CN111056930B - Methyl cyclopentenolone rearrangement optimization production device and method - Google Patents
Methyl cyclopentenolone rearrangement optimization production device and method Download PDFInfo
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- CN111056930B CN111056930B CN201911270416.4A CN201911270416A CN111056930B CN 111056930 B CN111056930 B CN 111056930B CN 201911270416 A CN201911270416 A CN 201911270416A CN 111056930 B CN111056930 B CN 111056930B
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- 230000008707 rearrangement Effects 0.000 title claims abstract description 112
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- CFAKWWQIUFSQFU-UHFFFAOYSA-N 2-hydroxy-3-methylcyclopent-2-en-1-one Chemical compound CC1=C(O)C(=O)CC1 CFAKWWQIUFSQFU-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000005457 optimization Methods 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title abstract description 12
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 246
- 238000006243 chemical reaction Methods 0.000 claims abstract description 108
- 238000004821 distillation Methods 0.000 claims abstract description 98
- 238000005576 amination reaction Methods 0.000 claims abstract description 83
- 238000010992 reflux Methods 0.000 claims abstract description 36
- 239000007788 liquid Substances 0.000 claims description 119
- 238000000926 separation method Methods 0.000 claims description 84
- 239000000047 product Substances 0.000 claims description 59
- 238000007142 ring opening reaction Methods 0.000 claims description 12
- 239000012043 crude product Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- -1 methylcyclopentenol ketone Chemical class 0.000 claims 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 239000000543 intermediate Substances 0.000 description 155
- 238000005507 spraying Methods 0.000 description 6
- 238000009434 installation Methods 0.000 description 4
- 229910001069 Ti alloy Inorganic materials 0.000 description 3
- 239000000956 alloy Substances 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000005902 aminomethylation reaction Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000006462 rearrangement reaction Methods 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/51—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition
- C07C45/54—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition of compounds containing doubly bound oxygen atoms, e.g. esters
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C221/00—Preparation of compounds containing amino groups and doubly-bound oxygen atoms bound to the same carbon skeleton
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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
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C45/82—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/06—Systems containing only non-condensed rings with a five-membered ring
- C07C2601/10—Systems containing only non-condensed rings with a five-membered ring the ring being unsaturated
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Abstract
The invention discloses a device and a method for rearrangement optimization production of methyl cyclopentenolone. The device comprises a rectifying tower, a condenser, a balance tank, a vacuum pump, a vacuum buffer tank, a benzene receiving tank, a front-distillation amination intermediate receiving tank, a main-distillation rearrangement intermediate refined product receiving tank, a vacuum pressure gauge, a thermometer, a pipeline and a valve. The process comprises (1) recycling a crude rearrangement intermediate; (2) separating benzene by vacuum rectification; (3) separating the prefractionated aminated intermediate by vacuum rectification; (4) and (4) separating the refined product of the main distillation rearrangement intermediate by reduced pressure rectification. The invention adopts the rectifying tower to replace the existing distilling still, optimizes and configures various parameters of temperature, vacuum degree, reflux ratio and the like of vacuum rectification, thoroughly separates three materials with different components, realizes higher conversion rate with lower production cost, solves the problems of difficult treatment and big smell of waste water, and has good economic and environmental protection benefits.
Description
Technical Field
The invention relates to the field of food additive production, in particular to a device and a method for rearrangement optimization production of methyl cyclopentenolone.
Background
Methyl cyclopentenolone (MCP for short) is a good food flavoring agent. The production process of the methyl cyclopentenolone mainly comprises amination salification, aminomethylation, alkalization, amination refining (distillation process), rearrangement (ring opening and ring closing), rearrangement refining (distillation process), hydrolysis, decoloration refining and fine crystallization.
In the existing rearrangement working section, the amination intermediate is subjected to ring opening and ring closing to obtain a rearrangement intermediate crude product, then the rearrangement intermediate refined product is obtained through reduced pressure distillation, and a part of separated front-run amination intermediate and solvent benzene are subjected to a recycling rearrangement reaction. After ring opening and ring closing in the existing rearrangement process, partial aminated intermediates still can not be completely reacted, and although the refined rearrangement intermediate product obtained by separating the aminated intermediates by reduced pressure distillation can meet the production requirement, the following defects also exist: the solvent (benzene), the prefractionation amination intermediate and the main distillation rearrangement intermediate refined product cannot be completely separated due to the problem of component boiling points, the obtained rearrangement intermediate refined product contains 88-92% of rearrangement intermediate, 8-10% of amination intermediate and 2-3% of impurities, the 8-10% of amination intermediate cannot be separated, and the amination intermediate mixed in the rearrangement intermediate refined product is soluble in water and cannot be recovered in the hydrolysis reaction process of the next procedure, so that the waste water is difficult to treat, the smell is large, the surrounding environment is influenced, the conversion rate is low, and the production cost is high.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a device and a method for rearrangement and optimization production of methyl cyclopentenolone.
