CN110229129A - A kind of device and method thereof preparing 4- chloride anhydride - Google Patents
A kind of device and method thereof preparing 4- chloride anhydride Download PDFInfo
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- CN110229129A CN110229129A CN201910545669.1A CN201910545669A CN110229129A CN 110229129 A CN110229129 A CN 110229129A CN 201910545669 A CN201910545669 A CN 201910545669A CN 110229129 A CN110229129 A CN 110229129A
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- phthalic anhydride
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- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a kind of device and method thereof for preparing 4- chloride anhydride, belong to field of fine chemical.A kind of equipment preparing 4- chloride anhydride, including circulation tower reactor；Chlorine pot is segmented to the circulation tower reactor by the first chlorination tube and the second chlorination tube and leads to chlorine；Phthalic anhydride dissolution kettle is fed by feed pipe to the circulation tower reactor；Condenser is arranged on circulation tower reactor；The present invention utilizes circulation tower reactor, is segmented logical chlorine, carries out high-efficiency and continuous chlorination reaction, circulation tower reactor effectively carries out depth chlorination；It is segmented logical chlorine in tower, is diluted chlorine in high position effective use hydrogen chloride, reduces the concentration of local chlorine, reduce dichloro phthalic anhydride and generate；Monochloro conversion ratio 35% is improved to > 57%；Dichloro phthalic anhydride is down to < 0.5% from 3%；50% or more equipment investment rate decline；Utilization rate of equipment and installations is improved in the way of continuous production, is carried out continuous production, is reduced security risk.
Description
Technical field
The present invention relates to technical field of fine more particularly to a kind of device and method thereof for preparing 4- chloride anhydride.
Background technique
4- chloride anhydride, also known as 4- chloro-benzoic anhydride, white crystalline solid, fusing point: 96 DEG C, CAS:118-45-6, currently used for
Prepare the fields such as new material polyimides, dyestuff, medicine intermediate and pesticide.
Currently, method of its preparation mainly have phthalic anhydride/sodium hypochlorite chloridising, single nitro phthalic anhydride/phosphorus pentachloride chloridising,
Phthalic anhydride chlorinated with chlorine method and 4- chloro-o-xylene catalytic oxidation etc.；Wherein, phthalic anhydride chlorinated with chlorine method is divided into phthalic anhydride liquid phase again
Chloro method and phthalic anhydride gas phase chloro method；Industrialized method is mainly phthalic anhydride and chlorine direct boiling and liquefaction process:
Phthalic anhydride and chlorine gasification, for reaction temperature at 360-400 DEG C, reaction speed is fast, thus security risk is very big, obtains
Product in dichloro phthalic anhydride content it is higher, raw material availability is low, and investment is big.
Phthalic anhydride and chlorine liquid phase chloridising, temperature is relatively low, and reaction temperature is reacted, instead at 200 DEG C in reaction kettle
Long between seasonable, monochloro reaction conversion ratio is low, and the time is long, and safety coefficient is low, and utilization rate of equipment and installations is low, monochloro (3- chlorine and 4- chlorine) phthalic anhydride
Content 35% or so, 65% is phthalic anhydride, and the reaction time 8 hours, in addition non-cutting time, single batch of material time wanted 12 hours.
Thus, the device and method for developing raising monochloro reaction conversion ratio and monochloro phthalic anhydride content are very necessary.
Summary of the invention
The purpose of the present invention is to solve the problems of the prior art, and a kind of method for preparing 4- chloride anhydride proposed
And its equipment.
To achieve the goals above, present invention employs following technical solutions:
A kind of equipment preparing 4- chloride anhydride, comprising: circulation tower reactor；Chlorine pot passes through the first chlorination tube and
Two chlorination tubes, which are segmented to the circulation tower reactor, leads to chlorine；Phthalic anhydride dissolution kettle, by feed pipe to the circulation tower
Formula reactor feed；Condenser is arranged on circulation tower reactor.
Further, above-mentioned consersion unit further includes phthalic anhydride tank, and the phthalic anhydride tank passes through feeder for solid materials to the benzene
The charging of acid anhydride dissolution kettle.
Preferably, in the above-mentioned technical solutions, blender is provided in the phthalic anhydride dissolution kettle.
