CN213555437U

CN213555437U - Purification device of 4-chloroacetoacetic acid methyl ester

Info

Publication number: CN213555437U
Application number: CN202021787663.XU
Authority: CN
Inventors: 王海根
Original assignee: Jiangsu Hengan Chemical Co ltd
Current assignee: Jiangsu Hengan Chemical Co ltd
Priority date: 2020-08-25
Filing date: 2020-08-25
Publication date: 2021-06-29
Anticipated expiration: 2030-08-25

Abstract

The utility model discloses a purification device of 4-chloroacetoacetic acid methyl ester, which relates to the technical field of chemical equipment and solves the problems that after the product is heated and evaporated by the prior distillation purification device, a small amount of steam can not be emitted out of the interior of the distillation box, the purity of the product is reduced, the technical scheme is characterized by comprising a distillation box, wherein a feeding pipe is arranged on the distillation box, a discharging pipe is arranged at the bottom of the distillation box, a valve is fixedly connected on the discharging pipe, and the effect is that an electric push rod and a movable cover are arranged, in the rectification process, the electric push rod drives the movable cover to move in the vertical direction, because the side surface of the movable cover is contacted with the side surface of the inner cavity of the distillation box, all of the steam will thus be discharged from the first connecting pipe through the moving hood, adjusted so that the bottom of the moving hood is always located a short distance above the material inside the distillation box. This ensures that all the steam in the distillation tank can be removed from the first connection.

Description

Purification device of 4-chloroacetoacetic acid methyl ester

Technical Field

The utility model relates to a chemical industry equipment technical field, more specifically say, it relates to a purification device of 4-chloroacetoacetic acid methyl ester.

Background

Methyl 4-chloroacetoacetate is an intermediate in organic synthesis, and is a pale yellow solid or liquid.

The conventional production method of the methyl 4-chloroacetoacetate mainly used in the industrial production at present comprises the following steps: the intermittent production method comprises the steps of dissolving diketene in a solvent, cooling and stirring the diketene, introducing a certain amount of chlorine into a reaction kettle at a certain flow rate, dripping a certain amount of methanol into the reaction kettle after chlorination reaction, neutralizing the reaction kettle with alkali after esterification reaction, evaporating the solvent, and then distilling under reduced pressure to obtain a colorless liquid product, namely 4-methyl chloroacetoacetate.

SUMMERY OF THE UTILITY MODEL

Aiming at the defects in the prior art, the utility model aims to provide a purification device of 4-chloroacetoacetic acid methyl ester, which can completely release steam obtained by distillation.

In order to achieve the above purpose, the utility model provides a following technical scheme: the utility model provides a purification device of 4-methyl chloroacetoacetate, includes the distillation box, be equipped with the inlet pipe on the distillation box, the bottom of distillation box is equipped with the discharging pipe, fixedly connected with valve on the discharging pipe, the inner chamber of distillation box is equipped with the zone of heating, the inside of zone of heating is equipped with the heating pipe, the inside of distillation box is equipped with movable cover, the side of activity cover and the side contact of distillation box inner chamber, and the top of distillation box is equipped with the actuating mechanism who drives movable cover oscilaltion, the first connecting pipe of top fixedly connected with of activity cover, the one end that absorbing mechanism was kept away from to first connecting pipe extends distillation box and fixedly connected with condensation mechanism, condensation mechanism's bottom is equipped with the receipts material pipe.

The utility model discloses a distillation box, including the distillation box, actuating mechanism, still, the top of distillation box is connected with the top of electric push rod, the top of push rod and activity cover is fixed connection, and the top of push rod extends the distillation box to with electric push rod fixed connection, the top fixedly connected with mounting bracket of distillation box, electric push rod fixed mounting is on the mounting bracket, fixedly connected with wavy pipe on the first connecting pipe, and the wavy pipe is located the inside of distillation box.

The heating layer the quantity of heating pipe is a plurality of, and a plurality of heating pipes evenly distributed is in the inside of heating layer.