The technical scheme of the invention is as follows:
the rearrangement optimization production device for the methyl cyclopentenolone comprises a rectifying tower, a condenser, a balance tank, a vacuum pump, a vacuum buffer tank, a benzene receiving tank, a front-distillation amination intermediate receiving tank, a main-distillation rearrangement intermediate refined product receiving tank, a vacuum pressure gauge, a thermometer, a pipeline and a valve; the vacuum pressure gauge comprises a first vacuum pressure gauge, a second vacuum pressure gauge, a third vacuum pressure gauge, a fourth vacuum pressure gauge and a fifth vacuum pressure gauge; the temperature meters comprise a first temperature meter, a second temperature meter and a third temperature meter; the lines include a vapor line, a liquid line, and a vacuum line; the valve comprises a liquid control valve and a vacuum valve, wherein the liquid control valve comprises a first liquid control valve, a second liquid control valve, a third liquid control valve, a fourth liquid control valve, a fifth liquid control valve and a sixth liquid control valve; the vacuum valves comprise a first vacuum valve, a second vacuum valve, a third vacuum valve, a fourth vacuum valve and a fifth vacuum valve; the rectifying tower comprises a tower body and a reaction kettle connected with the lower part of the tower body, a jacket is arranged on the periphery of the reaction kettle and is connected with a steam pipeline, a first vacuum pressure gauge and a first thermometer are arranged on the upper part of the reaction kettle and are connected with a feeding liquid pipeline through a first liquid control valve, and a second thermometer and a third thermometer are respectively arranged on the middle part and the upper part of the tower body; the steam inlet end of the condenser is connected with the top of the tower body through a steam pipeline, and the liquid outlet end of the condenser is connected with the top of the balance tank through a liquid pipeline; the top of the balance tank is connected with a vacuum pipeline provided with a first vacuum valve, the vacuum pipeline is respectively connected with a vacuum buffer tank, a main distillation rearrangement intermediate refined product receiving tank, a front distillation amination intermediate receiving tank and a benzene receiving tank through three branches of the vacuum pipeline, and a second vacuum valve, a third vacuum valve, a fourth vacuum valve and a fifth vacuum valve are respectively arranged on the three branches; the bottom of the balance tank is connected with a liquid pipeline which is divided into a first pipeline and a second pipeline; the tail end of the first pipeline extends into an inner cavity at the upper part of the tower body and is connected with a spraying mechanism, and a second liquid control valve is arranged on the pipeline; after a third liquid control valve is arranged on the second pipeline, the second pipeline is respectively connected with a vacuum buffer tank, a main distillation rearrangement intermediate refined product receiving tank, a front distillation amination intermediate receiving tank and a benzene receiving tank through three branches, and a fourth liquid control valve, a fifth liquid control valve and a sixth liquid control valve are respectively arranged on the three branches; the vacuum buffer tank, the main distillation rearrangement intermediate refined product receiving tank, the front distillation amination intermediate receiving tank and the benzene receiving tank are respectively provided with a second vacuum pressure gauge, a third vacuum pressure gauge, a fourth vacuum pressure gauge and a fifth vacuum pressure gauge; the vacuum buffer tank is connected with a vacuum pump through a vacuum pipeline.
The above technical solution can be further optimized as follows:
the rectifying tower adopts a packed tower.
The reaction kettle is made of titanium alloy materials.
And a sight glass valve is arranged on a liquid pipeline between the condenser and the balance tank.
The rearrangement optimization production method of methyl cyclopentenolone comprises the following steps:
(1) the crude rearrangement intermediate was subjected to a stream: transferring a rearrangement intermediate crude product obtained by ring opening and ring closing of the amination intermediate into a reaction kettle connected with the lower part of the rectifying tower body;
(2) benzene was separated by rectification under reduced pressure: when the vacuum degree of the reaction kettle is more than or equal to-0.06 MPa, opening steam for heating, enabling the temperature at the top of the tower to be more than or equal to 40 ℃, and enabling effluent liquid transferred from the condenser and the balance tank to flow into a benzene receiving tank; when the temperature at the top of the tower is more than or equal to 65 ℃, the temperature of the reaction kettle is more than or equal to 135 ℃, and the vacuum degree of the reaction kettle is more than or equal to-0.084 MPa, the benzene separation is finished; maintaining the reflux ratio of the rectifying tower to be 3-4 in the benzene separation process;
(3) separating the prefractionated aminated intermediate by rectification under reduced pressure: after the benzene separation is finished, the distillate transferred from the condenser through the balancing tank flows into a front-distillation amination intermediate receiving tank; when the temperature of the top of the tower is more than or equal to 105 ℃, the temperature of the reaction kettle is more than or equal to 140 ℃ and the vacuum degree of the reaction kettle is more than or equal to-0.088 MPa, the separation of the front-run amination intermediate is finished; keeping the reflux ratio of the rectifying tower to be 4-5 in the separation process of the prefractionation amination intermediate;
(4) separating the refined product of the main distillation rearrangement intermediate by reduced pressure rectification: after the separation of the front-distillation amination intermediate is finished, closing the vacuum of the balancing tank, avoiding the reflux of the rectifying tower, and enabling all liquid transferred from the condenser and the balancing tank to flow into the main-distillation rearrangement intermediate refined product receiving tank; and finishing the separation of the refined product of the main distillation rearrangement intermediate when the temperature at the top of the tower is more than or equal to 110 ℃, the temperature of the reaction kettle is more than or equal to 145 ℃ and the vacuum degree of the reaction kettle is more than or equal to-0.092 MPa.
The above technical solution can be further optimized as follows:
and when the temperature of the reaction kettle reaches 135 ℃ and the vacuum degree of the reaction kettle reaches-0.084 MPa, the benzene separation is finished.
The reflux ratio of the rectifying tower is kept to be 3.5 in the benzene separation process.
And when the temperature of the reaction kettle reaches 140 ℃ and the vacuum degree of the reaction kettle reaches-0.088 MPa, the separation of the front-distillation amination intermediate is finished.
The reflux ratio of the rectifying tower is kept to be 4.5 in the separation process of the front-end amination intermediate.
And finishing the separation of the refined product of the main distillation rearrangement intermediate when the temperature of the reaction kettle reaches 145 ℃ and the vacuum degree of the reaction kettle reaches-0.092 MPa.
Compared with the prior art, the invention has the prominent technical effects that:
1. the existing distillation still is replaced by the rectifying tower, parameters such as temperature, vacuum degree, reflux ratio and the like of reduced pressure rectification are optimally configured, materials of three different components are separated by tower-type gas-liquid two-phase continuous countercurrent contact, benzene, a front-distillation amination intermediate and a main-distillation rearrangement intermediate refined product are thoroughly separated, the content of a target product rearrangement intermediate in the main-distillation rearrangement intermediate refined product is more than or equal to 99%, high conversion rate is realized by using low production cost, and economic benefit is remarkable.
