CN106699560B - Separation equipment and separation method for methyl methacrylate-containing material flow - Google Patents
Separation equipment and separation method for methyl methacrylate-containing material flow Download PDFInfo
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- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 239000000463 material Substances 0.000 title claims abstract description 54
- 238000000926 separation method Methods 0.000 title claims abstract description 35
- 238000011084 recovery Methods 0.000 claims abstract description 108
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229940017219 methyl propionate Drugs 0.000 claims abstract description 60
- 238000000605 extraction Methods 0.000 claims abstract description 42
- -1 alcohol ester Chemical class 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 238000005882 aldol condensation reaction Methods 0.000 claims abstract description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 72
- PEDCQBHIVMGVHV-UHFFFAOYSA-N glycerol group Chemical group OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 18
- 239000000047 product Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000004064 recycling Methods 0.000 claims description 4
- 239000007795 chemical reaction product Substances 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 3
- 239000007788 liquid Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
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- 239000012071 phase Substances 0.000 description 13
- 239000000203 mixture Substances 0.000 description 10
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 4
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 3
- 239000004926 polymethyl methacrylate Substances 0.000 description 3
- HSJKGGMUJITCBW-UHFFFAOYSA-N 3-hydroxybutanal Chemical compound CC(O)CC=O HSJKGGMUJITCBW-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
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- 229920003023 plastic Polymers 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- MWFMGBPGAXYFAR-UHFFFAOYSA-N 2-hydroxy-2-methylpropanenitrile Chemical compound CC(C)(O)C#N MWFMGBPGAXYFAR-UHFFFAOYSA-N 0.000 description 1
- WBHAUHHMPXBZCQ-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound COC1=CC=CC(C)=C1O WBHAUHHMPXBZCQ-UHFFFAOYSA-N 0.000 description 1
- 239000004265 EU approved glazing agent Substances 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- STNJBCKSHOAVAJ-UHFFFAOYSA-N Methacrolein Chemical compound CC(=C)C=O STNJBCKSHOAVAJ-UHFFFAOYSA-N 0.000 description 1
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- 230000006315 carbonylation Effects 0.000 description 1
- 238000005810 carbonylation reaction Methods 0.000 description 1
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- 150000001875 compounds Chemical class 0.000 description 1
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
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- 230000000149 penetrating effect Effects 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/86—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/58—Separation; Purification; Stabilisation; Use of additives by liquid-liquid treatment
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of chemical separation, in particular to a separation device and a separation method for Methyl Methacrylate (MMA) -containing material flow, wherein the separation device comprises a solvent tank, an extraction tower, a methyl propionate recovery tower, an MMA recovery tower, an alcohol ester recovery tower and an extractant recovery tower, and the separation method comprises the following steps: 1) extracting MMA material flow in an extraction tower by using an extracting agent to obtain an extraction phase and a raffinate phase, 2) enabling the extraction phase to enter an alcohol ester recovery tower, recovering alcohol and ester at the tower top, enabling tower bottom liquid to enter an extracting agent recovery tower to recover the extracting agent and return to a solvent tank, and 3) enabling the raffinate phase to sequentially pass through a methyl propionate recovery tower to recover MP and an MMA recovery tower to recover MMA. Compared with the prior art, the method has simple flow, breaks a material azeotropic system by using the extracting agent, reduces the separation difficulty, has the recovery rates of MP and MMA of more than 99.9 percent and the purity of MMA of more than 99.8 percent, can be widely applied to the process for preparing MMA by using an aldol condensation method, and has good development prospect.
Description
Technical Field
The invention relates to the technical field of chemical separation, in particular to a separation device and a separation method for separating methyl methacrylate-containing material flow with high purity and high recovery rate.
Background
Methyl methacrylate is an organic compound, an important chemical raw material, and a monomer for producing transparent plastic polymethyl methacrylate (polymethyl methacrylate, PMMA). The product can be copolymerized with other vinyl monomers to obtain products with different properties, and can be used for manufacturing organic glass, coatings, lubricating oil additives, plastics, adhesives, resins, wood impregnating compounds, motor coil penetrating agents, ion exchange resins, paper glazing agents, textile printing and dyeing auxiliaries, leather treatment agents, printing and dyeing auxiliaries, insulating perfusion materials and the like.
