CN111644121A - Hydrogenation dechlorination device and method for trichloroacetone - Google Patents
Hydrogenation dechlorination device and method for trichloroacetone Download PDFInfo
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- CN111644121A CN111644121A CN202010526730.0A CN202010526730A CN111644121A CN 111644121 A CN111644121 A CN 111644121A CN 202010526730 A CN202010526730 A CN 202010526730A CN 111644121 A CN111644121 A CN 111644121A
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- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
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- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/087—Heating or cooling the reactor
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- 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
- C07C45/85—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to a chemical modification
Abstract
The invention discloses a hydrogenation dechlorination device of trichloroacetone and a method thereof, which relate to the technical field of chemical purification and comprise a reaction container and a base, wherein the reaction container is placed above the base, the reaction container is provided with a first bottle opening, a second bottle opening, a third bottle opening and a fourth bottle opening, the second bottle opening is positioned in the right center, and a stirring structure is arranged in the second bottle opening; the stirring mechanism comprises a stirring rod, an end cover plug and a sliding sleeve which are arranged on the outer side of the stirring rod, a stirring blade arranged at the bottom of the stirring rod and a connecting rod rotationally connected with the stirring blade, a feeding structure is arranged in the stirring rod, and the upper end of the stirring rod is connected with a driving mechanism; and the stirring blade is convenient to extend and retract, and is convenient to mount and dismount.
Description
Technical Field
The invention belongs to the technical field of chemical purification, and particularly relates to a trichloroacetone hydrodechlorination device and a trichloroacetone hydrodechlorination method.
Background
Trichloroacetone is an important industrial raw material, and trichloroacetone, in particular high-purity trichloroacetone, has extremely wide application, and can be used for synthesis and research of anti-HIV drugs, imidazole heterocyclic compounds and polycyclic or bridged compounds. The preparation method of trichloroacetone is generally a method for directly chlorinating acetone, and in the existing process, due to poor chlorination selectivity and low yield, monochloroacetone, dichloroacetone, tetrachloroacetone, pentachloroacetone and hexachloroacetone are contained in chlorination products besides trichloroacetone. Wherein tetrachloroacetone, pentachloroacetone and hexachloroacetone are difficult to dissolve in water, and after the reaction product is washed out of trichloroacetone by water, the remaining tetrachloroacetone, pentachloroacetone and hexachloroacetone are called perchloroacetone residue. The high chloropropanone has high toxicity, teratogenic, carcinogenic, mutagenic "triprodogenic" effects, irritation to eyes, skin, mucous membranes and upper respiratory tract, explosive properties and is a dangerous substance which threatens the environment and human health safety, so that trichloroacetone is dechlorinated, and the conventional treatment mode is hydrodechlorination.
The existing dechlorination device adopts a closed container to react in order to prevent toxic substances from leaking in the dechlorination process during dechlorination, and performs stirring and mixing through an external magnetic stirring device, a stirrer collides with an air inlet pipe arranged in the container during rotating and stirring, the stirring effect is poor, the existing closed container device is not suitable for batch dechlorination, and the dechlorination efficiency is low, so that the device and the method for hydrodechlorination of trichloroacetone are provided.
Disclosure of Invention
In view of the defects of the prior art, the present invention provides a hydrodechlorination apparatus for trichloroacetone and a method thereof, so as to solve the problems in the background art.
The purpose of the invention can be realized by the following technical scheme: a device and a method for hydrodechlorination of trichloroacetone comprise a reaction container and a base, wherein the reaction container is placed above the base, the reaction container is provided with a first bottle opening, a second bottle opening, a third bottle opening and a fourth bottle opening, the second bottle opening is positioned in the center, and a stirring structure is arranged in the second bottle opening;
the stirring mechanism comprises a stirring rod, an end cover plug and a sliding sleeve which are arranged on the outer side of the stirring rod, a stirring blade arranged at the bottom of the stirring rod and a connecting rod which is rotatably connected with the stirring blade, the sliding sleeve is positioned on the lower side of the end cover plug and is rotatably connected with the end cover plug, the end cover plug is tightly attached to the inner wall of the second bottle mouth, and the sliding sleeve is slidably connected with the stirring rod;
the improved stirring device is characterized in that a circular groove is formed in the lower end of the sliding sleeve, the lower end of the circular groove of the sliding sleeve is rotatably connected with one end of a connecting rod, the other end of the connecting rod is rotatably connected with a connecting rod support on the stirring blade, the stirring blade is rotatably connected with the stirring rod, a sliding groove is formed in the lower end of the stirring rod, the stirring blade is contained in the sliding groove, a feeding structure is arranged in the stirring rod, and the upper end of the stirring rod is connected with a.
