CN109133136B - Method for preparing strontium carbonate crystal by room temperature self-diffusion - Google Patents
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- CN109133136B CN109133136B CN201811336523.8A CN201811336523A CN109133136B CN 109133136 B CN109133136 B CN 109133136B CN 201811336523 A CN201811336523 A CN 201811336523A CN 109133136 B CN109133136 B CN 109133136B
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Abstract
The invention relates to a method for preparing strontium carbonate crystals by room-temperature self-diffusion, which takes strontium chloride hexahydrate and ammonium bicarbonate as reactants and glycine as a bionic control agent to prepare granular strontium carbonate crystals. Adding a first batch of strontium dichloride hexahydrate and ammonium bicarbonate into a reaction device, then adding a 0.020% glycine solution, standing at room temperature for 24 hours, and then supplementing a second batch of reactants and a third batch of reactants to continue standing and reacting for 24 hours respectively. Filtering the reaction product, washing with distilled water for 3 times, and drying at 105 deg.c for 1 hr to obtain granular strontium carbonate crystal of 110-440 nm grain size, product purity not lower than 99% and yield 96-98%. The reaction device consists of a first reactor (5), a second reactor (9) and a third reactor (13). The method has the advantages of high preparation efficiency, simple and convenient operation, high process stability, low energy consumption, low production cost and the like.
Description
Technical Field
The invention relates to a method for preparing strontium carbonate crystals by room-temperature self-diffusion, in particular to a method for preparing granular strontium carbonate crystals by taking strontium chloride hexahydrate and ammonium bicarbonate as reactants and glycine as a bionic control agent. The invention belongs to the technical field of preparation of strontium carbonate crystals.
Background
Strontium carbonate is an important industrial raw material, has a strong shielding function on X rays, can obviously improve the refractive index of glass and the flow energy of molten glass, and is widely used for producing electronic components such as a picture tube and the like and a display. The demand of high-purity strontium carbonate in modern society is increasing.
At present, the preparation methods of strontium carbonate crystals are many, and the main preparation methods comprise: precipitation method, homogeneous precipitation method, impinging stream reaction-precipitation method, hydrothermal method and microwave reaction method. The precipitation method is that strontium chloride hexahydrate and sodium citrate are mixed and dissolved, heated to 50 ℃, stirred and dropwise added with sodium carbonate aqueous solution, and then stirred and reacted for 1 hour after dropwise addition is finished, so as to generate strontium carbonate precipitate. The precipitation method needs heating and expensive sodium citrate, so the precipitation method has the defects of high energy consumption, slightly complex operation, high preparation cost and the like. The homogeneous precipitation method is to utilize urea to hydrolyze homogeneously at 85 ℃ so as to release the crystal-forming anion CO 32-in the solution uniformly and slowly, thereby slowly generating strontium carbonate precipitate with the crystal-forming cation Sr2+ in the solution. The homogeneous precipitation method has the disadvantages of high energy consumption, high preparation cost and the like because the reaction temperature required to be reached by the homogeneous precipitation method is 85 ℃ and the continuous heating time is long. The impinging stream reaction-precipitation method is to add ammonium bicarbonate solution with the temperature of 40 ℃ into the impinging stream reactor, and dropwise add strontium nitrate solution with the temperature of 85 ℃ to finally obtain the nano strontium carbonate. It is easy to see that the impinging stream reaction-precipitation method has the defects of high energy consumption, complex reaction equipment, low process stability, high preparation cost and the like. The hydrothermal method is that the block copolymer, strontium dichloride hexahydrate and hydrazine hydrate are dissolved in deionized water at room temperature, and then reacted at constant temperature of 160-200 ℃ for 12h, and then naturally cooled to room temperature to generate strontium carbonate precipitate. Obviously, the hydrothermal method has the disadvantages of high reaction temperature, high temperature resistance and pressure resistance of reaction equipment, high energy consumption, high equipment requirement, high preparation cost and the like. The microwave reaction method is to heat the reaction system by using a unique non-heat transfer heating mode, namely microwave, so that the heat effect and the non-heat effect of the microwave simultaneously influence the progress of the chemical reaction. The generation of microwaves requires external energy and local overheating is prone to occur. It is not difficult to discover that the microwave reaction method has the defects of complex reaction equipment, poor process stability, higher energy consumption, high preparation cost and the like. In summary, the existing preparation method of strontium carbonate crystals has the disadvantages of complex operation, low process stability, high energy consumption, high production cost and the like.
