CN110683985B - Method for recovering ethoxyquinoline from ethoxyquinoline waste - Google Patents
Method for recovering ethoxyquinoline from ethoxyquinoline waste Download PDFInfo
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- CN110683985B CN110683985B CN201910998935.6A CN201910998935A CN110683985B CN 110683985 B CN110683985 B CN 110683985B CN 201910998935 A CN201910998935 A CN 201910998935A CN 110683985 B CN110683985 B CN 110683985B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D215/00—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems
- C07D215/02—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom
- C07D215/16—Heterocyclic compounds containing quinoline or hydrogenated quinoline ring systems having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen atoms or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D215/20—Oxygen atoms
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Abstract
The invention provides a method for recovering ethoxyquinoline from ethoxyquinoline waste, and relates to the technical field of material purification. The method utilizes the vegetable oil to dissolve the ethyoxyl quinoline waste, effectively reduces the viscosity of the ethyoxyl quinoline waste, and increases the fluidity and the heat conductivity of the ethyoxyl quinoline waste; by utilizing the property that the boiling point of the vegetable oil is higher than that of the ethoxyquin, the ethoxyquin can be effectively separated from the ethoxyquin waste, and the yield and the purity are high. The results of the examples show that the yield of the ethoxyquinoline obtained by the method provided by the invention can reach more than 80%, and the purity can reach more than 90%.
Description
Technical Field
The invention relates to the technical field of material purification, in particular to a method for recovering ethoxyquinoline from ethoxyquinoline waste.
Background
In the ethoxyquinoline production process, the ethoxyquinoline generates part of ethoxyquinoline waste through vacuum rectification. The content of ethoxyquinoline in the waste is only about 50%, and the ethoxyquinoline is coagulated into solid and cannot be normally used. Therefore, ethoxyquinoline cannot be further distilled out by using a traditional vacuum rectification method, and although the waste can be dissolved by adding common organic solvents such as acetone, ethyl acetate and ethanol, the boiling points of the organic solvents are far lower than that of ethoxyquinoline, the organic solvents are firstly distilled out in the distillation process, and finally, the ethoxyquinoline still remains in the tower kettle as an effective component, so that the effect of recovering ethoxyquinoline cannot be achieved.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for recovering ethoxyquinoline from ethoxyquinoline waste. The method provided by the invention can be used for simply and quickly separating the ethoxyquinoline from the ethoxyquinoline waste, and has high yield and purity.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for recovering ethoxyquinoline from ethoxyquinoline waste, which comprises the following steps:
(1) Mixing the ethyoxyl quinoline waste with vegetable oil to obtain pretreated ethyoxyl quinoline waste;
(2) Adding the pretreated ethoxyquinoline waste into a rectifying tower, heating the tower kettle of the rectifying tower, and vacuumizing the top of the rectifying tower; the rectifying tower is provided with a tower top extraction outlet and a side extraction outlet;
(3) When the temperature at the top of the rectifying tower reaches 180 ℃, pure ethoxyquinoline is extracted from a top extraction outlet of the tower, and vegetable oil is extracted from a side extraction outlet;
(4) When the temperature at the top of the rectifying tower reaches 230 ℃, the rectification is finished.
Preferably, the vegetable oil in step (1) is one or more of soybean oil, peanut oil, palm oil, corn oil and rapeseed oil.
Preferably, the mass of the vegetable oil in the step (1) is 20-25% of the mass of the ethoxyquinoline waste.
Preferably, the rectification column is a batch rectification column.
Preferably, the temperature of the rectifying tower in the step (2) is 250-270 ℃.
Preferably, the tower pressure at the top of the rectifying tower in the step (2) is 1-10 kPa.
Preferably, the side draw outlet in the step (2) is positioned at 2 nd to 3 rd theoretical plates of the rectifying tower.
Preferably, the reflux ratio of pure ethoxyquinoline obtained in the step (3) is 2-3.
The invention provides a method for recovering ethoxyquin from ethoxyquin waste, which is characterized in that the ethoxyquin waste is dissolved by using vegetable oil, so that the viscosity of the ethoxyquin waste is effectively reduced, and the fluidity and the heat conductivity of the ethoxyquin waste are increased; by utilizing the property that the boiling point of the vegetable oil is higher than that of the ethoxyquin, the ethoxyquin can be effectively separated from the ethoxyquin waste, and the yield and the purity are high. The results of the examples show that the yield of the ethoxyquinoline obtained by the method provided by the invention can reach more than 80%, and the purity can reach more than 90%.
