KR100333497B1 - METHOD OF REMOVAL OF MgO AS CRYSTALLINE MgSO4·nH2O FROM THE REACTION PRODUCT MIXTURE OF B4C, MgO AND B2O3 BY SHS - Google Patents

METHOD OF REMOVAL OF MgO AS CRYSTALLINE MgSO4·nH2O FROM THE REACTION PRODUCT MIXTURE OF B4C, MgO AND B2O3 BY SHS Download PDF

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KR100333497B1
KR100333497B1 KR19990043290A KR19990043290A KR100333497B1 KR 100333497 B1 KR100333497 B1 KR 100333497B1 KR 19990043290 A KR19990043290 A KR 19990043290A KR 19990043290 A KR19990043290 A KR 19990043290A KR 100333497 B1 KR100333497 B1 KR 100333497B1
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mgo
powder
reaction product
unreacted
sulfuric acid
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KR20010036332A (en
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임경란
구희진
이준근
한경섭
김창삼
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박호군
한국과학기술연구원
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/90—Carbides
    • C01B32/914—Carbides of single elements
    • C01B32/991—Boron carbide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D43/00—Separating particles from liquids, or liquids from solids, otherwise than by sedimentation or filtration
    • 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
    • C01F5/00—Compounds of magnesium
    • C01F5/40—Magnesium sulfates

Abstract

본 발명은 자전 고온 반응 합성법에 의해 B2O3, C, Mg의 혼합물로 부터 B4C 분말을 제조할 때 동반되는 과량의 MgO을 유용한 Mg화합물로 회수하는 방법에 관한 것으로, B4C분말을 B2O3(또는 H3BO3)와 탄소 분말에 Mg분말을 혼합하여 SHS 방법에 의하여 제조함에 있어서, 반응 생성물을 증류수 또는 알콜로 세척하여 미반응 B2O3(또는 H3BO3)을 제거하고, 미반응 B2O3(또는 H3BO3)이 제거된 반응 생성물을 묽은 황산에 분산시킨 후 일정 시간 교반하여 미반응 Mg와 반응 생성물의 MgO를 황산과 반응시킨 후 필터로 B4C를 분리하고, B4C가 분리된 여과액을 농축시켜 결정상의 MgSO4·nH2O를 얻는 것으로 이루어지는 자전 고온반응 합성법에 의한 탄화붕소 분말 제조시 부산물 MgO의 환경 친화적 분리 방법을 제공한다. 본 발명에 의하면 비교적 간단한 공정에 의하여, 자전 고온 반응 합성법에 의해 B2O3, C, Mg의 혼합물로 부터 B4C 분말을 제조할 때 동반되는 과량의 MgO로부터 비료 성분인 결정상의 MgSO4을 얻을 수 있어 자원 재활용이 가능하고, 종래의 MgO 처리 방법인 폐산 처리에서 발생되는 환경 오염을 방지할 수 있게 된다.The present invention relates to a method for recovering excess MgO as a useful Mg compound when preparing B 4 C powder from a mixture of B 2 O 3 , C, Mg by a rotating high temperature reaction synthesis method, B 4 C powder Was prepared by the SHS method by mixing Mg powder with B 2 O 3 (or H 3 BO 3 ) and carbon powder, the reaction product was washed with distilled water or alcohol to react with unreacted B 2 O 3 (or H 3 BO 3 ), The reaction product from which unreacted B 2 O 3 (or H 3 BO 3 ) has been removed is dispersed in dilute sulfuric acid, and then stirred for a while to react unreacted Mg with MgO of the reaction product with sulfuric acid. Remove the B 4 C, and, B 4 C is an environment-friendly separation of by-products MgO manufacturing boron carbide powder method by rotating the high temperature reaction synthesis made to concentrate the filtrate was separated to obtain MgSO 4 · nH 2 O crystal phase do. According to the present invention, by the relatively simple process, MgSO 4 as a fertilizer component is obtained from an excess of MgO accompanying the preparation of B 4 C powder from a mixture of B 2 O 3 , C, and Mg by a rotating high temperature reaction synthesis method. As a result, it is possible to recycle resources and to prevent environmental pollution from waste acid treatment, which is a conventional MgO treatment method.

