CN110229129B - Equipment and method for preparing 4-chlorophthalic anhydride - Google Patents
Equipment and method for preparing 4-chlorophthalic anhydride Download PDFInfo
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- CN110229129B CN110229129B CN201910545669.1A CN201910545669A CN110229129B CN 110229129 B CN110229129 B CN 110229129B CN 201910545669 A CN201910545669 A CN 201910545669A CN 110229129 B CN110229129 B CN 110229129B
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D307/87—Benzo [c] furans; Hydrogenated benzo [c] furans
- C07D307/89—Benzo [c] furans; Hydrogenated benzo [c] furans with two oxygen atoms directly attached in positions 1 and 3
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Abstract
The invention discloses equipment and a method for preparing 4-chlorophthalic anhydride, and belongs to the field of fine chemical engineering. An apparatus for preparing 4-chlorophthalic anhydride comprises a loop column reactor; the chlorine tank is used for introducing chlorine into the circulating tower reactor in sections through the first chlorine introducing pipe and the second chlorine introducing pipe; the phthalic anhydride dissolving kettle is used for feeding materials into the circulating tower reactor through a feeding pipe; the condenser is arranged on the circulating tower reactor; the invention utilizes the circulating tower reactor to carry out the efficient continuous chlorination reaction by sectionally introducing chlorine, and the circulating tower reactor effectively carries out the deep chlorination; chlorine is introduced into the tower in sections, hydrogen chloride is effectively utilized at a high position to dilute chlorine, the concentration of partial chlorine is reduced, and the generation of dichlorobenzene anhydride is reduced; the conversion rate of the monochloro is increased to be more than 57 percent by 35 percent; the content of the dichlorophenolic anhydride is reduced to less than 0.5 percent from 3 percent; the equipment investment rate is reduced by more than 50 percent; the utilization rate of equipment is improved by utilizing a continuous production mode, continuous production is carried out, and the safety risk is reduced.
Description
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to equipment and a method for preparing 4-chlorophthalic anhydride.
Background
4-chlorophthalic anhydride, also known as 4-chlorophthalic anhydride, as a white crystalline solid, melting point: 96 ℃, CAS:118-45-6, which are currently used for preparing new material polyimide, dye, medical intermediate, pesticide and other fields.
At present, the preparation method mainly comprises a phthalic anhydride/sodium hypochlorite chlorination method, a mononitrobenzene anhydride/phosphorus pentachloride chlorination method, a phthalic anhydride chlorine chlorination method, a 4-chloro-o-xylene catalytic oxidation method and the like; wherein, the phthalic anhydride chlorine chlorination method is divided into a phthalic anhydride liquid-phase chlorination method and a phthalic anhydride gas-phase chlorination method; the industrialized method mainly comprises the steps of directly vaporizing and liquefying phthalic anhydride and chlorine:
the phthalic anhydride and chlorine vaporization process has reaction temperature of 360-400 deg.c and fast reaction speed, and this results in high safety risk, high dichlorobenzene anhydride content in the product, low material utilization and high investment.
The liquid-phase chlorination method for phthalic anhydride and chlorine has relatively low temperature, the reaction temperature is 200 ℃, the reaction is carried out in a reaction kettle, the reaction time is long, the single chlorine reaction conversion rate is low, the time is long, the safety coefficient is low, the equipment utilization rate is low, the content of single chlorine (3-chlorine and 4-chlorine) phthalic anhydride is about 35%, 65% is phthalic anhydride, the reaction time is 8 hours, the auxiliary time is added, and the single batch time is 12 hours.
Thus, it would be highly desirable to develop an apparatus and method for increasing the conversion of the monochloro reaction and the content of monochlorobenzene anhydride.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a method and equipment for preparing 4-chlorophthalic anhydride.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
an apparatus for preparing 4-chlorophthalic anhydride, comprising: a loop column reactor; the chlorine tank is used for introducing chlorine into the circulating tower reactor in sections through the first chlorine introducing pipe and the second chlorine introducing pipe; the phthalic anhydride dissolving kettle is used for feeding materials into the circulating tower reactor through a feeding pipe; and the condenser is arranged on the circulating tower reactor.
Further, the reaction equipment further comprises a phthalic anhydride tank, and the phthalic anhydride tank feeds the phthalic anhydride dissolution kettle through a solid feeder.
