KR19990032874A - Method for preparing powder carrier using oyster shell - Google Patents

Method for preparing powder carrier using oyster shell Download PDF

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KR19990032874A
KR19990032874A KR1019970054054A KR19970054054A KR19990032874A KR 19990032874 A KR19990032874 A KR 19990032874A KR 1019970054054 A KR1019970054054 A KR 1019970054054A KR 19970054054 A KR19970054054 A KR 19970054054A KR 19990032874 A KR19990032874 A KR 19990032874A
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powder
carrier
oyster shell
powder carrier
parts
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KR1019970054054A
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KR100218662B1 (en
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조명찬
신춘환
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신춘환
이창호
명광화학 주식회사
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0009Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0027Powdering
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/02Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/0081Preparation by melting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J37/00Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/08Heat treatment

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Cosmetics (AREA)

Abstract

해양에 폐기되는 굴패각을 이용 분말형 담체를 제조하는 방법으로 불순물을 제거한 굴패각을 분쇄하여 소성처리하고 소성처리된 분말을 산처리하여 불순물의 제거와 동시에 이온교환능을 갖는 활성화된 담체를 얻기 위하여 PH를 조절한 다음 건조하여 수화 시키고 다시 건조하여 분말화하므로서 분말형 담체를 제조하는 방법에 관한것임.A method of manufacturing a powder carrier using oyster shells discarded in the ocean is performed by pulverizing oyster shells from which impurities are removed and calcining the calcined powder by acid treatment to obtain an activated carrier having ion exchange ability at the same time as removing impurities. The present invention relates to a method for preparing a powder carrier by adjusting, drying, hydrating, drying, and powdering.

Description

굴패각을 이용한 분말형 담체의 제조방법Method for preparing powder carrier using oyster shell

본 발명은 해양에 폐기되는 굴패각을 사용하여 이온교환성이 우수한 순도높은 분말형 담체를 제조하는 것으로 상세하게는 수세과정을 거쳐 오물을 제거한 굴폐각을 상온 분쇄하여 이분말을 600-1200℃로 소성한 분말을 초산용액으로 PH를 조절하면서 교반하고 교반된 슬러리를 건조시킨 다음 다시 수화시켜 건조시킨 다음 분쇄하여 얻어지는 분말형 담체제조방법을 제공함에 있다.The present invention is to produce a high-purity powder carrier having excellent ion exchangeability by using the oyster shell discarded in the ocean, and in detail, by crushing the oyster waste angle to remove the dirt through water washing process at room temperature to sinter the powder to 600-1200 ℃ The present invention provides a method for preparing a powder carrier obtained by stirring a powder by adjusting pH with an acetic acid solution, drying the stirred slurry, then hydrating and drying the powder, and then grinding the powder.

본 발명은 분말형 담체의 제조방법에 관한 기술분야로 구체적으로는 이온교환능을 갖는 분말용 담체이면서 화장품 배합용 담체, 액상염료를 고화시키는 분말형담체 촉매용 담체등으로 널리 사용할수 있는 분말형 담체의 제조방법에 관한 기술분야로 종래의 분말형 담체로서는 제오라이트가 주로 사용되어 왔지만 제오라이트를 담체로 사용하기 위해서는 제조공정이 복잡하고 광물질의 불순물이 다량으로 함유되어 있어 순도를 높이기 위해서는 많은 경비가 소요되며 담체로서의 용도가 한정되는 문제점을 갖고 있다.The present invention relates to a powder carrier having a powder carrier having an ion-exchange capacity, which can be widely used as a carrier for cosmetic formulation, a carrier for a powder carrier catalyst for solidifying a liquid dye, and the like. Zeolite has been mainly used as a powder carrier in the technical field of the present invention, but the manufacturing process is complicated to use the zeolite as a carrier, and it contains a large amount of impurities in minerals, which requires a great expense to increase the purity. There is a problem that the use as a carrier is limited.

