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公开(公告)号：KR1020040002364A
公开(公告)日：2004-01-07
申请号：KR1020020071573
申请日：2002-11-18
CPC classification number: B01J37/18 , B01J23/8892 , C07C29/149 , C07C31/205
Abstract: PURPOSE: A hydrogenation catalyst which is capable of producing 1,3-propanediol at a high yield and has extended life time and industrial values is provided, and an optimized method for hydrogenating 3-hydroxy alkylpropane using the catalyst is provided. CONSTITUTION: The hydrogenation catalyst is characterized in that it is prepared by adding nano size colloidal silica to the produced particles and aging the nano size colloidal silica added particles after primarily producing particles in a mixed hydroxide form by adding an alkaline precipitant to an aqueous solution containing copper salt, manganese salt and zinc salt and represented as CuO(A)MnO2(B)ZnO(C)SiO2(D), where A is 40 to 85 wt.%, B is 0.15 to 4 wt.%, C is 0.001 to 2.5 wt.%, D is 10 to 60 wt.%, and the total sum of B and C is 5 wt.% or less. The method for preparing 1,3-propanediol comprises a step of activating the hydrogenation catalyst by reducing the hydrogenation catalyst in a stationary phase reactor using hydrogen gas or hydrogen contained gas; and a step of gas phase hydrogenating 3-hydroxy alkylpropane using hydrogen gas or hydrogen contained gas in the presence of the activated catalyst.
Abstract translation: 目的：提供能够以高产率生产1,3-丙二醇并延长使用寿命和工业价值的氢化催化剂，并提供使用该催化剂氢化3-羟基烷基丙烷的优化方法。 构成：氢化催化剂的特征在于，通过向生成的颗粒中加入纳米尺寸的胶态二氧化硅并且在主要通过混合氢氧化物形式生产颗粒之后老化纳米尺寸的胶体二氧化硅添加颗粒来制备，通过将碱性沉淀剂加入含有 铜盐，锰盐和锌盐，并表示为CuO（A）MnO 2（B）ZnO（C）SiO 2（D），其中A为40〜85重量％，B为0.15〜4重量％，C为0.001 至2.5重量％，D为10〜60重量％，B和C的总和为5重量％以下。 制备1,3-丙二醇的方法包括通过使用氢气或含氢气体在固定相反应器中还原加氢催化剂来活化氢化催化剂的步骤; 以及在活化催化剂存在下使用氢气或含氢气体气相氢化3-羟基烷基丙烷的步骤。
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82.发明公开복합금속산화물 촉매 및 이의 제조 방법, 및 이를이용하여 프탈산에스테르로부터 프탈라이드를 제조하는 방법 失效用于蒸气相氢化的复合金属氧化物催化剂，其制备方法以及使用复合金属氧化物催化剂制备邻苯二甲酸酯的方法
公开(公告)号：KR1020030083878A
公开(公告)日：2003-11-01
申请号：KR1020020022270
申请日：2002-04-23
Applicant: 한국화학연구원 , 에이케이홀딩스 주식회사
IPC: B01J23/889 , B01J23/80 , B82B1/00 , B82Y30/00
CPC classification number: B01J23/8892 , B01J23/8896 , B01J23/8986 , B01J37/038 , B01J37/06 , B01J37/08 , C07D307/85
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: 目的：提供一种用于汽相氢化的复合金属氧化物催化剂，其制备方法和使用该复合金属氧化物催化剂由邻苯二甲酸酯制备邻苯二甲酸酯的方法，其中该催化剂在该方法中表现出高选择性，生产率和延长的催化活性 即使在低温130〜220℃，低压1〜10大气压，低氢/酯邻苯二甲酸酯比例在500〜3000之间的温和条件下，通过气相氢化即可从邻苯二甲酸邻苯二甲酸酯制备苯酞。 构成：催化剂表示如下：CuO（a）ZnO（b）MnO 2（c）SiO 2（d）|（100-x）M（x），其中M是至少一种选自以下的氧化物： Re氧化物，Ru氧化物和Ag氧化物，a为20至90，b为0.01至10，c为0.01至5，d为5至65，x为0.001至5，其中a，b，c，d和x为 以重量为基础表达。 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的胶体二氧化硅，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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83.发明公开
