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21.发明授权복합금속산화물 촉매 및 이의 제조 방법, 및 이를이용하여 프탈산에스테르로부터 프탈라이드를 제조하는 방법 失效복합금속산화물촉매및이의제조방법，및이를이용하여프탈산에스테르로부프라이드를제조하는방복합
公开(公告)号：KR100457067B1
公开(公告)日：2004-11-12
申请号：KR1020020022270
申请日：2002-04-23
Applicant: 한국화학연구원 , 에이케이홀딩스 주식회사
IPC: B01J23/889 , B01J23/80 , B82B1/00 , B82Y30/00
Abstract: PURPOSE: Provided are a composite metal oxide catalyst for vapour phase hydrogenation, a preparation method thereof and a method for preparing phthalide from ester phthalate using the composite metal oxide catalyst, wherein the catalyst exhibits high selectivity, productivity and extended catalytic activity in the process of preparing phthalide from ester phthalate by vapour phase hydrogenation even under the mild conditions of low temperature at 130 to 220 deg.C, low pressure of 1 to 10 atm and low hydrogen/ester phthalate ratio ranging from 500 to 3,000. CONSTITUTION: The catalyst is represented as follows: £CuO(a)ZnO(b)MnO2(c)SiO2(d)|(100-x)M(x), where M is at least one oxide selected from the group consisting of Re oxides, Ru oxides and Ag oxides, a is 20 to 90, b is 0.01 to 10, c is 0.01 to 5, d is 5 to 65 and x is 0.001 to 5, wherein a, b, c, d and x are expressed on the basis of weight. The preparation method of the catalyst comprises the steps of preparing a mixed solution containing copper salt, zinc salt and manganese salt; adding an alkali solution to the mixed solution to coprecipitate copper, zinc and manganese in the form of hydrogel, wherein the temperature of the mixed solution is in the range of 1 to 30 deg.C and pH is kept in the range of 6 to 9; adding nano size colloidal silica to the hydrogel, thereby obtaining a mixed slurry, wherein the colloidal silica is stabilized by NH4¬+, Na¬+ and other alkali metal, and particle size and specific surface area thereof are 4 to 60 nm and 100 to 300 m¬2/g, respectively; hydrothermal aging the mixed slurry at 50 to 100 deg.C for more than 0.5 hr; filtering the mixed slurry after hydrothermal aging to separate cake, followed by washing the cake, wherein the washing is conducted until residual concentration of alkali metal is less than 1000 ppm; and drying and tableting the washed cake.
Abstract translation: 本发明提供一种用于气相氢化的复合金属氧化物催化剂，其制备方法和由该邻苯二甲酸酯用该复合金属氧化物催化剂制备邻苯二甲酸酯的方法，其中该催化剂在该方法中显示出高选择性，生产率和延长的催化活性 即使在130-220℃的低温，1-10atm的低压和500-3000的低氢/酯邻苯二甲酸酯比例的温和条件下，通过气相氢化由邻苯二甲酸酯制备苯酞。 构成：催化剂如下所示：CuO（a）ZnO（b）MnO 2（c）SiO 2（d）|（100-x）M（x），其中M是选自以下的至少一种氧化物： 的Re氧化物，Ru氧化物和Ag氧化物，a为20-90，b为0.01-10，c为0.01-5，d为5-65，x为0.001-5，其中a，b，c，d和x 以重量为基础表示。 该催化剂的制备方法包括以下步骤：制备含铜盐，锌盐和锰盐的混合溶液; 向混合溶液中添加碱溶液，以水凝胶形式共沉淀铜，锌和锰，其中混合溶液的温度在1至30℃的范围内并且pH保持在6至9的范围内 ; 将纳米胶体二氧化硅加入到水凝胶中，由此获得混合浆液，其中胶体二氧化硅通过NH 4 +，Na +和其它碱金属稳定，并且其粒径和比表面积分别为4至60nm和100至100nm 300m＆lt; 2 / g; 在50至100℃下水热老化混合浆料0.5小时以上; 过滤水热老化后的混合浆料以分离滤饼，然后洗涤滤饼，其中进行洗涤直至残余的碱金属浓度小于1000ppm; 并干燥和压片洗涤的蛋糕。
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22.发明授权
公开(公告)号：KR100455665B1
公开(公告)日：2004-11-06
申请号：KR1020020015828
