KR960034079A - Manufacturing method of ultrafine crystalline titanium dioxide - Google Patents

Manufacturing method of ultrafine crystalline titanium dioxide Download PDF

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Publication number
KR960034079A
KR960034079A KR1019960032842A KR19960032842A KR960034079A KR 960034079 A KR960034079 A KR 960034079A KR 1019960032842 A KR1019960032842 A KR 1019960032842A KR 19960032842 A KR19960032842 A KR 19960032842A KR 960034079 A KR960034079 A KR 960034079A
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South Korea
Prior art keywords
titanium dioxide
reaction
titanic acid
ion
acid
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KR1019960032842A
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Korean (ko)
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KR100224732B1 (en
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정홍섭
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정홍섭
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
    • C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
    • C01G23/0538—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts in the presence of seeds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/04—Oxides; Hydroxides
    • C01G23/047—Titanium dioxide
    • C01G23/08—Drying; Calcining ; After treatment of titanium oxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Cosmetics (AREA)

Abstract

본 발명은 자외선 차단성이 우수하고 비교적 큰 표면적을 지니고 있어 화장품 원료, 플라스틱 첨가제, 안경의 멀티코팅제 등에 널리 사용되고 있는 이산화티탄의 제조방법에 관한 것으로서, 특히 종래에 비해 제조공정이 단순화되고 최종 생성물의 입자가 초미립형으로 우수한 물성을 나타내는 결정성 이산화티탄을 제조하는 방법에 관한 것이다.The present invention relates to a method for producing titanium dioxide which is widely used for cosmetic raw materials, plastic additives, and multi-coating agents for glasses because of its excellent ultraviolet shielding property and relatively large surface area. In particular, The present invention relates to a method for producing crystalline titanium dioxide having fine particles and exhibiting excellent physical properties.

즉, 본 발명은 고순도의 염화티타늄 또는 티탄산 화합물을 물을 가해 가수분해반응을 행하고 회농도로 희석한 티탄산 용액 또는 티탄산화합물을 물을 가해 가수분해를 행한 수용액에 알카리 용액을 가해 중화시킴에 의해 생성된 수산화티탄 침전물을 여과, 수세한 침전물에 수소이온을 지닌 산을 가해 pH농도를 강산성으로 조절하고 침전제를 넣거나 무첨가한 후 적정온도로 가열승온시켜 숙성반응을 행하여 제조된 이산화티탄 침전물을 후처리 공정을 거쳐 제조하는 것을 특징으로 한 0.1u 이하의 초미립형 결정성 이산화티탄을 제조하는 방법에 관한 것이다.That is, the present invention relates to a method for producing a titanic acid or titanic acid compound by neutralizing a titanic acid solution or a titanic acid compound in which a high purity titanium chloride or titanic acid compound is subjected to a hydrolysis reaction by adding water and then diluted to a concentration, The precipitated titanium hydroxide precipitate is filtered and washed with an acid having a hydrogen ion to adjust the pH to a strong acidity. The precipitated titanium dioxide precipitate is subjected to an aging reaction by heating at an appropriate temperature after or without adding a precipitant. The present invention relates to a method for producing ultrafine crystalline titanium dioxide having a grain size of 0.1 .mu.m or less.

Description

초미립형 결정성 이산화티탄 제조방법Manufacturing method of ultrafine crystalline titanium dioxide

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음Since this is a trivial issue, I did not include the contents of the text.

Claims (5)

