CN112209426A - Basic zinc chloride and preparation method thereof - Google Patents
Basic zinc chloride and preparation method thereof Download PDFInfo
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Abstract
A preparation method of basic zinc chloride comprises the following steps: preparing a basic zinc chloride precursor system: providing a zinc-containing reaction system, setting reaction conditions and stirring the zinc-containing reaction system to prepare a basic zinc chloride precursor system; and preparing jewel flower-shaped crystalline basic zinc chloride by hydrothermal precipitation reaction: and (2) placing the basic zinc chloride precursor system in a hydrothermal reaction environment and stirring at a constant speed to enable the basic zinc chloride precursor to generate a hydrothermal reaction, filtering the reactant of the hydrothermal reaction to obtain white crystals, and washing and drying the white crystals to obtain the jewel flower-shaped crystalline basic zinc chloride. The invention also relates to basic zinc chloride. The basic zinc chloride and the preparation method thereof provided by the invention have the advantages of high synthesis yield, high purity, high particle crystallinity and obvious crystal characteristics.
Description
Technical Field
The invention relates to the field of chemical raw material preparation and material raw material preparation, in particular to basic zinc chloride and a preparation method thereof.
Background
Basic zinc chloride with molecular formula Zn5(OH)8Cl2·H2And O, the microscopic particles are white or colorless and transparent. Basic zinc chloride is poorly soluble in water and readily soluble in weak acids and bases. The basic zinc chloride has the characteristics of extremely low moisture absorption rate in air, weak oxidizability, small destructive effect on nutrient substances such as grease, vitamins, enzyme preparations and the like, and is used as a novel zinc source used as a feed additive in recent years and has a tendency of replacing inorganic zinc source additives such as zinc sulfate, zinc oxide and the like.
Most of the existing methods for preparing basic zinc chloride are liquid-liquid phase synthesis methods or liquid-solid phase synthesis methods at normal temperature, and ammonia water, ammonium chloride or organic amine salt and other substances are used as an inducer for induction synthesis. The methods have the defects of low synthesis yield of the basic zinc chloride, impure basic zinc chloride, low particle crystallinity, unobvious crystal characteristics and the like, thereby influencing the further wide application of the basic zinc chloride in the field of feed or materials.
Disclosure of Invention
In view of the above, the invention provides a preparation method of basic zinc chloride, which has high synthesis yield, high purity, high particle crystallinity and obvious crystal characteristics.
In addition, it is necessary to provide a basic zinc chloride prepared by the preparation method of the basic zinc chloride.
A preparation method of basic zinc chloride comprises the following steps: preparing a basic zinc chloride precursor system: providing a zinc-containing reaction system, setting reaction conditions and stirring the zinc-containing reaction system to prepare a basic zinc chloride precursor system; and preparing jewel flower-shaped crystalline basic zinc chloride by hydrothermal precipitation reaction: and (2) placing the basic zinc chloride precursor system in a hydrothermal reaction environment and stirring at a constant speed to enable the basic zinc chloride precursor to generate a hydrothermal reaction, filtering the reactant of the hydrothermal reaction to obtain white crystals, and washing and drying the white crystals to obtain the jewel flower-shaped crystalline basic zinc chloride.
Further, in the step of "preparing basic zinc chloride precursor system", the reaction conditions are as follows: the pH value is 4.8-5.8, the reaction temperature is not more than 60 ℃, and the charging and reaction time is 5-30 minutes.
Further, in the step of preparing the floriform crystalline basic zinc chloride by the hydrothermal precipitation reaction, the temperature of the hydrothermal reaction environment is 90-200 ℃, the pH value is 5.5-6, and the reaction time of the hydrothermal reaction is 1-8 hours.
Further, the zinc-containing reaction system is a first reaction system formed by reacting a zinc chloride solution with a zinc oxide slurry or a zinc hydroxide slurry or a sodium hydroxide solution.