Aiming at the defects of complex operation, low process stability, high energy consumption, high production cost and the like of the conventional preparation method of the strontium carbonate crystal, the invention provides the preparation method of the strontium carbonate crystal, which has the advantages of high preparation efficiency, simple and convenient operation, high process stability, low energy consumption and low cost.
Disclosure of Invention
The invention aims to provide a preparation method of strontium carbonate crystals, which has the advantages of high preparation efficiency, simple and convenient operation, high process stability, low energy consumption and low production cost, aiming at the defects of complex operation, difficult control of reaction, high energy consumption, high cost and the like of the existing preparation method of the strontium carbonate crystals.
The invention relates to a method for preparing strontium carbonate crystals by room-temperature self-diffusion, which takes strontium dichloride hexahydrate and ammonium bicarbonate as reactants and glycine as a bionic control agent to prepare granular strontium carbonate crystals.
The method comprises the following steps: in a reaction device, adding reactants of strontium dichloride hexahydrate and ammonium bicarbonate into the reaction device in three batches according to the mass ratio of the strontium dichloride hexahydrate to the ammonium bicarbonate being 1: 1.03-1.09, wherein the mass ratio of the reactants of the three batches is kept unchanged. Adding a first batch of strontium chloride hexahydrate into a first material tank (1) of a first reactor (5), adding a first batch of ammonium bicarbonate into a second material tank (3) of a third reactor (13), and opening a first valve (6), a second valve (8), a third valve (10) and a fourth valve (12) in a reaction device; 0.020 wt% glycine solution is added from the reactor II (9) to the water level mark (4), and the mixture is kept stand and reacted for 24 hours at room temperature. And adding a second batch of strontium chloride hexahydrate into the first material tank (1) of the first reactor (5), adding a second batch of ammonium bicarbonate into the second material tank (3) of the third reactor (13), and standing for reaction for 24 hours at room temperature. And adding a third batch of strontium chloride hexahydrate into the first material tank (1) of the first reactor (5), adding a third batch of ammonium bicarbonate into the second material tank (3) of the third reactor (13), standing for reaction for 48 hours at room temperature, and then closing the four valves. And (3) disassembling the first disassembling position (7) and the second disassembling position (11), filtering a product generated in the second reactor (9), washing the product for 3 times by using distilled water, and drying the product for 1h at 105 ℃ to obtain granular strontium carbonate crystals with the grain diameter of 110nm to 440nm, wherein the purity of the product is more than or equal to 99 percent, and the yield is 96 to 98 percent.
The reaction device is as follows: the reactor consists of a first reactor (5), a second reactor (9) and a third reactor (13). The three reactors are all cuboids with the length of 40cm, the width of 40cm and the height of 80cm, and the effective volume is 120L. The reactors are connected by a detachable pipeline, and a first valve (6) and a second valve (8) are arranged on the pipeline between the first reactor (5) and the second reactor (9); a third valve (10) and a fourth valve (12) are arranged on a pipeline between the second reactor (9) and the third reactor (13), whether the second reactor (9) is communicated with the third reactor (13) or not is controlled, the first reactor (5) and the third reactor (13) are respectively provided with a material groove and five horizontal separation plates (14), the upper edges of the two material grooves are lower than a water level scale mark (4) by 5cm, a 10cm interval is reserved between the horizontal separation plates (14) of the first reactor (5) and the third reactor (13), and each horizontal separation plate (14) is 5cm away from the wall of the reaction device. The second reactor (9) is provided with 3 vertical baffle plates (2), the bottom end of the middle vertical baffle plate (2) is spaced from the bottom of the second reactor (9) by 20cm, and the upper edges of the other two vertical baffle plates (2) are lower than the water level scale mark (4) by 5 cm.
