阅读说明：本技术 一种氢氧化锆的生产方法 (Method for producing zirconium hydroxide ) 是由 闫家臣 宋九洲 于 2020-04-28 设计创作，主要内容包括：本发明涉及氢氧化锆生产工艺技术领域,特别涉及一种氢氧化锆的生产方法。其方法包括氧氯化锆溶液的制备,称重配比,控制流量反应,陈化,补充氧氯化锆溶液重量,水洗和离心。本发明通过调节氧氯化锆和氨水/氢氧化钠的使用比例,设计合适的反应速度。分批次反应产生氢氧化锆颗粒,通过3倍去离子水洗涤得到Cl-＜200ppm的松散粉末状氢氧化锆,其中氧化锆含量可达40％。(The invention relates to the technical field of zirconium hydroxide production processes, in particular to a production method of zirconium hydroxide. The method comprises the steps of preparing a zirconium oxychloride solution, weighing and proportioning, controlling flow reaction, aging, supplementing the weight of the zirconium oxychloride solution, washing and centrifuging. The invention designs a proper reaction speed by adjusting the use ratio of zirconium oxychloride and ammonia water/sodium hydroxide. The zirconium hydroxide particles are produced by batch reaction, and are washed by 3 times of deionized water to obtain loose powdery zirconium hydroxide with Cl < -200 ppm, wherein the content of zirconium oxide can reach 40 percent.)

1. A method for producing zirconium hydroxide comprises the following steps:

A. preparing a zirconium oxychloride solution, dissolving 1 part by mass of zirconium oxychloride in 3 parts by mass of softened water, and filtering the solution into a storage tank after the dissolution is finished;

B. mixing 10% ammonia water and 30% sodium hydroxide according to a mass ratio of 5-8: 1, stirring and uniformly mixing to obtain an alkaline precipitator;

C. respectively weighing 1 part by mass of zirconium oxychloride solution and 1.8 parts by mass of alkaline precipitant, and feeding the zirconium oxychloride solution and the alkaline precipitant into a first elevated tank and a second elevated tank;

D. adding 0.1 part by mass of softened water into the reactor, enabling the solutions in the first elevated tank and the second elevated tank to automatically flow into the reactor within 2 hours by controlling a valve, and aging for 6 hours;

E. supplementing 0.2-0.5 part by mass of zirconium oxychloride solution into the first elevated tank, controlling a valve to ensure that the zirconium oxychloride solution in the first elevated tank is dropwise added within 2 hours, feeding the zirconium oxychloride solution into a reactor, and continuously aging for 2 hours;

F. and centrifuging the zirconium hydroxide slurry obtained after the reaction by using a centrifugal machine to remove the mother liquor, and adding softened water with the mass being 3 times that of the mother liquor to wash the mother liquor to obtain the zirconium hydroxide with the chloride ion being less than 200 ppm.

2. The method for producing zirconium hydroxide according to claim 1, wherein the mass ratio of 10% ammonia water to 30% sodium hydroxide is 5: 1.

3. the method for producing zirconium hydroxide according to claim 1, wherein the mass ratio of 10% ammonia water to 30% sodium hydroxide is 8: 1.

4. the method for producing zirconium hydroxide according to claim 1, wherein the mass ratio of 10% ammonia water to 30% sodium hydroxide is 6: 1.

5. the method for producing zirconium hydroxide according to claim 1, wherein the amount of the supplemented zirconium oxychloride solution in step E is 0.2 parts by mass.

6. The method for producing zirconium hydroxide according to claim 1, wherein the amount of the supplemented zirconium oxychloride solution in step E is 0.5 parts by mass.

7. The method for producing zirconium hydroxide according to claim 1, wherein the amount of the supplemented zirconium oxychloride solution in step E is 0.3 parts by mass.

Technical Field

The invention relates to the technical field of zirconium hydroxide production processes, in particular to a production method of zirconium hydroxide.

Background

The zirconium hydroxide is a water-insoluble amphoteric hydroxide with slightly strong alkalinity, is non-toxic and tasteless, is insoluble or slightly soluble in water, is insoluble in alcohol, alkali and ammonium salt solutions, is easily soluble in inorganic acids such as hydrochloric acid, and can be decomposed into zirconium dioxide and water at 500 ℃, and can react with acid and alkali to generate crystalline ortho-zirconate with strong alkali during melting due to the amphiphilicity.

