CN111375367A

CN111375367A - Purification device and method of 2, 4-dichlorophenol

Info

Publication number: CN111375367A
Application number: CN202010204451.2A
Authority: CN
Inventors: 谢良威; 朱良彬
Original assignee: Individual
Current assignee: Individual
Priority date: 2020-03-21
Filing date: 2020-03-21
Publication date: 2020-07-07

Abstract

The invention belongs to the technical field of chemical purification, and particularly relates to a device and a method for purifying 2, 4-dichlorophenol; comprises a tank body, wherein the upper end of the tank body is covered with a sealing cover in a sliding way; the supporting plate is fixedly arranged at the bottom end of the tank body, and the supporting column is rotatably arranged on the upper end surface of the supporting plate through a bearing sleeve; the reaction pot is movably arranged in the mounting sleeve through the mounting head; the driving motor is fixed on the supporting plate, and the output end of the driving motor is provided with a driving gear; a driven gear is arranged on the supporting column; the sealing cover is provided with a flow guide pipe, the circumferential direction of the bottom end of the flow guide pipe is obliquely provided with a plurality of stirring rods, and the bottom ends of the stirring rods are positioned on the upper surface of the reaction pot; a sealing plate is sleeved on the flow guide pipe in a sliding manner and is connected with the sealing cover through an electric telescopic rod; s1, crushing the raw materials; s2: injecting water for dissolution; s3, heating to dissolve; s4: extracting impurities; the method is convenient for experimenters to carry out purification experiments on small batches of 2, 4-dichlorophenol, and improves the rapid and efficient purification operation of the 2, 4-dichlorophenol.

Description

Purification device and method of 2, 4-dichlorophenol

Technical Field

The invention belongs to the technical field of chemical purification, and particularly relates to a device and a method for purifying 2, 4-dichlorophenol.

Background

2, 4-dichlorophenol is an important organic intermediate, and is mainly used for producing pesticides such as phenthoate, herbicide oxadiazon, aclonifen, 2, 4-dichlorophenoxy series acid and ester thereof in the pesticide industry; the insecticidal composition is used for producing the anthelmintic thiobis-dichlorophenol in the medical industry; is used for producing antifogging agents TCS in the auxiliary industry. Due to the increase of the development of downstream products of 2, 4-dichlorophenol in China in recent years, particularly the successful development of the antifogging agent TCS and the pesticide oxadiazon in China, the development of the 2, 4-dichlorophenol production industry in China is brought with great opportunity.

At present, 5 methods for producing 2, 4-dichlorophenol which has been industrialized in the world mainly comprise a phenol direct chlorination method, a mixed phenol chlorination method, an o-chlorophenol selective chlorination method, a p-chlorophenol catalytic chlorination method and a phenol catalytic chlorination method.

The existing purification device for 2, 4-dichlorophenol is complex in structure and complex in purification method, and the efficient purification operation of small-batch or experimental personnel on a small amount of 2, 4-dichlorophenol is difficult to realize; however, when the existing 2, 4-dichlorophenol is used in small batches, most beakers or test tubes are adopted for purification, but the purification is carried out independently, so that the purification effect is influenced, and the purity of the 2, 4-dichlorophenol is reduced.

Disclosure of Invention

In order to make up the defects of the prior art, the invention provides a device and a method for purifying 2, 4-dichlorophenol, which are mainly used for solving the problems that the existing device for purifying 2, 4-dichlorophenol is complex in structure and complicated in purification method, and the efficient purification operation of small-batch or experimenters on a small amount of 2, 4-dichlorophenol is difficult to realize; however, when the existing 2, 4-dichlorophenol is used in small batches, most beakers or test tubes are adopted for purification, but the purification is carried out independently, so that the purification effect is influenced, and the purity of the 2, 4-dichlorophenol is reduced.

The technical scheme adopted by the invention for solving the technical problems is as follows: the device and the method for purifying 2, 4-dichlorophenol comprise a tank body, wherein the upper end of the tank body is covered with a sealing cover in a sliding manner, and a reaction extraction device is arranged in the tank body; the reaction extraction device comprises a supporting plate, a supporting column, a mounting sleeve, a mounting head, a reaction pot, a driving motor, a driving gear and a driven gear; the supporting plate is fixedly arranged at the bottom end of the tank body, and the supporting column is rotatably arranged on the upper end face of the supporting plate through a bearing sleeve; the top end of the supporting column is fixed with a mounting sleeve, and a mounting head is electromagnetically adsorbed in the mounting sleeve; the reaction pot is movably arranged in the mounting sleeve through the mounting head; the driving motor is fixed on the supporting plate, and the output end of the driving motor is provided with a driving gear; the support column is provided with a driven gear, and the driven gear is meshed with the driving gear; the sealing cover is provided with a flow guide pipe, the circumferential direction of the bottom end of the flow guide pipe is obliquely provided with a plurality of stirring rods, and the bottom ends of the stirring rods are positioned on the upper surface of the reaction pot; flow guide cavities are formed in the stirring rods and communicated with the flow guide pipes; a plurality of flow guide holes are formed in the upper end face of the stirring rod and are communicated with the flow guide cavity; the guide pipe is sleeved with a sealing plate in a sliding mode, and the sealing plate is connected with the sealing cover through an electric telescopic rod; the sealing plate is arranged in the reaction pot in a sliding manner, and the side wall of the reaction pot is provided with an electric control valve pipe; a heating cavity is formed in the bottom end of the reaction pot, and an electric heating wire is arranged in the heating cavity;

