KR100915936B1 - Manufacturing method for zeolite - Google Patents

Manufacturing method for zeolite Download PDF

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KR100915936B1
KR100915936B1 KR1020090045886A KR20090045886A KR100915936B1 KR 100915936 B1 KR100915936 B1 KR 100915936B1 KR 1020090045886 A KR1020090045886 A KR 1020090045886A KR 20090045886 A KR20090045886 A KR 20090045886A KR 100915936 B1 KR100915936 B1 KR 100915936B1
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zeolite
reactor
reaction
adjusting
water
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김복용
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주식회사 지오테크
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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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
    • B01J20/3231—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the coating or impregnating layer
    • B01J20/3234—Inorganic material layers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • 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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • 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
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing

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  • Silicates, Zeolites, And Molecular Sieves (AREA)
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Abstract

A manufacturing method of active adsorbent zeolite is provided to absorb and remove an alkaline catalyst, non-reactive organic acid, remaining catalysts and by-products easily, and to increase solid content of the zeolite. A manufacturing method of active adsorbent zeolite includes the following steps of: maintaining reaction temperature of 15 ~ 25°C while adjusting mixing speed of a reactor to 4 ~ 6RPM(S11); adjusting pH by dissolving solid aluminum sulfate for 30 ~ 60 minutes after adding the solid aluminum sulfate 120 ~ 150g(S12); reacting diluted liquid for 1 ~ 2 hours after mixing sodium silicate and water with the aluminum sulfate(S13); and manufacturing the zeolite after pulverizing a dried material and drying a filtered material in a drying machine at temperature of 200 ~ 400°C(S14).

Description

활성흡착제 제올라이트 제조방법{Manufacturing method for Zeolite}Activating adsorbent zeolite manufacturing method {Manufacturing method for Zeolite}

본 발명은 활성흡착제 제올라이트 제조방법에 관한 것으로, 더욱 세부적으로는 상온반응에서의 제올라이트를 제조하는 활성흡착제 제올라이트 제조방법에 관한 것이다.The present invention relates to a method for preparing an active adsorbent zeolite, and more particularly to a method for preparing an active adsorbent zeolite for producing a zeolite in a room temperature reaction.

제올라이트는 나트륨, 칼륨의 알카리금속과 칼슘 등의 알카리토금속을 함유하고, 결정수를 함유한 알루미늄의 규산염 광물이며, 그 종류는 매우 많으나 보편적으로 분포하는 것은 클리놉틸롤라이트와 모우더나이트의 2종류가 있다.Zeolite contains alkali metals such as sodium and potassium and alkaline earth metals such as calcium, and is a silicate mineral of aluminum containing crystal water. There are many kinds, but two kinds of clinoptilolite and mordenite are widely distributed. There is.

천연 제올라이트의 생성조건과 환경의 해석은 광물학자들에 의해서 시작되었으며, 제올라이트 합성의 연구는 1940년대에 들어서 산업응용의 목적에서 유니온카바이트사를 중심으로 합성실험이 성공적으로 수행되면서 본격화 되었고, 제올라이트의 반응은 일반적으로 200℃이하의 온도에서 수열합성 반응이 이루어진다.The analysis of the production conditions and the environment of natural zeolites was started by mineral scientists, and the study of zeolite synthesis began in the 1940's as the synthesis experiments were successfully carried out by Union Carbide Co., Ltd. for the purpose of industrial application. The reaction is generally carried out hydrothermal synthesis reaction at a temperature of 200 ℃ or less.

제올라이트는 SiO4와 AlO4 사면체로 이루어진 다공성알루미노실리케이트 결정(Alumino Silicate Crystal)이며, 즉 O-Si(Aal)-O 단위가6-링을 이루는 것을 기본단위로 하여 6링 8개와 12개 기공을 형성하고 있다.Zeolite is a porous aluminosilicate crystal composed of SiO 4 and AlO 4 tetrahedron, that is, 8-rings and 12 pores based on 6-ring of O-Si (Aal) -O unit. To form.

출발물질을 이용한 제올라이트의 합성법은 알루미노실리케이크젤을 원료로 사용하는 방법과, 천연의 규산염을 이용하는 방법으로 구분할 수 있는데, 제올라이트의 합성과정에서는 특별한 압력조건이 필요로 하지 않고, 낮은 온도에서 반응이 이루어지므로 비교적 쉽게 제올라이트가 생성된다.The synthesis of zeolite using starting materials can be divided into aluminosilicate gel as a raw material and natural silicate. The synthesis process of zeolite does not require special pressure conditions and reacts at low temperatures. This is done so that zeolites are produced relatively easily.

