KR20020022309A - Ceric ammonium nitrate manufacture method - Google Patents

Ceric ammonium nitrate manufacture method Download PDF

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Publication number
KR20020022309A
KR20020022309A KR1020000055023A KR20000055023A KR20020022309A KR 20020022309 A KR20020022309 A KR 20020022309A KR 1020000055023 A KR1020000055023 A KR 1020000055023A KR 20000055023 A KR20000055023 A KR 20000055023A KR 20020022309 A KR20020022309 A KR 20020022309A
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KR
South Korea
Prior art keywords
cerium
ammonium nitrate
nitrate
hydroxide
hydrolysis
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KR1020000055023A
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Korean (ko)
Inventor
정지연
백귀종
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정지완
테크노세미켐 주식회사
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Priority to KR1020000055023A priority Critical patent/KR20020022309A/en
Publication of KR20020022309A publication Critical patent/KR20020022309A/en

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/20—Compounds containing only rare earth metals as the metal element
    • C01F17/276—Nitrates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/20—Compounds containing only rare earth metals as the metal element
    • C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Abstract

PURPOSE: Provided is a preparation method of high purity ceric ammonium nitrate, (NH4)2Ce(NO3)6, by adding the process of HNO3 dissolution and hydrolysis of raw materials(ceria, cerium hydroxide) to a conventional method. CONSTITUTION: Ceric ammonium nitrate, (NH4)2Ce(NO3)6, is prepared by the following steps of: forming cerium nitrate hydroxide, Ce(OH)x(NO3)y, by dissolving ceria(CeO2), ceria hydroxide or cerium hydroxide into HNO3 and hydrolyzing; dissolving it into HNO3; adding ammonium nitrate; and crystallizing.

Description

질산제2세륨암모늄의 제조방법{Ceric ammonium nitrate manufacture method}Ceric ammonium nitrate manufacture method

본 발명은 세륨화합물인 산화세륨, 산화세륨수화물 또는 수산화세륨을 질산용해와 가수분해 공정의 정제 공정에 의해 생성된 99.9% 이상의 고순도 가수분해케이크인 수산화질산세륨〔Ce(OH)x(NO3)y〕을 사용하여 고순도의 질산제2세륨암모늄〔(NH4)2Ce(NO3)6〕을 제조하는 질산제2세륨암모늄의 제조방법에 관한 것이다.According to the present invention, cerium nitrate [Ce (OH) x (NO 3 ), which is a high purity hydrolysis cake of at least 99.9%, produced by cerium oxide, cerium oxide hydrate, or cerium hydroxide, is purified by nitrate dissolution and hydrolysis. y] to a method for producing dibasic cerium ammonium nitrate [(NH 4 ) 2 Ce (NO 3 ) 6 ] with high purity.

질산제2세륨암모늄은 박막트랜지스터 액정표시장치 (TFT LCD)의 제조공정중에서 TFT 제조공정과 칼라필터 (Color Filter) 제조공정에서 사용되고 있는 크롬에천트의 제조시 산화제로서 주로 사용되며, 유기 합성용 촉매로서도 사용되고 있다.Cerium ammonium nitrate is mainly used as an oxidizing agent in the manufacture of chromium etchant, which is used in the TFT manufacturing process and the color filter manufacturing process in the thin film transistor liquid crystal display (TFT LCD) manufacturing process. It is also used as.

종래에는 원료정제공정인 가수분해공정을 수행하지 않고 질산에 의해 용해한 다음에 질산암모늄을 첨가하여 결정화공정을 거쳐 질산제2세륨암모늄을 제조하고 있다.Conventionally, diammonium nitrate is prepared by dissolving with nitric acid, followed by crystallization by adding ammonium nitrate without performing a hydrolysis process, which is a raw material refining process.

따라서, 고가인 고순도의 세륨화합물의 원료를 사용하지 않고서는 순도가높은 질산제2세륨암모늄을 제조하기가 어려운 과제를 가지고 있다.Therefore, it is difficult to produce high purity cerium ammonium nitrate without using an expensive raw material of high purity cerium compound.

본 발명이 이루고자 하는 기술적 과제는 본 발명제품의 원료인 산화세륨, 산화세륨수화물 또는 수산화세륨의 고순도 정제공정인 가수분해 공정을 적용함으로써 저순도의 공업용 원료를 사용하여도 고순도의 질산제2세륨암모늄을 제조할 수 있도록 한 것이다.The technical problem to be achieved by the present invention is to apply high-purity purification process of cerium oxide, cerium oxide hydrate or cerium hydroxide, which is a raw material of the present invention, and to use high purity industrial raw material of cerium nitrate. It is to be able to manufacture.

본 발명은 원료인 산화세륨, 산화세륨수화물 또는 수산화세륨을 질산에 용해한 다음 가수분해시켜 고순도의 세륨화합물 케이크인 수산화질산세륨〔Ce(OH)x(NO3)y〕을 제조한 다음에 이를 다시 질산 용해한 후 질산암모늄을 첨가하고 결정화 공정을 거치도록 하므로써 질산제2세륨암모늄을 제조하는 것이다.In the present invention, a cerium nitrate [Ce (OH) x (NO 3 ) y], a high-purity cerium compound cake, is prepared by dissolving raw material cerium oxide, cerium oxide hydrate or cerium hydroxide in nitric acid and then hydrolyzing the same. After dissolving nitric acid, ammonium nitrate is prepared by adding ammonium nitrate and undergoing a crystallization process.