申请日：2002-03-23
Applicant: 한국화학연구원
Abstract: PURPOSE: A method for preparing copper/silica catalyst used in hydrogenation and dehydrogenation of organic compounds using acidic waste solution containing copper is provided. CONSTITUTION: The method for preparing copper/silica catalyst comprises a step (a) of preparing an aqueous copper solution by adding copper compound and arbitrary zinc compound to an acidic waste solution containing copper; a step (b) of preparing a copper slurry solution by adding a precipitant solution to the aqueous copper solution; a step (c) of preparing copper/silica slurry solution by adding colloidal silica solution to the copper slurry solution and stirring the colloidal silica solution and copper slurry solution; a step (d) of separating sediment and rinsing the separated sediment after aging the copper/silica slurry solution at a temperature of 50 to 100 deg.C; and a step (e) of drying and firing the rinsed sediment, wherein the precipitant is ammonia, or bicarbonate, carbonate or hydroxide of alkali metal, wherein the colloidal silica solution is added to the copper slurry solution in such a way that a weight ratio (CuO/SiO2) of copper oxide to silica in produced catalyst is in the range of 0.3-9.0/1, wherein zinc compound is used, and the colloidal silica solution is added to the copper slurry solution in such a way that a weight ratio (CuO/ZnO/SiO2) of copper oxide to zinc oxide to silica in produced catalyst is in the range of 0.3-9.0/0.01-3.0/1, wherein colloidal silica is stabilized by ammonium (NH4¬+) or Na¬+ or other alkali metal and has particle size of 4 to 60 nm, surface area of 100 to 300 m¬2/g and concentration of 5 to 60 wt.% based on silica, and wherein the aging is performed at a temperature of 50 to 100 deg.C for 0.5 to 24 hours.
Abstract translation: 目的：提供一种使用含铜的酸性废溶液来制备用于有机化合物的氢化和脱氢的铜/二氧化硅催化剂的方法。 构成：铜/二氧化硅催化剂的制备方法包括：在含有铜的酸性废液中添加铜化合物和任意的锌化合物，制备铜水溶液的工序（a） 通过向所述铜水溶液中添加沉淀剂溶液来制备铜浆液的步骤（b）; 通过向所述铜浆液中添加胶态二氧化硅溶液并搅拌所述胶态二氧化硅溶液和铜浆液来制备铜/二氧化硅浆料溶液的步骤（c）; 步骤（d）：在50-100℃的温度下老化铜/二氧化硅浆料溶液后分离沉淀物并冲洗分离的沉淀物; （e）干燥并烧制漂洗过的沉淀物，其中沉淀剂是氨或碳酸氢盐，碱金属的碳酸盐或氢氧化物，其中将胶体二氧化硅溶液以这样的方式加入到铜浆液中，使得重量比 在生产的催化剂中氧化铜与二氧化硅的比例（CuO / SiO2）为0.3-9.0 / 1，其中使用锌化合物，并将胶体二氧化硅溶液加入铜浆液中，使得重量比 在生产的催化剂中氧化铜与氧化锌形成二氧化硅的氧化物（CuO / ZnO / SiO2）在0.3-9.0 / 0.01-3.0 / 1范围内，其中胶体二氧化硅通过铵（NH 4 +）或Na + 其它碱金属，并且具有4至60nm的粒度，100至300μm2 / g的表面积和基于二氧化硅的5至60重量％的浓度，并且其中老化在50至100℃的温度下进行 持续0.5至24小时。
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23.发明授权
公开(公告)号：KR100388097B1
公开(公告)日：2003-06-18
申请号：KR1020000029957
申请日：2000-06-01
Abstract: 고분자 물질 등에 첨가하기 위하여 적절한 입자크기를 갖고 얇은 판상을 이루며 표면적이 상대적으로 큰 범위에서 미세 특성제어가 용이한 결정성 층상 혼합금속 수산화물을 빠른 속도로 제조하는 방법이 개시되어 있다. 본 발명에 따르면, 결정성 M
(II) (OH)
2 (M
(II) 는 +2 산화상태를 갖는 금속원소)와 결정성 M
(III) (OH)
3 (M
(III) 는 +3 산화상태를 갖는 금속원소) 화합물의 물 분산물에, 이들 M
(II) 및
M
(III) 금속원소를 포함하는 수용성 화합물류와 층간 음이온 성분을 포함하는 화합물을 첨가하고, 혼합물 용액의 pH를 조절하여 수용성 금속 성분을 점성을 띠는 젤 형태의 혼합금속 수산화물로 변환시키고, 상기 결정성 M
(II) (OH)
2 , M
(III) (OH)
