CN110124590A - A kind of production equipment and its technique of 3- chlorpromazine chloride - Google Patents
A kind of production equipment and its technique of 3- chlorpromazine chloride Download PDFInfo
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- CN110124590A CN110124590A CN201910545684.6A CN201910545684A CN110124590A CN 110124590 A CN110124590 A CN 110124590A CN 201910545684 A CN201910545684 A CN 201910545684A CN 110124590 A CN110124590 A CN 110124590A
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- tower section
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- reaction tower
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 78
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims abstract description 68
- 239000007788 liquid Substances 0.000 claims abstract description 65
- 239000007789 gas Substances 0.000 claims abstract description 54
- 239000006193 liquid solution Substances 0.000 claims abstract description 40
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 38
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 38
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 22
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 22
- QEYMMOKECZBKAC-UHFFFAOYSA-N 3-chloropropanoic acid Chemical compound OC(=O)CCCl QEYMMOKECZBKAC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000007259 addition reaction Methods 0.000 claims abstract description 11
- 238000005516 engineering process Methods 0.000 claims abstract description 10
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 36
- 239000012530 fluid Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000004064 recycling Methods 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 3
- 239000008246 gaseous mixture Substances 0.000 claims 1
- 239000006227 byproduct Substances 0.000 abstract description 7
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 238000005917 acylation reaction Methods 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 5
- 238000011144 upstream manufacturing Methods 0.000 abstract description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- -1 3- chloropropionic acid Phosphorus Chemical compound 0.000 description 3
- 239000000460 chlorine Substances 0.000 description 3
- 229910052801 chlorine Inorganic materials 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- 230000010933 acylation Effects 0.000 description 2
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- GAWAYYRQGQZKCR-UHFFFAOYSA-N 2-chloropropionic acid Chemical class CC(Cl)C(O)=O GAWAYYRQGQZKCR-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J10/00—Chemical processes in general for reacting liquid with gaseous media other than in the presence of solid particles, or apparatus specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J14/00—Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/347—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups
- C07C51/363—Preparation of carboxylic acids or their salts, halides or anhydrides by reactions not involving formation of carboxyl groups by introduction of halogen; by substitution of halogen atoms by other halogen atoms
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/60—Preparation of carboxylic acid halides by conversion of carboxylic acids or their anhydrides or esters, lactones, salts into halides with the same carboxylic acid part
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the production technologies and its equipment of a kind of 3- chlorpromazine chloride, belong to fine chemistry industry production field.A kind of production equipment of 3- chlorpromazine chloride, including reaction tower, the reaction tower includes top expansion area, gas liquid reaction tower section and the reactive liquid solution tower section of connection, and the gas liquid reaction tower section top is equipped with acrylic acid entrance, and the reactive liquid solution tower section top is equipped with thionyl chloride entrance;When practical operation, acrylic acid entrance is equipped on gas liquid reaction tower section top, acrylic acid is added, be equipped with thionyl chloride entrance on reactive liquid solution tower section top and thionyl chloride is added;The acrylic acid of hydrogen chloride upstream and gas-liquid reaction tower section flows down in a device; it carries out addition reaction and generates 3- chloropropionic acid; the acylation reaction of 3- chloropropionic acid and thionyl chloride generates 3- chlorpromazine chloride; without adding water; addition reaction can be completed; process flow is succinct, and the danger wastes in addition avoiding by-product phosphorous acid generate, and protects environment.
Description
Technical field
The present invention relates to the production technology of fine chemistry industry production technical field more particularly to a kind of 3- chlorpromazine chloride and its set
It is standby.
