Zirconium hydroxide washing device and method

Abstract

The invention belongs to the technical field of preparation of zirconium hydroxide, and particularly relates to a zirconium hydroxide washing device which comprises a controller and a plurality of washing units, each washing unit comprises a washing pool, one end of each washing pool is provided with a water inlet pipe, and the other end of each washing pool is provided with a water outlet pipe; a water washing tank is detachably connected into the water washing pool, and zirconium hydroxide precipitates can be contained in the water washing tank; a plurality of through holes are respectively formed in the washing tank close to the water inlet pipe and the water outlet pipe; filter frames are detachably connected to the side, close to the water inlet pipe and the side, close to the water outlet pipe, in the washing tank, and filter cloth is clamped in the filter frames; a chloride ion concentration analyzer is mounted on the water outlet pipe, and the output end of the chloride ion concentration analyzer is in communication connection with the controller; compared with the prior art, the method has the advantages and positive effects that zirconium hydroxide is not washed by a filter press any more, white zirconium hydroxide precipitates are dispersed in deionized water instead of being in a filter cake shape, and thorough washing of the zirconium hydroxide precipitates is facilitated.

Description

Technical Field

[0001] The present invention belongs to the technical field of the preparation of zirconium hydroxide, and particularly relates to a zirconium hydroxide water washing device and method. Background Art

[0002] The preparation method of zirconium hydroxide is as follows: the raw material used is basic zirconium chloride, which is successively subjected to coprecipitation, washing, alcoholization, drying, and grinding, and finally the finished product is obtained. In the coprecipitation step, a colloidal or flocculent precipitate of zirconium hydroxide is generated, and in the washing step, the above-mentioned zirconium hydroxide precipitate is repeatedly washed with deionized water until there is no chloride ion in the washing water.

[0003] In the prior art, a filter press is used to wash and filter the colloidal or flocculent precipitate of zirconium hydroxide generated in the coprecipitation step. The zirconium hydroxide is in the form of a filter cake between the filter frames of the filter press. In order to achieve all-round water washing of the filter cake, an operation mode of repeatedly switching between corner washing and central washing is required, and a pressing operation is also required during the switching process; during the water washing process, in order to remove the residual filter cake at the edge of the filter plate (the filter cake in the central area of the filter plate is easy to fall off, but sticky materials are likely to accumulate in the corners due to structural dead corners) and restore the permeability of the filter cloth, a corner blowing operation is also required.

[0004] In addition, when using a filter press to wash zirconium hydroxide, the filter cloth is very likely to be blocked, and the replacement of the filter cloth of the plate and frame filter press is rather cumbersome (the filter cloth needs to be separately fixed on each filter plate and filter frame, and the installation and replacement processes are complex and time-consuming).

[0005] Therefore, the water washing operation of zirconium hydroxide using a filter press in the prior art is cumbersome, and due to reasons such as filter cloth blockage, the water washing effect is poor, resulting in an increase in the defective rate of the prepared zirconium hydroxide. Summary of the Invention

[0006] The present invention aims at the technical problems existing in the water washing of zirconium hydroxide using a filter press in the prior art, and provides a zirconium hydroxide water washing device and method.

[0007] In order to achieve the above object, the technical solution adopted by the present invention is as follows: a zirconium hydroxide water washing device includes a controller and a plurality of water washing units. Each water washing unit includes a water washing pool, an inlet pipe is installed at one end of the water washing pool, and an outlet pipe is installed at the other end; a water washing tank is detachably connected in the water washing pool, and the water washing tank can accommodate the zirconium hydroxide precipitate; a plurality of through holes are respectively opened on the side of the water washing tank close to the inlet pipe and the side close to the outlet pipe; filter frames are respectively detachably connected inside the water washing tank on the side close to the inlet pipe and the side close to the outlet pipe, and filter cloths are clamped in the filter frames; a chloride ion concentration analyzer is installed on the outlet pipe, and the output end of the chloride ion concentration analyzer is communicatively connected with the controller.

[0008] Preferably, the water washing tank is a hollow cuboid, and both ends of the water washing tank in the length direction are respectively clamped with corresponding positions of the water washing pool; a pool cover is installed on the upper part of the water washing pool.