3 와 수용성 금속 성분으로 부터 변형된 점성을 띠는 젤 형태의 금속수산화물을 포함하는 반응 혼합물로부터, 수열 반응과정을 거쳐, 결정성 층상 혼합금속 수산화물을 제조한다. 반응에 첨가되는 수용성 화합물류의 종류, 금속수산화물에 대한 수용성 금속화합물의 첨가 비율 및 방법, 층간 음이온 성분의 종류, 반응온도, 반응시간의 적절한 선택으로 생성물인 층상 혼합금속 수산화물의 입자크기를 0.2∼2μ범위, 입자형상을 규칙적인 육각 판상으로부터 불규칙적인 모양의 판상, 비표면적의 크기를 20∼90m
2 /g 범위, 두께대 직경비를 10∼50 범위에서 유연하게 제어한다.-
公开(公告)号：KR1020030029253A
公开(公告)日：2003-04-14
申请号：KR1020010061520
申请日：2001-10-05
Applicant: 한국화학연구원 , 여천엔씨씨 주식회사
IPC: B01J31/18
CPC classification number: B01J31/18 , B01J31/1805 , B01J2531/62 , C07C2/02
Abstract: PURPOSE: Provided is a catalytic system that consists of Cr compound, ligand, alkylaluminium and halogen compound and for increasing 1-hexene selectivity in ethylene trimerization. CONSTITUTION: The catalytic system consists of chrome compound, ligand, alkylaluminium and halogen compound, wherein the ligand is a complex ligand being comprised of 1-coordinate ligand and 2-coordinate ligand, and wherein the 2-coordinate ligand includes at least two elements selected from oxygen (O), nitrogen (N) and sulfur (S), and the 1-coordinate ligand includes one element selected from oxygen (O), nitrogen (N), phosphorous (P), and sulfur (S), and further wherein the 2-coordinate ligand and the 1-coordinate ligand are included in the catalytic system with a mole ratio to chrome 0.5-1.5:1.
Abstract translation: 目的：提供由Cr化合物，配体，烷基铝和卤素化合物组成的催化体系，并且用于在乙烯三聚中增加1-己烯选择性。 构成：催化体系由铬化合物，配位体，烷基铝和卤素化合物组成，其中配体是由1-配位配位体和2-配位配体构成的复合配体，其中2-配位配体包括至少两个选自 来自氧（O），氮（N）和硫（S），并且1-配位配体包括选自氧（O），氮（N），磷（P）和硫（S）中的一种元素， 其中2-配位配体和1-配位配位体以摩尔比为0.5-1.5:1包含在催化体系中。
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公开(公告)号：KR100369707B1
公开(公告)日：2003-02-05
申请号：KR1020010001196
申请日：2001-01-09
Applicant: 한국화학연구원
IPC: C07D251/56
Abstract: PURPOSE: A method for preparing a crystalline melamine cyanurate composite is provided, to control the shape and size of particles by controlling the content of water-insoluble metal oxides and water-soluble hydroxides and the reaction conditions. CONSTITUTION: The method comprises the step of reacting melamine and cyanuric acid with a water-insoluble metal hydroxide or metal oxide and a water-soluble hydroxide. Preferably the reaction is carried out at a temperature of 80-100 deg.C for 0.5-2 hours. The water-insoluble metal hydroxide is selected from the group consisting of Mg(OH)2, Al(OH)3, Ca(OH)2 and magnesium/aluminum composite hydroxide; the water-insoluble metal oxide is selected from the group consisting of MgO, Al2O3, CaO and magnesium/aluminum composite oxide; and the water-soluble hydroxide is selected from the group consisting of NH4OH, LiOH, NaOH and KOH. Preferably the particle size of the water-insoluble metal hydroxide or metal oxide is 0.5-10 micrometers. The content of the water-insoluble metal hydroxide or metal oxide is 0.1-5.0 wt% based on the weight of solid reactant; and the content of water-soluble hydroxide is less than 20 wt% based on the weight of the water-insoluble metal hydroxide or metal oxide.
