CN102925974B - Preparation method for high length-diameter ratio lead orthophosphate crystal whisker - Google Patents
Preparation method for high length-diameter ratio lead orthophosphate crystal whisker Download PDFInfo
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- CN102925974B CN102925974B CN201210448320.4A CN201210448320A CN102925974B CN 102925974 B CN102925974 B CN 102925974B CN 201210448320 A CN201210448320 A CN 201210448320A CN 102925974 B CN102925974 B CN 102925974B
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Abstract
The invention belongs to the field of inorganic nonmetal material preparation, and particularly relates to a preparation method for high length-diameter ratio lead orthophosphate crystal whisker. The preparation method comprises steps as follows: uniformly dissolving soluble bivalent lead salt and soluble pyrophosphoric salt in an alcohol/ water mixed solution based on a certain ratio; fully agitating for a reaction; then continuously carrying out a hydrothermal reaction in the alcohol/water mixed solution; filtering; washing; and drying, so as to obtain a target product. The preparation method is simple and convenient in technology, easy to implement, high in purity of products, and low in preparing cost; the prepared product is the crystal whisker with a length-diameter ratio more than 10, and the crystal whisker is 1 to 4 micrometers in diameter, and 30 to 60 micrometers in length; and the crystal whisker is high in uniformity and high in dispersity. The high length-diameter ratio lead orthophosphate crystal whisker prepared by the preparation method provided by the invention can be used as chemical modifying electrode material and a plastic sterilizer, and can be widely applied to fields, such as an automobile field, electronic and electrical fields, a mechanical field, a chemical field and a building field.
Description
Technical field
The invention belongs to the preparing technical field of ceramic, specifically relate to a kind of preparation method of high length-diameter ratio lead orthophosphate crystal whisker.
Background technology
Lead phosphate, molecular formula: Pb3 (PO4) 2; Molecular weight: 811.5 [g/mol]; English name: lead phosphate; CAS No 7446-27-7.Lead phosphate is often hexagon colourless crystallization or white powder, and water insoluble and alcohol, is dissolved in nitric acid, can not burn, and is a kind of important inorganic salt product, is industrially commonly used for electrode materials and stabilizer for plastics.At present, main production process both domestic and external is as follows: at ambient temperature, with lead nitrate and sodium phosphate for raw material, and direct precipitation method one-step synthesis lead phosphate in aqueous.Or reacted by Sodium phosphate dibasic and lead acetate and obtained.Also plumbous to carry out reaction with ammoniacal liquor obtained for phosphoric acid hydrogen.The lead phosphate purity that above-mentioned method is produced is low, foreign matter content is high, can not meet the requirement of modern industry to lead phosphate crystal whisker materials.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art part and provides a kind of technique simple, and object product yield is high, and preparation cost is low, and product purity is high, the preparation method of the easy-operating high length-diameter ratio lead orthophosphate crystal whisker of technique.
For achieving the above object, the present invention realizes like this.
A preparation method for high length-diameter ratio lead orthophosphate crystal whisker, it is uniform dissolution in alcohol/water mixed solution by solubility divalent lead salt and soluble pyrophosphate, stirs and carries out hydro-thermal reaction, obtaining object product.
As a kind of preferred version, solubility divalent lead salt of the present invention is one in lead nitrate or lead acetate or its mixture.
As another kind of preferred version, soluble pyrophosphate of the present invention is one in potassium pyrophosphate or trisodium phosphate or its mixture.
Further, the alcohol in alcohol/water mixed solution of the present invention is one or more the mixture in methyl alcohol, ethanol, ethylene glycol, n-propyl alcohol, Virahol, and the volume ratio of alcohol/water is 1: 0.1 ~ 50.
Further, the volumetric molar concentration of solubility divalent lead salt of the present invention and soluble pyrophosphate is 0.01 ~ 1.0 mol/L.
In addition, the mol ratio of solubility divalent lead salt of the present invention and soluble pyrophosphate is 1: 0.1 ~ 10.
Secondly, hydrothermal temperature of the present invention is at 150 ~ 220 DEG C, and the reaction times is 6 ~ 48 hours.
Finally, the present invention is uniform dissolution in alcohol/water mixed solution, after stirring reaction, continues and carry out hydro-thermal reaction in alcohol/water mixed solution, after filtration, washs, is drying to obtain object product; Described time of drying is 2 ~ 5 hours, and drying temperature is 30 ~ 50 DEG C.
Compared with prior art, the present invention has following features.
(1) the traditional method foreign matter content of lead phosphate is high, can not reach industrial application requirement.Present invention process route is simple, and preparation cost is low, easy to control, has higher production efficiency, the Hydrothermal Synthesis to high length-diameter ratio lead orthophosphate crystal whisker by the control realization of condition.