[0009] Preferably, clamping heads are respectively fixedly connected to both ends of the water washing tank in the length direction, clamping grooves I are respectively formed at corresponding positions of the water washing pool, and the clamping heads are clamped with the clamping grooves I; clamping grooves II are formed at positions of the water washing tank corresponding to the filter frame.

[0010] Preferably, pressing grooves are formed around the filter frame, and the edge of the filter cloth is fixed into the pressing grooves through a rubber strip to fix the filter cloth.

[0011] Preferably, a water level gauge is installed on the water washing pool, and the output end of the water level gauge is communicatively connected with the controller.

[0012] Preferably, the water inlet pipe is installed on the upper part of the water inlet end of the water washing pool, and a flow control valve I is installed on the water inlet pipe; the water outlet pipe is installed on the lower part of the water outlet end of the water washing pool, and a flow control valve II is installed on the water outlet pipe; the flow control valve I and the flow control valve II are respectively communicatively connected with the controller; a drain pipe is further installed on the lower part of the water inlet end of the water washing pool, an electromagnetic valve is installed on the drain pipe, and the electromagnetic valve is communicatively connected with the controller.

[0013] Preferably, a centrifugal dehydration device is further included; the centrifugal dehydration device includes a turntable and a centrifugal water collection tank; the centrifugal water collection tank is installed on the outer periphery of the turntable; a fixing device is installed on the turntable; the fixing device is clamped with the water washing tank.

[0014] Preferably, a deionized water recycling treatment device is further included, and the deionized water recycling treatment device uses the ion exchange method to recycle deionized water.

[0015] A method for washing zirconium hydroxide uses the zirconium hydroxide washing device to wash the zirconium hydroxide precipitate obtained by reacting zirconyl chloride with an alkali, and includes the following steps: Step 1: Pour the zirconium hydroxide precipitate and solution obtained by reacting zirconyl chloride with an alkali into the water washing tank, open the electromagnetic valve on the drain pipe and the flow control valve II on the water outlet pipe, and the solution in the water washing tank enters between the water washing tank and the water washing pool through the through holes and the filter cloth, and then is completely discharged through the drain pipe and the water outlet pipe; Step 2: Close the electromagnetic valve on the drain pipe and the flow control valve II on the water outlet pipe; open the flow control valve I on the water inlet pipe, and introduce deionized water into the water washing pool and the water washing tank until the set liquid level is reached. At this time, the white zirconium hydroxide precipitate in the water washing tank is dispersed in the deionized water; Step 3: Open the flow control valve II on the outlet pipe, and control the flow control valve II and the flow control valve I so that the water inflow rate and the water outflow rate per unit time are equal; the water flow velocity in the water washing tank is less than 0.5 cm / s; Step 4: After the water in the water washing tank flows for a period of time, when the chloride ion concentration in the water monitored by the chloride ion concentration analyzer is lower than the set value, the controller controls the flow control valve I to close, increases the opening degree of the flow control valve II, and opens the solenoid valve on the drain pipe; Step 5: After the water in the water washing tank is emptied, close the flow control valve II and the solenoid valve on the drain pipe; Remove the water washing tank with the filter cloth from the water washing tank and install it on the fixing device of the centrifugal dehydration device; The turntable rotates to further centrifuge and dehydrate the zirconium hydroxide in the water washing tank, and the discharged water enters the centrifugal water collection tank; Step 6: After the turntable runs for a certain period of time, stop rotating, take out the zirconium hydroxide in the water washing tank and enter the next process; Then take out the filter cloth in the filter frame, ultrasonically clean the filter cloth and reuse it; Repeat Steps 1 to 6.

[0016] Preferably, the filter cloth is made of polyester non-woven fabric.

