KR100596943B1 - Manufacturing method of multi-functional adsorbent which can simultaneously adsorb the ammonia, the phosphate and the organic materials - Google Patents

Manufacturing method of multi-functional adsorbent which can simultaneously adsorb the ammonia, the phosphate and the organic materials Download PDF

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KR100596943B1
KR100596943B1 KR1020040065610A KR20040065610A KR100596943B1 KR 100596943 B1 KR100596943 B1 KR 100596943B1 KR 1020040065610 A KR1020040065610 A KR 1020040065610A KR 20040065610 A KR20040065610 A KR 20040065610A KR 100596943 B1 KR100596943 B1 KR 100596943B1
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adsorbent
coal ash
precipitate
coal
lime
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KR20040085094A (en
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조헌영
서정목
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서정목
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3021—Milling, crushing or grinding
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
    • B29B9/00—Making granules
    • B29B9/12—Making granules characterised by structure or composition
    • B29B2009/125—Micropellets, microgranules, microparticles

Abstract

석탄 화력발전소에서 대량으로 발생되는 석탄재(SiO2 50∼56％, Al2O3 20∼32％, 미연탄소 3∼25％를 함유)를 주원료로 사용하여 다기능성 흡착제를 제조하는 방법을 특징으로 하며, 첫째로 석탄재를 오토클래이브에서 1∼5 M NaOH 수용액과 1∼3 M ZnCl2 혹은 Ca(OH)2로 100∼200℃에서 5∼24h 수열반응 처리하여 흡착제를 합성하고 미연탄소를 활성화 하는 공정, 두 번째로 합성된 흡착제 슬러리에 20∼50％ MgCl2 수용액이나 석회크림·석회 슬러리·석회유를 가하여 용액의 pH가 10∼12 정도가 되도록 중화 시켜서 음이온성을 나타내는 인산염들을 침전·회수 할 수 있는 기능을 부여하는 동시에 흡착제의 여과 특성을 개선시키는 공정을 특징으로 하는 석탄재로부터 다기능성 흡착제 제조방법.A method for producing a multifunctional adsorbent using coal ash (SiO 2 50-56%, Al 2 O 3 20-32%, unburned carbon 3-25%) as a main raw material produced in a coal-fired power plant Firstly, coal ash is treated with 1 ~ 5 M NaOH aqueous solution and 1 ~ 3 M ZnCl 2 or Ca (OH) 2 at 100 ~ 200 ℃ for 5 ~ 24h hydrothermal reaction in autoclave to synthesize adsorbent and activate unburned carbon. In the second process, 20-50% MgCl 2 aqueous solution, lime cream, lime slurry, or lime oil is added to the synthesized slurry to neutralize the solution to a pH of about 10 to 12 to precipitate and recover anionic phosphates. A method for producing a multifunctional adsorbent from coal ash, characterized in that the step of imparting a function capable of improving the filtration characteristics of the adsorbent.

다기능성 흡착제, 석탄재, 제올라이트, 활성탄, 인산염 침전제, 여과특성Multifunctional Adsorbent, Coal Ash, Zeolite, Activated Carbon, Phosphate Precipitant, Filtration Characteristics

Description

질소와 인 및 유기 화합물을 동시에 흡착 할 수 있는 다기능성 흡착제 제조방법{Manufacturing method of multi-functional adsorbent which can simultaneously adsorb the ammonia, the phosphate and the organic materials}Manufacturing method of multi-functional adsorbent which can simultaneously adsorb the ammonia, the phosphate and the organic materials}

본 발명은 이온교환성이 있는 제올라이트 기능과 유기물의 흡착 성능이 탁월한 활성탄 기능 및 인산이온 침전제 기능을 겸비한 다기능성 흡착제를 석탄재로부터 제조하는 방법에 관한 것이다.The present invention relates to a method for producing a multifunctional adsorbent having an activated carbon function having an ion exchangeable zeolite function, an excellent adsorption performance of an organic substance, and a phosphate ion precipitation agent function from coal ash.

하수 및 폐수 등의 처리에서 사용되는 흡착제로는 암모니아성 질소 흡착량이 큰 제올라이트와 유기물에 대한 흡착용량이 큰 활성탄이 지금까지 많이 사용되고 있으며, 올토 인산이온과 같은 음이온성 물질의 회수는 침전제를 사용하는 화학적인 방법이 쓰이고 있다.As adsorbents used in sewage and wastewater treatment, zeolites with large ammonia nitrogen adsorption and activated carbons with large adsorption capacities to organic materials have been used so far. Chemical methods are used.

