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A kind of preparation method of aluminum dihydrogen phosphate crystal powder

A technology of aluminum dihydrogen phosphate and crystals, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc. Drying and other issues, to achieve high economic and social value, suitable for long-distance transportation, high output effect

Inactive Publication Date: 2017-10-10
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the use of excessive phosphate in this method, there will be residual phosphoric acid and (or) phosphate in the final product, which will affect the performance and application of aluminum dihydrogen phosphate
In addition, Zhang Zhenxing et al. (Production and Application of Material Grade Aluminum Dihydrogen Phosphate, Chemical Times, Issue 9, 2011, pp. 20-22) prepared aluminum dihydrogen phosphate powdery solid by hot air centrifugal spray drying method, but this method The material is required to be dried instantly and quickly at a temperature of 480-520 °C, and the requirements for equipment and process conditions are relatively strict
[0003] In order to overcome the problems that aluminum dihydrogen phosphate is difficult to dry, impurities are easy to remain in the vacuum drying process, and hot air centrifugal spray drying is demanding on the process, the present invention provides an efficient, simple, safe, reliable, easy-to-operate, A method for preparing aluminum dihydrogen phosphate powder with low cost, high purity, and excellent water solubility. High-purity aluminum dihydrogen phosphate powder

Method used

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  • A kind of preparation method of aluminum dihydrogen phosphate crystal powder

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Effect test

Embodiment 1

[0013] The phosphoric acid solution with a concentration of 80 wt%, ammonia water and distilled water with a concentration of 30 wt% are formulated into a solution in a volume ratio of 10:3:5; then aluminum nitrate and urea are added to the solution, wherein aluminum nitrate, urea The addition amount is respectively 1 / 3 and 1 times of the molar number of phosphoric acid; Add iodine (I 2 ) powder, cetyl ethyl morpholine ethyl ammonium sulfate, and control the addition of iodine powder, cetyl ethyl morpholine ethyl ammonium sulfate to be 0.015%, 0.1% of the solution quality respectively; the solution is heated to 98°C, and continuously stirred with a stirrer for 5 hours; after the stirring, the solution was naturally cooled to room temperature, then stood still and aged for 3 hours, then filtered and separated, and the filtered product was washed with absolute ethanol for 3 times, and then in 60 °C for 4 hours. Find by XRD, infrared analysis: the crystalline phase of the powder...

Embodiment 2

[0015] Phosphoric acid solution with a concentration of 80 wt%, ammonia water and distilled water with a concentration of 30 wt% are formulated into a solution in a ratio of 10:3:5 by volume; then aluminum nitrate and urea are added to the solution, wherein aluminum nitrate, urea The addition amount is respectively 1 / 3 and 3 times of the molar number of phosphoric acid; Add iodine (I 2 ) powder, cetyl ethyl morpholine ethyl ammonium sulfate, and control the addition of iodine powder, cetyl ethyl morpholine ethyl ammonium sulfate to be 0.015%, 0.1% of the solution quality respectively; the solution is heated to 92°C, and continuously stirred with a stirrer for 7 hours; after the stirring, the solution was naturally cooled to room temperature, then stood still and aged for 3 hours, then filtered and separated, and the filtered product was washed with absolute ethanol for 3 times, and then at 70 °C for 4 hours. Find by XRD, infrared analysis: the crystalline phase of the powder ...

Embodiment 3

[0017] The phosphoric acid solution with a concentration of 80 wt%, ammonia water and distilled water with a concentration of 30 wt% are formulated into a solution in a volume ratio of 10:3:5; then aluminum nitrate and urea are added to the solution, wherein aluminum nitrate, urea The addition amount is respectively 1 / 3 and 4 times of the molar number of phosphoric acid; Add iodine (I 2 ) powder, cetyl ethyl morpholine ethyl ammonium sulfate, and control the addition of iodine powder, cetyl ethyl morpholine ethyl ammonium sulfate to be 0.015%, 0.1% of the solution quality respectively; the solution is heated to 85°C, and continuously stirred with a stirrer for 8 hours; after the stirring, the solution was naturally cooled to room temperature, then stood still and aged for 3 hours, then filtered and separated, and the filtered product was washed with absolute ethanol for 3 times, and then in 80 °C for 2 hours. Find by XRD, infrared analysis: the powder prepared by the technolo...

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Abstract

A high-efficiency preparation method of aluminum dihydrogen phosphate (Al(H2PO4)3) crystalline powder is characterized in that the following steps are adopted: (1) preparing a solution with phosphoric acid solution, ammonia water and distilled water; then adding aluminum nitrate and urea to the solution; (2) Add iodine (I2) powder and hexadecyl ethyl morpholine ammonium ethosulfate to the solution; (3) Heat the solution to 85~98 °C and keep stirring, then cool the solution naturally After reaching room temperature, let it stand still and age for 3 hours, then filter and separate, wash the product with absolute ethanol, and then dry it for 2 to 4 hours to prepare aluminum dihydrogen phosphate crystalline powder with excellent water solubility. The output rate of the aluminum dihydrogen phosphate prepared by the technology of the invention reaches up to 93.6 wt%, and has extremely high economic and social value.

Description

technical field [0001] What the invention provides is a kind of efficient aluminum dihydrogen phosphate (Al(H 2 PO 4 ) 3 ) The method for preparing crystalline powder belongs to the technical field of inorganic material preparation. Background technique [0002] Aluminum dihydrogen phosphate (Al(H 2 PO 4 ) 3 ) is widely used in industrial production, has the advantages of high temperature resistance, anti-stripping, anti-vibration, etc., and has excellent ultraviolet absorption, insulation performance, infrared absorption performance, electrical insulation performance, flame retardant performance, etc., can be used as refractory materials Binder for ceramic materials, reinforcing agent for ceramic materials, intumescent flame-retardant coatings for fibers, wood, paper, etc., heat-resistant insulation products, etc. Aluminum dihydrogen phosphate usually exists in liquid or powder form. However, liquid aluminum dihydrogen phosphate cannot be used alone, and is expensive...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/36
CPCC01B25/36C01P2006/80C01P2006/90
Inventor 白佳海刘洋盖超群李晓月高杰
Owner SHANDONG UNIV OF TECH
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