Drawings
FIG. 1 is a schematic structural diagram of a rectifying apparatus used in the present invention, wherein 1-a rectifying column, 2-a reboiler, 3-a condenser, 4-a reflux tank, 5-a vacuum pump, 6-a column bottom circulating pump, and 7-a reflux pump.
Detailed Description
The invention provides a method for recovering ethoxyquinoline from ethoxyquinoline waste, which comprises the following steps:
(1) Mixing the ethyoxyl quinoline waste with vegetable oil to obtain pretreated ethyoxyl quinoline waste;
(2) Adding the pretreated ethoxyquinoline waste into a rectifying tower, heating the tower kettle of the rectifying tower, and vacuumizing the top of the rectifying tower; the rectifying tower is provided with a tower top extraction outlet and a side extraction outlet;
(3) When the temperature at the top of the rectifying tower reaches 180 ℃, pure ethoxyquinoline is extracted from a top extraction outlet of the tower, and vegetable oil is extracted from a side extraction outlet;
(4) When the temperature at the top of the rectifying tower reaches 230 ℃, the rectification is finished.
The method mixes ethyoxyl quinoline waste with vegetable oil to obtain the pretreated ethyoxyl quinoline waste. In the invention, the vegetable oil is preferably one or more of soybean oil, peanut oil, palm oil, corn oil and rapeseed oil, and the mass of the vegetable oil is preferably 20-25% of the mass of the ethoxyquin waste, and more preferably 22-24%. The invention does not require any particular mixing means, such as stirring, known to the person skilled in the art. According to the invention, the ethyoxyl quinoline waste is mixed with the vegetable oil, so that the ethyoxyl quinoline waste can be dissolved, the viscosity of the ethyoxyl quinoline waste is reduced, the solid ethyoxyl quinoline waste is changed into a flowing liquid, and the fluidity and the heat conductivity are improved; meanwhile, because the boiling point of the vegetable oil is greater than that of the ethoxyquinoline, the ethoxyquinoline can be distilled out from the top of the rectifying tower in a flowing state to obtain pure ethoxyquinoline.
After the pretreated ethoxyquinoline waste is obtained, the pretreated ethoxyquinoline waste is added into a rectifying tower, and simultaneously, the tower kettle of the rectifying tower is heated, and the top of the rectifying tower is vacuumized. The schematic structural diagram of the rectifying device used in the invention is shown in fig. 1, and preferably comprises a rectifying tower 1, a reboiler 2, a condenser 3, a reflux tank 4, a vacuum pump 5, a tower bottom circulating pump 6 and a reflux pump 7.
In the invention, a side draw outlet is arranged at the 2 nd to 3 rd theoretical plates of the rectifying tower 1, and a tower top draw outlet is arranged at the tower top reflux part of the rectifying tower. In the present invention, the rectification column is preferably a batch rectification column; the rectifying tower is preferably a packed tower or a plate tower; the invention has no special requirements on the specification of the rectifying tower, and the rectifying tower with the specification known by the technical personnel in the field can be used.
In the present invention, the reboiler 2 is in circulating communication with the bottom of the rectification column; the reboiler is provided with a feed inlet and a waste outlet; the heat transfer medium of the reboiler is preferably a heat transfer oil. The invention has no special requirements on the specific model and specification of the reboiler, and the reboiler known by the technical personnel in the field can be used. In the invention, the function of the reboiler is to add the pretreated ethoxyquinoline waste and heat the tower kettle.
In the invention, the inlet of the condenser 3 is communicated with the outlet at the top of the rectifying tower; the cooling medium of the condenser is preferably cooling water. The invention has no special requirements on the specific model and specification of the condenser, and the condenser which is well known by the technical personnel in the field can be used.
In the invention, the inlet of the reflux tank 4 is communicated with the outlet of the condenser, and the outlet is communicated with the inlet at the top of the rectifying tower; in the invention, a tower top extraction outlet is arranged in a pipeline for communicating the reflux tank with the rectifying tower. The invention has no special requirements on the specific model and specification of the reflux tank, and the reflux tank known to a person skilled in the art can be used. In the invention, an outlet of the reflux tank is communicated with an inlet at the top of the rectifying tower, gas fraction distilled from the top of the rectifying tower enters a condensing tank for condensation, condensed fraction enters a reflux tank for reflux, a part of liquid after reflux is taken as a rectifying product and is taken out from a top extraction outlet of the rectifying tower, and the rest reflux liquid returns to the rectifying tower for continuous rectification.
