KR980009116A - Calcium Aluminum Chloride and Method for its Preparation - Google Patents
Calcium Aluminum Chloride and Method for its Preparation Download PDFInfo
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- KR980009116A KR980009116A KR1019960030191A KR19960030191A KR980009116A KR 980009116 A KR980009116 A KR 980009116A KR 1019960030191 A KR1019960030191 A KR 1019960030191A KR 19960030191 A KR19960030191 A KR 19960030191A KR 980009116 A KR980009116 A KR 980009116A
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- 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
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
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Abstract
본 발명은 고탁도, 저알칼리도 원수를 효과적으로 처리하는데 적합한 고염기도 알루미늄계 수처리용 응집제인 폴리염화알루미늄칼슘과 그의 제조방법에 관한 것이다. 본 응집제는 응집 성능 향상과 처리수의 pH 저하를 최소화 시킬 수 있는 신규의 처리용 응집제로서 하기의 일반식으로 표시된다.The present invention relates to a polychlorinated aluminum chloride as a coagulant for highly water-resistant aluminum-based water treatment suitable for effectively treating raw water with high turbidity and low alkalinity, and a process for producing the same. This flocculant is a new flocculant for treatment which can minimize the decrease in the pH of the treated water and the improvement of flocculation performance, and is represented by the following general formula.
[A1Cax(OH)yClz] (I)[AlCa x (OH) y Clz] (I)
상기 식에서 3 + 2x = y + z, x는 0.105x0.705, y는 1.5y2.7, z는 0.5z3 이다.In the above equation, 3 + 2x = y + z, x is 0.105 x 0.705, y is 1.5 y 2.7, z is 0.5 z 3.
상기 응집제를 고탁도의 원수를 대상으로 실험한 결과, 기존의 응집제보다 응집처리 후 알칼리도의 저하가 감소하였으며, 동시에 응집처리 효과는 상승하였다.When the coagulant was tested in raw water of high turbidity, the decrease in alkalinity was decreased after the coagulation treatment than that of the conventional coagulant, and at the same time, the coagulation treatment effect was increased.
Description
[발명의 명칭][Title of the Invention]
폴리염화알루미늄칼슘 및 그의 제조방법Calcium Aluminum Chloride and Method for its Preparation
[발명의 상세한 설명]DETAILED DESCRIPTION OF THE INVENTION [
[발명의 목적][Object of the invention]
본 발명은 신규한 폴리염화알루미늄칼슘(Poly Aluminum Calcium Chloride : 이하 PACC라 한다)과 그의 제조방법에 관한 것이다. 더욱 상세하게는 수처리제로서 응집성능이 우수한 신규의 폴리염화알루미늄 칼슘에 관한 것이다.The present invention relates to a novel polyaluminum calcium chloride (PACC) and a process for producing the same. More particularly, the present invention relates to a novel poly (aluminum chloride) calcium salt having excellent flocculation performance as a water treatment agent.