The main methods for producing MMA include acetone cyanohydrin method, t-butanol/isobutylene direct oxidation method, ethylene carbonylation method, methyl propionate aldol condensation method, and the like. The condensation method of methyl propionate aldol is a research hotspot in recent years, and the subsequent MMA product refining process is also a research hotspot. Chinese patent publication No. CN101020636A describes a method for purifying and separating methyl methacrylate in the process of producing methyl methacrylate from isobutylene (or tert-butyl alcohol). According to the method, unreacted methacrolein is removed by adopting ordinary rectification, then chloroform aqueous solution with the mass concentration of 20-100% and the temperature of 0-60 ℃ is used for extraction, methanol, water and organic impurities are removed, and finally flash evaporation and reduced pressure rectification are carried out to purify and refine MMA. Only MMA was obtained in the above separation process, and the rest was not recovered. Chinese patent publication No. CN103833551A describes a purification and separation method for producing methyl methacrylate by the oxidation of tert-butyl alcohol/isobutylene. The method comprises the steps of extracting by normal hexane and water, recovering the normal hexane from an extract phase, removing impurity ester, and recovering MMA. While MMA was obtained and n-hexane was recovered in the above separation process, other substances were not recovered. Chinese patent publication No. 103193640A describes a reactive distillation method for producing methyl methacrylate. The synthesis of methyl methacrylate is completed in a rectifying tower, the separation of target products and raw materials is completed through azeotropic rectification during the reaction, an organic phase which does not contain methacrylic acid and is rich in methyl methacrylate is obtained at the tower top, a solution containing a large amount of methacrylic acid is obtained at the tower bottom, and a film evaporator is connected in series at the tower bottom to further concentrate heavy components at the tower bottom. In the separation process, the material source is obtained by the reaction and rectification of methacrylic acid and methanol, and the system substance to be separated has simple composition and is difficult to be applied to the separation and refining process of the reaction product prepared by the aldol condensation of methyl propionate.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a separation device and a separation method for separating methyl methacrylate-containing material flow with high recovery rates of methyl methacrylate and methyl propionate in the product flow obtained by preparing methyl methacrylate by an aldol condensation method.
The purpose of the invention can be realized by the following technical scheme:
a separation apparatus for a methyl methacrylate-containing stream, the separation apparatus comprising an extraction column, a methyl propionate recovery column, an MMA recovery column, an alcohol ester recovery column, an extractant recovery column;
the extraction tower is respectively connected with an extractant feeding pipe, an MMA material flow feeding pipe, an extract liquid output pipe and a raffinate liquid output pipe; the top of the extraction tower is provided with raffinate phase which is connected with the methyl propionate recovery tower through a raffinate output pipe, and the bottom of the extraction tower is provided with extract phase which is connected with the alcohol ester recovery tower through an extract output pipe;
the top of the alcohol ester recovery tower is connected with the methyl propionate recovery tower, the tower kettle is connected with the extractant recovery tower, and the extractant is obtained by recovering the tower kettle of the extractant recovery tower;
the tower kettle of the methyl propionate recovery tower is connected with the MMA recovery tower, and the tower top is connected with a methyl propionate output pipe for recovering methyl propionate;
the top of the MMA recovery tower is connected with an MMA output pipe for recovering MMA.
The extractant is placed in a solvent tank, and the solvent tank is connected with the extraction tower through an extractant feeding pipe;
one end of the MMA material feeding pipe is connected with the extraction tower, and the other end of the MMA material feeding pipe is connected with a material discharging port for generating the material through the methyl propionate aldol condensation reaction.
The top of the extractant recovery tower is used for obtaining methanol which is recovered as a product, the tower kettle is connected with the solvent tank through a connecting pipe, one part of extractant is sent to the solvent tank, and the other part of extractant is directly output.