Background technique
3- chlorpromazine chloride is industrially mainly used for organic synthesis;Current production technology uses phosphorus trichloride method, uses water droplet
Add as in phosphorus trichloride, generates hydrogen chloride gas, by-product phosphorous acid;Concentrated hydrochloric acid is added in acrylic acid, is then passed through previous step again
Obtained hydrogen chloride gas;Gas liquid reaction obtains 3- chloropropionic acid, continuously reacts, then tri-chlorination is added dropwise into 3- chloropropionic acid
Phosphorus obtains 3- chlorpromazine chloride, by-product phosphorous acid;
In prior art, due to using reaction kettle to do gas liquid reaction, so gas residence time is short, it is necessary to add water, be made into
Hydrochloric acid could complete addition reaction, and process flow is cumbersome, in addition produce the danger wastes of by-product phosphorous acid, pollute environment.
Summary of the invention
The purpose of the present invention is to solve process flow in the prior art is cumbersome, the danger of by-product phosphorous acid is in addition produced
Dangerous waste, environmental pollution problem, and the production technology and its equipment of a kind of 3- chlorpromazine chloride proposed.
To achieve the goals above, present invention employs following technical solutions:
A kind of production equipment of 3- chlorpromazine chloride, including reaction tower, the reaction tower include the top expansion area of connection, gas
Liquid reaction tower section and reactive liquid solution tower section, the gas liquid reaction tower section top are equipped with acrylic acid entrance, the reactive liquid solution tower section
Top is equipped with thionyl chloride entrance.
Preferably, the reactive liquid solution tower section bottom is equipped with the circulating pump for the external circulation of material.
Preferably, the circulating pump feed end is connected to the bottom of the reactive liquid solution tower section by first pipe, described
Reactive liquid solution tower section is equipped with circulation fluid entrance, and the circulating pump discharge end is connected to circulation fluid inlet by second pipe,
The second pipe is equipped with the discharge nozzle with regulating valve.
Preferably, the second pipe is equipped with external heat exchanger.
Preferably, the external heat exchanger uses tube-type graphite heat exchanger or block hole-type graphite heat exchanger.
Preferably, the acrylic acid inlet is equipped with propylene acid spreader, and the thionyl chloride inlet is equipped with protochloride
Sulfone distributor, the circulation fluid inlet are equipped with recycle liquid distributor.
Preferably, the gas liquid reaction tower section and reactive liquid solution Ta Jienei are equipped with filler.
Preferably, top expansion area is equipped with sulfur dioxide (SO2) emissions mouth.
Preferably, the reaction tower is cased with collet.
A kind of production technology of 3- chlorpromazine chloride, comprising the following steps:
S1, it is equipped with acrylic acid entrance addition acrylic acid on gas liquid reaction tower section top, is equipped on reactive liquid solution tower section top
Thionyl chloride is added in thionyl chloride entrance;
S2, the continuous generation hydrogen chloride of reaction tower bottom liquid liquid reaction tower section reaction and sulfur dioxide mixture gas, mixing
Gas is upper;
The acrylic acid gas liquid reaction that hydrogen chloride in S3, the upper gas mixed enters with gas liquid reaction tower section top completes
Double bond addition reaction obtains 3- chloropropionic acid;
S4, it reacts with thionyl chloride to generate in the 3- chloropropionic acid that reactive liquid solution tower section generates and obtains 3- chlorpromazine chloride, simultaneously
The hydrogen chloride and sulfur dioxide mixture gas for generating step S2 carry out recycling continuous reaction;
S5, production 3- chlorpromazine chloride discharge from reactive liquid solution area, while liquid flow is sent as an envoy to obtain gas-liquid reaction tower section top
The acrylic acid being added equipped with acrylic acid entrance constantly walks downward, and adequately reacts with the hydrogen chloride in upper mixed gas.