when the device works, a certain amount of unpurified 2, 4-dichlorophenol blocky solid is taken and is stuck into powdery solid by a grinding device; then opening a sealing cover of the tank body, putting the powdery 2, 4-dichlorophenol into a reaction pot, covering the sealing cover on the tank body to enable a stirring rod to be positioned in the reaction pot, controlling a driving motor to rotate by a control unit, driving the driven gear to rotate by the driving motor through a driving gear, driving a reaction pot inserted with an installing head through an installing sleeve to rotate by a rotating supporting column, injecting water with a certain proportion into a guide pipe by an external water injection pipe, respectively flowing the aqueous solution in the guide pipe into a guide cavity, injecting the aqueous solution into the rotating reaction pot through a guide hole to infiltrate the 2, 4-dichlorophenol solid powder in the reaction pot, controlling the driving motor to stop rotating by the control unit to enable the infiltrated aqueous solution and the solid powder to stand, observing whether the liquid level of the aqueous solution flowing into the reaction pot is higher than 2-3 cm of the powder solid or not, then controlling an electric heating wire in a heating cavity by a control unit, heating the electric heating wire to 4-8 ℃, simultaneously driving a motor to rotate, keeping the mixing temperature of the aqueous solution and the solid powder in the reaction pot between 5-7 ℃, then injecting a certain amount of n-propanolamine into a flow guide pipe by an injection device, injecting the n-propanolamine into the mixed solution in the reaction pot through a flow guide hole, simultaneously rotating the reaction pot, injecting the n-propanolamine into a stirring rod, simultaneously mixing and stirring the mixed solution and the n-propanolamine for 25-35 min, simultaneously observing the color change of the mixed solution in the reaction pot, stopping the rotation of the motor after the mixed powder solution is changed into fine needle crystals, standing the fine needle crystal mixed solution in the reaction pot for 10-14 h; then the control unit controls the electric telescopic rod to extend out, the electric telescopic rod drives the sealing plate to slide downwards in the reaction pot, the sliding of the sealing plate can compress the volume in the reaction pot, meanwhile, the control unit controls the electric control valve pipe to open, a water layer generated after the reaction pot stands in the reaction pot can be discharged out of the reaction pot through the electric control valve pipe under the compression of the sealing plate, after the water layer is discharged, the electric control valve pipe is closed, the sealing plate slides upwards, then water solution is injected into the reaction pot through the flow guide pipe, then the reaction pot is driven to rotate by the driving motor, the injected water solution can wash the upper surface of the fine needle crystal-shaped 2, 4-dichlorophenol, the rotation of the reaction pot can accelerate the washing time, then the washing step is carried out for 2-3 times through the sealing plate, then the washing step is carried out for drying and heating through the electric heating wire, and then the, 4-dichlorophenol species; through the matching of the rotating reaction kettle and the static stirring rods, the solid 2, 4-dichlorophenol powder put into the rotating reaction kettle can be quickly dissolved into the aqueous solution under the filling of the aqueous solution filled into the stirring rods, and simultaneously, the phenomenon that the solid powder is bonded on the bottom wall of the reaction kettle due to the static state of the reaction kettle is prevented, so that the quick dissolution of the solid powder is influenced; meanwhile, n-propanolamine is simultaneously injected into the rotating reaction pot through the stirring rods to be in mixed contact with dissolved solid powder, so that the mixed contact of the n-propanolamine and the solid powder solution is increased, the extraction of impurity molecules in the 2, 4-dichlorophenol in an aqueous solution state is facilitated, the purification effect of the 2, 4-dichlorophenol is further improved, meanwhile, experimenters can conveniently carry out purification experiments on small batches of the 2, 4-dichlorophenol, and the rapid and efficient purification operation of the 2, 4-dichlorophenol is improved.

Preferably, the mounting head is of a semi-spherical structure, the bottom end of the mounting head is provided with a magnet block, and the upper end of the mounting head is made of elastic rubber; the mounting sleeve is of a bowl-shaped structure, the bottom end of the mounting sleeve is provided with an electromagnet, and the outer wall of the mounting sleeve is made of elastic rubber; during operation, when jar internal is installed with the reaction pot to needs, set up hemispherical installation head earlier and insert in the installation cover of bowl-shaped structure with the reaction pot bottom, then the control unit control electro-magnet is got electric, the electric meeting magnetic adsorption power that gets of electro-magnet can adsorb the magnet piece, and then in installing the head through the mode adsorption installation of magnetic adsorption, the elastic rubber material that installation cover upper end outer wall set up and the elastic rubber material that installs head upper end setting, make and to form the flexible coupling between reaction pot and the support column, and then the reaction pot of being convenient for can carry out the quick dismantlement installation, the reaction pot of being convenient for simultaneously carries out the whole rotation, mix the mixed solution in the reaction pot under the cooperation of puddler.

Preferably, the driving gear is connected with the output end of the driving motor through an electric cylinder, and a plurality of push rods are arranged on the upper end face of the driving gear; the push rods are all positioned at the bottom end of the reaction pot; a fixed column is arranged on the upper end face of the supporting plate, and a rubber spring is fixed at the top end of the fixed column; an electromagnet is fixed at the top end of the rubber spring and is positioned right below the reaction pot; the fixed columns and the electric telescopic rods are symmetrically arranged along the central line of the supporting column; when the device works, when the waste water solution in the reaction pot after washing needs to be discharged, an operator can not only discharge the waste water solution in the reaction pot in a way that the sealing plate compresses the space of the reaction pot, but also can control the electric cylinder to extend out through the control unit, the electromagnet on the rubber spring is electrified, so that the electromagnet can be adsorbed to the bottom end face of the reaction pot, the electric cylinder can drive the push rod arranged on the driving gear to move upwards, the push rod can push the reaction pot to incline to one side of the rubber spring due to the flexible connection formed between the mounting head and the mounting sleeve, so that the rubber spring is compressed, when the electric telescopic rod slides downwards, the compression rebound force of the rubber spring can lead the reaction pot to swing to one side of the push rod, and then the reciprocating swing reaction pot can discharge the cleaning waste water which is not compressed and discharged through the sealing plate out of the reaction pot through the electric, further improving the crystal washing effect of the 2, 4-dichlorophenol after standing in the reaction pot, and further improving the purification effect of the 2, 4-dichlorophenol; when the reaction pot swings, the sealing plate is separated from the reaction pot.

