CN103539099B - A kind of preparation method of nickel pyrophosphate micrometer fibers - Google Patents
A kind of preparation method of nickel pyrophosphate micrometer fibers Download PDFInfo
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- CN103539099B CN103539099B CN201310523289.0A CN201310523289A CN103539099B CN 103539099 B CN103539099 B CN 103539099B CN 201310523289 A CN201310523289 A CN 201310523289A CN 103539099 B CN103539099 B CN 103539099B
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Abstract
The invention belongs to ceramic preparation field, particularly relate to a kind of preparation method of nickel pyrophosphate micrometer fibers, it is with solubility divalent nickel salt and soluble pyrophosphate uniform dissolution in alcohol/water mixed solution according to a certain percentage, abundant stirring reaction after mixed, continues and in alcohol/water mixed solution, to carry out hydro-thermal reaction, filtration, washs, is drying to obtain object product.Present invention process is simple and easy to do, purity is high, product preparation cost is low, and products obtained therefrom diameter is between 20 ~ 200nm, and length-to-diameter ratio is greater than 10, and homogeneity and good dispersity.Nickel pyrophosphate micrometer fibers prepared by the present invention can be widely used in the fields such as industry plating, chemical industry, electric, mechanical and building.
Description
Technical field
The invention belongs to the preparing technical field of ceramic, specifically relate to
oneplant the preparation method of nickel pyrophosphate micrometer fibers.
Background technology
Nickel pyrophosphate, molecular formula: Ni
2p
2o
7; Molecular weight: 291.330124 [g/mol]; English name: Nickeldiphosphate; CASNo14448-18-1.Nickel pyrophosphate is a kind of important inorganic salt product, through being commonly used for the complexing agent in electroplate liquid, and the rust remover in mechanical workout.Dispersion agent and emulsifying agent is made in Chemical Manufacture.Water-softening chemicals is made, boiler detergent, metal ion chelation agent in water treatment.In middle LOW TEMPERATURE ELECTROLESS NICKEL PLATING PROCESS, because it has excellent solidity to corrosion and wear resistance, also there is stable non magnetic, high resistivity, low-temperature coefficient and the performance such as heat-resisting simultaneously, and be widely used in the aspects such as hard disc of computer, magnetic shield apparatus, electronic industry, petrochemical pipe equipment, automobile component.In such as 03805744.1 patent of invention disclosed in China national Department of Intellectual Property, the people such as Peter Lonard Stewart utilize the solution of nickel pyrophosphate to complete non-cyanide and form a kind of method of copper coating of attachment on the zinc or zinc alloy article as this process components (see Peter Lonard Stewart etc., for the non-cyanide copper electro-plating method of zinc and zinc alloy, 03805744.1).At present, main production process both domestic and external is as follows: at ambient temperature, and with nickel hydroxide and phosphoric acid for raw material, Direct precipitation obtains intermediate product in aqueous.Then, after heating and calcining, nickel pyrophosphate is formed.The nickel pyrophosphate purity that above-mentioned method is produced is low, foreign matter content is high, microscopic appearance heterogeneity, can not meet the requirement of modern industry to nickel pyrophosphate microfiber material.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art part and provides a kind of production technique simple, and object product yield is high, and preparation cost is low, and product purity is high, good dispersity, technique easy-operating nickel pyrophosphate micrometer fibers preparation method.
For achieving the above object, the present invention realizes like this.
A preparation method for nickel pyrophosphate micrometer fibers, it is uniform dissolution in alcohol/water mixed solution by solubility divalent nickel salt and soluble pyrophosphate, stirs and after carrying out hydro-thermal reaction after mixing, overanxious, wash, namely obtain object product after drying.
As a kind of preferred version, solubility divalent nickel salt of the present invention is one or more the mixture in nickelous chloride, single nickel salt, nickelous nitrate or nickelous acetate.
As another kind of preferred version, soluble pyrophosphate of the present invention is one in trisodium phosphate or potassium pyrophosphate 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 ~ 100.