Preferably, in the above-mentioned technical solutions, metering pump and the first hopper, the charging are connected on the feed pipe
Pipe is also connected with the spare pipe of first in parallel with metering pump, and it is standby that the feed pipe is also connected with second in parallel with the first hopper
With pipe.
Preferably, in the above-mentioned technical solutions, the second metering is respectively connected on first chlorination tube and the second chlorination tube
Tin, the spare pipe of the third in parallel with the second hopper is also respectively connected on first chlorination tube and the second chlorination tube.
Preferably, in the above-mentioned technical solutions, temperature is provided on the phthalic anhydride dissolution kettle and circulation tower reactor
Meter and pressure gauge are additionally provided with liquidometer in the phthalic anhydride dissolution kettle.
Using above equipment, the present invention also provides a kind of methods for preparing 4- chloride anhydride, specifically includes the following steps:
S1, the phthalic anhydride containing catalyst is continuously fed into phthalic anhydride dissolution kettle, keeps the temperature 150-160 DEG C；
S2, the phthalic anhydride dissolved in step S1 is continuously fed into circulation tower reactor；
S3, it is divided to two sections to be passed through chlorine in using circulation tower reactor；
The condenser control temperature coupled on S4, circulation tower reactor, it is continuous from circulation tower reactor upper end outlet
Output monochloro phthalic anhydride (4- chloride anhydride and 3- chloride anhydride, the two ratio are greater than 30:1), rectifying obtains 4- chloride anhydride.
Reaction equation is as follows:
Further, in the above-mentioned technical solutions, chlorine and phthalic anhydride molar ratio are 0.5-0.8:1, when more than 0.8:1, even
After continuous reaction outside 4,5- dichloro by-product of benzoic anhydride, 3,5- dichloro phthalic anhydride is also detected, when being lower than 0.5:1, phthalic anhydride surplus
It obviously increases.
Further, catalyst is selected from the medium one kind of ferric trichloride, alchlor, ferrous sulfate, Eorontrifluoride etherate
Or it is several, catalyst amount is the 0.1-0.25% of phthalic anhydride weight.
Compared with prior art, the present invention provides a kind of method and its equipment for preparing 4- chloride anhydride, having following has
Beneficial effect:
1, the device and method thereof for preparing 4- chloride anhydride, by be constantly added in phthalic anhydride dissolution kettle solid phthalic anhydride and
Catalyst keeps the temperature 150-160 DEG C, is melted, it is tower continuously to squeeze into circulation by the metering pump on feed pipe and feed pipe
Reactor, chlorine pot are segmented to the logical chlorine segmentation of circulation tower reactor by the first chlorination tube and the second chlorination tube and are passed through chlorine
The total ratio of the amount of gas, phthalic anhydride and chlorine species is 1:0.5-0.8, and continuous output monochloro phthalic anhydride obtains 4- chloride anhydride after rectifying.
2, the device and method thereof for preparing 4- chloride anhydride are segmented logical chlorine, carry out high by utilizing circulation tower reactor
Continuous chlorination reaction is imitated, circulation tower reactor effectively carries out depth chlorination；It is segmented logical chlorine in tower, efficiently uses chlorination in a high position
Hydrogen is diluted chlorine, reduces the concentration of local chlorine, reduces dichloro phthalic anhydride and generates；Monochloro conversion ratio 35% is improved to >
57%；Dichloro phthalic anhydride is down to < 0.5% from 3%；50% or more equipment investment rate decline；It is improved and is set in the way of continuous production
Standby utilization rate, continuous production reduce security risk.
Detailed description of the invention
Fig. 1 is a kind of flow chart for the equipment for preparing 4- chloride anhydride proposed by the present invention；
Fig. 2 is a kind of circulation tower reactor structure schematic diagram for the equipment for preparing 4- chloride anhydride proposed by the present invention；
Fig. 3 is a kind of phthalic anhydride dissolution kettle structure schematic diagram for the equipment for preparing 4- chloride anhydride proposed by the present invention.