Preferably, the stirring rods are movably arranged on the flow guide pipe, and the upper end faces of the stirring rods are connected to the bottom end face of the sealing plate through connecting springs; the electric telescopic rod is hinged to the upper end face of the sealing cover; when the stirring rod is required to extend into the bottom end surface of the reaction pot, an operator controls the electric telescopic rod to extend out, the sealing plate can slide downwards in the reaction pot, and then the stirring rod can swing to the bottom end of the reaction pot under the compression of the connecting spring, so that the mixed solution in the reaction pot can be fully mixed and stirred; meanwhile, when the reaction pot needs to swing, an operator can drive the sealing plate to slide upwards through the electric telescopic rod, the stirring rod can swing upwards under the driving of the connecting spring, and the phenomenon that needle crystals 2, 4-dichlorophenol standing in the reaction pot are collided and broken due to too low stirring rod when the reaction pot swings to discharge cleaning wastewater is effectively prevented, so that the sufficient washing effect of the needle crystals 2, 4-dichlorophenol is influenced.

Preferably, a sliding groove is formed in the mounting head, and a sliding rod is arranged in the sliding groove in a sliding manner; the sliding rod is connected to the bottom end surface of the reaction pot through a rubber spring; the bottom end of the fixed rod is provided with a fixed iron block, and the fixed iron block penetrates through the magnet block to be in sliding contact with the electromagnet; when the installation sleeve works, when the electromagnet in the installation sleeve is electrically adsorbed on the magnet block at the bottom end of the installation head, the fixed iron block and the electromagnet can be adsorbed and attached by the sliding rod arranged in the installation head in a sliding mode under the adsorption force of the electromagnet, so that the installation head and the installation sleeve can be flexibly connected and can be stably and rotatably connected; meanwhile, the control unit can control the gap of the electromagnet to be electrified, so that the reaction pot can stop suddenly, the mixed solution in the reaction pot can generate wave shaking due to the sudden stop of the reaction pot, and the mixed solution in the reaction pot can generate the effect of stirring and mixing; simultaneously the electro-magnet loses behind the electricity and can make rubber spring drive the slide bar and strike the heating intracavity for the heat in the heating intracavity can produce the orbit, and then the mixed solution of increase heating chamber in to the reaction kettle carries out abundant rapid heating operation.

The method for purifying 2, 4-dichlorophenol is suitable for the use of the 2, 4-dichlorophenol purified by the purification device, and comprises the following steps:

s, raw material crushing: taking a certain amount of unpurified 2, 4-dichlorophenol blocky solid, sticking the blocky solid into powdery solid by using a grinding device, then opening a sealing cover of a tank body, and then putting the powdery 2, 4-dichlorophenol into a reaction pot;

s: water injection dissolution: injecting water with a certain proportion into the guide pipe through an external water injection pipe, wherein the water solution in the guide pipe can respectively flow into the guide cavity and then is injected into the rotating reaction pot through the guide holes, so as to infiltrate the 2, 4-dichlorophenol solid powder in the reaction pot, the reaction pot intermittently rotates, and a plurality of stirring rods inject the water solution into the reaction pot, so that the solid powder can be fully dissolved into the water solution; the water solution filled in the stirring rods can be used for injecting water to dissolve 2, 4-dichlorophenol powder solid in the reaction kettle, and the stirring of the stirring rods can accelerate the dissolution speed, so that the dissolution of the solid powder into the water solution can be accelerated, and the phenomenon that the solid powder is bonded on the bottom wall of the reaction kettle due to the fact that the reaction kettle is in a static state, and the rapid dissolution of the solid powder is influenced;

s, heating and dissolving: the driving motor stops rotating to enable the soaked aqueous solution and the solid powder to stand still, whether the liquid level of the aqueous solution flowing into the reaction pot is higher than 2-3 cm of the powder solid or not is observed, then the control unit controls the electric heating wire in the heating cavity to enable the temperature of the electric heating wire to rise to 4-8 ℃, and meanwhile the driving motor rotates to enable the mixing temperature of the aqueous solution and the solid powder in the reaction pot to be kept between 5-7 ℃;

s: impurity extraction: injecting a certain amount of n-propanolamine into the flow guide pipe through the injection device, so that the n-propanolamine is injected into the mixed solution in the reaction pot through the flow guide hole, and simultaneously, the reaction pot intermittently rotates, so that the stirring rod can inject the n-propanolamine, and can also perform mixing and stirring operation on the mixed solution and the n-propanolamine, wherein the stirring time is 25-35 min, and the color change of the mixed solution in the reaction pot is observed; stopping rotating the driving motor to enable the fine needle crystal mixed solution in the reaction pot to stand for 10-14 hours; the intermittent rotation of the reaction pot can cause the reaction pot to stop suddenly when rotating, the stop of the reaction pot can cause the mixed solution in the reaction pot to generate wave shaking, further the mixed solution in the reaction pot can generate the effect of stirring and mixing, the n-propanolamine can be fully mixed with the mixed water solution, and the adsorption and extraction effect of the n-propanolamine on impurities in the 2, 4-dichlorophenol is further improved;

s: washing and purifying: and (2) injecting aqueous solution into the reaction kettle through the flow guide pipe, wherein the injected aqueous solution can wash the upper surface of the 2, 4-dichlorophenol in the fine needle crystal shape, the rotation of the reaction kettle can accelerate the washing time, then the water is compressed and discharged through the sealing plate, the washing steps are fully carried out for 2-3 times, and then the purified 2, 4-dichlorophenol substance can be obtained by drying and heating through an electric heating wire.