As a further proposal of the invention, a spring is arranged between the inner top surface of the circular groove and the upper top surface of the lower stepped shaft of the stirring rod.
As a further scheme of the invention, a material supporting rod is arranged in the through hole of the stirring rod, the material supporting rod is connected with the stirring rod in a sliding manner, a limit groove is formed in the outer circumference of the upper top end of the stirring rod, a lug matched with the limit groove for limiting is radially arranged at the top end of the material supporting rod, and a material supporting groove is formed at the lower end of the material supporting rod.
As a further scheme of the invention, a liquid injection pipe and a liquid suction pipe are arranged in the fourth bottle mouth, one end of the liquid suction pipe extends to the bottom surface inside the reaction container in the vertical direction and is attached to the bottom surface inside the reaction container, and the other end of the liquid suction pipe is connected with a pressure pump.
As a further scheme of the invention, an air inlet pipe is arranged in the first bottle mouth, and one end of the air inlet pipe extends to the bottom surface in the reaction container.
As a further scheme of the invention, a water spraying pipe is arranged in the third bottle mouth, the water spraying pipe is fixedly connected with a rubber plug, the rubber plug is fixedly connected with the third bottle mouth, and a nozzle is fixedly arranged at one end of the water spraying pipe close to the inner part of the reaction container.
As a further scheme of the invention, the outer circumference of the water spraying pipe is provided with a detection test paper which is adjacent to the spray head.
As a further scheme of the invention, the lower side of the bottom surface of the outer side of the reaction container is provided with an asbestos net which is attached to the asbestos net, and the asbestos net is suspended above the base.
As a further scheme of the invention, a groove and a heating rod are arranged in the base, and a liquid medium is arranged in the base.
The method for hydrodechlorinating the trichloroacetone comprises the following steps:
the first step is as follows: injecting the trichloroacetone solution into the reaction container through the liquid injection pipe, injecting a proper amount of water, and starting an external driving mechanism of the stirring rod to drive the stirring rod to rotate so as to fully mix the trichloroacetone solution with the water;
the second step is that: placing a carbon-based hydrogenation catalyst into a trichloroacetone aqueous solution in a reaction vessel through a material supporting rod;
the third step: and introducing hydrogen into the air inlet pipe, starting the heating rod to heat the liquid medium in the base, conducting heat to the reaction container through the liquid medium, stopping heating when the temperature rises to 90-100 ℃, and continuously preserving heat for 6-12 hours.
The invention has the beneficial effects that:
1. compared with the prior art, the invention eliminates the problem of interference between the stirrer and the inner pipe of the reaction vessel when the stirrer rotates, improves the stirring efficiency, and is suitable for batch dechlorination treatment; and the stirring blade is convenient to extend and retract, and is convenient to mount and dismount.
2. The invention utilizes the liquid medium to conduct and heat, the reaction vessel is uniformly heated, the explosion is not easy to occur, the temperature control is convenient, the reaction time is shortened, and the dechlorination efficiency is improved.
3. The reaction vessel is internally provided with a chlorine gas detection and treatment device, thereby avoiding the occurrence of chlorine gas leakage to influence the personal safety.