In figure: 1, circulation tower reactor；2, condenser；3, thermometer；4, pressure gauge；5, chlorine pot；6, the first logical chlorine
Pipe；7, the second chlorination tube；8, phthalic anhydride dissolution kettle；9, feed pipe；10, the second hopper；11, the spare pipe of third；12, the first metering
Cylinder；13, the second spare pipe；14, metering pump；15, the first spare pipe；16, blender；17, liquidometer；18, phthalic anhydride tank；19, solid
Body feeder.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.
In the description of the present invention, it is to be understood that, term " on ", "lower", "front", "rear", "left", "right", "top",
The orientation or positional relationship of the instructions such as "bottom", "inner", "outside" is to be based on the orientation or positional relationship shown in the drawings, merely to just
In description the present invention and simplify description, rather than the device or element of indication or suggestion meaning must have a particular orientation, with
Specific orientation construction and operation, therefore should not be understood as the limitation to invention.
Embodiment 1
Referring to Fig.1-3, a kind of equipment preparing 4- chloride anhydride, comprising:
Circulation tower reactor 1；
Chlorine pot 5 is segmented to circulation tower reactor 1 by the first chlorination tube 6 and the second chlorination tube 7 and leads to chlorine；
Phthalic anhydride dissolution kettle 8 is fed by feed pipe 9 to circulation tower reactor 1；
Condenser 2 is arranged on circulation tower reactor 1；By the way that solid phthalic anhydride is constantly added in phthalic anhydride dissolution kettle 8
And catalyst, 150-160 DEG C is kept the temperature, is melted, ring is continuously squeezed by the metering pump 14 on feed pipe 9 and feed pipe 9
Tower reactor 1 is flowed, chlorine pot 5 is segmented to circulation tower reactor 1 by the first chlorination tube 6 and the second chlorination tube 7 and leads to chlorine
It is segmented and is passed through chlorine, the total ratio of the amount of phthalic anhydride and chlorine species is 1:0.5-0.8, and continuous output monochloro phthalic anhydride obtains after rectifying
To 4- chloride anhydride.
It further include phthalic anhydride tank 18, phthalic anhydride tank 18 is fed by feeder for solid materials 19 to phthalic anhydride dissolution kettle 8, convenient for charging.
Blender 16 is provided in phthalic anhydride dissolution kettle 8, convenient for dissolution.
Metering pump 14 and the first hopper 12 are connected on feed pipe 9, feed pipe 9 is also connected in parallel with metering pump 14
First spare pipe 15, feed pipe 9 are also connected with the spare pipe 13 of second in parallel with the first hopper 12, can be with switch operating shape
State, the first spare pipe 15 and the second spare pipe 13 can the conducting when metering pump 14 and the first hopper 12 do not work, carry out into
Material.
The second hopper 10, the first chlorination tube 6 and the second logical chlorine are respectively connected on first chlorination tube 6 and the second chlorination tube 7
The spare pipe 11 of the third in parallel with the second hopper 10 is also respectively connected on pipe 7, it, can third when the second hopper 10 does not work
Spare pipe 11 leads to chlorine.
Thermometer 3 and pressure gauge 4 are provided in phthalic anhydride dissolution kettle 8 and circulation tower reactor 1, in phthalic anhydride dissolution kettle 8
It is additionally provided with liquidometer 17, convenient for monitoring the temperature and pressure of phthalic anhydride dissolution kettle 8 and circulation tower reactor 1.
By utilizing circulation tower reactor 1, it is segmented logical chlorine, carries out high-efficiency and continuous chlorination reaction, circulation tower reactor 1
Effectively carry out depth chlorination；It is segmented logical chlorine in tower, is diluted chlorine in high position effective use hydrogen chloride, reduces local chlorine
Concentration reduces dichloro phthalic anhydride generation probability；Utilization rate of equipment and installations is improved in the way of continuous production, continuous production reduces peace
Full blast danger.
Utilize the method for above equipment synthesis 4- chloride anhydride:
Comparative example:
In reaction kettle, 200 DEG C of temperature of the conduction oil control of 4000 kilograms of phthalic anhydrides and 4 kilograms of alchlors is first put into, it is even
Logical 1150 kilograms of the chlorine (1:0.6) of speed, reacts 8 hours；Reaction terminates, (the GC detection: 4- chloride anhydride of monitoring monochloro-benzene acid anhydride 35.2%
31.1%, 3- chloride anhydride 4.1%), 4,5- dichloro phthalic anhydrides 3.5%, phthalic anhydride 61.3%.