Abstract translation: 目的：提供一种制备结晶三聚氰胺氰尿酸酯复合物的方法，通过控制水不溶性金属氧化物和水溶性氢氧化物的含量以及反应条件来控制颗粒的形状和尺寸。 组成：该方法包括使三聚氰胺和氰尿酸与水不溶性金属氢氧化物或金属氧化物和水溶性氢氧化物反应的步骤。 优选反应在80-100℃的温度下进行0.5-2小时。 水不溶性金属氢氧化物选自Mg（OH）2，Al（OH）3，Ca（OH）2和镁/铝复合氢氧化物; 水不溶性金属氧化物选自MgO，Al 2 O 3，CaO和镁/铝复合氧化物; 并且水溶性氢氧化物选自由NH 4 OH，LiOH，NaOH和KOH组成的组。 优选水不溶性金属氢氧化物或金属氧化物的粒度为0.5-10微米。 基于固体反应物的重量，水不溶性金属氢氧化物或金属氧化物的含量为0.1-5.0重量％ 并且基于水不溶性金属氢氧化物或金属氧化物的重量，水溶性氢氧化物的含量小于20重量％。
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Patent Agency Ranking
公开(公告)号：KR100264966B1
公开(公告)日：2000-09-01
申请号：KR1019980005952
申请日：1998-02-25
Applicant: 한국화학연구원
IPC: B01J23/24
Abstract: PURPOSE: Disclosed are a complex metal oxide catalyst composed multiple metal elements and a preparing method of acrylic acid using the same. The catalyst has a composition form, Moa Vb Wc Pbd Cue Xf Yg (MhPMo12-i)jOk and the reaction for preparing acrylic acid is carried out under the reaction condition of low feed ratio of oxygen to acrolein and without a strong basic compound. CONSTITUTION: The complex metal oxide catalyst for preparing acrylic acid has a composition form, Moa Vb Wc Pbd Cue Xf Yg (MhPMo12-i)jOk, where X is one species of La, Ce, Sm, or Tl, Y is one species of Te, Sb, or Nb, M is Ce or Ru, and a, b, c, d, e, f, and g are atomic ratio values of respective elements. When a is 12, b, c, d, e, f, g, h, i, or j are 3-7, 1-6, 0.05-2, 0.5-4, 0.01-1, 0.01-1, 0-2, 0-3, and 0.01-0.2, respectively. And, silica, α-alumina, silicon carbide, or zirconium oxide may be used as a catalytic support. The preparation reaction of acrylic acid is carried out under the condition of temperature of 180-380deg.C, space velocity of 500-7000 h-1, feeding ratio of oxygen to acrolein of 0.5-2. Before the reaction, the catalyst is pre-treated at 200-450deg.C for 0.5-10 h in the mixed gas of acrolein, hydrocarbon such as propylene or methanol, and hydrogen.