[발명이 속하는 기술분야 및 이분야의 종래 기술][Technical Field of the Invention and Prior Art in the Field]
지금까지 국내에서는 수처리용 응집제로서 황산반토(Alum), 폴리황산알루미늄실리케이트(Poly Alumin um Sulfate Silicate : 이하 PASS라 한다), 폴리염화알루미늄(Poly Aluminum Choride : 이하 PAC라 한다), 폴리염화알루미늄실리케이트(Poly Aluminum Choride Silicate : 이하 PACS라 한다) 등이 주로 사용되어 왔다. 그러나 황산반토(Alum)와 같은 단분자 응집제는 가격이 비교적 저렴하다는 이점은 있으나 무기고분자 응집제에 비해 응집효과가 낮고 처리후 처리수의 알칼리도와 pH저하가 크다는 단점이 있다.. 이러한 단점을 개선하기 위해서 개발된 것이 고분자 형태인 PASS, PAC, PACS와 같은 고분자 무기 응집제이다. 이들 응집제와 황산반토와의 가장 큰 차이점은 양이온의 전하량이며, 알루미늄 복합체의 양이온 전하가 주로 +7가로서 응집력이 +3가의 황산반토에 비해 상당히 향상된다는 것이다. 이러한 폴리며 형태 응집제의 특성은 큰 염기도(40∼55%)를 나타내는 것이다. 이 분야에서 응집제의 염기도(Basicity)는 다음과 같이 나타낸다.So far, domestic water treatment coagulants such as Alum, Poly Aluminum Sulfate Silicate (PASS), Poly Aluminum Choride (PAC) and Poly Poly Aluminum Choride Silicate (hereinafter referred to as PACS). However, monomolecular flocculants such as Alum sulfate have the advantages of relatively low cost, but they have a lower coagulation effect than the inorganic polymer flocculant and have a disadvantage in that the alkalinity and pH of the treated water are significantly lowered after the treatment. It is a polymer inorganic coagulant such as PASS, PAC, PACS which is developed in the form of polymer. The most significant difference between these flocculants and the sulfate is the charge of the cation, which is significantly improved compared to the sulfate of the sulfate of + 7 in the cohesive force of +7 and the cation charge of the aluminum complex. The characteristics of these polydentate type flocculants represent a high basicity (40 to 55%). The basicity of the flocculant in this field is as follows.
대개는 염기도가 클수록 응집 주요 성분의 분자량이 커지기 때문에 침전성능이 크게 개선되고 정수처리 후 소석회 사용량을 줄일 수 있는 장점이 있다. 그러나 현재까지는 응집제의 안정성 문제로 염기도가 55% 이상인 응집제가 시판되거나 알려진 예가 없는 실정이다.Generally, the larger the basicity, the greater the molecular weight of the major components of the coagulation, so the precipitation performance is greatly improved and the amount of calcium hydroxide after the water treatment can be reduced. However, up to now, there is no commercially available or known example of a flocculant having a basicity of 55% or more due to the stability problem of the flocculant.
여기에서 안정성이 깨어진다는 것은 응집제가 용액 상태를 유지하지 못하고 응집제 자체가 침전을 일으키는 것을 말한다. 특히, 고탁도이면서 저알칼리도인 원수를 처리할 때 기존의 응집제를 사용하면 실험실적 투입량보다 더 많은 응집제를 사용하게 되고, 결과적으로 처리수의 pH가 상당히 저하되어 상응하는 정도의 중화제를 사용하여야 한다. 특히 홍수철이 오는 6∼9월에 정수장에서 빈번이 있는 경우로 정수처리의 효율성을 떨어뜨리는 원인이 되고 있다. 응집제의 투입량이 증가하게 되면 경제적으로 손실이 따를뿐 아니라 응집처리 후 잔류 알루미늄의 농도가 증가하여 수질이 나빠지는 원인이 된다. 또한 잔류탁도의 증가로 인하여 여과지의 역세척 주기의 증가를 유발하여 세척수의 증가와 처리효율의 감소를 가져오게 된다.The breakdown of stability here means that the coagulant does not maintain the solution state and the coagulant itself precipitates. Especially, when the raw water having high turbidity and low alkalinity is used, the existing flocculant is used more than the experimented amount of flocculant, and as a result, the pH of the treated water is considerably lowered, so that a corresponding degree of neutralizing agent should be used . In particular, flood irrigation is frequent in the water purification plant from June to September, which causes the efficiency of the water treatment to deteriorate. If the amount of coagulant is increased, not only economical loss is caused but also the concentration of residual aluminum is increased after coagulation treatment, which causes deterioration of water quality. Also, due to the increase of the residual turbidity, the backwash cycle of the filter paper is increased, thereby increasing the washing water and reducing the treatment efficiency.
