Zirconium oxychloride continuous crystallization device

Abstract

The utility model relates to a continuous crystallization device for zirconium oxychloride. The continuous zirconium oxychloride crystallization device comprises a reaction kettle array, an automatic centrifugal machine and a control system, the reaction kettle array comprises a plurality of cooling crystallization reaction kettles which are sequentially communicated end to end, and the cooling crystallization reaction kettle at the tail end is communicated with the automatic centrifugal machine; a cooling module is arranged on each cooling crystallization reaction kettle and comprises a cold water inlet and a hot water outlet; an electric valve is arranged at the front end of the cold water inlet, an electronic thermometer is arranged at the rear end of the hot water outlet, and the electronic thermometer and the electric valve are electrically connected with the control system. The continuous crystallization device for zirconium oxychloride disclosed by the utility model has the advantages of stable crystallization finished product and high crystallization efficiency.

Description

Technical Field

[0001] The utility model relates to the field of chemical equipment, in particular to a zirconium oxychloride continuous crystallization device. Background Art

[0002] The crystallization process in the production of zirconium oxychloride is as follows: after the liquid in the three-effect concentrated evaporator equipment reaches the process control index requirements, the material is discharged from the three-effect concentrated evaporator into multiple jacketed enamel crystallization pots, and cold water is passed into the enamel pot jacket for heat exchange, cooling and crystallization.

[0003] However, the existing jacketed enamel crystallization pot has a long cooling and crystallization time, and the crystallization quality of multiple jacketed enamel crystallization pots is different, resulting in a decrease in the quality of the final product. Utility Model Content

[0004] Based on this, the purpose of the utility model is to provide a zirconium oxychloride continuous crystallization device, which has the advantages of stable crystallization products and high crystallization efficiency.

[0005] A zirconium oxychloride continuous crystallization device comprises a reactor array, an automatic centrifuge and a control system; the reactor array comprises a plurality of cooling crystallization reactors which are connected end to end in sequence, and the terminal cooling crystallization reactor is connected to the automatic centrifuge; each cooling crystallization reactor is provided with a cooling module, and the cooling module comprises a cold water inlet and a hot water outlet; an electric valve is provided at the front end of the cold water inlet, and an electronic thermometer is provided at the rear end of the hot water outlet, and the electronic thermometer and the electric valve are electrically connected to the control system.

[0006] The zirconium oxychloride continuous crystallization device of the utility model obtains crystals with stable quality and high production efficiency through a reaction kettle with a stepwise decrease in working temperature.

[0007] Furthermore, it also includes a transfer tank, which is arranged between the reaction kettle array and the automatic centrifuge and is connected to the reaction kettle array and the automatic centrifuge respectively.

[0008] Furthermore, the transfer tank is provided with a transfer feed port and a transfer discharge port; the transfer feed port is provided on the upper side of the transfer tank and is connected to the terminal cooling crystallization reactor, the transfer discharge port is provided on the lower side of the transfer tank, and an extraction pump is provided at the rear end of the transfer discharge port.

[0009] Furthermore, the cold water inlet is arranged at the lower end of the cooling crystallization reactor, and the hot water outlet is arranged at the upper end of the cooling crystallization reactor.

[0010] Furthermore, each of the cooling crystallization reactors is provided with a feed inlet and a discharge port, wherein the feed inlet is provided above the cooling crystallization reactor, the discharge port is provided below the cooling crystallization reactor, and an extraction pump is provided at the rear end of the discharge port. Furthermore, the number of the cooling crystallization reactors is four or five.

[0011] In order to better understand and implement the present invention, the present invention is described in detail below with reference to the accompanying drawings. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 This is a schematic structural diagram of a continuous crystallization device for zirconium oxychloride according to an embodiment of the present utility model;

[0013] Figure 2 It is a schematic diagram of the structure of a cooling crystallization reactor according to an embodiment of the utility model. DETAILED DESCRIPTION

[0014] The following will be combined with the drawings in the embodiments of the utility model to clearly and completely describe the technical solutions in the embodiments of the utility model. Obviously, the described embodiments are only part of the embodiments of the utility model, not all of the embodiments. Based on the embodiments of the utility model, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the utility model.

[0015] In the description of the present invention, it should be noted that the terms "vertical direction", "upper", "lower", "horizontal" and the like indicate directions or positional relationships based on the directions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and therefore cannot be understood as limiting the present invention. In addition, "first", "second", "third", and "fourth" are only used for descriptive purposes and cannot be understood as indicating or implying relative importance.