2. The amination intermediate is thoroughly separated and recycled, the problems that the refined product of the main distillation rearrangement intermediate is difficult to treat and has large smell due to the fact that the refined product of the main distillation rearrangement intermediate is mixed into the amination intermediate are avoided, and the method is friendly to the surrounding environment and has good environmental protection benefits.
3. Reasonable structural layout, smooth process flow and simple and easy operation.
Drawings
FIG. 1 is a schematic view of the structure layout and process flow of the present invention;
in the figure: 1-tower body, 2-reaction kettle, 3-jacket, 4-steam pipeline, 5-first vacuum pressure gauge, 6-first temperature gauge, 7-first liquid control valve, 8-second temperature gauge, 9-third temperature gauge, 10-liquid pipeline, 11-condenser, 12-sight glass valve, 13-balance tank, 14-second liquid control valve, 15-third liquid control valve, 16-vacuum pipeline, 17-first vacuum valve, 18-second vacuum valve, 19-vacuum buffer tank, 20-second vacuum pressure gauge, 21-third vacuum valve, 22-third vacuum pressure gauge, 23-main distillation rearrangement intermediate refined product receiving tank, 24-fourth liquid control valve, 25-fourth vacuum pressure gauge, 26-a fourth vacuum valve, 27-a prefractionation amination intermediate receiving tank, 28-a benzene receiving tank, 29-a fifth liquid control valve, 30-a fifth vacuum pressure gauge, 31-a fifth vacuum valve, 32-a sixth liquid control valve, 33-a first pipeline, 34-a second pipeline, 35-a spraying mechanism and 36-a vacuum pump.
Detailed Description
The present invention will be described in detail below with reference to the following examples and accompanying drawings.
Example 1
See fig. 1. The rearrangement optimization production device of methyl cyclopentenolone comprises a rectifying tower, a condenser 11, a balance tank 13, a vacuum pump 36, a vacuum buffer tank 19, a benzene receiving tank 28, a front-distillation amination intermediate receiving tank 27, a main-distillation rearrangement intermediate refined product receiving tank 23, a vacuum pressure gauge, a thermometer, a pipeline and a valve. The vacuum pressure gauge includes a first vacuum pressure gauge 5, a second vacuum pressure gauge 20, a third vacuum pressure gauge 22, a fourth vacuum pressure gauge 25 and a fifth vacuum pressure gauge 30. The temperature meters comprise a first temperature meter 6, a second temperature meter 8 and a third temperature meter 9. The lines include a vapor line 4, a liquid line 10, and a vacuum line 16. The valve comprises a liquid control valve and a vacuum valve, and the liquid control valve comprises a first liquid control valve 7, a second liquid control valve 14, a third liquid control valve 15, a fourth liquid control valve 24, a fifth liquid control valve 29 and a sixth liquid control valve 32. The vacuum valves include a first vacuum valve 17, a second vacuum valve 18, a third vacuum valve 21, a fourth vacuum valve 26, and a fifth vacuum valve 31. Rectifying column includes tower body 1 and its sub-unit connection's reation kettle 2, and reation kettle 2 periphery is equipped with presss from both sides cover 3, presss from both sides cover 3 and connects steam line 4, and reation kettle 2's upper portion installation first vacuum pressure table 5 and first thermometer 6 and connect the liquid pipeline 10 of feeding through first liquid control valve 7, and second thermometer 8 and third thermometer 9 are installed respectively to the middle part and the upper portion of tower body 1. The steam inlet end of the condenser 11 is connected with the top of the tower body 1 through a steam pipeline 4, and the liquid outlet end of the condenser is connected with the top of the balancing tank 13 through a liquid pipeline 10. The top of the equalizing tank 13 is connected to a vacuum line 16 equipped with a first vacuum valve 17, and the vacuum line 16 is connected to a vacuum buffer tank 19, a main distillation rearrangement intermediate refined product receiving tank 23, a prefractionation amination intermediate receiving tank 27, and a benzene receiving tank 28 through three branches thereof, and is equipped with a second vacuum valve 18, a third vacuum valve 21, a fourth vacuum valve 26, and a fifth vacuum valve 31, respectively. The bottom of the equalization tank 13 is connected to a liquid line 10, and the liquid line 10 is divided into a first line 33 and a second line 34. The tail end of the first pipeline 33 extends into the inner cavity of the upper part of the tower body 1 and is connected with a spraying mechanism 35, and a second liquid control valve 14 is arranged on the pipeline. The second line 34 is connected to the vacuum buffer tank 19, the main distillation rearrangement intermediate refined product receiving tank 23, the prefractionation amination intermediate receiving tank 27, and the benzene receiving tank 28 through three branches of the third liquid control valve 15, and is provided with a fourth liquid control valve 24, a fifth liquid control valve 29, and a sixth liquid control valve 32. The vacuum buffer tank 19, the main distillation rearrangement intermediate refined product receiving tank 23, the front distillation amination intermediate receiving tank 27 and the benzene receiving tank 28 are respectively provided with a second vacuum pressure gauge 20, a third vacuum pressure gauge 22, a fourth vacuum pressure gauge 25 and a fifth vacuum pressure gauge 30. The vacuum buffer tank 19 is connected to a vacuum pump 36 through a vacuum line 16.