Preferably, in the above technical scheme, a stirrer is arranged on the phthalic anhydride dissolving kettle.
Preferably, in the above technical scheme, the feeding pipe is connected with a metering pump and a first metering cylinder, the feeding pipe is also connected with a first standby pipe connected with the metering pump in parallel, and the feeding pipe is also connected with a second standby pipe connected with the first metering cylinder in parallel.
Preferably, in the above technical scheme, the first chlorine introducing pipe and the second chlorine introducing pipe are both connected with a second metering cylinder, and the first chlorine introducing pipe and the second chlorine introducing pipe are both connected with a third standby pipe connected in parallel with the second metering cylinder.
Preferably, in the above technical scheme, the phthalic anhydride dissolving kettle and the circulating tower reactor are both provided with a thermometer and a pressure gauge, and the phthalic anhydride dissolving kettle is also provided with a liquid level gauge.
The invention also provides a method for preparing 4-chlorophthalic anhydride by using the equipment, which specifically comprises the following steps:
s1, continuously adding phthalic anhydride containing a catalyst into a phthalic anhydride dissolution kettle, and preserving heat at 150-160 ℃;
s2, continuously adding the phthalic anhydride dissolved in the step S1 into a circulating tower reactor;
s3, introducing chlorine into the circulating tower reactor in two sections;
s4, controlling the temperature by a condenser coupled with the circulating tower reactor, continuously producing monochlorophthalic anhydride (4-chlorophthalic anhydride and 3-chlorophthalic anhydride with the ratio of more than 30:1) from an outlet at the upper end of the circulating tower reactor, and rectifying to obtain the 4-chlorophthalic anhydride.
The reaction equation is as follows:
further, in the technical scheme, when the molar ratio of chlorine to phthalic anhydride is 0.5-0.8:1 and exceeds 0.8:1, 3, 5-dichlorophenoanhydride is detected in addition to the 4, 5-dichlorobenzene anhydride by-product after continuous reaction, and when the molar ratio is lower than 0.5:1, the residual amount of phthalic anhydride is obviously increased.
Further, the catalyst is one or more of ferric trichloride, aluminum trichloride, ferrous sulfate, boron trifluoride-diethyl ether and the like, and the dosage of the catalyst is 0.1-0.25% of the weight of phthalic anhydride.
Compared with the prior art, the invention provides a method and equipment for preparing 4-chlorophthalic anhydride, which have the following beneficial effects:
1. according to the equipment and the method for preparing the 4-chlorophthalic anhydride, solid phthalic anhydride and a catalyst are continuously added into a phthalic anhydride dissolving kettle, the temperature is kept at 150-160 ℃, the mixture is melted, the mixture is continuously injected into a circulating tower reactor through a feeding pipe and a metering pump on the feeding pipe, a chlorine tank is used for introducing chlorine into the circulating tower reactor in sections through a first chlorine introducing pipe and a second chlorine introducing pipe, the total ratio of the phthalic anhydride to the chlorine is 1:0.5-0.8, the monochlorophthalic anhydride is continuously produced, and the 4-chlorophthalic anhydride is obtained after rectification.
2. According to the equipment and the method for preparing the 4-chlorophthalic anhydride, the circulation tower reactor is utilized to carry out the efficient continuous chlorination reaction by sectionally introducing chlorine, and the circulation tower reactor effectively carries out deep chlorination; chlorine is introduced into the tower in sections, hydrogen chloride is effectively utilized at a high position to dilute chlorine, the concentration of partial chlorine is reduced, and the generation of dichlorobenzene anhydride is reduced; the conversion rate of the monochloro is increased to be more than 57 percent by 35 percent; the content of the dichlorophenolic anhydride is reduced to less than 0.5 percent from 3 percent; the equipment investment rate is reduced by more than 50 percent; the utilization rate of equipment is improved by utilizing a continuous production mode, continuous production is realized, and the safety risk is reduced.
Drawings
FIG. 1 is a flow chart of an apparatus for preparing 4-chlorophthalic anhydride according to the present invention;
FIG. 2 is a schematic diagram of the structure of a loop column reactor of an apparatus for preparing 4-chlorophthalic anhydride according to the present invention;
fig. 3 is a schematic diagram of a phthalic anhydride dissolving kettle of the equipment for preparing 4-chlorophthalic anhydride.