The invention has the following beneficial effects:

1. according to the invention, through the matching of the rotating reaction kettle and the static stirring rods, the solid 2, 4-dichlorophenol powder put into the rotating reaction kettle can be accelerated to be dissolved into the aqueous solution under the filling of the aqueous solution filled into the stirring rods, and the phenomenon that the solid powder is bonded on the bottom wall of the reaction kettle due to the static state of the reaction kettle is prevented, so that the rapid dissolution of the solid powder is influenced; meanwhile, n-propanolamine is simultaneously injected into the rotating reaction pot through a plurality of stirring rods to be in mixed contact with the dissolved solid powder, so that the mixed contact of the n-propanolamine and the solid powder solution is increased, the extraction of impurity molecules in the 2, 4-dichlorophenol in an aqueous solution state is facilitated, and the purification effect of the 2, 4-dichlorophenol is further improved; meanwhile, the method is convenient for experimenters to carry out purification experiments on small batches of 2, 4-dichlorophenol, and improves the rapid and efficient purification operation of the 2, 4-dichlorophenol.

2. According to the invention, the mounting sleeve is connected with the magnetic adsorption type of the mounting head, the control unit can control the gap of the electromagnet to be electrified, so that the reaction pot can generate sudden stop, the sudden stop of the reaction pot can enable the mixed solution in the reaction pot to generate wave shaking, and the mixed solution in the reaction pot can generate stirring and mixing effects; simultaneously the electro-magnet loses behind the electricity and can make rubber spring drive the slide bar and strike the heating intracavity for the heat in the heating intracavity can produce the orbit, and then the mixed solution of increase heating chamber in to the reaction kettle carries out abundant rapid heating operation.

Drawings

The invention will be further explained with reference to the drawings.

FIG. 1 is a perspective view of the present invention;

FIG. 2 is a cross-sectional view of the present invention;

FIG. 3 is an enlarged view of a portion of FIG. 2 in accordance with the present invention;

FIG. 4 is a flow diagram of a purification method of the present invention;

in the figure: the reaction extraction device comprises a tank body 1, a sealing cover 2, a reaction extraction device 3, a supporting plate 31, a supporting column 32, an installation sleeve 33, an installation head 34, a magnet block 341, a sliding groove 342, a reaction pot 35, a heating cavity 351, a driving motor 36, a driving gear 37, a driven gear 38, a guide pipe 4, a stirring rod 5, a guide cavity 51, a guide hole 52, an electric telescopic rod 6, a sealing plate 7, an electric control valve pipe 8, an electric heating wire 9, an electric cylinder 10, an electromagnet 11, a push rod 12, a fixed column 13, a rubber spring 14, a connecting spring 15, a sliding rod 16 and a fixed iron block 17.

Detailed Description

An apparatus and a method for purifying 2, 4-dichlorophenol according to an embodiment of the present invention will be described below with reference to fig. 1 to 4.

As shown in fig. 1-4, the purification apparatus for 2, 4-dichlorophenol according to the present invention comprises a tank 1, a sealing cover 2 is slidably covered on the upper end of the tank 1, and a reaction extraction apparatus 3 is disposed in the tank 1; the reaction extraction device 3 comprises a support plate 31, a support column 32, a mounting sleeve 33, a mounting head 34, a reaction pot 35, a driving motor 36, a driving gear 37 and a driven gear 38; the supporting plate 31 is fixedly arranged at the bottom end of the tank body 1, and the supporting column 32 is rotatably arranged on the upper end surface of the supporting plate 31 through a bearing sleeve; a mounting sleeve 33 is fixed at the top end of the supporting column 32, and a mounting head 34 is electromagnetically adsorbed in the mounting sleeve 33; the reaction pot 35 is movably arranged in the mounting sleeve 33 through a mounting head 34; the driving motor 36 is fixed on the supporting plate 31, and the output end of the driving motor 36 is provided with a driving gear 37; a driven gear 38 is mounted on the supporting column 32, and the driven gear 38 is meshed with the driving gear 37; a flow guide pipe 4 is arranged on the sealing cover 2, a plurality of stirring rods 5 are obliquely arranged at the bottom end of the flow guide pipe 4 in the circumferential direction, and the bottom ends of the stirring rods 5 are positioned on the upper surface of the reaction pot 35; flow guide cavities 51 are formed in the stirring rods 5, and the flow guide cavities 51 are communicated with the flow guide pipe 4; a plurality of flow guide holes 52 are formed in the upper end face of the stirring rod 5, and the flow guide holes 52 are communicated with the flow guide cavity 51; a sealing plate 7 is sleeved on the flow guide pipe 4 in a sliding mode, and the sealing plate 7 is connected with the sealing cover 2 through an electric telescopic rod 6; the sealing plate 7 is arranged in the reaction pot 35 in a sliding manner, and the side wall of the reaction pot 35 is provided with an electric control valve pipe 8; a heating cavity 351 is formed in the bottom end of the reaction pot 35, and an electric heating wire 9 is arranged in the heating cavity 351;