이와 같이 지금까지 주로 사용되고 있는 흡착 제거제는 그 제법과 작용기구가 다르므로 각기 다른 방법으로 제조하여 사용되고 있다.As such, the adsorption removal agent mainly used until now is manufactured and used in different methods because the manufacturing method and the functional mechanism are different.

제올라이트는 SiO2와 Al2O3를 주성분으로 하는 다공성 물질로서, 그 기공의 크기를 마음대로 조절할 수 있으며 다양한 양이온들에 대한 교환성능이 뛰어 나므 로, 산업폐수 및 하수 처리 공정에서 각종 이온들의 흡착 및 회수에 많이 사용되고 있다.Zeolite is a porous material composed mainly of SiO 2 and Al 2 O 3 , and can control the size of pores at will and has excellent exchange performance for various cations. Therefore, the adsorption of various ions in industrial wastewater and sewage treatment It is widely used for recovery.

유기물의 흡착성능이 탁월한 활성탄은 석탄 ·야자각 ·나무 등과 같은 유기물질을 불완전 연소하여 만든 제품으로, 각종 냄새 및 색소는 물론 기체 및 액체상에서 비이온성으로 존재하는 각종 유기물질의 흡착 및 회수에 많이 사용되고 있다.Activated carbon with excellent adsorption performance of organic matter is a product made by incomplete combustion of organic materials such as coal, palm shell, wood, etc. It is used.

석탄 화력발전소에서 대량으로 발생되는 석탄재는 SiO2 50∼56％, Al2O3 20∼32％, 미연탄소 3∼25％를 함유하고 있으므로, 일찍이 미국·일본 등과 같은 선진국에서는 이들을 원료로 하여 다양한 종류의 제올라이트를 제조하여 사용하여 왔다.Coal ash, which is generated in large quantities in coal-fired power plants, contains 50-56% SiO 2, 20-32% Al 2 O 3 , and 3-25% unburned carbon. Kinds of zeolites have been prepared and used.

지금까지 석탄재를 원료로 하여 개발된 흡착제 제품들은 주로 석탄재 중에서 SiO2 성분과 Al2O3 성분을 제올라이트 원료로 활용하는데 초점이 맞추어져 있으므로, 석탄재를 주원료로 하여 제올라이트를 합성할 때 또는 합성한 후에 합성 제올라이트로부터 미연탄소분과 기타 불순물들을 분리하는 것이 어려워서 실용화에 많은 제약이 되었다.So far, the adsorbent products developed from coal ash are mainly focused on using SiO 2 and Al 2 O 3 as coal raw materials in coal ash, and when or after synthesizing zeolite using coal ash as a main raw material. It has been difficult to separate unburned carbon powder and other impurities from synthetic zeolites, which has placed many limitations on practical use.

이에 본 발명은 이온교환성에 있는 제올라이트 기능과 유기물의 흡착성능이 탁월한 활성탄 기능 및 인산이온 침전제 기능을 겸비한 다기능성 흡착제를 석탄재로부터 제조하는 방법에 관한 것으로, 석탄재의 주성분인 실리카와 알루미나를 NaOH 수용액과 ZnCl2 혹은 Ca(OH)2로 처리하여 흡착제를 합성하는 동시에 석탄재 중에 함유되어 있는 미연탄소를 활성화 하여 유기물의 흡착성능이 탁월한 활성탄 기능을 부여하며, 합성된 흡착제 슬러리에 MgCl2 용액을 처리하여 음이온성을 나타내는 인산염들을 강력하게 침전 회수 할 수 있는 다기능성 흡착제를 제조하는 방법을 제공하는데 그 목적이 있다.Accordingly, the present invention relates to a method for preparing a multifunctional adsorbent having an active carbon function and an phosphate ion precipitant function having a zeolite function of ion exchangeability and an organic matter adsorbing ability, from coal ash. ZnCl 2 or Ca (OH) at the same time to synthesize the adsorbent by treatment with 2 to enable the unburned carbon contained in the coal ash, and give an excellent adsorption performance of the organic material of activated carbon functionality, anion by treatment with MgCl 2 solution in the synthetic adsorbent slurry It is an object of the present invention to provide a method for preparing a multifunctional adsorbent capable of strongly sedimenting and recovering phosphates.