公开(公告)号：KR1020030076851A
公开(公告)日：2003-09-29
申请号：KR1020020015828
申请日：2002-03-23
Applicant: 한국화학연구원
CPC classification number: B01J37/0009 , B01J23/80 , B01J37/038 , C07C5/322 , C07C29/149
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液进行有机化合物氢化脱氢的铜/二氧化硅催化剂的制备方法。 构成：制备铜/二氧化硅催化剂的方法包括通过在含铜的酸性废溶液中加入铜化合物和任意的锌化合物来制备铜水溶液的步骤（a） 通过向铜水溶液中添加沉淀剂溶液来制备铜浆液的步骤（b）; 通过向铜浆液中加入胶体二氧化硅溶液并搅拌胶体二氧化硅溶液和铜浆液，制备铜/二氧化硅浆料溶液的步骤（c）; 步骤（d）在50〜100℃的温度下对沉淀物进行分离并漂洗分离出的沉淀物; 以及干燥和烧制漂洗后的沉淀物的步骤（e），其中所述沉淀剂是氨，或碱金属的碳酸氢盐，碳酸盐或氢氧化物，其中所述胶体二氧化硅溶液以这样的方式加入到铜浆液中： 在制备的催化剂中氧化铜与二氧化硅的（CuO / SiO 2）在0.3-9.0 / 1的范围内，其中使用锌化合物，并将胶体二氧化硅溶液加入到铜浆液中，使得重量比 在所制备的催化剂中，氧化铜与氧化锌对二氧化硅的氧化铜（CuO / ZnO / SiO 2）在0.3-9.0 / 0.01-3.0 / 1的范围内，其中胶体二氧化硅通过铵（NH 4 +）或Na +或 其它碱金属，其粒径为4〜60nm，表面积为100〜300m2 / g，浓度为二氧化硅的5〜60重量％，其中老化在50〜100℃的温度下进行 摄氏0.5-2-24小时。
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公开(公告)号：KR1020030037474A
公开(公告)日：2003-05-14
申请号：KR1020010068514
申请日：2001-11-05
Applicant: 한국화학연구원 , 여천엔씨씨 주식회사
IPC: C08F4/69
CPC classification number: C08F4/622 , C08F10/00 , C08F110/02 , C08F210/16
Abstract: PURPOSE: Provided is a chrome-calixarene-organoaluminum catalyst which has excellent catalytic activity and is stable in polymerizing olefin. The catalyst is simple to synthesize and reproducible. It can be used in making specific polymers different from polymers made by usual Ziegler-Natta or chrome supported catalysts in molecular weight distribution and the degree of crystallinity and unsaturation. CONSTITUTION: The catalyst comprises 1 mole of chrome(III) compound, 0.5-2 moles of calixarene compound and 10-1000 moles of organic aluminum compound. The polymerization is carried out with the catalyst at 30-200deg.C under 3-50 atm and the catalyst is either added with molecular chrome-calixarene and organic aluminum respectively or in one shot of the mixed component.
Abstract translation: 目的：提供一种具有优异催化活性并在烯烃聚合中稳定的铬 - 杯芳烃 - 有机铝催化剂。 催化剂易于合成和再生。 它可以用于制造与通常的齐格勒 - 纳塔或铬载体催化剂在分子量分布和结晶度和不饱和度方面制备的聚合物不同的特定聚合物。 构成：催化剂包含1摩尔铬（III）化合物，0.5-2摩尔杯芳烃化合物和10-1000摩尔有机铝化合物。 聚合反应在30〜200℃，3-50大气压下进行，催化剂分别加入分子铬 - 杯芳烃和有机铝，或分别加入混合组分。
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公开(公告)号：KR100377504B1
公开(公告)日：2003-03-26
申请号：KR1020000025259
申请日：2000-05-12
Applicant: 에이케이홀딩스 주식회사 , 한국화학연구원
IPC: C07D207/26
Abstract: 본 발명은 감마-부티로락톤, 아민유도체 및 물을 반응시켜 피롤리돈 유도체를 제조하는 방법에 있어서, 산성형 실리카-알루미나 크레이(acid clay) 촉매하에서 감마-부티로락톤, 메틸아민 및 물의 몰비가 1:1~7:1~25이고, 반응온도 250~400℃, 공간속도 700hr
-1 ∼2000hr
-1 , 반응압력 상압~10기압인 조건에서 직접 기상촉매 반응시켜 N-메틸-2-피롤리돈을 제조하는 방법에 관한 것이다.
