CN114307217A - Device and method for extracting o-methallyloxyphenol from waste salt of furan phenol - Google Patents

Device and method for extracting o-methallyloxyphenol from waste salt of furan phenol Download PDF

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Publication number
CN114307217A
CN114307217A CN202111681687.6A CN202111681687A CN114307217A CN 114307217 A CN114307217 A CN 114307217A CN 202111681687 A CN202111681687 A CN 202111681687A CN 114307217 A CN114307217 A CN 114307217A
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evaporator
disc
pipeline
monoether
salt
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陈龙
匡彩远
李乃艳
席璐
江超
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Jiangsu Sanjili Chemical Co ltd
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Jiangsu Sanjili Chemical Co ltd
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Abstract

The invention discloses a device and a method for extracting o-methallyloxyphenol from waste salts of furan phenol, and the device comprises a primary centrifugal machine, a disc evaporator, a washing kettle, a secondary centrifugal machine and a horizontal wiped film evaporator, wherein the bottom of the primary centrifugal machine is connected with the disc evaporator, the washing kettle is connected onto a conveying disc evaporator, the bottom of the washing kettle is connected with the secondary centrifugal machine, and the bottom of the secondary centrifugal machine is connected with the horizontal wiped film evaporator. The method can treat the residual 0.1% of the monoether in the waste salt, solves the problem that the waste salt is difficult to treat into common solid waste because part of the monoether still enters a post-treatment device along with the waste salt after the waste salt is centrifuged in the etherification reaction, and improves the yield of the product.

Description

Device and method for extracting o-methallyloxyphenol from waste salt of furan phenol
Technical Field
The invention relates to the field of chemical industry, in particular to a device and a method for extracting o-methallyloxyphenol from waste salt of furan phenol.
Background
The chemical name of the furan phenol is 2, 3-dihydro-2, 2-dimethyl-7-benzofuranphenol, the furan phenol is mainly used for synthesizing important intermediates of carbamate pesticides such as carbofuran, carbosulfan, benfuracarb, haocarb, furacarb and the like, can be widely used for pest control of crops such as cotton, rice, corn, soybean, sugarcane, sorghum, fruit trees and the like, has the effects of shortening the production period of the crops, promoting the growth and development of the crops and can effectively improve the yield of the crops; and can also be used as a medical intermediate. The main method of the industrial production at home and abroad at present is that catechol and methyl allyl chloride are subjected to etherification reaction to prepare o-methyl allyloxyphenol (monoether), and then the o-methyl allyloxyphenol and the monoether are subjected to transposition and cyclization under the condition of a catalyst to generate the furan phenol. In the etherification reaction, partial monoether still enters a post-treatment device along with the waste salt after the waste salt is centrifuged, so that the waste salt is difficult to treat into common solid waste, and the product yield is low. Therefore, the device and the method for extracting the o-methallyloxyphenol from the waste salt of the furan phenol are provided.
Disclosure of Invention
The invention aims to provide a device and a method for extracting o-methallyloxyphenol from waste salt of furan phenol, aiming at overcoming the defects in the prior art and solving the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme: the device for extracting o-methallyloxyphenol from waste salts of furan phenol comprises a primary centrifuge, a disc evaporator, a washing kettle, a secondary centrifuge and a horizontal scraper film evaporator, wherein the bottom of the primary centrifuge is connected with the disc evaporator, the washing kettle is connected onto the conveying disc evaporator, the bottom of the washing kettle is connected with the secondary centrifuge, and the bottom of the secondary centrifuge is connected with the horizontal scraper film evaporator.
As a preferable technical scheme of the invention, a salt-containing reaction liquid feed pipeline of the furan phenol is arranged at the top of the primary centrifuge, and a filtrate conveying pipeline of the centrifuge is connected to the bottom of the primary centrifuge.
As a preferable technical scheme of the invention, the top of one side of the disc evaporator is connected with a disc evaporator steam inlet pipeline, the bottom of the side surface of the disc evaporator is connected with a disc evaporator steam outlet pipeline, and the top of the disc evaporator is provided with a disc evaporator drain pipeline.
