CN112169381A - Solid-liquid separation washing device and application thereof - Google Patents
Solid-liquid separation washing device and application thereof Download PDFInfo
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- CN112169381A CN112169381A CN202011103815.4A CN202011103815A CN112169381A CN 112169381 A CN112169381 A CN 112169381A CN 202011103815 A CN202011103815 A CN 202011103815A CN 112169381 A CN112169381 A CN 112169381A
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- washing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D21/00—Separation of suspended solid particles from liquids by sedimentation
- B01D21/02—Settling tanks with single outlets for the separated liquid
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/102—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration with means for agitating the liquid
- B08B3/104—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration with means for agitating the liquid using propellers
Abstract
The invention relates to a solid-liquid separation washing device and application thereof, wherein the solid-liquid separation washing device is sequentially provided with a settling chamber and a washing chamber from top to bottom; a packing layer and a grid for fixing the packing layer are arranged in the settling chamber; a stirring device is arranged in the washing chamber; the middle part of the settling chamber is provided with a material inlet, and the upper part of the settling chamber is provided with an overflow port; the overflow port is arranged higher than the packing layer; a concentrated solution outlet is formed in the lower part of the settling chamber; the side surface of the bottom of the washing chamber is provided with a detergent inlet; and a solid discharge port is formed in the bottom surface of the bottom of the washing chamber. The device provided by the invention can realize continuous washing, saves washing water or other washing solvents, has high washing efficiency and low labor intensity, and saves energy and reduces consumption.
Description
Technical Field
The invention relates to the field of separation and washing, in particular to a solid-liquid separation and washing device and application thereof.
Background
At present, in the production process of metal catalysts, soluble impurities are often contained in solid products, and the solid products need to be further separated and washed.
For example, WO2020000882A1 discloses a solid-liquid separation device and a method for repeatedly washing lignocellulose solid residues by adopting the device, wherein the solid-liquid separation device comprises a kettle body (1), a piston (2), a stirring paddle (3), a partition plate (4) provided with a filtering hole (41) and a filter screen (5); the axial direction of the kettle body (1) penetrates through the cavity to form a cavity, the partition plate (4) is installed in the cavity in a matched mode to divide the cavity into two parts, namely a washing cavity (11) and a drainage cavity (12), the piston (2) and the stirring paddle (3) are installed in the washing cavity (11) in a matched mode, and the filter screen (5) is arranged on the surface, facing the stirring paddle (3), of the partition plate (4) to cover the filter holes (41) in the partition plate (4); a feed inlet (13), a water inlet (14), a discharge outlet (15) and a liquid outlet (16) are respectively arranged in the kettle body (1); wherein, the feed inlet (13) and the discharge outlet (15) are communicated with the washing cavity (11), and the water inlet (14) and the liquid outlet (16) are communicated with the drainage cavity (12). The method comprises the following steps: material input, solid-liquid separation, washing and material output.
CN109092060A discloses a method and a system for continuous washing and separation of solid and liquid. The method comprises the following steps: diluting initial solid slurry to be treated by using a washing solvent at the temperature of 5-95 ℃ to obtain first diluent, inputting the first diluent into a filtering system, separating to obtain a liquid phase and solid slurry, diluting the solid slurry obtained by separation by using the washing solvent at the temperature of 5-95 ℃ to obtain second diluent, inputting the second diluent into a next filtering system, and separating again to obtain the liquid phase and the solid slurry, wherein the volume ratio of the washing solvent at the temperature of 5-95 ℃ to the initial solid slurry or the solid slurry obtained by separation is 0-100: 1; the foregoing operation was repeated more than once, and the concentration of impurity ions in the solid slurry obtained by each separation was tested until the measured concentration of impurity ions was reduced to the target concentration. The method and the system for continuously washing and separating solid and liquid can realize continuous washing and solid-liquid separation of powder materials and are easy to realize industrial automatic separation and washing.