[0017] Compared with the prior art, the advantages and positive effects of the present invention are as follows: (1) This application changes the prior art and no longer uses a filter press to wash zirconium hydroxide; In the zirconium hydroxide washing method of this application, the white zirconium hydroxide precipitate is dispersed in deionized water instead of in the form of a filter cake, which is beneficial to the thorough washing of the zirconium hydroxide precipitate; (2) The water flow velocity in the water washing tank and the water washing trough is less than 0.5 cm / s, and the zirconium hydroxide precipitate will not move towards the filter cloth with the water flow (the dynamic pressure of the water flow is not enough to overcome the floc or colloid strength, adhesion or static friction), avoiding the blockage of the filter cloth and being beneficial to ensuring the washing effect; (3) In the zirconium hydroxide washing method of this application, the zirconium hydroxide is continuously washed, the operation is simple, there is no need to switch between angle washing and central washing, and there is no need for intermediate pressure filtration; (4) The water washing trough can be detachably connected to both the water washing tank and the centrifugal dehydration device. The operation from water washing to centrifugal dehydration is simple and efficient; (5) The filter frame is clamped with the water washing trough, and the filter cloth is clamped with the filter frame. The filter cloth after centrifugal dehydration is very easy to take out for ultrasonic cleaning; (6) The filter cloth after ultrasonic cleaning is reused, and the permeability of the filter cloth before each water washing can be ensured; (7) A flow control valve I is installed on the water inlet pipe, and a flow control valve II is installed on the water outlet pipe. By controlling the flow control valve I and the flow control valve II, the liquid level in the water washing trough can be kept basically unchanged, and the water flow rate in the water washing tank and the water tank trough can be controlled. Description of the Drawings

[0018] To more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the attached drawings required for the description of the embodiments: Figure 1 Schematic diagram of the zirconium hydroxide water washing device Figure 1 ; Figure 2 Schematic diagram of the zirconium hydroxide water washing device Figure 2 ; Figure 3 Schematic diagram of the zirconium hydroxide water washing device Figure 3 ; Figure 4 Top view of the water washing unit in the zirconium hydroxide water washing device; Figure 5 Top view of the water washing tank in the water washing unit; Figure 6 Schematic diagram of the water washing tank in the water washing unit Figure 1 ; Figure 7 Schematic diagram of the water washing tank in the water washing unit Figure 2 ; Figure 8 Schematic diagram of the filter frame in the water washing unit; Figure 9 Schematic diagram of the centrifugal dewatering device in the operating state; Figure 10 Schematic diagram of the centrifugal dewatering device in the no-load state.

[0019] Explanation of the reference numerals in the drawings: 1. Water washing tank, 101. First clamping groove; 2. Tank cover, 3. Water inlet pipe, 4. Water outlet pipe, 5. Drain pipe; 6. Water washing tank, 61. Clamping head, 62. Through hole, 63. Second clamping groove; 7. Filter frame, 71. Filter cloth; 8. Centrifugal dewatering device, 81. Fixing device, 82. Turntable, 83. Centrifugal water collection tank. Specific embodiments

[0020] In order to be able to more clearly understand the above objects, features and advantages of the present invention, the following further describes the present invention with reference to the drawings and embodiments.

[0021] In the following description, many specific details are set forth in order to fully understand the present invention. However, the present invention may be implemented in other ways different from those described herein. Therefore, the present invention is not limited by the specific embodiments disclosed in the following specification.

[0022] Embodiment 1 The following combines with Figures 1 - 10A zirconium hydroxide washing device in Example 1 is further described as follows. Figures 1 to 3 As shown, the zirconium hydroxide washing device in this embodiment includes a controller and a plurality of washing units. Each washing unit includes a washing tank 1. A water inlet pipe 3 is installed at one end of the washing tank 1, and a water outlet pipe 4 is installed at the other end.

[0023] As Figures 4 to 8 shown, a washing trough 6 is detachably connected in the washing tank 1, and the washing trough 6 can accommodate zirconium hydroxide precipitates. A plurality of through holes 62 are respectively formed on the side of the washing trough 6 close to the water inlet pipe 3 and the side close to the water outlet pipe 4. Filter frames 7 are respectively detachably connected inside the washing trough 6 on the side close to the water inlet pipe 3 and the side close to the water outlet pipe 4, and filter cloths 71 are clamped in the filter frames 7. A chloride ion concentration analyzer is installed on the water outlet pipe 4, and the output end of the chloride ion concentration analyzer is communicatively connected to the controller.

