CN209052602U - A kind of chloroacetic device of differential circulation continuous production - Google Patents
A kind of chloroacetic device of differential circulation continuous production Download PDFInfo
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- CN209052602U CN209052602U CN201821769473.8U CN201821769473U CN209052602U CN 209052602 U CN209052602 U CN 209052602U CN 201821769473 U CN201821769473 U CN 201821769473U CN 209052602 U CN209052602 U CN 209052602U
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Abstract
The utility model provides a kind of chloroacetic device of differential circulation continuous production, including main reactor, pre-reactor, separator, circulating pump, first-stage condenser, secondary condenser, demister, discharging pump, pipeline and automatic instrument(s), the main reactor is that tubular type microchannel plate answers heat exchanger, it is internally provided with several microchannels, it is with multiple longitudinal main reactor tube sides and multiple lateral main reactor shell sides, the main reactor cooling water inlet and main reactor cooling water outlet of main reactor shell side connection main reactor two sides, the main reactor bottom is provided with gas-liquid mixed room, the utility model is compared with traditional technology, eliminate hydrogenation-dechlorination equipment and attached hydrogen chloride absorption device, reduce equipment investment cost, reduce the generation of polychloride in chlorated liquid by differential circle flow process, improve chloroacetic life Produce efficiency and quality.
Description
Technical field
The utility model relates to field of fine chemical more particularly to a kind of chloroacetic devices of differential circulation continuous production.
Background technique
Monoxone is the important source material and intermediate of organic synthesis, is occupied significantly in chlorine products and acetic acid derivative
Position.Monoxone contains-Cl and two important functional groups of-COOH, and Cl is replaced by groups such as F, Br, I, NH2, CN, SH, OH respectively
After can form a variety of chemical products, can be widely used for the industries such as medicine, dyeing and finishing, pesticide, papermaking, oil field.
Monoxone synthetic method is numerous, but is mainly acetic acid chlorination catalysis method in heavy industrialization.According to catalyst
Difference is divided into sulfur catalyst method and acetic anhydride catalyst method.
For sulfur catalyst method using chlorine and acetic acid as substrate, sulphur is catalyst, generates monoxone.Often lead in industrial production
One secondary reacting kettle of series connection is realized after crossing main reaction kettle, obtains chlorated liquid, secondary reacting kettle after chlorine acetic acid reaction in main reaction kettle
For absorbing the complete chlorine of unreacted, to improve the utilization rate of raw material.In chlorated liquid other than principal product chloroacetic acid, there are also two
Chloro, three chloro-products, chloroacetic chloride and the complete glacial acetic acid of unreacted, need to be purified by crystallisation.It is industrialized at present
Sulfur catalyst method is batch production technique, and simple process, flexible operation, equipment investment are few, but consumption of raw materials is high, production week
Phase is long, at high cost, seriously polluted.
For acetic anhydride catalyst method using chlorine and acetic acid as substrate, aceticanhydride is catalyst, generates monoxone.Current industrialized aceticanhydride
Catalysis method can be divided into batch production technique and two kinds of continous way production technology.
Switzerland's Sulzer patent uses batch production technique, and dynamic fusion crystallization technique is used in crystallization process, produces
Product purity can reach 99% or more, but still have the largely mother liquor generation containing various by-products.
Dutch Akzo Nobel N.V. has developed continous way production technology.Different from chlorination in batch production technique,
Independent reactions kettle, the Akzo Nobel N.V. such as crystallization form flow reactor.Chlorated liquid, will through palladium carbon catalysis selective hydrogenation
Dichloro-, three chloro-products are reduced to monoxone and glacial acetic acid, then rectification and purification, last cooling junction plate.Continous way produces work
The purification process that hydrogenating reduction and rectifying combine in skill is generated instead of the crystallization in batch production technique without mother liquor,
But reacting the generation heavy constituents such as acetaldehyde and chloroacetaldehyde with hydrogen due to chloracetyl and chloracetyl chloride before hydrogenating reduction is also pollution
Object.I.e. Dutch Akzo Nobel N.V.'s technique has automation advantage, but equipment investment is big, and high production cost does not have yet
Eliminate pollution.