본 발명은 석탄재를 주원료로 사용하여 다기능성 흡착제를 제조하는 방법을 특징으로 하며, 크게 나누어서 석탄재의 주성분인 실리카와 알루미나 혹은 뮬라이트를 NaOH 수용액과 ZnCl2 혹은 Ca(OH)2로 처리하여 흡착제를 합성하고 미연탄소를 활성화 하는 공정, 두 번째로 합성된 흡착제를 MgCl2, CaO 등과 같은 화학 약품으로 처리하여 음이온성을 나타내는 인산염들을 강력하게 침전 회수 할 수 있는 기능을 부여하는 동시에 흡착제의 여과 특성을 개선시키는 공정, 세 번째로 다기능성 흡착제를 여과·건조 후 2차 분쇄하는 공정으로 이루어지는 것을 특징으로 하는 석탄재로부터 다기능성 흡착제 제조방법에 관한 것이다.The present invention is characterized by a method of producing a multifunctional adsorbent using coal ash as a main raw material, and is divided into silica and alumina or mullite, the main components of coal ash, by treating with NaOH aqueous solution and ZnCl 2 or Ca (OH) 2 to synthesize an adsorbent. Process of activating unburned carbon and treating the second synthesized adsorbent with chemicals such as MgCl 2 , CaO, etc., giving the ability to strongly precipitate and recover anionic phosphates and at the same time improve the filtration characteristics of the adsorbent. And a third step of crushing and drying the multifunctional adsorbent and then secondly grinding the multifunctional adsorbent.

첫째로, 제올라이트를 합성하고 미연탄소를 활성화하는 공정은, 석탄재를 오토클래이브에서 1∼5 M NaOH 수용액과 1∼3 M ZnCl2 또는 Ca(OH)2로 100∼200℃에서 5∼24h 수열반응 처리하여 석탄재로부터 실리카 성분과 알루미나 성분을 용출시키고 미연탄소를 활성화하는 단계, 20∼30℃에서 10∼24h 숙성시켜서 합성제올라이트를 포함한 침전물을 정출시키는 단계, 100℃에서 1∼5시간 동안 가열하여 석출된 침전물을 제올라이트 결정으로 결정화 하는 단계로 구성되며, 이러한 공정을 통하여 고품질의 흡착제가 얻어진다.First, the process of synthesizing zeolite and activating unburned carbon is carried out by hydrothermal coal ash in an autoclave with 1 to 5 M NaOH aqueous solution and 1 to 3 M ZnCl 2 or Ca (OH) 2 at 100 to 200 ° C. for 5 to 24 h. Reaction treatment to elute the silica component and alumina component from the coal ash and to activate the unburned carbon, aged 10 to 24h at 20-30 ℃ to crystallize a precipitate containing synthetic zeolite, heated at 100 ℃ for 1 to 5 hours It is composed of the step of crystallizing the precipitate precipitate with zeolite crystals, through this process a high quality adsorbent is obtained.

두 번째로 인산염을 침착·회수하는 기능과 흡착제의 여과 특성을 개선시키는 공정은, 첫 번째 공정에서 얻어진 흡착제 슬러리에 20∼50％ MgCl2 수용액이나 석회크림·석회 슬러리·석회유를 가하여 용액의 pH가 10∼12 정도가 되도록 중화 시키는 공정으로, 이 공정을 통하여 흡착제 슬러리는 정치 조작에 의해서 고-액 분리가 쉽게 일어나고, 여과 시에 미분에 의해서 여과지 혹은 여과포가 막히는 현상이 없이 슬러리의 여과 특성이 개선된다.Secondly, the process of depositing and recovering phosphate and improving the filtration characteristics of the adsorbent is performed by adding 20-50% MgCl 2 aqueous solution, lime cream, lime slurry, or lime oil to the adsorbent slurry obtained in the first process. In this process, the adsorbent slurry is easily solid-liquid separated by a stationary operation, and the filtration characteristics of the slurry are improved without any clogging of filter paper or filter cloth by fine powder during filtration. do.

세 번째로 다기능성 흡착제를 여과 ·건조 후 2차 분쇄하는 공정은, 흡착제의 여과 ·건조 공정에서 형성된 2차 응집체를 롤러밀 혹은 볼밀 등을 사용하여 일정한 크기의 입상 흡착제 또는 분말상 흡착제를 제조하는 공정으로 흡착제의 취급을 용이 하게할 수 있게 된다.Third, the second step of filtration and drying of the multifunctional adsorbent is to prepare granular adsorbents or powdery adsorbents of a constant size using a roller mill or a ball mill on the secondary aggregate formed in the filtration and drying process of the adsorbent. This can facilitate the handling of the adsorbent.