Further, when the basic zinc chloride precursor system is prepared by adopting the first reaction system, the concentration of zinc in the used zinc chloride solution is 90-140 g/L, and the concentration of zinc in the used zinc oxide slurry is 200-280 g/L.
Further, when the basic zinc chloride precursor system is prepared by adopting the first reaction system, the concentration of zinc in the used zinc chloride solution is 90-140 g/L, and the mass fraction of the used sodium hydroxide solution is 30%.
Further, when the basic zinc chloride precursor system is prepared by adopting the first reaction system, the concentration of zinc in the used zinc chloride solution is 90-140 g/L, and the concentration of zinc in the used zinc hydroxide slurry is 200-280 g/L.
Further, the zinc-containing reaction system is a second reaction system formed by reacting hydrochloric acid with zinc oxide slurry or zinc hydroxide slurry.
Further, when the basic zinc chloride precursor system is prepared by adopting the second reaction system, the concentration of zinc in the used zinc oxide slurry is 200-280 g/L, and the mass fraction of the used hydrochloric acid solution is 15%.
Further, when the basic zinc chloride precursor system is prepared by adopting the second reaction system, the concentration of zinc in the used zinc hydroxide slurry is 150-200 g/L, and the mass fraction of the used hydrochloric acid solution is 15%.
Further, the zinc-containing reaction system is added simultaneously.
Further, in the step of preparing the jewel flower-shaped crystalline basic zinc chloride by the hydrothermal precipitation reaction, pure water is adopted for washing.
Further, in the step of preparing the jewel flower-shaped crystalline basic zinc chloride by the hydrothermal precipitation reaction, the drying temperature in the drying process is 50-105 ℃.
The basic zinc chloride prepared by the preparation method of the basic zinc chloride has a jewel flower-shaped crystal form, crystal particles of the jewel flower-shaped crystal are uniform, the overall size of the crystal is about 20-200 um, the length of petals is 1-100 um, the width of the petals is 1-100 um, and the thickness of the petals is 1-20 um.
The invention provides basic zinc chloride and a preparation method thereof, 1) firstly preparing a basic zinc chloride precursor system, then carrying out hydrothermal reaction to dissolve fine-particle basic zinc chloride in the precursor system to obtain a zinc source, and under the hydrothermal reaction condition, continuously carrying out precipitation reaction on the surface of large-particle basic zinc chloride according to the original crystal face. Under the 'poor-killing and rich-economy' environment, small particles disappear, large particles grow, and finally, the jewel flower-shaped basic zinc chloride with relatively thick particles is obtained. 2) The basic zinc chloride and the preparation method thereof provided by the invention do not use an induction synthesis agent, and the introduction of foreign impurities is reduced, so that the purity of the basic zinc chloride is improved. The basic zinc chloride prepared by the method has high purity, and the zinc content is up to 59%. 3) The basic zinc chloride prepared by the method has the characteristics of high purity, high crystallinity and less impurities; meanwhile, the prepared basic zinc chloride has stable jewel flower-shaped crystals, uniform crystal particles and the characteristic of insolubility in water, the content (mass fraction) of water-soluble chloride is lower than 0.1 percent, and the property is stable.
Drawings
FIG. 1 is an XRD pattern of the product produced in example 1 of the present invention and an XRD pattern of cards 77-2311.
FIG. 2 is a 500-fold micrograph of the product produced in example 1 of the present invention.
FIG. 3 is a DSC profile of the product produced in example 1 of the present invention.
FIG. 4 is a TGA/DrTGA profile of the product produced in example 1 of the present invention.
The following detailed description will further illustrate the invention in conjunction with the above-described figures.
Detailed Description
In order to further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be made on the specific embodiments, structures, characteristics and effects of the basic zinc chloride and the preparation method thereof provided by the present invention with reference to the accompanying drawings 1-4 and preferred embodiments. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The invention provides a preparation method of basic zinc chloride, which comprises the following steps:
the first step is as follows: preparing a basic zinc chloride precursor system.