Example 2
See fig. 1. The rearrangement optimization production device of methyl cyclopentenolone comprises a rectifying tower, a condenser 11, a balance tank 13, a vacuum pump 36, a vacuum buffer tank 19, a benzene receiving tank 28, a front-distillation amination intermediate receiving tank 27, a main-distillation rearrangement intermediate refined product receiving tank 23, a vacuum pressure gauge, a thermometer, a pipeline and a valve. The vacuum pressure gauge includes a first vacuum pressure gauge 5, a second vacuum pressure gauge 20, a third vacuum pressure gauge 22, a fourth vacuum pressure gauge 25 and a fifth vacuum pressure gauge 30. The temperature meters comprise a first temperature meter 6, a second temperature meter 8 and a third temperature meter 9. The lines include a vapor line 4, a liquid line 10, and a vacuum line 16. The valve comprises a liquid control valve and a vacuum valve, and the liquid control valve comprises a first liquid control valve 7, a second liquid control valve 14, a third liquid control valve 15, a fourth liquid control valve 24, a fifth liquid control valve 29 and a sixth liquid control valve 32. The vacuum valves include a first vacuum valve 17, a second vacuum valve 18, a third vacuum valve 21, a fourth vacuum valve 26, and a fifth vacuum valve 31. Rectifying column includes tower body 1 and its sub-unit connection's reation kettle 2, and reation kettle 2 periphery is equipped with presss from both sides cover 3, presss from both sides cover 3 and connects steam line 4, and reation kettle 2's upper portion installation first vacuum pressure table 5 and first thermometer 6 and connect the liquid pipeline 10 of feeding through first liquid control valve 7, and second thermometer 8 and third thermometer 9 are installed respectively to the middle part and the upper portion of tower body 1. The steam inlet end of the condenser 11 is connected with the top of the tower body 1 through a steam pipeline 4, and the liquid outlet end of the condenser is connected with the top of the balancing tank 13 through a liquid pipeline 10. The top of the equalizing tank 13 is connected to a vacuum line 16 equipped with a first vacuum valve 17, and the vacuum line 16 is connected to a vacuum buffer tank 19, a main distillation rearrangement intermediate refined product receiving tank 23, a prefractionation amination intermediate receiving tank 27, and a benzene receiving tank 28 through three branches thereof, and is equipped with a second vacuum valve 18, a third vacuum valve 21, a fourth vacuum valve 26, and a fifth vacuum valve 31, respectively. The bottom of the equalization tank 13 is connected to a liquid line 10, and the liquid line 10 is divided into a first line 33 and a second line 34. The tail end of the first pipeline 33 extends into the inner cavity of the upper part of the tower body 1 and is connected with a spraying mechanism 35, and a second liquid control valve 14 is arranged on the pipeline. The second line 34 is connected to the vacuum buffer tank 19, the main distillation rearrangement intermediate refined product receiving tank 23, the prefractionation amination intermediate receiving tank 27, and the benzene receiving tank 28 through three branches of the third liquid control valve 15, and is provided with a fourth liquid control valve 24, a fifth liquid control valve 29, and a sixth liquid control valve 32. The vacuum buffer tank 19, the main distillation rearrangement intermediate refined product receiving tank 23, the front distillation amination intermediate receiving tank 27 and the benzene receiving tank 28 are respectively provided with a second vacuum pressure gauge 20, a third vacuum pressure gauge 22, a fourth vacuum pressure gauge 25 and a fifth vacuum pressure gauge 30. The vacuum buffer tank 19 is connected to a vacuum pump 36 through a vacuum line 16.
The rectifying tower adopts a packed tower.
Example 3
See fig. 1. The rearrangement optimization production device for methyl cyclopentenolone comprises a rectifying tower, a condenser 11, a balance tank 13, a vacuum pump 36, a vacuum buffer tank 19, a benzene receiving tank 28, a front-distillation amination intermediate receiving tank 27, a main-distillation rearrangement intermediate refined product receiving tank 23, a vacuum pressure gauge, a thermometer, pipelines and valves. The vacuum pressure gauge comprises a first vacuum pressure gauge 5, a second vacuum pressure gauge 20, a third vacuum pressure gauge 22, a fourth vacuum pressure gauge 25 and a fifth vacuum pressure gauge 30. The temperature meters comprise a first temperature meter 6, a second temperature meter 8 and a third temperature meter 9. The lines include a vapor line 4, a liquid line 10, and a vacuum line 16. The valve comprises a liquid control valve and a vacuum valve, and the liquid control valve comprises a first liquid control valve 7, a second liquid control valve 14, a third liquid control valve 15, a fourth liquid control valve 24, a fifth liquid control valve 29 and a sixth liquid control valve 32. The vacuum valves include a first vacuum valve 17, a second vacuum valve 18, a third vacuum valve 21, a fourth vacuum valve 26, and a fifth vacuum valve 31. Rectifying column includes tower body 1 and its sub-unit connection's reation kettle 2, and reation kettle 2 periphery is equipped with presss from both sides cover 3, presss from both sides cover 3 and connects steam line 4, and reation kettle 2's upper portion installation first vacuum pressure table 5 and first thermometer 6 and connect the liquid pipeline 10 of feeding through first liquid control valve 7, and second thermometer 8 and third thermometer 9 are installed respectively to the middle part and the upper portion of tower body 1. The steam inlet end of the condenser 11 is connected with the top of the tower body 1 through a steam pipeline 4, and the liquid outlet end of the condenser is connected with the top of the balancing tank 13 through a liquid pipeline 10. The top of the equalizing tank 13 is connected to a vacuum line 16 equipped with a first vacuum valve 17, and the vacuum line 16 is connected to a vacuum buffer tank 19, a main distillation rearrangement intermediate refined product receiving tank 23, a prefractionation amination intermediate receiving tank 27, and a benzene receiving tank 28 through three branches thereof, and is equipped with a second vacuum valve 18, a third vacuum valve 21, a fourth vacuum valve 26, and a fifth vacuum valve 31, respectively. The bottom of the equalization tank 13 is connected to a liquid line 10, and the liquid line 10 is divided into a first line 33 and a second line 34. The tail end of the first pipeline 33 extends into the inner cavity of the upper part of the tower body 1 and is connected with a spraying mechanism 35, and a second liquid control valve 14 is arranged on the pipeline. The second line 34 is connected to the vacuum buffer tank 19, the main distillation rearrangement intermediate refined product receiving tank 23, the prefractionation amination intermediate receiving tank 27, and the benzene receiving tank 28 through three branches of the third liquid control valve 15, and is provided with a fourth liquid control valve 24, a fifth liquid control valve 29, and a sixth liquid control valve 32. The vacuum buffer tank 19, the main distillation rearrangement intermediate refined product receiving tank 23, the front distillation amination intermediate receiving tank 27 and the benzene receiving tank 28 are respectively provided with a second vacuum pressure gauge 20, a third vacuum pressure gauge 22, a fourth vacuum pressure gauge 25 and a fifth vacuum pressure gauge 30. The vacuum buffer tank 19 is connected to a vacuum pump 36 through a vacuum line 16.