Currently, under the new demand of " efficiency multiplication, sustainable economic development ", need it is a kind of it is novel " energy conservation, consumption reduction,
The production of chloroacetic acid method of environmental protection ".
Utility model content
The purpose of this utility model is to provide a kind of chloroacetic devices of differential circulation continuous production, to solve above-mentioned set
Standby investment is big, it is at high cost to produce, has the technical issues of environmental pollution.
The utility model using following technical scheme in order to solve the above technical problems, realized:
A kind of chloroacetic device of differential circulation continuous production, including main reactor, pre-reactor, separator, circulating pump,
First-stage condenser, secondary condenser, demister, discharging pump, distillation system and pipeline and automatic instrument(s), the main reactor are
Tubular type microchannel plate answers heat exchanger, main with multiple longitudinal main reactor tube sides and multiple lateral main reactor shell sides
Reactor shell side both ends are separately connected the main reactor cooling water inlet and main reactor cooling water outlet of main reactor two sides, institute
It states main reactor bottom and is provided with gas-liquid mixed room, gas-liquid mixed room bottom offers main reactor gas access, side
It offers main reactor liquid inlet, is equipped with efficient mixed structure body in the gas-liquid mixed room, on the main reactor tube side
Lower both ends are separately connected main reactor discharge port and gas-liquid mixing chamber at the top of main reactor；
The pre-reactor is that tubular type microchannel plate answers heat exchanger, with multiple longitudinal pre-reactor tube sides and multiple
Lateral pre-reactor shell side, pre-reactor shell side both ends be separately connected the pre-reactor cooling waters of pre-reactor two sides into
Mouth and pre-reactor cooling water outlet, the pre-reactor bottom are equipped with pre-reactor mixing chamber, pre-reactor mixing chamber bottom
Equipped with pre-reactor mixture export, side is equipped with pre-reactor gas access, is equipped with pre-reactor in the middle part of pre-reactor and recycles
Room, pre-reactor recovery room are equipped with aceticanhydride feed opening, are equipped with pre-reactor discharge chamber, pre-reactor discharge chamber at the top of pre-reactor
Side is equipped with acetic acid feed opening, and top is equipped with pre-reactor discharge port, pre-reactor tube side connection pre-reactor mixing chamber,
Pre-reactor recovery room and pre-reactor discharge chamber.
Preferably, being filled with microchannel ceramic packing in the main reactor tube side and pre-reactor shell side, this is micro-
Channel ceramic packing diameter be 8~100mm, main reactor tube side diameter be 10~110mm, pre-reactor tube side diameter be 8~
Aluminium oxide honeycomb ceramic packing is equipped with inside 120mm, main reactor and pre-reactor.
Preferably, the microchannel ceramic packing diameter be 14~64mm, main reactor tube side diameter be 15~
65mm, pre-reactor tube side diameter are 30~100mm.
Preferably, the main body of the main reactor and pre-reactor is by titanium alloy, impregnated graphite, carbon steel, carbonization
The one or more of silicon are made, and the shell of main reactor and pre-reactor is carbon steel.
Preferably, the separator is jacketed enamelled vessel, top is equipped with separator entry to mixed solution and divides
From device gas vent, bottom is equipped with separator liquid outlet, which connects main reactor discharge port, this point
Pre-reactor gas access is connected from device gas vent, which is equipped with circulating pump and discharging pump, and circulating pump connects
Main reactor liquid inlet is connect, discharging pump connects distillation system.
Preferably, the entrance of the pre-reactor discharge port connection first-stage condenser, the outlet connection of first-stage condenser
The entrance of secondary condenser, the entrance of the entrance connection demister of secondary condenser, the outlet of demister connects lower process, described
First-stage condenser, secondary condenser, demister are equipped with reflux line, which converges with pre-reactor mixture export
After connect circulating pump.
Above-mentioned technique controls chlorated liquid by circulating pump and reacts in the microchannel of main reactor with chlorine, and gas-liquid sufficiently connects
Touching, increases its residence time, while controlling the temperature of reaction process, evades depth chlorination generation, can be referred to as differential circulation skill
Art.
The beneficial effects of the utility model are:
(1) low equipment investment:
Due to reducing the generation of polychloride in chlorated liquid by differential circle flow process, compared with traditional technology,
Hydrogenated dechlorination process and equipment are eliminated, attached hydrogen chloride absorption device is eliminated, reduces integral device investment.
