:12.This processing method has the higher acetic acid rate of taking off and lower vinylformic acid is taken rate out of, can obtain purity and be higher than 99% vinylformic acid, and acrylic acid rectification flow is shortened greatly, and having overcome oneself has the long defective of technical process in the technology.
U.S. Pat 7189872 disclose a kind of from the acrylic acid aqueous solution that propane, propylene or propenal vapor phase catalytic oxidation method make process for purifying acrylic acid.Add entrainment agent in acrylic acid aqueous solution, be sent in the dehydration tower, waste water is got rid of by cat head, obtains containing the crude acrylic acid of little acetic acid at the bottom of tower.Crude acrylic acid at first enters lower-boiling impurity and removes tower and remove wherein materials such as acetic acid, enters high-boiling-point impurity then and removes tower and remove wherein high boiling substance, thereby obtain highly purified acrylic products.In addition, aldehyde material is converted into heavy seeds in the vinylformic acid of having purified phenomenon may occur, need further to separate to purify.But this method continuous and stable production, but facility investment is too big, and energy consumption is very high.
U.S. Pat 6084127 discloses a kind of method that adopts azeotropic distillation acrylic acid from the acrylic acid aqueous solution that propylene or propenal vapor phase catalytic oxidation method obtain, the mixture of this method employing A (ethyl propenoate, methyl methacrylate etc.) and B (dimethylbenzene, heptane etc.) is as entrainment agent or use A as entrainment agent separately, the operation of employing four-column process flow, acrylic acid yield is higher, but flow process is longer, the process cost height.
Japanese Patent JP-A-10-120618 discloses a kind of process for purifying acrylic acid.This method adopts azeotropic dehydration tower and takes off the operation of acetic acid tower double tower, is sent into by the logistics of extraction at the bottom of the azeotropic dehydration Tata and takes off the acetic acid tower and further remove acetic acid, obtains acrylic products at the bottom of taking off the acetic acid Tata, and overhead stream returns feeding line and continues to remove acetic acid.In this method, in order to improve the separation efficiency of acetic acid, liquid is cooled earlier at the bottom of the azeotropic dehydration Tata, and then sends into and take off in the acetic acid tower, but does not improve the polymerization situation of azeotropic dehydration tower inner propene acid.
U.S. Pat 4021310 discloses a kind of method of the acrylic acid aqueous solution that rectification and purification is obtained by propylene or propenal vapor phase catalytic oxidation method under the condition that stopper exists, this stopper is composite component, comprises A (Resorcinol, cresols, pentanoic, phenol, Vermitin and methylenum coeruleum etc. wherein at least a), B (dimethyl dithiocarbamate ester copper, diethyldithiocarbamate copper and dibutyl two thiocarbamate ester copper wherein a kind of) and C (molecular oxygen).Use a large amount of stoppers may fully stop polymerizing acrylic acid, but infeasible economically, and can produce problems such as equipment corrosion and wastewater treatment.
In the above-mentioned patent, the flow process complexity, the investment cost that have are higher, have be corrosive, energy consumption is higher, utilizes the bulkhead azeotropy rectification column technology among the present invention effectively to address the above problem.Bulkhead azeotropy rectification column is that the azeotropic distillation process is applied in the tower of next door, is the integrated chemical production device of a kind of height.In the next door azeotropy rectification column, vinylformic acid is by the extraction of tower still, waste water and most of acetic acid are discharged system as water by phase splitter, side line rectifying section top extraction liquid returns feeding line, in a tower, finish the vinylformic acid dehydration simultaneously, take off tasks such as acetic acid and entrainment agent recovery, and can control tower still temperature about 85 ℃, slowed down polymerizing acrylic acid reaction in the tower still effectively, simultaneously, the present invention has saved a rectifying tower and a reboiler, and has avoided the back-mixing effect in the old process, and the thermodynamic(al) efficiency of this process is higher, therefore can cut down the consumption of energy effectively and facility investment, increase economic efficiency.
