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KR100823119B1 - Manufacture method of synthesis adsorbent - Google Patents

Manufacture method of synthesis adsorbent Download PDF

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Publication number
KR100823119B1
KR100823119B1 KR1020060029356A KR20060029356A KR100823119B1 KR 100823119 B1 KR100823119 B1 KR 100823119B1 KR 1020060029356 A KR1020060029356 A KR 1020060029356A KR 20060029356 A KR20060029356 A KR 20060029356A KR 100823119 B1 KR100823119 B1 KR 100823119B1
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precipitate
adsorption
industrial water
synthetic adsorbent
mixing
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KR1020060029356A
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KR20070098111A (en
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김수용
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김수용
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
    • B01J20/02—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
    • B01J20/3021—Milling, crushing or grinding
    • 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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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

본 발명은 합성흡착제 제조방법에 관한 것으로, 그 구성은 (a) 용해조에 규산소다와 공업용수를 투입하여 1차 혼합하는 단계와, (b) 반응조에 수산화알루미늄과 가성소다와 공업용수를 투입하여 2차 혼합하는 단계와, (c) 상기 (a)단계와 (b)단계에서 생성된 생성물질들을 상호 반응시키는 단계와, (d) 상기 (c)단계에서 생성된 침전물을 여과시키는 단계와, (e) 상기 여과를 거친 침전물을 구상으로 성형시키는 단계와, (f) 상기 구상으로 성형된 침전물을 건조시키는 단계와, (g) 상기 건조된 침전물을 분쇄시키는 단계를 포함하는 것을 특징으로 하는 것으로서, 그 단가가 저렴하며, 이온교환성과 흡착력이 매우 우수하며, 그 입자가 다공질의 구조로써 표면적이 극대화되어 각종 산이나 알카리의 흡착능력과 탈색능력이 뛰어나며, 종래 활성탄이나 이온교환수지만으로는 흡착제거가 불가능했던 미량의 잔존촉매나 미반응유기산이나 알카리성촉매나 부생성물 등의 흡착제거를 용이하게 할 수 있는 효과가 있다.The present invention relates to a method for preparing a synthetic adsorbent, the composition of which comprises (a) adding sodium silicate and industrial water to a dissolution tank for the first mixing, and (b) adding aluminum hydroxide, caustic soda and industrial water to the reaction tank. Performing a second mixing, (c) reacting the products produced in steps (a) and (b) with each other, (d) filtering the precipitate produced in step (c), (e) forming the filtered precipitate into a globular form, (f) drying the spherically shaped precipitate, and (g) pulverizing the dried precipitate. Its price is low, its ion exchangeability and adsorption power are very good. The porous structure of the particles maximizes the surface area, so it is excellent in adsorption capacity and discoloration ability of various acids and alkalis. Alone is effective to facilitate the removal of such traces of residual adsorption catalyst, unreacted organic acid or alkali catalyst, by-products that are not removed by adsorption.

Description

합성흡착제 제조방법{Manufacture method of synthesis adsorbent}Manufacture method of synthesis adsorbent

본 발명은 흡착제 제조방법에 관한 것으로, 더욱 상세하게는 합성흡착제 제조방법에 관한 것이다.The present invention relates to a method for producing an adsorbent, and more particularly, to a method for preparing a synthetic adsorbent.

산업이 다양화, 고도화됨에 따라 발생하는 공업배기가스나 산업폐수 등 각 분야에서 발생하는 환경오염물질의 발생을 최소화하기 위하여 활성탄이나 이온교환수지 등의 흡착제가 사용되고 있다. Adsorbents such as activated carbon and ion exchange resins are used to minimize the generation of environmental pollutants generated in various fields such as industrial exhaust gas and industrial wastewater generated as the industry diversifies and advances.

특히, 국내 수많은 폴리올 생산 공장에서는 폴리올 촉매인 칼륨(K+)이온을 물리적 흡착을 통하여 제거하기 위하여 마그네솔을 투입하고 있는데, 이는 전량 수입에 의존함으로써 그 단가가 고가라는 문제점이 있었다. In particular, many polyol production plants in Korea are putting a magnetic sol in order to remove the potassium (K +) ions as a polyol catalyst through physical adsorption, which has a problem that the unit price is expensive by relying on the total amount of imports.