The rectifying tower adopts a packed tower. The reaction kettle is made of titanium alloy materials, so that the strength of the reaction kettle is improved, and the corrosion resistance and the heat resistance of the reaction kettle are enhanced.
Example 4
See fig. 1. The rearrangement optimization production device of methyl cyclopentenolone comprises a rectifying tower, a condenser 11, a balance tank 13, a vacuum pump 36, a vacuum buffer tank 19, a benzene receiving tank 28, a front-distillation amination intermediate receiving tank 27, a main-distillation rearrangement intermediate refined product receiving tank 23, a vacuum pressure gauge, a thermometer, a pipeline and a valve. The vacuum pressure gauge includes a first vacuum pressure gauge 5, a second vacuum pressure gauge 20, a third vacuum pressure gauge 22, a fourth vacuum pressure gauge 25 and a fifth vacuum pressure gauge 30. The temperature meters comprise a first temperature meter 6, a second temperature meter 8 and a third temperature meter 9. The lines include a vapor line 4, a liquid line 10, and a vacuum line 16. The valve comprises a liquid control valve and a vacuum valve, and the liquid control valve comprises a first liquid control valve 7, a second liquid control valve 14, a third liquid control valve 15, a fourth liquid control valve 24, a fifth liquid control valve 29 and a sixth liquid control valve 32. The vacuum valves include a first vacuum valve 17, a second vacuum valve 18, a third vacuum valve 21, a fourth vacuum valve 26, and a fifth vacuum valve 31. Rectifying column includes tower body 1 and its sub-unit connection's reation kettle 2, and reation kettle 2 periphery is equipped with presss from both sides cover 3, presss from both sides cover 3 and connects steam line 4, and reation kettle 2's upper portion installation first vacuum pressure table 5 and first thermometer 6 and connect the liquid pipeline 10 of feeding through first liquid control valve 7, and second thermometer 8 and third thermometer 9 are installed respectively to the middle part and the upper portion of tower body 1. The steam inlet end of the condenser 11 is connected with the top of the tower body 1 through a steam pipeline 4, and the liquid outlet end of the condenser is connected with the top of the balancing tank 13 through a liquid pipeline 10. The top of the equalizing tank 13 is connected to a vacuum line 16 equipped with a first vacuum valve 17, and the vacuum line 16 is connected to a vacuum buffer tank 19, a main distillation rearrangement intermediate refined product receiving tank 23, a prefractionation amination intermediate receiving tank 27, and a benzene receiving tank 28 through three branches thereof, and is equipped with a second vacuum valve 18, a third vacuum valve 21, a fourth vacuum valve 26, and a fifth vacuum valve 31, respectively. The bottom of the equalization tank 13 is connected to a liquid line 10, and the liquid line 10 is divided into a first line 33 and a second line 34. The tail end of the first pipeline 33 extends into the inner cavity of the upper part of the tower body 1 and is connected with a spraying mechanism 35, and a second liquid control valve 14 is arranged on the pipeline. The second line 34 is connected to the vacuum buffer tank 19, the main distillation rearrangement intermediate refined product receiving tank 23, the prefractionation amination intermediate receiving tank 27, and the benzene receiving tank 28 through three branches of the third liquid control valve 15, and is provided with a fourth liquid control valve 24, a fifth liquid control valve 29, and a sixth liquid control valve 32. The vacuum buffer tank 19, the main distillation rearrangement intermediate refined product receiving tank 23, the front distillation amination intermediate receiving tank 27 and the benzene receiving tank 28 are respectively provided with a second vacuum pressure gauge 20, a third vacuum pressure gauge 22, a fourth vacuum pressure gauge 25 and a fifth vacuum pressure gauge 30. The vacuum buffer tank 19 is connected to a vacuum pump 36 through a vacuum line 16.
The rectifying tower adopts a packed tower. The reaction kettle is made of titanium alloy materials, so that the strength of the reaction kettle is improved, and the corrosion resistance and the heat resistance of the reaction kettle are enhanced. A sight glass valve was installed on the liquid line between the condenser and the surge tank to observe the distillate size.
Example 5
See fig. 1. The rearrangement optimization production method of methyl cyclopentenolone comprises the following steps:
(1) the crude rearrangement intermediate was subjected to a stream: the rearrangement intermediate crude product obtained by the amination intermediate through ring opening and ring closing is transferred into a reaction kettle 2 connected with the lower part of a rectifying tower body 1;
(2) benzene was separated by rectification under reduced pressure: when the vacuum degree of the reaction kettle is more than or equal to-0.06 MPa, opening steam for heating, leading the temperature at the top of the tower to be more than or equal to 40 ℃, and leading the distillate transferred from the condenser 11 and the balancing tank 13 to flow into a benzene receiving tank 28; when the temperature of the top of the tower is more than or equal to 65 ℃, the temperature of the reaction kettle 2 is more than or equal to 135 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.084 MPa, the benzene separation is finished; maintaining the reflux ratio of the rectifying tower to be 3-4 in the benzene separation process;
(3) separating the prefractionated aminated intermediate by rectification under reduced pressure: after the benzene separation is finished, the distillate transferred from the condenser 11 through the balancing tank 13 flows into a front-distillation amination intermediate receiving tank 27; when the temperature of the top of the tower is more than or equal to 105 ℃, the temperature of the reaction kettle 2 is more than or equal to 140 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.088 MPa, the separation of the front-run amination intermediate is finished; keeping the reflux ratio of the rectifying tower between 4 and 5 in the separation process of the prefractionation amination intermediate;
(4) separating the refined product of the main distillation rearrangement intermediate by reduced pressure rectification: after the separation of the front-distillation amination intermediate is finished, the vacuum of the balancing tank 13 is closed, the rectifying tower does not reflux any more, and all the liquid transferred from the condenser 11 through the balancing tank 13 flows into the main-distillation rearrangement intermediate refined product receiving tank 23; and finishing the separation of the refined product of the main distillation rearrangement intermediate when the temperature at the top of the tower is more than or equal to 110 ℃, the temperature of the reaction kettle 2 is more than or equal to 145 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.092 MPa.
