CN211134940U

CN211134940U - Device for hydrolyzing and filtering filter residues of cold hydrogenation slag slurry

Info

Publication number: CN211134940U
Application number: CN201922231061.XU
Authority: CN
Inventors: 吴军甫; 谢岩; 周程; 冯晓春; 吴伟; 吕亘亘; 魏亚魁
Original assignee: Xinjiang Xixixin New Energy Material Technology Co ltd
Current assignee: Xinjiang Xixixin New Energy Material Technology Co ltd
Priority date: 2019-12-12
Filing date: 2019-12-12
Publication date: 2020-07-31
Anticipated expiration: 2029-12-12

Abstract

The utility model discloses a device of filter treatment is hydrolysised to cold hydrogenation sediment thick liquid filter residue, including neutralization pond, bubbling device, the absorption tower, the mummification pond, sedimentation tank and effluent water sump, in neutralization pond, a certain amount of waste residue and lime aqueous solution carry out neutralization reaction, the waste gas of production sprays the processing in introducing glass steel acid mist absorption tower through the fan pipeline, discharge to the atmosphere through the aiutage, sediment thick liquid pH control after the reaction is in 6-9's within range, the pump sending is to the mummification pond, the neutral clear water in mummification bottom of the pool passes through the sediment processing, then get into the effluent water sump and collect, preferentially circulate and use, the water source is practiced thrift to the at utmost, waste residue after the mummification of mummification pond transports to the unified processing of sediment field through fork truck. The utility model discloses a gaseous tympanic bulla effect for the waste residue that cold hydrogenation technology produced can obtain the complete hydrolysis in, guarantees the abundant reaction of waste residue, guarantees simultaneously that solid particle thing is not at the bottom of the pool deposit, avoids unable normal operating of circulating pump and stifled pipe phenomenon.

Description

Device for hydrolyzing and filtering filter residues of cold hydrogenation slag slurry

Technical Field

The utility model belongs to polycrystalline silicon production field, concretely relates to cold hydrogenation technology, especially a device of filter treatment is hydrolysised to cold hydrogenation sediment thick liquid filter residue.

Background

The cold hydrogenation slag slurry is a mixture with the silicon powder content of 30-35% in the chlorosilane liquid discharged out of a system after washing and concentrating in the production process of a cold hydrogenation device, and slag slurry filter residue with the chlorosilane content of less than 1% is obtained after filtering and drying the slag slurry, and is commonly called waste slag.

In the production of polycrystalline silicon, the device is inevitably overhauled, and especially, waste silicon powder containing chlorosilane and waste liquid containing more silicon powder in a hydrogenation system cannot be recycled before the hydrogenation device is overhauled. At present, slag slurry generated in the normal operation of a cold hydrogenation system is effectively treated by various large enterprises in the polysilicon industry, while the treatment of a large amount of waste slag in a cold hydrogenation reactor in the overhaul process is neglected, and the waste slag is inevitably mixed with a small amount of chlorosilane and still needs further hydrolysis filtration treatment.

SUMMERY OF THE UTILITY MODEL

The utility model aims to solve the technical problem that to prior art not enough, provide a cold hydrogenation sediment thick liquid filter residue filter device of hydrolysising, make the neutralization pond reaction abundant, avoid the hydrolysis product when sending to the mummification pond, the unable normal operating of circulating pump perhaps takes place stifled pipe phenomenon.

In order to achieve the above purpose, the utility model adopts the following technical scheme:

a device for filter treatment of filter residue hydrolysis of cold hydrogenation slag slurry comprises:

the neutralization tank is used as a tank body for carrying out neutralization reaction on waste residues generated in the cold hydrogenation process and a lime water solution, and is a closed tank body provided with a waste residue feeding hole, a waste gas discharging hole and a residue slurry discharging hole.