[발명이 이루고자한 기술적 과제][Technical Problems to be Solved by the Invention]
본 발명자들은 이러한 점들을 착안하여 수년간 다방면으로 연구한 결과, 기존의 응집제가 염기도가 약 55%만 되어도 불안정하여 침전하는 반면, 본 발명에서는 염기도가 90%까지 올라가도 안정하면서 응집력이 우수한 고염기도 응집제를 개발하기에 이르렀다.The inventors of the present invention have studied various aspects of these points for many years and found that the conventional coagulant is unstable and precipitates even when the basicity reaches about 55%. On the other hand, in the present invention, the high coagulant coagulant Development.
[발명의 구성 및 작용][Structure and operation of the invention]
폴리염화알루미늄과 석회석 또는 소석회를 적당한 반응 조건하에서 반응시켜 다음과 같은 일반식을 갖는 폴리염화알루미늄칼슘을 제조하였다.Poly (aluminum chloride) and limestone or slaked lime were reacted under suitable reaction conditions to prepare poly (aluminum chloride) chloride having the following general formula.
[A1Cax(OH)yClz] (I)[AlCa x (OH) y Clz] (I)
상기 식에서 3 + 2x = y + z, x는 0.105x0.705, y는 1.5y2.7, z는 0.5z3 이다.In the above equation, 3 + 2x = y + z, x is 0.105 x 0.705, y is 1.5 y 2.7, z is 0.5 z 3.
상기 폴리염화알루미늄칼슘은 Al이 2.5∼10.5 wt%, OH/Al의 몰비가 1.5∼2.7, Ca가 0.1∼8 wt%일 때 응집제로서 우수한 성능을 나타냈다. 본 응집제의 물리적 성질은 다음과 같다.The polychlorinated aluminum chloride exhibited excellent performance as a coagulant when Al was 2.5 to 10.5 wt%, the molar ratio of OH / Al was 1.5 to 2.7, and Ca was 0.1 to 8 wt%. The physical properties of the coagulant are as follows.
·형상 : 약간 노란색을 띄거나 무색인 투명한 액체이며 이를 건조시키면 하얀 분말 상태로 됨.· Shape: A transparent liquid with a little yellow color or colorless, and when dried, it becomes a white powder.
·비중 : Al2O3의 함량과 액체의 온도에 따라 다르나 1.2∼1.41 범위를 유지함.Specific gravity: It is in the range of 1.2 ~ 1.41 depending on the content of Al 2 O 3 and the temperature of the liquid.
· 용해도 : 물에 쉽게 용해됨.· Solubility: Easily soluble in water.
· 끓는점 : 100kpa에서 100℃· Boiling point: 100kpa to 100 ℃
· 결정화점 : 14% Al2O3제품의 경우 -20℃· Crystallization point: -20 ° C for 14% Al 2 O 3 product
상기의 특성을 가지는 폴리염화알루미늄칼슘은 폴리아크릴아마이드,폴리디메틸디에틸암모늄클로라이드와 같은 공지의 유기응집제와 혼합하여 사용할 경우 원수특성에 따라 처리효율을 더욱 향상시킬 수 있다.When the aluminum polychloride chloride having the above characteristics is mixed with a known organic coagulant such as polyacrylamide or polydimethyldiethylammonium chloride, the treatment efficiency can be further improved according to the raw water characteristics.
상기 폴리염화알루미늄칼슘의 제조방법은 하기와 같다. 먼저 수산화알루미늄을 염산과 혼합한 후 고온·고압에서 반응시켜 폴리염화알루미늄 용액을 제조한 후 원하는 만큼의 염기도를 함유할 수 있도록 석회석이나 소석회를 첨가한다. 이때, 안정한 폴리염화알루미늄 용액을 제조하기 위해서는 적당량의 숙성시간이 필요하다. 이러한 폴리염화알루미늄칼슘의 제조방법에 있어 음이온 염인 염산의 약 20%정도를 황산,인산, 질산 등으로 교체하여 사용할 수도 있다.The production method of the above-described poly (aluminum chloride) calcium is as follows. First, aluminum hydroxide is mixed with hydrochloric acid and reacted at high temperature and high pressure to produce poly-aluminum chloride solution, and then limestone or lime is added so as to contain the desired basicity. At this time, an appropriate amount of aging time is required to produce a stable poly (aluminum chloride) solution. In the process for producing such aluminum polychlorinated calcium chloride, about 20% of the hydrochloric acid, which is an anion salt, may be replaced with sulfuric acid, phosphoric acid, nitric acid or the like.