또한, 상기 종래의 흡착제는 이온 교환성과 흡착력이 저조하여 산이나 알카리의 흡착능력이 떨어지며, 특히 알카리의 흡착능력은 상대적으로 더욱 떨어진다는 문제점이 있었다.In addition, the conventional adsorbent is poor in the ion exchangeability and adsorptivity, so that the adsorption capacity of the acid or alkali is poor, in particular, there is a problem that the adsorption capacity of the alkali is relatively lower.

또한, 종래의 흡착제로는 미량의 잔존촉매나 미반응유기산이나 알카리성촉매나 부생성물 등의 흡착제거가 불가능하다는 문제점이 있었다.In addition, the conventional adsorbent has a problem that it is impossible to remove and adsorb a small amount of residual catalyst, an unreacted organic acid, an alkaline catalyst, or a by-product.

본 발명은 상기한 바와 같은 제반 문제점을 해결하기 위하여 제안된 것으로, 그 목적은 그 단가가 저렴하며, 이온교환성과 흡착력이 매우 우수하며, 그 입자가 다공질의 구조로써 표면적이 극대화되어 각종 산이나 알카리의 흡착능력과 탈색능력이 뛰어나며, 종래 활성탄이나 이온교환수지만으로는 흡착제거가 불가능했던 미량의 잔존촉매나 미반응유기산이나 알카리성촉매나 부생성물 등의 흡착제거를 용이하게 할 수 있는 합성흡착제 제조방법을 제공함에 있다.The present invention has been proposed in order to solve the above problems, the object of which is low cost, excellent ion exchange and adsorptive power, the surface of the particles with a porous structure to maximize the surface area of various acids or alkali It has excellent adsorption capacity and discoloration ability, and it is possible to manufacture synthetic adsorbent which can easily remove adsorption of trace amount of remaining catalyst, unreacted organic acid, alkaline catalyst or by-product, which was not able to be removed by conventional activated carbon or ion exchange resin alone. In providing.

상기와 같은 목적을 달성하기 위한 본 발명에 따른 합성흡착제 제조방법은 (a) 용해조에 규산소다와 공업용수를 투입하여 1차 혼합하는 단계와, (b) 반응조에 수산화알루미늄과 가성소다와 공업용수를 투입하여 2차 혼합하는 단계와, (c) 상기 (a)단계와 (b)단계에서 생성된 생성물질들을 상호 반응시키는 단계와, (d) 상기 (c)단계에서 생성된 침전물을 여과시키는 단계와, (e) 상기 여과를 거친 침전물을 구상으로 성형시키는 단계와, (f) 상기 구상으로 성형된 침전물을 건조시키는 단계와, (g) 상기 건조된 침전물을 분쇄시키는 단계를 포함하는 것을 특징으로 한다. Synthetic adsorbent manufacturing method according to the present invention for achieving the above object comprises the steps of (a) adding sodium silicate and industrial water to the dissolution tank and mixing first, (b) aluminum hydroxide and caustic soda and industrial water in the reaction tank Adding a second mixture, (c) reacting the products produced in the steps (a) and (b) with each other, and (d) filtering the precipitate produced in the step (c). And (e) forming the filtered precipitate into a globular form, (f) drying the spherically shaped precipitate, and (g) pulverizing the dried precipitate. It is done.

또한, 본 발명에 따른 합성흡착제 제조방법의 상기 (c)단계는, 저온가수분해를 위하여 온도 15 ℃ 내지 25 ℃에서 반응되는 것을 특징으로 한다. In addition, the step (c) of the method for preparing a synthetic adsorbent according to the present invention is characterized in that the reaction at a temperature of 15 ℃ to 25 ℃ for low temperature hydrolysis.

또한, 본 발명에 따른 합성흡착제 제조방법의 상기 (f)단계는, 구조파괴현상을 막기 위하여, 온도 200 ℃ 내지 350 ℃에서 건조되는 것을 특징으로 한다. In addition, the step (f) of the method for preparing a synthetic adsorbent according to the present invention is characterized in that the drying at a temperature of 200 ℃ to 350 ℃ to prevent structural breakdown.

이하, 본 발명의 바람직한 실시예에 따른 합성흡착제 제조방법을 더욱 상세히 설명한다.Hereinafter, a method for preparing a synthetic adsorbent according to a preferred embodiment of the present invention will be described in more detail.