Drawings
In order to more clearly illustrate the embodiments or technical solutions in the prior art of the present invention, the drawings used in the description of the embodiments or prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a cross-sectional view of the present invention;
FIG. 3 is a cross-sectional view (taken perpendicular to the view of FIG. 2) of another aspect of the present invention;
FIG. 4 is a schematic structural view of the stirring mechanism of the present invention;
FIG. 5 is a schematic view of the construction of the stirring rod of the present invention;
FIG. 6 is a schematic structural view of a stirring vane of the present invention;
FIG. 7 is a schematic structural view of the lifter bar of the present invention;
in the figure: the device comprises a base-1, a reaction container-2, an air inlet pipe-3, a rubber plug-4, a stirring rod-5, a material supporting rod-6, an end cover plug-7, a water spraying pipe-8, a liquid injection pipe-9, a pressure pump-10, a liquid suction pipe-11, a heating rod-12, an asbestos net-13, a water discharge pipe-14, a sliding sleeve-15, a spring-16, a connecting rod-17, a stirring blade-18, detection test paper-19, a spray head-20, a first bottle opening-21, a second bottle opening-22, a third bottle opening-23, a fourth bottle opening-24, a limiting groove-51, a sliding groove-52, a through hole-53, a material supporting groove-61 and a connecting rod support-181.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1 to 7, in the embodiment of the present invention, a trichloroacetone hydrodechlorination apparatus and a method thereof include a reaction container 2 and a base 1, where the reaction container 2 is placed above the base 1, the reaction container 2 is provided with a first bottle opening 21, a second bottle opening 22, a third bottle opening 23, and a fourth bottle opening 24, the second bottle opening 22 is located at the center, a stirring mechanism is disposed in the second bottle opening 22, and a feeding mechanism is disposed in the center of the stirring mechanism;
a liquid injection pipe 9 and a liquid suction pipe 11 are arranged in the fourth bottle opening 24, the liquid injection pipe 9 and the liquid suction pipe 11 are both fixedly connected with a rubber plug 4, the rubber plug 4 and one end of the liquid suction pipe 11 vertically extend to the bottom surface inside the reaction container 2 and are attached to the bottom surface inside the reaction container 2, and the other end of the rubber plug is connected with a pressure pump 10;
be provided with intake pipe 3 in the first bottleneck 21, intake pipe 3 and rubber buffer 4 fixed connection, 3 one end of intake pipe extends to the inside bottom surface of reaction vessel 2.
During operation, add trichloroacetone and the residue solution that is thoughtlessly has chloropropanone to reaction vessel 2 inside through annotating liquid pipe 9, mix through annotating liquid pipe 9 and adding the deionized water of certain proportion, start rabbling mechanism and stir evenly, after stopping the stirring, add carbon base hydrogenation fixed catalyst to reaction vessel 2 in through the feeding mechanism at rabbling mechanism center, inject hydrogen in intake pipe 3 and begin to carry out dechlorination.
As shown in fig. 2, the stirring mechanism includes a stirring rod 5, an end cap plug 7 and a sliding sleeve 15 which are arranged outside the stirring rod 5, a stirring blade 18 which is arranged at the bottom of the stirring rod 5, and a connecting rod 17 which is rotatably connected with the stirring blade 18, the sliding sleeve 15 is positioned at the lower side of the end cap plug 7 and is rotatably connected with the end cap plug 7, the end cap plug 7 is closely attached to the inner wall of the second bottle mouth 22, the sliding sleeve 15 is slidably connected with the stirring rod 5, the lower end of a circular groove of the sliding sleeve 15 is rotatably connected with one end of the connecting rod 17, and the other end of the connecting rod 17 is rotatably connected with a connecting rod. Spout 52 has been seted up to puddler 5 lower extreme, stirring leaf 18 is arranged in spout 52, and stirring leaf 18 rotates with puddler 5 and is connected, for the convenience of installation, stirring leaf 18 can be accomodate in spout 52, and does not surpass the outer circumference side of puddler 5, connect stirring leaf 18 to dismantle when taking out and can not cause the interference, when stirring simultaneously, stirring leaf 18 is at the descending of sliding sleeve 15 and is expanded to both sides, and can not take place to interfere with pipette 11 and intake pipe 3 in the reaction vessel 2, stirring efficiency is higher compared with magnetic stirring device, can not produce the inner structure that interferes damage reaction vessel 2 simultaneously. Meanwhile, for installation convenience, the material supporting rod 6, the sliding sleeve 15, the connecting rod 17 and the stirring blade 18 are assembled and then placed into the reaction container 2 through the second bottle opening 22, the end cover plug 7 penetrates into the stirring rod 5 and is installed on the second bottle opening 22, and the upper portion of the stirring rod 5 is fixedly installed with the driving motor.
A circular groove is formed in the lower end of the sliding sleeve 15, and a spring 16 is arranged between the inner top surface of the circular groove and the upper top surface of the lower stepped shaft of the stirring rod 5; the retraction of the stirring blade 18 can be prevented, and the connection tightness between the parts is improved.