The condensing mechanism comprises a condensing box, an air pump and a spiral pipe, the spiral pipe is located inside the condensing box, the condensing box is extended from two ends of the spiral pipe, which are extended from the condensing box, are located at the upper end and the lower end of the side surface of the condensing box respectively, a second connecting pipe is fixedly connected with one end of the spiral pipe and is located at the upper end of the side surface of the condensing box, one end of the spiral pipe, which is far away from the spiral pipe, is fixedly connected with the first connecting pipe, the air pump is located below the second connecting pipe, a material receiving pipe is fixedly connected with the bottom of the spiral pipe, the material receiving pipe extends out of the condensing box, and an A mechanism for spraying cold water on the spiral.

The spiral pipe is of a spiral structure.

The utility model discloses a mechanism, the mechanism of A includes water-cooling tank and shower nozzle, water-cooling tank fixed mounting is at the top of condensing box, and the top fixedly connected with water tank of condensing box, through third connecting pipe fixed connection between water tank and the water-cooling tank, the top fixed connection of fourth connecting pipe and condensing box is passed through to the bottom of water-cooling tank, the fifth connecting pipe of top fixedly connected with of condensing box inner chamber, the sixth connecting pipe of bottom fixedly connected with of fifth connecting pipe, and the sixth connecting pipe is located the inside of spiral pipe, the shower nozzle is evenly installed in the bottom of fifth connecting pipe and the side of sixth connecting pipe, the top fixed connection of seventh connecting pipe and water-cooling tank is passed through to the bottom of condensing box, and fixed mounting has the water pump on the seventh connecting pipe.

The sixth connecting pipe is of a spiral structure, and the spiral curvature of the sixth connecting pipe is the same as the spiral curvature of the spiral pipe.

The second connecting pipe is of an inclined structure, and the connecting end of the second connecting pipe and the first connecting pipe is lower in height.

By adopting the technical scheme, the method has the advantages that,

1. through setting up electric push rod and movable cover, at the in-process of rectification, utilize the electric push rod to drive the movable cover and move in vertical direction, because the side of movable cover contacts with the side of distillation retort inner chamber, then all steam can be followed through the movable cover and discharged from first connecting pipe like this, adjust the bottom that makes the movable cover be located the distillation retort inside material top very near distance all the time. This ensures that all the steam in the distillation tank can be removed from the first connection.

2. Through setting up fifth connecting pipe and sixth connecting pipe, the shower nozzle that utilizes on the fifth connecting pipe sprays from the top of spiral pipe to can spray the outside of spiral pipe, utilize the sixth connecting pipe to spray the inside of spiral pipe, because sixth connecting pipe and spiral pipe all are helical structure, and the degree of their spiral is the same, make shower nozzle on the sixth connecting pipe can spray all corners of spiral pipe medial surface to, improve the refrigerated effect of device.

Drawings

FIG. 1 is a schematic diagram of an embodiment of the present invention;

FIG. 2 is a sectional view of a condenser case according to an embodiment of the present invention;

fig. 3 is a top view of a sixth connecting pipe according to an embodiment of the present invention;

fig. 4 is a cross-sectional view of a distillation box according to an embodiment of the present invention.

1. A distillation box; 2. a first connecting pipe; 3. a feed pipe; 4. a valve; 5. a discharge pipe; 6. A water pump; 7. a seventh connecting pipe; 8. a spiral tube; 9. an air pump; 10. a second connecting pipe; 11. A condenser tank; 12. a water tank; 13. a third connecting pipe; 14. a water cooling tank; 15. a wave tube; 16. A material receiving pipe; 17. a fifth connecting pipe; 18. a sixth connecting pipe; 19. a fourth connecting pipe; 20. A spray head; 21. a mounting frame; 22. an electric push rod; 23. a heating layer; 24. heating a tube; 25. a push rod; 26. a movable cover.

Detailed Description

The utility model relates to a purification device of 4-methyl chloroacetoacetate, which is disclosed by the invention, by referring to figures 1 to 4. The examples are further illustrated.