when the device works, a certain amount of unpurified 2, 4-dichlorophenol blocky solid is taken and is stuck into powdery solid by a grinding device; then the sealing cover 2 of the tank body 1 is opened, then the powdery 2, 4-dichlorophenol is put into the reaction pot 35, then the sealing cover 2 is covered on the tank body 1, so that the stirring rod 5 is positioned in the reaction pot 35, then the control unit controls the driving motor 36 to rotate, the driving motor 36 drives the driven gear 38 to rotate through the driving gear 37, further the rotating support column 32 drives the reaction pot 35 which is inserted with the mounting head 34 through the mounting sleeve 33 to rotate, then the external water injection pipe injects a certain proportion of water into the flow guide pipe 4, the aqueous solution in the flow guide pipe 4 respectively flows into the flow guide cavity 51, then the aqueous solution is injected into the rotating reaction pot 35 through the flow guide hole 52, further the 2, 4-dichlorophenol solid powder in the reaction pot 35 is infiltrated, then the control unit controls the driving motor 36 to stop rotating, so that the infiltrated aqueous solution and the solid powder are kept standing, observing whether the liquid level of the aqueous solution flowing into the reaction kettle 35 is higher than 2-3 cm of the powder solid, controlling the electric heating wire 9 in the heating cavity 351 through the control unit to heat the electric heating wire 9 to 4-8 ℃, simultaneously driving the motor 36 to rotate to keep the mixing temperature of the aqueous solution and the solid powder in the reaction kettle 35 between 5-7 ℃, then injecting a certain amount of n-propanolamine into the flow guide pipe 4 through the injection device to inject the n-propanolamine into the mixed solution in the reaction kettle 35 through the flow guide hole 52, simultaneously rotating the reaction kettle 35 to inject the n-propanolamine into the stirring rod 5, simultaneously mixing and stirring the mixed solution and the n-propanolamine, wherein the stirring time is 25-35 min, simultaneously observing the color change of the mixed solution in the reaction kettle 35, and simultaneously stopping the rotation of the motor 36 after the mixed powder solution is changed into fine needle-shaped crystals, standing the fine needle crystal mixed solution in the reaction pot 35 for 10-14 h; then the control unit controls the electric telescopic rod 6 to extend out, the electric telescopic rod 6 can drive the sealing plate 7 to slide downwards in the reaction pot 35, the sliding of the sealing plate 7 can compress the volume in the reaction pot 35, meanwhile, the control unit controls the electric control valve pipe 8 to open, a water layer generated after the reaction pot 35 is stood still can be discharged out of the reaction pot 35 through the electric control valve pipe 8 under the compression of the sealing plate 7, after the water layer is discharged, the electric control valve pipe 8 is closed, the sealing plate 7 slides upwards, then water solution is injected into the reaction pot 35 through the guide pipe 4, then the driving motor 36 drives the reaction pot 35 to rotate, the injected water solution can wash the upper surface of the fine needle crystal-shaped 2, 4-dichlorophenol, the rotation of the reaction pot 35 can accelerate the washing time, then the water is compressed and discharged through the sealing plate 7, the steps are fully performed for 2-3 times, then drying and heating are performed through the electric heating wire 9, so as to obtain the purified 2, 4-dichlorophenol substance; through the matching of the rotating reaction kettle 35 and the static stirring rods 5, the solid 2, 4-dichlorophenol powder put into the rotating reaction kettle 35 can be accelerated to be dissolved into the aqueous solution under the filling of the aqueous solution filled into the stirring rods 5, and meanwhile, the phenomenon that the solid powder is bonded on the bottom wall of the reaction kettle 35 due to the fact that the reaction kettle 35 is in a static state is prevented, and the rapid dissolution of the solid powder is influenced; meanwhile, n-propanolamine is simultaneously injected into the rotating reaction pot 35 through the stirring rods 5 to be in mixed contact with dissolved solid powder, so that the mixed contact of n-propanolamine and solid powder solution is increased, the extraction of impurity molecules in the 2, 4-dichlorophenol in an aqueous solution state is facilitated, the purification effect of the 2, 4-dichlorophenol is further improved, meanwhile, the experiment for purifying the 2, 4-dichlorophenol in small batches is facilitated for experimenters, and the rapid and efficient purification operation of the 2, 4-dichlorophenol is improved.

As an embodiment of the present invention, the mounting head 34 is configured as a semi-spherical structure, the bottom end of the mounting head 34 is provided with a magnet block 341, and the upper end of the mounting head 34 is made of an elastic rubber material; the mounting sleeve 33 is of a bowl-shaped structure, the electromagnet 11 is arranged at the bottom end of the mounting sleeve 33, and the outer wall of the mounting sleeve 33 is made of elastic rubber; the during operation, when the jar body 1 is installed with reaction kettle 35 to needs in, earlier set up hemispherical installation head 34 with reaction kettle 35 bottom and insert in the installation cover 33 of bowl-shaped structure, then the control unit control electro-magnet 11 gets electricity, the electric meeting magnetic adsorption power that gets of electro-magnet 11 can adsorb magnet piece 341, and then adsorb installation head 34 in installation cover 33 through the mode of magnetic adsorption, the elastic rubber material that the outer wall of installation cover 33 upper end set up and the elastic rubber material that installs head 34 upper end set up, make and to form the flexible connection between reaction kettle 35 and the support column 32, and then be convenient for reaction kettle 35 can carry out quick dismantlement installation, the reaction kettle 35 of being convenient for simultaneously carries out whole rotation, carry out the stirring and mix to the mixed solution in the reaction kettle 35 under the cooperation of puddler 5.