제올라이트의 합성원료는 알루민산소다, 규산소다 및 가성성분을 주원료로 하여 합성되며, 통상적으로 알루민산소다는 수산화 알루미늄을 가성소다에 용해하여 제조하고, 규산소다는 규사를 가성소다와 함께 고온고압에서 녹인 통상적인 2호 규산소다용액을 사용하거나, 고체 규산을 수열하에 녹인 3호 규산소다에 가성성분 50%의 가성소다를 희석하여 사용하게 된다.Synthetic raw materials of zeolite are synthesized using sodium aluminate, sodium silicate and caustic as the main raw materials.Sodium aluminate is prepared by dissolving aluminum hydroxide in caustic soda and sodium silicate together with caustic soda at high temperature and high pressure. Ordinary No. 2 sodium silicate solution is used, or 50% caustic soda is diluted with sodium silicate No. 3 in which solid silicic acid is dissolved under hydrothermal treatment.

제올라이트의 결정수는 일반구조수와는 달리 물분자로 존재하기 때문에 불석수라 하고, 가열에 따라 탈수하여 그 구조는 파괴되지 않고 물분자가 있던 곳을 그대로 해면구조 또는 기공으로 남아 수분이나 가스를 흡착하여 원상으로 복귀하는 특징이 있고, 그 용도는 흡착, 흡습, 양이온 교환성, 탈취 등의 이용이 점점 증가하고 있다.Since zeolite's crystal water exists as a water molecule, unlike ordinary structure water, it is called non-stone water and dehydrated by heating, and its structure is not destroyed, and the water molecule remains as a sponge structure or pores, adsorbing water or gas. The use of adsorption, hygroscopicity, cation exchangeability, deodorization, etc. is increasing.

제올라이트는 흡착제, 촉매 및 세제용 빌더로 사용되고 있는 물질로 비표면적이 넓고 균일한 세공을 갖고 있으며, 양이온 교환성과 흡착성이 강하고, 다공성이 있는 물질로 상업적으로 생산되고 있는 4A형 제올라이트의 경우 입자 크기가 2 ~ 3um로 흡착제나 촉매와 세제용 빌더 사용시에는 문제가 있지만, 입자의 크기가 미립화되면 비표면적의 증대와 이온교환 속도의 향상으로 빌더의 경우 흡유능력의 향상으로 고농축 세제의 제조가 가능하며, 흡착제의 경우에는 비표면적의 증대로 인하여 흡착능력을 최대로 향상시킬 수 있다.Zeolite is a material used as builders for adsorbents, catalysts and detergents. It has a large specific surface area and uniform pores, and has a particle size in the case of 4A type zeolite commercially produced as a porous material with strong cation exchange and adsorption. It is a problem when using builders for adsorbents, catalysts and detergents at 2 ~ 3um, but when the particle size is atomized, the builder can manufacture high-concentrated detergents by increasing specific surface area and improving ion exchange rate. In the case of the adsorbent, the adsorption capacity can be maximized due to the increase of the specific surface area.

제올라이트의 합성은 알카리하에서 합성되어 세척과정이 필수적이고, 세척과정에서 모액의 재사용 및 세척의 효율증대를 위하여 여과과정이 필수공정이며, 제올라이트의 입도가 미립화되면 여과속도가 늦어지거나 거의 여과가 되지 않는 등의 문제점이 있다.The synthesis of zeolite is synthesized under alkali, and the washing process is essential. In the washing process, the filtration process is an essential process for reusing the mother liquor and increasing the efficiency of washing.When the particle size of the zeolite is atomized, the filtration rate is slowed or hardly filtered. There is such a problem.

제올라이트의 반응인 수열합성반응은 밀폐용기내 80℃ ~ 200℃ 온도의 자기 발생 압력하에서 가열 교반으로 반응되며, 현재 국내의 폴리올 정제 제품은 전량 수입에 의존하고 있는 실정으로, 수입제품은 이온교환성과 흡착력이 떨어지고, 산이나 알카리의 흡착능력이 떨어지며, 폴리올 반응품의 미량이 잔존 촉매나 미반응 유기산이나 알카리성 촉매와 부생성물 등의 흡착제거가 불가능하다는 문제점이 있다.The hydrothermal synthesis reaction, which is a reaction of zeolite, is reacted by heating and stirring under a self-generating pressure of 80 ° C to 200 ° C in an airtight container. Currently, domestic polyol refined products are dependent on imports of all products. There is a problem that the adsorption power is poor, the adsorption capacity of acid or alkali is poor, and the trace amount of the polyol reactant is impossible to remove adsorption of remaining catalyst or unreacted organic acid or alkaline catalyst and by-products.