However, in the current process, in the production process of the metal catalyst, after the temperature reduction of the solid-liquid-containing mixed material is finished, the reaction kettle is kept stand, the solution is extracted by vacuum, then water is added for washing, standing separation and water pumping, and the washing is repeated for 4-5 times, wherein the washing process is intermittent operation, the operation is complex due to large labor amount, the consumed washing water amount is high, the electric energy consumption is large, the working efficiency is low, the operation time of each ton of products needs more than 40 hours, and each ton of products needs more than 40 tons of washing water.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a solid-liquid separation washing device and application thereof, wherein the washing device realizes continuous washing, saves washing water or other washing solvents, and has the advantages of high washing efficiency, low labor intensity, energy conservation and consumption reduction.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a solid-liquid separation washing device, which is provided with a settling chamber and a washing chamber in sequence from top to bottom;
a packing layer and a grid for fixing the packing layer are arranged in the settling chamber;
a stirring device is arranged in the washing chamber;
the middle part of the settling chamber is provided with a material inlet, and the upper part of the settling chamber is provided with an overflow port;
the overflow port is arranged higher than the packing layer;
a concentrated solution outlet is formed in the lower part of the settling chamber;
the side surface of the bottom of the washing chamber is provided with a detergent inlet;
and a solid discharge port is formed in the bottom surface of the bottom of the washing chamber.
The device provided by the invention can be used for putting a material containing solid-liquid mixture into a container at one time, discharging a concentrated solution through standing separation, continuously washing with water or other light-component detergents, and discharging the solid through the bottom after washing. The method realizes continuous washing, saves washing water or other washing solvents, has high washing efficiency and low labor intensity, and saves energy and reduces consumption.
In a preferred embodiment of the present invention, the volume of the washing chamber is 5 to 35% of the volume of the settling chamber, for example, 5%, 10%, 15%, 20%, 25%, 30%, or 35%, but not limited to the above-mentioned values, and other values not shown in the above range are also applicable, preferably 10 to 25%.
As a preferred technical solution of the present invention, the stirring device in the washing chamber is one of a ribbon paddle, a pitched blade paddle or an anchor frame paddle, and is preferably an up-turning down-pressing type double ribbon paddle.
In the invention, the ribbon-type paddles can be turned up and down and pressed double ribbon-type paddles RF77-1.5/27 and the like.
In the present invention, the pitched blade type blade may be a double pitched blade XJ446 or the like.
In the invention, the anchor frame type paddle can be frame type paddle LSJB-2.2 and the like.
In a preferred embodiment of the present invention, the dope outlet is 2 to 10cm higher than the surface of the settled solids, and may be, for example, 2cm, 3cm, 4cm, 5cm, 6cm, 7cm, 8cm, 9cm or 10cm, but is not limited to the above-mentioned values, and other values not mentioned in the above-mentioned range are also applicable.
In a preferred embodiment of the present invention, the height of the filler layer in the settling chamber is 10 to 30cm, for example, 10cm, 12cm, 14cm, 16cm, 18cm, 20cm, 22cm, 24cm, 26cm, 28cm, or 30cm, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable, and preferably 10 to 20 cm.
Preferably, the grid of fixed packing layers is distributed above and below the packing layers.
Preferably, the grid at the bottom of the fixed packing layer is located at 1/4-1/3 from the top of the settling chamber, and may be, for example, 1/4, 0.26, 0.27, 0.28, 0.29, 0.30, 0.31, 0.32, 1/3, etc., but is not limited to the values recited, and other values not recited in this range are equally applicable.
Preferably, the packing layer includes 250Y-type packing and/or pall ring packing.
As a preferred technical scheme of the invention, the settling chamber is a cylindrical settling chamber.
Preferably, the washing chamber is a conical washing chamber.
In a second aspect, the present invention provides a separation and washing method of a metal catalyst slurry based on the solid-liquid separation and washing device of the first aspect, the separation and washing method comprising the steps of:
(1) introducing the metal catalyst slurry into a settling chamber from a material inlet for standing, discharging clear liquid from an overflow port, and introducing solid materials into a washing chamber;
(2) after standing, discharging the concentrated solution from a concentrated solution outlet, introducing a detergent from a detergent inlet, starting a stirring device to start washing, continuously discharging washing water from an overflow port in the washing process, and discharging solid materials through a solid discharge port after washing.
In a preferred embodiment of the present invention, the volume of the solid in the metal catalyst slurry in the step (1) is 0.8 to 1 times the volume of the washing chamber of the solid-liquid separation washing apparatus, and may be, for example, 0.8, 0.82, 0.84, 0.86, 0.88, 0.9, 0.92, 0.94, 0.96, 0.98 or 1, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
In the invention, the volume of the solid in the metal catalyst slurry can be obtained by measuring the volume of the sediment after sampling and standing for 30min by using a 250mL measuring cylinder, and then the volume of the solid in the slurry is obtained by data fitting and amplification.