종래에 석회석으로 생석회를 제조하는 방법은 소성과정을 통해 제조할수 있으나 여기서 사용되는 석회석은 탄산칼슘의 함유량이 85-90% 정도에 불과하고 실리카, 알루미나, 철분, 산화마그네슘 등의 무기질 성분이 포함되어 이를 정제해서 사용하기엔 많은 경비가 소요되고 공정이 복잡하므로 본방법에서 요구되는 분말형담체로서는 사용하기 곤란하며 주로 시멘트의 원료로서 널리 사용되고 있는 실정이다.Conventionally, the method of preparing quicklime with limestone can be prepared by calcining process, but limestone used here contains only about 85-90% of calcium carbonate and contains inorganic components such as silica, alumina, iron, and magnesium oxide. It is difficult to use the powdery carrier required by this method because of the high cost and complexity of the process to refine and use it, and is widely used as a raw material for cement.

또 종래 패각을 소성해서 얻어지는 소석회는 요업분야에서 융점강하제, 유약등으로 사용되어 왔으며 본방법에서와 같이 분말형 담체제조의 원료로서는 시도된바 없다.In addition, slaked lime obtained by calcining shells has been used as a melting point lowering agent, a glaze, etc. in the ceramics field, and has not been attempted as a raw material for preparing a powder carrier as in the present method.

해변에 다량으로 폐기되는 굴패각 분말을 재활용함에 1차적인 목적이 있고 굴패각의 분말형 담체를 얻으므로서 공정의 단순화와 순도높은 분말형 담체를 제조할수 있음에도 또하나의 목적이 있으며 굴패각을 이용하므로서 이온 교환능이 우수한 담체와 다용도의 담체를 제조할수 있는 기술을 해결함에 목적이 있다 하겠다.Its primary purpose is to recycle oyster shell powder that is discarded in large quantities on the beach, and has another purpose in simplifying the process and manufacturing high purity powder carrier by obtaining powder carrier of oyster shell. It is an object of the present invention to solve a technology capable of producing a carrier having excellent exchangeability and a multipurpose carrier.

굴패각 분말의 X-Ray 회절에 의한 조성분석결과 전형적인 이온교환 담체인 제오라이트 기본 골격과 극히 유사함에 착안하여 본발명자는 해양에 폐기되는 굴패각을 이용 이온교환능을 가지면서 다용도의 담체에 적합한 순도높은 분말형 담체 제조를 시도한 것으로 이를 구체적으로 설명하면 수세과정을 거쳐 표면 불순물을 제거한 굴패각을 상온에서 분쇄하고 분쇄된 굴패각 분말을 600℃-1200℃ 범위에서 소성하여 CO2개스를 휘산시켜 CaO를 얻고 여기에서 생석회 2중량부에 초산 1-1.5 중량부 및 물 10부를 첨가 배합하여 이 수용액의 PH 범위가 7-8로 될 때까지 약 1-2시간 교반하고 교반된 슬러리(slurry)를 105℃에서 24시간 건조시키고 건조된 분말중량에 대하여 30배에 해당하는 25℃ 물에 침적시켜 다시 수화시킨다음 여과하거나 청징수를 제거하고 105℃에서 2시간 건조시킨후 용도에 따라 분말화하므로서 분말형 담체를 얻을수 있다.As a result of X-ray diffraction analysis of oyster shell powder, it was found that the composition is very similar to that of zeolite base skeleton which is a typical ion exchange carrier. In detail, this is an attempt to prepare a carrier, and pulverized oyster shells from which surface impurities are removed by washing with water at room temperature, and pulverized crushed oyster shell powders at 600 ° C. to 1200 ° C. are volatilized to CO 2 to obtain CaO, wherein quicklime 1-1.5 parts by weight of acetic acid and 10 parts of water are added to 2 parts by weight, and the mixture is stirred for about 1-2 hours until the pH range of the aqueous solution is 7-8, and the stirred slurry is dried at 105 ° C for 24 hours. And hydrated again by dipping in water at 25 ° C. equal to 30 times the weight of the dried powder, followed by filtration or removal of clarified water. After drying liver it can obtain a powdery carrier hameuroseo powdered according to the application.