The bubbling device is positioned in the neutralization tank, is connected with an external gas source and is used for bubbling the reaction liquid in the neutralization tank, and bubbling gas comprises but is not limited to nitrogen, hydrogen and the like;

the absorption tower is used for spraying and cleaning the waste gas generated by the neutralization tank, is communicated with the waste gas outlet of the neutralization tank, and is provided with a gas outlet at the top and a waste liquid outlet at the bottom;

the drying tank is used for filtering the slag slurry generated by the neutralization tank, is connected with a slag slurry discharge port of the neutralization tank through a pipeline, and is provided with a filter screen and a liquid discharge port at the bottom;

the sedimentation tank is used for carrying out sedimentation treatment on the waste liquid discharged by the drying tank and is connected with a liquid outlet of the drying tank;

the sewage tank is connected with the sedimentation tank and receives the clear liquid discharged by the sedimentation tank; a sewage pump is arranged in the sewage pool, one part of liquid in the sewage pool is used as liquid for spraying treatment in the absorption tower, the other part of liquid is used as liquid for spraying treatment in the absorption tower, and the sewage pool is connected with a lime water solution replenishing pipe; and the waste liquid discharge port of the absorption tower is communicated with the sewage tank, and the waste liquid generated by the absorption tower is discharged into the sewage tank.

Furthermore, a gas outlet at the top of the absorption tower is connected with an exhaust funnel through a pipeline, and a fan is arranged on the pipeline.

Furthermore, the drying pool is more than one, and fine sand and fine stones which are thickened from top to bottom are filled in the drying pool.

Furthermore, a heating pipeline is sleeved on the outer wall of the bottom of the drying pool, so that the evaporation speed is increased, and draining and drying are realized.

Preferably, the outer wall of the sedimentation tank is provided with an overflow port, and the upper clear liquid is discharged into the sewage tank through the overflow port.

Furthermore, a steam pipe is connected in the sewage tank and used for maintaining the temperature in the sewage tank and ensuring that the sewage tank is not frozen in winter.

The main technical principle of the utility model is as follows: in the neutralization tank, a certain amount of waste residues and a lime water solution are subjected to neutralization reaction, generated waste gas is introduced into a glass fiber reinforced plastic acid mist absorption tower through a fan pipeline for spraying treatment, the waste gas is discharged to the atmosphere through an exhaust funnel, the pH value of the reacted residue slurry is controlled within the range of 6-9, the reacted residue slurry is pumped to a drying tank for drying, neutral clear water at the bottom of the drying tank is subjected to precipitation treatment and then enters a sewage tank for collection, the neutral clear water is preferentially recycled, a water source is saved to the maximum extent, and the dried waste residues are conveyed to a residue yard for uniform treatment through a forklift.

Has the advantages that:

1. the utility model discloses processing method passes through the effect of gas bubbling for the waste residue that cold hydrogenation technology produced can obtain the complete hydrolysis and neutralize, guarantees the abundant reaction of waste residue, guarantees simultaneously that solid particle thing is not at the bottom of the pool deposit, avoids unable normal operating of circulating pump and stifled pipe phenomenon.

2. The neutralization tank of the utility model adopts a closed negative pressure device, acid gas is generated by reaction in the tank and can not overflow into the atmosphere, the environment is protected, and the corrosion of the device is greatly reduced; the sewage produced by the process can be recycled, has no discharged sewage, and is suitable for northern arid areas or areas with serious water shortage.

3. The drying tank has high water filtering speed, meets the production requirements, and ensures the stable operation of the device; the sewage tank and the drying tank are insulated and heated, and normal production under the weather condition of-40 ℃ can be completely met.

Drawings

These and/or other advantages of the present invention will become more apparent from the following detailed description of the present invention when taken in conjunction with the accompanying drawings and the following detailed description.

FIG. 1 is a schematic structural diagram of a filter residue hydrolysis and filtration treatment device for cold hydrogenation slag slurry in example 1.

FIG. 2 is a schematic structural diagram of the filter residue hydrolysis and filtration treatment device of the cold hydrogenation residue slurry in embodiment 2.

Wherein each reference numeral represents: 1-a neutralization pond; 11-a waste residue feed inlet; 12-exhaust gas outlet; 13-slag slurry discharge port; 14-sealing steel plate; 15-bubbling air pipe; 16-neutralization tank spray header; 2-a delivery pump; 3-a first drying tank; 31-a first drying tank feed inlet; 32-a first drying pool liquid outlet; 33-a first drying tank filter screen; 34-first drying bed filling; 35-a first drying tank heating pipe; 4-a second drying tank; 41-a feed inlet of a second drying tank; 42-a liquid discharge port of a second drying pool; 43-a second drying tank filter screen; 44-second drying bed packing; 45-a second drying tank heating pipe; 5-a sedimentation tank; 51-first feeding pipe of sedimentation tank; 52-second feed pipe of settling tank; 53-overflow port of sedimentation tank; 6-a sewage tank; 61-a first return pipe of the sewage pool; 62-a sewage pool liquid supplementing pipe; 63-a second return pipe of the sewage pool; 64-steam pipes; 7-a lift pump; 71-a first shower; 72-a second shower; 8-glass fiber reinforced plastic acid mist absorption tower; 81-absorption tower inlet; 82-an upper spray header of the absorption tower; 83-lower spray header of absorption tower; 84-an air inlet liquid outlet of the absorption tower; 85-absorption tower exhaust port; 9-a fan; 10-exhaust funnel.