상술한 바와 같은 문제점을 해결하기 위하여, 본 발명에서는 상온에서의 제올라이트 제조 과정시 발생되는 여과세척 문제와 고온에서의 수열 합성반응 문제점을 개선하고, 제올라이트 합성과정에서 제올라이트의 고체 함량을 증가시키며, 반응기 크기 및 수열 합성에 필요한 에너지를 줄이고, 이온 교환성과 흡착력이 우수하며 그 입자가 다공질의 구조로써 표면적이 극대화되어 각종 산이나 알카리의 흡착능력 및 탈색능력이 뛰어나고, 활성탄이나 이온교환 수지만으로는 흡착제거가 불가능 하였던 미량의 잔존 촉매나 미반응 유기산이나 알카리성 촉매 및 부생성물의 흡착제거를 용이하게 할 수 있는 활성흡착제 제올라이트 제조방법을 제공하는데 목적이 있다.In order to solve the problems described above, the present invention improves the problem of filtration washing during the manufacturing process of zeolite at room temperature and hydrothermal synthesis reaction at high temperature, increases the solids content of zeolite in the process of zeolite synthesis, and Its size and energy required for hydrothermal synthesis are reduced, its ion exchangeability and adsorption power are excellent, and its particles have a porous structure that maximizes the surface area, so it is excellent in adsorption and decolorization ability of various acids and alkalis. It is an object of the present invention to provide a method for preparing an active adsorbent zeolite which can facilitate the adsorption and removal of trace amounts of residual catalysts or unreacted organic acids or alkaline catalysts and by-products that were impossible.

목적을 달성하기 위한 제조방법으로는 교반기가 있는 반응기에 물 2ℓ를 넣고, 반응기의 교반속도를 4 ~ 6RPM으로 조정하면서 15 ~ 25℃의 반응온도를 유지하는 제1단계와; 상기 반응기에 고체 황산알루미늄을 120 ~ 150g 첨가하고, 30분에서 1시간동안 용해시켜 PH를 3 ~ 5 사이로 조정하는 제2단계와; 상기 용해시킨 황산알루미늄에 규산소다와 물을 1:1 비율로 조정하여 희석시킨 용액을 투입하면서 반응을 조정하고, 반응기의 교반기를 작동시키면서 1 ~ 2시간동안 반응시키는 제3단계와; 반응이 종료된 반응액을 여과기를 통해 여과시키고, 여과된 물질을 건조기에서 200 ~ 400℃ 사이 온도로 건조시키고, 건조가 종료된 물질을 분쇄기로 분쇄하여 제 올라이트를 제조하는 제4단계를 포함한다.In order to achieve the object, the first step of maintaining the reaction temperature of 15 ~ 25 ℃ while putting 2 liter of water in the reactor with a stirrer, while adjusting the stirring speed of the reactor to 4 ~ 6RPM; Adding a solid aluminum sulfate to the reactor 120-150g, dissolving for 30 minutes at 1 hour to adjust the pH between 3 and 5; A third step of adjusting the reaction by adding a diluted solution of sodium silicate and water to the dissolved aluminum sulfate at a 1: 1 ratio, and reacting for 1 to 2 hours while operating a stirrer of the reactor; A fourth step of preparing a zeolite by filtering the reaction solution after the reaction is filtered through a filter, drying the filtered material to a temperature between 200 and 400 ° C. in a dryer, and grinding the finished material with a grinder. do.

