CN116836048A - Production process of high-purity trichloroacetone - Google Patents
Production process of high-purity trichloroacetone Download PDFInfo
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- CN116836048A CN116836048A CN202310615223.8A CN202310615223A CN116836048A CN 116836048 A CN116836048 A CN 116836048A CN 202310615223 A CN202310615223 A CN 202310615223A CN 116836048 A CN116836048 A CN 116836048A
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- trichloroacetone
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- purity
- chlorine
- reaction
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- SMZHKGXSEAGRTI-UHFFFAOYSA-N 1,1,1-trichloropropan-2-one Chemical compound CC(=O)C(Cl)(Cl)Cl SMZHKGXSEAGRTI-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 37
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000000460 chlorine Substances 0.000 claims abstract description 35
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 35
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 34
- CSVFWMMPUJDVKH-UHFFFAOYSA-N 1,1-dichloropropan-2-one Chemical compound CC(=O)C(Cl)Cl CSVFWMMPUJDVKH-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 238000002425 crystallisation Methods 0.000 claims abstract description 24
- 230000008025 crystallization Effects 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000005086 pumping Methods 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000013078 crystal Substances 0.000 claims abstract description 4
- BULLHNJGPPOUOX-UHFFFAOYSA-N chloroacetone Chemical compound CC(=O)CCl BULLHNJGPPOUOX-UHFFFAOYSA-N 0.000 claims description 17
- 238000004821 distillation Methods 0.000 claims description 15
- 239000007789 gas Substances 0.000 claims description 10
- 239000007791 liquid phase Substances 0.000 claims description 10
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 239000000498 cooling water Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 5
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 5
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 5
- 125000004122 cyclic group Chemical group 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 3
- 239000012452 mother liquor Substances 0.000 claims description 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims 1
- 238000007086 side reaction Methods 0.000 abstract description 5
- 238000000746 purification Methods 0.000 abstract description 4
- OVBPIULPVIDEAO-LBPRGKRZSA-N folic acid Chemical compound C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)N[C@@H](CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-LBPRGKRZSA-N 0.000 description 10
- 239000000047 product Substances 0.000 description 6
- OVBPIULPVIDEAO-UHFFFAOYSA-N N-Pteroyl-L-glutaminsaeure Natural products C=1N=C2NC(N)=NC(=O)C2=NC=1CNC1=CC=C(C(=O)NC(CCC(O)=O)C(O)=O)C=C1 OVBPIULPVIDEAO-UHFFFAOYSA-N 0.000 description 5
- 229960000304 folic acid Drugs 0.000 description 5
- 235000019152 folic acid Nutrition 0.000 description 5
- 239000011724 folic acid Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 230000002411 adverse Effects 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- DJWVKJAGMVZYFP-UHFFFAOYSA-N 1,1,3,3-tetrachloropropan-2-one Chemical compound ClC(Cl)C(=O)C(Cl)Cl DJWVKJAGMVZYFP-UHFFFAOYSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- ZWILTCXCTVMANU-UHFFFAOYSA-N tetrachloroacetone Natural products ClCC(=O)C(Cl)Cl ZWILTCXCTVMANU-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/63—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by introduction of halogen; by substitution of halogen atoms by other halogen atoms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/42—Regulation; Control
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/02—Crystallisation from solutions
-
- 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
- B01J19/0006—Controlling or regulating processes
-
- 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
- B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
-
- 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
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/81—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Crystallography & Structural Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of trichloroacetone production, in particular to a high-purity trichloroacetone production process, which comprises the following steps of: step 1, mixing acetone and a catalyst, and then pumping the mixture into a first-stage reactor to react with chlorine; step 2, mixing the reaction liquid after the reaction in the first-stage reactor with dichloroacetone, pumping the mixture into a second-stage reactor, and reacting with chlorine; step 3, sending the reaction solution after the reaction in the secondary reactor into a crystallization kettle, and separating out trichloroacetone crystals; step 4, performing solid-liquid separation to obtain a high-purity trichloroacetone finished product; the high-purity trichloroacetone production process provided by the invention adopts a sectional reaction to prepare trichloroacetone, firstly, the trichloroacetone is rapidly reacted through the first-stage reactor to generate a large amount of dichloroacetone, then, the dichloroacetone is rapidly reacted through the second-stage reactor to generate a large amount of trichloroacetone, the generation of side reaction is effectively reduced, the purity of the trichloroacetone is improved, and the purity of the trichloroacetone obtained after purification through the crystallization kettle can reach more than 90%.