(2) the object product high length-diameter ratio lead orthophosphate crystal whisker prepared of the present invention, its purity high (95% ~ 99%), foreign matter content is low, and good dispersity (can be found out by SEM figure), can meet the requirement of industrial application to lead phosphate crystal whisker products.
Accompanying drawing explanation
Below in conjunction with the drawings and specific embodiments, the invention will be further described.Protection scope of the present invention is not only confined to the statement of following content.
The infrared spectrum of the high length-diameter ratio lead orthophosphate crystal whisker of Fig. 1 prepared by the present invention.
The X-ray diffractogram of the high length-diameter ratio lead orthophosphate crystal whisker of Fig. 2 prepared by the present invention.
The SEM shape appearance figure of the high length-diameter ratio lead orthophosphate crystal whisker of Fig. 3 prepared by the present invention.
The SEM shape appearance figure of the high length-diameter ratio lead orthophosphate crystal whisker of Fig. 4 prepared by the present invention.
The SEM shape appearance figure of the high length-diameter ratio lead orthophosphate crystal whisker of Fig. 5 prepared by the present invention.
Embodiment
The present invention with solubility divalent lead salt and soluble pyrophosphate for raw material, by solubility divalent lead salt and soluble pyrophosphate uniform dissolution in alcohol/water mixed solution according to a certain percentage, abundant stirring reaction, continue and in alcohol/water mixed solution, carry out hydro-thermal reaction (temperature is at 150 ~ 220 DEG C, time is 6 ~ 48 hours), namely obtain object product after filtration, washing, drying.Its preparation process is.
(1) solubility divalent lead salt and pyrophosphate salt are all made into the alcohol/water mixed solution of 0.01 ~ 1.0 mol/L, at room temperature soluble pyrophosphate is slowly added drop-wise in solubility divalent lead salt solution, the add-on of soluble pyrophosphate by the molar ratio computing of solubility divalent lead salt/pyrophosphate salt 1:0.1 ~ 10, with 50 ~ 100 revs/min of stirring velocity stirring reactions 5 ~ 30 minutes.
(2) by the mixed solution that obtains at a certain temperature, carry out hydro-thermal reaction, hydrothermal temperature is at 150 ~ 220 DEG C, and the hydro-thermal reaction time is 6 ~ 48 hours.
(3) hydro-thermal reaction terminates, and after naturally cooling to room temperature, puts into baking oven after being filtered by the product be obtained by reacting, under 30 ~ 50 DEG C of conditions, and dry 2 ~ 5 hours, i.e. obtained high length-diameter ratio lead orthophosphate crystal crystal whisker materials.
The infrared spectrum of the high length-diameter ratio lead orthophosphate crystal whisker of Fig. 1 prepared by the present invention.
The X-ray diffractogram of the high length-diameter ratio lead orthophosphate crystal whisker of Fig. 2 prepared by the present invention.
Shown in Fig. 3 ~ 5, the scanning electron microscope (SEM) that high length-diameter ratio lead orthophosphate crystal whisker prepared by the present invention carries out is analyzed, and consequently, products obtained therefrom high length-diameter ratio lead orthophosphate crystal whisker length-to-diameter ratio is greater than 10, products obtained therefrom diameter is between 1 ~ 4 μm, and length is at 30 ~ 60 μm.
Embodiment 1.
Be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.3 mol/L trisodium phosphate to 0.3 mol/L lead acetate alcohol water mixed solution by concentration.Wherein alcohol water mixed solution is that second alcohol and water is prepared according to 1:10 volume ratio, lead acetate and trisodium phosphate with the molar ratio computing of 2:1, with 60 revs/min of stirring velocity stirring reactions 10 minutes.The mixed solution obtained is carried out hydro-thermal reaction, and hydrothermal temperature is at 180 DEG C, and the hydro-thermal reaction time is 24 hours.After hydro-thermal reaction terminates, naturally cool to room temperature, put into baking oven after the product be obtained by reacting is filtered washing, under 40 DEG C of conditions, drying 4 hours, obtains high length-diameter ratio lead orthophosphate crystal crystal whisker materials.
Embodiment 2.
Be that to be slowly added drop-wise to concentration be in the aqueous solution of 0.1 mol/L trisodium phosphate for the aqueous solution of 0.2 mol/L lead acetate by concentration.Lead acetate and trisodium phosphate with the molar ratio computing of 2:1, with 60 revs/min of stirring velocity stirring reactions 20 minutes.The mixed solution obtained is carried out hydro-thermal reaction, and hydrothermal temperature is at 180 DEG C, and the hydro-thermal reaction time is 24 hours.After hydro-thermal reaction terminates, naturally cool to room temperature, put into baking oven after the product be obtained by reacting is filtered washing, under 40 DEG C of conditions, drying 4 hours, obtains high length-diameter ratio lead orthophosphate crystal crystal whisker materials.