본 발명의 다른 제조방법으로는 교반기가 있는 반응기에 물 2ℓ를 넣고, 반응기의 교반속도를 4 ~ 6RPM으로 조정하면서 15 ~ 25℃의 반응온도를 유지하는 제1단계와; 상기 반응기에 규조토를 300 ~ 500g 첨가하고, 30분에서 1시간동안 용해시켜 PH를 3 ~ 5 사이로 조정하는 제2단계와; 상기 용해시킨 규조토에 규산소다와 물을 1:1 비율로 조정하여 희석시킨 용액을 투입하면서 반응을 조정하고, 반응기의 교반기를 작동시키면서 1 ~ 2시간동안 반응시키는 제3단계와; 반응이 종료된 반응액을 여과기를 통해 여과시키고, 여과된 물질을 건조기에서 200 ~ 400℃ 사이 온도로 건조시키고, 건조가 종료된 물질을 분쇄기로 분쇄하여 제올라이트를 제조하는 제4단계를 포함한다.Another manufacturing method of the present invention comprises the first step of putting 2 liter of water in the reactor with a stirrer, while maintaining the reaction temperature of 15 ~ 25 ℃ while adjusting the stirring speed of the reactor to 4 ~ 6RPM; Adding a diatomaceous earth (300-500 g) to the reactor, and dissolving for 30 minutes at 1 hour to adjust the pH between 3 and 5; A third step of adjusting the reaction by adding a diluted solution of sodium silicate and water to the dissolved diatomaceous earth at a ratio of 1: 1 and operating the stirrer of the reactor for 1 to 2 hours; The fourth step of preparing the zeolite by filtration of the reaction solution is completed through a filter, drying the filtered material to a temperature between 200 ~ 400 ℃ in a dryer, and grinding the finished material by a pulverizer.

상기한 바와 같이, 본 발명은 상온에서의 제올라이트 제조 과정시 발생되는 여과세척 문제와 고온에서의 수열 합성반응 문제점을 개선하고, 제올라이트 합성과정에서 제올라이트의 고체 함량을 증가시키며, 반응기 크기 및 수열 합성에 필요한 에너지를 줄이고, 이온 교환성과 흡착력이 우수하며 그 입자가 다공질의 구조로써 표면적이 극대화되어 각종 산이나 알카리의 흡착능력 및 탈색능력이 뛰어나고, 활성탄이나 이온교환 수지만으로는 흡착제거가 불가능 하였던 미량의 잔존 촉매나 미반응 유기산이나 알카리성 촉매 및 부생성물의 흡착제거를 용이하게 하는 효과가 있다.As described above, the present invention improves the problem of filtration washing during the production of zeolite at room temperature and the problem of hydrothermal synthesis at high temperature, increases the solids content of zeolite in the process of zeolite synthesis, and improves reactor size and hydrothermal synthesis. Reduces the energy required, has excellent ion exchange and adsorption power, and its particles have a porous structure that maximizes the surface area, so it is excellent in adsorption and decolorization ability of various acids and alkalis, and trace residues that cannot be removed by active carbon or ion exchange resin alone. There is an effect that facilitates the adsorption and removal of catalysts, unreacted organic acids, alkaline catalysts and by-products.

도 1은 본 발명에 따른 활성흡착제 제올라이트 제조방법의 제1실시 예에 따른 순서도이고, 도 2는 본 발명에 따른 활성흡착제 제올라이트 제조방법의 제2실시 예에 따른 순서도이다.1 is a flow chart according to the first embodiment of the method for producing an active adsorbent zeolite according to the present invention, Figure 2 is a flow chart according to the second embodiment of the method for producing an active adsorbent zeolite according to the present invention.

이하, 도면을 참고로 활성흡착제 제올라이트 제조방법을 설명하면 다음과 같다.Hereinafter, an active adsorbent zeolite manufacturing method will be described with reference to the accompanying drawings.