상기 제조방법들에 있어서 고염기도를 갖는 응집제를 안정화시키고 응집능력을 향상시키는 한 방법으로 폴리아크릴아마이드(Poly Acrylamide : 이하 PAM 이라 한다.), 폴리디메틸디에틸암모늄클로라이드(Poly Dimethyl Diethyl Ammonium Chloride)등의 유기응집제를 0.01~0.2 wt% 정도 첨가하여 사용할 수도 있다Polyacrylamide (hereinafter referred to as "PAM"), polydimethyldiethyl ammonium chloride ("PAM") and the like may be used as a method for stabilizing a coagulant having high salt intolerance and improving cohesion ability in the above- Of organic coagulant may be added in an amount of 0.01 to 0.2 wt%
[실시예 1][Example 1]
분말상 수산화알루미늄 280g과 물400g을 혼합하여 수산화알루미늄 슬러리를 제조한다. 상기 슬러리에 염산 340g을 첨가하면서 승온시킨다. 60∼80。C에서 2∼3시간 교반하면서 숙성하여 염화알루미늄(AlCl3)용액과 미반응 수산화알루미늄의 혼합물로 제조한다. 한편 석회석분 148g에 물 355g을 혼합하여 석회석 슬러리를 제조한다.280 g of powdered aluminum hydroxide and 400 g of water were mixed to prepare an aluminum hydroxide slurry. 340 g of hydrochloric acid was added to the slurry and the temperature was raised. And aged at 60 to 80.C for 2 to 3 hours to prepare a mixture of aluminum chloride (AlCl 3 ) solution and unreacted aluminum hydroxide. On the other hand, 148 g of limestone is mixed with 355 g of water to prepare a limestone slurry.
염화알루미늄과 수산화알루미늄의 혼합물 슬러리를 먼저 반응기에 넣고, 여기에 상기의 석회석 슬러리를 서서히 첨가한다. 반응이 완전히 진행되기 위해서는 190C의 반응온도와 12 atm의 반응압력이 필요하다. 반응기의 온도를 190℃까지 상승시키면 내용물에 의한 압력은 9.5 atm이 된다. 나머지 2.5 atm은 반응시 생성되는 이산화탄소(CO2) 가스에 의한 분압으로 충분히 보충할 수 있다. 이러한 방법으로 폴리염화알루미늄칼슘을 제조한다. 분석결과 제품의 성분은 Al2O3가 10 wt%, Ca가 4.0 wt% 그리고 염기도가 85%이고, 다음의 화학식으로 표시되는 화합물임을 확인할 수 있었다.The slurry of the mixture of aluminum chloride and aluminum hydroxide is first added to the reactor, and the limestone slurry is gradually added thereto. A reaction temperature of 190C and a reaction pressure of 12 atm are required for the reaction to proceed fully. When the temperature of the reactor is increased to 190 ° C, the pressure due to the contents is 9.5 atm. The remaining 2.5 atm can be sufficiently replenished by the partial pressure of the carbon dioxide (CO 2 ) gas produced during the reaction. In this way, poly aluminum chloride is prepared. As a result of the analysis, it was confirmed that the components of the product were Al 2 O 3 of 10 wt%, Ca of 4.0 wt%, and basicity of 85%.
[AlCa0.52(OH)2.55Cl1.50][AlCa 0.52 (OH) 2.55 Cl 1.50 ]
상기 제조된 폴리염화알루미늄칼슘은 수화물 형태로 존재하게 되며 수처리시의 응집 실험 결과는 다음과 같다.The prepared poly (aluminum chloride) calcium was present in the form of hydrate, and the result of flocculation test at the time of water treatment is as follows.