A process for separating a methyl methacrylate-containing stream using the above separation apparatus, the separation process comprising the steps of:
(1) an extractant feeding pipe is positioned at the top of the extraction tower, an MMA-containing material flow feeding pipe is positioned at the bottom of the extraction tower, MMA-containing material flow is extracted by the extractant in the extraction tower, raffinate phase is obtained at the top of the extraction tower, and extract phase is obtained at the bottom of the extraction tower; the raffinate phase enters the methyl propionate recovery tower; the extraction phase enters the alcohol ester recovery tower;
(2) part of methanol and almost all methyl propionate dissolved in the solvent are obtained at the top of the alcohol ester recovery tower and are conveyed to the methyl propionate recovery tower through a pipeline for further separation; materials at the bottom of the alcohol ester recovery tower are an extracting agent and part of unrecyclable methanol, and enter the extracting agent recovery tower;
(3) residual methanol recovered from the top of the extractant recovery tower is directly output as a product, the extractant obtained from the bottom of the extractant recovery tower is partially returned to the solvent tank for recycling, and the partially directly output;
(4) recycling the top of the methyl propionate recovery tower to obtain a small amount of methanol and almost all methyl propionate, directly outputting the methanol and almost all the methyl propionate, and enabling the heavy component material flow at the bottom of the methyl propionate recovery tower to enter an MMA recovery tower for further separation and recovery of MMA;
(5) and obtaining MMA material flow at the top of the MMA recovery tower, directly outputting the MMA material flow, and obtaining heavy components at the bottom of the tower.
The MMA-containing stream described in step (1) is a methyl propionate aldol condensation reaction product comprising: methanol, methyl propionate, methyl methacrylate, propionic acid, methacrylic acid and water.
The extractant in the step (1) is one or more selected from water, glycol, glycerol, toluene or n-hexane, and preferably glycerol aqueous solution. The mass flow ratio of the using amount of the extracting agent to the MMA-containing material flow is 0.1-5: 1;
the operating pressure of the extraction tower is 0-1 MPa, and the operating temperature is 20-80 ℃.
The extracting agent is a glycerol aqueous solution, and the mass flow ratio of the using amount of the extracting agent to the MMA-containing material flow is preferably 0.5-3: 1.
The operating pressure of the alcohol ester recovery tower in the step (2) is-0.06-0.5 MPa, and the operating temperature is 50-150 ℃;
the operating pressure of the extractant recovery tower in the step (3) is-0.08-0.5 MPa, and the operating temperature is 50-150 ℃;
the operating pressure of the methyl propionate recovery tower in the step (4) is-0.05-0 MPa, and the operating temperature is 20-100 ℃;
the operation pressure of the MMA recovery tower in the step (5) is-0.098-0 MPa, and the operation temperature is 50-150 ℃.
The operating pressure of the separation equipment is-0.098-1.0 MPa, and the operating temperature is 20-150 ℃.
The invention uses the extractant to break a material azeotropic system, greatly reduces the separation difficulty, and finally, the recovery rate of methyl propionate is more than 99.8 percent, the recovery rate of MMA is more than 99.8 percent, and the purity of MMA is more than 99.5 percent.
Compared with the prior art, the beneficial effects of the invention are embodied in the following two aspects:
(1) particularly aiming at the process of generating methyl methacrylate by methyl propionate aldol condensation reaction, the method conforms to the trend of adjusting the production process of methyl methacrylate and has good market prospect in the future.
(2) The invention uses the extractant to break a material azeotropic system, greatly reduces the separation difficulty, and has the MMA recovery rate of more than 99.9 percent, the MMA purity of more than 99.8 percent, the methyl propionate recovery rate of more than 99.8 percent, and the purity and the recovery rate higher than those of other separation methods.
