CN108946693B - Method for preparing high-purity zinc phosphate by mechanical activation continuous reaction - Google Patents
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Abstract
The invention discloses a method for preparing high-purity zinc phosphate by mechanical activation continuous reaction, which comprises the following steps of S1: respectively dissolving soluble carbonate or bicarbonate and soluble zinc salt in water to prepare carbonate or bicarbonate solution and zinc salt solution; s2: performing mechanical activation on a zinc salt solution and a carbonate or bicarbonate solution in a first reaction kettle in cooperation with a wet method to perform reaction to prepare a precipitate; s3: and (3) conveying the precipitate and the solution into a second reaction kettle, adding a phosphoric acid solution, and reacting under the condition of synergetic wet mechanical activation to obtain the zinc phosphate. The yield of the product obtained by the invention reaches 97.89-98.34%, the content of the zinc phosphate dihydrate is 99.27-99.56%, the content of the sulfate radical is 0.032-0.041%, the content of the chloride ion is 0.028-0.042%, and the content of the lead is 0.0012-0.0019%, which are superior to the yield and the quality of the product prepared by the prior art.
Description
[ technical field ] A method for producing a semiconductor device
The invention belongs to the technical field of preparation of inorganic salt, and particularly relates to a method for preparing high-purity zinc phosphate by mechanical activation continuous reaction.
[ background of the invention ]
Zinc phosphate is a novel nontoxic antirust pigment with excellent performance, and is applied to the paint industry for preparing various antirust paints and water aqua paints. With the development of science and technology and the enhancement of environmental awareness, low-toxic and nontoxic rust-preventive pigments represented by zinc phosphate and the like must gradually replace traditional and toxic rust-preventive pigments containing lead and chromium. At present, the method is used for producing various anticorrosive and antirust pigments, coatings, phosphating agents for metal surfaces such as steel, medical adhesives and dental adhesives, and is also used for producing chlorinated rubber, flame retardants, fire extinguishing agents, phosphors and the like. It is also used in the manufacture of electronic functional materials, fluorescent materials, etc. abroad. The yield and demand of zinc phosphate are rising year by year, and a wide space is provided for the development, production, application and development of zinc phosphate. But also has the disadvantages of high cost and high price. How to reduce the cost, develop high-efficiency, low-price, high-performance and fine powder products is a problem which needs to be solved urgently in developing the zinc phosphate industry at present.
The conventional production methods of zinc phosphate mainly fall into two categories: direct and indirect processes. The direct method takes zinc oxide and phosphoric acid as raw materials to directly react to prepare zinc phosphate, has simple process and no by-product, and is a production method commonly used in China at present. However, the direct method has the following disadvantages: firstly, the purity requirement of zinc oxide is high; secondly, the reaction is a solid-liquid reaction, and the produced zinc phosphate is easy to wrap the surface of the unreacted zinc oxide, so that the conversion rate of the zinc oxide is low, and the product quality of the zinc phosphate is reduced; thirdly, the main raw materials of phosphoric acid and zinc oxide have high market price and high product cost. The indirect method takes zinc salt and phosphate as raw materials to prepare the zinc phosphate, and the method has the advantages of high reaction speed, poor control, relatively complex production process, more byproducts, difficult product washing, easily caused overhigh water-soluble substance, difficult product control, low price of main raw materials, low product cost and price advantage. The invention patent CN101708835B (issued publication number) of this research subject group discloses a method for preparing high-purity zinc phosphate by mechanical activation continuous reaction, which is characterized in that: dissolving soluble zinc salt in water to obtain a zinc salt solution with the weight content of 0-30%, adding zinc powder, wherein the adding amount of the zinc salt solution is 1-10% of the weight of the soluble zinc salt, stirring, standing for a period of time, filtering, dissolving soluble carbonate or bicarbonate in water, reacting at 30-100 ℃ according to the molar ratio of carbonate ions to zinc ions of 0.9-2:1 to obtain zinc carbonate or basic zinc carbonate precipitate, reacting for 10-50 minutes under heat preservation, and reacting according to the molar ratio of phosphate ions to zinc ions of 0.7-1: 1, slowly adding phosphoric acid under stirring to react to prepare zinc phosphate, keeping the temperature at 50-100 ℃ to react for 10-50 minutes, filtering, washing, drying and crushing to obtain the high-purity zinc phosphate dihydrate. The method belongs to an indirect method, and because the intermittent reaction is adopted, the yield is low, water-soluble impurities are easily wrapped in the product, the product is not easy to wash away, the quality of the product is influenced, the reaction speed is high, the control is difficult, the product quality is unstable, and the control is not easy.