As a preferred technical scheme of the invention, the top of the washing kettle is provided with a methyl isobutyl ketone feeding pipeline and a stirring motor, and the bottom of the stirring motor is connected with a stirring paddle through a coupling.
As a preferable technical scheme of the invention, one side of the bottom of the secondary centrifuge is connected with a filtrate pipeline of the secondary centrifuge.
As a preferable technical scheme, a secondary centrifuge waste salt discharging pipeline, a horizontal wiped film evaporator steam inlet pipeline and a wiped film evaporator gas phase discharging pipeline are arranged at the top of the horizontal wiped film evaporator, one end of the horizontal wiped film evaporator is connected with the wiped film evaporator salt discharging pipeline, and the bottom of the horizontal wiped film evaporator is connected with the wiped film evaporator drain pipeline.
As a preferable technical scheme of the invention, a discharge port at the bottom of the primary centrifugal machine is connected with a feed port at the top of a disc evaporator through a pipeline, the bottom of the disc evaporator is connected with a feed port at the top of a washing kettle through a pipeline, a discharge port at the bottom of the washing kettle is connected with a feed port of a secondary centrifugal machine through a pipeline, and a discharge port at the bottom of the secondary centrifugal machine is connected with a feed port at the top of a horizontal scraper-type film evaporator through a waste salt discharge pipeline of the secondary centrifugal machine.
A method for efficiently extracting a furan phenol intermediate monoether, comprising the steps of:
s1, primary centrifugation: conveying the salt-containing reaction liquid of the furan phenol etherification liquid into a primary centrifuge for separation through a furan phenol salt-containing reaction liquid feeding pipeline, and extracting glycol monomethyl ether and monoether from filtrate to a rectifying device for post-treatment;
s2, primary drying: the centrifugal solid waste salt contains a small amount of glycol methyl ether and monoether and enters a disc of a disc evaporator, the disc is heated by steam input by a steam inlet pipeline of the disc evaporator, the waste salt is dried by the disc, the glycol methyl ether is extracted in a gas phase, the monoether has a high boiling point, and part of the monoether remains in the dried waste salt, and the monoether is a heat-sensitive substance, so that the monoether can be polymerized if the heating temperature is high;
s3, washing: and (3) allowing the salt dried by the disc evaporator to enter a washing kettle with the methyl isobutyl ketone, and electrifying a stirring motor on the washing kettle to work to drive a stirring paddle to stir so that the monoether in the disc enters the methyl isobutyl ketone.
S4, secondary centrifugation: discharging the material from the bottom of the washing kettle, feeding the discharged material into a secondary centrifuge, and collecting the methyl isobutyl ketone containing monoether in the filtrate in the secondary centrifuge to a post-treatment device.
S5, secondary drying, collecting the salt containing methyl isobutyl ketone after the secondary centrifuge centrifugation into a horizontal wiped film evaporator, heating the film, evaporating the methyl isobutyl ketone out of the system for post-treatment, collecting the waste salt containing no monoether methyl isobutyl ketone at the bottom of the film, and removing the waste salt containing no monoether methyl isobutyl ketone from the bottom of the film to a post-treatment device.
The invention has the beneficial effects that: the method can treat the residual 0.1% of the monoether in the waste salt, solves the problem that the waste salt is difficult to treat into common solid waste because part of the monoether still enters a post-treatment device along with the waste salt after the waste salt is centrifuged in the etherification reaction, and improves the yield of the product.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
In the figure: the device comprises a furan phenol salt-containing reaction liquid feeding pipeline 1, a primary centrifuge 2, a centrifuge filtrate conveying pipeline 3, a disc evaporator 4, a disc evaporator steam inlet pipeline 5, a disc evaporator steam outlet pipeline 6, a washing kettle 7, a methyl isobutyl ketone feeding pipeline 8, a secondary centrifuge filtrate pipeline 9, a secondary centrifuge waste salt discharging pipeline 10, a horizontal wiped film evaporator steam inlet pipeline 11, a wiped film evaporator drain pipeline 12, a wiped film evaporator gas phase discharging pipeline 13, a wiped film evaporator salt discharging pipeline 14, a secondary centrifuge 15, a horizontal wiped film evaporator 16 and a disc evaporator drain pipeline 17.