도 1은 본 발명의 활성흡착제 제올라이트 제조방법의 제1실시 예에 따른 순서도로서, 교반기가 있는 반응기에 물 2ℓ를 넣고, 반응기의 교반속도를 4 ~ 6RPM으로 조정하면서 15 ~ 25℃의 반응온도를 유지하는 제1단계(S11)와, 상기 반응기에 고체 황산알루미늄을 120 ~ 150g 첨가하고, 30분에서 1시간동안 용해시켜 PH를 3 ~ 5 사이로 조정하는 제2단계(S12)와, 상기 용해시킨 황산알루미늄에 규산소다와 물을 1:1 비율로 조정하여 희석시킨 용액을 투입하면서 반응을 조정하고, 반응기의 교반기를 작동시키면서 1 ~ 2시간동안 반응시키는 제3단계(S13)와, 반응이 종료된 반응액을 여과기를 통해 여과시키고, 여과된 물질을 건조기에서 200 ~ 400℃ 사이 온도로 건조시키고, 건조가 종료된 물질을 분쇄기로 분쇄하여 제올라이트를 제조하는 제4단계(S14)로 구성된다.1 is a flow chart according to the first embodiment of the method for preparing the active adsorbent zeolite of the present invention, the reaction temperature of 15 ~ 25 ℃ while putting 2 liter of water in the reactor with a stirrer, while adjusting the stirring speed of the reactor to 4 ~ 6RPM Maintaining the first step (S11) and 120 to 150g of solid aluminum sulfate to the reactor, and dissolution for 30 minutes for 1 hour to adjust the pH between 3 and 5 (S12) and the dissolved The reaction was adjusted by adding a diluted solution of sodium silicate and water to aluminum sulfate in a 1: 1 ratio, and reacting for 1 to 2 hours while operating the stirrer of the reactor, and the reaction was completed. The reaction solution is filtered through a filter, and the filtered material is dried in a dryer at a temperature between 200 and 400 ° C., and the finished material is pulverized with a pulverizer to prepare a zeolite.

또한, 도 2는 본 발명의 활성흡착제 제올라이트 제조방법의 제2실시 예에 따른 순서도로서, 교반기가 있는 반응기에 물 2ℓ를 넣고, 반응기의 교반속도를 4 ~ 6RPM으로 조정하면서 15 ~ 25℃의 반응온도를 유지하는 제1단계(S21)와, 상기 반응기에 규조토를 300 ~ 500g 첨가하고, 30분에서 1시간동안 용해시켜 PH를 3 ~ 5 사이로 조정하는 제2단계(S22)와, 상기 용해시킨 규조토에 규산소다와 물을 1:1 비율 로 조정하여 희석시킨 용액을 투입하면서 반응을 조정하고, 반응기의 교반기를 작동시키면서 1 ~ 2시간동안 반응시키는 제3단계(S23)와, 반응이 종료된 반응액을 여과기를 통해 여과시키고, 여과된 물질을 건조기에서 200 ~ 400℃ 사이 온도로 건조시키고, 건조가 종료된 물질을 분쇄기로 분쇄하여 제올라이트를 제조하는 제4단계(S24)로 구성된다.In addition, Figure 2 is a flow chart according to a second embodiment of the active adsorbent zeolite manufacturing method of the present invention, 2 liters of water in the reactor with a stirrer, reaction of 15 ~ 25 ℃ while adjusting the stirring speed of the reactor to 4 ~ 6RPM The first step (S21) to maintain the temperature, 300 to 500g of diatomaceous earth is added to the reactor, and the second step (S22) to dissolve in 30 minutes for 1 hour to adjust the pH between 3 and 5, and the dissolved The third step (S23) of reacting for 1 to 2 hours while adjusting the reaction by adding a diluted solution by adjusting the sodium silicate and water to the diatomaceous earth in a 1: 1 ratio, and the reaction is completed The reaction solution is filtered through a filter, and the filtered material is dried in a dryer at a temperature between 200 and 400 ° C., and the finished material is pulverized with a pulverizer to prepare a zeolite in a fourth step (S24).

상기 제1단계에 있어, 반응기의 교반속도를 4 ~ 6RPM으로 조정하면서 15 ~ 25℃의 온도에서 반응시키는 것은 상기와 같은 조건하에서의 반응시 결정구조를 극대화 시킬 수 있으며, 상기 제4단계 있어, 반응된 침전물을 여과기로 여과하여 케이크 상태로 생성된 물질을 성형기로 구상으로 성형시킨 다음 그 구상품을 건조기에서 건조시키되, 건조온도를 200 ~ 400℃ 사이로 하는 이유는 건조기의 온도가 500℃이상이면 제품의 구조가 파괴되는 현상이 발생되어 그 성능이 저하되는 문제점이 발생될 수 있기 때문이다.In the first step, the reaction at a temperature of 15 ~ 25 ℃ while adjusting the stirring speed of the reactor to 4 ~ 6RPM can maximize the crystal structure during the reaction under the above conditions, there is the fourth step, the reaction The precipitate formed is filtered through a filter to form a cake-like material into a sphere, and then the spherical product is dried in a dryer, but the drying temperature is between 200 and 400 ° C. This is because a phenomenon in which the structure of the structure is destroyed may cause a problem in that its performance is degraded.