Example 6
See fig. 1. The rearrangement optimization production method of methyl cyclopentenolone comprises the following steps:
(1) the crude rearrangement intermediate was subjected to a stream: the rearrangement intermediate crude product obtained by the amination intermediate through ring opening and ring closing is transferred into a reaction kettle 2 connected with the lower part of a rectifying tower body 1;
(2) benzene was separated by rectification under reduced pressure: when the vacuum degree of the reaction kettle is more than or equal to-0.06 MPa, opening steam for heating, leading the temperature at the top of the tower to be more than or equal to 40 ℃, and leading the distillate transferred from the condenser 11 and the balancing tank 13 to flow into a benzene receiving tank 28; when the temperature of the top of the tower is more than or equal to 65 ℃, the temperature of the reaction kettle 2 is more than or equal to 135 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.084 MPa, the benzene separation is finished; maintaining the reflux ratio of the rectifying tower to be 3-4 in the benzene separation process;
(3) separating the prefractionated aminated intermediate by rectification under reduced pressure: after the benzene separation is finished, the distillate transferred from the condenser 11 through the balancing tank 13 flows into a front-distillation amination intermediate receiving tank 27; when the temperature of the top of the tower is more than or equal to 105 ℃, the temperature of the reaction kettle 2 is more than or equal to 140 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.088 MPa, the separation of the front-run amination intermediate is finished; keeping the reflux ratio of the rectifying tower to be 4-5 in the separation process of the prefractionation amination intermediate;
(4) separating the refined product of the main distillation rearrangement intermediate by reduced pressure rectification: after the separation of the front-distillation amination intermediate is finished, the vacuum of the balancing tank 13 is closed, the rectifying tower does not reflux any more, and all the liquid transferred from the condenser 11 through the balancing tank 13 flows into the main-distillation rearrangement intermediate refined product receiving tank 23; and finishing the separation of the refined product of the main distillation rearrangement intermediate when the temperature at the top of the tower is more than or equal to 110 ℃, the temperature of the reaction kettle 2 is more than or equal to 145 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.092 MPa.
The step (2) can be optimized as follows: and when the temperature of the reaction kettle 2 reaches 135 ℃ and the vacuum degree of the reaction kettle 2 reaches-0.084 MPa, the benzene separation is finished.
Example 7
See fig. 1. The rearrangement optimization production method of methyl cyclopentenolone comprises the following steps:
(1) the crude rearrangement intermediate was subjected to a stream: the rearrangement intermediate crude product obtained by the amination intermediate through ring opening and ring closing is transferred into a reaction kettle 2 connected with the lower part of a rectifying tower body 1;
(2) benzene was separated by rectification under reduced pressure: when the vacuum degree of the reaction kettle is more than or equal to-0.06 MPa, opening steam for heating, leading the temperature at the top of the tower to be more than or equal to 40 ℃, and leading the distillate transferred from the condenser 11 and the balancing tank 13 to flow into a benzene receiving tank 28; when the temperature of the top of the tower is more than or equal to 65 ℃, the temperature of the reaction kettle 2 is more than or equal to 135 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.084 MPa, the benzene separation is finished; maintaining the reflux ratio of the rectifying tower to be 3-4 in the benzene separation process;
(3) separating the prefractionated aminated intermediate by rectification under reduced pressure: after the benzene separation is finished, the distillate transferred from the condenser 11 through the balancing tank 13 flows into a front-distillation amination intermediate receiving tank 27; when the temperature of the top of the tower is more than or equal to 105 ℃, the temperature of the reaction kettle 2 is more than or equal to 140 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.088 MPa, the separation of the front-run amination intermediate is finished; keeping the reflux ratio of the rectifying tower to be 4-5 in the separation process of the prefractionation amination intermediate;
(4) separating the refined product of the main distillation rearrangement intermediate by reduced pressure rectification: after the separation of the front-distillation amination intermediate is finished, the vacuum of the balancing tank 13 is closed, the rectifying tower does not reflux any more, and all the liquid transferred from the condenser 11 through the balancing tank 13 flows into the main-distillation rearrangement intermediate refined product receiving tank 23; and finishing the separation of the refined product of the main distillation rearrangement intermediate when the temperature at the top of the tower is more than or equal to 110 ℃, the temperature of the reaction kettle 2 is more than or equal to 145 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.092 MPa.
The step (2) can be optimized as follows: when the temperature of the reaction kettle 2 reaches 135 ℃ and the vacuum degree of the reaction kettle 2 reaches-0.084 MPa, the benzene separation is finished; the reflux ratio of the rectifying tower is kept to be 3.5 in the benzene separation process.