The utility model provides a purification device of 4-methyl chloroacetoacetate, see figure 1 and 4, including distillation box 1, be equipped with inlet pipe 3 on the distillation box 1, the bottom of distillation box 1 is equipped with discharging pipe 5, fixedly connected with valve 4 on the discharging pipe 5, the inner chamber of distillation box 1 is equipped with zone of heating 23, the inside of zone of heating 23 is equipped with heating pipe 24, the inside of distillation box 1 is equipped with movable cover 26, the side of movable cover 26 contacts with the side of distillation box 1 inner chamber, and the top of distillation box 1 is equipped with the actuating mechanism who drives movable cover 26 oscilaltion, the first connecting pipe 2 of top fixedly connected with of movable cover 26, the one end that absorbing mechanism was kept away from to first connecting pipe 2 extends distillation box 1 and fixedly connected with condensation mechanism, the bottom of condensation mechanism is equipped with receipts material. Introducing the material into the distillation box 1 from the feeding pipe 3, heating the material in the distillation box 1 by using the heating pipe 24, keeping the temperature in the distillation box 1 within a certain range, discharging impurities into steam from the first connecting pipe 2, leaving methyl 4-chloroacetoacetate which does not become steam in the distillation box 1, condensing the discharged steam by using a condensing mechanism, discharging the liquid obtained by condensation from the material receiving pipe 16, because the side surface of the movable cover 26 is contacted with the side surface of the inner cavity of the distillation box 1, the steam is always positioned below the movable cover 26, the movable cover 26 is driven by the driving mechanism to move in the vertical direction, even if only a small amount of steam exists in the interior of the final distillation box 1, the small amount of steam can still be discharged from the first connecting pipe 2, the distillation purity of the device is improved, finally, the valve 4 is opened, and the purified methyl 4-chloroacetoacetate is discharged from the discharging pipe 5.

See fig. 4, actuating mechanism includes push rod 25 and electric push rod 22, the top fixed connection of push rod 25 and movable cover 26, and the top of push rod 25 extends distillation box 1 to with electric push rod 22 fixed connection, the top fixed connection of distillation box 1 has mounting bracket 21, electric push rod 22 fixed mounting is on mounting bracket 21, fixedly connected with wavy pipe 15 on first connecting pipe 2, and wavy pipe 15 is located the inside of distillation box 1. The electric push rod 22 is used for driving the push rod 25 and the movable cover 26 to move in the vertical direction, and the wavy tube 15 has a shrinking function, so that the movable cover 26 can stably slide in the vertical direction.

Referring to fig. 4, the heating layer 23 includes a plurality of heating pipes 24, and the plurality of heating pipes 24 are uniformly distributed inside the heating layer 23. The heating pipes 24 are uniformly distributed, so that the materials in the distillation box 1 can be uniformly heated, and the evaporation effect of the materials is improved.

See fig. 1 and 2, condensation mechanism includes condensing box 11, air pump 9 and spiral pipe 8, spiral pipe 8 is located the inside of condensing box 11, condensing box 11 all extends at the both ends of spiral pipe 8, and the both ends that spiral pipe 8 extends are located the upper and lower both ends of condensing box 11 side respectively, spiral pipe 8's one end fixedly connected with second connecting pipe 10, second connecting pipe 10 is located the upper end of condensing box 11 side, spiral pipe 8's other end second connecting pipe 10 is kept away from the one end of spiral pipe 8 all with first connecting pipe 2 fixed connection,

air pump

9 and 2 fixed connection of first connecting pipe, and air pump 9 is located the below of second connecting pipe 10, receive the bottom fixed connection of material pipe 16 with spiral pipe 8, and receive material pipe 16 and extend condensing box 11, condensing box 11's inside is equipped with the a mechanism that sprays cold water to spiral pipe 8. The steam emitted from the first connecting pipe 2 is pumped into the spiral pipe 8 by the air pump 9, the mechanism A cools the steam positioned inside the spiral pipe 8, the cooled liquid is discharged from the material receiving pipe 16, and the steam which is not changed into liquid enters the first connecting pipe 2 again along the second connecting pipe 10, and the circulation is repeated until all the steam is condensed and is called liquid discharge.

Referring to fig. 2, the spiral tube 8 has a spiral structure. The spiral structure of the spiral pipe 8 prolongs the stay time of the steam in the spiral pipe 8, and also prolongs the cooling time of the steam, and improves the cooling effect.