상기 건조가 완료된 제품을 분쇄기로 분쇄작업을 하여 분말상태로 하며, 이때 제품의 상태는 입자가 균일하고, 입자의 크기가 일정하며, 다공성을 이루어 흡착력이 우수하다.The dried product is pulverized by a pulverizer to a powder state, wherein the state of the product is uniform, the size of the particles is uniform, and excellent porosity.

하기의 표는 본 발명의 제올라이트와 일반적으로 사용되는 실라카젤의 흡습율을 비교한 것으로, 본 발명에 의해 제조된 제올라이트가 우수한 흡습율을 나타냄을 알 수 있다.The following table compares the moisture absorption of the zeolite of the present invention and the silica gel generally used, and it can be seen that the zeolite prepared by the present invention shows excellent moisture absorption.

- 본 발명의 제올라이트와 실라카젤의 흡수율을 비교한 표.-Table comparing the absorption of zeolite and silica gel of the present invention.

시험항목Test Items 단위unit 본 발명의 제올라이트Zeolite of the Invention 실리카젤 A형Silica Gel Type A 실라카젤 B형Silacagel Type B 흡습률(상대습도20%)Hygroscopicity (relative humidity 20%) %% 11.1411.14 8.0 8.0 3.0 3.0 흡습률(상대습도50%)Hygroscopicity (relative humidity 50%) %% 26.3726.37 20.020.0 10.010.0 흡습률(상대습도90%)Hygroscopicity (relative humidity 90%) %% 66.7066.70 30.030.0 50.050.0

따라서, 본 발명에 의해 제조되는 활성흡착제 제올라이트는 흡수제, 이온교환제로서 사용되고, 구조에 따른 세공의 크기가 분자크기의 범위이며, 제올라이트 종류와 포함하는 양이온에 따라 세공의 크기가 다르므로 분자체로서 사용되어 혼합물에서의 선택적 흡착 또는 분리에 사용되고, 결정내부에 포함되는 양이온의 성질과 결정구조의 독특한 성질이 있으며, 그 용도는 수처리제, 탈취제, 항균 및 살균제, 유기물 흡착제, 수분 흡착제, 공기 분리제 등의 넓은 용도로 사용된다.Therefore, the active adsorbent zeolite prepared according to the present invention is used as an absorbent and an ion exchanger, and the pore size according to the structure is in the range of molecular size, and the pore size varies depending on the type of zeolite and the cations included. It is used for selective adsorption or separation in a mixture, and has the unique properties of the cation and crystal structure contained in the crystal, its use is water treatment agent, deodorant, antibacterial and bactericide, organic adsorbent, moisture adsorbent, air separator, etc. Used for a wide range of applications.

본 발명은 특정의 실시 예와 관련하여 도시 및 설명하였지만, 첨부된 특허청구범위에 의해 나타난 발명의 사상 및 영역으로부터 벗어나지 않는 한도 내에서 다양한 개조 및 변화가 가능하다는 것을 당업계에서 통상의 지식을 가진 자라면 누구나 쉽게 알 수 있을 것이다.While the invention has been shown and described with respect to particular embodiments, it will be apparent to those skilled in the art that various modifications and variations can be made without departing from the spirit and scope of the invention as set forth in the appended claims. Anyone can grow up easily.

도 1은 본 발명에 따른 활성흡착제 제올라이트 제조방법의 제1실시 예에 따른 순서도.1 is a flow chart according to the first embodiment of the method for preparing an active adsorbent zeolite according to the present invention.

도 2는 본 발명에 따른 활성흡착제 제올라이트 제조방법의 제2실시 예에 따른 순서도.Figure 2 is a flow chart according to a second embodiment of the active adsorbent zeolite manufacturing method according to the present invention.

Claims (2)