Detailed Description
The following detailed description of the preferred embodiments of the present invention, taken in conjunction with the accompanying drawings, will make the advantages and features of the invention more readily understood by those skilled in the art, and thus will more clearly and distinctly define the scope of the invention.
Referring to fig. 1, the present invention provides a technical solution: the device for extracting o-methallyloxyphenol from waste furan phenol salt comprises a primary centrifugal machine 2, a disc evaporator 4, a washing kettle 7, a secondary centrifugal machine 15 and a horizontal wiped film evaporator 16, wherein the bottom of the primary centrifugal machine 2 is connected with the disc evaporator 4, the conveying disc evaporator 4 is connected with the washing kettle 7, the bottom of the washing kettle 7 is connected with the secondary centrifugal machine 15, and the bottom of the secondary centrifugal machine 15 is connected with the horizontal wiped film evaporator 16.
The top of the primary centrifuge 2 is provided with a furan phenol saliferous reaction liquid feeding pipeline 1, and the bottom of the primary centrifuge 2 is connected with a centrifuge filtrate conveying pipeline 3.
The top of one side of the disc evaporator 4 is connected with a disc evaporator steam inlet pipeline 5, the bottom of the side surface of the disc evaporator 4 is connected with a disc evaporator steam outlet pipeline 6, and the top of the disc evaporator 4 is provided with a disc evaporator drainage pipeline 17.
The top of the washing kettle 7 is provided with a methyl isobutyl ketone feeding pipeline 8 and a stirring motor, and the bottom of the stirring motor is connected with a stirring paddle through a coupling.
The secondary centrifuge filtrate line 9 is connected to one side of the bottom of the secondary centrifuge 15.
The top of the horizontal wiped film evaporator 16 is provided with a secondary centrifuge waste salt lower discharge pipeline 10, a horizontal wiped film evaporator steam inlet pipeline 11 and a wiped film evaporator gas phase discharge pipeline 13, one end of the horizontal wiped film evaporator 16 is connected with a wiped film evaporator lower salt pipeline 14, and the bottom of the horizontal wiped film evaporator 16 is connected with a wiped film evaporator drain pipeline 12.
The bottom discharge hole of the primary centrifugal machine 2 is connected with the feed inlet at the top of the disc evaporator 4 through a pipeline, the bottom of the disc evaporator 4 is connected with the feed inlet at the top of the washing kettle 7 through a pipeline, the discharge hole at the bottom of the washing kettle 7 is connected with the feed inlet of the secondary centrifugal machine 15 through a pipeline, and the discharge hole at the bottom of the secondary centrifugal machine 15 is connected with the feed inlet at the top of the horizontal wiped film evaporator 16 through a secondary centrifugal machine waste salt discharging pipeline 10.
A method for efficiently extracting a furan phenol intermediate monoether, comprising the steps of:
s1, primary centrifugation: conveying the salt-containing reaction liquid of the furan phenol etherification liquid into a primary centrifuge 2 through a furan phenol salt-containing reaction liquid feeding pipeline 1 for separation, and extracting glycol monomethyl ether and monoether from filtrate to a rectifying device for post-treatment;
s2, primary drying: the centrifugal solid waste salt contains a small amount of ethylene glycol monomethyl ether and monoether and enters a disc of a disc evaporator 4, the disc is heated by steam input by a steam inlet pipeline 5 of the disc evaporator, the waste salt is dried by the disc, the ethylene glycol monomethyl ether is extracted in a gas phase, the monoether has a high boiling point, and part of the monoether remains in the dried waste salt, and the monoether is a heat-sensitive substance, so that the monoether can be polymerized if the heating temperature is high;
s3, washing: the salt dried by the disc evaporator 4 enters a washing kettle 7 with methyl isobutyl ketone, and a stirring motor on the washing kettle 7 is electrified to work to drive a stirring paddle to stir, so that the monoether in the disc enters the methyl isobutyl ketone.
S4, secondary centrifugation: discharging the material from the bottom of the washing kettle 7, feeding the discharged material into a secondary centrifuge 15, and collecting the methyl isobutyl ketone containing monoether from the filtrate in the secondary centrifuge 15 to a post-processing device.