The invention has the beneficial effects that: 1) the preparation efficiency is high: the purity of the strontium carbonate crystal is more than or equal to 99 percent, the yield is 96 to 98 percent, and the product of the strontium carbonate has high purity and high yield. 2) The operation is simple and convenient: at room temperature and standing, the reactants are free to diffuse to form strontium carbonate crystals. 3) The process stability is high: the reaction condition is mild, and the preparation parameters are easy to control. 4) The energy consumption is low: the reaction process is carried out spontaneously at room temperature without providing external energy. 5) The production cost is low: the reactant is strontium dichloride hexahydrate, ammonium bicarbonate is cheap and easy to obtain, and the consumption of glycine is low.
Drawings
FIG. 1 is an SEM image of strontium carbonate crystals prepared by the present invention;
FIG. 2 is an XRD pattern of strontium carbonate crystals prepared according to the present invention;
FIG. 3 is a schematic view of a reaction apparatus for preparing strontium carbonate crystals according to the present invention;
in fig. 3: 1. a first material groove; 2. a vertical barrier plate; 3. a second material groove; 4. water level scale lines; 5. a reactor No. one; 6. a first valve; 7. a first disassembly position; 8. a second valve; 9. a reactor II; 10. a third valve; 11. a second disassembly bit; 12. a valve number four; 13. a reactor III; 14. a horizontal barrier plate.
Detailed Description
The method for preparing strontium carbonate crystal by room temperature self-diffusion according to the present invention is further described below with reference to the following specific examples.
Example 1
In a reaction device, 0.60kg of strontium dichloride hexahydrate is added into a first material tank (1) of a first reactor (5), 0.64kg of ammonium bicarbonate is added into a second material tank (3) of a third reactor (13), a first valve (6), a second valve (8), a third valve (10) and a fourth valve (12) in the reaction device are opened, 0.020% glycine solution is added into the second reactor (9) to reach a water level scale line (4), and standing reaction is carried out for 24 hours at room temperature. 0.60kg of strontium dichloride hexahydrate is added into a first material tank (1) of a first reactor (5), 0.64kg of ammonium bicarbonate is added into a second material tank (3) of a third reactor (13), and standing reaction is carried out for 24 hours under the condition of room temperature. Adding 0.60kg of strontium chloride hexahydrate into a first material tank (1) of a first reactor (5), adding 0.64kg of ammonium bicarbonate into a second material tank (3) of a third reactor (13), standing for reaction for 48 hours at room temperature, closing four valves, disassembling a first disassembling position (7) and a second disassembling position (11), filtering a product generated in the second reactor (9), washing for 3 times by using distilled water, and drying for 1 hour at 105 ℃ to obtain granular strontium carbonate crystals with the grain diameter of 110-440 nm, wherein the purity of the product is more than or equal to 99%, and the yield is 97%.
The reaction device is as follows: the reactor consists of a first reactor (5), a second reactor (9) and a third reactor (13). The three reactors are all cuboids with the length of 40cm, the width of 40cm and the height of 80cm, and the effective volume is 120L. The reactors are connected by a detachable pipeline, and a first valve (6) and a second valve (8) are arranged on the pipeline between the first reactor (5) and the second reactor (9); a third valve (10) and a fourth valve (12) are arranged on a pipeline between the second reactor (9) and the third reactor (13), whether the second reactor (9) is communicated with the third reactor (13) or not is controlled, the first reactor (5) and the third reactor (13) are respectively provided with a material groove and five horizontal separation plates (14), the upper edges of the two material grooves are lower than a water level scale mark (4) by 5cm, a 10cm interval is reserved between the horizontal separation plates (14) of the first reactor (5) and the third reactor (13), and each horizontal separation plate (14) is 5cm away from the wall of the reaction device. The second reactor (9) is provided with 3 vertical baffle plates (2), the bottom end of the middle vertical baffle plate (2) is spaced from the bottom of the second reactor (9) by 20cm, and the upper edges of the other two vertical baffle plates (2) are lower than the water level scale mark (4) by 5 cm.