Summary of the invention
The purpose of this invention is to provide a kind of bulkhead azeotropy rectification column acrylic purification process and device of utilizing.The present invention with vinylformic acid dehydration, take off acetic acid and entrainment agent and reclaim to be integrated in the same tower and carry out, can directly obtain highly purified vinylformic acid, simplified general conventional azeotropic distillation flow process, reduced energy consumption and facility investment expense effectively.
The device that the present invention is adopted for its purpose of realization is bulkhead azeotropy rectification column (1), and the next door (5) that the top from tower extends to the bottom of tower promptly is set on the vertical direction in the conventional rectification tower, right side, next door (5) top seal.Because the adding in next door (5), bulkhead azeotropy rectification column (1) is divided into four zones, comprising: rectifying section (I), stripping section (II), side line rectifying section (III) and public stripping section (IV).Next door (5) is that off-centre or center are provided with, and makes the stripping section (II) and the cross-sectional area ratio of side line rectifying section (III) be 0.5:1～10:1.Bulkhead azeotropy rectification column (1) can be tray column, packing tower or both arbitrary combination.
Method of the present invention is that the acrylic acid aqueous solution that contains acetic acid impurity is entered in the tower by rectifying section (I) bottom, light constituent wherein (water, acetic acid) and entrainment agent form azeotrope and are steamed by cat head, after overhead vapours enters condenser (2) condensation, enter in the phase splitter (3), be divided into two-phase liquid in phase splitter (3), organic phase (entrainment agent) refluxes, water (moisture, acetic acid) discharge system, replenish entrainment agent by phase splitter (3) charging, this entrainment agent can be: ethers, as isopropyl ether; Aliphatic hydrocarbon is as heptane; Aromatic hydrocarbon is as dimethylbenzene; Lipid is as isobutyl ester; Ketone is as methyl n-propyl ketone; Halohydrocarbon is as zellon; The complex solvent that also comprises above different sorts entrainment agent: aromatic hydrocarbon and halohydrocarbon complex solvent, as toluene and zellon mixture; Lipid and aromatic hydrocarbon complex solvent are as isobutyl ester and xylene mixture; Lipid and aliphatic hydrocarbon complex solvent are as ethyl propenoate and heptane mixture etc.The part vapor phase stream enters side line rectifying section (III) by next door (5) bottom, remove contained vinylformic acid through its refinery distillation, obtain containing a small amount of acrylic acid mixture flow at side line rectifying section (III) top, return feeding line and recycle, obtain highly purified acrylic products in public stripping section (IV) bottom.Next door (5) bottom vapour phase flows into stripping section (II) and side line rectifying section (III) by a certain percentage respectively, and the ratio of vapour phase mass rate that enters stripping section (II) and side line rectifying section (III) is between 0.8:1～9:1.Tower top temperature is 35～50 ℃, and tower top pressure is 10～20KPa, and tower still temperature is 80～90 ℃, and the phase splitter temperature is 40～50 ℃.
Among the present invention at the bottom of the tower vinylformic acid massfraction reach more than 99%, entrainment agent is almost all recycled, and reaches that same product purity is required can the conventional azeotropic distillation flow process of loss-rate save 10%～30%, facility investment saves 20%～45%.
Description of drawings
Fig. 1 bulkhead azeotropy rectification column flow process purification vinylformic acid synoptic diagram
The conventional azeotropic distillation flow process of Fig. 2 purification vinylformic acid synoptic diagram
Wherein, I is a rectifying section, and II is a stripping section, and III is the side line rectifying section, and IV is public stripping section, and 1 is bulkhead azeotropy rectification column, and 2,4,7,11 is condenser, and 3,8 is phase splitter, and 5 is the next door, and 6,10,13 is reboiler, and 9 is lightness-removing column, and 12 for taking off the acetic acid tower
Specific embodiments
The invention will be further described below in conjunction with drawings and Examples, but the present invention is not subjected to the limitation of embodiment.
