CN211570501U

CN211570501U - Hexabromocyclododecane production device

Info

Publication number: CN211570501U
Application number: CN201922490089.5U
Authority: CN
Inventors: 孙仿建; 单体明; 袁令华; 王艳红
Original assignee: WEIFANG YUKAI CHEMICAL CO Ltd
Current assignee: WEIFANG YUKAI CHEMICAL CO Ltd
Priority date: 2019-12-31
Filing date: 2019-12-31
Publication date: 2020-09-25
Anticipated expiration: 2029-12-31

Abstract

The utility model discloses a hexabromocyclododecane apparatus for producing, including reation kettle, the reation kettle intercommunication has first centrifuge, and the export of pans communicates stills, reation kettle and first centrifuge's liquid return mouth respectively, stills's upper portion intercommunication has first condenser, stills's lower part export intercommunication has the mother liquor jar, the mother liquor jar intercommunication reation kettle, the lower part export intercommunication of alkali wash cauldron has second centrifuge. Can realize that first centrifuge reaches reation kettle and stills to two kinds of ways of returning the cover back of reation kettle, increase the reuse to the waste material, improve the productivity of hexabromocyclododecane product, the solvent purity that centrifugation and distillation obtained is higher, can used repeatedly, has practiced thrift the cost.

Description

Hexabromocyclododecane production device

Technical Field

The utility model relates to the field of mechanical equipment, concretely relates to hexabromocyclododecane apparatus for producing.

Background

The product is white crystalline powder with theoretical bromine content of 74.71% and density of 2.36g/cm³The flame retardant has excellent thermal stability and good dispersibility, is an alicyclic flame retardant with high bromine content, and has the characteristics of low consumption, good flame retardant effect, small influence on the physical properties of materials and the like. The flame retardant is used for flame retardance of polypropylene plastics, fibers and polystyrene foam plastics, and can also be used for flame retardant after-finishing of polyester fabrics and flame retardance of vinylon plastic-coated double-sided leather. The flame retardant is used as an additive type flame retardant and is suitable for polystyrene, unsaturated polyester, polycarbonate, polypropylene, synthetic rubber and the like.

At present, most Hexabromocyclododecane (HBCD) is prepared by carrying out bromination addition reaction on 1,5, 9-Cyclododecatriene (CDT) and bromine in several mixed solvents such as isobutanol and trichloromethane, the yield of hexabromocyclododecane obtained after alkali washing is about 86%, the yield is low, the solvent can be recovered after centrifugation, but a large amount of hexabromocyclododecane exists in the solvent after centrifugation, so that serious waste is caused, the purity of the solvent is influenced, meanwhile, the mother liquor generated after distillation is difficult to process, and in addition, more hexabromocyclododecane exists in the mother liquor, so that the waste is caused when the hexabromocyclododecane is directly treated as hazardous waste.

Disclosure of Invention

The utility model discloses the technical problem that will solve is: to the not enough that prior art exists, provide a hexabromocyclododecane apparatus for producing, the liquid material that produces the centrifugation that can be selective and the mother liquor that the distillation produced carry out the returning cover and handle, improved hexabromocyclododecane's rate of recovery greatly, avoided the waste, the waste that causes when mother liquor returning cover handles and has also reduced the independent processing mother liquor simultaneously.

In order to solve the technical problem, the technical scheme of the utility model is that:

a hexabromocyclododecane production device comprises a reaction kettle, wherein a material outlet of the reaction kettle is communicated with a first centrifugal machine, the first centrifugal machine is provided with a liquid material outlet, a solid material outlet and a liquid return port, the liquid material outlet is communicated with an intermediate tank, and the solid material outlet is communicated with an alkaline washing kettle;

an outlet of the intermediate tank is respectively communicated with a distillation kettle, the reaction kettle and a liquid return port of the first centrifuge, the upper part of the distillation kettle is communicated with a first condenser, a lower outlet of the distillation kettle is communicated with a mother liquor tank, the mother liquor tank is communicated with the reaction kettle, the first condenser is communicated with a first solvent collecting tank, and the first condenser is connected with a vacuum system;

and an outlet at the upper part of the alkaline washing kettle is communicated with a second condenser, the second condenser is communicated with a second solvent collecting tank, an outlet at the lower part of the alkaline washing kettle is communicated with a second centrifuge, a liquid material outlet of the second centrifuge is communicated with a waste liquid tank, and a solid material outlet of the second centrifuge is communicated with a finished product transfer tank.

As a preferred technical scheme, a liquid outlet of the first centrifuge is connected with an inlet of a centrifugal pump, the first centrifuge is provided with a liquid return pipe, the liquid return pipe is provided with a liquid return port and a pressurization port, an outlet of the centrifugal pump is respectively communicated with the distillation kettle and the liquid return port, and valves are respectively arranged between the centrifugal pump and the distillation kettle and between the centrifugal pump and the liquid return pipe; the first centrifugal machine comprises an outer barrel and a rotary drum, the liquid return pipe extends into the rotary drum and is provided with a plurality of spray headers in a vertically staggered manner, outlets of the spray headers face the inner wall of the rotary drum, and the liquid return pipe is fixedly connected with the outer barrel; the rotary drum is characterized by further comprising a motor, wherein the motor is rotatably connected with a rotating shaft, and the rotating shaft penetrates through the outer barrel and is fixedly connected with the bottom of the rotary drum.

