CN103030167A

CN103030167A - Method for preparing spherical neodymium carbonate peroxide

Info

Publication number: CN103030167A
Application number: CN2012103834557A
Authority: CN
Inventors: 张瑞祥; 郝先库; 赵永志; 王士智; 汪立新; 刘海旺; 胡珊珊; 马显东; 许宗泽
Original assignee: JINGRUI NEW MATERIAL CO Ltd BAOTOU
Current assignee: JINGRUI NEW MATERIAL CO Ltd BAOTOU
Priority date: 2012-09-22
Filing date: 2012-09-22
Publication date: 2013-04-10
Anticipated expiration: 2032-09-22
Also published as: CN103030167B

Abstract

The invention relates to a method for preparing spherical neodymium carbonate peroxide, belonging to a material preparing process. The method comprises the following steps of: preparing an ammonium bicarbonate solution by using ammonium bicarbonate, ammonia water and deionized water; adding a neodymium nitrate solution into the ammonium bicarbonate solution to obtain a mixed solution of the ammonium bicarbonate, the ammonia water and the neodymium nitrate; adding hydrogen peroxide into the mixed solution to generate neodymium carbonate peroxide sediments; and aging, and filtering and cleaning the sediments to obtain a spherical neodymium carbonate peroxide product which is uniform in size and good in fluidity.

Description

The method for preparing spherical peroxide neodymium carbonate

Technical field

The present invention relates to a kind of method for preparing spherical peroxide neodymium carbonate, belong to a kind of material preparation process.

Background technology

The peroxide neodymium carbonate is a kind of solid active oxygenant, the alkene epoxidation in organic synthesis, oxidation of ketones etc. the reaction in as oxygenant.Utilize the peroxide carbonate to be the active oxygen donor, the catalyzer synthetic by the special electronic structure of neodymium and peroxide carbonate forms active peralcohol, auxiliary enhancement is played in reaction, the peroxide neodymium carbonate is a kind of reactive oxygen compounds, has high-energy, active oxygen is because higher than the energy state of ground state oxygen molecule, therefore shown the reactive behavior far above the ground state oxygen molecule, oxygen is passed to reaction substrate alkene, ketone etc., thereby realize the selective oxidation synthesize epoxide, in the organic synthesis catalyzed reaction, have a extensive future.The compounds process for production thereof such as peroxide neodymium carbonate preparation method and sodium carbonate peroxide, peroxide four potassium wolframates are completely different, because neodymium carbonate is not soluble in water, as with neodymium carbonate and water furnishing pulpous state, add hydrogen peroxide, after stirring certain hour, the precipitation that obtains detects by analysis, and precipitation still is neodymium carbonate; As being joined, hydrogen peroxide adds again ammonium bicarbonate soln in the neodymium nitrate solution, or hydrogen peroxide joined join again in the neodymium nitrate solution in the ammonium bicarbonate soln, two kinds of methods are through after fully reacting, the precipitation that obtains still is neodymium carbonate, and it is infeasible utilizing traditional method to prepare the peroxide neodymium carbonate.

Summary of the invention

The object of the present invention is to provide a kind of uniform particles, good fluidity, pattern is the preparation method of the spherical peroxide neodymium carbonate that is comprised of many squares, sheet structure.

Technical solution: it is 28% ammoniacal liquor that the present invention adds bicarbonate of ammonia and concentration in the reactor, bicarbonate of ammonia and ammoniacal liquor mol ratio are 1: 0.66-1.17, add again deionized water, bicarbonate of ammonia and deionized water mol ratio are 1: 6-9.1, obtaining concentration is the 3.7-4.5mol/L ammonium bicarbonate soln, at room temperature, adding concentration in the ammonium bicarbonate soln is the neodymium nitrate solution of 0.49-1.06mol/L, bicarbonate of ammonia and neodymium nitrate mol ratio are 1: 0.012-0.02 obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; Add concentration in the mixing solutions and be 30% hydrogen peroxide, neodymium nitrate and hydrogen peroxide mol ratio are 1: 3.2-9.5, reacted 1-4 hour, produce peroxide neodymium carbonate precipitation, static ageing 24-36 hour, with sedimentation and filtration, washing, obtain uniform particles, good fluidity, the peroxide neodymium carbonate product that pattern is spherical in shape.