활성흡착제 제올라이트 제조방법에 있어서,In the active adsorbent zeolite manufacturing method, 교반기가 있는 반응기에 물 2ℓ를 넣고, 반응기의 교반속도를 4 ~ 6RPM으로 조정하면서 15 ~ 25℃의 반응온도를 유지하는 제1단계(S11)와;Putting 1 liter of water into the reactor with a stirrer, and adjusting the stirring speed of the reactor to 4 to 6 RPM and maintaining a reaction temperature of 15 to 25 ° C. (S11); 상기 반응기에 고체 황산알루미늄을 120 ~ 150g 첨가하고, 30분에서 1시간동안 용해시켜 PH를 3 ~ 5 사이로 조정하는 제2단계(S12)와;120 to 150 g of solid aluminum sulfate is added to the reactor, and a second step (S12) of dissolving at 30 minutes for 1 hour to adjust the pH to 3 to 5; 상기 용해시킨 황산알루미늄에 규산소다와 물을 1:1 비율로 조정하여 희석시킨 용액을 투입하면서 반응을 조정하고, 반응기의 교반기를 작동시키면서 1 ~ 2시간동안 반응시키는 제3단계(S13)와;A third step (S13) of adjusting the reaction by adding a diluted solution of sodium silicate and water to the dissolved aluminum sulfate at a ratio of 1: 1 and operating a stirrer of the reactor; 반응이 종료된 반응액을 여과기를 통해 여과시키고, 여과된 물질을 건조기에서 200 ~ 400℃ 사이 온도로 건조시키고, 건조가 종료된 물질을 분쇄기로 분쇄하여 제올라이트를 제조하는 제4단계(S14)를 포함하는 것을 특징으로 하는 활성흡착제 제올라이트 제조방법.After the reaction is completed, the reaction solution is filtered through a filter, the filtered material is dried at a temperature between 200 and 400 ° C. in a dryer, and the dried material is pulverized with a grinder to prepare a zeolite (S14). Active adsorbent zeolite production method comprising a. 활성흡착제 제올라이트 제조방법에 있어서,In the active adsorbent zeolite manufacturing method, 교반기가 있는 반응기에 물 2ℓ를 넣고, 반응기의 교반속도를 4 ~ 6RPM으로 조정하면서 15 ~ 25℃의 반응온도를 유지하는 제1단계(S21)와;Putting 1 liter of water into the reactor with a stirrer, and adjusting the stirring speed of the reactor to 4 to 6 RPM and maintaining a reaction temperature of 15 to 25 ° C. (S21); 상기 반응기에 규조토를 300 ~ 500g 첨가하고, 30분에서 1시간동안 용해시켜 PH를 3 ~ 5 사이로 조정하는 제2단계(S22)와;Adding a diatomaceous earth to 300 to 500g in the reactor, dissolving for 30 minutes at 1 hour to adjust the pH between 3 and 5 (S22); 상기 용해시킨 규조토에 규산소다와 물을 1:1 비율로 조정하여 희석시킨 용액을 투입하면서 반응을 조정하고, 반응기의 교반기를 작동시키면서 1 ~ 2시간동안 반응시키는 제3단계(S23)와;A third step (S23) of adjusting the reaction while adding a diluted solution of sodium silicate and water to the dissolved diatomaceous earth at a ratio of 1: 1 and operating a stirrer of the reactor; 반응이 종료된 반응액을 여과기를 통해 여과시키고, 여과된 물질을 건조기에서 200 ~ 400℃ 사이 온도로 건조시키고, 건조가 종료된 물질을 분쇄기로 분쇄하여 제올라이트를 제조하는 제4단계(S24)를 포함하는 것을 특징으로 하는 활성흡착제 제올라이트 제조방법.After the reaction is completed, the reaction solution is filtered through a filter, the filtered material is dried at a temperature between 200 and 400 ° C. in a dryer, and the dried material is pulverized with a grinder to prepare a zeolite (S24). Active adsorbent zeolite production method comprising a.
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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10167719A (en) 1996-12-17 1998-06-23 Tosoh Corp Production of thin film-like zeolite having no substrate
KR20000006090A (en) * 1998-06-12 2000-01-25 헨미 데루오 Method of producing artificial zeolite
KR20060077938A (en) * 2004-12-30 2006-07-05 학교법인 서강대학교 Method for preparing long zeolite crystal with flat facets
KR20070020354A (en) * 2005-08-15 2007-02-21 차이나 페트로리움 앤드 케미컬 코포레이션 Process for producing binder-free ZSM-5 zeolite in small crystal size

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10167719A (en) 1996-12-17 1998-06-23 Tosoh Corp Production of thin film-like zeolite having no substrate
KR20000006090A (en) * 1998-06-12 2000-01-25 헨미 데루오 Method of producing artificial zeolite
KR20060077938A (en) * 2004-12-30 2006-07-05 학교법인 서강대학교 Method for preparing long zeolite crystal with flat facets
KR20070020354A (en) * 2005-08-15 2007-02-21 차이나 페트로리움 앤드 케미컬 코포레이션 Process for producing binder-free ZSM-5 zeolite in small crystal size

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