Abstract translation: 目的：公开了一种复合金属氧化物催化剂和多种金属元素的制备方法和丙烯酸的制备方法。 催化剂具有组成形式，Moa Vb Wc Pbd Cue Xf Yg（MhPMo12-i）jOk和制备丙烯酸的反应在氧气与丙烯醛的低进料比和没有强碱性化合物的反应条件下进行。 构成：用于制备丙烯酸的复合金属氧化物催化剂具有组成形式，Moa Vb Wc Pbd Cue Xf Yg（MhPMo12-i）jOk，其中X是La，Ce，Sm或Tl的一种，Y是一种 Te，Sb或Nb，M是Ce或Ru，a，b，c，d，e，f和g是各元素的原子比值。 当a为12时，b，c，d，e，f，g，h，i或j为3-7,1-6,0.05-2,0.5-4,0.01-1,0.01-1,0- 2，0-3和0.01-0.2。 并且，可以使用二氧化硅，α-氧化铝，碳化硅或氧化锆作为催化剂载体。 丙烯酸的制备反应在180-380℃，空速500-7000h-1，氧气与丙烯醛的进料比为0.5-2的条件下进行。 在反应之前，将催化剂在丙烯醛，烃类如丙烯或甲醇和氢气的混合气体中，在200-450℃预处理0.5-10小时。
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公开(公告)号：KR100165620B1
公开(公告)日：1999-03-20
申请号：KR1019950009575
申请日：1995-04-24
Applicant: 한국화학연구원
Abstract: 본 발명은 사이클로헥센과 아세트산을 반응시켜 사이클로헥실아세테이트를 제조하는 방법에 있어서, 하기 일반식(1)의 헤테로폴리산 금속이온 염을 고체산 촉매로 사용하여 사이클로헥실아세테이프의 생산성을 향상시키는 방법에 관한 것으로, 상기 산촉매는 대상 반응계에서 활성이 장기간 유지되며, 반응물에 대한 용해도가 낮고, 활성이 감소하였을 때 쉽게 재생시킬 수 있다.
A
x H
nx SM
12 O
40 bH
2 O (I)
상기 식에서, A는 K 또는 C
s 이고,
x 는 0.1 내지 3 또는 4이고, n은 3 또는 4이고, S는 P 또는 Si 이고, M은 Mo 또는 W, 또는 이들의 조합이며, b는 0 내지 20이다.-
28.发明公开전이금속 이온으로 부분치환된 헤테로폴리산 음이온을 이온교환수지에 고정한 촉매 조성물 및 이의 제조방법 失效其中用过渡金属离子部分取代的杂多酸阴离子固定在离子交换树脂上的催化剂组合物及其制备方法
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29.发明授权
公开(公告)号：KR1019960003798B1
公开(公告)日：1996-03-22
申请号：KR1019930006151
申请日：1993-04-13
Applicant: 한국화학연구원
IPC: B01J31/24
CPC classification number: Y02P20/584
Abstract: This relates to preparing aldehyde from olefin and synthetic gas using solid catalyst in which aqueous metal phosphine complex is fixed with hydrotalcite type inorganic support. The above catalyst is expressed as formula (I). In formula T is Rh, Co or its mixture; L is Cl, CO, NO, COD, H, SR, phosphine; SP is carboxylated or sulfonated phosphine; HT is hydrotalcite. Hydroformylation is conducting under the condition of 50-200deg.C and 20-200atm of synthetic gas atmosphere. The above metal phosphine complex is such as rodium phosphine or cobalt phosphine, and phosphine ligand is such as phosphine triphenyltrisulfonate and triphenyltricarbonate.
Abstract translation: 这涉及使用固体催化剂由烯烃和合成气制备醛，其中水性金属络合物用水滑石型无机载体固定。 上述催化剂表示为式（I）。 式中，T是Rh，Co或其混合物; L是Cl，CO，NO，COD，H，SR，膦; SP是羧化或磺化膦; HT是水滑石。 加氢甲酰化在50-200℃和20-200atm的合成气体气氛条件下进行。 上述金属膦配合物如磷鎓膦或膦膦，膦配体如膦三苯基三磺酸盐和三苯基三碳酸酯。
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