[0024] The bottom of the washing trough 6 contacts the bottom of the washing tank 1 to prevent water from passing through the washing trough 6 without going through it.

[0025] As Figure 6 and Figure 7 shown, the washing trough 6 is in the shape of a hollow cuboid, and both ends in the length direction of the washing trough 6 are respectively clamped with the corresponding positions of the washing tank 1. As Figure 3 shown, a tank cover 2 is installed on the upper part of the washing tank 1.

[0026] As Figure 5 and Figure 6 shown, clamping heads 61 are respectively fixedly connected to both ends in the length direction of the washing trough 6, and clamping grooves one 101 are respectively formed at the corresponding positions of the washing tank 1, and the clamping heads 61 are clamped with the clamping grooves one 101. Clamping grooves two 63 are formed at the corresponding positions of the washing trough 6 and the filter frames 7.

[0027] As Figure 8 shown, pressing grooves are formed around the filter frames 7, and the edges of the filter cloths 71 are fixed to the pressing grooves through rubber strips to fix the filter cloths 71.

[0028] A water level gauge is installed on the washing tank 1, and the output end of the water level gauge is communicatively connected to the controller.

[0029] The water inlet pipe 3 is installed at the upper part of the water inlet end of the washing tank 1, and a flow control valve one is installed on the water inlet pipe 3. The water outlet pipe 4 is installed at the lower part of the water outlet end of the washing tank 1, and a flow control valve two is installed on the water outlet pipe 4. The flow control valve one and the flow control valve two are respectively communicatively connected to the controller. A drain pipe 5 is also installed at the lower part of the water inlet end of the washing tank 1, and an electromagnetic valve is installed on the drain pipe 5, and the electromagnetic valve is communicatively connected to the controller.

[0030] As Figure 9 and Figure 10As shown in the figure, the zirconium hydroxide water washing device further includes a centrifugal dehydration device 8; the centrifugal dehydration device 8 includes a turntable 82 and a centrifugal water collecting tank 83; the centrifugal water collecting tank 83 is installed on the outer periphery of the turntable 82; a fixing device 81 is installed on the turntable 82; the fixing device 81 is snap-connected to the water washing tank 6.

[0031] The zirconium hydroxide water washing device further includes a deionized water recycling treatment device, and the deionized water recycling treatment device uses the ion exchange method to recycle deionized water.

[0032] A method for washing zirconium hydroxide uses the above zirconium hydroxide water washing device to wash the zirconium hydroxide precipitate obtained by reacting basic zirconium chloride with an alkali, including the following steps: Step 1: Pour the zirconium hydroxide precipitate and solution obtained by reacting basic zirconium chloride with an alkali (ammonia water in this embodiment) into the water washing tank 6, open the solenoid valve on the drain pipe 5 and the flow control valve II on the water outlet pipe 4, and the solution in the water washing tank 6 enters between the water washing tank 6 and the water washing pool 1 through the through holes 62 and the filter cloth 71, and then is completely discharged through the drain pipe 5 and the water outlet pipe 4; Step 2: Close the solenoid valve on the drain pipe 5 and the flow control valve II on the water outlet pipe 4; open the flow control valve I on the water inlet pipe 3, and introduce deionized water into the water washing pool 1 and the water washing tank 6 until the set liquid level is reached. At this time, the white zirconium hydroxide precipitate in the water washing tank 6 is dispersed in the deionized water; Step 3: Open the flow control valve II on the water outlet pipe 4, and control the flow control valve II and the flow control valve I so that the water inflow rate and the water outflow rate per unit time are equal; the water flow rate in the water washing pool 1 is less than 0.5 cm / s (a flow velocity meter is installed at the bottom of the water outlet side of the water washing pool 1 near the water washing tank 6, and the flow velocity meter is communicatively connected to the controller); the water flow rate in the water washing pool 1 and the water washing tank 6 is less than 0.5 cm / s, and the zirconium hydroxide precipitate will not move towards the filter cloth 71 with the water flow (the dynamic pressure of the water flow is not enough to overcome the floc or colloid strength, adhesion force or static friction force), avoiding the blockage of the filter cloth and also being beneficial to ensuring the water washing effect; Step 4: After the water in the water washing pool 1 has flowed for a period of time, when the chloride ion concentration in the water monitored by the chloride ion concentration analyzer is lower than the set value, the controller controls the flow control valve I to close, increases the opening degree of the flow control valve II and opens the solenoid valve on the drain pipe 5; Step 5: After the water in the water washing pool 1 is emptied, close the flow control valve II and the solenoid valve on the drain pipe 5; remove the water washing tank 6 with the filter cloth 71 from the water washing pool 1 and install it on the fixing device 81 of the centrifugal dehydration device 8; the turntable 82 rotates to further centrifugally dehydrate the zirconium hydroxide in the water washing tank 6, and the separated water enters the centrifugal water collecting tank 83; during the centrifugal dehydration process, the zirconium hydroxide will move towards the outer filter cloth 71; Step 6: After the turntable 82 runs for a certain period of time, it stops rotating. Take out the zirconium hydroxide in the water washing tank 6 and enter the next process. Then take out the filter cloth 71 in the filter frame 7, ultrasonically clean the filter cloth 71 and reuse it. Repeat Steps 1 to 6. The zirconium hydroxide washed off from the filter cloth 71 is recycled.