Description

자전 고온반응 합성법에 의한 탄화붕소 분말 제조시 부산물 ＭｇＯ의 환경 친화적 분리 방법{METHOD OF REMOVAL OF ＭｇＯ AS CRYSTALLINE MgSO4·nH2O FROM THE REACTION PRODUCT MIXTURE OF B4C, ＭｇＯ AND B2O3 BY SHS}Environmentally friendly separation method of by-product MgO in the production of boron carbide powder by the autogenous high-temperature reaction synthesis method.

본 발명은 자전 고온 반응 합성법에 의해 B2O3, C, Mg의 혼합물로 부터 B4C 분말을 제조할 때 동반되는 과량의 MgO을 산으로 녹여 폐산으로 처리하는 일반적인 방법 대신, 유용한 Mg화합물로 회수하는 방법에 관한 것이다.The present invention provides a useful Mg compound instead of the general method of dissolving excess MgO as acid and treating it with waste acid when preparing B 4 C powder from a mixture of B 2 O 3 , C, Mg by a rotating high temperature reaction synthesis method. It relates to a method of recovery.

B4C분말 합성 방법에는 B2O3(또는 H3BO3)을 탄소분말과 혼합한 후 전기 아크를 이용하는 강한열로 반응시키는 탄소환원법, 비교적 저온에서 B4C을 얻을 수 있는 Mg환원법, 그리고 원소상태의 직접 반응법등이 있다. 이중 B2O3을 탄소속에서 Mg으로 환원시켜 B4C와 MgO을 생성하는 방법은 SHS(self-propagation high temperature synthesis, 자전 고온 반응 합성)를 이용할 수 있다. 이 방법에 의한 반응식은 아래와 같다.The method for synthesizing B 4 C powder includes a carbon reduction method in which B 2 O 3 (or H 3 BO 3 ) is mixed with carbon powder and reacted with strong heat using an electric arc, Mg reduction method for obtaining B 4 C at a relatively low temperature, And the direct reaction of elemental state. The method of producing B 4 C and MgO by reducing B 2 O 3 to Mg in carbon may use self-propagation high temperature synthesis (SHS). The reaction scheme by this method is shown below.

2B2O3+ C + 6Mg → B4C + 6MgO2B 2 O 3 + C + 6Mg → B 4 C + 6MgO

상기 반응은 수초안에 진행되나, 반응이 완결되지 않아 반응 생성물에서 과량의 MgO을 제거하여 순수 B4C를 분리하는 방법이 산업적으로 문제가 되고 있다. 현재까지는 상기 SHS 반응 생성물을 염산, 불산, 황산 또는 이들의 혼합산 등을 사용하여 미반응 Mg 및 B2O3와 생성물 MgO을 녹여 B4C를 분리하고 있다. 그런데 이 과정에서 많은 산을 사용하게 되므로 이때 발생되는 폐수가 환경 오염을 야기한다.The reaction proceeds in a few seconds, but the reaction is not completed and the method of separating the pure B 4 C by removing excess MgO from the reaction product is an industrial problem. To date, the SHS reaction product is dissolved in unreacted Mg and B 2 O 3 and the product MgO using hydrochloric acid, hydrofluoric acid, sulfuric acid, or a mixed acid thereof to separate B 4 C. However, since a lot of acid is used in this process, wastewater generated at this time causes environmental pollution.

