KR970061780A - Manufacturing method of silica sol - Google Patents

Manufacturing method of silica sol Download PDF

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Publication number
KR970061780A
KR970061780A KR1019960003249A KR19960003249A KR970061780A KR 970061780 A KR970061780 A KR 970061780A KR 1019960003249 A KR1019960003249 A KR 1019960003249A KR 19960003249 A KR19960003249 A KR 19960003249A KR 970061780 A KR970061780 A KR 970061780A
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KR
South Korea
Prior art keywords
sol
cation exchange
alkali
silica sol
solution
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KR1019960003249A
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Korean (ko)
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KR0153136B1 (en
Inventor
안건영
웨이 데 시
Original Assignee
김창식
오공산업 주식회사
웨이 데 시
천진시 넘버원 케미칼 리전트 팩토리
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Priority to KR1019960003249A priority Critical patent/KR0153136B1/en
Publication of KR970061780A publication Critical patent/KR970061780A/en
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Publication of KR0153136B1 publication Critical patent/KR0153136B1/en

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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/146After-treatment of sols
    • C01B33/148Concentration; Drying; Dehydration; Stabilisation; Purification
    • C01B33/1485Stabilisation, e.g. prevention of gelling; Purification
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/51Particles with a specific particle size distribution
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)

Abstract

본 발명은 실리카졸의 제조방법에 관한 것으로, 상세하게는 규산염을 양이온 수지로 교환하여 산성 실리카졸을 얻고, 착화합물 처리 공정 후 미량의 금속이온을 양, 음이온 교환으로 제거하고, 상압, 끓는 상태의 안정화된 K+상태하에서 입자성장을 시킨 후, 암모니아 상 양이온 수지를 이용하여 K+를 제거하고, 박막 농축 및 한외 여과막 체처리를 통해 고순도, 고농도, 고균일도의 대립(大粒) 실리카졸을 제조하는 방법에 관한 것으로, 본 발명에서는 암모니아상 양이온 수지를 사용하여 K+를 교환하여 즉시 고순도의 암모니아로 안정화된 졸을 얻을 수 있어 본 발명의 제조 방법은 실리카졸을 공업적으로 제조하는데 있어서 진보되고 효과적인 방법인 것이다.More particularly, the present invention relates to a process for producing a silica sol, which comprises the steps of: exchanging a silicate with a cationic resin to obtain an acidic silica sol; removing a trace amount of metal ions by a positive and anion exchange; After growing the particles under a stabilized K + state, K + was removed by using an ammonia-based cationic resin, and high-purity, high-concentration, and high-uniformity large-size silica sols were prepared by thin-film concentration and ultrafiltration membrane treatment In the present invention, it is possible to obtain a sol which is stabilized with ammonia at a high purity immediately by exchanging K + by using an ammonia-based cationic resin. Thus, the production method of the present invention is an advanced and effective method for industrially producing silica sol .

Description

실리카졸의 제조방법Manufacturing method of silica sol

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

Claims (1)