Embodiment 2:
A method of 4- chloride anhydride being prepared, as shown in Figure 1, passing through feeder for solid materials 19 for phthalic anhydride and 1 ‰ tri-chlorinations
Aluminium is continuously fed into phthalic anhydride dissolution kettle 8, keeps the temperature 150 DEG C, phthalic anhydride is constantly added to circulation tower reactor 1 by metering pump 14
In, 200 DEG C of temperature or so are controlled using the condenser 2 coupled on circulation tower reactor 1；The mass ratio of the material of phthalic anhydride and chlorine
For 1:0.8, two sections of logical chlorine is divided to enter tower circulation tower reactor 1, is 4 hours when empty, is brought out from circulation tower reactor 1
101 continuous output monochloro phthalic anhydrides of mouth, rectifying obtain 4- chloride anhydride；
3700 kilograms of reaction material liquid of full tower are first added, controls 190 DEG C of temperature, serialization is added 900 kgs/hour of phthalic anhydride
{ 0.1% weight ratio alchlor is wherein mixed in phthalic anhydride }, 345 kgs/hour of chlorine, successive reaction 24 hours；Product prison
Control, 4- chloride anhydride and 3- chloride anhydride total 65.5% (GC detection: 4- chloride anhydride 63.2%, 3- chloride anhydride 2.3%), 4,5- dichloros
Phthalic anhydride 0.2%, phthalic anhydride 34.2%.
Embodiment 3:
A method of 4- chloride anhydride being prepared, as shown in Figure 1, passing through feeder for solid materials 19 for phthalic anhydride and 1 ‰ tri-chlorinations
Aluminium is continuously fed into phthalic anhydride dissolution kettle 8, keeps the temperature 150 DEG C, phthalic anhydride is constantly added to circulation tower reactor 1 by metering pump 14
In, 200 DEG C of temperature or so are controlled using the condenser 2 coupled on circulation tower reactor 1；The mass ratio of the material of phthalic anhydride and chlorine
For 1:0.6, two sections of logical chlorine is divided to enter tower circulation tower reactor 1, is 4 hours when empty, is brought out from circulation tower reactor 1
101 continuous output monochloro phthalic anhydrides of mouth, rectifying obtain 4- chloride anhydride；
3700 kilograms of reaction material liquid of full tower are first added, controls 200 DEG C of temperature, serialization is added 900 kgs/hour of phthalic anhydride
{ 0.1% weight ratio alchlor is wherein mixed in phthalic anhydride }, 259 kgs/hour of chlorine, successive reaction 24 hours；Product prison
Control, 4- chloride anhydride and 3- chloride anhydride total 57.0% (GC detection: 4- chloride anhydride 55.2%, 3- chloride anhydride 1.8%), 4,5- dichloros
Phthalic anhydride 0.1%, phthalic anhydride 42.9%.
Embodiment 4:
A method of 4- chloride anhydride being prepared, as shown in Figure 1, phthalic anhydride is continuously fed into phthalic anhydride by feeder for solid materials 19
In dissolution kettle 8,150 DEG C are kept the temperature, phthalic anhydride is constantly added in circulation tower reactor 1 by metering pump 14, it is tower using circulation
The condenser 2 coupled on reactor 1 controls 200 DEG C of temperature or so；The mass ratio of the material of phthalic anhydride and chlorine is 1:0.8, is divided to two sections
Logical chlorine enters tower circulation tower reactor 1, is 4 hours when empty, from the continuous output of 1 upper end outlet of circulation tower reactor 101
Monochloro phthalic anhydride, rectifying obtain 4- chloride anhydride；
3700 kilograms of reaction material liquid of full tower are first added, controls 220 DEG C of temperature, serialization is added 900 kgs/hour of phthalic anhydride
{ 0.1% weight ratio alchlor is wherein mixed in phthalic anhydride }, 345 kgs/hour of chlorine, successive reaction 24 hours；Product prison
Control, 4- chloride anhydride and 3- chloride anhydride total 78.8% (GC detection: 4- chloride anhydride 75.8%, 3- chloride anhydride 2.5%), 4,5- dichloros
Phthalic anhydride 0.4%, phthalic anhydride 20.8%.