본 발명은 상기의 문제점을 해결하기 위하여, SHS방법으로 B4C를 생성할 때 부산물로 생기는 MgO를 효과적으로 분리시키고 재활용할 수 있는 방법을 모색하여 오염 물질의 발생을 방지하는데 그 목적을 두고 있다.In order to solve the above problems, the present invention aims to prevent the generation of contaminants by searching for a method for effectively separating and recycling MgO generated as a by-product when generating B 4 C by the SHS method.

본 발명은 B4C분말을 B2O3(또는 H3BO3)와 탄소 분말에 Mg분말을 혼합하여 SHS 방법에 의하여 제조함에 있어서, 반응 생성물을 증류수 또는 알콜로 세척하여 미반응 B2O3(또는 H3BO3)을 제거하고, 미반응 B2O3(또는 H3BO3)이 제거된 반응 생성물을 묽은 황산에 분산시킨 후 일정 시간 교반하여 미반응 Mg와 반응 생성물의 MgO를 황산과 반응시킨 후 필터로 B4C를 분리하고, B4C가 분리된 여과액을 농축시켜 결정상의 MgSO4·nH2O를 얻는 것으로 이루어지는 자전 고온반응 합성법에 의한 탄화붕소 분말 제조시 부산물 MgO의 환경 친화적 분리 방법을 제공한다.The present invention is prepared by mixing the B 4 C powder with B 2 O 3 (or H 3 BO 3 ) and Mg powder to the carbon powder by the SHS method, the reaction product is washed with distilled water or alcohol to react with unreacted B 2 O 3 (or H 3 BO 3 ) is removed, and the reaction product from which unreacted B 2 O 3 (or H 3 BO 3 ) is removed is dispersed in dilute sulfuric acid and stirred for a period of time to remove unreacted Mg and MgO of the reaction product. after the sulfuric acid and the reaction to remove the B 4 C as a filter and, B 4 C is a by-product in the manufacture boron carbide powder by rotating the high temperature reaction synthesis made to concentrate the filtrate was separated to obtain MgSO 4 · nH 2 O crystal phase MgO Provide an environmentally friendly separation method.

상기 세척 단계에서 증류수 또는 알콜의 온도는 상온에서 100℃, 바람직하게는 50 ~ 100℃의 범위가 적당하다. 또한 반응 생성물을 황산에 분산시킬 때, 황산은 2 ~ 5배로 희석시킨 것을 사용하는 것이 바람직하다.In the washing step, the temperature of the distilled water or alcohol is suitably in the range of 100 ℃, preferably 50 ~ 100 ℃ at room temperature. In addition, when the reaction product is dispersed in sulfuric acid, it is preferable to use sulfuric acid diluted 2 to 5 times.

황산에 분산된 반응 생성물은 30분 ~ 1시간 동안 교반하는 것이 적당하다.The reaction product dispersed in sulfuric acid is suitably stirred for 30 minutes to 1 hour.

상기 방법에 의하여 얻어지는 결정상의 MgSO4·nH2O는 비료 성분으로 사용될 수 있어 자원 재활용과 환경 오염 방지의 두 가지 목적을 달성할 수 있게 된다.MgSO 4 · nH 2 O in the crystalline phase obtained by the above method can be used as a fertilizer component to achieve the two purposes of resource recycling and environmental pollution prevention.