[0016] In the description of the present invention, it is also necessary to explain that, unless otherwise clearly specified and limited, the terms "set", "install", "connect", and "connect" should be understood in a broad sense, for example, it can be a heat-conducting connection, a detachable connection, or an integral connection, a mechanical connection, an electrical connection, a direct connection, or a connection through an intermediate medium, or the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.

[0017] Example

[0018] The present invention provides a method for producing continuous crystallization of zirconium oxychloride, which specifically comprises the following steps:

[0019] S1: Alkali fusion: zircon is decomposed at high temperature with alkali, quenched with water, and most of the sodium and silicon are removed.

[0020] S2: Acid conversion; using hydrochloric acid to react with the hydrated zirconium oxide obtained in S1 to obtain a zirconate compound.

[0021] Step 3: Acid dissolution and aging: Add industrial hydrochloric acid to the zirconate compound obtained in S2 to react, and age the obtained acid-soluble material to produce silicon crystals.

[0022] S4: silicon removal; add water to the aged material obtained from S3, beat it into pulp, filter press and separate the crystalline silica gel to obtain zirconium oxychloride liquid.

[0023] S5: Concentration; the zirconium oxychloride liquid obtained in S4 is concentrated to a certain concentration through an evaporation concentration device.

[0024] S6: Cooling and crystallizing; placing the concentrated liquid obtained in S5 into a jacketed enamel pot, cooling and crystallizing to obtain zirconium oxychloride crystals.

[0025] The concentration of ZrO2 in the zirconium oxychloride solution obtained in step S4 is 90-120 g / L. The concentration of ZrO2 in the zirconium oxychloride solution obtained in step S5 is 200-240 g / L, and the concentration of HCl is 3.5-5.5 mol / L.

[0026] After studying the above-mentioned production method of continuous crystallization of zirconium oxychloride, the inventors found that during cooling crystallization, the existing jacketed enamel pot has a long cooling crystallization time and low efficiency, and the crystal quality between each crystallization pot is different, resulting in poor crystallization effect.

[0027] See also Figure 1 to Figure 2 The embodiment of the present application provides a zirconium oxychloride continuous crystallization device. The zirconium oxychloride continuous crystallization device includes a reactor array automatic centrifuge 2. The reactor array is connected to the automatic centrifuge 2, and the reactor array is used to cool and crystallize the concentrated feed liquid to obtain a crystallization feed liquid with zirconium oxychloride crystals; and then the crystallization feed liquid is pumped to the automatic centrifuge 2 for centrifugal separation.

[0028] The reactor array includes a plurality of cooling crystallization reactors that are connected in sequence. In this embodiment, the cooling crystallization reactor includes a first reactor 11, a second reactor 12, a third reactor 13, and a fourth reactor 14. The first reactor 11, the second reactor 12, the third reactor 13, and the fourth reactor 14 are connected in sequence, and the fourth reactor 14 is connected to the automatic centrifuge 2. The working temperature in the first reactor 11 to the fourth reactor 14 decreases in a stepwise manner, and the temperature difference intervals between the first reactor 11 to the fourth reactor 14 are equal.

[0029] Among them, the working temperature in the first reactor 11 is 70-60°C, the working temperature in the second reactor 12 is 60-50°C, the working temperature in the third reactor 13 is 50-40°C, and the working temperature in the fourth reactor 14 is 40-30°C. By setting four cooling crystallization reactors with step-down working temperatures, the crystallization time is reduced and the quality stability of the crystals obtained by each cooling crystallization reactor is improved.

[0030] Furthermore, the zirconium oxychloride continuous crystallization device also includes a control system; each cooling crystallization reactor is provided with a cooling module, the cooling module includes a cold water inlet 101 and a hot water outlet 102, an electric valve 101a is provided at the front end of the cold water inlet 101, and an electronic thermometer 102a is provided at the rear end of the hot water outlet 102, and the electronic thermometer 102a and the electric valve 101a are electrically connected to the control system. The electric valve 101a is connected to the cold water source, and the cooling water enters the cooling module from the cold water inlet 101 to cool the inside of the cooling crystallization reactor, and then is sent out from the hot water outlet 102; the water temperature of the sent hot water is measured by the electronic thermometer 102a, and a signal is fed back to the electric valve 101a to control the water intake of the cooling water inlet, thereby controlling the water temperature inside the cooling crystallization reactor.

[0031] In some embodiments, the cold water inlet 101 is arranged at the lower side of the cooling crystallization reactor, and the hot water outlet is arranged at the upper side of the cooling crystallization reactor. The cooling water enters the cooling module from the lower side and leaves from the upper side, thereby increasing the contact time and contact area between the cooling water and the cooling crystallization reactor and improving the cooling efficiency.