Preferably, the liquid return pipe is provided with a pressurizing port, and the pressurizing port is connected with an air source.

As an improved technical scheme, the second condenser is connected with a vacuum pump.

As an improved technical scheme, a vacuum catcher is arranged between the first solvent collecting tank and the vacuum system.

Since the technical scheme is used, the beneficial effects of the utility model are that:

the utility model discloses a hexabromocyclododecane production device, which comprises a reaction kettle, wherein a material outlet of the reaction kettle is communicated with a first centrifugal machine, the first centrifugal machine is provided with a liquid material outlet, a solid material outlet and a liquid return port, the liquid material outlet is communicated with a middle tank, and the solid material outlet is communicated with an alkali washing kettle; an outlet of the intermediate tank is respectively communicated with a distillation kettle, the reaction kettle and a liquid return port of the first centrifuge, the upper part of the distillation kettle is communicated with a first condenser, a lower outlet of the distillation kettle is communicated with a mother liquor tank, the mother liquor tank is communicated with the reaction kettle, the first condenser is communicated with a first solvent collecting tank, and the first condenser is connected with a vacuum system; and an outlet at the upper part of the alkaline washing kettle is communicated with a second condenser, the second condenser is communicated with a second solvent collecting tank, an outlet at the lower part of the alkaline washing kettle is communicated with a second centrifuge, a liquid material outlet of the second centrifuge is communicated with a waste liquid tank, and a solid material outlet of the second centrifuge is communicated with a finished product transfer tank. The utility model discloses a production device can realize first centrifuge and to reation kettle and stills to two kinds of ways of returning the cover of reation kettle, can adopt first centrifuge's liquid product to reation kettle's way of returning the cover when detecting final product index not very ideal, can adopt stills's mother liquor to reation kettle's way of returning the cover when detecting final product index can also, the reuse to the waste material has been realized, the productivity of hexabromocyclododecane product has been improved, the cost that the mother liquor caused has been reduced to the while, the solvent purity that centrifugation and distillation obtained is higher, can used repeatedly, and the cost is saved.

The second condenser of the utility model is connected with a vacuum pump, and can accelerate the cooling absorption of the gaseous solvent in the alkaline washing kettle.

The vacuum catcher is arranged between the first solvent collecting tank and the vacuum system, the barrier is additionally arranged between the first solvent collecting tank and the vacuum system, the solvent is prevented from being sucked into the vacuum system, on one hand, the waste of the solvent is reduced, and on the other hand, the solvent is prevented from damaging the vacuum system equipment.

Drawings

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

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

FIG. 2 is a schematic illustration of the first centrifuge of FIG. 1;

in the figure, 1, a reaction kettle; 2. a first centrifuge; 21. a liquid discharge port; 22. a centrifugal pump; 23. a liquid return pipe; 231. a liquid return port; 232. a pressurizing port; 233. a shower head; 24. a valve; 25. an outer cylinder; 26. a drum; 27. a motor; 28. a rotating shaft; 29. mechanical sealing; 3. an intermediate tank; 4. an alkaline washing kettle; 5. a distillation kettle; 6. a first condenser; 7. a first solvent collection tank; 8. a mother liquor tank; 9. a second condenser; 10. a second solvent collection tank; 11. a second centrifuge; 12. a waste liquid tank; 13. a finished product transfer tank; 14. a vacuum system.

Detailed Description

The invention is further explained below with reference to the drawings and examples.

As shown in fig. 1, a hexabromocyclododecane production apparatus includes a reaction kettle 1, the reaction kettle 1 is connected with a first centrifuge 2, the first centrifuge 2 is provided with a liquid material outlet, a solid material outlet and a liquid return port, the liquid return port is provided with a liquid return pipe in a penetrating manner, the liquid return pipe is provided with a pressure port, the pressure port is connected with an air source, the air source is provided with a pressure reducing valve, and the speed of liquid in the liquid return pipe entering the first centrifuge 2 can be adjusted, so that the wall-mounted material of the first centrifuge 2 is washed, the frequency of manual cleaning of the wall-mounted material dismantling device of the first centrifuge 2 is greatly reduced, the liquid return pipe is provided with a plurality of spray headers in an up-and-down staggered manner, the outlets of the spray headers face the side wall of the drum of the first centrifuge 2, the liquid material outlet is communicated with an intermediate tank 3, and;