The research subject group combines a mechanical activation method and a continuous reaction to improve the production method, and overcomes the defects of impurity wrapping of products, low yield and difficult control of reaction speed in the prior art. Because the reaction speed of zinc ions and phosphate ions for generating zinc phosphate sediment is high, soluble ions can be wrapped in the zinc phosphate sediment in the process of generating the sediment, and the elution is not easy to cause influence on the quality of zinc phosphate. According to the invention, the ball grinding device is arranged in the reaction kettle, so that the reaction is carried out under the condition of wet mechanical activation, and the friction between the balls enables the precipitate generated by the reaction to be continuously crushed, so that the precipitate is changed between continuous enlargement and crushing, and finally, dynamic balance is formed, the excessive growth of the precipitate is avoided, and the coating of the precipitate on soluble ions is also avoided. The invention improves the intermittent reaction into semi-continuous reaction, simplifies the production process, reduces the reaction time, improves the yield and has wide popularization and application prospect.
[ summary of the invention ]
In order to overcome the defects of low yield and insufficient inclusion of impurities in the prior art, a method for preparing high-purity zinc phosphate by mechanical activation continuous reaction is provided. The method has the characteristics of continuous reaction, high yield, low impurity content and low cost.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for preparing high-purity zinc phosphate by mechanical activation continuous reaction comprises the following steps:
s1: respectively dissolving soluble carbonate or bicarbonate and soluble zinc salt in water, and preparing a carbonate or bicarbonate solution and a zinc salt solution according to the molar ratio of carbonate ions to zinc ions in unit volume;
s2: conveying a zinc salt solution into a first reaction kettle once, continuously adding a carbonate or bicarbonate solution, stopping feeding after adding the same volume of the carbonate or bicarbonate solution, enabling the two solutions to be cooperated with wet mechanical activation in the first reaction kettle, reacting to obtain zinc carbonate or basic zinc carbonate, precipitating, and then carrying out heat preservation reaction;
s3: and conveying the reacted precipitate and solution to a second reaction kettle, preparing a phosphoric acid solution according to the molar ratio of phosphate ions to zinc ions in unit volume, continuously adding the phosphoric acid solution at a certain flow rate, stopping feeding after adding the phosphoric acid solution with the same volume, reacting under the condition of synergetic wet mechanical activation to prepare zinc phosphate, and filtering, washing, drying and crushing after reaction to obtain the high-purity zinc phosphate dihydrate.
Preferably, the soluble carbonate described in step S1 includes one or more of ammonium carbonate, sodium carbonate, and potassium carbonate.
Preferably, the soluble bicarbonate described in step S1 includes one or more of ammonium bicarbonate, sodium bicarbonate, and potassium bicarbonate.
Preferably, the soluble zinc salt in step S1 includes one or more of zinc sulfate, zinc chlorate and zinc nitrate.
Preferably, the temperature of the two solutions in the first reaction kettle for synergic wet mechanical activation in the step S2 is 25-80 ℃.
Preferably, the incubation reaction time in step S2 is 5-20 minutes.
Preferably, the molar ratio of phosphate ions to zinc ions in step S3 is 0.7-1: 1.
preferably, the collaborative wet mechanical activation in step S3 is performed at 30-100 ℃.