In the figure: 1. a loop column reactor; 2. a condenser; 3. a thermometer; 4. a pressure gauge; 5. a chlorine tank; 6. a first chlorine pipe; 7. a second chlorine pipe; 8. a phthalic anhydride dissolving kettle; 9. a feed pipe; 10. a second metering cylinder; 11. a third backup pipe; 12. a first metering cylinder; 13. a second backup pipe; 14. a metering pump; 15. a first reserve tube; 16. a stirrer; 17. a liquid level gauge; 18. a phthalic anhydride tank; 19. a solids feeder.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments.
In the description of the present invention, it should be understood that the terms "upper," "lower," "front," "rear," "left," "right," "top," "bottom," "inner," "outer," and the like indicate or are based on the orientation or positional relationship shown in the drawings, merely to facilitate description of the present invention and to simplify the description, and do not indicate or imply that the devices or elements referred to must have a particular orientation, be configured and operated in a particular orientation, and thus should not be construed as limiting the invention.
Example 1
Referring to fig. 1 to 3, an apparatus for preparing 4-chlorophthalic anhydride, comprising:
a loop column reactor 1;
chlorine gas tank 5, through first chlorine pipe 6 and second chlorine pipe 7 section to circulate the tower reactor 1 and let in chlorine gas;
a phthalic anhydride dissolution kettle 8 is used for feeding materials into the circulating tower reactor 1 through a feeding pipe 9;
a condenser 2 disposed on the loop column reactor 1; solid phthalic anhydride and a catalyst are continuously added into a phthalic anhydride dissolving kettle 8, the temperature is kept between 150 ℃ and 160 ℃, the mixture is melted, the mixture is continuously injected into a circulating tower reactor 1 through a feeding pipe 9 and a metering pump 14 on the feeding pipe 9, a chlorine tank 5, chlorine is introduced into the circulating tower reactor 1 in a sectional manner through a first chlorine introducing pipe 6 and a second chlorine introducing pipe 7, the total proportion of the phthalic anhydride and the chlorine is 1:0.5-0.8, the monochlorophthalic anhydride is continuously produced, and the 4-chlorophthalic anhydride is obtained after rectification.
The phthalic anhydride dissolving kettle 8 is further provided with a phthalic anhydride tank 18, and the phthalic anhydride tank 18 is used for feeding materials to the phthalic anhydride dissolving kettle 8 through a solid feeder 19, so that the materials are convenient to feed.
The phthalic anhydride dissolving kettle 8 is provided with a stirrer 16, which is convenient for dissolving.
The feeding pipe 9 is connected with a metering pump 14 and a first metering cylinder 12, the feeding pipe 9 is also connected with a first standby pipe 15 connected with the metering pump 14 in parallel, the feeding pipe 9 is also connected with a second standby pipe 13 connected with the first metering cylinder 12 in parallel, the working state can be switched, and the first standby pipe 15 and the second standby pipe 13 can be conducted when the metering pump 14 and the first metering cylinder 12 do not work so as to feed.
The first chlorine pipe 6 and the second chlorine pipe 7 are connected with a second measuring cylinder 10, the first chlorine pipe 6 and the second chlorine pipe 7 are also connected with a third standby pipe 11 connected with the second measuring cylinder 10 in parallel, and when the second measuring cylinder 10 does not work, the third standby pipe 11 can be used for chlorine communication.
The phthalic anhydride dissolving kettle 8 and the circulating tower reactor 1 are both provided with a thermometer 3 and a pressure meter 4, and the phthalic anhydride dissolving kettle 8 is also provided with a liquid level meter 17, so that the temperature and the pressure of the phthalic anhydride dissolving kettle 8 and the circulating tower reactor 1 can be monitored conveniently.
By utilizing the circulating tower reactor 1, chlorine is introduced in sections to carry out efficient continuous chlorination reaction, and the circulating tower reactor 1 effectively carries out deep chlorination; chlorine is introduced into the tower in sections, hydrogen chloride is effectively utilized at a high position to dilute chlorine, the concentration of partial chlorine is reduced, and the generation probability of dichlorobenzene anhydride is reduced; the utilization rate of equipment is improved by utilizing a continuous production mode, continuous production is realized, and the safety risk is reduced.