From comparative example and the present embodiment it is found that from intermittent reaction to continuous reaction: monochloro conversion ratio 35% is improved to >
57%；Dichloro phthalic anhydride is down to < 0.5% from 3%；Equipment investment rate decline 50%.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of equipment for preparing 4- chloride anhydride characterized by comprising circulation tower reactor (1)；Chlorine pot (5), passes through
First chlorination tube (6) and the second chlorination tube (7), which are segmented to the circulation tower reactor (1), leads to chlorine；Phthalic anhydride dissolution kettle
(8), it is fed by the circulation tower reactor (1) of feed pipe (9) Xiang Suoshu；Condenser (2) is arranged in circulation tower reactor
(1) on.
2. a kind of equipment for preparing 4- chloride anhydride according to claim 1, it is characterised in that: it further include phthalic anhydride tank (18),
The phthalic anhydride tank (18) is fed by the phthalic anhydride dissolution kettle (8) of feeder for solid materials (19) Xiang Suoshu.
3. a kind of equipment for preparing 4- chloride anhydride according to claim 1 or 2, it is characterised in that: the phthalic anhydride dissolution kettle
(8) blender (16) are provided on.
4. a kind of equipment for preparing 4- chloride anhydride according to claim 1, it is characterised in that: connect on the feed pipe (9)
It is connected to metering pump (14) and the first hopper (12), it is standby that the feed pipe (9) is also connected with first in parallel with metering pump (14)
With pipe (15), the feed pipe (9) is also connected with the spare pipe of second in parallel with the first hopper (12) (13).
5. a kind of equipment for preparing 4- chloride anhydride according to claim 1, it is characterised in that: first chlorination tube (6)
With the second hopper (10) are respectively connected on the second chlorination tube (7), on first chlorination tube (6) and the second chlorination tube (7) also
It is respectively connected with the spare pipe of the third in parallel with the second hopper (10) (11).
6. a kind of equipment for preparing 4- chloride anhydride according to claim 1, it is characterised in that: the phthalic anhydride dissolution kettle (8)
With thermometer (3) and pressure gauge (4) are provided on circulation tower reactor (1), be additionally provided on the phthalic anhydride dissolution kettle (8)
Liquidometer (17).
7. a kind of method for preparing 4- chloride anhydride, which is characterized in that specifically includes the following steps:
S1, the phthalic anhydride dissolved with catalyst is continuously fed into phthalic anhydride dissolution kettle (8), keeps the temperature 150-160 DEG C；
S2, the phthalic anhydride dissolved in step S1 is continuously fed into circulation tower reactor (1)；
S3, it is divided to two sections to be passed through chlorine into utilization circulation tower reactor (1)；
Condenser (2) the control temperature coupled on S4, circulation tower reactor (1), from circulation tower reactor (1) upper end outlet
(101) continuous output monochloro phthalic anhydride, rectifying obtain 4- chloride anhydride.
8. preparing the method for 4- chloride anhydride according to claim 7, it is characterised in that: catalyst is selected from ferric trichloride, three
One or more of aluminium chloride, ferrous sulfate, Eorontrifluoride etherate.
9. preparing the method for 4- chloride anhydride according to claim 7, it is characterised in that: phthalic anhydride is 1 with chlorine molar ratio:
0.5-0.8。
10. preparing the method for 4- chloride anhydride according to claim 8, it is characterised in that: catalyst charge is phthalic anhydride weight
The 0.1-0.25% of amount.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910545669.1A CN110229129B (en) | 2019-06-22 | 2019-06-22 | Equipment and method for preparing 4-chlorophthalic anhydride |
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|---|---|---|---|
| CN201910545669.1A CN110229129B (en) | 2019-06-22 | 2019-06-22 | Equipment and method for preparing 4-chlorophthalic anhydride |
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| CN110229129B CN110229129B (en) | 2023-07-25 |
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Cited By (1)
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| CN112079803A (en) * | 2020-09-11 | 2020-12-15 | 山东润科化工股份有限公司 | Synthesis method of 4-halogenated phthalic anhydride and derivatives thereof |
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| CN110229129B (en) | 2023-07-25 |
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