[0033] Before taking out the zirconium hydroxide in the water washing tank 6 in Step 6, use compressed air to blow the surface of the filter cloth 71 from the outside to preliminarily clean the zirconium hydroxide on the surface of the filter cloth 71.

[0034] The filter cloth 71 is made of polyester non-woven fabric.

[0035] Embodiment 2 The difference between this embodiment and Embodiment 1 is that the upper edge of the water washing tank 6 overlaps on the pool wall of the water washing pool 1 and the two are bolted together.

[0036] Embodiment 3 The difference between this embodiment and Embodiment 1 is that the filter cloth 71 is wrapped around the outer periphery of the water washing tank 6.

[0037] The above are only the preferred embodiments of the present invention, and are not limitations on the present invention in other forms. Any person skilled in the art may use the disclosed technical content to make changes or modifications into equivalent embodiments with equivalent changes and apply them to other fields. However, as long as it does not depart from the technical solution content of the present invention, any simple modification or equivalent change made to the above embodiments based on the technical essence of the present invention still belongs to the protection scope of the technical solution of the present invention.

Claims

1. A zirconium hydroxide water washing device, characterized in that, It includes a controller and multiple water washing units. Each water washing unit includes a water washing tank (1). A water inlet pipe (3) is installed at one end of the water washing tank (1), and a water outlet pipe (4) is installed at the other end. A water washing trough (6) is detachably connected inside the water washing tank (1), and zirconium hydroxide precipitate can be accommodated in the water washing trough (6). A plurality of through holes (62) are respectively formed on the side of the water washing trough (6) close to the water inlet pipe (3) and the side close to the water outlet pipe (4). Filter frames (7) are respectively detachably connected inside the water washing trough (6) on the side close to the water inlet pipe (3) and the side close to the water outlet pipe (4), and filter cloths (71) are clamped inside the filter frames (7). A chloride ion concentration analyzer is installed on the water outlet pipe (4), and the output end of the chloride ion concentration analyzer is communicatively connected with the controller.

2. The zirconium hydroxide washing device according to claim 1, wherein, The water washing trough (6) is in a hollow cuboid shape, and both ends in the length direction of the water washing trough (6) are respectively clamped with corresponding positions of the water washing tank (1). A tank cover (2) is installed on the upper part of the water washing tank (1).

3. The zirconium hydroxide water washing device according to claim 2, characterized in that, Both ends in the length direction of the water washing trough (6) are respectively fixedly connected with clamping heads (61), and clamping grooves one (101) are respectively formed at the corresponding positions of the water washing tank (1). The clamping heads (61) are clamped with the clamping grooves one (101). Clamping grooves two (63) are formed at the positions of the water washing trough (6) corresponding to the filter frames (7).