Specifically, the method for preparing the basic zinc chloride precursor system comprises the following steps: providing a zinc-containing reaction system, and stirring the zinc-containing reaction system under certain reaction conditions to prepare a basic zinc chloride precursor system.
Wherein, in the step of preparing the basic zinc chloride precursor system, the reaction conditions are as follows: the pH value is 4.8-5.8, the reaction temperature is not more than 60 ℃, and the charging and reaction time is 5-30 minutes.
In one embodiment of the present invention, the zinc-containing reaction system is a first reaction system formed by reacting a zinc chloride solution with a zinc oxide slurry or a zinc hydroxide slurry or a sodium hydroxide solution.
When the basic zinc chloride precursor system is prepared by adopting the first reaction system, the concentration of zinc in the used zinc chloride solution is 90-140 g/L, and the concentration of zinc in the used zinc oxide slurry is 200-280 g/L.
When the basic zinc chloride precursor system is prepared by adopting the first reaction system, the concentration of zinc in the used zinc chloride solution is 90-140 g/L, and the mass fraction of the used sodium hydroxide solution is 30%.
When the basic zinc chloride precursor system is prepared by adopting the first reaction system, the concentration of zinc in the used zinc chloride solution is 90-140 g/L, and the concentration of zinc in the used zinc hydroxide slurry is 200-280 g/L.
In another embodiment of the present invention, the zinc-containing reaction system is a second reaction system consisting of a reaction of hydrochloric acid with a zinc oxide slurry or a zinc hydroxide slurry.
When the basic zinc chloride precursor system is prepared by adopting the second reaction system, the concentration of zinc in the used zinc oxide slurry is 200-280 g/L, and the mass fraction of the used hydrochloric acid solution is 15%.
When the basic zinc chloride precursor system is prepared by adopting the second reaction system, the concentration of zinc in the used zinc hydroxide slurry is 150-200 g/L, and the mass fraction of the used hydrochloric acid solution is 15%.
Wherein the zinc-containing reaction system is added simultaneously.
The second step is that: gem flower-shaped crystal basic zinc chloride is prepared through hydrothermal precipitation reaction.
Specifically, the method for preparing the jewel flower-shaped crystalline basic zinc chloride by the hydrothermal precipitation reaction comprises the following steps: and (2) placing the basic zinc chloride precursor system in a hydrothermal reaction environment and stirring at a constant speed to enable the basic zinc chloride precursor to generate a hydrothermal reaction, filtering the reactant of the hydrothermal reaction to obtain white crystals, and washing and drying the white crystals to obtain the jewel flower-shaped crystalline basic zinc chloride.
In the step of preparing the floriform crystalline basic zinc chloride by the hydrothermal precipitation reaction, the temperature of the hydrothermal reaction environment is 90-200 ℃, the pH value is 5.5-6, and the reaction time of the hydrothermal reaction is 1-8 hours.
Wherein, in the step of preparing the jewel flower-shaped crystal basic zinc chloride by the hydrothermal precipitation reaction, pure water is adopted for washing.
Wherein in the step of preparing the jewel flower-shaped crystalline basic zinc chloride by the hydrothermal precipitation reaction, the drying temperature in the drying process is 50-105 ℃.
The invention also provides the basic zinc chloride prepared by the preparation method of the basic zinc chloride, wherein the basic zinc chloride has a jewel flower-shaped crystal form, crystal particles of the jewel flower-shaped crystal are uniform, the whole crystal size is about 20-200 um, the length of petals is 1-100 um, the width of the petals is 1-100 um, and the thickness of the petals is 1-20 um.
The method for producing basic zinc chloride of the present invention and the performance thereof will be described in detail below with reference to specific examples.
Example 1
Adding 400L zinc chloride solution containing 120g/L zinc and 770L zinc oxide slurry containing 250g/L zinc into a 2-cubic stirring mixing reactor, uniformly stirring, controlling the pH to be 5.4, heating the materials in the reactor to 50 ℃, and controlling the feeding and reaction time to be 15 minutes to prepare the basic zinc chloride precursor system.