Zirconium hydroxide is used to make other zirconium compounds, pigments, dyes, glasses, and the like. It is mainly used for preparing zirconium and zirconium compounds, and also used as fillers, catalysts, deodorants, pigments and the like in the industries of plastics, rubber, ion exchange resin and the like. Used as analytical reagent, and also used for preparing chromium compounds and preparing pigments; used as other zirconium product intermediates.

The zirconium hydroxide with high quality required in the current market has the zirconium oxide content of 36% or more, and the preparation of the zirconium hydroxide in the prior art generally adopts zirconium oxychloride to dissolve, and the zirconium oxychloride is mixed with ammonia water or sodium hydroxide to react, and then the zirconium hydroxide is washed, dehydrated and packaged. The slurry produced in the production process is viscous and is not easy to dehydrate, and a large amount of deionized water is consumed for removing impurity ions; the production process can only produce zirconium hydroxide with zirconium oxide content lower than 30%, and has difficult impurity ion removal and low purity.

Zirconium hydroxide with the content of 36 percent or more is generally obtained by a drying process, the production cost is wasted, and the material content is not uniform.

Disclosure of Invention

In order to solve the problems of the prior art, the invention provides a production method of zirconium hydroxide, which can produce zirconium hydroxide with the zirconium oxide content of 40-46%.

The technical scheme adopted by the invention is as follows:

a method for producing zirconium hydroxide comprises the following steps:

A. preparing a zirconium oxychloride solution, dissolving 1 part by mass of zirconium oxychloride in 3 parts by mass of softened water, and filtering the solution into a storage tank after the dissolution is finished;

B. mixing 10% ammonia water and 30% sodium hydroxide according to a mass ratio of 5-8: 1, stirring and uniformly mixing to obtain an alkaline precipitator;

C. respectively weighing 1 part by mass of zirconium oxychloride solution and 1.8 parts by mass of alkaline precipitant, and feeding the zirconium oxychloride solution and the alkaline precipitant into a first elevated tank and a second elevated tank;

D. adding 0.1 part by mass of softened water into the reactor, enabling the solutions in the first elevated tank and the second elevated tank to automatically flow into the reactor within 2 hours by controlling a valve, and aging for 6 hours;

E. supplementing 0.2-0.5 part by mass of zirconium oxychloride solution into the first elevated tank, controlling a valve to ensure that the zirconium oxychloride solution in the first elevated tank is dropwise added within 2 hours, feeding the zirconium oxychloride solution into a reactor, and continuously aging for 2 hours;

F. and centrifuging the zirconium hydroxide slurry obtained after the reaction by using a centrifugal machine to remove the mother liquor, and adding softened water with the mass being 3 times that of the mother liquor to wash the mother liquor to obtain the zirconium hydroxide with the chloride ion being less than 200 ppm.

The technical scheme provided by the invention has the beneficial effects that:

the principle of the invention is as follows: controlling the concentration of Zr4+ in the reaction system and OH-in the precipitator, rapidly agglomerating Zr4+ and OH-after combination to form zirconium hydroxide particles by controlling the flow rate, and gradually growing the particles into larger particles (D50: 30-40 μm) along with the proceeding of the reaction and the prolonging of the aging time; meanwhile, due to the dispersing effect of the dispersing agent, the formed zirconium hydroxide particles can not be adhered together to form a jelly; when impurities are washed in a centrifugal machine, as zirconium hydroxide particles are large and gaps are formed among the particles, a bridge can be quickly formed in a filter cake, impurities such as Cl & lt- & gt, Na & lt + & gt and the like can be quickly washed away by using deionized water, and the water consumption for removing the impurities is reduced; meanwhile, the capacity of the filter cake for storing free water is weakened, the zirconium oxide content in the zirconium hydroxide after centrifugation can be directly over 40 percent, the zirconium hydroxide content is prevented from being continuously improved by using drying and other modes, and the production cost is greatly reduced.

The obtained granular zirconium hydroxide changes the gel state of reaction slurry, improves the water passing efficiency and reduces the water consumption.

Controlling the configuration mode of the alkaline precipitant to be 5-8: 1, the dosage of the chloride ion washing water in the product can be effectively controlled and reduced from 6 times to 3 times.

By controlling the part of the supplementary zirconium oxychloride to be 0.2-0.5 part by mass, the size of the particles can be effectively controlled, and the centrifugal dehydration effect and content are ensured. After modification, the zirconium hydroxide particles obtained by the reaction can be prepared in a manner that D50: 30-40 μm, and the particle size before modification is generally about 15 μm.

Drawings

In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.

FIG. 1 is a schematic view of an apparatus for producing zirconium hydroxide according to the present invention.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.