The method for synthesizing 4-chlorophthalic anhydride by using the equipment comprises the following steps:
comparative examples:
firstly, 4000 kg of phthalic anhydride and 4 kg of aluminum trichloride are added into a reaction kettle, the temperature is controlled to be 200 ℃ by using heat conduction oil, 1150 kg of chlorine (1:0.6) is introduced at a constant speed, and the reaction is carried out for 8 hours; after the reaction was completed, 35.2% of monochlorobenzene anhydride (GC detection: 31.1% of 4-chlorobenzoic anhydride, 4.1% of 3-chlorobenzoic anhydride), 3.5% of 4, 5-dichlorobenzene anhydride and 61.3% of phthalic anhydride was monitored.
Example 2:
as shown in figure 1, the method for preparing 4-chlorophthalic anhydride comprises the steps of continuously adding phthalic anhydride and 1%o of aluminum trichloride into a phthalic anhydride dissolution kettle 8 through a solid feeder 19, preserving heat at 150 ℃, continuously adding phthalic anhydride into a circulating tower reactor 1 through a metering pump 14, and controlling the temperature to about 200 ℃ by using a condenser 2 coupled on the circulating tower reactor 1; the mass ratio of phthalic anhydride to chlorine is 1:0.8, chlorine is introduced into the tower circulation tower reactor 1 in two sections, the space time is 4 hours, monochlorophthalic anhydride is continuously produced from the outlet 101 at the upper end of the circulation tower reactor 1, and 4-chlorophthalic anhydride is obtained by rectification;
adding 3700 kg of reaction liquid in a full tower, controlling the temperature to 190 ℃, continuously adding 900 kg/h of phthalic anhydride { 0.1% weight ratio of aluminum trichloride in phthalic anhydride }, and continuously reacting for 24 hours with 345 kg/h of chlorine; product monitoring, total of 4-chlorophthalic anhydride and 3-chlorophthalic anhydride 65.5% (GC detection: 4-chlorophthalic anhydride 63.2%, 3-chlorophthalic anhydride 2.3%), 4, 5-dichlorophenylanhydride 0.2%, phthalic anhydride 34.2%.
Example 3:
as shown in figure 1, the method for preparing 4-chlorophthalic anhydride comprises the steps of continuously adding phthalic anhydride and 1%o of aluminum trichloride into a phthalic anhydride dissolution kettle 8 through a solid feeder 19, preserving heat at 150 ℃, continuously adding phthalic anhydride into a circulating tower reactor 1 through a metering pump 14, and controlling the temperature to about 200 ℃ by using a condenser 2 coupled on the circulating tower reactor 1; the mass ratio of phthalic anhydride to chlorine is 1:0.6, chlorine is introduced into the tower circulation tower reactor 1 in two sections, the space time is 4 hours, monochlorophthalic anhydride is continuously produced from the outlet 101 at the upper end of the circulation tower reactor 1, and 4-chlorophthalic anhydride is obtained by rectification;
adding 3700 kg of reaction liquid in a full tower, controlling the temperature to be 200 ℃, continuously adding 900 kg/h of phthalic anhydride { wherein 0.1% weight ratio of aluminum trichloride is mixed in the phthalic anhydride }, and continuously reacting for 24 hours with 259 kg/h of chlorine; product monitoring, total of 4-chlorophthalic anhydride and 3-chlorophthalic anhydride 57.0% (GC detection: 4-chlorophthalic anhydride 55.2%, 3-chlorophthalic anhydride 1.8%), 4, 5-dichlorophenylanhydride 0.1%, phthalic anhydride 42.9%.
Example 4:
in the method for preparing 4-chlorophthalic anhydride, as shown in figure 1, phthalic anhydride is continuously added into a phthalic anhydride dissolution kettle 8 through a solid feeder 19, the temperature is kept at 150 ℃, phthalic anhydride is continuously added into a circulating tower reactor 1 through a metering pump 14, and the temperature is controlled to be about 200 ℃ by a condenser 2 coupled on the circulating tower reactor 1; the mass ratio of phthalic anhydride to chlorine is 1:0.8, chlorine is introduced into the tower circulation tower reactor 1 in two sections, the space time is 4 hours, monochlorophthalic anhydride is continuously produced from the outlet 101 at the upper end of the circulation tower reactor 1, and 4-chlorophthalic anhydride is obtained by rectification;
adding 3700 kg of reaction liquid in a full tower, controlling the temperature to 220 ℃, continuously adding 900 kg/h of phthalic anhydride { 0.1% weight ratio of aluminum trichloride in phthalic anhydride }, and continuously reacting for 24 hours with 345 kg/h of chlorine; product monitoring, total of 78.8% 4-chlorophthalic anhydride and 3-chlorophthalic anhydride (GC detection: 75.8% 4-chlorophthalic anhydride, 2.5% 3-chlorophthalic anhydride), 0.4% 4, 5-dichlorophenolic anhydride, 20.8% phthalic anhydride.