(2) production cost is low:
Since there is no hydrogenated dechlorination process, the use of expensive palladium-carbon catalyst is eliminated；Due to this technique chlorination reaction
Selectivity improve (dichloroacetic acid production quantity is extremely low), no rectifying heavy constituent raffinate generates, and the rate of recovery of product increases substantially；
Using hydrogen chloride tail gas purified treatment, chloroacetic chloride " escape " is greatly reduced, while to aceticanhydride in pre-reactor and distillation system
Recycling and reusing is carried out with chloroacetic chloride.
(3) high production efficiency, good product quality:
Due to making that continuous production is integrally formed by differential circle flow process, reaction efficiency is substantially increased, and then improve
Subsequent chloroacetic generating rate improves production efficiency, while reducing the generation of by-product, guarantees product quality.
(4) environmentally protective:
Since there is no hydrogenated dechlorination process, hydrogen feedstock major hazard source is not present；Heavy constituent raffinate is not generated.It does not use
Method for crystallising, there is no mother liquors difficult to degrade in monoxone and dichloroacetic acid separation；The high-purity hydrogen chloride that tail gas generates can be used for giving birth to
Give birth to trip hydrogen chloride product.Prior art is compared, entire production process no three wastes generates, is automatically cleaning chemical industry skill, reaches circulation
Economic aim.
Detailed description of the invention
Fig. 1 is the structure flow chart of the utility model entirety；
Fig. 2 is the structural schematic diagram of the utility model main reactor；
Fig. 3 is the structural schematic diagram of the utility model pre-reactor.
In figure: 1 main reactor, 101 main reactor cooling water inlets, 102 main reactor cooling water outlets, 103 main reactions
Device gas access, 104 main reactor liquid inlets, 105 main reactor discharge ports, 106 efficient mixed structure bodies, 107 gas-liquids are mixed
Close room, 108 main reactor tube sides, 109 main reactor shell sides, 2 circulating pumps, 3 pre-reactors, 301 pre-reactor mixture exports,
302 pre-reactor discharge ports, 303 aceticanhydride feed openings, 304 acetic acid feed openings, 305 pre-reactor gas accesses, 306 pre-reactions
Device tube side, 307 pre-reactor shell sides, 308 pre-reactor cooling water inlets, 309 pre-reactor cooling water outlets, 310 pre-reactions
Device mixing chamber, 311 pre-reactor recovery rooms, 312 pre-reactor discharge chambers, 4 separators, 401 separator entry to mixed solution, 402
Separator gas outlet, 403 separator liquid outlets, 5 discharging pumps, 6 first-stage condensers, 7 secondary condensers, 8 demisters, 9 essences
Evaporate system, 10 shells, 11 microchannel ceramic packings, aluminium oxide honeycomb ceramic packing.
Specific embodiment
In order to be easy to understand the technical means, creative features, achievement of purpose, and effectiveness of the utility model, under
In conjunction with specific embodiments, the utility model is further described, but following embodiments are only the preferred implementation of the utility model in face
Example, and it is not all.Based on the implementation example in the implementation mode, those skilled in the art are without making creative work
Obtained other embodiments, belong to the protection scope of the utility model.Experimental method in following embodiments, such as without special theory
It is bright, it is conventional method, the materials, reagents and the like used in the following examples commercially obtains unless otherwise specified
It arrives.