As an embodiment of the present invention, the driving gear 37 is connected to the output end of the driving motor 36 through the electric cylinder 10, and the upper end surface of the driving gear 37 is provided with a plurality of ejector rods 12; the push rods 12 are all positioned at the bottom end of the reaction pot 35; a fixed column 13 is arranged on the upper end face of the supporting plate 31, and a rubber spring 14 is fixed at the top end of the fixed column 13; the top end of the rubber spring 14 is fixed with an electromagnet 11, and the electromagnet 11 is positioned right below the reaction pot 35; the fixed column 13 and the electric telescopic column are symmetrically arranged along the central line of the supporting column 32; when the automatic cleaning device works, when the waste water solution in the reaction pot 35 after being washed is required to be discharged, an operator can not only discharge the waste water solution in the reaction pot 35 through a mode that the sealing plate 7 compresses the space of the reaction pot 35, meanwhile, the operator can control the electric cylinder 10 to extend out through the control unit, the electromagnet 11 on the rubber spring 14 is electrified, the electromagnet 11 can be adsorbed to the bottom end face of the reaction pot 35, the electric cylinder 10 can drive the push rod 12 arranged on the driving gear 37 to move upwards, a flexible connection is formed between the mounting head 34 and the mounting sleeve 33, the push rod 12 can push the reaction pot 35 to incline towards one side of the rubber spring 14, the rubber spring 14 is compressed, when the electric telescopic rod 6 slides downwards, the compression rebound force of the rubber spring 14 can enable the reaction pot 35 to swing towards one side of the push rod 12, and then the reciprocating swing reaction pot 35 can discharge the cleaning waste water which is not compressed and discharged through the sealing plate 7 through the electric control valve pipe 8 Further improving the crystal washing effect of the 2, 4-dichlorophenol after standing in the reaction kettle 35, and further improving the purification effect of the 2, 4-dichlorophenol; when the reaction pot 35 swings, the sealing plate 7 is disengaged from the inside of the reaction pot 35.

As an embodiment of the present invention, a plurality of the stirring rods 5 are movably installed on the draft tube 4, and the upper end surfaces of the stirring rods 5 are connected to the bottom end surface of the sealing plate 7 through the connecting spring 15; the electric telescopic rod 6 is hinged on the upper end surface of the sealing cover 2; when the reaction kettle 35 rotates, the stirring rod 5 can stir the mixed solution in the reaction kettle 35, when the stirring rod 5 needs to extend into the bottom end surface of the reaction kettle 35, an operator controls the electric telescopic rod 6 to extend out, the sealing plate 7 can slide downwards in the reaction kettle 35, then the stirring rod 5 can swing to the bottom end of the reaction kettle 35 under the compression of the connecting spring 15, and the mixed solution in the reaction kettle 35 can be fully mixed and stirred; meanwhile, when the reaction pot 35 needs to swing, an operator can drive the sealing plate 7 to slide upwards through the electric telescopic rod 6, the stirring rod 5 can swing upwards under the driving of the connecting spring 15, and the phenomenon that needle crystals 2, 4-dichlorophenol standing in the reaction pot 35 are impacted and broken due to too low stirring rod 5 when the reaction pot 35 swings to discharge cleaning wastewater is effectively prevented, so that the sufficient washing effect of the needle crystals 2, 4-dichlorophenol is influenced.

As an embodiment of the present invention, a sliding groove 342 is formed in the mounting head 34, and a sliding rod 16 is slidably disposed in the sliding groove 342; the sliding rod 16 is connected to the bottom end surface of the reaction pot 35 through a rubber spring 14; a fixed iron block 17 is arranged at the bottom end of the fixed rod, and the fixed iron block 17 penetrates through the magnet block 341 to be in sliding contact with the electromagnet 11; when the installation sleeve 33 works, when the electromagnet 11 in the installation sleeve 33 is electrically adsorbed on the magnet block at the bottom end of the installation head 34, the sliding rod 16 arranged in the installation head 34 in a sliding mode enables the fixed iron block 17 to be adsorbed and attached to the electromagnet 11 under the adsorption force of the electromagnet 11, so that the installation head 34 and the installation sleeve 33 can be in flexible connection and can be in stable rotating connection; meanwhile, the control unit can control the gap of the electromagnet 11 to be electrified, so that the reaction pot 35 can generate sudden stop, and the sudden stop of the reaction pot 35 can enable the mixed solution in the reaction pot 35 to generate wave shaking, so that the mixed solution in the reaction pot 35 can generate the effect of stirring and mixing; meanwhile, after the electromagnet 11 is powered off, the rubber spring 14 can drive the sliding rod 16 to impact the heating cavity 351, so that the heat in the heating cavity 351 can be in an orbit, and then the heating cavity 351 can be increased to perform sufficient and rapid heating operation on the mixed solution in the reaction pot 35.

As shown in fig. 4, the method for purifying 2, 4-dichlorophenol according to the present invention is suitable for use of 2, 4-dichlorophenol purified by the above purification apparatus, and comprises the following steps:

s1, crushing the raw materials: taking a certain amount of unpurified 2, 4-dichlorophenol blocky solid, sticking the blocky solid into powdery solid by using a grinding device, then opening a sealing cover 2 of a tank body 1, and then putting the powdery 2, 4-dichlorophenol into a reaction pot 35;

s2: water injection dissolution: water with a certain proportion is injected into the guide pipe 4 through an external water injection pipe, the water solution in the guide pipe 4 respectively flows into the guide cavity 51 and then is injected into the rotating reaction pot 35 through the guide holes 52, so as to infiltrate the 2, 4-dichlorophenol solid powder in the reaction pot 35, the reaction pot 35 intermittently rotates, and the water solution is injected into the reaction pot 35 through the stirring rods 5, so that the solid powder can be fully dissolved into the water solution; the water solution filled in the stirring rods 5 can be used for injecting water to dissolve the 2, 4-dichlorophenol powder solid in the reaction kettle 35, and the stirring of the stirring rods 5 can accelerate the dissolving speed, so that the solid powder can be dissolved in the water solution, and the phenomenon that the solid powder is bonded on the bottom wall of the reaction kettle 35 due to the fact that the reaction kettle 35 is in a static state, and the rapid dissolving of the solid powder is influenced;