Description
Technical Field
The invention relates to the technical field of trichloroacetone production, in particular to a production process of high-purity trichloroacetone.
Background
The trichloroacetone is used as a main raw material of crude folic acid, and the stable quality of the trichloroacetone is ensured by the quality of folic acid. However, the content of trichloroacetone in the domestic market is 50% -70%, and low-purity trichloroacetone can improve the production cost of folic acid and reduce the production efficiency of folic acid.
Trichloroacetone is generally prepared by directly reacting chlorine and acetone, the reaction period is as long as 48 hours, and because the chlorine has high activity and a large number of acetone reaction sites, chlorinated products are disordered, only about 17% of yield (calculated by acetone) can be obtained through a rectification mode, separation and purification are difficult, the production cost of folic acid is improved, and a large amount of tetrachloroacetone generated by excessive reaction is contained in byproducts, so that the tetrachloroacetone is difficult to degrade and is easy to cause serious environmental protection problems.
Disclosure of Invention
The invention aims to solve the defects in the prior art, and provides a high-purity trichloroacetone production process.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a production process of high-purity trichloroacetone comprises the following steps:
step 1, mixing acetone and a catalyst, pumping into a primary reactor, inputting chlorine from a distributor at the lower end of the primary reactor, reacting with the chlorine, and controlling the reaction temperature to be 35-65 ℃;
step 2, mixing the reaction solution reacted by the primary reactor with dichloroacetone, pumping the mixture into a secondary reactor, inputting chlorine from a distributor at the lower end of the secondary reactor, reacting with the chlorine, and controlling the reaction temperature to be 35-65 ℃;
step 3, the reaction solution after the reaction in the secondary reactor is sent into a crystallization kettle, the temperature of the crystallization kettle is controlled to be 15 ℃ below zero to 5 ℃, and the reaction solution is stirred and cooled to separate out trichloroacetone crystals;
and 4, carrying out solid-liquid separation on the materials in the crystallization kettle to obtain a high-purity trichloroacetone finished product.
Preferably, in the step 4, after solid-liquid separation of materials in the crystallization kettle, the mother liquor is sent into a distillation kettle for distillation, the distillation temperature is controlled to be 70-120 ℃, the monochloroacetone and the dichloroacetone are distilled, the monochloroacetone is pumped into a first-stage reactor for cyclic reaction, and the dichloroacetone is pumped into a second-stage reactor for cyclic reaction.
Preferably, in step 4, the monochloroacetone is mixed with the other reaction liquids when pumped into the primary reactor, and the dichloroacetone is mixed with the other reaction liquids when pumped into the secondary reactor.
Preferably, in step 1, the ratio of chlorine to acetone mass is (2.5-3.5): 1, a step of; in step 2, the ratio of the amounts of chlorine to acetone is (1.5-2): 1.
preferably, in the step 1, the residence time of the chlorine in the primary reactor is 5-30s, and in the step 2, the residence time of the chlorine in the secondary reactor is 5-30s.
Preferably, the primary reactor and the secondary reactor are tubular reactors, and the inner diameters of the primary reactor and the secondary reactor are smaller than 50cm.
Preferably, the catalyst is one of diethylamine or triethylamine.
Preferably, a high-purity trichloroacetone production system comprises a first-stage reactor and a second-stage reactor, wherein an acetone feeding pipe and a chlorine feeding pipe are arranged at the lower end of the first-stage reactor, a gas-liquid separator is arranged at the outlet end of the first-stage reactor, a liquid phase discharged by the first-stage reactor is connected with a feeding port of the second-stage reactor, a chlorine feeding pipe is also arranged at the lower end of the second-stage reactor, a gas-liquid separator is arranged at the outlet end of the second-stage reactor, a liquid phase discharged by the first-stage reactor is connected with a feeding port of a crystallization kettle, a solid-liquid separator is connected with a discharging port of the crystallization kettle, a liquid phase outlet end of the solid-liquid separator is connected with an inlet end of a distillation tower, a dichloroacetone receiving kettle and a monochloroacetone receiving kettle are sequentially connected with a feeding port of the second-stage reactor, and a discharging port of the monochloroacetone receiving kettle is connected with a feeding port of the first-stage reactor.