※NTU : 용액중 현탁물질의 양(Nephelometric Turbidity Unit)※ NTU: Amount of suspended matter in solution (Nephelometric Turbidity Unit)
탁도의 측정은 ASTMD-1889-81의 방법에 따름. The measurement of turbidity is according to the method of ASTM D-1889-81.
※NTU : 용액중 현탁물질의 양(Nephelometric Turbidity Unit)※ NTU: Amount of suspended matter in solution (Nephelometric Turbidity Unit)
탁도의 측정은 ASTMD-1889-81의 방법에 따름. The measurement of turbidity is according to the method of ASTM D-1889-81.
PACC + PAM(1ppm) : PAM을 1ppm 혼합한 조성물. PACC + PAM (1 ppm): 1 ppm mixture of PAM.
[실시예 2][Example 2]
실시예 1에서 제조한 염화알루미늄과 미반응 수산화알루미늄의 혼합물을 578g 준비한다. 한편 소석회(CaO) 42.2g과 물 379.8g을 혼합하여 수산화칼슘을 제조한다. 상기 염화알루미늄과 수산화알루미늄의 혼합용액을 가열하면서 상기 소석회 슬러리를 아주 서서히 첨가하면서 고속혼합기(homogenizer)를 작동시켜준다. 고속혼합기를 이용함으로써 실시예 1의 반응조건을 완화할 수 있다. 반응 온도는 150℃이며, 반응 압력은 4.7 atm이다. 상기 조건 하에서 1000g의 폴리염화알루미늄칼슘을 제조할 수 있었으며, 이 제품의 성분은 Al2O310 wt%, Ca 3.2 wt%, 염기도 70%이고 다음의 화학식으로 표시되는 화합물임을 확인할 수 있었다.578 g of a mixture of aluminum chloride prepared in Example 1 and unreacted aluminum hydroxide was prepared. On the other hand, 42.2 g of calcium hydroxide (CaO) and 379.8 g of water are mixed to prepare calcium hydroxide. The slurry is slowly added while the mixed solution of aluminum chloride and aluminum hydroxide is heated, and a homogenizer is operated. The reaction conditions of Example 1 can be alleviated by using a high-speed mixer. The reaction temperature is 150 占 폚, and the reaction pressure is 4.7 atm. Under the above conditions, 1000 g of poly (aluminum chloride) chloride could be produced. The composition of this product was 10 wt% of Al 2 O 3 , 3.2 wt% of Ca, and 70% of basicity.
[AlCa0.42(OH)2.10Cl1.74)[AlCa 0.42 (OH) 2.10 Cl 1.74 )
상기 수득한 폴리염화알루미늄칼슘에 의한 수처리시의 응집 실험 결과는 다음과 같다.The results of the flocculation test at the time of water treatment with the obtained calcium aluminum chloride were as follows.
표 1：원수 : 알칼리도(CaCO3) 20mg/ l, pH=7.8, 탁도 = 85 NTUTable 1: Raw water: alkalinity (CaCO 3 ) 20 mg / l, pH = 7.8, turbidity = 85 NTU
※NTU : 용액중 현탁물질의 양(Nephelometric Turbidity Unit).※ NTU: Amount of suspended material in solution (Nephelometric Turbidity Unit).
탁도의 측정은 ASTMD-1889-81의 방법에 따름. The measurement of turbidity is according to the method of ASTM D-1889-81.
[발명의 효과][Effects of the Invention]
본 응집제는 기존응집제 투입 설비를 그대로 사용하면서 고탁도·저알칼리도의 원수에 적용할 수 있는 새로 개발된 고성능응집제로, 수처리시 경제적이고 효율적인 처리를 가능하게 할 수 있는 특수한 성능을 보일 수 있다.This coagulant is a newly developed high performance coagulant that can be applied to raw water of high turbidity and low alkalinity while using existing coagulant input facilities as it is, and it can show a special performance that enables economical and efficient treatment in water treatment.
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