Further, the volumetric molar concentration of solubility divalent nickel salt of the present invention is 0.01 ~ 1mol/L.
In addition, the mol ratio of solubility divalent nickel salt of the present invention and soluble pyrophosphate is 1: 0.1 ~ 10.
Secondly, hydrothermal temperature of the present invention is at 180 ~ 280 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 10 ~ 20 hours, and drying temperature is 100 ~ 200 DEG C.
Compared with prior art, the present invention has following features.
(1) the traditional method complex process of nickel pyrophosphate micrometer fibers, can not reach the requirement of topography uniformity.Present invention process route is simple, and preparation cost is low, easy to control, has higher production efficiency, is achieved synthesize the morphology control of nickel pyrophosphate micrometer fibers by the composition of condition solvent.
(2) the object product nickel pyrophosphate micrometer fibers prepared of the present invention, its purity high (98% ~ 99%), foreign matter content is low, good dispersity (can be found out by SEM figure), there is fibrous pattern, the requirement of industrial application to nickel pyrophosphate micrometer fibers product can be met.
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 X-ray diffractogram of the nickel pyrophosphate micrometer fibers of Fig. 1 prepared by the present invention.
The IR figure of the nickel pyrophosphate micrometer fibers of Fig. 2 prepared by the present invention.
The SEM shape appearance figure of the nickel pyrophosphate micrometer fibers of Fig. 3 prepared by the present invention.
The SEM shape appearance figure of the nickel pyrophosphate micrometer fibers of Fig. 4 prepared by the present invention.
The SEM shape appearance figure of the nickel pyrophosphate micrometer fibers of Fig. 5 prepared by the present invention.
The SEM shape appearance figure of the nickel pyrophosphate micrometer fibers of Fig. 6 prepared by the present invention.
Embodiment
The present invention with solubility divalent nickel salt and soluble pyrophosphate for raw material, by nickel salt and soluble pyrophosphate uniform dissolution in alcohol/water mixed solution according to a certain percentage, abundant stirring reaction after mixed, continue and carry out hydro-thermal reaction (at 180 ~ 280 DEG C, the time is 6 ~ 48 hours to temperature) in alcohol/water mixed solution.Namely object product is obtained after filtration, washing, drying.Its preparation process is.
(1) solubility divalent nickel salt and pyrophosphate salt are all made into the alcohol water mixed solution of 0.01 ~ 1.0mol/L, at room temperature pyrophosphate salt is slowly added drop-wise in nickel salt solution, the add-on of soluble pyrophosphate pressed the molar ratio computing of nickel salt/pyrophosphate salt according to 1:0.1 ~ 10, with 60 ~ 120 revs/min of stirring velocity stirring reactions 30 ~ 60 minutes.
(2) by the mixed solution that obtains at a certain temperature, carry out hydro-thermal reaction, hydrothermal temperature is at 180 ~ 280 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 100 ~ 200 DEG C of conditions, and dry 10 ~ 20 hours, i.e. obtained nickel pyrophosphate microfiber material.
The infrared spectrum of the fibrous nickel pyrophosphate micrometer fibers of Fig. 1 prepared by the present invention.The X-ray diffractogram of the fibrous nickel pyrophosphate micrometer fibers of Fig. 2 prepared by the present invention.
Shown in Fig. 3 ~ 6, the scanning electron microscope (SEM) that the fibrous nickel pyrophosphate micrometer fibers prepared by the present invention carries out is analyzed, consequently, products obtained therefrom has the micro-crystal of fiber morphology, diameter is between 20 ~ 200nm, and length-to-diameter ratio is greater than 10, and homogeneity, good dispersity.
embodiment 1.
Be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.05mol/L trisodium phosphate to 0.05mol/L single nickel salt alcohol water mixed solution by concentration.Wherein alcohol water mixed solution is that second alcohol and water is prepared according to 1:20 volume ratio, single nickel salt and trisodium phosphate with the molar ratio computing of 1:1, with 60 revs/min of stirring velocity stirring reactions 30 minutes.The mixed solution obtained is carried out hydro-thermal reaction, and hydrothermal temperature is at 200 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 150 DEG C of conditions, drying 10 hours, obtains sheet tetra-sodium microfiber material.After measured, its diameter is between 30 ~ 100nm, and length-to-diameter ratio between 10 ~ 50, and is uniformly dispersed for product.
embodiment 2.