본 발명에 사용되는 원료는 산화세륨, 산화세륨수화물 또는 수산화세륨으로서 이들 원료중에는 란탄, 프라세디움, 네어디움, 사마륨, 가드리늄 등의 세륨 이외의 희토류 원소 뿐만 아니라 철, 망간, 칼슘 등의 금속 불순물과 각종 음이온 불순물들을 함유하고 있다.The raw materials used in the present invention are cerium oxide, cerium oxide hydrate or cerium hydroxide, and among these raw materials, iron, manganese, calcium and the like, as well as rare earth elements other than cerium such as lanthanum, prasedium, nedium, samarium, and gadrinium It contains metal impurities and various anionic impurities.

이들의 불순물은 TFT LCD 제조공정과 같은 정밀 에칭공정에서는 잔사 발생등의 문제점을 유발시키는 요인이 되고 있다.These impurities are causing a problem such as residue generation in a precision etching process such as a TFT LCD manufacturing process.

따라서, 본 발명은 수산화세륨등의 원료를 질산용해와 가수분해의 정제공정을 적용시킴으로써 저순도의 공업용 원료를 사용하면서도 고순도의 질산제2세륨암모늄을 제조하여 종래와 같이 불순물에 의한 문제점 유발을 방지하는 것이다.Therefore, the present invention by using the purification process of nitrate dissolution and hydrolysis of raw materials, such as cerium hydroxide, by using a high purity industrial raw material, while producing a high-purity cerium ammonium nitrate to prevent problems caused by impurities as in the prior art It is.

이상과 같이 본발명은, 가수분해 공정을 적용하게 되면 동일원료를 사용 할 때 종래의 제조방법과 유사한 수율을 유지하면서 종래의 제조방법보다 고순도의 질산제2세륨암모늄을 제조하는 것이 가능하며 공업적으로 적용시 저품위의 공업용 원료도 적용이 가능하여 원료 선정의 다양화와 제조원가 절감효과를 가져올 수 있다.As described above, according to the present invention, when the same raw material is used, it is possible to manufacture higher purity dicerium ammonium nitrate than the conventional manufacturing method while maintaining the yield similar to that of the conventional manufacturing method. In addition, low-grade industrial raw materials can be applied, resulting in diversification of raw material selection and manufacturing cost reduction.

Claims (2)

산화세륨, 산화세륨수화물 또는 수산화세륨을 질산용해와 가수분해에 의한 정제공정을 거쳐 얻어진 가수분해케이크인 수산화질산세륨〔Ce(OH)x(NO3)y〕을 다시 질산용해 한 후 이 용해액에 질산암모늄을 첨가한 다음 결정화 공정을 수행하여 질산제2세륨암모늄을 제조하는 질산제2세륨암모늄의 제조방법.After dissolving cerium oxide, cerium oxide hydrate, or cerium hydroxide by nitric acid dissolution and hydrolysis, a solution of cerium nitrate [Ce (OH) x (NO 3 ) y], a hydrolysis cake, was dissolved again. A method of producing ammonium dicerium nitrate, wherein ammonium nitrate is added to the mixture to form ammonium diacetate. 청구항 1에 있어서, 수산화세륨등의 원료를 정제하기 위해 가수분해법을 적용하는 질산제2세륨암모늄의 제조방법.The method for producing dicerium ammonium nitrate according to claim 1, wherein a hydrolysis method is applied to purify raw materials such as cerium hydroxide.
KR1020000055023A 2000-09-19 2000-09-19 Ceric ammonium nitrate manufacture method KR20020022309A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100391715B1 (en) * 2000-10-05 2003-07-16 일동화학 주식회사 Method for preparing ceric ammonium nitrate with high purity
KR100605365B1 (en) * 2004-12-23 2006-07-31 재단법인 포항산업과학연구원 Method for manufacturing cerium ammonium nitrate and withdrawing nitric acid from waste chrome etching solution

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR910009578A (en) * 1989-11-03 1991-06-28 헬렌 에이. 파블릭크 Neutral gray low permeability nickel-free glass
JPH03153520A (en) * 1989-11-08 1991-07-01 Sumitomo Chem Co Ltd Production of ceric ammonium nitrate
KR0149935B1 (en) * 1995-07-14 1999-04-15 이정성 Manufacturing method of cecium oxide
KR20010049291A (en) * 1999-04-27 2001-06-15 미우라 아끼라 Process for recovering a cerium from the solution containing a chromium and a cerium

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR910009578A (en) * 1989-11-03 1991-06-28 헬렌 에이. 파블릭크 Neutral gray low permeability nickel-free glass
JPH03153520A (en) * 1989-11-08 1991-07-01 Sumitomo Chem Co Ltd Production of ceric ammonium nitrate
KR0149935B1 (en) * 1995-07-14 1999-04-15 이정성 Manufacturing method of cecium oxide
KR20010049291A (en) * 1999-04-27 2001-06-15 미우라 아끼라 Process for recovering a cerium from the solution containing a chromium and a cerium

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100391715B1 (en) * 2000-10-05 2003-07-16 일동화학 주식회사 Method for preparing ceric ammonium nitrate with high purity
KR100605365B1 (en) * 2004-12-23 2006-07-31 재단법인 포항산업과학연구원 Method for manufacturing cerium ammonium nitrate and withdrawing nitric acid from waste chrome etching solution

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