s3, heating and dissolving: the driving motor 36 stops rotating to enable the soaked aqueous solution and solid powder to stand still, whether the liquid level of the aqueous solution flowing into the reaction pot 35 is higher than 2-3 cm of the solid powder or not is observed, then the control unit controls the electric heating wire 9 in the heating cavity 351 to enable the temperature of the electric heating wire 9 to rise to 4-8 ℃, and meanwhile, the driving motor 36 rotates to enable the mixing temperature of the aqueous solution and the solid powder in the reaction pot 35 to be kept between 5-7 ℃;

s4: impurity extraction: injecting a certain amount of n-propanolamine into the flow guide pipe 4 through the injection device, so that the n-propanolamine is injected into the mixed solution in the reaction pot 35 through the flow guide hole 52, and simultaneously the reaction pot 35 intermittently rotates, so that the stirring rod 5 can inject the n-propanolamine and can perform mixing and stirring operation on the mixed solution and the n-propanolamine, the stirring time is 25-35 min, and the color change of the mixed solution in the reaction pot 35 is observed; stopping rotating the driving motor 36 to allow the fine needle crystal mixed solution in the reaction pot 35 to stand for 10-14 hours; the intermittent rotation of the reaction pot 35 can enable the reaction pot 35 to stop suddenly when rotating, the sudden stop of the reaction pot 35 can enable the mixed solution inside to shake in a wave mode, and further enable the mixed solution inside the reaction pot 35 to generate a stirring and mixing effect, so that n-propanolamine can be fully mixed with the mixed water solution, and the adsorption and extraction effects of the n-propanolamine on impurities in 2, 4-dichlorophenol are further improved;

s5: washing and purifying: injecting aqueous solution into the reaction pot 35 through the flow guide pipe 4, wherein the injected aqueous solution can wash the upper surface of the fine needle crystal-shaped 2, 4-dichlorophenol, the rotation of the reaction pot 35 can accelerate the washing time, then the fine needle crystal-shaped 2, 4-dichlorophenol is compressed and discharged through the sealing plate 7, the washing steps are fully carried out for 2-3 times, and then the purified 2, 4-dichlorophenol substance can be obtained by drying and heating through the electric heating wire 9.

The specific working process is as follows:

when the device works, a certain amount of unpurified 2, 4-dichlorophenol blocky solid is taken and is stuck into powdery solid by a grinding device; then, the sealing cover 2 of the tank body 1 is opened, then, powdery 2, 4-dichlorophenol is put into the reaction kettle 35, then, the sealing cover 2 is covered on the tank body 1, then, an external water injection pipe injects a certain proportion of water into the guide pipe 4, the water solution in the guide pipe 4 respectively flows into the guide cavity 51, then, the water solution is injected into the rotating reaction kettle 35 through the guide hole 52, then, 2, 4-dichlorophenol solid powder in the reaction kettle 35 is infiltrated, then, the control unit controls the driving motor 36 to stop rotating, so that the infiltrated water solution and the solid powder are kept standing, whether the liquid level of the water solution flowing into the reaction kettle 35 is higher than 2-3 cm of the powder solid is observed, then, the control unit controls the electric heating wire 9 in the heating cavity 351 to heat the electric heating wire 9 to 4-8 ℃, and then, a certain amount of n-propanolamine is injected into the guide pipe 4 through the injection device, injecting n-propanolamine into the mixed solution in the reaction pot 35 through the diversion holes 52, rotating the reaction pot 35 at the same time, injecting the n-propanolamine into the stirring rod 5, mixing and stirring the mixed solution and the n-propanolamine for 25-35 min, observing the color change of the mixed solution in the reaction pot 35, and stopping rotating the driving motor 36 after the mixed powder solution is changed into fine needle crystals, so that the fine needle crystal mixed solution in the reaction pot 35 is kept stand for 10-14 h; then the control unit controls the electric telescopic rod 6 to extend out, the electric telescopic rod 6 can drive the sealing plate 7 to slide downwards in the reaction pot 35, the sliding of the sealing plate 7 can compress the volume in the reaction pot 35, meanwhile, the control unit controls the electric control valve pipe 8 to open, a water layer generated after the reaction pot 35 is stood still can be discharged out of the reaction pot 35 through the electric control valve pipe 8 under the compression of the sealing plate 7, after the water layer is discharged, the electric control valve pipe 8 is closed, the sealing plate 7 slides upwards, then water solution is injected into the reaction pot 35 through the guide pipe 4, then the driving motor 36 drives the reaction pot 35 to rotate, the injected water solution can wash the upper surface of the fine needle crystal-shaped 2, 4-dichlorophenol, the rotation of the reaction pot 35 can accelerate the washing time, then the water is compressed and discharged through the sealing plate 7, the steps are fully performed for 2-3 times, then drying and heating are performed through the electric heating wire 9, so as to obtain the purified 2, 4-dichlorophenol substance.

In the description of the present invention, it is to be understood that the terms "center", "front", "rear", "vertical", "horizontal", "top", "bottom", "inner", "outer", etc., indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore, should not be taken as limiting the scope of the present invention.

While the invention has been described with reference to specific embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the scope of the invention. In addition, many modifications may be made to adapt a particular situation or material to the teachings of the invention without departing from its scope. Therefore, it is intended that the invention not be limited to the particular embodiment disclosed, but that the invention will include all embodiments falling within the scope of the appended claims.

