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Surface-modified ammonium phosphotungstate/ammonium phosphomolybdate ultrafine particle and preparation method thereof

A technology of surface modification and ultrafine particles, which is applied in dyeing polymer organic compound treatment, fibrous fillers, etc., can solve the problems of poor dispersion, unsatisfactory application effect, and large size of ultrafine particles, and achieve low production cost and high yield High and easy-to-obtain raw materials

Active Publication Date: 2013-05-01
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, ordinary ammonium phosphotungstic (molybdenum) acid has a large superparticle size, poor dispersion in polymers, lubricating oils and metal cutting fluids, and the application effect is not ideal.

Method used

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  • Surface-modified ammonium phosphotungstate/ammonium phosphomolybdate ultrafine particle and preparation method thereof
  • Surface-modified ammonium phosphotungstate/ammonium phosphomolybdate ultrafine particle and preparation method thereof
  • Surface-modified ammonium phosphotungstate/ammonium phosphomolybdate ultrafine particle and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Weigh 14.4g (0.005mol) phosphotungstic acid, 0.8g ammonium chloride, 1.44g polyvinylpyrrolidone (PVP, K16-18, weight average molecular weight 8000) into a 2L reactor, add 50ml distilled water and 950ml ethanol, stir React for 0.5h, and the reaction temperature is controlled at 20°C. After the reaction is completed, filter and dry, and the product obtained is ammonium phosphotungstate superfine particles whose surface is modified with polyvinylpyrrolidone.

[0025] figure 1 It is a scanning electron micrograph of the product obtained, and it can be seen from the figure that its particle size is 200-300nm. Figure 7 Curve a in the middle is the XRD pattern of the product obtained in Example 1, and the product obtained in Example 1 is confirmed to be the target product after analysis.

[0026] Weighed 0.1g, 0.5g, 1g, 5g of the product obtained in this example in turn, and added them to 1000g of water respectively, all of which were well dispersed and remained...

Embodiment 2

[0027] Example 2: Weigh 57.6g (0.02mol) of phosphotungstic acid, 0.54g of ammonium chloride, and 0.035g of polyethylene glycol (PEG, number average molecular weight 6000) into a 2L reactor, add 950ml of distilled water and 50ml of ethanol, and stir for 8 hours. The reaction temperature of the system is controlled at 80°C. After the reaction is completed, it is filtered and dried, and the product obtained is ultrafine ammonium phosphotungstate particles whose surface is modified with polyethylene glycol.

[0028] figure 2 It is a scanning electron micrograph of the resulting product, and it can be seen from the figure that its particle size is 500-800nm. Figure 7 Middle b curve is the XRD pattern of the product obtained in Example 2, and the product obtained in Example 2 is confirmed to be the target product after analysis.

[0029] Weighed 0.1g, 0.5g, 1g, 5g of the product obtained in this example in turn, and added them to 1000g of water respectively, all of which were w...

Embodiment 3

[0030] Example 3: Weigh 86.4g (0.03mol) of phosphotungstic acid, 2.7g of urea, and 6.9g of polyethylene glycol (PEG, number average molecular weight 2000) into a 2L reactor, add 1000ml of distilled water, control the system temperature to 100°C, and stir the reaction After 12 hours, filter and dry after the reaction, the product obtained is the superfine ammonium phosphotungstate particles whose surface is modified with polyethylene glycol.

[0031] image 3 It is a scanning electron micrograph of the product obtained, and it can be seen from the figure that its particle size is 200-500nm. Figure 7 The middle c curve is the XRD pattern of the product obtained in Example 3, and the product obtained in Example 3 is confirmed to be the target product after analysis.

[0032] Weighed 0.1g, 0.5g, 1g, 5g of the product obtained in this example in turn, and added them to 1000g of water respectively, all of which were well dispersed and remained unchanged for 3 months.

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Abstract

The invention discloses a surface-modified ammonium phosphotungstate / ammonium phosphomolybdate ultrafine particle and a preparation method thereof, and belongs to the technical field of ultrafine particles. The surface-modified ammonium phosphotungstate / ammonium phosphomolybdate ultrafine particle means that the surface of the ammonium phosphotungstate / ammonium phosphomolybdate ultrafine particle is coated with a polyvinylpyrrolidone modification substance or a polyethylene glycol modification substance, the particle size is 200-1000nm, and the weight of the modification substance accounts for 0.05-10% of the total weight of the ultrafine particle. The preparation method comprises the following steps of adding phosphotungstic acid / phosphomolybdic acid, ammonium salt or urea, polyvinylpyrrolidone or polyethylene glycol into a reaction medium, stirring for reaction for 0.5-12h at 20-100 DEG C, filtering after the reaction, drying, and obtaining the ultrafine particle. The method has the characteristics that the steps are simple, raw materials are cheap and easy to obtain, and the reaction conditions are mild. The method is high in yield, and low in production cost, and is suitable for large-scale industrial production. As surface modification is conducted on ammonium phosphotungstate or ammonium phosphomolybdate with polyvinylpyrrolidone or polyethylene glycol, the dispersion stability of the particle in water can be greatly improved.

Description

technical field [0001] The invention belongs to the technical field of ultrafine particles, and in particular relates to an ammonium phosphotungstate or ammonium phosphomolybdate ultrafine particle whose surface is in-situ modified by an organic compound, and also relates to a preparation method of the product. Background technique [0002] The molecular structure of ammonium phosphotungstate and ammonium phosphomolybdate not only contains phosphorus and nitrogen elements with good flame retardancy, but also contains tungsten or molybdenum elements with high smoke suppression effect, so they have good flame retardancy and smoke suppression functions, and can be As a flame retardant and smoke suppressant additive for polymer materials. At the same time, nitrogen, phosphorus, and tungsten (molybdenum) elements in ammonium phosphotungstate (ammonium phosphomolybdate) have excellent friction activity and can react with many friction pairs, so they can be used as lubricating oil ...

Claims

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Application Information

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IPC IPC(8): C09C1/00C09C3/10
Inventor 张治军李志伟贺洁马会超李小红
Owner HENAN UNIVERSITY
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