Be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.1mol/L trisodium phosphate to 0.1mol/L single nickel salt alcohol water mixed solution by concentration.Wherein alcohol water mixed solution is that second alcohol and water is prepared according to 1:20 volume ratio, single nickel salt and trisodium phosphate with the molar ratio computing of 1:2, with 60 revs/min of stirring velocity stirring reactions 30 minutes.The mixed solution obtained is carried out hydro-thermal reaction, and hydrothermal temperature is at 200 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 160 DEG C of conditions, drying 20 hours, obtains sheet tetra-sodium microfiber material.After measured, its diameter is between 30 ~ 80nm, and length-to-diameter ratio between 10 ~ 60, and is uniformly dispersed for product.
embodiment 3.
Be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.05mol/L trisodium phosphate to 0.05mol/L nickelous acetate alcohol water mixed solution by concentration.Wherein alcohol water mixed solution is that second alcohol and water is prepared according to 1:20 volume ratio, nickelous acetate and trisodium phosphate with the molar ratio computing of 1:1, with 60 revs/min of stirring velocity stirring reactions 30 minutes.The mixed solution obtained is carried out hydro-thermal reaction, and hydrothermal temperature is at 200 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 180 DEG C of conditions, drying 10 hours, obtains sheet tetra-sodium microfiber material.After measured, its diameter is between 20 ~ 80nm, and length-to-diameter ratio between 10 ~ 60, and is uniformly dispersed for product.
embodiment 4.
Be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.2mol/L trisodium phosphate to 0.2mol/L nickelous chloride alcohol water mixed solution by concentration.Wherein alcohol water mixed solution is that second alcohol and water is prepared according to 1:20 volume ratio, nickelous chloride and trisodium phosphate with the molar ratio computing of 1:1, with 60 revs/min of stirring velocity stirring reactions 30 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 200 DEG C of conditions, drying 10 hours, obtains sheet tetra-sodium microfiber material.After measured, its diameter is between 30 ~ 60nm, and length-to-diameter ratio between 15 ~ 60, and is uniformly dispersed for product.
embodiment 5.
Be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.1mol/L trisodium phosphate to 0.1mol/L nickelous nitrate alcohol water mixed solution by concentration.Wherein alcohol water mixed solution is that second alcohol and water is prepared according to 1:20 volume ratio, nickelous nitrate and trisodium phosphate with the molar ratio computing of 1:1, with 60 revs/min of stirring velocity stirring reactions 30 minutes.The mixed solution obtained is carried out hydro-thermal reaction, and hydrothermal temperature is at 190 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 180 DEG C of conditions, drying 10 hours, obtains sheet tetra-sodium microfiber material.After measured, its diameter is between 30 ~ 90nm, and length-to-diameter ratio between 20 ~ 60, and is uniformly dispersed for product.
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 (5)
1. a preparation method for nickel pyrophosphate micrometer fibers, is characterized in that: be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.05mol/L trisodium phosphate to 0.05mol/L single nickel salt alcohol water mixed solution by concentration; Wherein alcohol water mixed solution is that second alcohol and water is prepared according to 1:20 volume ratio, single nickel salt and trisodium phosphate with the molar ratio computing of 1:1, with 60 revs/min of stirring velocity stirring reactions 30 minutes; The mixed solution obtained is carried out hydro-thermal reaction, and hydrothermal temperature is at 200 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 150 DEG C of conditions, drying 10 hours, obtains sheet tetra-sodium microfiber material; Its diameter of product is between 30 ~ 100nm, and length-to-diameter ratio between 10 ~ 50, and is uniformly dispersed.