Preferably, the standing time in step (1) is 20-50min, such as 20min, 22min, 24min, 26min, 28min, 30min, 32min, 34min, 36min, 38min, 40min or 50min, but not limited to the recited values, and other values not recited in the range are also applicable.
The standing time is related to the settling velocity of the solid particles in the fed slurry, and the slower the settling velocity, the longer the standing time.
In a preferred embodiment of the present invention, the washing in step (2) is terminated at a washing solution pH of 7 to 8, for example, 7, 7.2, 7.4, 7.6, 7.8 or 8, but is not limited to the values listed, and other values not listed in the range are also applicable.
As a preferred technical scheme of the invention, the separation washing method comprises the following steps:
(1) introducing the metal catalyst slurry into a settling chamber from a material inlet, standing for 20-50min, discharging clear liquid from an overflow port, and introducing solid materials into a washing chamber; the volume of the solid in the metal catalyst slurry is 0.8-1 time of the volume of a washing chamber of the solid-liquid separation washing device;
(2) and after the standing is finished, discharging the concentrated solution from a concentrated solution outlet, introducing a detergent from a detergent inlet, starting a stirring device to start washing until the pH value of the washing solution is 7-8, and discharging the solid material through a solid discharge port after the washing is finished.
In the invention, the filler layer can reduce the fluid disturbance of the settling chamber during stirring during washing and increase the settling of solid particles. The washing agents such as washing water enter from the straight pipe section at the bottom of the device, the contact effect of the washing water and the materials is improved, the stirring torque is reduced, and the mixed liquid containing the solute flows out from the top of the device after contacting the materials. The detergent inlet may be a forward inlet or a tangential inlet to the apparatus along the vessel.
In the present invention, the driving member of the stirring device can be disposed at an appropriate position according to actual selection.
In the present invention, the initial pH of the metal catalyst slurry is about 14, and the detergent may be water or other agent that does not affect the catalyst performance.
Compared with the prior art, the invention has the following beneficial effects:
(1) the device provided by the invention can be used for feeding solid-liquid mixed materials into a container at one time, discharging concentrated solution through standing separation, continuously feeding water or continuously washing other light-component detergents, and discharging the solid through the bottom after washing. The method realizes continuous washing, saves washing water or other washing solvents, has high washing efficiency, low labor intensity, energy conservation and consumption reduction, reduces the generation amount of washing waste liquid, reduces the washing liquid amount used by each ton of products from the original 40 tons to within 20 tons, and reduces the washing liquid amount to within 50 percent of the prior art.
(2) According to the washing method provided by the invention, the newly designed washing device is utilized, so that the catalyst can be efficiently washed and separated, and the washing time is shortened to be within 12 hours from 40 hours.
Drawings
FIG. 1 shows a solid-liquid separator provided in example 1 of the present invention.
In the figure: 1-a drive mechanism;
2-a settling chamber, 2.1-a filler layer, 2.2-an overflow port, 2.3-a grid, 2.4-a material inlet and 2.5-a concentrated solution outlet;
3-washing chamber, 3.1-stirring device, 3.2-detergent inlet, 3.3-solid discharge outlet.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
The present embodiment provides a solid-liquid separation washing apparatus, as shown in fig. 1, which is provided with a settling chamber 2 and a washing chamber 3 in this order from top to bottom;
a filler layer 2.1 and a grid 2.3 for fixing the filler layer are arranged in the settling chamber 2;
a stirring device 3.1 is arranged in the washing chamber 3;
a material inlet 2.4 is formed in the middle of the settling chamber 2, and an overflow port 2.2 is formed in the upper part of the settling chamber 2;
the overflow port 2.2 is arranged higher than the filler layer 2.1;
a concentrated solution outlet 2.5 is arranged at the lower part of the settling chamber 2;
the side surface of the bottom of the washing chamber 3 is provided with a detergent inlet 3.2;
the bottom surface of the washing chamber 3 is provided with a solid discharge port 3.3.
And the concentrated solution outlet 2.5 is 7cm higher than the liquid level of the settled solids.
The height of the filler layer 2.1 in the settling chamber 2 is 20 cm;
the grids 2.3 for fixing the filler layer are distributed above and below the filler layer 2.1;
the grid 2.3 at the bottom of the fixed packing layer is arranged at 1/4 from the top of the settling chamber 2;
the filler layer 2.1 is 250Y-shaped filler;
the settling chamber 2 is a cylindrical settling chamber, and the washing chamber 3 is a conical washing chamber.