위의 방법에서 수세과정은 굴패각을 살수여상형태의 수세과정을 거치고 건조는 진공건조공정으로 행하고 진공조건은 15mmHg 이하로 하는 것이 바람직하다.In the above method, the washing process is preferably the oyster shell and the washing process in the form of a watering phase.

상온 분쇄는 볼밀 분쇄기로 분쇄하여 직경 0.5cm-2.0cm 범위내에 있는 볼을 혼합하여 분쇄하는 것이 효과적이라 할수 있고 동 공정으로 1차 분쇄된 분말에 함수율이 습식기준으로 50%가 되도록 물을 분사하여 굴패각 분말사이에 형성된 공극의 비율을 줄이도록하여 2차 건조시킨다.In normal temperature grinding, it is effective to grind by grinding with a ball mill grinder and mix the balls in the range of 0.5cm-2.0cm in diameter and spray water so that the water content becomes 50% on wet basis in the powder ground first. Secondary drying is performed to reduce the percentage of voids formed between the oyster shell powder.

또 소성온도 범위는 600℃-1200℃ 로서 소성온도를 1200℃ 이상으로 점차적으로 상승시키면 담체기능이 점점 떨어지고 더욱 높이면 결정화를 거쳐 유리화로 진행되면서 담체로서의 기능은 전혀 기대할수 없다. 그리고 본 발명에서 한정하고 있는 소성온도 범위에서도 높은 온도에서 소성된 분말은 염기도가 높고 낮은 온도 범위에서 소성된 분말은 염기도가 낮다.In addition, the firing temperature ranges from 600 ° C to 1200 ° C, and gradually increases the firing temperature to 1200 ° C or higher. As a result, the carrier function gradually decreases. In addition, even in the firing temperature range defined in the present invention, the powder calcined at a high temperature has a high basicity and the powder calcined at a low temperature range has a low basicity.

이를 표(1)로 나타내면 아래와 같다.This is shown in Table (1).

이상의 표(1)에서 500℃에서 PH 8.3이나 CaCO3성분이 다량으로 포함되어 있는 상태이고 1300℃ 에서는 염기도가 높으나 분말형 담체로서의 기능이 크게 떨어진다.In Table 1 above, PH 8.3 or CaCO 3 component is contained in a large amount at 500 ° C., and the basicity is high at 1300 ° C., but its function as a powder carrier is greatly deteriorated.

또 표(1)에서와 같은 PH 범위에서도 활성화된 담체를 얻기 위해서는 초산을 첨가 PH 범위를 7-8로 낮추어야 한다.In addition, in order to obtain an activated carrier in the pH range as shown in Table (1), the pH range of addition of acetic acid should be lowered to 7-8.

이와같이 활성화된 담체를 얻기 위해서는 고온에서 소성된 분말을 다량의 초산량을 첨가해야하고 저온에서 소성된 분말은 고온에서 소성된 분말보다 적은량의 초산량을 사용하게 된다,In order to obtain the activated carrier, a large amount of acetic acid should be added to the powder calcined at a high temperature, and the powder calcined at a low temperature will use a smaller amount of acetic acid than a powder calcined at a high temperature.

그밖에도 소성분말에 초산을 첨가하므로서 백색도를 높일수 있고 순도 또한 향상 시킬수 있다.In addition, the addition of acetic acid to the small powder can increase the whiteness and improve the purity.

또 소성된 분말을 수회에 걸쳐 수화공정 및 건조공정을 거치므로서 백색도를 높일수 있고 불순물을 제거하여 순도를 높힘에 효과가 있으며 경도를 낮게하여 입자미분쇄화를 용이하게 할 수 있다.In addition, the calcined powder may be subjected to a hydration process and a drying process several times, thereby increasing whiteness, removing impurities, and increasing purity, and lowering hardness to facilitate particle pulverization.