Example 2
In a reaction device, 0.60kg of strontium chloride hexahydrate is added into a first material tank (1) of a first reactor (5), 0.62kg of ammonium bicarbonate is added into a second material tank (3) of a third reactor (13), a first valve (6), a second valve (8), a third valve (10) and a fourth valve (12) in the reaction device are opened, 0.020% glycine solution is added into the second reactor (9) to reach a water level scale line (4), and standing reaction is carried out for 24 hours at room temperature. 0.60kg of strontium dichloride hexahydrate is added into a first material tank (1) of a first reactor (5), 0.62kg of ammonium bicarbonate is added into a second material tank (3) of a third reactor (13), and standing reaction is carried out for 24 hours under the condition of room temperature. Adding 0.60kg of strontium chloride hexahydrate into a first material tank (1) of a first reactor (5), adding 0.62kg of ammonium bicarbonate into a second material tank (3) of a third reactor (13), standing for reaction for 48 hours at room temperature, closing four valves, disassembling a first disassembling position (7) and a second disassembling position (11), filtering a product generated in the second reactor (9), washing for 3 times by using distilled water, and drying for 1 hour at 105 ℃ to obtain granular strontium carbonate crystals with the grain diameter of 110-440 nm, wherein the purity of the product is more than or equal to 99%, and the yield is 96%.
The reaction device is as follows: the reactor consists of a first reactor (5), a second reactor (9) and a third reactor (13). The three reactors are all cuboids with the length of 40cm, the width of 40cm and the height of 80cm, and the effective volume is 120L. The reactors are connected by a detachable pipeline, and a first valve (6) and a second valve (8) are arranged on the pipeline between the first reactor (5) and the second reactor (9); a third valve (10) and a fourth valve (12) are arranged on a pipeline between the second reactor (9) and the third reactor (13), whether the second reactor (9) is communicated with the third reactor (13) or not is controlled, the first reactor (5) and the third reactor (13) are respectively provided with a material groove and five horizontal separation plates (14), the upper edges of the two material grooves are lower than a water level scale mark (4) by 5cm, a 10cm interval is reserved between the horizontal separation plates (14) of the first reactor (5) and the third reactor (13), and each horizontal separation plate (14) is 5cm away from the wall of the reaction device. The second reactor (9) is provided with 3 vertical baffle plates (2), the bottom end of the middle vertical baffle plate (2) is spaced from the bottom of the second reactor (9) by 20cm, and the upper edges of the other two vertical baffle plates (2) are lower than the water level scale mark (4) by 5 cm.
Example 3
In a reaction device, 0.60kg of strontium chloride hexahydrate is added into a first material tank (1) of a first reactor (5), 0.66kg of ammonium bicarbonate is added into a second material tank (3) of a third reactor (13), a first valve (6), a second valve (8), a third valve (10) and a fourth valve (12) in the reaction device are opened, 0.020% glycine solution is added into the second reactor (9) to reach a water level scale line (4), and standing reaction is carried out for 24 hours at room temperature. 0.60kg of strontium dichloride hexahydrate is added into a first material tank (1) of a first reactor (5), 0.66kg of ammonium bicarbonate is added into a second material tank (3) of a third reactor (13), and standing reaction is carried out for 24 hours under the condition of room temperature. Adding 0.60kg of strontium chloride hexahydrate into a first material tank (1) of a first reactor (5), adding 0.66kg of ammonium bicarbonate into a second material tank (3) of a third reactor (13), standing for reaction for 48 hours at room temperature, closing four valves, disassembling a first disassembling position (7) and a second disassembling position (11), filtering a product generated in the second reactor (9), washing for 3 times by using distilled water, and drying for 1 hour at 105 ℃ to obtain granular strontium carbonate crystals with the grain diameter of 110-440 nm, wherein the purity of the product is more than or equal to 99%, and the yield is 98%.
The reaction device is as follows: the reactor consists of a first reactor (5), a second reactor (9) and a third reactor (13). The three reactors are all cuboids with the length of 40cm, the width of 40cm and the height of 80cm, and the effective volume is 120L. The reactors are connected by a detachable pipeline, and a first valve (6) and a second valve (8) are arranged on the pipeline between the first reactor (5) and the second reactor (9); a third valve (10) and a fourth valve (12) are arranged on a pipeline between the second reactor (9) and the third reactor (13), whether the second reactor (9) is communicated with the third reactor (13) or not is controlled, the first reactor (5) and the third reactor (13) are respectively provided with a material groove and five horizontal separation plates (14), the upper edges of the two material grooves are lower than a water level scale mark (4) by 5cm, a 10cm interval is reserved between the horizontal separation plates (14) of the first reactor (5) and the third reactor (13), and each horizontal separation plate (14) is 5cm away from the wall of the reaction device. The second reactor (9) is provided with 3 vertical baffle plates (2), the bottom end of the middle vertical baffle plate (2) is spaced from the bottom of the second reactor (9) by 20cm, and the upper edges of the other two vertical baffle plates (2) are lower than the water level scale mark (4) by 5 cm.