Embodiment 3.
Be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.3 mol/L trisodium phosphate to 0.3 mol/L lead nitrate alcohol water mixed solution by concentration.Wherein alcohol water mixed solution is that second alcohol and water is prepared according to 1:10 volume ratio, lead nitrate and trisodium phosphate with the molar ratio computing of 2:1, with 60 revs/min of stirring velocity stirring reactions 10 minutes.The mixed solution obtained is carried out hydro-thermal reaction, and hydrothermal temperature is at 180 DEG C, and the hydro-thermal reaction time is 12 hours.After hydro-thermal reaction terminates, naturally cool to room temperature, put into baking oven after the product be obtained by reacting is filtered washing, under 40 DEG C of conditions, drying 4 hours, obtains high length-diameter ratio lead orthophosphate crystal crystal whisker materials.
Embodiment 4.
Be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.3 mol/L potassium pyrophosphate to 0.2 mol/L lead nitrate alcohol water mixed solution by concentration.Wherein alcohol water mixed solution is that second alcohol and water is prepared according to 1:10 volume ratio, lead nitrate and potassium pyrophosphate with the molar ratio computing of 3:2, with 60 revs/min of stirring velocity stirring reactions 10 minutes.The mixed solution obtained is carried out hydro-thermal reaction, and hydrothermal temperature is at 180 DEG C, and the hydro-thermal reaction time is 24 hours.After hydro-thermal reaction terminates, naturally cool to room temperature, put into baking oven after the product be obtained by reacting is filtered washing, under 40 DEG C of conditions, drying 4 hours, obtains high length-diameter ratio lead orthophosphate crystal crystal whisker materials.
Embodiment 5.
Be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.3 mol/L trisodium phosphate to 0.3 mol/L lead acetate alcohol water mixed solution by concentration.Wherein alcohol water mixed solution is that first alcohol and water is prepared according to 1:5 volume ratio, lead acetate and trisodium phosphate with the molar ratio computing of 1:1, with 60 revs/min of stirring velocity stirring reactions 20 minutes.The mixed solution obtained is carried out hydro-thermal reaction, and hydrothermal temperature is at 180 DEG C, and the hydro-thermal reaction time is 24 hours.After hydro-thermal reaction terminates, naturally cool to room temperature, put into baking oven after the product be obtained by reacting is filtered washing, under 40 DEG C of conditions, drying 4 hours, obtains high length-diameter ratio lead orthophosphate crystal crystal whisker materials.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. the preparation method of a high length-diameter ratio lead orthophosphate crystal whisker, it is characterized in that: the uniform dissolution in alcohol/water mixed solution by solubility divalent lead salt and soluble pyrophosphate, after stirring reaction, continue and carry out hydro-thermal reaction in alcohol/water mixed solution, obtain object product; Described solubility divalent lead salt is one in lead nitrate or lead acetate or its mixture; Described soluble pyrophosphate is one in potassium pyrophosphate or trisodium phosphate or its mixture; Alcohol in described alcohol/water mixed solution is one or more the mixture in methyl alcohol, ethanol, ethylene glycol, n-propyl alcohol, Virahol, and the volume ratio of alcohol and water is 1: 0.1 ~ 50; The volumetric molar concentration of described solubility divalent lead salt and soluble pyrophosphate is 0.01 ~ 1.0 mol/L; Described hydrothermal temperature is at 150 ~ 220 DEG C, and the reaction times is 6 ~ 48 hours; Uniform dissolution in alcohol/water mixed solution, after stirring reaction, continues and carry out hydro-thermal reaction in alcohol/water mixed solution, after filtration, washs, is drying to obtain object product; Described time of drying is 2 ~ 5 hours, and drying temperature is 30 ~ 50 DEG C.
2. the preparation method of a kind of high length-diameter ratio lead orthophosphate crystal whisker according to claim 1, is characterized in that: the mol ratio of described solubility divalent lead salt and soluble pyrophosphate is 1: 0.1 ~ 10.
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| CN103539098B (en) * | 2013-10-30 | 2015-09-23 | 渤海大学 | A kind of preparation method of sheet-like morphology manganese pyrophosphate crystallite |
| CN103539099B (en) * | 2013-10-30 | 2016-04-06 | 渤海大学 | A kind of preparation method of nickel pyrophosphate micrometer fibers |
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Non-Patent Citations (1)
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| Hydrothermal synthesis of potassium copper phosphate hydrate and ludjibaite microcrystals;Jiasheng Xu等;《Journal of Alloys and Compounds》;20100115;第494卷;319-322 * |
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