S5, secondary drying, collecting the salt containing methyl isobutyl ketone after being centrifuged by the secondary centrifuge 15 into the horizontal wiped film evaporator 16, heating the film, evaporating the methyl isobutyl ketone out of the system for post-treatment, collecting the waste salt containing no monoether methyl isobutyl ketone at the bottom of the film, and removing the waste salt containing no monoether methyl isobutyl ketone from the bottom of the film to a post-treatment device.
Example (b): a device and a method for extracting o-methallyloxyphenol from furan phenol waste salt comprise a primary centrifuge 2, a disc evaporator 4, a washing kettle 7, a secondary centrifuge 15 and a horizontal wiped film evaporator 16;
the method comprises the following steps:
s1, primary centrifugation: separating the saliferous reaction liquid of the furan phenol etherification liquid in a primary centrifuge 2, and extracting glycol monomethyl ether and monoether from the filtrate to a rectification device for post-treatment;
s2, primary drying: the centrifugal solid waste salt contains a small amount of 3-5% of glycol methyl ether and 2-3% of monoether, the salt content is 95-92%, the disc is heated by a steam heating device with 0.3mpa steam, the waste salt is dried by the disc, the glycol methyl ether is extracted from gas phase, and the monoether has higher boiling point, so that part of monoether remains in the dried waste salt; since monoether is a heat-sensitive substance, if the heating temperature is too high, monoether polymerization may be caused; controlling the drying time of the waste salt to be 10-15min through the rotating speed of a motor of the disc dryer; the content of the monoether of the waste salt after drying is 4-5%;
s3, washing: and (3) putting the disc dry salt into a washing kettle 7 with methyl isobutyl ketone, stirring by a stirring paddle in the washing kettle 7 to extract the monoether in the disc into the methyl isobutyl ketone, wherein the mass ratio of the methyl isobutyl ketone to the waste salt is 1: 1.5;
s4, secondary centrifugation: discharging methyl isobutyl ketone, monoether and salt at the bottom of the washing kettle, feeding the discharged materials into a secondary centrifuge 15, and collecting the methyl isobutyl ketone containing monoether from the filtrate of the secondary centrifuge 15 to a post-treatment device.
S5, secondary drying, extracting the salt containing methyl isobutyl ketone into the horizontal wiped film evaporator 16 after centrifugation, heating the salt containing methyl isobutyl ketone by using 0.4mpa steam of a film, evaporating the methyl isobutyl ketone out of the system for post-treatment, and extracting the waste salt containing no monoether methyl isobutyl ketone from the bottom of the film to be removed to a post-treatment device; the monoether content in the salt is reduced to 0.1%.
The method can treat the residual 0.1% of the monoether in the waste salt, solves the problem that the waste salt is difficult to treat into common solid waste because part of the monoether still enters a post-treatment device along with the waste salt after the waste salt is centrifuged in the etherification reaction, and improves the yield of the product.
The above examples only show some embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.

Claims (8)

1. The device for extracting o-methallyloxyphenol from waste salts of furan phenol comprises a primary centrifuge (2), a disc evaporator (4), a washing kettle (7), a secondary centrifuge (15) and a horizontal wiped film evaporator (16), and is characterized in that: the bottom of the primary centrifugal machine (2) is connected with a disc evaporator (4), a washing kettle (7) is connected to the conveying disc evaporator (4), the bottom of the washing kettle (7) is connected with a secondary centrifugal machine (15), and the bottom of the secondary centrifugal machine (15) is connected with a horizontal scraper-type film evaporator (16).
2. The device for extracting o-methallyloxyphenol from waste salts of furan phenol as claimed in claim 1, wherein: the top of the primary centrifuge (2) is provided with a furan phenol salt-containing reaction liquid feeding pipeline (1), and the bottom of the primary centrifuge (2) is connected with a centrifuge filtrate conveying pipeline (3).
