Organic phase back-extraction method for preparing cerium terbium lanthanum phosphate

A technology of lanthanum cerium terbium phosphate and organic phase is applied in the preparation of lanthanum cerium terbium phosphate and the preparation of rare earth phosphate, which can solve the problem that the ratio of rare earth elements and phosphate radicals cannot be accurately controlled, and the particle size and particle size distribution of products cannot be effectively controlled. The synthetic product is mixed with impurities and other problems, so as to avoid the phenomenon of local over-concentration of ions, the manufacturing process is novel and unique, and the effect of reducing the impurity content is achieved.

Active Publication Date: 2009-12-02
江阴加华新材料资源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of this process are: phosphorus oxide volatilization is easy to occur at high temperature, so that the ratio of rare earth elements and phosphate radicals in the product cannot be accurately controlled; the burning temperature is high, and the energy consumption is large; the synthetic product is mixed with impuritie

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Dissolve 20g of lanthanum oxide, 10g of cerium oxide, and 5g of terbium oxide with hydrochloric acid, and the combined volume of the three chloride solutions is 250ml, and the concentration is 0.8mol / L; P507) 50ml is mixed with 350ml sulfonated kerosene, saponified to 0.35M by adding NaOH; move the rare earth solution and mixed extractant into the reactor, adjust the oscillation frequency to 60HZ, and after the oscillation time is 3 minutes, let the mixed solution stand still to separate the loaded rare earth 400ml of the organic phase solution; measure 25ml of high-concentration phosphoric acid solution (14N), add 325ml of deionized water to prepare a phosphoric acid solution with a hydrogen ion concentration of 1.0mol / L; add 200ml of deionized water to the reactor, At a stirring speed of 1 minute, the automatic flow control device simultaneously adds the loaded organic phase and phosphoric acid solution to the reactor, keeping the adding speed at 60ml / minute, and the t...

Embodiment 2

[0018] Dissolve 20g of lanthanum oxide, 10g of cerium oxide, and 5g of terbium oxide with nitric acid, and mix the three nitrate solutions to a total volume of 250ml, with a concentration of 0.8mol / L; mix 50ml of naphthenic acid with 350ml of sulfonated kerosene, and add NaOH for saponification to 0.35M; move the rare earth solution and the mixed extractant into the reactor, adjust the oscillation frequency to 60HZ, and after the oscillation time is 3 minutes, leave the mixed solution to separate 400ml of the organic phase solution loaded with rare earth; measure the high-concentration phosphoric acid solution ( 14N) 25ml, add deionized water 325ml to be deployed into the phosphoric acid solution that the hydrogen ion concentration is 1.0mol / L; Add 200ml deionized water in the reactor, under the stirring speed of 200 rev / mins, by the automatic flow control device simultaneously to Add the loaded organic phase and phosphoric acid solution into the reactor, keep the adding speed ...

Embodiment 3

[0020]Dissolve 25g of lanthanum oxide, 10g of cerium oxide, and 5g of terbium oxide with hydrochloric acid, and the combined volume of the three chloride solutions is 250ml, and the concentration is 0.8mol / L; P507) 40ml, Cyanex27210ml, sulfonated kerosene 350ml mixed, add NaOH saponification to 0.4M; move the rare earth solution and mixed extractant into the reactor, adjust the oscillation frequency to 60HZ, the oscillation time is 3 minutes, then stand the mixed solution to separate Load rare earth organic phase solution 400ml; measure high-concentration phosphoric acid solution (14N) 30ml, add deionized water 320ml to be deployed into the phosphoric acid solution that hydrogen ion concentration is 1.0mol / L; Add 200ml deionized water in the reactor, at 200 Under the stirring speed of rev / min, the automatic flow control device simultaneously adds the load organic phase and the phosphoric acid solution to the reactor, keeping the adding speed at 60ml / min, and the two are added a...

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PUM

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Abstract

The invention relates to an organic phase back-extraction method for preparing cerium terbium lanthanum phosphate, which comprises the following process steps: (1) using hydrochloric acid or nitric acid to dissolve lanthana, cerium oxide and terbia respectively to obtain first solution; (2) preparing organic extractant solution which consists of one or two extractants of 2-ethylhexyl phosphate 2-ethylhexyl ester, trioctyl tertiary amine, dioctylphosphoric acid ester, tributyl phosphate, Cyanex272 and naphthenic acid and sulfonated kerosene to obtain second solution; (3) adding the first solution and the second solution into a reactor to prepare third solution; (4) preparing solution containing phosphate groups to form rare-earth phosphate sediment; and (5) after the precipitation reaction is finished, washing products by water, performing centrifugal dehydration on the product, mixing the product and absolute ethanol into slurry, placing the slurry, carrying out drying treatment on the slurry and calcinating the dried slurry to obtain a cerium terbium lanthanum phosphate powder body. The cerium terbium lanthanum phosphate prepared by the method has low content of impurity, controllability of the granularity of particles, even distribution of the granularity of the particles and good crystal morphology.

Description

(1) Technical field [0001] The invention relates to a preparation method of rare earth phosphate, in particular to a preparation method of lanthanum cerium terbium phosphate, which belongs to the technical field of rare earth new materials in the field of inorganic materials. (2) Background technology [0002] Rare earth phosphate is a kind of fluorescent light-emitting material that is widely used, and the most representative one is lanthanum cerium terbium phosphate green phosphor, which is a kind of green phosphor widely used in rare earth three primary color fluorescent lamps and other purposes, and its molecular formula is ( LaCeTb)PO4, referred to as LAP. Compared with the conventional aluminate green powder (CAT), this material has the advantages of high luminous brightness, moderate synthesis temperature, and large color coordinate X value. It is a new generation of green phosphor products that replace CAT, and has become a rare earth One of the hotspots in the fiel...

Claims

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Application Information

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IPC IPC(8): C01B25/46
Inventor 史卫东肖睿朱荣华王金飞
Owner 江阴加华新材料资源有限公司
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