Drawings
FIG. 1 is a schematic connection diagram of the present invention:
wherein V101 is a solvent tank; c101 is an extraction tower; t101 is a methyl propionate recovery tower; t102 is a methyl methacrylate recovery tower; t103 is an alcohol ester recovery tower; t104 is a solvent recovery tower.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
As shown in FIG. 1, a separation apparatus for a separation containing methyl methacrylate, which comprises a solvent tank V101, an extraction column C101, a methyl propionate recovery column T101, an MMA recovery column T102, an alcohol ester recovery column T103, an extractant recovery column T104;
the extraction tower C101 is respectively connected with an extractant feeding pipe, an MMA material flow feeding pipe, an extract liquid output pipe and a raffinate output pipe, the extractant is placed in a solvent tank V101, the solvent tank V101 is connected with the extraction tower C101 through the extractant feeding pipe, one end of the MMA material flow feeding pipe is connected with the extraction tower C101, and the other end of the MMA material flow feeding pipe is connected with a material discharge port for generating a material through a methyl propionate aldol condensation reaction; the tower top of the extraction tower C101 is connected with the methyl propionate recovery tower T101 through a raffinate output pipe, and the tower kettle of the extraction tower C101 is connected with the alcohol ester recovery tower T103 through an extract output pipe;
the top of the alcohol ester recovery tower T103 is connected with a methyl propionate recovery tower T101, the bottom of the tower is connected with an extractant recovery tower T104, and the bottom of the extractant recovery tower T104 is recovered to obtain an extractant; and the extractant T104 is recovered from the tower top to obtain methanol which is recovered as a product, the tower kettle is connected with the solvent tank V101 through a connecting pipe, and part of the extractant is sent to the solvent tank V101.
The bottom of the methyl propionate recovery tower T101 is connected with an MMA recovery tower T102, and the top of the tower is connected with a methyl propionate output pipe for recovering methyl propionate;
the top of the MMA recovery column T102 is connected with an MMA output pipe, MMA is recovered, and the bottom of the column is recovered to obtain heavy components.
The method for separating the material containing the methyl methacrylate by adopting the respective devices comprises the following steps:
the raw material is a material flow containing MMA, and the composition of the material flow is as follows: 9% of methanol, 3% of water, 70% of methyl propionate, 15% of methyl methacrylate, 1.5% of propionic acid and 1.5% of methacrylic acid.
The MMA-containing material flow is input from the lower end of an extraction tower C101, the extractant glycerol aqueous solution which is conveyed from a solvent tank V101 is input from the top of the extraction tower, the mass concentration of the glycerol is 30 percent, and the mass flow ratio of the extractant to the MMA material flow is 0.1: 1.
The theoretical version number of the extraction tower C101 is 5, the operation pressure is 0.1MPa, the operation temperature is 40 ℃, the extraction raffinate phase at the top of the extraction tower C101 enters a methyl propionate recovery tower T101, and the extraction extract phase at the bottom of the extraction tower C101 enters an alcohol ester recovery tower T103.
The number of theoretical plates of the alcohol ester recovery tower T103 is 35, the feeding position is 17, the pressure at the top of the tower is atmospheric pressure, the temperature at the top of the tower is 71 ℃, and the temperature at the bottom of the tower is 105 ℃.
The number of theoretical plates of the methyl propionate recovery tower T101 is 38, the raffinate feeding position is 20, the overhead stream feeding position of the methyl propionate recovery tower T103 is 18, the overhead pressure is-0.06 MPa, methyl propionate is obtained at the top of the tower, the temperature is 60 ℃, the tower kettle stream temperature is 95 ℃, and the methyl propionate enters an MMA recovery tower T102.
The number of theoretical plates of the MMA recovery column T102 is 45, the feeding position is the 20 th block, the pressure at the top of the column is-0.08 MPa, the temperature is 61 ℃, the temperature is methyl methacrylate, and the temperature at the bottom of the column is 125 ℃.
The number of theoretical plates of the extraction agent recovery T104 is 20, the feeding position is 12 th, the pressure at the top of the tower is atmospheric pressure, methanol material flow is obtained at the top of the tower, the temperature is 64 ℃, the temperature of the bottom of the tower is 118 ℃, part of the methanol material flow is discharged, and part of the methanol material flow returns to the solvent tank V101.
The compositions of the materials at the top and bottom of each column are shown in Table 1.