본 발명의 방법은 감마-부티로락톤으로부터 피롤리돈 유도체를 제조함에 있어서, 온화한 반응 조건하에서 높은 선택율과 고수율로 피롤리돈 유도체를 제조할 수 있는 효과를 갖는다.-
Patent Agency Ranking
公开(公告)号：KR100352031B1
公开(公告)日：2002-09-11
申请号：KR1020000025258
申请日：2000-05-12
Applicant: 에이케이홀딩스 주식회사 , 한국화학연구원
IPC: C07D307/32
Abstract: 본 발명은 무수말레인산이나 무수석신산을 니켈 또는 코발트를 주성분으로 하는 촉매를 사용하여 수소화 촉매 반응시켜 감마-부티로락톤을 제조하는 방법에 있어서, 반응계 중에 반응물과 함께 할로겐 화합물을 반응물 중량에 0.0001~1.0중량%를 공급하여 반응시키는 것을 특징으로 하는 감마-부티로락톤의 제조방법에 관한 것이다.
본 발명의 방법은 무수말레인산이나 무수석신산을 수소화 반응시켜 감마-부티로락톤을 제조하는 방법에 있어서, 반응물에 0.1중량% 이하의 할로겐화합물을 공급함으로서 상기 수소화 반응에서 과수소화 반응이 일어나지 않도록 하여 푸로판산이나 부탄산과 같은 부산물의 생성을 억제시켜 높은 수율로 감마-부티로락톤을 제조할 수 있는 효과를 갖는다.-
公开(公告)号：KR1020010103947A
公开(公告)日：2001-11-24
申请号：KR1020000025260
申请日：2000-05-12
Applicant: 에이케이홀딩스 주식회사 , 한국화학연구원
IPC: B01J23/755 , B01J23/44 , B01J23/28
CPC classification number: B01J23/002 , B01J2523/00 , B01J2523/48 , B01J2523/68 , B01J2523/824 , B01J2523/847 , C07D307/33
Abstract: 본 발명은 다음 일반식(Ⅰ)로 표시되는 수소화 반응촉매와
Ni
9 Pd
a Mo
b N
c Zr
d O
x … (Ⅰ)
상기식에서 N은 Co, Cu, Zn, Ag, Pb, Ru 중에서 선택되는 금속원소이고, a는 0.001~0.5, b는 0.01~5, C는 0.001~1.0, d는 0.5~12.0, x는 각성분의 원자가 및 조성비에 따른 화학 양론적 값을 나타낸다.
이 촉매를 이용하는 감마-부티로락톤의 제조방법에 관한 것이다.
본 발명의 촉매를 이용하는 본 발명의 방법은 온화한 반응조건하에서 높은 선택율과 높은 수율로 무수말레인산이나 무수석신산으로부터 감마-부티로락톤을 제조할 수 있는 효과를 갖는다.-
公开(公告)号：KR1020010100206A
公开(公告)日：2001-11-14
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：KR1019900004119B1
公开(公告)日：1990-06-16
申请号：KR1019880008100
申请日：1988-06-30
Abstract: A catalyst of formula P1Mo12AsaTlbVcCudOe+ X3PM12O40(f%) [where X= NH4, K or Cs; M= Mo or W; a= 0.2-2.0, b= 0.1-2.0, c= 0.2-2.1, d= 0.1- 1.0, e= bal. no., f= wt.%, 30-75 for prepg. methacrylic acid[from methacrolein with O is prepd. by (a) adding X3PM12O40 soln. to a soln. (contg. H3PMo12O40, H3AsO4 and V2O5), (b) co-pptg. with a soln. (contg. Tl(C2H3O2) and Cu(NO3)2. 2.5H2O, (c) heating at 40-100 deg. C on a stirrer to obtain slurry, (d) vacuum drying at 20-100 deg. C and molding, and (e) calcining at 320-400 deg. C.
Abstract translation: 式P1Mo12AsaTlbVcCudOe + X3PM12O40（f％）[其中X = NH4，K或Cs; M = Mo或W; a = 0.2-2.0，b = 0.1-2.0，c = 0.2-2.1，d = 0.1- 1.0，e = bal。 编号，f =重量％，30-75。 甲基丙烯酸[来自具有O的甲基丙烯醛]制备。 （a）加入X3PM12O40 soln。 到一个soln （不包括H3PMo12O40，H3AsO4和V2O5），（b）共聚物。 用一个soln （不包括Tl（C2H3O2）和Cu（NO3 )2.2.5H2O，（c）在搅拌器上在40-100℃下加热得到浆料，（d）在20-100℃真空干燥并成型， 和（e）在320-400℃下煅烧
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