Detailed Description

The invention will be better understood from the following examples.

The drawings in the specification show the structure, ratio, size, etc. only for the purpose of matching with the content disclosed in the specification, so as to be known and read by those skilled in the art, and not for the purpose of limiting the present invention, so the present invention does not have the essential meaning in the art, and any structure modification, ratio relationship change or size adjustment should still fall within the scope covered by the technical content disclosed in the present invention without affecting the function and achievable purpose of the present invention. Meanwhile, the terms "upper", "lower", "front", "rear", "middle", and the like used in the present specification are for the sake of clarity only, and are not intended to limit the scope of the present invention, and changes or adjustments of the relative relationship thereof are also considered to be the scope of the present invention without substantial changes in the technical content.

Example 1

As shown in fig. 1, the filter residue hydrolysis and filtration treatment device for the cold hydrogenation slag slurry comprises a neutralization tank 1, a delivery pump 2, a first drying tank 3, a second drying tank 4, a sedimentation tank 5, a sewage tank 6, a lift pump 7, a glass fiber reinforced plastic acid mist absorption tower 8, a fan 9 and an exhaust funnel 10.

The neutralization tank 1 is a closed device, the top of the neutralization tank is closed through a sealing steel plate 14, and the side waste residue feed port 11 is opened except when feeding materials, and is closed except when feeding materials. The side surface of the upper part is provided with an exhaust outlet 12 which is communicated with an absorption tower air inlet 81 of the glass reinforced plastic acid mist absorption tower 8 through a pipeline, the glass reinforced plastic acid mist absorption tower 8 is used for spraying and cleaning, and the cleaned exhaust enters the exhaust funnel 10 from an absorption tower exhaust outlet 85 so as to be exhausted into the atmosphere. The draught fan 9 is arranged on a pipeline between the exhaust port 85 of the absorption tower and the exhaust funnel 10, when the draught fan 9 operates, the whole neutralization pond 1 is in a negative pressure state, and waste gas flows from a high-pressure area of the liquid level of the neutralization pond 1 to a low-pressure area of the waste gas exhaust port 12.

The bottom of the neutralization tank 1 is provided with a slag slurry discharge port 13, the slag slurry obtained by reaction in the neutralization tank 1 is conveyed into a first drying tank 3 and a second drying tank 4 through a conveying pump 2, waste slag generated by the cold hydrogenation process is added into the neutralization tank 1 through a waste slag feed port 11 and then undergoes hydrolysis neutralization reaction with lime water solution, bubbling is uniform under the action of nitrogen introduced through a bubbling air pipe 15, the reaction is fully contacted, HC L gas generated by the reaction enters a glass fiber reinforced plastic acid mist absorption tower 8 through four DN600 glass fiber reinforced plastic air pipes connected with a waste gas discharge port 12 on the side of the neutralization tank, the solid content of mixed solution in the tank is gradually increased along with the increase of the waste slag added into the neutralization tank 1, when the solid content of the mixed solution reaches 20%, the waste slag reception is stopped, the bubbling amount of the neutralization nitrogen tank is increased, solid particles are prevented from depositing at the bottom of the neutralization tank, waste liquid is pumped into the drying tank through a conveying pump 2, the neutralization tank is replaced for three times or more, and the solid content of the neutralization tank is reduced to about 1-2% and then the material reception is recovered.