2. a preparation method for nickel pyrophosphate micrometer fibers, is characterized in that: be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.1mol/L trisodium phosphate to 0.1mol/L single nickel salt alcohol water mixed solution by concentration; Wherein alcohol water mixed solution is that second alcohol and water is prepared according to 1:20 volume ratio, single nickel salt and trisodium phosphate with the molar ratio computing of 1:2, with 60 revs/min of stirring velocity stirring reactions 30 minutes; The mixed solution obtained is carried out hydro-thermal reaction, and hydrothermal temperature is at 200 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 160 DEG C of conditions, drying 20 hours, obtains sheet tetra-sodium microfiber material; Product diameter is between 30 ~ 80nm, and length-to-diameter ratio between 10 ~ 60, and is uniformly dispersed.
3. a preparation method for nickel pyrophosphate micrometer fibers, is characterized in that: be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.05mol/L trisodium phosphate to 0.05mol/L nickelous acetate alcohol water mixed solution by concentration; Wherein alcohol water mixed solution is that second alcohol and water is prepared according to 1:20 volume ratio, nickelous acetate and trisodium phosphate with the molar ratio computing of 1:1, with 60 revs/min of stirring velocity stirring reactions 30 minutes; The mixed solution obtained is carried out hydro-thermal reaction, and hydrothermal temperature is at 200 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 180 DEG C of conditions, drying 10 hours, obtains sheet tetra-sodium microfiber material; After measured, its diameter is between 20 ~ 80nm, and length-to-diameter ratio between 10 ~ 60, and is uniformly dispersed for product.
4. a preparation method for nickel pyrophosphate micrometer fibers, is characterized in that: be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.2mol/L trisodium phosphate to 0.2mol/L nickelous chloride alcohol water mixed solution by concentration; Wherein alcohol water mixed solution is that second alcohol and water is prepared according to 1:20 volume ratio, nickelous chloride and trisodium phosphate with the molar ratio computing of 1:1, with 60 revs/min of stirring velocity stirring reactions 30 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 200 DEG C of conditions, drying 10 hours, obtains sheet tetra-sodium microfiber material; Product diameter is between 30 ~ 60nm, and length-to-diameter ratio between 15 ~ 60, and is uniformly dispersed.
5. a preparation method for nickel pyrophosphate micrometer fibers, is characterized in that: be that to be slowly added drop-wise to concentration be in the alcohol water mixed solution of 0.1mol/L trisodium phosphate to 0.1mol/L nickelous nitrate alcohol water mixed solution by concentration; Wherein alcohol water mixed solution is that second alcohol and water is prepared according to 1:20 volume ratio, nickelous nitrate and trisodium phosphate with the molar ratio computing of 1:1, with 60 revs/min of stirring velocity stirring reactions 30 minutes; The mixed solution obtained is carried out hydro-thermal reaction, and hydrothermal temperature is at 190 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 180 DEG C of conditions, drying 10 hours, obtains sheet tetra-sodium microfiber material; Product diameter is between 30 ~ 90nm, and length-to-diameter ratio between 20 ~ 60, and is uniformly dispersed.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1750877A (en) * | 2003-01-03 | 2006-03-22 | 科学与工业研究委员会 | Process for preparing vanadyl pyrophosphate catalyst |
| CN102910609A (en) * | 2012-11-12 | 2013-02-06 | 渤海大学 | Preparation method of microcrystal with dumbbell feature and zinc phosphate grade structure |
| CN102925974A (en) * | 2012-11-12 | 2013-02-13 | 渤海大学 | Preparation method for high length-diameter ratio lead orthophosphate crystal whisker |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1750877A (en) * | 2003-01-03 | 2006-03-22 | 科学与工业研究委员会 | Process for preparing vanadyl pyrophosphate catalyst |
| CN102910609A (en) * | 2012-11-12 | 2013-02-06 | 渤海大学 | Preparation method of microcrystal with dumbbell feature and zinc phosphate grade structure |
| CN102925974A (en) * | 2012-11-12 | 2013-02-13 | 渤海大学 | Preparation method for high length-diameter ratio lead orthophosphate crystal whisker |
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