Compared with prior art, the present invention provides the production technology and its equipment of a kind of 3- chlorpromazine chloride, have following
The utility model has the advantages that
1, the production technology and its equipment of the 3- chlorpromazine chloride is 3- chloropropionic acid by acrylic acid and the addition of hydrogen chloride elder generation,
Then 3- chlorpromazine chloride is obtained with thionyl chloride acylation again;Acrylic acid is equipped with acrylic acid entrance from the gas liquid reaction tower section top of tower
Charging, into gas liquid reaction tower section, reactive liquid solution tower section top is equipped with thionyl chloride entrance and thionyl chloride is added, and bottom liquid liquid is anti-
The third of the mixed gas of hydrogen chloride and sulfur dioxide that Ying Tajie reaction production is gone up, hydrogen chloride upstream and gas-liquid reaction tower section
Olefin(e) acid flows down, progress addition reaction generation 3- chloropropionic acid, and the acylation reaction of 3- chloropropionic acid and thionyl chloride generates 3- chlorpromazine chloride,
Without adding water, addition reaction can be completed, process flow is succinct, and by recycling continuous reaction, in addition high production efficiency avoids
The danger wastes of by-product phosphorous acid generate, and protect environment.
Detailed description of the invention
Fig. 1 is a kind of production technology of 3- chlorpromazine chloride proposed by the present invention and its structural schematic diagram of equipment.
In figure: 1, top expansion area;2, gas liquid reaction tower section;3, reactive liquid solution tower section;4, filler;5, acrylic acid entrance;
6, thionyl chloride entrance;7, circulation fluid entrance;8, circulating pump;9, regulating valve;10, sulfur dioxide (SO2) emissions mouth;11, external heat exchange
Device.
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 be not considered as limiting the invention.
Referring to Fig.1, a kind of production equipment of 3- chlorpromazine chloride, including reaction tower, reaction tower include that the top of connection expands
Area 1, gas liquid reaction tower section 2 and reactive liquid solution tower section 3,2 top of gas liquid reaction tower section are equipped with acrylic acid entrance 5, reactive liquid solution tower
3 tops are saved equipped with thionyl chloride entrance 6;
It is 3- chloropropionic acid by acrylic acid and the addition of hydrogen chloride elder generation, then obtains 3- chlorine propionyl with thionyl chloride acylation again
Chlorine;Acrylic acid is fed from 2 top of gas liquid reaction tower section of tower equipped with acrylic acid entrance 5, and into gas liquid reaction tower section 2, liquid liquid is anti-
3 top Ying Tajie is equipped with thionyl chloride entrance 6 and thionyl chloride is added, and the chlorine come is gone up in the reaction production of bottom liquid liquid reaction tower section 3
The acrylic acid of the mixed gas of change hydrogen and sulfur dioxide, hydrogen chloride upstream and gas-liquid reaction tower section 2 flows down, and it is raw to carry out addition reaction
At 3- chloropropionic acid, the acylation reaction of 3- chloropropionic acid and thionyl chloride generates 3- chlorpromazine chloride, and without adding water, it is anti-that addition can be completed
It answers, process flow is succinct, and by recycling continuous reaction, in addition high production efficiency avoids the dangerous waste of by-product phosphorous acid
Object generates, and protects environment.
3 bottom of reactive liquid solution tower section is equipped with the circulating pump 8 for the external circulation of material;8 feed end of circulating pump passes through first
Pipeline is connected to the bottom of reactive liquid solution tower section 3, and reactive liquid solution tower section 3 is equipped with circulation fluid entrance 7, and 8 discharge end of circulating pump is logical
It crosses second pipe to be connected at circulation fluid entrance 7, second pipe is equipped with the discharge nozzle with regulating valve 9;It is set on second pipe
There is external heat exchanger 11;External heat exchanger 11 uses tube-type graphite heat exchanger or block hole-type graphite heat exchanger, with external circulation
Final 8's system circulation and mixed heat transfer are pumped, the reaction of thionyl chloride and 3- chloropropionic acid is completed.And generate hydrogen chloride and sulfur dioxide
Gas.
The circulating pump 8 of bottom one realizes the external circulation of material, reinforces the reactive liquid solution of thionyl chloride and 3- chloropropionic acid,
Reaction heat is taken away by external heat exchanger 11, reactive liquid solution is more abundant;
There can be radar level gauge on reaction tower top, monitor the whole liquid level of tower;
Outlet for product discharge nozzle controls to adjust 9 aperture of valve by the liquid level of tower using the regulating valve 9 of lining tetrafluoro.