See fig. 2 and 3, the a mechanism includes a water cooling tank 14 and a spray head 20, the water cooling tank 14 is fixedly installed at the top of the condensation tank 11, and the top fixedly connected with water tank 12 of the condensation tank 11, through a third connecting pipe 13 fixedly connected between the water tank 12 and the water cooling tank 14, the bottom of the water cooling tank 14 is fixedly connected with the top of the condensation tank 11 through a fourth connecting pipe 19, the top fixedly connected with fifth connecting pipe 17 of the inner cavity of the condensation tank 11, the bottom fixedly connected with sixth connecting pipe 18 of the fifth connecting pipe 17, and the sixth connecting pipe 18 is located inside the spiral pipe 8, the spray head 20 is uniformly installed at the bottom of the fifth connecting pipe 17 and the side of the sixth connecting pipe 18, the bottom of the condensation tank 11 is fixedly connected with the top of the water cooling tank 14 through a seventh connecting pipe 7, and a water pump 6 is fixedly installed on the. The water-cooling box 14 cools off water, and refrigerated water passes through fifth connecting pipe 17 and sixth connecting pipe 18, and shower nozzle 20 spun water is the cooling water, and shower nozzle 20 on the fifth connecting pipe 17 sprays from the top of spiral pipe 8 to irrigate spiral pipe 8's lateral surface is whole, and sixth connecting pipe 18 is located spiral pipe 8's inside, sprays spiral pipe 8's medial surface.

Referring to fig. 3, the sixth connecting pipe 18 has a spiral structure, and the spiral of the sixth connecting pipe 18 has the same curvature as that of the spiral pipe 8. Thus, the spray head 20 fixedly connected with the sixth connecting pipe 18 sprays cold water to all corners of the inner side surface of the spiral pipe 8, and the cooling effect of the device is improved.

Referring to fig. 1, the second connection pipe 10 has an inclined structure, and the height of the connection end of the second connection pipe 10 and the first connection pipe 2 is relatively low. The steam which is not cooled into liquid in the spiral pipe 8 enters the first connecting pipe 2 from the second connecting pipe 10, and the inclined structure of the second connecting pipe 10 can ensure that the steam which is not cooled in the first connecting pipe 2 cannot directly enter the spiral pipe 8 from the top of the spiral pipe 8 through the second connecting pipe 10, so that all the steam can enter the spiral pipe 8 from the bottom of the spiral pipe 8.

The working principle is as follows: firstly, the movable cover 26 is lifted to the highest position, then the material to be purified is introduced into the distillation box 1 from the feeding pipe 3, the heating pipe 24 heats the material in the distillation box 1, the temperature in the distillation box 1 is controlled within a certain range, the material which becomes steam within the range enters the spiral pipe 8 in the condensation box 11 from the first connecting pipe 2, the spray head 20 sprays the spiral pipe 8, so that the material in the spiral pipe 8 is cooled, the cooled liquid is discharged from the material receiving pipe 16, when the steam is cooled, the electric push rod 22 can be used for driving the wave pipe 15 and the movable cover 26 to move downwards, all the steam in the distillation box 1 is ensured to be discharged from the first connecting pipe 2, the distillation is finished, finally, the valve 4 is opened, and the purified 4-methyl chloroacetoacetate is discharged from the discharging pipe 5.

It is above only the utility model discloses a preferred embodiment, the utility model discloses a scope of protection does not only confine above-mentioned embodiment, the all belongs to the utility model discloses a technical scheme under the thinking all belongs to the utility model discloses a scope of protection. It should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims

1. A purification device of 4-methyl chloroacetoacetate comprises a distillation box (1) and is characterized in that: the distillation box (1) is provided with a feeding pipe (3), the bottom of the distillation box (1) is provided with a discharging pipe (5), a valve (4) is fixedly connected on the discharge pipe (5), a heating layer (23) is arranged in the inner cavity of the distillation box (1), a heating pipe (24) is arranged inside the heating layer (23), a movable cover (26) is arranged inside the distillation box (1), the side surface of the movable cover (26) is contacted with the side surface of the inner cavity of the distillation box (1), and the top of the distillation box (1) is provided with a driving mechanism for driving the movable cover (26) to lift up and down, the top of the movable cover (26) is fixedly connected with a first connecting pipe (2), one end of the first connecting pipe (2) far away from the absorption mechanism extends out of the distillation box (1) and is fixedly connected with a condensation mechanism, and a material receiving pipe (16) is arranged at the bottom of the condensation mechanism.