Example 1: flow process as shown in Figure 1.It is the tray column of 1200mm that bulkhead azeotropy rectification column (1) adopts tower diameter, tower height 18000mm, and the stage number in zone (I)～(IV) is respectively 14,15,15,4, and stripping section (II) is 3.17:1 with the cross-sectional area ratio of side line rectifying section (III).Bottom, next door (5) vapour phase flows into stripping section (II) and side line rectifying section (III) by a certain percentage respectively, and the ratio that enters the vapour phase mass rate of stripping section (II) and side line rectifying section (III) is 3.38:1.With dimethylbenzene is entrainment agent, and the acrylic acid aqueous solution that raw material contains acetic acid impurity is entered in the tower by the 14th block of plate in rectifying section (I) bottom (counting from top to bottom, down together), replenishes entrainment agent and is added by phase splitter (3).Tower top temperature is 38.7 ℃, and tower still temperature is 85.8 ℃, and phase splitter (3) temperature is 45.0 ℃, and tower top pressure is 14.2KPa.Each charging or extraction logistics flux and composition see Table 1.
The massfraction of table 1 example 1 each logistics flux and each component
| Extraction/charging position | Mass rate/(kg/h) | Vinylformic acid/% | Water/% | Acetic acid/% | Dimethylbenzene/% |
| The acrylic acid aqueous solution charging | 600.000 | 48.000 | 48.000 | 4.000 | 0.000 |
| Replenish the entrainment agent charging | 0.490 | 0.000 | 0.000 | 0.000 | 100.000 |
| The water extraction | 312.490 | 0.885 | 91.499 | 7.459 | 0.157 |
| The top extraction of side line rectifying section | 96.770 | 18.021 | 0.189 | 81.780 | 0.010 |
| The extraction of tower still vinylformic acid | 288.00 | 99.040 | 0.720 | 0.240 | 0.000 |
Example 2: flow process as shown in Figure 1.It is the tray column of 1200mm that bulkhead azeotropy rectification column (1) adopts tower diameter, tower height 18000mm, and stripping section (II) is 0.89:1, the stage number such as the example 1 in zone (I)～(IV) with the cross-sectional area ratio of side line rectifying section (III).Bottom, next door (5) vapour phase flows into stripping section (II) and side line rectifying section (III) by a certain percentage respectively, and the ratio that enters the vapour phase mass rate of stripping section (II) and side line rectifying section (III) is 0.97:1.With toluene and zellon complex solvent is entrainment agent, and toluene and zellon mass ratio are 3:1, and the acrylic acid aqueous solution that raw material contains acetic acid impurity is entered in the tower by the 14th block of plate in rectifying section (I) bottom, replenishes entrainment agent and is added by phase splitter (3).Tower top temperature is 38.7 ℃, and tower still temperature is 85.8 ℃, and phase splitter (3) temperature is 45.1 ℃, and tower top pressure is 13.9KPa.Each charging or extraction logistics flux and composition see Table 2.
The massfraction of table 2 example 2 each logistics flux and each component
| Extraction/charging position | Mass rate/(kg/h) | Vinylformic acid/% | Water/% | Acetic acid/% | Complex solvent/% |
| The acrylic acid aqueous solution charging | 600.000 | 48.000 | 48.000 | 4.000 | 0.000 |
| Replenish the entrainment agent charging | 0.510 | 0.000 | 0.000 | 0.000 | 100.000 |
| The water extraction | 312.510 | 0.802 | 91.558 | 7.477 | 0.163 |
| The top extraction of side line rectifying section | 107.800 | 16.031 | 0.169 | 83.770 | 0.030 |
| The extraction of tower still vinylformic acid | 288.000 | 99.130 | 0.650 | 0.220 | 0.000 |
Example 3: flow process as shown in Figure 1.It is the packing tower of 1400mm that bulkhead azeotropy rectification column (1) adopts tower diameter, tower height 14000mm, the packed height in zone (I)～(IV) is respectively 3200mm, 3500mm, 3200mm, 1200mm, and stripping section (II) is 2.45:1 with the cross-sectional area ratio of side line rectifying section (III).Bottom, next door (5) vapour phase flows into stripping section (II) and side line rectifying section (III) by a certain percentage respectively, and the ratio that enters the vapour phase mass rate of stripping section (II) and side line rectifying section (III) is 2.08:1.With the isopropyl ether is entrainment agent, and the acrylic acid aqueous solution that raw material contains acetic acid impurity is entered in the tower by rectifying section (I) bottom, replenishes entrainment agent and is added by phase splitter (3).Tower top temperature is 43.2 ℃, and tower still temperature is 86.3 ℃, and phase splitter (3) temperature is 44.6 ℃, and tower top pressure is 14.0KPa.Each charging or extraction logistics flux and composition see Table 3.
