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111.发明公开수소화 반응촉매 및 그의 제조방법, 및 이 촉매를이용하여 무수말레인산으로부터 감마-부티로락톤을제조하는 방법 有权用于蒸气相氢化的催化剂及其制备方法及使用催化剂制备马来酸酐（GBL）的甘氨酸丁酯（GBL）的方法
公开(公告)号：KR1020030083844A
公开(公告)日：2003-11-01
申请号：KR1020020022029
申请日：2002-04-22
Applicant: 한국화학연구원 , 에이케이홀딩스 주식회사
IPC: B01J23/889 , B01J23/80 , B82B1/00 , B82Y30/00
CPC classification number: B01J37/036 , B01J23/002 , B01J23/8892 , B01J2523/00 , B01J2523/17 , B01J2523/27 , B01J2523/41 , B01J2523/72
Abstract: PURPOSE: Provided are a catalyst for vapour phase hydrogenation, a preparation method thereof and a method for preparing gamma-butyrolactone (GBL) from maleic anhydride (MAn) using the catalyst, wherein the catalyst exhibits high selectivity, productivity and extended catalytic activity in the process of preparing gamma-butyrolactone (GBL) from maleic anhydride (MAn) by vapour phase hydrogenation even under the mild conditions of low temperature, low pressure and low hydrogen/maleic anhydride ratio. CONSTITUTION: The catalyst is represented as follows: CuO(a)ZnO(b)MnO2(c)SiO2(d), where a is 20 to 90, b is 0.01 to 10, c is 0.01 to 5 and d is 5 to 50, wherein a, b, c and d 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: 目的：提供一种气相氢化催化剂，其制备方法和使用该催化剂由马来酸酐（MAn）制备γ-丁内酯（GBL）的方法，其中该催化剂表现出高选择性，生产率和延长的催化活性 即使在低温，低压和低氢/马来酸酐比的温和条件下，也通过汽相氢化从马来酸酐（MAn）制备γ-丁内酯（GBL）的方法。 构成：催化剂表示如下：CuO（a）ZnO（b）MnO 2（c）SiO 2（d），其中a为20〜90，b为0.01〜10，c为0.01〜5，d为5〜50 ，其中a，b，c和d基于重量来表示。 催化剂的制备方法包括制备含有铜盐，锌盐和锰盐的混合溶液的步骤; 向混合溶液中加入碱溶液以共沉淀水凝胶形式的铜，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 ; 向水凝胶中加入纳米尺寸胶体二氧化硅，从而得到混合浆料，其中胶体二氧化硅通过NH 4 +，Na + +和其它碱金属稳定，其粒度和比表面积为4〜60nm，100〜 分别为300m2 / g; 将混合浆液在50〜100℃水热老化超过0.5小时; 在水热老化后过滤混合浆料分离滤饼，然后洗涤滤饼，其中进行洗涤直到碱金属的残留浓度小于1000ppm; 并将洗涤的蛋糕干燥并压片。
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公开(公告)号：KR1020030036951A
公开(公告)日：2003-05-12
申请号：KR1020010067901
申请日：2001-11-01
IPC: C07C29/141
CPC classification number: B01J23/8892 , B01J21/08 , B01J23/72 , B01J37/0009 , B01J37/03 , B01J37/18 , C07C29/149 , C07C31/205
Abstract: PURPOSE: Provided is a method for producing 1,3-alkanediol from 3-hydroxyester compound, which can increase the selectivity of 1,3-alkanediol by 90% or more, and improve the stability of catalyst. CONSTITUTION: The method comprises the steps of (i) adding an alkaline precipitating agent to aqueous copper solution to form a particle, adding a colloidal silica to the solution and aging the solution to form a catalyst, (ii) activating the formed catalyst by reducing the catalyst in the presence of activating solvent at 100-250 deg.C by using hydrogen gas or mixed hydrogen/nitrogen gas having pressure of 5-2000 psig and activating the, and (iii) hydrogenating 3-hydroxyester compound at 100-250 deg.C by using hydrogen gas or mixed hydrogen/nitrogen gas in the presence of the activated catalyst and reaction solvent by an liquid slurry method .