Preferably, the reaction is carried out for 5 to 30 minutes in step S3, and then the mixture is filtered, washed, dried and crushed.
The invention has the following beneficial effects:
(1) the production method is a semi-continuous reaction process, the reaction processes are respectively carried out in two reaction kettles and are connected through a pipeline, and the semi-continuous operation process is realized.
(2) The production process of the invention is improved from the original intermittent reaction process to the continuous reaction process, thereby simplifying the production process, reducing the reaction time, improving the yield and having wide popularization and application prospects.
(3) The yield of the zinc phosphate dihydrate is high, and the product yield reaches 97.89-98.34%; the quality is high, the content of the zinc phosphate dihydrate is 99.27-99.56%, the content of the sulfate radical is 0.032-0.041%, the content of the chloride ion is 0.028-0.042%, the content of the lead is 0.0012-0.0019%, and the content of the cadmium is 0.0016-0.0021%, which are both superior to the yield and the quality of the comparative example 1 and the comparative example 2 (the prior art).
(4) From the results of the properties and the product yields of the products obtained in examples 1 to 3 and comparative example 2 (prior art) it can be seen that: the mechanical activation method is adopted, so that the yield and the quality of the product are obviously improved. The method of comparative example 2 (prior art) is indirect, and the batch reaction is adopted, so the yield is low, and the product is easy to wrap water-soluble impurities and is not easy to wash off, thereby affecting the quality of the product. And in the embodiment 1-3, the ball grinding device is arranged in the reaction kettle, so that the reaction is carried out under the condition of wet mechanical activation, the friction between the balls enables the precipitate generated by the reaction to be continuously crushed, the precipitate is changed between continuous increase and crushing, and finally, dynamic balance is formed, the excessive growth of the precipitate is avoided, the coating of the precipitate on soluble ions is also avoided, and the yield and the quality of the product are improved.
[ description of the drawings ]
FIG. 1 is a system for preparing high purity zinc phosphate.
[ detailed description ] embodiments
The following is a detailed description of specific embodiments.
Example 1
A method for preparing high-purity zinc phosphate by mechanical activation continuous reaction is carried out in a system for preparing high-purity zinc phosphate, wherein the system comprises a first reaction kettle and a second reaction kettle, and the method comprises the following steps:
s1: respectively dissolving soluble ammonium carbonate and soluble zinc sulfate in water, wherein the molar ratio of carbonate ions to zinc ions in unit volume is 1: 1 preparing an ammonium carbonate solution and a zinc sulfate solution;
s2: conveying the zinc sulfate solution into a first reaction kettle once, continuously adding an ammonium carbonate solution, stopping feeding after adding the ammonium carbonate solution with the same volume, enabling the two solutions to be cooperated with wet mechanical activation in the first reaction kettle at 25 ℃, reacting to obtain zinc carbonate or basic zinc carbonate precipitate, and keeping the temperature for reaction for 5 minutes; the first reaction kettle 1 comprises a first ball milling device 11 and a first reaction kettle shell 12; the first ball milling device 11 comprises a first motor 111, a first stirring paddle 112 and a sphere A113; the first motor 111 is arranged above the top of the first reaction kettle shell 12, the first stirring paddle 112 is connected with the first motor 111, and the spherical body A113 is arranged in the first reaction kettle shell 12; the top of the first reaction kettle shell 12 is respectively provided with a zinc salt solution inlet 121 and a carbonate or bicarbonate solution inlet 122; the round ball A113 is a glass ball, and the diameter of the round ball A113 is 8 mm;
s3: conveying the reacted precipitate and solution to a second reaction kettle 2, wherein an outlet 123 at the bottom of the first reaction kettle is connected with a first inlet 221 at the top of a second reaction kettle shell through a pipeline, and the second reaction kettle 2 comprises a second ball milling device 21 and a second reaction kettle shell 22; the second ball milling device 21 comprises a second motor 211, a second stirring paddle 212 and a sphere B213; the second motor 211 is arranged above the top of the second reaction kettle shell 22, the second stirring paddle 212 is connected with the second motor 211, and the spherical body B213 is arranged in the second reaction kettle shell 22; the top of the second reaction kettle shell 22 is respectively provided with a first inlet 221 and a sulfuric acid solution inlet 222; the round ball B213 is a zirconia ball, and the diameter of the round ball B213 is 8 mm; then according to the molar ratio of phosphate ions to zinc ions in unit volume of 0.7: 1 preparing a phosphoric acid solution, continuously adding the phosphoric acid solution at a certain flow rate, stopping feeding after adding the phosphoric acid solution with the same volume, reacting at the temperature of 30 ℃ under the condition of cooperation with wet mechanical activation to prepare zinc phosphate, and filtering, washing, drying and crushing after reacting for 5 minutes to obtain the high-purity zinc phosphate dihydrate.