The massfraction of table 3 example 3 each logistics flux and each component
| Extraction/charging position | Mass rate/(kg/h) | Vinylformic acid/% | Water/% | Acetic acid/% | Isopropyl ether/% |
| The acrylic acid aqueous solution charging | 800.000 | 50.000 | 46.000 | 4.000 | 0.000 |
| Replenish the entrainment agent charging | 0.530 | 0.000 | 0.000 | 0.000 | 100.000 |
| The water extraction | 400.550 | 0.884 | 91.205 | 7.779 | 0.132 |
| The top extraction of side line rectifying section | 98.110 | 19.130 | 0.170 | 80.690 | 0.010 |
| The extraction of tower still vinylformic acid | 399.980 | 99.120 | 0.670 | 0.210 | 0.000 |
Example 4: flow process as shown in Figure 1.It is the tray column of 1200mm that bulkhead azeotropy rectification column (1) adopts tower diameter, tower height 18000mm, and each regional stage number is with example 1, and stripping section (II) is 2.88:1 with the cross-sectional area ratio of side line rectifying section (III).Bottom, next door (5) vapour phase flows into stripping section (II) and side line rectifying section (III) by a certain percentage respectively, and the ratio that enters the vapour phase mass rate of stripping section (II) and side line rectifying section (III) is 2.59:1.With methyl n-propyl ketone is entrainment agent, and the acrylic acid aqueous solution that raw material contains acetic acid impurity is entered in the tower by the 14th block of plate in rectifying section (I) bottom, replenishes entrainment agent and is added by phase splitter (3).Tower top temperature is 38.3 ℃, and tower still temperature is 84.6 ℃, and phase splitter (3) temperature is 45.2 ℃, and tower top pressure is 14.3KPa.Each charging or extraction logistics flux and composition see Table 4.
The massfraction of table 4 example 4 each logistics flux and each component
| Extraction/charging position | Mass rate/(kg/h) | Vinylformic acid/% | Water/% | Acetic acid/% | Methyl n-propyl ketone/% |
| The acrylic acid aqueous solution charging | 600.000 | 48.000 | 48.000 | 4.000 | 0.000 |
| Replenish the entrainment agent charging | 0.470 | 0.000 | 0.000 | 0.000 | 100.000 |
| The water extraction | 311.420 | 0.602 | 91.750 | 7.498 | 0.150 |
| The top extraction of side line rectifying section | 102.650 | 20.029 | 0.301 | 79.670 | 0.000 |
| The extraction of tower still vinylformic acid | 288.150 | 99.330 | 0.470 | 0.200 | 0.000 |
Example 5: flow process as shown in Figure 1.It is column plate and the filler mixing column of 1600mm that bulkhead azeotropy rectification column (1) adopts tower diameter, tower height 16000mm, and wherein rectifying section (I) and public stripping section (IV) adopt tray column, and stage number is respectively 14 and 4; Stripping section (II) adopts packing tower with side line rectifying section (III), and packed height is 3000mm, and stripping section (II) is 3.05:1 with the cross-sectional area ratio of side line rectifying section (III).Bottom, next door (5) vapour phase flows into stripping section (II) and side line rectifying section (III) by a certain percentage respectively, and the ratio that enters the vapour phase mass rate of stripping section (II) and side line rectifying section (III) is 3.12:1.With the heptane is entrainment agent, and the acrylic acid aqueous solution that raw material contains acetic acid impurity is entered in the tower by the 14th block of plate in rectifying section (I) bottom, replenishes entrainment agent and is added by phase splitter (3).Tower top temperature is 38.6 ℃, and tower still temperature is 85.3 ℃, and phase splitter temperature (3) degree is 46.1 ℃, and tower top pressure is 14.3KPa.Each charging or extraction logistics flux and composition see Table 5.