It is equipped with propylene acid spreader at acrylic acid entrance 5, thionyl chloride distributor, circulation are equipped at thionyl chloride entrance 6
Recycle liquid distributor is equipped at liquid entrance 7;
The gas-liquid separation zone size in top expansion area 1, diameter 600-1000mm, height: corrosion resistant is arranged at the top 800-1200mm
The demister of erosion;
The middle part gas liquid reaction area of gas liquid reaction tower section 2: diameter 400-600mm, height: 4000-8000mm;
The filler 4 of gas liquid reaction tower section 2 and reactive liquid solution tower section 3 uses polytetrafluoroethylene (PTFE) structured packing, is divided into 4-5 sections,
The height of each section of filler is 1.2-1.5 times of tower internal diameter;The redistributor of polytetrafluoroethylene (PTFE) is set between each section, it is more uniform
Adequately reaction;
The reactive liquid solution area of reactive liquid solution tower section 3, diameter 600-1000mm, height 800-1200mm;
Circulating pump 8 uses flow 2-5m3/h, lift 15-30m;Use lining teflon centrifugal pump or magnetic drive pump;
External heat exchanger 11 uses tube-type graphite heat exchanger or block hole-type graphite heat exchanger, the heat-transfer surface of heat exchanger
Product is 10-30 square metres.
It is equipped with filler 4 in gas liquid reaction tower section 2 and reactive liquid solution tower section 3, so that reaction more ingredient.
Top expansion area 1 is equipped with sulfur dioxide (SO2) emissions mouth 10, convenient for discharging and collecting sulfur dioxide.
Reaction tower is cased with collet;Addition reaction has heat release, takes away reaction heat by the collet of reaction tower, maintains reaction
Temperature, 13 DEG C of acrylic acid fusing point, so reaction tower all uses collet, in winter when collet heat, it is ensured that acrylic acid is liquid.
A kind of production technology of 3- chlorpromazine chloride, comprising the following steps:
S1, acrylic acid entrance 5 is equipped with by metering pump addition acrylic acid, in reactive liquid solution on 2 top of gas liquid reaction tower section
3 top of tower section is equipped with thionyl chloride entrance 6 and thionyl chloride is added;
S2, reaction tower bottom liquid liquid reaction tower section 3 react continuous and generate hydrogen chloride and sulfur dioxide mixture gas, mixing
Gas is upper;
The acrylic acid gas liquid reaction that S3, the hydrogen chloride in the upper gas mixed and 2 top of gas liquid reaction tower section enter is completed
Double bond addition reaction obtains 3- chloropropionic acid;
S4, it reacts with thionyl chloride to generate in the 3- chloropropionic acid that reactive liquid solution tower section 3 generates and obtains 3- chlorpromazine chloride, simultaneously
The hydrogen chloride and sulfur dioxide mixture gas for generating step S2 carry out recycling continuous reaction;
S5, production 3- chlorpromazine chloride discharge from reactive liquid solution area, while liquid flow is sent as an envoy to obtain 2 top of gas-liquid reaction tower section
The acrylic acid being added equipped with acrylic acid entrance 5 constantly walks downward, and adequately reacts with the hydrogen chloride in upper mixed gas.
The whole residence time is calculated according to liquid:
The gas liquid reaction area of gas liquid reaction tower section 2: 4-5 hours;
The reactive liquid solution area of reactive liquid solution tower section 3: 2-3 hours;
70-80 DEG C of temperature of gas liquid reaction area;
60-70 DEG C of temperature of reactive liquid solution area;
Reaction pressure: synthesis under normal pressure;
The charging rate of acrylic acid are as follows: 100-300kg/h;
The charging rate of thionyl chloride are as follows: 150-400kg/h;
The gas-liquid mixed of tower adverse current is realized, the addition reaction of acrylic acid and hydrogen chloride is very sufficiently and complete, whole
Water is avoided in a technique;It is found in afterbody sample detection, the content of 3 chloropropionic acids has been over 90%;Due to reducing
The dosage of water, the dosage of thionyl chloride is also substantially close to theoretical value.