Example 2
A method for preparing high-purity zinc phosphate by mechanical activation continuous reaction is carried out in a system for preparing high-purity zinc phosphate, wherein the system comprises a first reaction kettle and a second reaction kettle, and the method comprises the following steps:
s1: respectively dissolving soluble sodium bicarbonate and soluble zinc nitrate in water, wherein the molar ratio of carbonate ions to zinc ions in unit volume is 1.5: 1, preparing a sodium bicarbonate solution and a zinc nitrate solution;
s2: conveying the zinc sulfate solution into a first reaction kettle once, continuously adding an ammonium carbonate solution, stopping feeding after adding the ammonium carbonate solution with the same volume, enabling the two solutions to be cooperated with wet mechanical activation in the first reaction kettle at 50 ℃, reacting to obtain zinc carbonate or basic zinc carbonate precipitate, and keeping the temperature for reaction for 10 minutes; the first reaction kettle 1 comprises a first ball milling device 11 and a first reaction kettle shell 12; the first ball milling device 11 comprises a first motor 111, a first stirring paddle 112 and a sphere A113; the first motor 111 is arranged above the top of the first reaction kettle shell 12, the first stirring paddle 112 is connected with the first motor 111, and the spherical body A113 is arranged in the first reaction kettle shell 12; the top of the first reaction kettle shell 12 is respectively provided with a zinc salt solution inlet 121 and a carbonate or bicarbonate solution inlet 122; the sphere A113 is a glass sphere, and the diameter of the sphere A113 is 1 mm;
s3: conveying the reacted precipitate and solution to a second reaction kettle 2, wherein an outlet 123 at the bottom of the first reaction kettle is connected with a first inlet 221 at the top of a second reaction kettle shell through a pipeline, and the second reaction kettle 2 comprises a second ball milling device 21 and a second reaction kettle shell 22; the second ball milling device 21 comprises a second motor 211, a second stirring paddle 212 and a sphere B213; the second motor 211 is arranged above the top of the second reaction kettle shell 22, the second stirring paddle 212 is connected with the second motor 211, and the spherical body B213 is arranged in the second reaction kettle shell 22; the top of the second reaction kettle shell 22 is respectively provided with a first inlet 221 and a sulfuric acid solution inlet 222; the round ball B213 is a zirconia ball, and the diameter of the round ball B213 is 1 mm; and then according to the molar ratio of phosphate ions to zinc ions in unit volume of 0.8: 1 preparing phosphoric acid solution, continuously adding the phosphoric acid solution at a certain flow rate, stopping feeding after adding the phosphoric acid solution with the same volume, reacting at 60 ℃ under the condition of cooperation with wet mechanical activation to prepare zinc phosphate, and filtering, washing, drying and crushing after reacting for 15 minutes to obtain the high-purity zinc phosphate dihydrate.