The massfraction of table 5 example 5 each logistics flux and each component
| Extraction/charging position | Mass rate/(kg/h) | Vinylformic acid/% | Water/% | Acetic acid/% | Heptane/% |
| The acrylic acid aqueous solution charging | 1000.00 | 48.000 | 48.000 | 4.000 | 0.000 |
| Replenish the entrainment agent charging | 0.780 | 0.000 | 0.000 | 0.000 | 100.000 |
| The water extraction | 520.800 | 0.686 | 91.677 | 7.487 | 0.150 |
| The top extraction of side line rectifying section | 132.290 | 18.010 | 0.110 | 81.880 | 0.000 |
| The extraction of tower still vinylformic acid | 479.98 | 99.260 | 0.530 | 0.210 | 0.000 |
Claims (7)
1. the tripping device of an acrylic acid aqueous solution comprises bulkhead azeotropy rectification column, condenser, reboiler, phase splitter and other utility appliance.Bulkhead azeotropy rectification column (1) inside is provided with a vertical next door (5), next door (5) extends to the bottom of tower from the top of tower, right side, next door (5) top seal, because the adding in next door (5), bulkhead azeotropy rectification column (1) is divided into four zones, comprise: rectifying section (I), stripping section (II), side line rectifying section (III) and public stripping section (IV).
2. device as claimed in claim 1 is characterized in that bulkhead azeotropy rectification column (1) can be tray column, packing tower or both arbitrary combination.
3. device as claimed in claim 1 is characterized in that next door (5) is off-centre or center setting, makes the stripping section (II) and the cross-sectional area ratio of side line rectifying section (III) be 0.5:1～10:1.
4. the separating process of an acrylic acid aqueous solution, it is characterized in that the acrylic acid aqueous solution that contains acetic acid impurity is entered in the tower by rectifying section (I) bottom, light constituent wherein (water, acetic acid) and entrainment agent form azeotrope and are steamed by cat head, after overhead vapours enters condenser (2) condensation, enter in the phase splitter (3), be divided into two-phase liquid in phase splitter (3), organic phase (entrainment agent) refluxes, water (moisture, acetic acid) discharge system replenishes entrainment agent by phase splitter (3) charging.The part vapor phase stream enters side line rectifying section (III) by next door (5) bottom, remove contained vinylformic acid through its refinery distillation, obtain containing a small amount of acrylic acid mixture flow at side line rectifying section (III) top, return feeding line and recycle, obtain massfraction in public stripping section (IV) bottom and be higher than 99% acrylic products.
5. processing method as claimed in claim 4, it is characterized in that next door (5) bottom vapour phase flows into stripping section (II) and side line rectifying section (III) by a certain percentage respectively, the ratio of vapour phase mass rate that enters stripping section (II) and side line rectifying section (III) is between 0.8:1～9:1.
6. processing method as claimed in claim 4 is characterized in that entrainment agent can be: ethers, as isopropyl ether; Aliphatic hydrocarbon is as heptane; Aromatic hydrocarbon is as dimethylbenzene; Lipid is as isobutyl ester; Ketone is as methyl n-propyl ketone; Halohydrocarbon is as zellon; The complex solvent that also comprises above different sorts entrainment agent: aromatic hydrocarbon and halohydrocarbon complex solvent, as toluene and zellon mixture; Lipid and aromatic hydrocarbon complex solvent are as isobutyl ester and xylene mixture; Lipid and aliphatic hydrocarbon complex solvent are as ethyl propenoate and heptane mixture.