시판 규산 나트륨을 순수로 희석하여 4~8%(SiO2기준) 농도의 규산 나트륨을 제조하는 공정과; 상기 규산 나트륨 용액에 강산 양이온 교환수지를 통과시켜 산성 실리카졸을 얻는 양이온 교환 공정; 상기 실리카졸에 0.1 내지 0.5% 옥살산(SiO2기준) 및 0.25 내지 1% 무기산(SiO2기준)을 가하여 숙성시키는 옥살산 및 무기산 처리공정; 상기 숙성된 용액을 음이온 교환수지에 통과시켜 PH 4 내지 5인 금속함량이 적은 산성졸을 만든 후, 바로 양이온 교환수지에 통과시키는 음이온 및 양이온 교환공정; 상기 공정에서 생성된 산성졸에 수산화 칼률(KOH)를 교반하면서 가하여 PH=9.0 내지 10.0으로 조정한 후 끓을 때까지 가열하는 알칼리 안정화 공정; 상기 공정에서 생성된 알칼리 용액에 음이온 및 양이온 교환 공정에서 생성된 산성졸을 교반하면서 8 내지 12시간 동안 일정속도로 가하여 15 내지 25㎚ 입자 크기의 알칼리 실리카졸을 얻은 후, 이 알칼리용액을 다시 끓을때까지 가열하면서 음이온 및 양이온 교환 공정에서 생성된 산성졸을 교반하면서 20 내지 40시간동안 일정속도로 가하여 35 내지 70㎚ 입자크기의 알칼리 실리카졸을 얻는 입자 성장 공정; 상기 공정에서 생성된 알칼리 졸을 암모니아상 양이온 수지에 통과시켜 암모니아로 안정화된 고순도 실리카졸을 얻는 암모니아상 양이온 교환 공정; 상기 공정에서 생성된 용액을 박막 농축시켜 30 내지 50%(SiO2기준) 농도인 알칼리 졸을 얻는 박막 농축공정; 및 상기 공정에서 수집된 용액을 10 내지 100㎚ 입경의 미세한 다공성 여과막에 통과시켜 입자를 선별하는 한외 여과막 체처리 공정으로 구성됨을 특징으로 하는 고순도, 고농도, 고균일도의 대립 실리카졸의 제조방법.Diluting commercial sodium silicate with pure water to prepare sodium silicate with a concentration of 4 to 8% (based on SiO 2 ); A cation exchange step of passing a strong acid cation exchange resin through the sodium silicate solution to obtain an acidic silica sol; An oxalic acid and inorganic acid treatment step in which the silica sol is aged by adding 0.1 to 0.5% of oxalic acid (based on SiO 2 ) and 0.25 to 1% of inorganic acid (based on SiO 2 ); An anion and a cation exchange process in which the aged solution is passed through an anion exchange resin to make an acidic sol having a low metal content of PH 4 to 5 and then passed directly through a cation exchange resin; An alkali stabilization step in which the hydroxyl value (KOH) is added to the acidic sol produced in the above step while stirring to adjust the pH to 9.0 to 10.0 and then heating until boiling; The anion and the acidic sol generated in the cation exchange process are added to the alkali solution produced in the above step at a constant rate for 8 to 12 hours to obtain an alkali silica sol having a particle size of 15 to 25 nm and then the alkali solution is boiled again , An acidic sol produced in an anion and a cation exchange process is added at a constant rate for 20 to 40 hours while stirring to obtain an alkali silica sol having a particle size of 35 to 70 nm; An ammonia phase cation exchange process in which an alkali sol produced in the above process is passed through a cationic resin in an ammonia phase to obtain a high purity silica sol stabilized with ammonia; A thin film thickening step of obtaining an alkali sol having a concentration of 30 to 50% (based on SiO 2 ) by concentrating the thin film of the solution produced in the above step; And an ultrafiltration membrane body treatment step of passing the solution collected in the above step through a fine porous filtration membrane having a particle size of 10 to 100 nm to select particles. ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: It is disclosed by the contents of the first application.
KR1019960003249A 1996-02-10 1996-02-10 Method of processing silica sol KR0153136B1 (en)

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KR1019960003249A KR0153136B1 (en) 1996-02-10 1996-02-10 Method of processing silica sol

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KR970061780A true KR970061780A (en) 1997-09-12
KR0153136B1 KR0153136B1 (en) 1998-11-16

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100349632B1 (en) * 2000-08-04 2002-08-24 주식회사영일화성 The manufacturing method of silica sol
KR102657883B1 (en) * 2021-08-02 2024-04-17 (주)에이스나노켐 Method for removing impurities from silicic acid, high-purity silicic acid and high-purity colloidal silica
KR102650839B1 (en) * 2021-09-01 2024-03-26 (주)에이스나노켐 Method for preparing high-purity colloidal silica and high-purity colloidal silica

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