Example 3
A method for preparing high-purity zinc phosphate by mechanical activation continuous reaction is carried out in a system for preparing high-purity zinc phosphate, wherein the system comprises a first reaction kettle and a second reaction kettle, and the method comprises the following steps:
s1: respectively dissolving soluble potassium carbonate and soluble zinc chlorate in water, wherein the molar ratio of carbonate ions to zinc ions in unit volume is 2:1, preparing a potassium carbonate solution and a zinc salt solution;
s2: conveying the zinc chlorate solution into a reaction kettle once, continuously adding the potassium carbonate solution, stopping adding the potassium carbonate solution with the same volume, performing mechanical activation on the two solutions in a first reaction kettle in cooperation with a wet method at the temperature of 80 ℃, reacting to prepare zinc carbonate or basic zinc carbonate precipitate, and performing heat preservation reaction for 20 minutes; the first reaction kettle 1 comprises a first ball milling device 11 and a first reaction kettle shell 12; the first ball milling device 11 comprises a first motor 111, a first stirring paddle 112 and a sphere A113; the first motor 111 is arranged above the top of the first reaction kettle shell 12, the first stirring paddle 112 is connected with the first motor 111, and the spherical body A113 is arranged in the first reaction kettle shell 12; the top of the first reaction kettle shell 12 is respectively provided with a zinc salt solution inlet 121 and a carbonate or bicarbonate solution inlet 122; the round ball A113 is a glass ball, and the diameter of the round ball A113 is 10 mm;
s3: conveying the reacted precipitate and solution to a second reaction kettle 2, wherein an outlet 123 at the bottom of the first reaction kettle is connected with a first inlet 221 at the top of a second reaction kettle shell through a pipeline, and the second reaction kettle 2 comprises a second ball milling device 21 and a second reaction kettle shell 22; the second ball milling device 21 comprises a second motor 211, a second stirring paddle 212 and a sphere B213; the second motor 211 is arranged above the top of the second reaction kettle shell 22, the second stirring paddle 212 is connected with the second motor 211, and the spherical body B213 is arranged in the second reaction kettle shell 22; the top of the second reaction kettle shell 22 is respectively provided with a first inlet 221 and a sulfuric acid solution inlet 222; the round ball B213 is a zirconia ball, and the diameter of the round ball B213 is 10 mm; and then according to the molar ratio of phosphate ions to zinc ions in unit volume of 1: 1 preparing phosphoric acid solution, continuously adding the phosphoric acid solution at a certain flow rate, stopping feeding after adding the phosphoric acid solution with the same volume, reacting under the condition of 100 ℃ and wet mechanical activation to prepare zinc phosphate, and filtering, washing, drying and crushing after reacting for 30 minutes to obtain the high-purity zinc phosphate dihydrate.
Comparative example 1
The process parameters were substantially the same as in example 2, except that the mechanical activation reaction was not performed in steps S2 and S3, and zinc phosphate dihydrate was prepared by a conventional dropping method.
Comparative example 2
Zinc phosphate dihydrate was prepared in examples 1 to 7 according to "a method for preparing high purity zinc phosphate by mechanical activation continuous reaction (grant No. CN 101708835B)".
Product performance test experiment
The properties and the product yields of the products obtained in examples 1 to 3 and comparative examples 1 to 2 were measured, respectively, and the results are shown in the following tables.
From the above table, it can be seen that: the yield of the zinc phosphate dihydrate is high, and the product yield reaches 97.89-98.34%; the quality is high, the content of the zinc phosphate dihydrate is 99.27-99.56%, the content of the sulfate radical is 0.032-0.041%, the content of the chloride ion is 0.028-0.042%, the content of the lead is 0.0012-0.0019%, and the content of the cadmium is 0.0016-0.0021%, which are both superior to the yield and the quality of the comparative example 1 and the comparative example 2 (the prior art).
In addition, as can be seen from the test results of comparative example 1 and example 2: the mechanical activation method is adopted, so that the yield and the quality of the product are obviously improved. This is embodiment 2 installs the ball-milling device in the reation kettle, makes the reaction go on under the condition of wet process mechanical activation, and the friction between ball makes the deposit that the reaction produced constantly suffer to pulverize, makes the deposit change between constantly increasing and breakage, forms dynamic balance at last, avoids deposit to grow too big, has also avoided the parcel of deposit to soluble ion simultaneously, has improved the output and the quality of product.