As shown in fig. 2 and 7, a material supporting rod 6 is arranged in a through hole 53 in the stirring rod 5, the material supporting rod 6 is connected with the stirring rod 5 in a sliding manner, a limiting groove 51 is formed in the outer circumference of the upper top end of the stirring rod 5, a protruding block matched with the limiting groove 51 for limiting is radially arranged at the top end of the material supporting rod 6, and a material supporting groove 61 is formed at the lower end of the material supporting rod 6; after the carbon-based hydrogenation catalyst in the reaction vessel 2 is consumed, the carbon-based hydrogenation catalyst is placed on the material supporting groove 61 and is placed into the solution in the reaction vessel 2 through the through hole 53 of the stirring rod 5, and the trichloroacetone and the high chloropropanone in the mixed solution thereof have toxicity, so that the leakage can be avoided and the contact of personnel can be reduced through the pipeline feeding, the safe operation performance is improved, and meanwhile, the entering of impurities and dust is reduced, and the purity of reaction products is influenced.
As shown in fig. 3, a spray pipe 8 is arranged in a third bottle mouth 23, the spray pipe 8 is fixedly connected with a rubber plug 4, the rubber plug 4 is fixedly connected with the third bottle mouth 23, a nozzle 20 is fixedly arranged at one end of the spray pipe 8 close to the inside of the reaction container 2, a detection test paper 19 is arranged on the outer circumference of the spray pipe 8, the detection test paper 19 is arranged on the upper side of the nozzle 20, the detection test paper 19 is composed of wet potassium iodide test paper, the detection test paper 19 mainly functions to detect whether chlorine gas is generated in reactants in the reaction container 2, and the detection test paper 19 turns blue after observation proves that chlorine gas is generated in the reaction container 2, in order to prevent the chlorine gas from leaking and harming the health of people, the other end of the spray pipe 8 is connected with a water pump, water is sprayed out through the nozzle 20 and chemically reacts with the chlorine gas in the reaction container 2, effectively preventing the leakage.
As shown in fig. 1, an asbestos mesh 13 is arranged on the lower side of the bottom surface of the outer side of the reaction container 2, the asbestos mesh 13 is attached to the asbestos mesh 13, a groove is formed in the base 1, a heating rod 12 is arranged in the groove, a liquid medium is arranged in the groove, the reaction container 2 is heated by heating the liquid medium through the heating rod 12, the reaction container 2 is uniformly heated, the heat preservation is convenient to control, after the reaction is finished, the liquid medium in the base 1 is discharged through a water discharge pipe 14, the reaction container 2 is naturally cooled on the asbestos mesh 13, and after the cooling is finished, a pressure pump 10 is started to pump the solution in the reaction container 2 out to a glass container.
The method for hydrodechlorinating the trichloroacetone comprises the following steps:
the first step is as follows: injecting the trichloroacetone solution into the reaction container 2 through the liquid injection pipe 9, injecting a proper amount of water, starting an external driving mechanism of the stirring rod 5 to drive the stirring rod 5 to rotate, and fully mixing the trichloroacetone solution with the water;
the second step is that: placing the carbon-based hydrogenation catalyst into the trichloroacetone aqueous solution in the reaction vessel 2 through a material supporting rod 6;
the third step: introducing hydrogen into the air inlet pipe 3, starting the heating rod 12 to heat the liquid medium in the base 1, conducting heat to the reaction container 2 through the liquid medium, stopping heating when the temperature rises to 80-90 ℃, and continuously preserving heat for 6-12 hours by the heating rod.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "left", "right", etc., indicating an orientation or positional relationship are based on the orientation or positional relationship shown in the drawings and are used merely for convenience in describing the present invention and for simplifying the description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed in a specific orientation, or be operated, and thus, should not be construed as limiting the present invention.
Furthermore, the method is simple. The terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. In the description of the present invention, "a plurality" means two or more unless specifically limited otherwise.
It will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the spirit and scope of the invention, and any equivalents thereto, such as those skilled in the art, are intended to be embraced therein.
Claims (9)
1. A hydrogenation dechlorination device of trichloroacetone and a method thereof comprise a reaction container (2) and a base (1), wherein the reaction container (2) is placed above the base (1), and is characterized in that the reaction container (2) is provided with a first bottle opening (21), a second bottle opening (22), a third bottle opening (23) and a fourth bottle opening (24), the second bottle opening (22) is positioned in the center of the center, and a stirring structure is arranged in the second bottle opening (22);
the stirring mechanism comprises a stirring rod (5), an end cover plug (7) and a sliding sleeve (15) which are arranged on the outer side of the stirring rod (5), a stirring blade (18) which is arranged at the bottom of the stirring rod (5) and a connecting rod (17) which is rotatably connected with the stirring blade (18), the sliding sleeve (15) is positioned on the lower side of the end cover plug (7) and is rotatably connected with the end cover plug (7), the end cover plug (7) is tightly attached to the inner wall of the second bottle mouth (22), and the sliding sleeve (15) is slidably connected with the stirring rod (5);
the inside circular slot of having seted up of sliding sleeve (15) lower extreme, sliding sleeve (15) circular slot lower extreme rotates with connecting rod (17) one end to be connected, connecting rod support (181) on connecting rod (17) other end and stirring leaf (18) rotate to be connected, stirring leaf (18) rotate with puddler (5) to be connected, spout (52) have been seted up to puddler (5) lower extreme, stirring leaf (18) are accomodate in spout (52), set up by the pay-off structure in 05, and the 05 upper end is connected with actuating mechanism.