7. processing method as claimed in claim 4, it is characterized in that the operational condition of bulkhead azeotropy rectification column (1) is: tower top temperature is 35～50 ℃, and tower top pressure is 10～20KPa, and tower still temperature is 80～90 ℃, and the phase splitter temperature is 40～50 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101400580A CN101367720A (en) | 2008-09-18 | 2008-09-18 | Acrylic purification process and apparatus of bulkhead azeotropy rectification column |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101400580A CN101367720A (en) | 2008-09-18 | 2008-09-18 | Acrylic purification process and apparatus of bulkhead azeotropy rectification column |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101367720A true CN101367720A (en) | 2009-02-18 |
Family
ID=40411750
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008101400580A Pending CN101367720A (en) | 2008-09-18 | 2008-09-18 | Acrylic purification process and apparatus of bulkhead azeotropy rectification column |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101367720A (en) |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102188835A (en) * | 2010-03-03 | 2011-09-21 | 中国石油化工股份有限公司 | Extractive distillation separation tower body |
| CN102355929A (en) * | 2009-03-19 | 2012-02-15 | Lg化学株式会社 | Dividing wall distillation column for producing high purity acrylic acid and fractional distillation method using the same |
| CN103012108A (en) * | 2011-09-26 | 2013-04-03 | 中国石油天然气股份有限公司 | Method for removing water in acrylic acid aqueous solution |
| CN104707354A (en) * | 2015-04-02 | 2015-06-17 | 山东开泰石化股份有限公司 | Methylbenzene separation system in acrylic acid device and method |
| US9944582B2 (en) | 2013-05-20 | 2018-04-17 | Saudi Basic Industries Corporation | Method for the purification of acetic acid and acrylic acid |
| CN108137475A (en) * | 2015-10-14 | 2018-06-08 | 陶氏环球技术有限责任公司 | For the method for purifying methacrylic acid methyl esters |
| WO2018118702A1 (en) * | 2016-12-22 | 2018-06-28 | Eastman Chemical Company | Acrylic acid purification via dividing wall columns |
| CN108473412A (en) * | 2016-01-21 | 2018-08-31 | 阿肯马法国公司 | Method for purifying (methyl) acrylate |
| CN109320431A (en) * | 2018-10-24 | 2019-02-12 | 福建师范大学福清分校 | A method of N-METHYLFORMAMIDE and diethylene glycol monomethyl ether in recycling paint stripper waste liquid |
| CN109608319A (en) * | 2018-12-23 | 2019-04-12 | 中国科学院山西煤炭化学研究所 | A kind of technique of higher ketone, water and carbon dioxide mixture separation |
| CN110028385A (en) * | 2019-04-26 | 2019-07-19 | 山东科技大学 | A kind of method and apparatus of separating isopropanol diisopropyl ether aqueous solution |
| CN110833701A (en) * | 2019-11-20 | 2020-02-25 | 榆林学院 | Device for purifying acetic acid in vinyl acetate production by ethylene method |
| CN111989142A (en) * | 2018-03-29 | 2020-11-24 | 环球油品有限责任公司 | Controlling split flow of liquid reflux in divided wall column |
| CN112221181A (en) * | 2019-07-15 | 2021-01-15 | 中国石油化工股份有限公司 | Organic solvent recovery processing device and processing method |
| US10968160B2 (en) | 2016-12-22 | 2021-04-06 | Eastman Chemical Company | Separation of propionic acid from acrylic acid via azeotropic distillation |
| CN113440883A (en) * | 2021-08-31 | 2021-09-28 | 山东蓝湾新材料有限公司 | Refining distillation tower for preparing acrylic acid by circulating propylene oxidation method |
| CN115397553A (en) * | 2020-04-16 | 2022-11-25 | 凯洛格·布朗及鲁特有限公司 | Integrated stabilizer in deisobutanizer for isomerization of hydrocarbons and product separation |
| CN115448834A (en) * | 2022-09-16 | 2022-12-09 | 卫星化学股份有限公司 | Method for refining acrylic acid aqueous solution |