Preferably, the primary reactor and the secondary reactor are both provided with cooling jackets, and the cooling jackets are provided with a cooling water inlet pipe and a cooling water inlet pipe.
Preferably, the outlet end of the gas phase of the gas-liquid separator is connected with a hydrogen chloride gas absorption pipe.
The beneficial effects of the invention are as follows:
1. the high-purity trichloroacetone production process provided by the invention adopts a sectional reaction to prepare trichloroacetone, firstly, the trichloroacetone is rapidly reacted through the first-stage reactor to generate a large amount of dichloroacetone, then, the dichloroacetone is rapidly reacted through the second-stage reactor to generate a large amount of trichloroacetone, the generation of side reaction is effectively reduced, the purity of the trichloroacetone is improved, and the purity of the trichloroacetone obtained after purification through the crystallization kettle can reach more than 90%.
2. According to the high-purity trichloroacetone production process, the primary reactor and the secondary reactor are tubular reactors, and the diameter of the reactors is small, so that the liquid phase and the gas phase can be fully contacted, the reaction speed is high, the reaction can be completed in a short time, the production efficiency is improved, and meanwhile, the occurrence of side reactions is reduced.
3. According to the high-purity trichloroacetone production process provided by the invention, dichloroacetone and monochloroacetone generated by reaction are put into the secondary reactor and the primary reactor for recycling, so that the raw material use is saved, and the adverse effect of byproducts on the environment is reduced.
Drawings
Fig. 1 is a schematic flow chart of a high-purity trichloroacetone production system provided by the invention.
In the figure: a first-stage reactor 1, a second-stage reactor 2, a crystallization kettle 3, a distillation tower 4, a dichloroacetone receiving kettle 5, a monochloroacetone receiving kettle 6, a gas-liquid separator 7, a solid-liquid separator 8, an acetone feeding pipe 11, a chlorine feeding pipe 12, a cooling water feeding pipe 13, a cooling water feeding pipe 14, a trichloroacetone finished product outlet 15 and a hydrogen chloride gas absorbing pipe 16.
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.
Referring to fig. 1, a process for producing high purity trichloroacetone comprises the steps of:
step 1, mixing acetone and a catalyst, pumping into a primary reactor 1, inputting chlorine from a distributor at the lower end of the primary reactor 1, reacting with the chlorine, and controlling the reaction temperature to be 35-65 ℃;
step 2, mixing the reaction solution reacted in the first-stage reactor 1 with dichloroacetone, pumping the mixture into a second-stage reactor 2, inputting chlorine from a distributor at the lower end of the second-stage reactor 2, reacting with the chlorine, and controlling the reaction temperature to be 35-65 ℃;
step 3, delivering the reaction solution after the reaction in the secondary reactor 2 into a crystallization kettle 3, controlling the temperature of the crystallization kettle 3 to be-15-5 ℃, stirring and cooling, and separating out trichloroacetone crystals;
and 4, carrying out solid-liquid separation on the materials in the crystallization kettle 3 to obtain a high-purity trichloroacetone finished product.
In the step 4, after solid-liquid separation of materials in the crystallization kettle 3, the mother liquor is sent into a distillation kettle for distillation, the distillation temperature is controlled to be 70-120 ℃, monochloroacetone and dichloroacetone are distilled out, the monochloroacetone is pumped into a primary reactor 1 for circular reaction, and the dichloroacetone is pumped into a secondary reactor 2 for circular reaction.
In step 4, the monochloroacetone is mixed with other reaction liquids when pumped into the primary reactor 1, and the dichloroacetone is mixed with other reaction liquids when pumped into the secondary reactor 2.