비료중 엽록소로 사용되는 MgSO4·nH2O는 Mg 또는 MgO을 H2SO4으로 처리하여 결정상의 MgSO4·6H2O, MgSO4·4H2O 등으로 제조한다. 그런데 B4C분말을 B2O3(또는 H3BO3)와 탄소 분말에 Mg분말을 혼합하여 SHS 방법에 의하여 제조할 때 발생되는 반응 혼합물을 바로 황산으로 처리하여 액상을 고상으로부터 분리하고 액상을 가열 농축하여도 MgSO4결정 분말은 생성되지 않는다. 따라서 이 여과액은 폐수 처리되고 있는데, SHS 반응시 반응의 미완결로 인하여 잔존하는 B2O3가 MgSO4·nH2O의 결정 생성을 방해하는 것으로 여겨진다.MgSO 4 nH 2 O, which is used as chlorophyll in fertilizers, is prepared from MgSO 4 · 6H 2 O, MgSO 4 · 4H 2 O, etc. by treating Mg or MgO with H 2 SO 4 . However, when the B 4 C powder is mixed with B 2 O 3 (or H 3 BO 3 ) and carbon powder, Mg powder is produced by the SHS method, the reaction mixture is directly treated with sulfuric acid to separate the liquid phase from the solid phase and the liquid phase. MgSO 4 crystal powder is not produced even by heating and concentrating. Therefore, this filtrate is treated with wastewater, and it is believed that the remaining B 2 O 3 interferes with the crystal formation of MgSO 4 nH 2 O due to incomplete reaction during the SHS reaction.

그러나 SHS 방법에 의하여 제조할 때 발생되는 반응생성물을 먼저 뜨거운 물로 세척하여 미반응된 B2O3또는 수용성의 다른 불순물을 제거한 후, 묽은 황산에 분산시키고 교반하여 MgO와의 반응을 촉진시킨 다음, 황산과 반응한 액상의 MgO을 분리시켜 농축시키면 결정상의 MgSO4·nH2O을 수율 95% 이상으로 얻을 수 있다. 한편 반응 생성물을 물에서 습식 밀링하여 분쇄한 후 더운 물로 세척하면 반응성이 촉진되어 MgSO4·nH2O의 생성이 더욱 효과적이다.However, the reaction product produced by the SHS method is first washed with hot water to remove unreacted B 2 O 3 or other water-soluble impurities, and then dispersed in dilute sulfuric acid and stirred to promote reaction with MgO, and then sulfuric acid When the liquid phase MgO reacted with is separated and concentrated, MgSO 4 · nH 2 O in crystalline phase can be obtained in yield of 95% or more. On the other hand, when the reaction product is wet milled in water, pulverized and washed with hot water, the reactivity is promoted, and thus the production of MgSO 4 · nH 2 O is more effective.

상기 방법에 의하면 분리된 B4C의 XRD 분석에서는 MgO가 나타나지 않았다. 즉, 본 발명에 의하여 효과적으로 MgO을 분리시킬 수 있다. 뿐만 아니라 비료 성분으로 재활용이 가능한 MgSO4·nH2O을 얻을 수 있다.According to the method, MgO did not appear in the XRD analysis of the separated B 4 C. That is, MgO can be effectively separated by the present invention. In addition, MgSO 4 · nH 2 O can be obtained that can be recycled as a fertilizer.

이하 본 발명의 실시예는 다음과 같으며, 본 발명의 범의를 이에 제한하는 것은 아니다.Hereinafter, embodiments of the present invention are as follows, but the scope of the present invention is not limited thereto.

실시예 1Example 1

B2O3, C, Mg의 혼합물을 SHS방법으로 반응시켜 얻은 반응 생성물(150g)을 증류수에 분산시킨 후 교반 가열한 다음 가라 앉힌 후 윗물을 쏟아 버렸다. Buchner funnel과 거름 종이를 이용하여 걸른 필터케익(filter cake)을 온수로 두번 더 세척한 후, 물 150ml오 황산 45ml의 혼합 용액에 다시 분산시켰다. 거름종이를 이용하여 B4C을 분리하였고, 걸른 용액을 가열 농축하여 MgSO4·nH2O의 결정으로 회수하였다. 분리된 B4C 필터케익은 잔존하는 산을 제거하기 위해 증류수로 세척한 후 건조하여 23g의 B4C 분말을 얻었다. 이것의 XRD 분석 결과는 B4C와 일치하며, 미량의 C 피크가 나타났고, MgO 피크는 나타나지 않았다.The reaction product (150 g) obtained by reacting a mixture of B 2 O 3 , C, and Mg in the SHS method was dispersed in distilled water, stirred and heated, then settled, and the top water was poured out. The filter cake filtered using Buchner funnel and manure paper was washed twice with hot water, and then dispersed again in a mixed solution of 150 ml of water and 45 ml of sulfuric acid. B 4 C was isolated using a filter paper, and the filtered solution was concentrated by heating and recovered as crystals of MgSO 4 nH 2 O. The separated B 4 C filter cake was washed with distilled water to remove residual acid and dried to obtain 23 g of B 4 C powder. Its XRD analysis was consistent with B 4 C, with trace C peaks and no MgO peaks.