Claims (1)
1. A method for preparing strontium carbonate crystals by self-diffusion at room temperature is characterized by comprising the following steps: the method takes strontium chloride hexahydrate and ammonium bicarbonate as reactants and glycine as a bionic control agent to prepare granular strontium carbonate crystals;
the method comprises the following steps: in a reaction device, adding reactants of strontium dichloride hexahydrate and ammonium bicarbonate into the reaction device in three batches according to the mass ratio of the strontium dichloride hexahydrate to the ammonium bicarbonate being 1: 1.03-1.09, wherein the mass ratio of the reactants of the three batches is kept unchanged; adding a first batch of strontium chloride hexahydrate into a first material tank (1) of a first reactor (5), adding a first batch of ammonium bicarbonate into a second material tank (3) of a third reactor (13), and opening a first valve (6), a second valve (8), a third valve (10) and a fourth valve (12) in a reaction device; adding 0.020 wt% of glycine solution from the reactor II (9) to a water level scale mark (4), and standing for reaction for 24 hours at room temperature; adding a second batch of strontium chloride hexahydrate into a first material tank (1) of a first reactor (5), adding a second batch of ammonium bicarbonate into a second material tank (3) of a third reactor (13), and standing and reacting for 24 hours at room temperature; adding a third batch of strontium chloride hexahydrate into a first material tank (1) of a first reactor (5), adding a third batch of ammonium bicarbonate into a second material tank (3) of a third reactor (13), standing for reaction for 48 hours at room temperature, and then closing the four valves; disassembling the first disassembling position (7) and the second disassembling position (11), filtering a product generated in the second reactor (9), washing the product for 3 times by using distilled water, and drying the product for 1h at 105 ℃ to obtain granular strontium carbonate crystals with the grain diameter of 110nm to 440nm, wherein the purity of the product is more than or equal to 99 percent, and the yield is 96 to 98 percent;
the reaction device comprises: the device consists of a first reactor (5), a second reactor (9) and a third reactor (13); the three reactors are cuboids with the length of 40cm, the width of 40cm and the height of 80cm, and the effective volumes are all 120L; the reactors are connected by a detachable pipeline, and a first valve (6) and a second valve (8) are arranged on the pipeline between the first reactor (5) and the second reactor (9); a third valve (10) and a fourth valve (12) are arranged on a pipeline between the second reactor (9) and the third reactor (13); the first reactor (5) and the third reactor (13) are both provided with a material groove and five staggered horizontal baffle plates (14), and the upper edges of the two material grooves are 5cm lower than the water level scale mark (4); 10cm of interval is reserved between each horizontal baffle plate (14) of the first reactor (5) and the third reactor (13), and each horizontal baffle plate (14) is 5cm away from the wall of the first reactor or the second reactor; the second reactor (9) is provided with three staggered vertical baffle plates (2), the bottom end of the middle vertical baffle plate (2) is spaced from the bottom of the second reactor (9) by 20cm, and the upper edges of the left and right vertical baffle plates (2) are lower than the water level scale mark (4) by 5 cm.
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CN207221923U (en) * | 2017-09-11 | 2018-04-13 | 西南科技大学 | A kind of strontium carbonate crystallization reactor |
CN108675335A (en) * | 2018-09-03 | 2018-10-19 | 南昌航空大学 | A kind of bionical method for preparing carbonic acid strontium crystal |
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CN207221923U (en) * | 2017-09-11 | 2018-04-13 | 西南科技大学 | A kind of strontium carbonate crystallization reactor |
CN108675335A (en) * | 2018-09-03 | 2018-10-19 | 南昌航空大学 | A kind of bionical method for preparing carbonic acid strontium crystal |
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