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Preparation method for high length-diameter ratio lead orthophosphate crystal whisker

A high aspect ratio, lead phosphate technology, applied in the field of preparation of inorganic non-metallic materials, can solve the problems of low purity of lead phosphate, unsatisfactory requirements, and high impurity content, and achieves good dispersibility, easy operation and control, and low impurity content. Effect

Inactive Publication Date: 2013-02-13
BOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The lead phosphate produced by the above method has low purity and high impurity content, which cannot meet the requirements of modern industry for lead phosphate whisker materials.

Method used

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  • Preparation method for high length-diameter ratio lead orthophosphate crystal whisker
  • Preparation method for high length-diameter ratio lead orthophosphate crystal whisker
  • Preparation method for high length-diameter ratio lead orthophosphate crystal whisker

Examples

Experimental program
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Effect test

Embodiment 1

[0030] Slowly add the 0.3 mol / L lead acetate alcohol-water mixed solution dropwise into the 0.3 mol / L sodium pyrophosphate alcohol-water mixed solution. The alcohol-water mixed solution is prepared by ethanol and water in a volume ratio of 1:10, lead acetate and sodium pyrophosphate in a molar ratio of 2:1, and stirred and reacted at a stirring speed of 60 rpm for 10 minutes. The obtained mixed solution was subjected to hydrothermal reaction, the hydrothermal reaction temperature was 180° C., and the hydrothermal reaction time was 24 hours. After the hydrothermal reaction, cool down to room temperature naturally, filter and wash the product obtained by the reaction, put it in an oven, and dry it at 40 °C for 4 hours to obtain a high aspect ratio lead phosphate whisker material.

Embodiment 2

[0032] Slowly add an aqueous solution with a concentration of 0.2 mol / L lead acetate dropwise into an aqueous solution with a concentration of 0.1 mol / L sodium pyrophosphate. The molar ratio of lead acetate and sodium pyrophosphate is 2:1, and the reaction is stirred and reacted at a stirring speed of 60 rpm for 20 minutes. The obtained mixed solution was subjected to hydrothermal reaction, the hydrothermal reaction temperature was 180° C., and the hydrothermal reaction time was 24 hours. After the hydrothermal reaction, cool down to room temperature naturally, filter and wash the product obtained by the reaction, put it in an oven, and dry it at 40 °C for 4 hours to obtain a high aspect ratio lead phosphate whisker material.

Embodiment 3

[0034] Slowly add the 0.3 mol / L lead nitrate alcohol-water mixed solution dropwise into the 0.3 mol / L sodium pyrophosphate alcohol-water mixed solution. The alcohol-water mixed solution is prepared by ethanol and water according to the volume ratio of 1:10, and the lead nitrate and sodium pyrophosphate are prepared according to the molar ratio of 2:1, and the reaction is stirred and reacted at a stirring speed of 60 rpm for 10 minutes. The obtained mixed solution was subjected to hydrothermal reaction, the hydrothermal reaction temperature was 180° C., and the hydrothermal reaction time was 12 hours. After the hydrothermal reaction, cool down to room temperature naturally, filter and wash the product obtained by the reaction, put it in an oven, and dry it at 40 °C for 4 hours to obtain a high aspect ratio lead phosphate whisker material.

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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 [0001] The invention belongs to the technical field of preparation of inorganic non-metallic materials, and in particular relates to a preparation method of lead phosphate whiskers with high aspect ratio. Background technique [0002] 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 usually a hexagonal colorless crystal or white powder, insoluble in water and alcohol, soluble in nitric acid, and incombustible. It is an important inorganic salt product and is often used as an electrode material and plastic stabilizer in industry. At present, the main production methods at home and abroad are as follows: at room temperature, lead phosphate is synthesized in one step by direct precipitation in aqueous solution using lead nitrate and sodium phosphate as raw materials. Or by the reaction of disodium hydrogen phosphate and lead acetate. It can also be prepared by react...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/14C30B29/62C30B7/10
Inventor 张杰许家胜张贺王莉丽崔岩
Owner BOHAI UNIV
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