Heating the basic zinc chloride precursor system to 95 ℃, keeping the pH value in a hydrothermal reaction environment of 5.5-6 by adding hydrochloric acid or a sodium hydroxide solution, and stirring to perform a hydrothermal reaction for 2 hours.
After the reaction is finished, discharging the materials in the reactor into a vacuum suction filter for suction filtration, washing and drying the materials by using tap water, and drying the materials to constant weight at 105 ℃ to obtain about 410Kg of basic zinc chloride product.
The product obtained in example 1 above was subjected to XRD pattern, 500-fold magnified micrograph, DSC pattern and TGA/DrTGA pattern.
The product obtained in example 1 was white in appearance and good in flowability. Through analysis, the zinc content of the product is 59.1 percent, the water-soluble chloride content (mass fraction) is 0.08 percent, and heavy metal impurity elements such As As, Cd, Hg, Pb and the like are lower than the detection limit of ICP-OES and are not detected.
Example 2
Adding 1000L zinc chloride solution containing 130g/L zinc and 2170L zinc hydroxide slurry containing 240g/L zinc into an 8-cubic stirring mixing reactor, uniformly stirring, heating the materials in the reactor to 55 ℃, reacting at a pH value of 5.3, and controlling the adding and reacting time within 30 minutes to prepare the basic zinc chloride precursor system.
Heating the basic zinc chloride precursor system to 105 ℃, keeping the pH value in a hydrothermal reaction environment of 5.5-6 by the addition of hydrochloric acid or a sodium hydroxide solution, and stirring for hydrothermal reaction for 5 hours.
After the reaction is finished, discharging the materials in the reactor into a vacuum suction filter for suction filtration, washing and drying the materials by using tap water, and drying the materials to constant weight at 105 ℃ to obtain about 1100Kg of basic zinc chloride product.
The product obtained in example 2 above was subjected to XRD pattern, 500-fold magnified micrograph, DSC pattern and TGA/DrTGA pattern.
The product obtained in example 2 was white in appearance and good in flowability. Through analysis, the zinc content in the product is 58.4 percent, the water-soluble chloride content (mass fraction) is 0.1 percent, and heavy metal impurity elements such As As, Cd, Hg, Pb and the like are lower than the detection limit of ICP-OES and are not detected.
Example 3
Adding 600L of 15% hydrochloric acid solution and 1650L of zinc oxide slurry containing 260g/L of zinc into a 3-cubic stirring mixing reactor, uniformly stirring, heating the materials in the reactor to 55 ℃, controlling the reaction pH to 5.1, and controlling the charging and reaction time to be 10 minutes to prepare the basic zinc chloride precursor system.
Heating the basic zinc chloride precursor system to 105 ℃, keeping the pH value in a hydrothermal reaction environment of 5.5-6 by the addition of hydrochloric acid or a sodium hydroxide solution, and stirring for hydrothermal reaction for 1 hour.
After the reaction is finished, discharging the materials in the reactor into a vacuum filter for suction filtration, washing and drying the materials by tap water, and drying the materials to constant weight at 105 ℃ to obtain about 723Kg of basic zinc chloride product.
The product obtained in example 3 above was subjected to XRD pattern, 500-fold magnified micrograph, DSC pattern and TGA/DrTGA pattern.
The product obtained in example 3 was white in appearance and good in flowability. Through analysis, the zinc content in the product is 58.9 percent, the water-soluble chloride content (mass fraction) is 0.09 percent, and heavy metal impurity elements such As As, Cd, Hg, Pb and the like are lower than the detection limit of ICP-OES and are not detected.