TABLE 1 Tower top and Tower bottom Material composition of each Tower
As can be seen from the above table: the MMA concentration at the top of the T102 tower reaches 99.80 percent, the purity is higher, the top grade product is reached, the recovery rate of the methyl propionate is 99.97 percent, and the recovery rate of the MMA is 99.87 percent.
Example 2
The composition of the raw materials was the same as in example 1.
An MMA-containing stream was fed from the lower end of the extraction column C101, and the extractant water fed from the solvent pot V101 was fed to the top of the extraction column at a mass flow ratio of 5:1 of water to MMA stream.
The theoretical plate number of the C101 extraction tower is 6, the operation pressure is 0.1MPa, the operation temperature is 30 ℃, the raffinate phase at the top of the C101 tower enters a T101 methyl propionate recovery tower, and the extract phase at the bottom of the C101 tower enters a T103 alcohol ester recovery tower.
The theoretical plate number of the T103 alcohol ester recovery tower is 40, the feeding position is the 20 th block, the pressure at the top of the tower is atmospheric pressure, the temperature at the top of the tower is 73 ℃, and the temperature at the bottom of the tower is 102 ℃.
The number of theoretical plates of the T101 methyl propionate recovery tower is 40, the raffinate feeding position is 22, the T103 overhead stream feeding position is 23, the overhead pressure is-0.05 MPa, methyl propionate is obtained at the top of the tower, the temperature is 50 ℃, the tower kettle stream temperature is 85 ℃, and the methyl propionate enters the T102 methyl methacrylate recovery tower.
The theoretical plate number of the T102 methyl methacrylate recovery tower is 40, the feeding position is the 20 th block, the pressure at the top of the tower is-0.07 MPa, the temperature is 61 ℃, the temperature is methyl methacrylate, and the temperature at the bottom of the tower is 117 ℃.
The number of theoretical plates of the T104 extractant recovery tower is 20, the feeding position is the 8 th block, the pressure at the top of the tower is atmospheric pressure, methanol material flow is obtained at the top of the tower, the temperature is 64 ℃, the temperature of a tower kettle is 99 ℃, part of the methanol material flow is discharged, and part of the methanol material flow returns to the V101 extractant storage tank.
The composition of the top and bottom materials is shown in Table 2.
TABLE 2 Tower top and Tower bottom Material composition of each Tower
As can be seen from the above table: the MMA concentration at the top of the T102 tower reaches 99.80 percent, the purity is higher, the top grade product is reached, the recovery rate of the methyl propionate is 99.94 percent, and the recovery rate of the MMA is 100 percent.
Example 3
The composition of the raw materials was the same as in example 1.
An MMA-containing stream was fed from the lower end of the extraction column C101, and the extractant water fed from the solvent pot V101 was fed to the top of the extraction column at a mass flow ratio of water to MMA stream of 0.4: 1.
The theoretical plate number of the C101 extraction tower is 6, the operation pressure is 0.1MPa, the operation temperature is 30 ℃, the raffinate phase at the top of the C101 tower enters a T101 methyl propionate recovery tower, and the extract phase at the bottom of the C101 tower enters a T103 alcohol ester recovery tower.
The theoretical plate number of the T103 alcohol ester recovery tower is 40, the feeding position is 20, the pressure at the top of the tower is atmospheric pressure, the temperature at the top of the tower is 64 ℃, and the temperature at the bottom of the tower is 88 ℃.
The number of theoretical plates of the T101 methyl propionate recovery tower is 40, the raffinate feeding position is 22, the T103 overhead stream feeding position is 23, the overhead pressure is-0.05 MPa, methyl propionate is obtained at the top of the tower, the temperature is 50 ℃, the tower kettle stream temperature is 81 ℃, and the methyl propionate enters a T102 methyl methacrylate recovery tower.
The theoretical plate number of the T102 methyl methacrylate recovery tower is 40, the feeding position is the 20 th block, the pressure at the top of the tower is-0.07 MPa, the temperature is 64 ℃, the temperature is methyl methacrylate, and the temperature at the bottom of the tower is 117 ℃.