In step 1, the ratio of chlorine to acetone is (2.5-3.5): 1, a step of; in step 2, the ratio of the amounts of chlorine to acetone is (1.5-2): 1.
the residence time of the chlorine in the primary reactor 1 in the step 1 is 5-30s, and the residence time of the chlorine in the secondary reactor 2 in the step 2 is 5-30s.
The primary reactor 1 and the secondary reactor 2 are tubular reactors, and the inner diameters of the primary reactor 1 and the secondary reactor 2 are smaller than 50cm.
The catalyst is one of diethylamine or triethylamine.
The utility model provides a high purity trichloroacetone production system, includes first order reactor 1 and second grade reactor 2, the lower extreme of first order reactor 1 is provided with acetone inlet pipe 11 and chlorine inlet pipe 12, the exit end of first order reactor 1 is provided with gas-liquid separator 7, first order reactor 1 exhaust liquid phase is connected with the feed inlet of second grade reactor 2, the lower extreme of second grade reactor 2 still is provided with chlorine inlet pipe 12, the exit end of second grade reactor 2 is provided with gas-liquid separator 7, first order reactor 1 exhaust liquid phase is connected with the feed inlet of crystallization kettle 3, the discharge gate of crystallization kettle 3 is connected with solid-liquid separator 8, the exit end of solid-liquid separator 8 is connected with the entrance end of distillation column 4, the lower extreme of solid-liquid separator 8 is provided with trichloroacetone finished product export 15, the exit end of distillation column 4 is connected with dichloro acetone and accepts cauldron 5 and monochloroacetone and accept 6 in proper order, the discharge gate of dichloro acetone accepts cauldron 5 is connected with the feed inlet of second grade reactor 2, the discharge gate of crystallization kettle 3 is connected with the feed inlet of first order reactor 1.
The primary reactor 1 and the secondary reactor 2 are respectively provided with a cooling jacket, the cooling jackets are provided with a cooling water inlet pipe 13 and a cooling water inlet pipe 14, and the primary reactor 1 or the secondary reactor 2 is rapidly cooled through the cooling jackets, so that the reaction can be ensured to be normally carried out.
The outlet end of the gas phase of the gas-liquid separator 7 is connected with a hydrogen chloride gas absorption pipe 16, so that adverse effects of unreacted chlorine and hydrogen chloride gas on the environment are avoided.
The high-purity trichloroacetone production process provided by the invention adopts the sectional reaction to prepare the trichloroacetone, firstly, the trichloroacetone is rapidly reacted through the primary reactor 1 to generate a large amount of dichloroacetone, then, the dichloroacetone is rapidly reacted through the secondary reactor 2 to generate a large amount of trichloroacetone, the generation of side reaction is effectively reduced, the purity of the trichloroacetone is improved, the purity of the trichloroacetone obtained after purification through the crystallization kettle 3 can reach more than 90%, and the purity of the trichloroacetone is high, so that the production of subsequent products is facilitated.
According to the high-purity trichloroacetone production process, the primary reactor 1 and the secondary reactor 2 are tubular reactors, and the diameter of the reactors is small, so that the liquid phase and the gas phase can be fully contacted, the reaction speed is high, the reaction can be completed in a short time, the production efficiency is improved, and meanwhile, the occurrence of side reactions is reduced.
According to the high-purity trichloroacetone production process provided by the invention, dichloroacetone and monochloroacetone generated by reaction are put into the secondary reactor 2 and the primary reactor 1 for recycling, so that the raw material use is saved, and the adverse effect of byproducts on the environment is reduced.
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 (10)
1. The production process of the high-purity trichloroacetone is characterized by comprising the following steps of:
step 1, mixing acetone and a catalyst, pumping into a primary reactor, inputting chlorine from a distributor at the lower end of the primary reactor, reacting with the chlorine, and controlling the reaction temperature to be 35-65 ℃;
step 2, mixing the reaction solution reacted by the primary reactor with dichloroacetone, pumping the mixture into a secondary reactor, inputting chlorine from a distributor at the lower end of the secondary reactor, reacting with the chlorine, and controlling the reaction temperature to be 35-65 ℃;
step 3, the reaction solution after the reaction in the secondary reactor is sent into a crystallization kettle, the temperature of the crystallization kettle is controlled to be 15 ℃ below zero to 5 ℃, and the reaction solution is stirred and cooled to separate out trichloroacetone crystals;
and 4, carrying out solid-liquid separation on the materials in the crystallization kettle to obtain a high-purity trichloroacetone finished product.