TiCl4, TiOCl2화합물 중에서 선택된 티탄산화합물에 물을 가해 가수분해반응을 행하여 5~20 용적 % 티탄산 용액을 제조한 후, 서서히 교반하면서 숙성반응 온도를 30~100℃로 승온 유지시키면서 숙성반응을 행하여 제조된 이산화티탄 침전액을 여과, 수세, 건조와 같은 후처리 공정을 거쳐 제조하는 것을 특징으로 하는 초미립형 결정성 이산화티탄을 제조방법.TiCl 4 and TiOCl 2 compound is added to the hydrolysis reaction to prepare a 5 to 20 volume% titanic acid solution, and the aging reaction is carried out while the temperature of the aging reaction is maintained at 30 to 100 ° C with gentle stirring Wherein the produced titanium dioxide precipitate is subjected to post-treatment such as filtration, washing with water, and drying. TiCl4,TiSO4,TiOCl2화합물 중에서 선택된 티탄산화합물 가수분해반응을 행하여 생성된 산성수용액에 염기성 알카리 수용액을 가해 중화반응을 행하여 생성된 수산화티탄 침전물을 여과, 세척한 침전물에 수소이온을 지닌 산을 가해 5~20 용적% 티탄산 수용액을 만든 다음 반응 온도를 30~110℃로 승온 유지시키면서 숙성반응을 행하여 제조된 이산화티탄 침전액을 여과, 수세, 건조와 같은 후처리 공정을 거쳐 제조하는 것을 특징으로 하는 초미립형 결정성 이산화 티탄을 제조방법.TiCl 4 , TiSO 4 and TiOCl 2 compound, and neutralizing reaction is carried out by adding a basic aqueous alkali solution to the acidic aqueous solution produced by the hydrolysis reaction of the titanic acid compound. The resultant titanium hydroxide precipitate is filtered, And a titanium dioxide precipitate prepared by performing an aging reaction while maintaining the reaction temperature at 30 to 110 ° C. while maintaining the reaction temperature at 30 to 110 ° C. is subjected to post treatment such as filtration, By weight based on the total weight of the titanium dioxide fine particles. 제2항에 있어서, 수소이온을 지닌 산을 황산, 질산, 염산 중에서 선택된 것임을 특징으로 하는 초미립형 결정성 이산화티탄을 제조방법.The method according to claim 2, wherein the acid having a hydrogen ion is selected from sulfuric acid, nitric acid, and hydrochloric acid. 제1항 및 제2항에 있어서, 숙성 반응시 침전제로 초미립 이산화티탄 및 산과 알카리 반응에 의하여 생성된 염화합물 중에서 선택된 것을 사용함을 특징으로 하는 초미립형 결정성 이산화티탄을 제조하는 방법.The method of claim 1 or 2, wherein the precipitating agent used in the aging reaction is selected from ultrafine titanium dioxide and a salt compound formed by an acid and an alkali reaction. 제4항에 있어서, 염화합물은 염소이온, 질산이온, 탄산이온, 암모늄이온, 황산이온, 나트륨이온 중에서 선택된 이온을 함유한 것임을 특징으로 하는 초미립형 결정성 이산화티탄 제조방법.5. The method according to claim 4, wherein the salt compound contains ions selected from the group consisting of chloride ion, nitrate ion, carbonate ion, ammonium ion, sulfate ion and sodium ion. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: It is disclosed by the contents of the first application.
KR1019960032842A 1996-08-07 1996-08-07 Process for producing a micropowder type crystalline titanium oxide KR100224732B1 (en)

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KR1019960032842A KR100224732B1 (en) 1996-08-07 1996-08-07 Process for producing a micropowder type crystalline titanium oxide

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100350226B1 (en) * 2000-02-29 2002-08-27 나노케미칼 주식회사 Photocatalytic TiO2 powder with large specific surface area by homogeneous precipitation process at low temperature and method for manufacturing
KR100404449B1 (en) * 2001-02-16 2003-11-05 한상목 The manufacturing method of titanium oxide powder by dropping precipitant
KR100475551B1 (en) * 2002-10-08 2005-03-10 (주)아해 Preparation of Nanosized brookite-phase Titanium Dioxide Powder from Titanium Tetrachloride and Aqueous Hydrochloric Acid

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100420275B1 (en) * 2001-04-06 2004-03-02 (주)아해 Preparation of TiO2 fine powder from titanium tetrachloride with inorganic acid
KR100420277B1 (en) * 2001-04-27 2004-03-02 (주)아해 Preparation of TiO2 fine powder from titanium tetrachloride with Alcohol or Acetone
KR100424069B1 (en) * 2001-06-04 2004-03-22 (주)아해 Preparation of TiO2 ultrafine powders from titanium tetrachloride with inorganic acid solution by the advanced washing method
KR101307970B1 (en) 2011-02-11 2013-10-15 주식회사 예일전자 Synthesis method of BaTiO3 nanotube powder

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100350226B1 (en) * 2000-02-29 2002-08-27 나노케미칼 주식회사 Photocatalytic TiO2 powder with large specific surface area by homogeneous precipitation process at low temperature and method for manufacturing
KR100404449B1 (en) * 2001-02-16 2003-11-05 한상목 The manufacturing method of titanium oxide powder by dropping precipitant
KR100475551B1 (en) * 2002-10-08 2005-03-10 (주)아해 Preparation of Nanosized brookite-phase Titanium Dioxide Powder from Titanium Tetrachloride and Aqueous Hydrochloric Acid

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