A kind of chloroacetic device of differential circulation continuous production, including main reactor 1, pre-reactor 3, separator 4, circulation
Pump 2, first-stage condenser 6, secondary condenser 7, demister 8, discharging pump 5, distillation system 9 and pipeline and automatic instrument(s), it is described
Main reactor 1 is that tubular type microchannel plate answers heat exchanger, with multiple longitudinal main reactor tube sides 108 and multiple lateral masters
Reactor shell side 109,109 both ends of main reactor shell side are separately connected the main reactor cooling water inlet 101 of 1 two sides of main reactor
With main reactor cooling water outlet 102,1 bottom of main reactor is provided with gas-liquid mixed room 107, the gas-liquid mixed room
107 bottoms offer main reactor gas access 103, and side offers main reactor liquid inlet 104, the gas-liquid mixed room
Efficient mixed structure body 106 is equipped in 107,108 upper and lower ends of main reactor tube side are separately connected 1 top of main reactor
Main reactor discharge port 105 and gas-liquid mixing chamber 107；
The pre-reactor 3 is that tubular type microchannel plate answers heat exchanger, with multiple longitudinal pre-reactor tube sides 306
With multiple lateral pre-reactor shell sides 307,307 both ends of pre-reactor shell side are separately connected the pre- of 3 two sides of pre-reactor
Reactor cooling water import 308 and pre-reactor cooling water outlet 309,3 bottom of pre-reactor are mixed equipped with pre-reactor
Room 310,310 bottom of pre-reactor mixing chamber are equipped with pre-reactor mixture export 301, and side is equipped with pre-reactor gas access
305, pre-reactor recovery room 311 is equipped in the middle part of pre-reactor 3, pre-reactor recovery room 311 is equipped with aceticanhydride feed opening 303, in advance
Pre-reactor discharge chamber 312 is equipped at the top of reactor 3,312 side of pre-reactor discharge chamber is equipped with acetic acid feed opening 304, top
Equipped with pre-reactor discharge port 302, the pre-reactor tube side 306 connects pre-reactor mixing chamber 310, pre-reactor recovery room
311 and pre-reactor discharge chamber 312.
Wherein, it is filled with microchannel ceramic packing 11 in the main reactor tube side 108 and pre-reactor tube side 306,
The microchannel ceramic packing diameter is 8~100mm, and 108 diameter of main reactor tube side is 10~110mm, pre-reactor tube side 306
Diameter is 8~120mm, is equipped with aluminium oxide honeycomb ceramic packing 12 inside main reactor 1 and pre-reactor 3.
Further, 11 diameter of microchannel ceramic packing be 14~64mm, 108 diameter of main reactor tube side be 15~
65mm, pre-reactor tube side diameter are 30~100mm.
Wherein, the main body of the main reactor 1 and pre-reactor 3 is by titanium alloy, impregnated graphite, carbon steel, silicon carbide
One or more be made, the shell 10 of main reactor 1 and pre-reactor 3 is carbon steel.
Wherein, the separator 4 is jacketed enamelled vessel, and top is equipped with separator entry to mixed solution 401 and divides
From device gas vent 402, bottom is equipped with separator liquid outlet 403, which connects main reactor
Discharge port 105,402 connection pre-reactor gas access 305 of separator gas outlet, the separator liquid outlet 403 are equipped with
Circulating pump 2 and discharging pump 5, circulating pump 2 connect main reactor liquid inlet 104, and discharging pump 5 connects distillation system 9.
Wherein, the pre-reactor discharge port 302 connects the entrance of first-stage condenser 6, the outlet connection of first-stage condenser 6
The entrance of secondary condenser 7, the entrance of the entrance connection demister 8 of secondary condenser 7, the outlet of demister 8 connects lower work
Sequence, the first-stage condenser 6, secondary condenser 7, demister 8 are equipped with reflux line, which mixes with pre-reactor
Liquid outlet 301 connects circulating pump 2 after converging.
Basic principles, main features, and advantages of the present invention has been shown and described above.Current row
The technical staff of industry is described in above embodiments and description it should be appreciated that the present utility model is not limited to the above embodiments
Be only the utility model preference, be not intended to limit the utility model, do not departing from the spirit and scope of the utility model
Under the premise of, the utility model also has various changes and improvements, these changes and improvements both fall within claimed it is practical
In novel range.The protection scope of the present invention is defined by the appended claims and their equivalents.