From the comparative example and the present example, it is known that from batch reaction to continuous reaction: the conversion rate of the monochloro is increased to be more than 57 percent by 35 percent; the content of the dichlorophenolic anhydride is reduced to less than 0.5 percent from 3 percent; the equipment investment rate is reduced by 50 percent.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (8)
1. An apparatus for preparing 4-chlorophthalic anhydride, comprising: a loop column reactor (1); a chlorine tank (5) for introducing chlorine gas into the circulating tower reactor (1) in sections through a first chlorine introducing pipe (6) and a second chlorine introducing pipe (7); a phthalic anhydride dissolving kettle (8) is used for feeding the circulating tower reactor (1) through a feeding pipe (9); a condenser (2) arranged on the circulating tower reactor (1); the phthalic anhydride dissolving kettle also comprises a phthalic anhydride tank (18), wherein the phthalic anhydride tank (18) feeds the phthalic anhydride dissolving kettle (8) through a solid feeder (19); the feeding pipe (9) is connected with a metering pump (14) and a first metering cylinder (12), the feeding pipe (9) is also connected with a first standby pipe (15) connected with the metering pump (14) in parallel, and the feeding pipe (9) is also connected with a second standby pipe (13) connected with the first metering cylinder (12) in parallel.
2. An apparatus for producing 4-chlorophthalic anhydride according to claim 1, characterized in that: the phthalic anhydride dissolving kettle (8) is provided with a stirrer (16).
3. An apparatus for producing 4-chlorophthalic anhydride according to claim 1, characterized in that: the first chlorine passing pipe (6) and the second chlorine passing pipe (7) are both connected with a second metering cylinder (10), and the first chlorine passing pipe (6) and the second chlorine passing pipe (7) are both connected with a third standby pipe (11) connected with the second metering cylinder (10) in parallel.
4. An apparatus for producing 4-chlorophthalic anhydride according to claim 1, characterized in that: the phthalic anhydride dissolving kettle (8) and the circulating tower reactor (1) are both provided with a thermometer (3) and a pressure gauge (4), and the phthalic anhydride dissolving kettle (8) is also provided with a liquid level gauge (17).
5. A method for preparing 4-chlorophthalic anhydride, which is characterized by comprising the following steps:
s1, continuously adding phthalic anhydride dissolved with a catalyst into a phthalic anhydride dissolution kettle (8), and preserving heat at 150-160 ℃;
s2, continuously adding the phthalic anhydride dissolved in the step S1 into a circulating tower reactor (1);
s3, introducing chlorine into the circulating tower reactor (1) in a sectional manner through the first chlorine introducing pipe (6) and the second chlorine introducing pipe (7);
s4, controlling the temperature of a condenser (2) coupled to the circulating tower reactor (1), continuously producing monochlorobenzene anhydride from an outlet at the upper end of the circulating tower reactor (1), and rectifying to obtain 4-chlorophthalic anhydride.
6. The method for producing 4-chlorophthalic anhydride according to claim 5, characterized in that: the catalyst is one or more of ferric trichloride, aluminum trichloride, ferrous sulfate and boron trifluoride-diethyl ether.
7. The method for producing 4-chlorophthalic anhydride according to claim 5, characterized in that: the molar ratio of phthalic anhydride to chlorine is 1:0.5-0.8.
8. The method for producing 4-chlorophthalic anhydride according to claim 6, characterized in that: the addition amount of the catalyst is 0.1-0.25% of the weight of phthalic anhydride.
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| CN210150994U (en) * | 2019-06-22 | 2020-03-17 | 栎安化学(上海)有限公司 | Equipment for preparing 4-chlorophthalic anhydride |
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| IN188690B (en) * | 1994-03-29 | 2002-10-26 | Council Of Scient And Indust6R |
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| US5574172A (en) * | 1993-05-27 | 1996-11-12 | Mitsubishi Chemical Corporation | Process for producing halogenated phthalic anhydride |
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