Specifically, fig. 1 is an XRD spectrum of the product obtained in embodiment 1 of the present invention, the analyzer is an X-ray diffractometer (SHIMADZU XRD-6000, D/max 2500v/pc, Cu K α radiation), the scanning mode is Fix Time, the scanning range is 10-75 deg, scanning step0.02deg/min, Preset Time 1.00sec, voltage 40kV, and current 30 mA. From the figure, the XRD pattern of the product obtained in example 1 of the present invention can be seen together with that of card 77-2311 (Zn)5(OH)8Cl2·H2O, Zinc hydroxide Chloride Hydrate) has a good match, the product belongs to the hexagonal system R-3m (166), and the unit cell parameter is 6.34X 6.34 (90.0X 120.0).
FIG. 2 is a 500-fold micrograph of the product obtained in example 1 of the present invention. The analytical instrument is a metallographic microscope (analytical instrument: comes card DM2500M, germany). From the micrograph, the product crystal is white transparent precious stone flower form, and the crystal granule is even, and the whole size of crystal is about 20 ~ 200um, and petal length is at 1 ~ 100um, and the width is at 1 ~ 100um, and thickness is 1 ~ 20 um.
FIG. 3 is a DSC chart of the product obtained in example 1 of the present invention, and the analytical instrument is a differential scanning calorimeter (SHIMADZU DSC-60). An aluminum crucible is adopted, the sampling amount is 5-8 mg, the temperature is increased from room temperature to 600 ℃, the temperature increase rate is controlled at 15 ℃/min, the sample is protected by high-purity nitrogen in the heating process, and the nitrogen flow rate is controlled at 50 ml/min. From the figure, two endothermic peaks are seen, with peak temperatures of 203.59 ℃ and 236.77 ℃ respectively, indicating good thermal stability of the product.
FIG. 4 is a TGA/DrTGA profile of the product of example 1 of the present invention, the analytical instrument being a thermogravimetric analyzer (SHIMADZU TGA-50). An aluminum crucible is adopted, the sampling amount is 5-8 mg, the temperature is increased from room temperature to 600 ℃, the temperature increase rate is controlled at 15 ℃/min, the sample is protected by high-purity nitrogen in the heating process, and the nitrogen flow rate is controlled at 20 ml/min. From the figure, it can be seen that there are two accelerated weight loss processes, with DrTGA showing peak temperatures of 211.21 ℃ and 492.88 ℃ respectively, again indicating good thermal stability of the product.
The invention provides basic zinc chloride and a preparation method thereof, 1) firstly preparing a basic zinc chloride precursor system, then carrying out hydrothermal reaction to dissolve fine-particle basic zinc chloride in the precursor system to obtain a zinc source, and under the hydrothermal reaction condition, continuously carrying out precipitation reaction on the surface of large-particle basic zinc chloride according to the original crystal face. Under the 'poor-killing and rich-economy' environment, small particles disappear, large particles grow, and finally, the jewel flower-shaped basic zinc chloride with relatively thick particles is obtained. 2) The basic zinc chloride and the preparation method thereof provided by the invention do not use an induction synthesis agent, and the introduction of foreign impurities is reduced, so that the purity of the basic zinc chloride is improved. The basic zinc chloride prepared by the method has high purity, and the zinc content is up to 59%. 3) The basic zinc chloride prepared by the method has the characteristics of high purity, high crystallinity and less impurities; meanwhile, the prepared basic zinc chloride has stable jewel flower-shaped crystals, uniform crystal particles and the characteristic of insolubility in water, the content (mass fraction) of water-soluble chloride is lower than 0.1 percent, and the property is stable.
Although the present invention has been described with reference to the above preferred embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (14)
1. A preparation method of basic zinc chloride is characterized by comprising the following steps:
preparing a basic zinc chloride precursor system: providing a zinc-containing reaction system, setting reaction conditions and stirring the zinc-containing reaction system to prepare a basic zinc chloride precursor system; and
preparing jewel flower-shaped crystalline basic zinc chloride by hydrothermal precipitation reaction: and (2) placing the basic zinc chloride precursor system in a hydrothermal reaction environment and stirring at a constant speed to enable the basic zinc chloride precursor to generate a hydrothermal reaction, filtering the reactant of the hydrothermal reaction to obtain white crystals, and washing and drying the white crystals to obtain the jewel flower-shaped crystalline basic zinc chloride.