In the present invention, the vacuum pump 5 is in communication with the reflux drum; the invention can control the vacuum degree in the reflux tank, the condenser and the rectifying tower through the vacuum pump. The invention has no special requirements on the specific specification and model of the vacuum pump, and the vacuum pump known by the technical personnel in the field can be used.
The rectification device used in the invention preferably also comprises a pump, and the smooth flow of the raw materials and the liquid among the devices is realized through the pump. In the invention, the pump preferably comprises a tower kettle circulating pump 6 and a reflux pump 7, wherein the tower kettle circulating pump is positioned between the bottom outlet of the rectifying tower and the inlet of the reboiler and is used for realizing the circulating heating of the raw materials between the tower kettle and the reboiler; and the reflux pump is positioned between the outlet of the reflux tank and the inlet at the top of the rectifying tower and is used for feeding the residual reflux liquid into the rectifying tower to continue rectifying.
In the invention, the temperature of the bottom of the rectifying tower is preferably 250-270 ℃, more preferably 255-265 ℃, and the pressure at the top of the rectifying tower is preferably 1-10 kPa, more preferably 4-8 kPa.
When the temperature at the top of the rectifying tower reaches 180 ℃, pure ethoxyquinoline is extracted from a top extraction outlet of the tower, and vegetable oil is extracted from a side extraction outlet. In the present invention, the reflux ratio of the pure ethoxyquinoline is preferably 2 to 3. In the invention, the extracted vegetable oil can be recycled and can be used as a rectification solvent for the next batch of waste.
When the temperature at the top of the rectifying tower reaches 230 ℃, the rectification is finished. According to the invention, by cutting the fraction at 180-230 ℃, the yield and the purity of the obtained ethoxyquinoline are high.
The following examples are provided to illustrate the method for recovering ethoxyquinoline from ethoxyquinoline waste according to the present invention, but they should not be construed as limiting the scope of the present invention.
Example 1
The device shown in fig. 1 is used for recovering ethoxyquinoline in ethoxyquinoline waste, and the specific method is as follows:
(1) Mixing the ethyoxyl quinoline waste (the mass content of the ethyoxyl quinoline is 51.5%) with soybean oil, wherein the mass of the soybean oil is 20% of that of the ethyoxyl quinoline waste, so as to obtain pretreated ethyoxyl quinoline waste;
(2) Feeding the pretreated ethoxyquin waste into a rectifying tower through a feed inlet of a reboiler, and heating a tower kettle of the rectifying tower by using the reboiler to ensure that the temperature of the tower kettle is 270 ℃; vacuumizing the top of the rectifying tower by using a vacuum pump to ensure that the tower pressure at the top of the tower is 10kPa;
(3) When the temperature at the top of the rectifying tower reaches 180 ℃, pure ethoxyquinoline starts to be extracted from a top extraction outlet, the reflux ratio is controlled to be 2;
(4) When the temperature at the top of the rectifying tower reaches 230 ℃, the rectification is finished.
The yield of the pure ethoxyquinoline is 84.3 percent by calculation; the purity of the obtained pure ethoxyquinoline is detected, and the purity of the obtained pure ethoxyquinoline is 93.5% through detection.
Example 2
The device shown in fig. 1 is used for recovering ethoxyquinoline from ethoxyquinoline waste, and the specific method is as follows:
(1) Mixing the ethyoxyl quinoline waste (the mass content of the ethyoxyl quinoline is 48%) with palm oil, wherein the mass of the palm oil is 25% of that of the ethyoxyl quinoline waste, and obtaining the pretreated ethyoxyl quinoline waste;
(2) The pretreated ethoxyquin waste material enters a rectifying tower through a reboiler charging hole, and a reboiler is used for heating a tower kettle of the rectifying tower to ensure that the temperature of the tower kettle is 260 ℃; vacuumizing the top of the rectifying tower by using a vacuum pump to ensure that the tower pressure at the top of the tower is 5kPa;
(3) When the temperature at the top of the rectifying tower reaches 180 ℃, pure ethoxyquinoline starts to be extracted from a top extraction outlet, the reflux ratio is controlled to be 2;
(4) When the temperature at the top of the rectifying tower reaches 230 ℃, the rectification is finished.
The yield of the obtained pure ethoxyquinoline is 81.2 percent by calculation; the purity of the obtained pure ethoxyquinoline is detected, and the purity of the obtained pure ethoxyquinoline is 90.8% through detection.