-
2008
- 2008-09-18 CN CNA2008101400580A patent/CN101367720A/en active Pending
Cited By (29)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8932434B2 (en) | 2009-03-19 | 2015-01-13 | Lg Chem, Ltd. | Dividing wall distillation column for producing high purity acrylic acid and fractional distillation method using the same |
| CN102355929A (en) * | 2009-03-19 | 2012-02-15 | Lg化学株式会社 | Dividing wall distillation column for producing high purity acrylic acid and fractional distillation method using the same |
| CN102355929B (en) * | 2009-03-19 | 2014-07-30 | Lg化学株式会社 | Dividing wall distillation column for producing high purity acrylic acid and fractional distillation method using the same |
| CN104174180A (en) * | 2009-03-19 | 2014-12-03 | Lg化学株式会社 | Divided wall distillation column for producing high purity acrylic acid and fractional distillation method using the same |
| CN104174180B (en) * | 2009-03-19 | 2017-01-04 | Lg化学株式会社 | Dividing wall distillation column for producing high-purity acrylic acid and fractionation method using the same |
| US9884264B2 (en) | 2009-03-19 | 2018-02-06 | Lg Chem, Ltd. | Divided wall distillation column for producing high purity acrylic acid and fractional distillation method using the same |
| CN102188835B (en) * | 2010-03-03 | 2014-10-15 | 中国石油化工股份有限公司 | Extractive distillation separation tower body |
| CN102188835A (en) * | 2010-03-03 | 2011-09-21 | 中国石油化工股份有限公司 | Extractive distillation separation tower body |
| CN103012108A (en) * | 2011-09-26 | 2013-04-03 | 中国石油天然气股份有限公司 | Method for removing water in acrylic acid aqueous solution |
| CN103012108B (en) * | 2011-09-26 | 2016-01-20 | 中国石油天然气股份有限公司 | A kind of method removing moisture in acrylic acid aqueous solution |
| US9944582B2 (en) | 2013-05-20 | 2018-04-17 | Saudi Basic Industries Corporation | Method for the purification of acetic acid and acrylic acid |
| CN104707354A (en) * | 2015-04-02 | 2015-06-17 | 山东开泰石化股份有限公司 | Methylbenzene separation system in acrylic acid device and method |
| CN108137475A (en) * | 2015-10-14 | 2018-06-08 | 陶氏环球技术有限责任公司 | For the method for purifying methacrylic acid methyl esters |
| CN108473412A (en) * | 2016-01-21 | 2018-08-31 | 阿肯马法国公司 | Method for purifying (methyl) acrylate |
| US11214534B2 (en) | 2016-12-22 | 2022-01-04 | Eastman Chemical Company | Acrylic acid purification via dividing wall columns |
| WO2018118702A1 (en) * | 2016-12-22 | 2018-06-28 | Eastman Chemical Company | Acrylic acid purification via dividing wall columns |
| US10968160B2 (en) | 2016-12-22 | 2021-04-06 | Eastman Chemical Company | Separation of propionic acid from acrylic acid via azeotropic distillation |
| CN111989142A (en) * | 2018-03-29 | 2020-11-24 | 环球油品有限责任公司 | Controlling split flow of liquid reflux in divided wall column |
| CN111989142B (en) * | 2018-03-29 | 2022-06-21 | 环球油品有限责任公司 | Controlling split flow of liquid reflux in divided wall column |
| CN109320431A (en) * | 2018-10-24 | 2019-02-12 | 福建师范大学福清分校 | A method of N-METHYLFORMAMIDE and diethylene glycol monomethyl ether in recycling paint stripper waste liquid |
| CN109608319A (en) * | 2018-12-23 | 2019-04-12 | 中国科学院山西煤炭化学研究所 | A kind of technique of higher ketone, water and carbon dioxide mixture separation |
| CN110028385A (en) * | 2019-04-26 | 2019-07-19 | 山东科技大学 | A kind of method and apparatus of separating isopropanol diisopropyl ether aqueous solution |
| CN110028385B (en) * | 2019-04-26 | 2022-08-09 | 山东科技大学 | Method and device for separating isopropyl alcohol diisopropyl ether aqueous solution |