4. The zirconium hydroxide washing device according to claim 1, characterized in that, Pressing grooves are formed around the filter frame (7), and the edge of the filter cloth (71) is fixed into the pressing grooves through rubber strips to fix the filter cloth (71).

5. The zirconium hydroxide water washing device according to claim 4, characterized in that, A water level gauge is installed on the water washing tank (1), and the output end of the water level gauge is communicatively connected with the controller.

6. The zirconium hydroxide washing device according to claim 5, wherein The water inlet pipe (3) is installed on the upper part of the water inlet end of the water washing tank (1), and a flow control valve one is installed on the water inlet pipe (3). The water outlet pipe (4) is installed on the lower part of the water outlet end of the water washing tank (1), and a flow control valve two is installed on the water outlet pipe (4). The flow control valve one and the flow control valve two are respectively communicatively connected with the controller. A drain pipe (5) is further installed on the lower part of the water inlet end of the water washing tank (1), and an electromagnetic valve is installed on the drain pipe (5). The electromagnetic valve is communicatively connected with the controller.

7. The zirconium hydroxide washing device according to claim 6, wherein, It further includes a centrifugal dewatering device (8). The centrifugal dewatering device (8) includes a turntable (82) and a centrifugal water collection trough (83). The centrifugal water collection trough (83) is installed on the outer periphery of the turntable (82). A fixing device (81) is installed on the turntable (82). The fixing device (81) is clamped with the water washing trough (6).

8. The zirconium hydroxide water washing device according to claim 7, characterized in that, It further includes a deionized water recycling treatment device, and the deionized water recycling treatment device uses the ion exchange method to recycle deionized water.

9. A method for washing zirconium hydroxide, characterized in that, Using the zirconium hydroxide water washing device according to claim 8 to wash the zirconium hydroxide precipitate obtained by the reaction of basic zirconium chloride and an alkali includes the following steps: Step 1: Pour the zirconium hydroxide precipitate and solution obtained by reacting zirconium oxychloride with an alkali into the water washing tank (6). Open the solenoid valve on the drain pipe (5) and the flow control valve II on the water outlet pipe (4). The solution in the water washing tank (6) enters between the water washing tank (6) and the water washing pool (1) through the through hole (62) and the filter cloth (71), and then is completely discharged through the drain pipe (5) and the water outlet pipe (4). Step 2: Close the solenoid valve on the drain pipe (5) and the flow control valve II on the water outlet pipe (4). Open the flow control valve I on the water inlet pipe (3) and introduce deionized water into the water washing pool (1) and the water washing tank (6) until the set liquid level is reached. At this time, the white zirconium hydroxide precipitate in the water washing tank (6) is dispersed in the deionized water. Step 3: Open the flow control valve II on the water outlet pipe (4) and control the flow control valve II and the flow control valve I so that the water inflow rate and the water outflow rate per unit time are equal. The water flow rate in the water washing pool (1) is less than 0.5 cm / s. Step 4: After the water in the water washing pool (1) flows for a period of time, when the chloride ion concentration in the water monitored by the chloride ion concentration analyzer is lower than the set value, the controller controls the flow control valve I to close, increases the opening degree of the flow control valve II, and opens the solenoid valve on the drain pipe (5). Step 5: After the water in the water washing pool (1) is emptied, close the flow control valve II and the solenoid valve on the drain pipe (5). Remove the water washing tank (6) with the filter cloth (71) from the water washing pool (1) and install it on the fixing device (81) of the centrifugal dehydration device (8). The turntable (82) rotates to further dehydrate the zirconium hydroxide in the water washing tank (6), and the discharged water enters the centrifugal water collection tank (83). Step 6: After the turntable (82) operates for a certain period of time, it stops rotating. Take out the zirconium hydroxide in the water washing tank (6) and enter the next process. Then take out the filter cloth (71) in the filter frame (7), ultrasonically clean the filter cloth (71) and reuse it. Repeat Steps 1 to 6.

10. The zirconium hydroxide washing method according to claim 9, characterized in that, The filter cloth (71) is made of polyester non-woven fabric.

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