The side surface of the first drying tank 3 is provided with a first drying tank feed inlet 31, the side surface of the second drying tank is provided with a second drying tank feed inlet 41, and the first drying tank feed inlet 31 and the second drying tank feed inlet 41 are respectively connected with a neutralization tank slag slurry discharge outlet 13 through pipelines. The bottom of the first drying pool 3 is provided with a first drying pool liquid discharge port 32, a first drying pool filter screen 33 with 150-mesh aperture is arranged at the first drying pool liquid discharge port 32, the first drying pool filler 34 is fine sand and fine stone which are thickened from top to bottom, and the outer wall of the bottom of the first drying pool 3 is sleeved with a first drying pool heating pipe 35. The bottom of the second drying pool 4 is provided with a second drying pool liquid discharge port 42, a second drying pool filter screen 43 with 150-mesh aperture is arranged at the second drying pool liquid discharge port 42, second drying pool fillers 44 are fine sand and fine stone which are thickened from top to bottom, and a second drying pool heating pipe 45 is sleeved on the outer wall of the bottom of the second drying pool 4. The slag slurry in the neutralization tank 1 is filtered by thin sand and thin stone which are thin and thick from top to bottom at the bottom of the drying tank, the filter residue is gradually increased in the drying tank until the feeding is stopped more than two thirds of the depth of the drying tank, the heating pipe at the bottom of the drying tank is used for heating, the evaporation speed is increased, the draining and drying are realized, when the surface of the filter residue is cracked, the water content in the filter residue is low, the filter residue in the tank can be emptied, and the material can be continuously received for drying. The water without turbid liquid flowing out of the drying tank bottom is filtered by a 150-mesh filter screen, then enters the sedimentation tank through the first feeding pipe 51 of the sedimentation tank and the second feeding pipe 52 of the sedimentation tank respectively for further sedimentation, and the supernatant enters the sewage tank 6 through the overflow port 53 of the sedimentation tank and the first return pipe 61 of the sewage tank for cyclic utilization.

Replenishing lime water solution into the sewage pool 6 through a sewage pool liquid replenishing pipe 62, and controlling the pH value to be within the range of 6-9; meanwhile, steam is introduced into the tank through a steam pipe 64 to maintain the temperature in the tank, so that the ice does not freeze in winter. Liquid in the sewage pool 6 is pressurized by the lifting pump 7 and is conveyed to the spray header 82 on the upper layer of the absorption tower and the spray header 83 on the lower layer of the absorption tower through the first spray pipe 71 to form spray liquid drops, waste gas entering the glass fiber reinforced plastic acid mist absorption tower 8 is sprayed and cleaned, and the cleaned liquid flows into the sewage pool 6 from the air inlet liquid outlet 84 of the absorption tower through the second sewage pool liquid return pipe 63 for cyclic utilization.

Example 2

On the basis of the device in the embodiment 1, the liquid in the sewage tank 6 is pressurized by the lifting pump 7 and is divided into two parts, one part is conveyed to the spray header 82 on the upper layer of the absorption tower and the spray header 83 on the lower layer of the absorption tower through the first spray pipe 71 to form spray liquid drops, and the waste gas entering the glass fiber reinforced plastic acid mist absorption tower 8 is sprayed and cleaned. The other part of the sewage is conveyed to the spray header 16 of the neutralization tank through a second spray pipe 72 to form spray liquid drops, acid mist generated by reaction in the neutralization tank is absorbed, the pH value of reaction slag slurry in the neutralization tank is regulated to be controlled to be 6-9, the sewage is recycled in the system, and energy conservation and emission reduction are really achieved.

The utility model is suitable for an area that the temperature is low, the water supply is not enough, sewage treatment capacity is low. The current devices applied to industrial production are normally operated at-38 ℃ in a dry climate environment. Because the treatment capacity of the original sewage treatment device is low, the discharge capacity of sewage of all other devices is limited. Through the upgrading to former system, adopt the utility model discloses system design, the sewage volume of production is low, can accomplish 0.5m³The external sewage discharge amount per hour is met with the maintenance of the sewage treatment device, so that the sewage is not discharged outside, zero discharge is realized, and the pressure of the sewage treatment device is greatly reduced; the wall body of the drying pool is made of a heat-insulating wall body, the bottom of the drying pool is provided with a heating coil, the top of the drying pool is provided with a heat-insulating cover plate, pipelines communicated among the neutralization pool, the drying pool and the sewage pool are wound by self-temperature-limiting tracing bands, the constant temperature in the pipelines is kept at 30 ℃, and the normal operation of the device in winter is ensured.