실시예 2Example 2

SHS에 의한 반응 생성물(713g)을 SiC(직경 10mm)와 증류수를 사용하여 2ℓ 용량의 폴리프로필렌 통에서 40분간 밀링한 후, 그 슬러리를 2ℓ짜리 비이커에 옮긴후 교반하여 가열한 다음, 거름종이를 이용하여 걸렀다. 뜨거운 물로 한 번 더 세척하였다. 이 필터케익을 물 1000ml와 황산 850mL의 혼합 용액 분산시킨 후 약 30분간 교반한 후 거름 종이를 이용하여 걸렀다. 걸른 용액을 가열 농축하여 MgSO4·nH2O을 결정으로 회수하였다. 필터케익은 잔존하는 산을 제거하기 위해 물로 서너번 세척한 후 건조하여 B4C(101g, 14.4%)을 얻었다.The reaction product (713 g) by SHS was milled in a 2 L polypropylene barrel for 40 minutes using SiC (diameter 10 mm) and distilled water, then the slurry was transferred to a 2 L beaker, stirred and heated, and then the filter paper was removed. Filtered by. Washed once more with hot water. The filter cake was dispersed with a mixed solution of 1000 ml of water and 850 mL of sulfuric acid, stirred for about 30 minutes, and filtered using a filter paper. The filtered solution was concentrated by heating to recover MgSO 4 nH 2 O as crystals. The filter cake was washed three or four times with water to remove the residual acid and dried to obtain B 4 C (101 g, 14.4%).

비교예 1Comparative Example 1

SHS에 의한 반응 생성물(50g)을 황산 15ml와 증류수 50ml의 혼합용액에 분산한 후 2시간 동안 교반한 후 거름 종이를 이용하여 걸렀다. 걸른 용액을 농축 가열하였으나 결정은 생성되지 않았고, 끈끈한 액체가 되었다. 필터케익을 물로 세척한 후 건조하여 XRD분석을 조사한 결과 MgO가 많이 남아 있음을 발견하였다.The reaction product (50 g) by SHS was dispersed in a mixed solution of 15 ml of sulfuric acid and 50 ml of distilled water, stirred for 2 hours, and filtered using a filter paper. The filtered solution was concentrated to heat, but no crystals formed, resulting in a sticky liquid. After washing the filter cake with water and drying it, XRD analysis showed that much MgO remained.

본 발명에 의하면 비교적 간단한 공정에 의하여, 자전 고온 반응 합성법에 의해 B2O3, C, Mg의 혼합물로 부터 B4C 분말을 제조할 때 동반되는 과량의 MgO로부터 비료 성분인 결정상의 MgSO4을 얻을 수 있어 자원 재활용이 가능하고, 종래의 MgO 처리 방법인 폐산 처리에서 발생되는 환경 오염을 방지할 수 있게 된다.According to the present invention, by the relatively simple process, MgSO 4 as a fertilizer component is obtained from an excess of MgO accompanying the preparation of B 4 C powder from a mixture of B 2 O 3 , C, and Mg by a rotating high temperature reaction synthesis method. As a result, it is possible to recycle resources and to prevent environmental pollution from waste acid treatment, which is a conventional MgO treatment method.