The invention effect

Bicarbonate of ammonia concentration and digestion time are crucial among the present invention, add ammoniacal liquor and can improve bicarbonate of ammonia concentration in the solution, when bicarbonate of ammonia concentration is lower than 3.7mol/L, it is dissolved that adding neodymium nitrate solution has a small amount of flocks to be difficult for, the concentration of neodymium nitrate in ammonium bicarbonate soln is less, product yield is low, along with bicarbonate of ammonia concentration in the solution raises, neodymium nitrate concentration also raises, the yield height of peroxide neodymium carbonate precipitation that generates, only have the mixing solutions that forms bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate, could generate peroxide neodymium carbonate precipitation when adding hydrogen peroxide; Digestion time is the key factor that determined peroxide neodymium carbonate granularity, and digestion time was less than 4 hours, and peroxide neodymium carbonate deposit seeds is very thin, extremely sad filter, still aging more than 24 hours, be precipitated uniform particles, good fluidity, pattern is spherical peroxide neodymium carbonate.The present invention is convenient to realize suitability for industrialized production, utilizes factory's tradition neodymium carbonate precipitation operation, just can prepare peroxide neodymium carbonate product.

Description of drawings

Fig. 1 is the XRD figure spectrum of the spherical peroxide neodymium carbonate of the present invention;

Fig. 2 is the infrared spectrogram of the spherical peroxide neodymium carbonate of the present invention;

Fig. 3 is the SEM figure of the spherical peroxide neodymium carbonate of the present invention.

Embodiment

Embodiment 1

In reactor, add 560g bicarbonate of ammonia and 28% ammoniacal liquor 480ml, add deionized water 832ml, obtaining concentration is the 4.43mol/L ammonium bicarbonate soln, at room temperature, adding 115ml concentration in the ammonium bicarbonate soln is the neodymium nitrate solution of 1.06mol/L, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; Add 80ml concentration in the mixing solutions and be 30% hydrogen peroxide, react 2.5 hours, produce the peroxide neodymium carbonate and precipitate, static ageing 28 hours with sedimentation and filtration, washing, obtains uniform particles, good fluidity, the peroxide neodymium carbonate product that pattern is spherical in shape.

Embodiment 2

In reactor, add 735g bicarbonate of ammonia and 28% ammoniacal liquor 420ml, add deionized water 1302ml, obtaining concentration is the 4.43mol/L ammonium bicarbonate soln, at room temperature, adding 185ml concentration in the ammonium bicarbonate soln is the neodymium nitrate solution of 0.78mol/L, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; Add 84ml concentration in the mixing solutions and be 30% hydrogen peroxide, react 4 hours, produce the peroxide neodymium carbonate and precipitate, static ageing 36 hours with sedimentation and filtration, washing, obtains uniform particles, good fluidity, the peroxide neodymium carbonate product that pattern is spherical in shape.

Embodiment 3

In reactor, add 510g bicarbonate of ammonia and 28% ammoniacal liquor 510ml, add deionized water 935ml, obtaining concentration is the 3.8mol/L ammonium bicarbonate soln, at room temperature, adding 178.5ml concentration in the ammonium bicarbonate soln is the neodymium nitrate solution of 0.49mol/L, obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; Add 44ml concentration in the mixing solutions and be 30% hydrogen peroxide, react 2 hours, produce the peroxide neodymium carbonate and precipitate, static ageing 24 hours with sedimentation and filtration, washing, obtains uniform particles, good fluidity, the peroxide neodymium carbonate product that pattern is spherical in shape.

Claims

1. the method for preparing spherical peroxide neodymium carbonate, it is characterized in that, add bicarbonate of ammonia and concentration in the reactor and be 28% ammoniacal liquor, bicarbonate of ammonia and ammoniacal liquor mol ratio are 1: 0.66-1.17, add again deionized water, bicarbonate of ammonia and deionized water mol ratio are 1: 6-9.1, obtaining concentration is the 3.7-4.5mol/L ammonium bicarbonate soln, at room temperature, adding concentration in the ammonium bicarbonate soln is the neodymium nitrate solution of 0.49-1.06mol/L, bicarbonate of ammonia and neodymium nitrate mol ratio are 1: 0.012-0.02 obtains the mixing solutions of bicarbonate of ammonia, ammoniacal liquor and neodymium nitrate; Add concentration in the mixing solutions and be 30% hydrogen peroxide, neodymium nitrate and hydrogen peroxide mol ratio are 1: 3.2-9.5, reacted 1-4 hour, produce peroxide neodymium carbonate precipitation, static ageing 24-36 hour, with sedimentation and filtration, washing, obtain uniform particles, good fluidity, the peroxide neodymium carbonate product that pattern is spherical in shape.