Application example 1
In this embodiment, the solid-liquid separation washing apparatus provided in embodiment 1 is used to perform a separation and washing method of a metal catalyst slurry, where the separation and washing method includes the following steps:
(1) introducing metal catalyst slurry (the volume ratio of liquid to solid of the slurry is 25:1) into a settling chamber from a material inlet, standing for 30min, discharging clear liquid from an overflow port, and introducing solid material into a washing chamber; the volume of the solid in the metal catalyst slurry is 0.9 times of the volume of a washing chamber of the solid-liquid separation washing device; the volume of the washing chamber is 8% of the volume of the settling chamber; the stirring paddle is an RF77-1.5/27 up-turning down-pressing type double-helical-belt paddle;
(2) and after the standing is finished, discharging the concentrated solution from a concentrated solution outlet, introducing a detergent from a detergent inlet, starting a stirring device to start washing until the pH value of the washing solution is 8, and discharging the solid material through a solid discharge port after the washing is finished.
The indexes of the amount of detergent and the washing time are shown in Table 1.
Application example 2
The difference from application example 1 is that the volume of the washing chamber is 12% of the volume of the settling chamber; the stirring paddle is an RF77-1.5/27 up-turning down-pressing type double-helical-belt paddle; the indexes of the amount of detergent and the washing time are shown in Table 1.
Application example 3
The difference from application example 1 is that the volume of the washing chamber is 18% of the volume of the settling chamber; the stirring paddle is an RF77-1.5/27 up-turning down-pressing type double-helical-belt paddle; the indexes of the amount of detergent and the washing time are shown in Table 1.
Application example 4
The difference from application example 1 is that the volume of the washing chamber is 22% of the volume of the settling chamber; the stirring paddle is an RF77-1.5/27 up-turning down-pressing type double-helical-belt paddle; the indexes of the amount of detergent and the washing time are shown in Table 1.
Application example 5
In this embodiment, the solid-liquid separation washing apparatus provided in embodiment 1 is used to perform a separation and washing method of a metal catalyst slurry, where the separation and washing method includes the following steps:
(1) introducing metal catalyst slurry (the volume ratio of liquid to solid in the slurry is 25:1) into a settling chamber from a material inlet, standing for 40min, discharging clear liquid from an overflow port, and introducing solid material into a washing chamber; the volume of the solid in the metal catalyst slurry is 1 time of the volume of a washing chamber of the solid-liquid separation washing device; the volume of the washing chamber is 12% of the volume of the settling chamber; the stirring paddle is an inclined blade type paddle XJ 446;
(2) and after the standing is finished, discharging the concentrated solution from a concentrated solution outlet, introducing a detergent from a detergent inlet, starting a stirring device to start washing until the pH value of the washing solution is 8, and discharging the solid material through a solid discharge port after the washing is finished. The indexes of the amount of detergent and the washing time are shown in Table 1.
Application example 6
In this embodiment, the solid-liquid separation washing apparatus provided in embodiment 1 is used to perform a separation and washing method of a metal catalyst slurry, where the separation and washing method includes the following steps:
(1) introducing metal catalyst slurry (the volume ratio of liquid to solid in the slurry is 25:1) into a settling chamber from a material inlet, standing for 35min, discharging clear liquid from an overflow port, and introducing solid material into a washing chamber; the volume of the solid in the metal catalyst slurry is 1 time of the volume of a washing chamber of the solid-liquid separation washing device; the volume of the washing chamber is 12% of the volume of the settling chamber; the stirring paddle is LSJB-2.2 anchor frame type slurry;
(2) and after the standing is finished, discharging the concentrated solution from a concentrated solution outlet, introducing a detergent from a detergent inlet, starting a stirring device to start washing until the pH value of the washing solution is 8, and discharging the solid material through a solid discharge port after the washing is finished.
The indexes of the amount of detergent and the washing time are shown in Table 1.
TABLE 1 application examples 1-6 for washing time and detergent dosage
From the results of the above application examples, it is clear that the apparatus provided by the present invention can be used for feeding a material containing a mixture of solid and liquid into a container at one time, discharging a concentrated solution by standing separation, continuously feeding water or continuously washing with other light-component detergents, and discharging the solid through the bottom after washing. The method realizes continuous washing, saves washing water or other washing solvents, has high washing efficiency, low labor intensity, energy conservation and consumption reduction, and reduces the generation amount of washing waste liquid.