먼저, 용해조에 규산소다와 공업용수를 투입하여 1차 혼합한다. First, sodium silicate and industrial water are put into a dissolution tank, and it mixes first.

이때의 반응식은 아래와 같다. The reaction formula at this time is as follows.

Na2SiO3(CONC) + H2O → Na2SiO3XH2O (묽은 규산소다) Na 2 SiO 3 (CONC) + H 2 O → Na 2 SiO 3 XH 2 O (dilute sodium silicate)

이 반응은 1차 혼합시 겔(Gel)화를 용이하게 하기 위해서 이루어진다. This reaction takes place to facilitate gelation during the first mixing.

이어서, 반응조에 수산화알루미늄과 가성소다와 공업용수를 투입하여 2차 혼합한다. Subsequently, aluminum hydroxide, caustic soda, and industrial water are added to the reactor, followed by secondary mixing.

이때의 반응식은 아래와 같다. The reaction formula at this time is as follows.

Al(OH)3 + NaOH + H2O → NaAlO4XH2O (알루민산소다) Al (OH) 3 + NaOH + H 2 O → NaAlO 4 XH 2 O (Sodium aluminate)

이어서, 1차 혼합에서 생성된 생성물질과 2차 혼합에서 생성된 생성물질을 상호 반응시킨다. 이 때의 반응식은 아래와 같다. Subsequently, the product produced in the first mixture and the product produced in the second mixture are reacted with each other. The reaction formula at this time is as follows.

NaAlO4XH2O + Na2SiO3XH2O → Na2OAl2O3SiO2XH2O + H2O NaAlO 4 XH 2 O + Na 2 SiO 3 XH 2 O → Na 2 OAl 2 O 3 SiO 2 XH 2 O + H 2 O

여기서 Na2OAl2O3SiO2XH2O 는 침전되어 침전물이 된다. 이 반응은 저온가수분해 반응으로 이루어지며, 그 온도는 15 ℃ 내지 25 ℃에서 이루어지는 것이 바람직하다. 또한 이 반응은 반응시 결정구조를 극대화시키기 위하여 이루어지는 것이다. Na 2 OAl 2 O 3 SiO 2 XH 2 O is precipitated to form a precipitate. This reaction is a low-temperature hydrolysis reaction, the temperature is preferably made at 15 ℃ to 25 ℃. This reaction is also performed to maximize the crystal structure during the reaction.

이어서, 상기 침전물을 여과시킨다. 이는 강제 압착식으로 여과시키며 작업시간을 단축하여 함수분을 최소화하기 위한 것이다. The precipitate is then filtered off. This is forcibly filtration and to minimize the water content by reducing the working time.

이어서 상기 여과를 거친 침전물을 구상으로 성형시킨다. The filtered precipitate is then shaped into spheres.

이어서 상기 구상으로 성형된 침전물을 건조시킨다. The precipitate shaped into the spheres is then dried.

이때의 건조온도가 500 ℃ 이상이면 구조가 파괴되는 현상이 발생되어 그 성 능이 저하된다. 따라서 본 실시예에서는 그 건조온도를 200 ℃ 내지 350 ℃로 하는 것이 바람직하다. At this time, if the drying temperature is 500 ° C. or more, a phenomenon occurs in which the structure is destroyed, and its performance is reduced. Therefore, in the present embodiment, the drying temperature is preferably set to 200 ° C to 350 ° C.

이어서 상기 건조된 침전물을 분쇄시킨다. The dried precipitate is then comminuted.

상술한 과정을 거치면 입자가 균일하고 여과성이 최적인 합성흡착제가 생성되는 것이다. Through the above-described process is to produce a synthetic adsorbent with uniform particles and optimal filterability.