2. The apparatus for purifying methyl 4-chloroacetoacetate of claim 1, wherein: actuating mechanism includes push rod (25) and electric push rod (22), the top fixed connection of push rod (25) and activity cover (26), and the top of push rod (25) extends distillation case (1) to with electric push rod (22) fixed connection, the top fixedly connected with mounting bracket (21) of distillation case (1), electric push rod (22) fixed mounting is on mounting bracket (21), fixedly connected with wave pipe (15) on first connecting pipe (2), and wave pipe (15) are located the inside of distillation case (1).

3. The apparatus for purifying methyl 4-chloroacetoacetate of claim 1, wherein: the heating pipes (24) are distributed in a plurality, and the heating pipes (24) are uniformly distributed in the heating layer (23).

4. The apparatus for purifying methyl 4-chloroacetoacetate of claim 1, wherein: the condensation mechanism comprises a condensation box (11), an air pump (9) and a spiral pipe (8), the spiral pipe (8) is positioned inside the condensation box (11), the condensation box (11) extends out of the two ends of the spiral pipe (8), the two extending ends of the spiral pipe (8) are respectively positioned at the upper end and the lower end of the side surface of the condensation box (11), one end of the spiral pipe (8) is fixedly connected with a second connecting pipe (10), the second connecting pipe (10) is positioned at the upper end of the side surface of the condensation box (11), one end, far away from the spiral pipe (8), of the second connecting pipe (10) at the other end of the spiral pipe (8) is fixedly connected with a first connecting pipe (2), the air pump (9) is fixedly connected with the first connecting pipe (2), the air pump (9) is positioned below the second connecting pipe (10), and the material receiving pipe (16) is fixedly connected with the bottom of the spiral pipe (, and the material receiving pipe (16) extends out of the condensation box (11), and an A mechanism for spraying cold water on the spiral pipe (8) is arranged in the condensation box (11).

5. The apparatus for purifying methyl 4-chloroacetoacetate of claim 4, wherein: the spiral tube (8) is of a spiral structure.

6. The apparatus for purifying methyl 4-chloroacetoacetate of claim 4, wherein: the A mechanism comprises a water cooling tank (14) and a spray head (20), the water cooling tank (14) is fixedly installed at the top of a condensation tank (11), the top of the condensation tank (11) is fixedly connected with a water tank (12), the water tank (12) and the water cooling tank (14) are fixedly connected through a third connecting pipe (13), the bottom of the water cooling tank (14) is fixedly connected with the top of the condensation tank (11) through a fourth connecting pipe (19), the top of the inner cavity of the condensation tank (11) is fixedly connected with a fifth connecting pipe (17), the bottom of the fifth connecting pipe (17) is fixedly connected with a sixth connecting pipe (18), the sixth connecting pipe (18) is located inside a spiral pipe (8), the spray head (20) is uniformly installed at the bottom of the fifth connecting pipe (17) and the side face of the sixth connecting pipe (18), the bottom of the condensation tank (11) is fixedly connected with the top of the water cooling tank (14) through a seventh connecting pipe (7), and a water pump (6) is fixedly arranged on the seventh connecting pipe (7).

7. The apparatus for purifying methyl 4-chloroacetoacetate of claim 6, wherein: the sixth connecting pipe (18) is of a spiral structure, and the spiral curvature of the sixth connecting pipe (18) is the same as the spiral curvature of the spiral pipe (8).

8. The apparatus for purifying methyl 4-chloroacetoacetate of claim 4, wherein: the second connecting pipe (10) is of an inclined structure, and the height of the connecting end of the second connecting pipe (10) and the first connecting pipe (2) is lower.