The applicant declares that the present invention illustrates the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the above detailed structural features, that is, it does not mean that the present invention must be implemented depending on the above detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. A solid-liquid separation washing device is characterized in that a settling chamber and a washing chamber are sequentially arranged on the solid-liquid separation washing device from top to bottom;
a packing layer and a grid for fixing the packing layer are arranged in the settling chamber;
a stirring device is arranged in the washing chamber, and a material inlet is formed in the middle of the settling chamber;
an overflow port is arranged at the upper part of the settling chamber;
the overflow port is arranged higher than the packing layer;
a concentrated solution outlet is formed in the lower part of the settling chamber;
the side surface of the bottom of the washing chamber is provided with a detergent inlet;
and a solid discharge port is formed in the bottom surface of the bottom of the washing chamber.
2. The solid-liquid separation washing apparatus according to claim 1, characterized in that the volume of the washing chamber is 5-35%, preferably 10-25% of the volume of the settling chamber.
3. The solid-liquid separation washing apparatus of claim 1 or 2, wherein the stirring device in the washing chamber is one of a ribbon paddle, a pitched blade paddle or an anchor frame paddle, preferably a double ribbon paddle of an upturned and downturned type.
4. The solid-liquid separation washing apparatus according to any one of claims 1 to 3, wherein the dope outlet is 2 to 10cm higher than the liquid surface of the settled solids.
5. The solid-liquid separation washing apparatus according to any one of claims 1 to 4, characterized in that the height of the packing layer in the settling chamber is 10 to 30cm, preferably 10 to 20 cm;
preferably, the grid of the fixed packing layer is distributed above and below the packing layer;
preferably, the grid at the bottom of the fixed packing layer is arranged at 1/4-1/3 from the top of the settling chamber;
preferably, the packing layer includes 250Y-type packing and/or pall ring packing.
6. The solid-liquid separation washing apparatus according to any one of claims 1 to 5, wherein the settling chamber is a cylindrical settling chamber;
preferably, the washing chamber is a conical washing chamber.
7. A method for separating and washing a metal catalyst slurry based on the solid-liquid separation and washing device of any one of claims 1 to 6, wherein the method for separating and washing comprises the steps of:
(1) introducing the metal catalyst slurry into a settling chamber from a material inlet for standing, discharging clear liquid from an overflow port, and introducing solid materials into a washing chamber;
(2) after standing, discharging the concentrated solution from a concentrated solution outlet, introducing a detergent from a detergent inlet, starting a stirring device to start washing, continuously discharging washing water from an overflow port in the washing process, and discharging solid materials through a solid discharge port after washing.
8. The separation washing method according to claim 7, wherein the volume of the solid in the metal catalyst slurry in the step (1) is 0.8 to 1 times the volume of the washing chamber of the solid-liquid separation washing device;
preferably, the standing time of the step (1) is 20-50 min.
9. The separation washing method according to claim 7 or 8, wherein the washing in step (2) is terminated by a washing solution having a pH of 7 to 8.
10. A separation and washing process according to any one of claims 7 to 9, characterised in that it comprises the following steps:
(1) introducing the metal catalyst slurry into a settling chamber from a material inlet, standing for 20-50min, discharging clear liquid from an overflow port, and introducing solid materials into a washing chamber; the volume of the solid in the metal catalyst slurry is 0.8-1 time of the volume of a washing chamber of the solid-liquid separation washing device;
(2) and after the standing is finished, discharging the concentrated solution from a concentrated solution outlet, introducing a detergent from a detergent inlet, starting a stirring device to start washing until the pH value of the washing solution is 7-8, and discharging the solid material through a solid discharge port after the washing is finished.
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| CN202011103815.4A CN112169381A (en) | 2020-10-15 | 2020-10-15 | Solid-liquid separation washing device and application thereof |
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| CN202011103815.4A CN112169381A (en) | 2020-10-15 | 2020-10-15 | Solid-liquid separation washing device and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113666805A (en) * | 2021-08-23 | 2021-11-19 | 山东新和成维生素有限公司 | Method and production system for continuously producing 4-chloro-3, 5-dimethylphenol |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113666805A (en) * | 2021-08-23 | 2021-11-19 | 山东新和成维生素有限公司 | Method and production system for continuously producing 4-chloro-3, 5-dimethylphenol |
| CN113666805B (en) * | 2021-08-23 | 2023-08-25 | 山东新和成维生素有限公司 | Method and system for continuously producing 4-chloro-3, 5-dimethylphenol |
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