본 발명을 통하여 SiO2 50∼56％, Al2O3 20∼32％, 미연탄소 3∼25％가 함유된 석탄재로부터 다기능성 흡착제를 제조하여 각종 물성을 시험을 한 결과, 원래의 석탄재에 비하여 25 mg NH4 +-N/L 용액에서 NH4 +-N의 흡착용량이 4,000∼6,000 mg/100g 흡착제, 5 mg PO4 3--P 용액에서 P의 침착·제거 용량이 1,000∼2,000 mg/100g 흡착제, 12,700 mg I2/L 용액에서의 I2 흡착용량이 1,500∼2,000 mg I2/100g 흡착제, 1200 mg 메틸렌블루/L 용액에서의 메틸렌블루 흡착용량이 6,000∼8,000 mg 메틸렌블루/100g 흡착제 정도로 흡착·제거 효과가 증진된다.According to the present invention, a multifunctional adsorbent was prepared from coal ash containing 50 to 56% of SiO 2 , 20 to 32% of Al 2 O 3 , and 3 to 25% of unburned carbon, and tested various physical properties. Adsorption capacity of NH 4 + -N in 25 mg NH 4 + -N / L solution is 4,000-6,000 mg / 100g adsorbent, P deposition and removal capacity of P in 5 mg PO 4 3- -P solution is 1,000-2,000 mg / Adsorption capacity of I 2 in 100g adsorbent, 12,700 mg I 2 / L solution is 1,500-2,000 mg I 2 / 100g Adsorbent, methylene blue adsorption capacity of 1200 mg methylene blue / L solution 6,000-8,000 mg Methylene blue / 100g adsorbent Adsorption / removal effect is improved to such an extent.

Claims (1)

석탄 화력발전소에서 대량으로 발생되는 석탄재(SiO2 50∼56％, Al2O3 20∼32％, 미연탄소 3∼25％를 함유)를 주원료로 사용하여 다기능성 흡착제를 제조하는 방법에 있어서, 다음에서 제시하는 3 공정을 포함하는 것을 특징으로 하는 다기능성 흡착제 제조방법.In the method for producing a multifunctional adsorbent using a coal material (containing 50 to 56% of SiO 2 , 20 to 32% of Al 2 O 3 , 3 to 25% unburned carbon) generated in a coal-fired power plant as a main raw material, Versatile, characterized in that it comprises three processes presented below Method for preparing adsorbent. 제 1 공정은 석탄재를 오토클래이브에서 1∼5 M NaOH 수용액과 1∼3 M의 ZnCl2 또는 Ca(OH)2로 100∼200℃에서 5∼24h 수열반응 처리하여 석탄재로부터 실리카와 알루미나 성분을 용출시키고 미연탄소를 활성화하는 단계, 20∼30℃에서 10∼24h 숙성시켜서 합성제올라이트를 포함한 침전물을 정출시키는 단계, 100℃에서 1∼5시간 동안 가열하여 석출된 침전물을 제올라이트 결정으로 결정화 하는 단계로 구성된 흡착제 슬러리 제조공정.In the first step, the coal ash is hydrothermally reacted with 1 to 5 M NaOH aqueous solution and 1 to 3 M ZnCl 2 or Ca (OH) 2 at 100 to 200 ° C. in an autoclave to remove silica and alumina components from the coal ash. Eluting and activating unburned carbon, aging for 10 to 24 h at 20 to 30 ° C. to precipitate a precipitate containing synthetic zeolite, and heating the mixture to 100 ° C. for 1 to 5 hours to crystallize the precipitate to zeolite crystals. Configured adsorbent slurry manufacturing process. 제 2 공정은 제 1 공정에서 합성된 흡착제 슬러리에 20∼50％ MgCl2 용액이나 석회크림·석회슬러리·석회유를 가하여 용액의 pH가 10∼12 정도가 되도록 중화 시켜서 음이온성을 나타내는 인산염을 침전·회수 할 수 있는 기능을 부여하는 동시에 흡착제의 여과 특성을 개선시키는 공정.In the second step, 20-50% MgCl 2 solution, lime cream, lime slurry, and lime oil are added to the adsorbent slurry synthesized in the first step, and the solution is neutralized to a pH of about 10 to 12 to precipitate and phosphate showing anionicity. The process of improving the filtration characteristics of the adsorbent while at the same time giving a recoverable function. 제 3 공정은 제 2 공정의 여과·건조 과정에서 형성된 2차 응집체를 롤러밀 또는 볼밀을 사용하여 일정한 크기의 분말상 흡착제를 제조하는 공정.The third step is a step of producing a powdery adsorbent of a constant size using a roller mill or a ball mill on the secondary aggregate formed in the filtration and drying processes of the second process.
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