3. The device for extracting o-methallyloxyphenol from waste salts of furan phenol as claimed in claim 1, wherein: the device is characterized in that a disc evaporator steam inlet pipeline (5) is connected to the top of one side of the disc evaporator (4), a disc evaporator steam outlet pipeline (6) is connected to the bottom of the side face of the disc evaporator (4), and a disc evaporator drain pipeline (17) is installed on the top of the disc evaporator (4).
4. The device for extracting o-methallyloxyphenol from waste salts of furan phenol as claimed in claim 1, wherein: the top of the washing kettle (7) is provided with a methyl isobutyl ketone feeding pipeline (8) and a stirring motor, and the bottom of the stirring motor is connected with a stirring paddle through a coupler.
5. The device for extracting o-methallyloxyphenol from waste salts of furan phenol as claimed in claim 1, wherein: one side of the bottom of the secondary centrifugal machine (15) is connected with a secondary centrifugal machine filtrate pipeline (9).
6. The device for extracting o-methallyloxyphenol from waste salts of furan phenol as claimed in claim 1, wherein: the horizontal wiped film evaporator is characterized in that a secondary centrifuge waste salt discharging pipeline (10), a horizontal wiped film evaporator steam inlet pipeline (11) and a wiped film evaporator gas phase discharging pipeline (13) are arranged at the top of the horizontal wiped film evaporator (16), one end of the horizontal wiped film evaporator (16) is connected with a wiped film evaporator salt discharging pipeline (14), and the bottom of the horizontal wiped film evaporator (16) is connected with a wiped film hydrophobic film evaporator pipeline (12).
7. The device for extracting o-methallyloxyphenol from waste salts of furan phenol as claimed in claim 1, wherein: the bottom discharge hole of the primary centrifugal machine (2) is connected with the feed inlet at the top of the disc evaporator (4) through a pipeline, the bottom of the disc evaporator (4) is connected with the feed inlet at the top of the washing kettle (7) through a pipeline, the discharge hole at the bottom of the washing kettle (7) is connected with the feed inlet of the secondary centrifugal machine (15) through a pipeline, and the discharge hole at the bottom of the secondary centrifugal machine (15) is connected with the feed inlet at the top of the horizontal scraper-type film evaporator (16) through a discharge pipeline (10) under the waste salt of the secondary centrifugal machine.
8. The method for efficiently extracting the monoether of the furan phenol intermediate as claimed in claim 1, wherein: the method comprises the following steps:
s1, primary centrifugation: conveying the salt-containing reaction liquid of the furan phenol etherification liquid into a primary centrifuge (2) through a furan phenol salt-containing reaction liquid feeding pipeline (1) for separation, and extracting glycol monomethyl ether and monoether from filtrate to a rectifying device for post-treatment;
s2, primary drying: the centrifugal solid waste salt contains a small amount of glycol methyl ether and monoether and enters a disc of a disc evaporator (4), the disc is heated by steam input through a steam inlet pipeline (5) of the disc evaporator, the waste salt is dried by the disc, the glycol methyl ether is extracted in a gas phase, the monoether has a high boiling point, and the dried waste salt still contains part of the monoether, and the monoether is a heat-sensitive substance and can cause polymerization of the monoether if the heating temperature is higher;
s3, washing: the salt dried by the disc evaporator (4) enters a washing kettle (7) with methyl isobutyl ketone, and a stirring motor on the washing kettle (7) is electrified to work to drive a stirring paddle to stir, so that the monoether in the disc enters the methyl isobutyl ketone.
S4, secondary centrifugation: discharging the material from the bottom of the washing kettle (7) and feeding the material into a secondary centrifuge (15), and extracting the methyl isobutyl ketone containing monoether from the filtrate in the secondary centrifuge (15) to a post-treatment device.
S5, secondary drying, collecting the salt containing methyl isobutyl ketone after being centrifuged by the secondary centrifuge (15) into the horizontal wiped film evaporator (16), heating the film, evaporating the methyl isobutyl ketone out of the system for post-treatment, and collecting the waste salt containing no monoether methyl isobutyl ketone at the bottom of the film to be removed to a post-treatment device.
CN202111681687.6A 2021-12-30 2021-12-30 Device and method for extracting o-methallyloxyphenol from waste salt of furan phenol Pending CN114307217A (en)

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Application publication date: 20220412