Claims

1. A purification device of 2, 4-dichlorophenol is characterized in that: comprises a tank body (1), wherein the upper end of the tank body (1) is covered with a sealing cover (2) in a sliding way, and a reaction extraction device (3) is arranged in the tank body (1); the reaction extraction device (3) comprises a support plate (31), a support column (32), a mounting sleeve (33), a mounting head (34), a reaction pot (35), a driving motor (36), a driving gear (37) and a driven gear (38); the support plate (31) is fixedly arranged at the bottom end of the tank body (1), and the support column (32) is rotatably arranged on the upper end surface of the support plate (31) through a bearing sleeve; a mounting sleeve (33) is fixed at the top end of the supporting column (32), and a mounting head (34) is electromagnetically adsorbed in the mounting sleeve (33); the reaction pot (35) is movably arranged in the mounting sleeve (33) through a mounting head (34); the driving motor (36) is fixed on the supporting plate (31), and the output end of the driving motor (36) is provided with a driving gear (37); a driven gear (38) is mounted on the supporting column (32), and the driven gear (38) is meshed with the driving gear (37); the sealing cover (2) is provided with a flow guide pipe (4), a plurality of stirring rods (5) are obliquely arranged at the bottom end of the flow guide pipe (4) in the circumferential direction, and the bottom ends of the stirring rods (5) are positioned on the upper surface of the reaction pot (35); flow guide cavities (51) are formed in the stirring rods (5), and the flow guide cavities (51) are communicated with the flow guide pipe (4); a plurality of flow guide holes (52) are formed in the upper end face of the stirring rod (5), and the flow guide holes (52) are communicated with the flow guide cavity (51); a sealing plate (7) is sleeved on the flow guide pipe (4) in a sliding mode, and the sealing plate (7) is connected with the sealing cover (2) through an electric telescopic rod (6); the sealing plate (7) is arranged in the reaction pot (35) in a sliding manner, and the side wall of the reaction pot (35) is provided with an electric control valve pipe (8); heating cavity (351) has been seted up to the bottom inside of reaction pot (35), and is provided with electric heating wire (9) in heating cavity (351).

2. The purification device of 2, 4-dichlorophenol according to claim 1, characterized in that: the mounting head (34) is of a semi-spherical structure, the bottom end of the mounting head (34) is provided with a magnet block (341), and the upper end of the mounting head (34) is made of elastic rubber; the mounting sleeve (33) is of a bowl-shaped structure, the bottom end of the mounting sleeve (33) is provided with the electromagnet (11), and the outer wall of the mounting sleeve (33) is made of elastic rubber.

3. The purification device of 2, 4-dichlorophenol according to claim 2, characterized in that: the driving gear (37) is connected with the output end of the driving motor (36) through the electric cylinder (10), and a plurality of ejector rods (12) are arranged on the upper end face of the driving gear (37); the push rods (12) are all positioned at the bottom end of the reaction pot (35); a fixed column (13) is arranged on the upper end face of the supporting plate (31), and a rubber spring (14) is fixed at the top end of the fixed column (13); an electromagnet (11) is fixed at the top end of the rubber spring (14), and the electromagnet (11) is positioned right below the reaction pot (35); the fixed column (13) and the electric telescopic device are symmetrically arranged along the center line of the supporting column (32).

4. The purification device of 2, 4-dichlorophenol according to claim 1, characterized in that: the stirring rods (5) are movably arranged on the flow guide pipe (4), and the upper end faces of the stirring rods (5) are connected to the bottom end face of the sealing plate (7) through connecting springs (15); the electric telescopic rod (6) is hinged on the upper end face of the sealing cover (2).

5. The apparatus for purifying 2, 4-dichlorophenol according to claim 4, wherein: a sliding groove (342) is formed in the mounting head (34), and a sliding rod (16) is arranged in the sliding groove (342) in a sliding manner; the sliding rod (16) is connected to the bottom end surface of the reaction pot (35) through a rubber spring (14); the bottom end of the fixed rod is provided with a fixed iron block (17), and the fixed iron block (17) penetrates through the magnet block (341) to be in sliding contact with the electromagnet (11).

6. A method for purifying 2, 4-dichlorophenol is characterized by comprising the following steps: the method is suitable for the 2, 4-dichlorophenol purified by the purification device of any one of claims 1 to 5, and comprises the following steps:

s1, crushing the raw materials: taking a certain amount of unpurified 2, 4-dichlorophenol blocky solid, sticking the blocky solid into powdery solid by using a grinding device, then opening a sealing cover (2) of a tank body (1), and then putting the powdery 2, 4-dichlorophenol into a reaction pot (35);

s2: water injection dissolution: water with a certain proportion is injected into the guide pipe (4) through an external water injection pipe, water solution in the guide pipe (4) can respectively flow into the guide cavity (51), then the water solution is injected into the rotating reaction pot (35) through the guide holes (52), then 2, 4-dichlorophenol solid powder in the reaction pot (35) is infiltrated, the reaction pot (35) intermittently rotates, and the water solution is injected into the reaction pot (35) through the stirring rods (5) so that the solid powder can be fully dissolved into the water solution;

s3, heating and dissolving: the driving motor (36) stops rotating, so that the soaked aqueous solution and solid powder are allowed to stand, whether the liquid level of the aqueous solution flowing into the reaction pot (35) is higher than 2-3 cm of the powder solid or not is observed, then the control unit controls the electric heating wire (9) in the heating cavity (351) to heat the electric heating wire (9) to 4-8 ℃, and meanwhile, the driving motor (36) rotates, so that the mixing temperature of the aqueous solution and the solid powder in the reaction pot (35) is kept between 5-7 ℃;

s4: impurity extraction: injecting a certain amount of n-propanolamine into the flow guide pipe (4) through the injection device, so that the n-propanolamine is injected into the mixed solution in the reaction pot (35) through the flow guide hole (52), and meanwhile, the reaction pot (35) intermittently rotates, so that the stirring rod (5) can inject the n-propanolamine and can also perform mixing and stirring operation on the mixed solution and the n-propanolamine, the stirring time is 25-35 min, and meanwhile, the color change of the mixed solution in the reaction pot (35) is observed; and (3) stopping the rotation of the driving motor (36) to enable the fine needle-shaped crystal mixed solution in the reaction pot (35) to stand for 10-14 hours.