[0032] Further, the cooling crystallization reactor is provided with a feed port 103 and a discharge port 104, the feed port 103 is provided above the cooling crystallization reactor, the discharge port 104 is provided below the cooling crystallization reactor, and an extraction pump 105 is provided at the rear end of the discharge port 104, and the extraction pump 105 is used to extract the feed liquid into the reactor at the rear end. In some embodiments, the cooling crystallization reactor is also provided with a radar level gauge 106, the radar level gauge 106 and the extraction pump 105 are electrically connected to the control system, and the radar level gauge 106 detects the liquid level in the cooling crystallization reactor and feeds back a signal to the extraction pump 105, thereby controlling the extraction of the feed liquid.

[0033] Furthermore, the zirconium oxychloride continuous crystallization device of the embodiment of the utility model further includes a transfer tank 3, which is arranged between the reactor array and the automatic centrifuge 2, and is respectively connected to the reactor array and the automatic centrifuge 2. The reactor array obtains a crystallization liquid, which is first pumped into the transfer tank 3, and then pumped into the automatic centrifuge 2 for centrifugal separation after the crystallization liquid is stored to a certain capacity, so as to prevent the automatic centrifuge 2 from idling.

[0034] Furthermore, the transfer tank 3 is provided with a transfer feed port and a transfer discharge port, the transfer feed port is provided at the upper side of the transfer tank 3, the transfer discharge port is provided at the lower side of the transfer tank 3, and an extraction pump 105 is provided at the rear end of the transfer discharge port. The crystallization liquid of the reactor array is fed into the transfer tank 3 through the transfer feed port, and then pumped out from the transfer discharge port and fed into the automatic centrifuge 2. Since both the cooling crystallization reactor and the transfer tank 3 take materials from the lower side, it is possible to prevent solid crystals from accumulating on the lower side of the cooling crystallization reactor and the transfer tank 3, thereby improving the overall efficiency.

[0035] In some embodiments, the reactor array further includes a fifth reactor 15, which is disposed between the fourth reactor 14 and the automatic centrifuge 2, and the working temperature in the fifth reactor 15 is 40-30° C. By providing the fifth reactor 15, the utilization rate of the reactor array 1 for the feed liquid can be improved, thereby reducing the cost.

[0036] Compared with the prior art, the zirconium oxychloride continuous crystallization device of the utility model embodiment improves the cooling crystallization efficiency, and the quality of crystals obtained in multiple cooling crystallization reactors is close, which improves the yield rate and effectively reduces the cost.

[0037] The above-mentioned embodiments only express several implementation methods of the utility model, and the description is relatively specific and detailed, but it cannot be understood as limiting the scope of the utility model patent. It should be pointed out that for ordinary technicians in this field, several modifications and improvements can be made without departing from the concept of the utility model, and the utility model is also intended to include these modifications and modifications.

Claims

1. A zirconium oxychloride continuous crystallization device, characterized in that: It comprises a reactor array, an automatic centrifuge and a control system; the reactor array comprises a plurality of cooling crystallization reactors which are connected end to end in sequence, and the terminal cooling crystallization reactor is connected to the automatic centrifuge; each cooling crystallization reactor is provided with a cooling module, and the cooling module comprises a cold water inlet and a hot water outlet; an electric valve is provided at the front end of the cold water inlet, and an electronic thermometer is provided at the rear end of the hot water outlet, and the electronic thermometer and the electric valve are electrically connected to the control system.

2. The zirconium oxychloride continuous crystallization device according to claim 1, characterized in that: It also includes a transfer tank, which is arranged between the reaction kettle array and the automatic centrifuge and is connected to the reaction kettle array and the automatic centrifuge respectively.

3. The zirconium oxychloride continuous crystallization device according to claim 2, characterized in that: The transfer tank is provided with a transfer feed port and a transfer discharge port; the transfer feed port is provided on the upper side of the transfer tank and is connected to the terminal cooling crystallization reactor, the transfer discharge port is provided on the lower side of the transfer tank, and an extraction pump is provided at the rear end of the transfer discharge port.

4. The zirconium oxychloride continuous crystallization device according to claim 3, characterized in that: The cold water inlet is arranged at the lower end of the cooling crystallization reactor, and the hot water outlet is arranged at the upper end of the cooling crystallization reactor.

5. The zirconium oxychloride continuous crystallization device according to claim 4, characterized in that: Each of the cooling crystallization reactors is provided with a feed port and a discharge port. The feed port is arranged above the cooling crystallization reactor, the discharge port is arranged below the cooling crystallization reactor, and an extraction pump is arranged at the rear end of the discharge port.

6. The zirconium oxychloride continuous crystallization device according to claim 5, characterized in that: The number of the cooling crystallization reactors is four or five.

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