Example 8
See fig. 1. The rearrangement optimization production method of methyl cyclopentenolone comprises the following steps:
(1) the crude rearrangement intermediate was subjected to a stream: the rearrangement intermediate crude product obtained by the amination intermediate through ring opening and ring closing is transferred into a reaction kettle 2 connected with the lower part of a rectifying tower body 1;
(2) benzene was separated by rectification under reduced pressure: when the vacuum degree of the reaction kettle is more than or equal to-0.06 MPa, opening steam for heating, leading the temperature at the top of the tower to be more than or equal to 40 ℃, and leading the distillate transferred from the condenser 11 and the balancing tank 13 to flow into a benzene receiving tank 28; when the temperature of the top of the tower is more than or equal to 65 ℃, the temperature of the reaction kettle 2 is more than or equal to 135 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.084 MPa, the benzene separation is finished; maintaining the reflux ratio of the rectifying tower to be 3-4 in the benzene separation process;
(3) separating the prefractionated aminated intermediate by rectification under reduced pressure: after the benzene separation is finished, the distillate transferred from the condenser 11 through the balancing tank 13 flows into a front-distillation amination intermediate receiving tank 27; when the temperature of the top of the tower is more than or equal to 105 ℃, the temperature of the reaction kettle 2 is more than or equal to 140 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.088 MPa, the separation of the front-run amination intermediate is finished; keeping the reflux ratio of the rectifying tower to be 4-5 in the separation process of the prefractionation amination intermediate;
(4) separating the refined product of the main distillation rearrangement intermediate by reduced pressure rectification: after the separation of the front-distillation amination intermediate is finished, the vacuum of the balancing tank 13 is closed, the rectifying tower does not reflux any more, and all the liquid transferred from the condenser 11 through the balancing tank 13 flows into the main-distillation rearrangement intermediate refined product receiving tank 23; and finishing the separation of the refined product of the main distillation rearrangement intermediate when the temperature at the top of the tower is more than or equal to 110 ℃, the temperature of the reaction kettle 2 is more than or equal to 145 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.092 MPa.
The step (2) can be optimized as follows: when the temperature of the reaction kettle 2 reaches 135 ℃ and the vacuum degree of the reaction kettle 2 reaches-0.084 MPa, the benzene separation is finished; the reflux ratio of the rectifying tower is kept to be 3.5 in the benzene separation process. The step (3) can be optimized as follows: and when the temperature of the reaction kettle 2 reaches 140 ℃ and the vacuum degree of the reaction kettle 2 reaches-0.088 MPa, the separation of the front-distillation amination intermediate is finished.
Example 9
See fig. 1. The rearrangement optimization production method of methyl cyclopentenolone comprises the following steps:
(1) the crude rearrangement intermediate was subjected to a stream: the rearrangement intermediate crude product obtained by the amination intermediate through ring opening and ring closing is transferred into a reaction kettle 2 connected with the lower part of a rectifying tower body 1;
(2) benzene was separated by rectification under reduced pressure: when the vacuum degree of the reaction kettle is more than or equal to-0.06 MPa, opening steam for heating, leading the temperature at the top of the tower to be more than or equal to 40 ℃, and leading the distillate transferred from the condenser 11 and the balancing tank 13 to flow into a benzene receiving tank 28; when the temperature of the top of the tower is more than or equal to 65 ℃, the temperature of the reaction kettle 2 is more than or equal to 135 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.084 MPa, the benzene separation is finished; maintaining the reflux ratio of the rectifying tower to be 3-4 in the benzene separation process;
(3) separating the prefractionated aminated intermediate by rectification under reduced pressure: after the benzene separation is finished, the distillate transferred from the condenser 11 through the balancing tank 13 flows into a front-distillation amination intermediate receiving tank 27; when the temperature of the top of the tower is more than or equal to 105 ℃, the temperature of the reaction kettle 2 is more than or equal to 140 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.088 MPa, the separation of the front-run amination intermediate is finished; keeping the reflux ratio of the rectifying tower to be 4-5 in the separation process of the prefractionation amination intermediate;
(4) separating the refined product of the main distillation rearrangement intermediate by reduced pressure rectification: after the separation of the front-distillation amination intermediate is finished, the vacuum of the balancing tank 13 is closed, the rectifying tower does not reflux any more, and all the liquid transferred from the condenser 11 through the balancing tank 13 flows into the main-distillation rearrangement intermediate refined product receiving tank 23; and finishing the separation of the refined product of the main distillation rearrangement intermediate when the temperature at the top of the tower is more than or equal to 110 ℃, the temperature of the reaction kettle 2 is more than or equal to 145 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.092 MPa.
The step (2) can be optimized as follows: when the temperature of the reaction kettle 2 reaches 135 ℃ and the vacuum degree of the reaction kettle 2 reaches-0.084 MPa, the benzene separation is finished; the reflux ratio of the rectifying tower is kept to be 3.5 in the benzene separation process. The step (3) can be optimized as follows: when the temperature of the reaction kettle 2 reaches 140 ℃ and the vacuum degree of the reaction kettle 2 reaches-0.088 MPa, the separation of the front-distillation amination intermediate is finished; the reflux ratio of the rectifying tower is kept to be 4.5 in the separation process of the front-end amination intermediate.
Example 10
See fig. 1. The rearrangement optimization production method of methyl cyclopentenolone comprises the following steps:
(1) the crude rearrangement intermediate was subjected to a stream: the rearrangement intermediate crude product obtained by the amination intermediate through ring opening and ring closing is transferred into a reaction kettle 2 connected with the lower part of a rectifying tower body 1;
(2) benzene was separated by rectification under reduced pressure: when the vacuum degree of the reaction kettle is more than or equal to-0.06 MPa, opening steam for heating, leading the temperature at the top of the tower to be more than or equal to 40 ℃, and leading the distillate transferred from the condenser 11 and the balancing tank 13 to flow into a benzene receiving tank 28; when the temperature of the top of the tower is more than or equal to 65 ℃, the temperature of the reaction kettle 2 is more than or equal to 135 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.084 MPa, the benzene separation is finished; maintaining the reflux ratio of the rectifying tower to be 3-4 in the benzene separation process;
(3) separating the prefractionated aminated intermediate by rectification under reduced pressure: after the benzene separation is finished, the distillate transferred from the condenser 11 through the balancing tank 13 flows into a front-distillation amination intermediate receiving tank 27; when the temperature of the top of the tower is more than or equal to 105 ℃, the temperature of the reaction kettle 2 is more than or equal to 140 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.088 MPa, the separation of the front-run amination intermediate is finished; keeping the reflux ratio of the rectifying tower to be 4-5 in the separation process of the prefractionation amination intermediate;
(4) separating the refined product of the main distillation rearrangement intermediate by reduced pressure rectification: after the separation of the front-distillation amination intermediate is finished, the vacuum of the balancing tank 13 is closed, the rectifying tower does not reflux any more, and all the liquid transferred from the condenser 11 through the balancing tank 13 flows into the main-distillation rearrangement intermediate refined product receiving tank 23; and finishing the separation of the refined product of the main distillation rearrangement intermediate when the temperature at the top of the tower is more than or equal to 110 ℃, the temperature of the reaction kettle 2 is more than or equal to 145 ℃, and the vacuum degree of the reaction kettle 2 is more than or equal to-0.092 MPa.