the liquid outlet 21 of the first centrifuge 2 is connected with the inlet of a centrifugal pump 22, the first centrifuge 2 is provided with a liquid return pipe 23, the liquid return pipe 23 is provided with a liquid return port 231 and a pressurization port 232, the outlet of the centrifugal pump 22 is respectively communicated with the distillation kettle 5 and the liquid return port 231, and valves 24 are respectively arranged between the centrifugal pump 22 and the distillation kettle 5 and between the centrifugal pump 22 and the liquid return pipe 23; the first centrifuge 2 comprises an outer cylinder 25 and a rotating drum 26, the liquid return pipe 23 extends into the rotating drum 26 and is provided with a plurality of spray headers 233 in a vertically staggered manner, outlets of the spray headers 233 face the inner wall of the rotating drum 26, and the liquid return pipe 23 is fixedly connected with the outer cylinder 25; the device is characterized by further comprising a motor 27, wherein the motor 27 is rotatably connected with a rotating shaft 28, the rotating shaft 28 penetrates through the outer cylinder 25 and is fixedly connected with the bottom of the rotating drum 26, and a mechanical seal 29 is arranged between the rotating shaft 28 and the outer cylinder 25.

The outlet of the intermediate tank 3 is respectively communicated with the feed inlet of the distillation kettle 5, the feed inlet of the reaction kettle 1 and the liquid return pipe of the first centrifuge 2, the upper part of the distillation kettle 5 is communicated with a first condenser 6, the lower part outlet of the distillation kettle 5 is communicated with a mother liquor tank 8, the mother liquor tank 8 is communicated with the feed inlet of the reaction kettle 1, so that the mother liquor is sleeved on the reaction kettle 1, the first condenser 6 is connected with a first solvent collecting tank 7, the first condenser 6 is connected with a vacuum system 14, a vacuum catcher is arranged between the first solvent collecting tank 7 and the vacuum system 14 and is used for condensing and absorbing the solvent which is not condensed by the first condenser 6, a barrier is additionally arranged between the first solvent collecting tank 7 and the vacuum system 14 to prevent the solvent from being sucked into the vacuum system 14, thereby reducing the waste of the solvent on one hand, on the other hand, the solvent is prevented from damaging equipment of the vacuum system 14, the intermediate tank 3 is provided with a jacket, and the jacket is provided with a steam inlet, a steam outlet and a regulating valve for controlling the intermediate tank 3 to preheat and preserve heat of liquid in the tank in advance, so that the adverse effect on the reaction caused by the excessively low temperature of the material when the intermediate tank is sleeved back to the reaction kettle 1 is prevented;

the upper portion of the alkaline washing kettle 4 is connected with a second condenser 9, the second condenser 9 is connected with a second solvent collecting tank 10, the lower outlet of the alkaline washing kettle 4 is connected with a second centrifuge 11, a liquid material outlet of the second centrifuge 11 is communicated with a waste liquid tank 12, a solid material outlet of the second centrifuge 11 is communicated with a finished product transfer tank 13, the finished product transfer tank 13 can be conveyed to a dryer to be dried by a tank cart after the finished product transfer tank 13 is full of materials, and the second condenser 9 is connected with a vacuum pump and can accelerate cooling absorption of a gaseous solvent in the alkaline washing kettle.

It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes and modifications of the present invention may be made by those skilled in the art after reading the teachings of the present invention, and these equivalents also fall within the scope of the appended claims.

Claims

1. A hexabromocyclododecane apparatus for producing, its characterized in that: the alkaline washing device comprises a reaction kettle, wherein a material outlet of the reaction kettle is communicated with a first centrifugal machine, the first centrifugal machine is provided with a liquid material outlet, a solid material outlet and a liquid return port, the liquid material outlet is communicated with an intermediate tank, and the solid material outlet is communicated with an alkaline washing kettle;

2. The hexabromocyclododecane production apparatus according to claim 1, wherein: the liquid outlet of the first centrifugal machine is connected with the inlet of a centrifugal pump, the first centrifugal machine is provided with a liquid return pipe, the liquid return pipe is provided with a liquid return port and a pressurizing port, the outlet of the centrifugal pump is respectively communicated with the distillation kettle and the liquid return port, and valves are respectively arranged between the centrifugal pump and the distillation kettle as well as between the centrifugal pump and the liquid return pipe; the first centrifugal machine comprises an outer barrel and a rotary drum, the liquid return pipe extends into the rotary drum and is provided with a plurality of spray headers in a vertically staggered manner, outlets of the spray headers face the inner wall of the rotary drum, and the liquid return pipe is fixedly connected with the outer barrel; the rotary drum is characterized by further comprising a motor, wherein the motor is rotatably connected with a rotating shaft, and the rotating shaft penetrates through the outer barrel and is fixedly connected with the bottom of the rotary drum.

3. The hexabromocyclododecane production apparatus according to claim 2, wherein: the liquid return pipe is provided with a pressurizing port, and the pressurizing port is connected with an air source.

4. The hexabromocyclododecane production apparatus according to claim 1, wherein: the second condenser is connected with a vacuum pump.

5. The hexabromocyclododecane production apparatus according to claim 1, wherein: and a vacuum catcher is arranged between the first solvent collecting tank and the vacuum system.