2. The apparatus and method for hydrodechlorination of trichloroacetone according to claim 1, wherein a spring (16) is provided between the inner top surface of the circular tank and the upper top surface of the lower stepped shaft of the stirring rod (5).
3. The hydrodechlorination device of trichloroacetone and the method thereof according to claim 1, wherein a material supporting rod (6) is arranged in the through hole (53) of the stirring rod (5), the material supporting rod (6) is connected with the stirring rod (5) in a sliding manner, a limiting groove (51) is formed in the outer circumference of the upper top end of the stirring rod (5), a protruding block matched with the limiting groove (51) for limiting is radially arranged at the top end of the material supporting rod (6), and a material supporting groove (61) is formed in the lower end of the material supporting rod (6).
4. The device and the method for hydrodechlorination of trichloroacetone according to claim 1, wherein a liquid injection pipe (9) and a liquid suction pipe (11) are arranged in the fourth bottle opening (24), one end of the liquid suction pipe (11) extends to the bottom surface of the interior of the reaction vessel (2) in the vertical direction, is attached to the bottom surface of the interior of the reaction vessel (2), and the other end is connected with the pressure pump (10).
5. The device and the method for hydrodechlorination of trichloroacetone according to claim 1, wherein an air inlet pipe (3) is arranged in the first bottle mouth (21), and one end of the air inlet pipe (3) extends to the bottom surface of the interior of the reaction vessel (2).
6. The device and the method for hydrodechlorination of trichloroacetone according to claim 1, wherein a water spray pipe (8) is arranged in the third bottle mouth (23), the water spray pipe (8) is fixedly connected with a rubber plug (4), the rubber plug (4) is fixedly connected with the third bottle mouth (23), and a nozzle (20) is fixedly installed at one end of the water spray pipe (8) close to the inside of the reaction vessel (2).
7. The apparatus and method for hydrodechlorination of trichloroacetone according to claim 1, wherein the outer circumference of the water spraying pipe (8) is provided with a detection test paper (19), and the detection test paper (19) is adjacent to the spray head (20).
8. The device and the method for hydrodechlorination of trichloroacetone according to claim 1, wherein an asbestos cloth (13) is arranged on the lower side of the bottom surface of the outer side of the reaction vessel (2), and is attached to the asbestos cloth (13), and the asbestos cloth (13) is suspended above the base (1).
9. The apparatus and method for hydrodechlorination of trichloroacetone according to claim 8, wherein the base (1) is provided with a groove and a heating rod (12) disposed in the groove, and the base (1) is provided with a liquid medium.
The method for hydrodechlorinating the trichloroacetone comprises the following steps:
the first step is as follows: injecting the trichloroacetone solution into the reaction container (2) through the liquid injection pipe (9), injecting a proper amount of water, starting an external driving mechanism of the stirring rod (5) to drive the stirring rod (5) to rotate, and fully mixing the trichloroacetone solution with the water;
the second step is that: placing a carbon-based hydrogenation catalyst into a trichloroacetone aqueous solution in a reaction vessel (2) through a material supporting rod (6);
the third step: hydrogen is introduced into the air inlet pipe (3), the heating rod (12) is started to heat the liquid medium in the base (1), heat is conducted to the reaction container (2) through the liquid medium, heating is stopped when the temperature rises to 80-90 ℃, and heat is continuously preserved for 6-12 hours.
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| CN202010526730.0A CN111644121B (en) | 2020-06-09 | 2020-06-09 | Hydrogenation dechlorination device and method for trichloroacetone |
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| CN202010526730.0A CN111644121B (en) | 2020-06-09 | 2020-06-09 | Hydrogenation dechlorination device and method for trichloroacetone |
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