Claims (6)
1. a kind of chloroacetic device of differential circulation continuous production, including main reactor, pre-reactor, separator, circulating pump, one
Grade condenser, secondary condenser, demister, discharging pump, distillation system and pipeline and automatic instrument(s), it is characterised in that: described
Main reactor is that tubular type microchannel plate answers heat exchanger, with multiple longitudinal main reactor tube sides and multiple lateral main reactions
Device shell side, main reactor shell side both ends are separately connected main reactor cooling water inlet and the main reactor cooling of main reactor two sides
Water out, the main reactor bottom are provided with gas-liquid mixed room, and gas-liquid mixed room bottom offers main reactor gas
Entrance, side offer main reactor liquid inlet, are equipped with efficient mixed structure body, the main reaction in the gas-liquid mixed room
Device tube side upper and lower ends are separately connected main reactor discharge port and gas-liquid mixing chamber at the top of main reactor；
The pre-reactor is that tubular type microchannel plate answers heat exchanger, with multiple longitudinal pre-reactor tube sides and multiple transverse directions
Pre-reactor shell side, pre-reactor shell side both ends be separately connected pre-reactor two sides pre-reactor cooling water inlet and
Pre-reactor cooling water outlet, the pre-reactor bottom are equipped with pre-reactor mixing chamber, and pre-reactor mixing chamber bottom is equipped with
Pre-reactor mixture export, side are equipped with pre-reactor gas access, are equipped with pre-reactor recovery room in the middle part of pre-reactor, in advance
Reactor recovery room is equipped with aceticanhydride feed opening, is equipped with pre-reactor discharge chamber, pre-reactor discharge chamber side at the top of pre-reactor
Equipped with acetic acid feed opening, top is equipped with pre-reactor discharge port, the pre-reactor tube side connection pre-reactor mixing chamber, pre- anti-
Answer device recovery room and pre-reactor discharge chamber.
2. a kind of chloroacetic device of differential circulation continuous production according to claim 1, it is characterised in that: the master is anti-
It answers in device tube side and pre-reactor shell side filled with microchannel ceramic packing, which is 8~
100mm, main reactor tube side diameter are 10~110mm, and pre-reactor tube side diameter is 8~120mm, main reactor and pre-reaction
Aluminium oxide honeycomb ceramic packing is equipped with inside device.
3. a kind of chloroacetic device of differential circulation continuous production according to claim 2, it is characterised in that: described micro- logical
Road ceramic packing diameter be 14~64mm, main reactor tube side diameter be 15~65mm, pre-reactor tube side diameter be 30~
100mm。
4. a kind of chloroacetic device of differential circulation continuous production according to claim 1, it is characterised in that: the master is anti-
Answer the main body of device and pre-reactor by being made of the one or more of titanium alloy, impregnated graphite, carbon steel, silicon carbide, main reaction
The shell of device and pre-reactor is carbon steel.
5. a kind of chloroacetic device of differential circulation continuous production according to claim 1, it is characterised in that: the separation
Device is jacketed enamelled vessel, and top is equipped with separator entry to mixed solution and separator gas exports, and bottom is equipped with separation
Device liquid outlet, the separator entry to mixed solution connect main reactor discharge port, separator gas outlet connection pre-reactor
Gas access, the separator liquid outlet are equipped with circulating pump and discharging pump, and circulating pump connects main reactor liquid inlet, discharging pump
Connect distillation system.
6. a kind of chloroacetic device of differential circulation continuous production according to claim 1, it is characterised in that: described pre- anti-
Answer the entrance of device discharge port connection first-stage condenser, the entrance of the outlet connection secondary condenser of first-stage condenser, B-grade condensation
The entrance of the entrance connection demister of device, the outlet of demister connect lower process, and the first-stage condenser, is removed secondary condenser
Day with fog is equipped with reflux line, which connects circulating pump after converging with pre-reactor mixture export.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201821769473.8U CN209052602U (en) | 2018-10-30 | 2018-10-30 | A kind of chloroacetic device of differential circulation continuous production |
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| CN201821769473.8U CN209052602U (en) | 2018-10-30 | 2018-10-30 | A kind of chloroacetic device of differential circulation continuous production |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU211529U1 (en) * | 2021-09-17 | 2022-06-10 | Общество с ограниченной ответственностью "Базис" | Device for chlorination of acetic acid |
-
2018
- 2018-10-30 CN CN201821769473.8U patent/CN209052602U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU211529U1 (en) * | 2021-09-17 | 2022-06-10 | Общество с ограниченной ответственностью "Базис" | Device for chlorination of acetic acid |
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| GR01 | Patent grant | ||
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| CB03 | Change of inventor or designer information |
Inventor after: Qiu Zhenzhong Inventor after: Wang Meizhen Inventor after: Wang Zhenhua Inventor before: Qiu Zhenzhong Inventor before: Wang Meizhen Inventor before: Wang Zhenhua |