Claims (4)

B4C분말을 B2O3와 탄소 분말에 Mg분말을 혼합하여 자전 고온반응 합성법에 의하여 제조함에 있어서, 반응 생성물을 증류수 또는 알콜로 세척하여 미반응 B2O3을 제거하고, 미반응 B2O3이 제거된 반응 생성물을 묽은 황산에 분산시킨 후 일정 시간 교반하여 미반응 Mg와 반응 생성물의 MgO를 황산과 반응시킨 후 필터로 B4C를 분리하고, B4C가 분리된 여과액을 농축시켜 결정상의 MgSO4·nH2O를 얻는 것으로 이루어지는 자전 고온반응 합성법에 의한 탄화붕소 분말 제조시 부산물 MgO의 환경 친화적 분리 방법.In preparing B 4 C powder by mixing Mg powder with B 2 O 3 and carbon powder by autogenous high temperature reaction method, the reaction product was washed with distilled water or alcohol to remove unreacted B 2 O 3 and unreacted B 2 O 3 a is dispersed in dilute the removed reaction product of sulfuric acid and then separating the B 4 C the MgO of the unreacted Mg and the reaction product was stirred for a while as a filter, then sulfuric acid and the reaction and, B 4 C the separated filtrate A method for environmentally friendly separation of by-product MgO in the preparation of boron carbide powder by the autogenous high-temperature reaction synthesis method comprising concentrating to obtain MgSO 4 · nH 2 O in a crystalline phase. 제 1 항에 있어서, 상기 세척 단계에서 증류수 또는 알콜의 온도는 50 ~ 100℃의 범위인 자전 고온반응 합성법에 의한 탄화붕소 분말 제조시 부산물 MgO의 환경 친화적 분리 방법.The method of claim 1, wherein the temperature of the distilled water or alcohol in the washing step ranges from 50 to 100 ° C. 제 1 항에 있어서, 상기 황산은 2∼5배로 희석시킨 것을 사용하는 자전 고온반응 합성법에 의한 탄화붕소 분말 제조시 부산물 MgO의 환경 친화적 분리 방법.The method of claim 1, wherein the sulfuric acid is 2 to 5 times diluted by the method of environmentally friendly separation of by-product MgO in the preparation of boron carbide powder by a high-temperature reaction synthesis method. 제 1 항에 있어서, 상기 반응 생성물을 증류수 또는 알콜로 세척하는 단계 전에 반응 생성물을 물에서 습식 밀링하는 단계를 추가적으로 포함하는 자전 고온반응합성법에 의한 탄화붕소 분말 제조시 부산물 MgO의 환경 친화적 분리 방법.The method of claim 1, further comprising wet milling the reaction product in water prior to washing the reaction product with distilled water or alcohol.
KR19990043290A 1999-10-07 1999-10-07 METHOD OF REMOVAL OF MgO AS CRYSTALLINE MgSO4·nH2O FROM THE REACTION PRODUCT MIXTURE OF B4C, MgO AND B2O3 BY SHS KR100333497B1 (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007027053A1 (en) * 2005-08-30 2007-03-08 Lg Chem. Ltd. Gathering method and apparatus of powder separated soluble component
KR20220083039A (en) * 2020-12-11 2022-06-20 한국세라믹기술원 Manufacturing method of needle-typed magnesium sulfate compound using magnesium oxide

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007027053A1 (en) * 2005-08-30 2007-03-08 Lg Chem. Ltd. Gathering method and apparatus of powder separated soluble component
US7799236B2 (en) 2005-08-30 2010-09-21 Lg Chem, Ltd. Gathering method and apparatus of powder separated soluble component
KR20220083039A (en) * 2020-12-11 2022-06-20 한국세라믹기술원 Manufacturing method of needle-typed magnesium sulfate compound using magnesium oxide
KR102451364B1 (en) * 2020-12-11 2022-10-06 한국세라믹기술원 Manufacturing method of needle-typed magnesium sulfate compound using magnesium oxide

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