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 production equipment of 3- chlorpromazine chloride, which is characterized in that including reaction tower, the reaction tower includes the top of connection
Expand area (1), gas liquid reaction tower section (2) and reactive liquid solution tower section (3), the gas liquid reaction tower section (2) top is equipped with acrylic acid
Entrance (5), the reactive liquid solution tower section (3) top are equipped with thionyl chloride entrance (6).
2. the production equipment of 3- chlorpromazine chloride according to claim 1, which is characterized in that the reactive liquid solution tower section (3)
Bottom is equipped with the circulating pump (8) for the external circulation of material.
3. the production equipment of 3- chlorpromazine chloride according to claim 2, which is characterized in that circulating pump (8) feed end
The bottom of the reactive liquid solution tower section (3) is connected to by first pipe, the reactive liquid solution tower section (3) enters equipped with circulation fluid
Mouth (7), circulating pump (8) discharge end are connected at circulation fluid entrance (7) by second pipe, and the second pipe is equipped with
Discharge nozzle with regulating valve (9).
4. the production equipment of 3- chlorpromazine chloride according to claim 3, which is characterized in that the second pipe is equipped with outer
Set heat exchanger (11).
5. the production equipment of 3- chlorpromazine chloride according to claim 4, which is characterized in that the external heat exchanger (11) is adopted
With tube-type graphite heat exchanger or block hole-type graphite heat exchanger.
6. the production equipment of 3- chlorpromazine chloride according to claim 3, which is characterized in that at the acrylic acid entrance (5)
Equipped with propylene acid spreader, thionyl chloride distributor is equipped at the thionyl chloride entrance (6), at the circulation fluid entrance (7)
Equipped with recycle liquid distributor.
7. the production equipment of 3- chlorpromazine chloride according to claim 1, which is characterized in that the gas liquid reaction tower section (2)
With reactive liquid solution tower section (3) in be equipped with filler (4).
8. the production equipment of 3- chlorpromazine chloride according to claim 1-7, which is characterized in that the top expands
Area (1) is equipped with sulfur dioxide (SO2) emissions mouth (10).
9. the production equipment of 3- chlorpromazine chloride according to claim 1-7, which is characterized in that the reaction tower set
There is collet.
10. a kind of production technology of 3- chlorpromazine chloride, which comprises the following steps:
S1, it is equipped with acrylic acid entrance (5) addition acrylic acid on gas liquid reaction tower section (2) top, on reactive liquid solution tower section (3) top
Thionyl chloride is added equipped with thionyl chloride entrance (6);
S2, the continuous generation hydrogen chloride of reaction tower bottom liquid liquid reaction tower section (3) reaction and sulfur dioxide mixture gas, gaseous mixture
Body is upper;
The acrylic acid gas liquid reaction that hydrogen chloride in S3, the upper gas mixed enters with gas liquid reaction tower section (2) top completes
Double bond addition reaction obtains 3- chloropropionic acid;
S4, react with thionyl chloride to generate in the 3- chloropropionic acid that reactive liquid solution tower section (3) generates and obtain 3- chlorpromazine chloride, give birth to simultaneously
At the hydrogen chloride and sulfur dioxide mixture gas of step S2, carry out recycling continuous reaction;
S5, production 3- chlorpromazine chloride from reactive liquid solution area discharge, while liquid flow send as an envoy to gas-liquid reaction tower section (2) top is set
The acrylic acid for having acrylic acid entrance (5) to be added constantly walks downward, and adequately reacts with the hydrogen chloride in upper mixed gas.
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Cited By (1)
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CN112759513A (en) * | 2021-01-07 | 2021-05-07 | 郑州大学 | Preparation method of 3-chloropropionyl chloride |
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CN112759513A (en) * | 2021-01-07 | 2021-05-07 | 郑州大学 | Preparation method of 3-chloropropionyl chloride |
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