The step (2) can be optimized as follows: when the temperature of the reaction kettle 2 reaches 135 ℃ and the vacuum degree of the reaction kettle 2 reaches-0.084 MPa, the benzene separation is finished; the reflux ratio of the rectifying tower is kept to be 3.5 in the benzene separation process. The step (3) can be optimized as follows: when the temperature of the reaction kettle 2 reaches 140 ℃ and the vacuum degree of the reaction kettle 2 reaches-0.088 MPa, the separation of the front-distillation amination intermediate is finished; the reflux ratio of the rectifying tower is kept to be 4.5 in the separation process of the front-end amination intermediate. The step (4) can be optimized as follows: and finishing the separation of the refined product of the main distillation rearrangement intermediate when the temperature of the reaction kettle reaches 145 ℃ and the vacuum degree of the reaction kettle reaches-0.092 MPa.
The basic working principle of the invention is as follows:
after the device is installed in place, starting a vacuum pump, starting steam for heating, and ending benzene separation when the temperature of the tower top reaches 65 ℃, the distillate is obviously reduced and the distillate becomes clear; when the temperature at the top of the tower reaches 105 ℃, the distillate is obviously reduced, the separation of the amination intermediate is distilled before the end, and the content of the amination intermediate is more than or equal to 98.5 percent by sampling analysis; when the temperature at the top of the tower reaches 110 ℃, the distillation is obviously reduced, the end point is observed, the separation of the refined products of the main distillation rearrangement intermediates is finished, and the content of the rearrangement intermediates is more than or equal to 99 percent by sampling analysis. The recovered benzene is continuously returned to the rearrangement as a solvent; the separated aminated intermediate can be used for rearrangement ring-opening and ring-closing reaction after being collected.
Claims (6)
1. The rearrangement optimization production method of methyl cyclopentenolone is characterized by comprising the following steps:
(1) the crude rearrangement intermediate was subjected to a stream: transferring a rearrangement intermediate crude product obtained by ring opening and ring closing of the amination intermediate into a reaction kettle connected with the lower part of the rectifying tower body;
(2) benzene was separated by rectification under reduced pressure: when the vacuum degree of the reaction kettle is more than or equal to-0.06 MPa, opening steam for heating, enabling the temperature at the top of the tower to be more than or equal to 40 ℃, and enabling effluent liquid transferred from the condenser and the balance tank to flow into a benzene receiving tank; when the temperature at the top of the tower is more than or equal to 65 ℃, the temperature of the reaction kettle is more than or equal to 135 ℃, and the vacuum degree of the reaction kettle is more than or equal to-0.084 MPa, the benzene separation is finished; maintaining the reflux ratio of the rectifying tower to be 3-4 in the benzene separation process;
(3) separating the prefractionated aminated intermediate by rectification under reduced pressure: after the benzene separation is finished, the distillate transferred from the condenser through the balancing tank flows into a front-distillation amination intermediate receiving tank; when the temperature of the top of the tower is more than or equal to 105 ℃, the temperature of the reaction kettle is more than or equal to 140 ℃ and the vacuum degree of the reaction kettle is more than or equal to-0.088 MPa, the separation of the front-run amination intermediate is finished; keeping the reflux ratio of the rectifying tower to be 4-5 in the separation process of the prefractionation amination intermediate;
(4) separating the refined product of the main distillation rearrangement intermediate by reduced pressure rectification: after the separation of the front-distillation amination intermediate is finished, closing the vacuum of the balancing tank, avoiding the reflux of the rectifying tower, and enabling all liquid transferred from the condenser and the balancing tank to flow into the main-distillation rearrangement intermediate refined product receiving tank; finishing the separation of the refined product of the main distillation rearrangement intermediate when the temperature at the top of the tower is more than or equal to 110 ℃, the temperature of the reaction kettle is more than or equal to 145 ℃ and the vacuum degree of the reaction kettle is more than or equal to-0.092 MPa;
the production method relies on a methyl cyclopentenolone rearrangement optimization production device, which comprises a rectifying tower, a condenser, a balance tank, a vacuum pump, a vacuum buffer tank, a benzene receiving tank, a front-distillation amination intermediate receiving tank, a main-distillation rearrangement intermediate refined product receiving tank, a vacuum pressure gauge, a thermometer, a pipeline and a valve.
2. The rearrangement optimization production method of methylcyclopentenol ketone according to claim 1, wherein the benzene separation is finished when the temperature of the reaction kettle reaches 135 ℃ and the vacuum degree of the reaction kettle reaches-0.084 MPa.
3. The rearrangement optimized production method of methylcyclopentenolone according to claim 1, wherein the rectification column reflux ratio is maintained at 3.5 during benzene separation.
4. The rearrangement optimization production method of methylcyclopentenol ketone according to claim 1, wherein the separation of the front-distilled aminated intermediate is terminated when the temperature of the reaction kettle reaches 140 ℃ and the vacuum degree of the reaction kettle reaches-0.088 MPa.
5. The rearrangement optimized production method of methylcyclopentenolone according to claim 1, wherein the rectification column reflux ratio is maintained at 4.5 during the separation of the prefractionated aminated intermediate.
6. The rearrangement optimization production method of methylcyclopentenol ketone according to claim 1, wherein the separation of the refined product of the main distillation rearrangement intermediate is finished when the temperature of the reaction kettle reaches 145 ℃ and the vacuum degree of the reaction kettle reaches-0.092 MPa.
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