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A kind of preparation method of praseodymium yellow pigment

A pigment, the technology of praseodymium yellow, which is applied in the field of preparation of praseodymium yellow pigment, can solve the problems of easy harm to human body and natural environment safety, large pigment particles, and difficulty in using yellow pigment, and achieve fine particle size, short production process, shorten the effect of time

Active Publication Date: 2016-07-20
昆明先导新材料科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Chinese patent CN102627478A discloses a solid material prepared by mixing zirconium oxychloride, cadmium sulfate, sodium sulfide, caustic soda, and zinc chloride in the liquid phase. After mixing white carbon black and multiple groups of mineralizers containing fluorine, it is calcined, A method for preparing a yellow pigment after acidification, ball milling, acid bleaching, and alkali boiling processes, but the heavy metal cadmium is used in the production process of the pigment, which is used in the production of pigments, the long-term use of subsequent products, and the scrapping process The cadmium contained in the pigment is extremely harmful to the safety of the human body and the natural environment
This method requires multiple crushing and grinding, and the prepared pigment particles are relatively large, making it difficult for the yellow pigment to be used in the fields of coatings, plastics, inks, glazes, etc.

Method used

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  • A kind of preparation method of praseodymium yellow pigment
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  • A kind of preparation method of praseodymium yellow pigment

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preparation example Construction

[0029] The invention provides a kind of preparation method of praseodymium yellow pigment, comprises the following steps:

[0030] In the mixed solution of C1-C4 alcohol solvent, water and surfactant, soluble zirconium source, soluble praseodymium source and soluble silicon source react under the condition of pH value of 6-11 to obtain precipitate;

[0031] mixing the precipitate with a mineralizer and water and then spray-drying to obtain granules;

[0032] After the particles are calcined, they are sequentially pulverized and ground to obtain ultrafine particles;

[0033] The ultrafine particles are post-treated to obtain praseodymium yellow pigment.

[0034] In the present invention, the soluble zirconium source, soluble praseodymium source and soluble silicon source are used in liquid phase conditions to generate precipitates with uniform microscopic components, fine particle size and high surface activity, which can effectively reduce subsequent mineralization The amoun...

Embodiment 1

[0053] A 10L aqueous solution dissolved with 110g of praseodymium nitrate hexahydrate, 2000g of zirconium nitrate trihydrate and a 10L aqueous solution dissolved with 615g of sodium silicate were simultaneously dropped into a reaction kettle with a 13L mixed solution, the mixed solution including water, ethanol, TritonX -100 and cyclohexane, the volume fraction of ethanol is 30%, the concentration of TritonX-100 is 5mL / L, and the concentration of cyclohexane is 13mL / L; Add a solution containing 0.5wt% sodium oxalate and 50wt% sodium hydroxide to maintain the pH of the reaction solution at 8.5, stir while adding dropwise, stop the dropwise addition after 2 hours, and continue the constant temperature reaction for 2 hours under stirring;

[0054] After the reaction is completed, filter and dehydrate the reaction product, take out the filter cake and add pure water of 1 times the mass of the filter cake, 5wt% sodium chloride, 0.1wt% potassium chloride, 1.5wt% ammonium chloride 1, ...

Embodiment 2

[0058] A 10L aqueous solution in which 110g of praseodymium nitrate hexahydrate and 2000g of zirconium nitrate trihydrate were dissolved and a 10L aqueous solution in which 735g of sodium silicate was dissolved were simultaneously dropped into a reaction kettle with a 13L mixed solution, the mixed solution comprising water , ethanol, n-octanol and polyethylene glycol, the volume fraction of ethanol is 45%, the concentration of n-octanol is 5mL / L, and the concentration of polyethylene glycol is 8g / L; the material obtained is reacted at 45°C During the reaction, add dropwise a solution containing 2wt% sodium oxalate and 30wt% sodium hydroxide to keep the pH of the reaction solution at 9.5, stir while adding dropwise, stop the dropwise addition after 2.5h, and continue the constant temperature reaction for 1h under stirring ;

[0059] After the reaction is completed, the reaction product is filtered and dehydrated, the filter cake is taken out and pure water of 1 times the mass o...

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Abstract

The invention provides a preparation method of a praseodymium yellow pigment. The preparation method comprises the following steps: reacting a soluble zirconium source, a soluble praseodymium source and a soluble silicon source in a mixed solution of a C1-C4 alcohol type solvent, water and a surfactant under the condition that the pH value is 6-11 to obtain a precipitate; mixing the precipitate with a mineralizer and water, and then spray-drying to obtain particles; calcining the particles, and then sequentially crushing and grinding to obtain ultrafine particles; and performing post-treatment on the ultrafine particles to obtain the praseodymium yellow pigment. According to the preparation method provided by the invention, the precipitate with homogeneous microcomponents, relatively small particle size and relatively high surface activity is generated from the soluble zirconium source, the soluble praseodymium source and the soluble silicon source under a liquid-phase condition by adopting a liquid-phase precipitation method, so that the using amount of the subsequent mineralizer can be effectively reduced, the solid-phase reaction time can be shortened, the energy consumption in the calcination process can be reduced, and the difficulty in subsequent crushing can be also reduced.

Description

technical field [0001] The invention belongs to the technical field of pigment preparation, in particular to a preparation method of praseodymium yellow pigment. Background technique [0002] Praseodymium yellow, also known as zirconium praseodymium yellow in the ceramic industry, is mainly used in the coloring of ceramic glazes. Its main component is zirconium silicate, and an appropriate amount of Pr 3+ and other ions to make a series of yellow pigments. [0003] The traditional method of preparing praseodymium yellow uses zircon sand as the main raw material, praseodymium oxide or praseodymium oxalate and other auxiliary materials are mixed by wet physical ball milling, and the base material is formed by calcining at a high temperature of about 1000 °C for a long time, and then pulverized, washed, dried, Grinding and sieving to make glaze pigments; or physically mixing zirconia, silicon dioxide, praseodymium oxide or praseodymium oxalate, and various mineralizers, calcin...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/20
Inventor 裴志明朱刘陈志波刘华胜
Owner 昆明先导新材料科技有限责任公司
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