해양에 폐기되는 다량의 굴껍질을 활용하므로서 담체제조원가를 절감할수 있고 종래 석회석이나 지오나이트를 원료로하는 생석회에 비하여 광물성 불순물이 적은 순도 및 백색도가 우수한 담체를 얻을 수 있으며 공정의 간편화로 용이하게 분말형 담체를 얻을수 있는 제조방법으로 제품 또한 활성화시킨 분말형 담체로서 이온교환능이 우수하여 이온교환 담체는 물론이고 순도가 99% 이상이여서 화장품 배합용담체, 염료고화용담체, 촉매용담체, 식품첨가용등으로 사용할수 있어 용도가 광범위한 분말형담체 제조방법이라 할수 있다.By using a large amount of oyster shells discarded in the ocean, it is possible to reduce the cost of manufacturing the carrier, and to obtain a carrier with excellent purity and whiteness with less mineral impurities than conventional limestone or zeolite as raw material. It is a powder type carrier that also activates the product as a manufacturing method to obtain a type carrier, and has excellent ion exchange ability, and has a purity of 99% or more as well as an ion exchange carrier, so it can be used as a cosmetic compound carrier, dye solidification carrier, catalyst carrier, food additive, etc. It can be used as a wide range of powder type carrier manufacturing method.

Claims (1)

불순물을 제거한 굴패각을 상온 분쇄하고 분쇄한 굴패각 분말을 600℃-1200℃에서 소성하여 소성분말을 얻고 이소성분말 2중량부에 초산 1-1.5부 및 물 10부를 배합하여 수용액의 PH가 7-8로 될 때까지 교반하고 교반된 슬러리를 105℃에서 24시간 건조시켜 건조된 분말중량에 대해 3 이내에 해당하는 상온수에 침적시켜 수화시킨 다음 이를 다시 건조 분말화함을 특징으로 하는 굴패각을 이용한 분말형 담체의 제조방법.The oyster shells from which impurities were removed were pulverized at room temperature, and the pulverized oyster shell powder was calcined at 600 ° C. to 1200 ° C. to obtain a small component powder, and 1 to 1.5 parts of acetic acid and 10 parts of water were mixed with 2 parts of isotropic powder to obtain a pH of 7-8 Stirred until the slurry was dried at 105 ° C. for 24 hours, hydrated by immersion in room temperature water corresponding to the dried powder weight within 3 for hydration, and then dried and powdered again to form a powder carrier using oyster shells. Way.
KR1019970054054A 1997-10-21 1997-10-21 Method of making powdered carrier using oyster shell KR100218662B1 (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100431634B1 (en) * 2001-09-19 2004-05-17 대우조선해양 주식회사 Absorbing material using a granular acid white clay and a granular oyster shells
KR100568855B1 (en) * 2004-08-02 2006-04-26 (주)에스비아이 환경 Ball manufacturing method for the production of multipurpose compound functions that activate the living body
KR100604353B1 (en) * 2005-02-28 2006-07-28 김덕현 The manufacturing method of calcium ionic water using a shell and equipment thereof

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102203072B1 (en) 2019-03-18 2021-01-14 군산대학교산학협력단 Method and System for making Lime Slurry using Oyster Shell

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100431634B1 (en) * 2001-09-19 2004-05-17 대우조선해양 주식회사 Absorbing material using a granular acid white clay and a granular oyster shells
KR100568855B1 (en) * 2004-08-02 2006-04-26 (주)에스비아이 환경 Ball manufacturing method for the production of multipurpose compound functions that activate the living body
KR100604353B1 (en) * 2005-02-28 2006-07-28 김덕현 The manufacturing method of calcium ionic water using a shell and equipment thereof

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