Additionally from the results of the properties and product yields of the products obtained in examples 1-3 and comparative example 2 (prior art) it is clear that: the mechanical activation method is adopted, so that the yield and the quality of the product are obviously improved. The method of comparative example 2 (prior art) is indirect, and the batch reaction is adopted, so the yield is low, and the product is easy to wrap water-soluble impurities and is not easy to wash off, thereby affecting the quality of the product. And in the embodiment 1-3, the ball grinding device is arranged in the reaction kettle, so that the reaction is carried out under the condition of wet mechanical activation, the friction between the balls enables the precipitate generated by the reaction to be continuously crushed, the precipitate is changed between continuous increase and crushing, and finally, dynamic balance is formed, the excessive growth of the precipitate is avoided, the coating of the precipitate on soluble ions is also avoided, and the yield and the quality of the product are improved.
The above description should not be taken as limiting the invention to the embodiments, but rather, as will be apparent to those skilled in the art to which the invention pertains, numerous simplifications or substitutions may be made without departing from the spirit of the invention, which shall be deemed to fall within the scope of the invention as defined by the claims appended hereto.
Claims (4)
1. A method for preparing high-purity zinc phosphate by mechanical activation continuous reaction is characterized by comprising the following steps:
s1: respectively dissolving soluble carbonate or bicarbonate and soluble zinc salt in water, and preparing a carbonate or bicarbonate solution and a zinc salt solution according to the molar ratio of carbonate ions to zinc ions in unit volume, wherein the molar ratio of carbonate ions to zinc ions is 1-2: 1;
s2: conveying a zinc salt solution into a first reaction kettle once, continuously adding a carbonate or bicarbonate solution, stopping feeding after adding the same volume of the carbonate or bicarbonate solution, enabling the two solutions to cooperate with wet mechanical activation in the first reaction kettle, reacting to obtain zinc carbonate or basic zinc carbonate, precipitating, and carrying out heat preservation reaction, wherein the temperature of the two solutions cooperating with the wet mechanical activation in the first reaction kettle is 25-80 ℃, and the time of the heat preservation reaction is 5-20 minutes;
s3: conveying the reacted precipitate and solution to a second reaction kettle, and preparing a phosphoric acid solution according to the molar ratio of phosphate ions to zinc ions in unit volume, wherein the molar ratio of the phosphate ions to the zinc ions is 0.7-1: continuously adding phosphoric acid solution at a certain flow rate, stopping feeding after adding the phosphoric acid solution with the same volume, reacting under the condition of synergetic wet-process mechanical activation to obtain zinc phosphate, reacting for 5-30 minutes, filtering, washing, drying and crushing to obtain high-purity zinc phosphate dihydrate, wherein the synergetic wet-process mechanical activation is carried out at 30-100 ℃.
2. The method for preparing high purity zinc phosphate by mechanically activating a continuous reaction according to claim 1, wherein: the soluble carbonate described in step S1 includes one or more of ammonium carbonate, sodium carbonate, and potassium carbonate.
3. The method for preparing high purity zinc phosphate by mechanically activating a continuous reaction according to claim 1, wherein: the soluble bicarbonate described in step S1 includes one or more of ammonium bicarbonate, sodium bicarbonate, and potassium bicarbonate.
4. The method for preparing high purity zinc phosphate by mechanically activating a continuous reaction according to claim 1, wherein: the soluble zinc salt in the step S1 includes one or more of zinc sulfate, zinc chlorate and zinc nitrate.
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| CN117550574A (en) * | 2023-07-21 | 2024-02-13 | 四川科尔瑞环保科技有限责任公司 | Synthetic method for preparing zinc phosphate by taking zinc-containing solution as raw material |
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