The utility model discloses in order to make neutralization tank bottom not deposit solid particle, nitrogen gas bubbling pipeline adopts evenly distributed aeration form, and the gas outlet is just to the tank bottom, avoids solid particle to pile up and causes the jam at the gas outlet, makes neutralization tank in the turbid liquid homogeneous mixing, can not cause neutralization tank pump suction tube to block up, and pump suction tube adopts from top bayonet, and the bottommost mouth of pipe is 300mm from the tank bottom to install the tetrafluoro material filter tip that the aperture is 8mm, filter large granule debris; the unit operation in the neutralization pond of the system needs to strictly control the input amount of filter residues, the input amount is strictly controlled below 30 kilograms each time, obvious floaters do not exist on the surface of the pond, the temperature of the pond water does not exceed 50 ℃, samples are taken every day to analyze the solid content in the neutralization pond, the operation period of the pump is effectively prolonged, and the operation period of the neutralization pond is ensured to be up to one year.

The utility model discloses mummification bottom of the pool waterlogging caused by excessive rainfall form adopts fishbone-shaped ditch, and the aperture is 10 mm's glass steel grating plate is laid at the top, prevents diameter 11mm fine stone, 5mm coarse sand, and thickness is 200mm, and the infiltration layer of constituteing leaks into in the ditch, has both increased the area of waterlogging caused by excessive rainfall, can reduce the condition that the filtration pore is blockked up again, and drainage speed is by 1m condition that the filtration pore is blockked up³H is increased to 3.5m³The treatment capacity is improved by 3.5 times, the waiting time caused by low water filtering speed is greatly saved, the replacement capacity after the hydrolysis and the neutralization of the neutralization tank is met, the time for reducing the solid content of the mixed solution in the neutralization tank to 1-2% is reduced, and the time is reduced from 96 hours to 24 hours.

The utility model discloses the acid mist scrubbing tower sprays and adopts the hollow circular cone nozzle of spiral to use tower cross-section centre of a circle as the center, every interval 300mm is the circle form and arranges, every layer is total to be counted nozzle 7, the toper water column covers the sectional area of whole tower, 600mm department under the nozzle, it passes through 500 mm's high pall ring packing layer to spray liquid, both guarantee to spray liquid can with HC L gaseous abundant contact absorption in with, can play the effect of washing filler again, it is big finally to form the flux, the resistance is little, the characteristics that separation efficiency is high and operation elasticity is big, the operating cycle of scrubbing tower has been prolonged, reduce the maintenance number of times that causes because of packing the jam, tail gas washes the tower even running one year among the present practical application, it once is the most ideal state to overhaul every year.

The utility model provides a thinking and method of cold hydrogenation sediment thick liquid filter residue hydrolysis filtration treatment's device specifically realize that this technical scheme's method and approach are many, above only the utility model discloses a preferred embodiment should point out, to the ordinary technical personnel in this technical field, not deviating from the utility model discloses under the prerequisite of principle, can also make a plurality of improvements and moist decorations, these improvements should also be regarded as with moist decorations the utility model discloses a protection range. All the components not specified in the present embodiment can be realized by the prior art.

Claims

1. The utility model provides a device of cold hydrogenation sediment thick liquid filter residue hydrolysis filtration treatment which characterized in that includes:

the neutralization tank is used as a tank body for carrying out neutralization reaction on waste residues generated in the cold hydrogenation process and the lime water solution, is a closed tank body and is provided with a waste residue feeding hole, a waste gas discharging hole and a residue slurry discharging hole;

the bubbling device is positioned in the neutralization tank, is connected with an external gas source and is used for bubbling the reaction liquid in the neutralization tank;

2. The device for the filter residue hydrolysis and filtration treatment of the cold hydrogenation slag slurry as claimed in claim 1, wherein the gas outlet at the top of the absorption tower is connected with an exhaust funnel through a pipeline, and a fan is arranged on the pipeline.

3. The device for filter residue hydrolysis and filtration of cold hydrogenation slag slurry according to claim 1, wherein the number of the drying pools is more than one, and fine sand and fine stone which are thickened from top to bottom are filled in the drying pools.

4. The device for filter residue hydrolysis and filtration of cold hydrogenated slag slurry according to claim 3, wherein the outer wall of the bottom of the drying pool is sleeved with a heating pipeline.

5. The apparatus according to claim 3, wherein the outer wall of the sedimentation tank is provided with an overflow port through which the supernatant is discharged into the sewage tank.

6. The apparatus according to claim 3, wherein a steam pipe is connected to the inside of the wastewater tank for maintaining the temperature inside the wastewater tank.