Abstract translation: 目的：提供从3-羟基酯化合物生产1,3-链烷二醇的方法，其可使1,3-链烷二醇的选择性提高90％以上，提高催化剂的稳定性。 方案：该方法包括以下步骤：（i）将碱性沉淀剂加入到铜溶液中以形成颗粒，向溶液中加入胶态二氧化硅并使溶液老化形成催化剂，（ii）通过还原活化形成的催化剂 通过使用氢气或压力为5-2000psig的混合氢/氮气，在活化溶剂存在下在100-250℃下活化催化剂，并且（iii）在100-250℃氢化3-羟基酯化合物 在活化催化剂和反应溶剂的存在下，通过液体浆料法使用氢气或混合氢/氮气。
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公开(公告)号：KR1020020082574A
公开(公告)日：2002-10-31
申请号：KR1020010022042
申请日：2001-04-24
IPC: C07C29/74
Abstract: PURPOSE: Provided is a method for separating a liquid alkoxylation product efficiently from an alkoxylation product containing a gel type by-product, which can increase filtering velocity and maximize the yield of the alkoxylation product. CONSTITUTION: The method is performed by adding 10-100vol%(based on an alkoxylation mixture) of a C1-C4 alcohol having a boiling point of 50-100deg.C to the alkoxylation mixture comprising the alkoxylation product produced by alkoxylation of an aliphatic alcohol or an aliphatic acid ester in the presence of a solid catalyst, the gel type by-product, and a catalyst residue to disperse uniformly and filtering the dispersed solution and then distilling and removing the alcohol from the filtrate.
Abstract translation: 目的：提供一种从含有凝胶型副产物的烷氧基化产物有效分离液体烷氧基化产物的方法，其可提高过滤速度并使烷氧基化产物的产率最大化。 构成：该方法通过将含有沸点为50-100℃的C 1 -C 4醇的10-100vol％（基于烷氧基化混合物）加入到通过脂族醇的烷氧基化产生的烷氧基化产物的烷氧基化混合物 或脂肪酸酯在固体催化剂，凝胶型副产物和催化剂残余物的存在下均匀分散并过滤分散的溶液，然后从滤液中蒸馏除去醇。
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公开(公告)号：KR100349974B1
公开(公告)日：2002-08-23
申请号：KR1020000013292
申请日：2000-03-16
Abstract: 본 발명은 표면 활성금속 농도가 제어된 혼합금속 산화물 촉매 및 이의 제조방법에 관한 것으로, 더욱 상세하게는 다음 화학식 1로 표시되는 하이드로탈사이트 형태의 혼합금속 수산화물의 표면에 3가금속(M(Ⅲ)) 이온을 흡착시킨 후, 분리하고, 일정 온도범위에서 열처리하므로써 촉매 표면의 활성금속 성분의 농도가 증가되고 또 활성금속이온이 촉매 표면에 균일하게 분포되어 있어 알콕시 부가반응에 촉매로 적용되어서는 알콕시 부가수 분포를 좁은 범위로 제어하고 기존의 촉매와 비교하여 반응속도를 크게 증가시킬 수 있으므로 최소량의 촉매 사용으로도 반응기내에서 균일성 확보가 가능하고, 촉매잔유물과 반응생성물의 젤(gel)형 복합체 생성을 크게 감소시켜 반응후 처리단계에서 생산성을 향상시키는 등의 우수성을 가지게 되는 표면 활성금 속 농도가 제어된 혼합금속 산화물 촉매와 이의 제조방법에 관한 것이다.
[M(Ⅱ)
1-x M(Ⅲ)
x ](OH)
2 A nH
2 O-
公开(公告)号：KR1020020060000A
公开(公告)日：2002-07-16
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脲酸酯复合物的方法，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。 构成：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。 优选地，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，Al2O3，CaO和镁/铝复合氧化物; 水溶性氢氧化物选自NH 4 OH，LiOH，NaOH和KOH。 优选地，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％ 并且水溶性氢氧化物的含量相对于水不溶性金属氢氧化物或金属氧化物的重量小于20重量％。
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Patent Agency Ranking116.发明公开
公开(公告)号：KR1020010108920A
公开(公告)日：2001-12-08
申请号：KR1020000029957
申请日：2000-06-01
CPC classification number: C01G1/00 , C01B13/145 , C01F7/021 , C01G37/02 , C01G53/04 , C01P2002/22 , C01P2004/84
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.-
117.发明授权
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公开(公告)号：KR101808824B1
公开(公告)日：2017-12-14
申请号：KR1020160088031
申请日：2016-07-12
Applicant: 한국화학연구원
IPC: C07D317/72
Abstract: 본발명은글리세롤및 헥시톨로부터모사이동층크로마토그래피를이용한광학이성질체의분리에관한것으로, 본발명에따른광학이성질체분리방법또는정제방법은모사이동층크로마토그래피를이용하여종래보다간단한공정을통해글리세롤및 소비톨로부터 C-3 광학이성질체를 99.9% 이상의고순도및 고수율로정제할수 있는것으로확인되어, 이로부터고부가가치키랄신톤(chiral synthon) 등을수득할수 있는유용한효과가있다.
Abstract translation: 本发明是甘油，和涉及使用从己糖醇，旋光异构体分离方法或纯化方法以模拟移动床色谱法根据通过比使用色谱现有技术的简单的过程本发明的甘油的光学异构体的模拟移动床分离 和被发现是从以高纯度和99.9％以上的高收率的山梨糖醇的C-3的纯化对映异构体，存在能够得到高附加值，例如手性辛顿（手性合成子）从其一个有用的效果。
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