The number of theoretical plates of the T104 extractant recovery tower is 20, the feeding position is the 8 th block, the pressure at the top of the tower is atmospheric pressure, methanol material flow is obtained at the top of the tower, the temperature is 64 ℃, the temperature of a tower kettle is 99 ℃, part of the methanol material flow is discharged, and part of the methanol material flow returns to the V101 extractant storage tank.
The composition of the top and bottom materials is shown in Table 2.
TABLE 3 Tower top and Tower bottom Material composition of each Tower
As can be seen from the above table: the MMA concentration at the top of the T102 tower reaches 99.83 percent, the purity is higher, the top grade product is reached, the recovery rate of the methyl propionate is 99.98 percent, and the recovery rate of the MMA is 100 percent.
Claims (1)
1. A process for separating a methyl methacrylate-containing stream, the process comprising the steps of:
(1) extracting the MMA-containing material flow in an extraction tower by using an extracting agent to obtain a raffinate phase at the top of the tower and an extract phase at the bottom of the tower; the raffinate phase enters the methyl propionate recovery tower; the extraction phase enters the alcohol ester recovery tower;
(2) methanol and methyl propionate dissolved in a solvent are obtained at the top of the alcohol ester recovery tower and are conveyed to the methyl propionate recovery tower through a pipeline for further separation; materials at the bottom of the alcohol ester recovery tower are an extracting agent and part of unrecyclable methanol, and enter the extracting agent recovery tower;
(3) residual methanol recovered from the top of the extractant recovery tower is directly output as a product, the extractant obtained from the bottom of the extractant recovery tower is partially returned to the solvent tank for recycling, and the partially directly output;
(4) recycling the top of the methyl propionate recovery tower to obtain methyl propionate, and feeding heavy component material flow at the bottom of the methyl propionate recovery tower into an MMA recovery tower for further separating and recovering MMA;
(5) obtaining MMA material flow at the top of the MMA recovery tower and heavy components at the bottom of the tower;
the MMA-containing stream described in step (1) is a methyl propionate aldol condensation reaction product comprising: methanol, methyl propionate, methyl methacrylate, propionic acid, methacrylic acid, and water;
the operating pressure of the extraction tower in the step (1) is 0-1 MPa, and the operating temperature is 20-80 ℃;
the extracting agent is a glycerol aqueous solution, and the mass flow ratio of the using amount of the extracting agent to the MMA-containing material flow is 0.5-3: 1;
the operating pressure of the alcohol ester recovery tower in the step (2) is-0.06-0.5 MPa, and the operating temperature is 50-150 ℃;
the operating pressure of the extractant recovery tower in the step (3) is-0.08-0.5 MPa, and the operating temperature is 50-150 ℃;
the operating pressure of the methyl propionate recovery tower in the step (4) is-0.05-0 MPa, and the operating temperature is 20-100 ℃;
the operation pressure of the MMA recovery tower in the step (5) is-0.098-0 MPa, and the operation temperature is 50-150 ℃;
the operating pressure of the separation equipment is-0.098-1.0 MPa, and the operating temperature is 20-150 ℃.
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| CN112374989B (en) * | 2020-11-25 | 2022-05-17 | 西南化工研究设计院有限公司 | Separation method of mixture containing formaldehyde and methanol |
| CN115246773B (en) * | 2021-04-26 | 2024-05-10 | 上海浦景化工技术股份有限公司 | System for separating MMA from aldol condensation product |
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Effective date of registration: 20240709 Address after: 201512 No. 555 Huatong Road, Jinshanwei Town, Jinshan District, Shanghai Patentee after: SHANGHAI PUJING CHEMICAL NEW MATERIALS CO.,LTD. Country or region after: China Address before: Room 1401, building 1, 688 Qiushi Road, Jinshanwei Town, Jinshan District, Shanghai, May 12, 2015 Patentee before: PUJING CHEMICAL INDUSTRY Co.,Ltd. Country or region before: China Patentee before: SHANGHAI PUJING CHEMICAL NEW MATERIALS CO.,LTD. |