2. The process for producing high-purity trichloroacetone according to claim 1, wherein in the step 4, after solid-liquid separation of materials in the crystallization kettle, mother liquor is sent into a distillation kettle for distillation, the distillation temperature is controlled to be 70-120 ℃, monochloroacetone and dichloroacetone are distilled out, the monochloroacetone is pumped into a primary reactor for cyclic reaction, and the dichloroacetone is pumped into a secondary reactor for cyclic reaction.
3. The process for producing high-purity trichloroacetone according to claim 1, wherein in step 4, the monochloroacetone is mixed with other reaction liquids when pumped into the primary reactor, and the dichloroacetone is mixed with other reaction liquids when pumped into the secondary reactor.
4. The process for producing high-purity trichloroacetone according to claim 1, wherein in step 1, the ratio of the amounts of chlorine gas to acetone is (2.5-3.5): 1, a step of; in step 2, the ratio of the amounts of chlorine to acetone is (1.5-2): 1.
5. the process for producing high-purity trichloroacetone according to claim 1, wherein the residence time of chlorine in the primary reactor in step 1 is 5 to 30s, and the residence time of chlorine in the secondary reactor in step 2 is 5 to 30s.
6. The process for producing high-purity trichloroacetone according to claim 1, wherein the primary reactor and the secondary reactor are tubular reactors, and the inner diameters of the primary reactor and the secondary reactor are smaller than 50cm.
7. The process for producing high-purity trichloroacetone according to claim 1, wherein the catalyst is one of diethylamine and triethylamine.
8. The high-purity trichloroacetone production system according to any one of claims 1 to 7, comprising a primary reactor and a secondary reactor, wherein an acetone feed pipe and a chlorine feed pipe are arranged at the lower end of the primary reactor, a gas-liquid separator is arranged at the outlet end of the primary reactor, a liquid phase discharged by the primary reactor is connected with a feed inlet of the secondary reactor, a chlorine feed pipe is also arranged at the lower end of the secondary reactor, a gas-liquid separator is arranged at the outlet end of the secondary reactor, a liquid phase discharged by the primary reactor is connected with a feed inlet of a crystallization kettle, a solid-liquid separator is connected with a discharge outlet of the crystallization kettle, a liquid phase outlet end of the solid-liquid separator is connected with an inlet end of a distillation tower, a dichloroacetone receiving kettle and a monochloroacetone receiving kettle are sequentially connected at the outlet end of the distillation tower, a discharge outlet of the dichloroacetone receiving kettle is connected with a feed inlet of the secondary reactor, and a discharge outlet of the monochloroacetone receiving kettle is connected with a feed inlet of the primary reactor.
9. The high-purity trichloroacetone production system according to claim 8, wherein the primary reactor and the secondary reactor are provided with cooling jackets, and the cooling jackets are provided with a cooling water inlet pipe and a cooling water inlet pipe.
10. The system for producing high-purity trichloroacetone according to claim 8, wherein an outlet end of the gas phase of the gas-liquid separator is connected to a hydrogen chloride gas absorption tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310615223.8A CN116836048A (en) | 2023-05-29 | 2023-05-29 | Production process of high-purity trichloroacetone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310615223.8A CN116836048A (en) | 2023-05-29 | 2023-05-29 | Production process of high-purity trichloroacetone |
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| CN116836048A true CN116836048A (en) | 2023-10-03 |
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| CN202310615223.8A Withdrawn CN116836048A (en) | 2023-05-29 | 2023-05-29 | Production process of high-purity trichloroacetone |
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| CN (1) | CN116836048A (en) |
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- 2023-05-29 CN CN202310615223.8A patent/CN116836048A/en not_active Withdrawn
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