Example 3
The device shown in fig. 1 is used for recovering ethoxyquinoline from ethoxyquinoline waste, and the specific method is as follows:
(1) Mixing the ethyoxyl quinoline waste (the mass content of the ethyoxyl quinoline is 53.6%) with corn oil, wherein the mass of the corn oil is 22% of that of the ethyoxyl quinoline waste, so as to obtain pretreated ethyoxyl quinoline waste;
(2) Feeding the pretreated ethoxyquin waste into a rectifying tower through a feed inlet of a reboiler, and heating a tower kettle of the rectifying tower by using the reboiler to ensure that the temperature of the tower kettle is 250 ℃; vacuumizing the top of the rectifying tower by using a vacuum pump to ensure that the tower pressure at the top of the tower is 1kPa;
(3) When the temperature at the top of the rectifying tower reaches 180 ℃, pure ethoxyquinoline starts to be extracted from a top extraction outlet, the reflux ratio is controlled to be 2;
(4) When the temperature at the top of the rectifying tower reaches 230 ℃, the rectification is finished.
The yield of the obtained pure ethoxyquinoline is 85.2 percent by calculation; the purity of the obtained pure ethoxyquinoline is detected, and the purity of the obtained pure ethoxyquinoline is 92.7% through detection.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (7)
1. The method for recovering ethoxyquinoline from ethoxyquinoline waste is characterized by comprising the following steps of:
(1) Mixing the ethyoxyl quinoline waste with vegetable oil to obtain pretreated ethyoxyl quinoline waste;
the vegetable oil is one or more of soybean oil, palm oil and corn oil;
(2) Adding the pretreated ethoxyquinoline waste into a rectifying tower, heating the tower kettle of the rectifying tower, and vacuumizing the top of the rectifying tower; the rectifying tower is provided with a tower top extraction outlet and a side extraction outlet;
(3) When the temperature at the top of the rectifying tower reaches 180 ℃, pure ethoxyquinoline is collected from a top collection port of the tower, and vegetable oil is collected from a side collection port;
(4) When the temperature at the top of the rectifying tower reaches 230 ℃, the rectification is finished.
2. The method according to claim 1, wherein the mass of the vegetable oil in the step (1) is 20 to 25 percent of the mass of the ethoxyquinoline waste.
3. The method of claim 1, wherein the rectification column is a batch rectification column.
4. The method as claimed in claim 1, wherein the temperature of the bottom of the rectifying tower in the step (2) is 250 to 270 ℃.
5. The method as claimed in claim 1, wherein the pressure at the top of the rectification column in the step (2) is 1 to 10kPa.
6. The method as claimed in claim 1, wherein the side draw in step (2) is located at 2 to 3 theoretical plates of the rectification column.
7. The method according to claim 1, wherein the reflux ratio of pure ethoxyquinoline extracted in step (3) is 2 to 3.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201264977Y (en) * | 2008-05-19 | 2009-07-01 | 江苏中丹集团股份有限公司 | Continuous treater for ethoxyquin synthetic liquid |
| CN101514187A (en) * | 2009-04-07 | 2009-08-26 | 三门峡市峡威化工有限公司 | Method for producing ethoxyquinoline |
| CN101823998A (en) * | 2010-05-05 | 2010-09-08 | 江苏利田科技有限公司 | Pollution-free production process for ethoxy quinoline by coupling reactor and simulation moving bed |
| CN105968044A (en) * | 2016-05-11 | 2016-09-28 | 张加明 | Industrial production method for ethoxy quinoline |
| CN107417610A (en) * | 2016-05-24 | 2017-12-01 | 华东理工大学 | A kind of advanced high-purity ethoxyquinoline separation purifying technique |
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2019
- 2019-10-21 CN CN201910998935.6A patent/CN110683985B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201264977Y (en) * | 2008-05-19 | 2009-07-01 | 江苏中丹集团股份有限公司 | Continuous treater for ethoxyquin synthetic liquid |
| CN101514187A (en) * | 2009-04-07 | 2009-08-26 | 三门峡市峡威化工有限公司 | Method for producing ethoxyquinoline |
| CN101823998A (en) * | 2010-05-05 | 2010-09-08 | 江苏利田科技有限公司 | Pollution-free production process for ethoxy quinoline by coupling reactor and simulation moving bed |
| CN105968044A (en) * | 2016-05-11 | 2016-09-28 | 张加明 | Industrial production method for ethoxy quinoline |
| CN107417610A (en) * | 2016-05-24 | 2017-12-01 | 华东理工大学 | A kind of advanced high-purity ethoxyquinoline separation purifying technique |
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