2. A method of making basic zinc chloride according to claim 1 wherein in the step of "making a basic zinc chloride precursor system", the reaction conditions are: the pH value is 4.8-5.8, the reaction temperature is not more than 60 ℃, and the charging and reaction time is 5-30 minutes.
3. The method for preparing basic zinc chloride according to claim 1, wherein in the step of preparing the floriform crystalline basic zinc chloride through the hydrothermal precipitation reaction, the temperature of the hydrothermal reaction environment is 90-200 ℃, the pH value is 5.5-6, and the reaction time of the hydrothermal reaction is 1-8 hours.
4. A process for the preparation of zinc chlorohydrate according to claim 1, wherein the zinc-containing reaction system is a first reaction system consisting of reacting a zinc chloride solution with a zinc oxide slurry or a zinc hydroxide slurry or a sodium hydroxide solution.
5. The method for preparing basic zinc chloride according to claim 4, wherein when the first reaction system is adopted to prepare the basic zinc chloride precursor system, the concentration of zinc in a zinc chloride solution is 90-140 g/L, and the concentration of zinc in a zinc oxide slurry is 200-280 g/L.
6. The method for preparing basic zinc chloride according to claim 4, wherein when the first reaction system is adopted to prepare the basic zinc chloride precursor system, the concentration of zinc in the used zinc chloride solution is 90-140 g/L, and the mass fraction of the used sodium hydroxide solution is 30%.
7. The method for preparing basic zinc chloride according to claim 4, wherein when the first reaction system is adopted to prepare the basic zinc chloride precursor system, the concentration of zinc in a zinc chloride solution is 90-140 g/L, and the concentration of zinc in a zinc hydroxide slurry is 200-280 g/L.
8. A process for the preparation of zinc chlorohydrate according to claim 1, wherein the zinc-containing reaction system is a second reaction system consisting of a reaction of hydrochloric acid with a zinc oxide slurry or a zinc hydroxide slurry.
9. The method for preparing basic zinc chloride according to claim 8, wherein when the second reaction system is adopted to prepare the basic zinc chloride precursor system, the concentration of zinc in the zinc oxide slurry is 200-280 g/L, and the mass fraction of the hydrochloric acid solution is 15%.
10. The method for preparing basic zinc chloride according to claim 8, wherein when the second reaction system is adopted to prepare the basic zinc chloride precursor system, the concentration of zinc in the zinc hydroxide slurry is 150-200 g/L, and the mass fraction of the hydrochloric acid solution is 15%.
11. A process for the preparation of zinc chlorohydrate according to claim 1 wherein the zinc-containing reaction system is fed simultaneously.
12. A method of producing basic zinc chloride according to claim 1, wherein in the step of producing jewel flower-like crystalline basic zinc chloride by hydrothermal precipitation reaction, washing is carried out with pure water.
13. The method for preparing basic zinc chloride according to claim 1, wherein in the step of preparing the floriform crystalline basic zinc chloride through the hydrothermal precipitation reaction, the drying temperature in the drying process is 50-105 ℃.
14. Basic zinc chloride prepared by the method for preparing basic zinc chloride according to any one of claims 1 to 13, wherein the basic zinc chloride has a jewel flower-like crystal morphology, crystal particles of the jewel flower-like crystal are uniform, the overall size of the crystal is about 20 to 200um, the length of petals is 1 to 100um, the width of the petals is 1 to 100um, and the thickness of the petals is 1 to 20 um.
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| CN114057218B (en) * | 2021-11-29 | 2024-03-26 | 天宝动物营养科技股份有限公司 | Preparation method of basic zinc chloride |
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