| CN112221181A (en) * | 2019-07-15 | 2021-01-15 | 中国石油化工股份有限公司 | Organic solvent recovery processing device and processing method |
| CN110833701A (en) * | 2019-11-20 | 2020-02-25 | 榆林学院 | Device for purifying acetic acid in vinyl acetate production by ethylene method |
| CN115397553A (en) * | 2020-04-16 | 2022-11-25 | 凯洛格·布朗及鲁特有限公司 | Integrated stabilizer in deisobutanizer for isomerization of hydrocarbons and product separation |
| CN113440883B (en) * | 2021-08-31 | 2021-12-07 | 山东蓝湾新材料有限公司 | Refining distillation tower for preparing acrylic acid by circulating propylene oxidation method |
| CN113440883A (en) * | 2021-08-31 | 2021-09-28 | 山东蓝湾新材料有限公司 | Refining distillation tower for preparing acrylic acid by circulating propylene oxidation method |
| CN115448834A (en) * | 2022-09-16 | 2022-12-09 | 卫星化学股份有限公司 | Method for refining acrylic acid aqueous solution |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101367720A (en) | Acrylic purification process and apparatus of bulkhead azeotropy rectification column | |
| CN101811965B (en) | Process for separating and recovering butyl acetate and butyl alcohol in wastewater by using azeotropic rectification | |
| JP4410935B2 (en) | Process for producing acrylic acid and acrylic ester | |
| CN101367724B (en) | Method and apparatus for synthesis of isopropyl acetate | |
| CN107032966A (en) | A kind of method of liquid-liquid extraction separation of extractive distillation methyl proxitol and water | |
| CN109232232A (en) | A kind of refining methd of acrylic acid | |
| CN111574375A (en) | Separation method and separation equipment for methyl acrylate crude product gas | |
| CN107098810B (en) | Separation and purification method for preparing electronic-grade propylene glycol monomethyl ether acetate | |
| CN101589015A (en) | Produce acrylic acid | |
| US7491841B2 (en) | Process for producing acrylic ester | |
| CN114315522B (en) | Purification method of cyclohexanol and preparation method of cyclohexanone | |
| CN101830788A (en) | Method for separating azeotropic mixture of ethyl methyl ketone and water through variable-pressure rectification | |
| CN105152855B (en) | A kind of method and device of azeotropic distillation separating methyl acetate ester and carbinol mixture | |
| CN102795961A (en) | Device and method for synthesizing sec-butyl alcohol by continuous reaction-rectification | |
| CN102766036A (en) | Method for recycling water from separation system for acetic acid and water | |
| WO2020015321A1 (en) | Method and device for separating isopropanol | |
| CN103980115A (en) | Method for recycling acetic acid sec-butyl ester from reaction product during preparation of acetic acid sec-butyl ester with high efficiency | |
| CN104119225A (en) | New technology for producing ethyl acetate through reactive distillation by taking mixed ionic liquid as catalyst | |
| CN109467497B (en) | Recovery process and device for polyvinyl alcohol alcoholysis mother liquor | |
| CN107011171A (en) | The system and method for variable-pressure rectification separating ethyl acetate and n-hexane azeotropic system | |
| CN216129524U (en) | Separation refining plant for preparing methyl acetate from industrial tail gas | |
| JP6391596B2 (en) | Separation of acrolein from process gas of oxidation by heterogeneous catalysis of propene | |
| US20210163433A1 (en) | Method and System for Producing Epoxyalkane | |
| CN103012102B (en) | Method of recovering acetic acid and water in production of aromatic carboxylic acid | |
| CN105175203A (en) | Method for preparing isobutene by MTBE (Methyl Tertiary Butyl Ether) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20090218 |