이상에서와 같이 본 발명에 따른 합성흡착제 제조방법에 의하면, 그 단가가 저렴하며, 이온교환성과 흡착력이 매우 우수하며, 그 입자가 다공질의 구조로써 표면적이 극대화되어 각종 산이나 알카리의 흡착능력과 탈색능력이 뛰어나며, 종래 활성탄이나 이온교환수지만으로는 흡착제거가 불가능했던 미량의 잔존촉매나 미반응유기산이나 알카리성촉매나 부생성물 등의 흡착제거를 용이하게 할 수 있는 효과가 있다. As described above, according to the method for preparing a synthetic adsorbent according to the present invention, the unit price is low, the ion exchangeability and the adsorption power are very excellent, and the particles have a porous structure, which maximizes the surface area, and the adsorption capacity and discoloration of various acids or alkalis. It is excellent in the ability and can easily remove the adsorption of a small amount of remaining catalyst, unreacted organic acid, alkaline catalyst or by-products, etc. which was not previously adsorbed and removed only by activated carbon or ion exchange resin.

본 발명은 첨부된 도면에 도시된 실시예를 참고로 설명되었으나, 이는 예시적인 것이며, 당해 분야에서 통상의 지식을 가진 자라면 이로부터 다양한 변형 및 균등한 실시예가 가능하다는 점을 이해할 수 있을 것이다. 따라서 본 발명의 진정한 보호범위는 첨부된 청구범위에 의해서만 정해져야 할 것이다. Although the present invention has been described with reference to the embodiments shown in the accompanying drawings, it is intended to be illustrative, and those skilled in the art will understand that various modifications and equivalent embodiments are possible from this. Therefore, the true scope of protection of the present invention should be defined only by the appended claims.

Claims (3)

(a) 용해조에 규산소다와 공업용수를 투입하여 1차 혼합하는 단계;(a) firstly mixing sodium silicate and industrial water in a dissolution tank; (b) 반응조에 수산화알루미늄과 가성소다와 공업용수를 투입하여 2차 혼합하는 단계;(b) adding aluminum hydroxide, caustic soda and industrial water to the reactor for second mixing; (c) 상기 (a)단계와 (b)단계에서 생성된 생성물질들을 상호 반응시키는 단계;(c) reacting the products produced in steps (a) and (b) with each other; (d) 상기 (c)단계에서 생성된 침전물을 여과시키는 단계;(d) filtering the precipitate produced in step (c); (e) 상기 여과를 거친 침전물을 구상으로 성형시키는 단계;(e) forming the filtered precipitate into spheres; (f) 상기 구상으로 성형된 침전물을 건조시키는 단계;(f) drying the spherically shaped precipitate; (g) 상기 건조된 침전물을 분쇄시키는 단계;를 포함하는 것을 특징으로 하는 합성흡착제 제조방법.(g) pulverizing the dried precipitate; manufacturing method of a synthetic adsorbent comprising a. 제 1 항에 있어서, 상기 (c)단계는, The method of claim 1, wherein step (c) comprises: 저온가수분해를 위하여 온도 15 ℃ 내지 25 ℃에서 반응되는 것을 특징으로 하는 합성흡착제 제조방법.Method for producing a synthetic adsorbent, characterized in that the reaction at a temperature of 15 ℃ to 25 ℃ for low temperature hydrolysis. 제 1 항에 있어서, 상기 (f)단계는, The method of claim 1, wherein step (f) comprises: 구조파괴현상을 막기 위하여, 온도 200 ℃ 내지 350 ℃에서 건조되는 것을 특징으로 하는 합성흡착제 제조방법.Method of producing a synthetic adsorbent, characterized in that the drying at a temperature of 200 ℃ to 350 ℃ to prevent structural breakdown.
KR1020060029356A 2006-03-31 2006-03-31 Manufacture method of synthesis adsorbent KR100823119B1 (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR960010078B1 (en) * 1993-08-26 1996-07-25 박태영 Process for the preparation of x-type zeolite absorbent
KR960010897B1 (en) * 1993-08-05 1996-08-13 코스모산업주식회사 Process for preparing zeolite absorbent having an increased specific surface
KR100668203B1 (en) 2006-06-08 2007-01-11 학교법인 포항공과대학교 Absorbent for removing methanol in ethanol

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR960010897B1 (en) * 1993-08-05 1996-08-13 코스모산업주식회사 Process for preparing zeolite absorbent having an increased specific surface
KR960010078B1 (en) * 1993-08-26 1996-07-25 박태영 Process for the preparation of x-type zeolite absorbent
KR100668203B1 (en) 2006-06-08 2007-01-11 학교법인 포항공과대학교 Absorbent for removing methanol in ethanol

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