公开(公告)号：KR1020040050998A

公开(公告)日：2004-06-18

申请号：KR1020020078815

申请日：2002-12-11

Applicant: 한국화학연구원

Inventor： 박대철 ,  백진욱 ,  박양진 ,  박주은

IPC: C07C67/38

CPC classification number: Y02P20/544

Abstract: PURPOSE: A method for preparing an ester derivative by using supercritical carbon dioxide as a reaction solvent is provided, to prevent the problems such as toxicity, corrosion and flammability due to the use of an organic solvent. CONSTITUTION: The method comprises the step of preparing an ester derivative from an olefin by using a palladium compound as a catalyst, a phosphine ligand material as an electron donor, an acid material as a reaction accelerator and supercritical fluid as a reaction solvent (See the reaction scheme II), wherein R is an alkyl or aryl group substituted with a functional group. Preferably the supercritical fluid is carbon dioxide. Preferably the acid material is p-toluenesulfonic acid; the palladium compound is selected from the group consisting of palladium acetate (Pd(OAc)2), palladium trifluoroacetate (Pd(tfOAc)2) and tetrakis(triphenylphosphine) palladium (Pd(PPh3)4); and the phosphine ligand material is selected from the group consisting of PPh3, P(p-toly)3, P(p-ClC6H4)3, P(p-FC6H4)3 and P(p-CF3(C6H4))3.

Abstract translation: 目的：提供通过使用超临界二氧化碳作为反应溶剂制备酯衍生物的方法，以防止由于使用有机溶剂而引起的毒性，腐蚀和可燃性等问题。 方案：该方法包括通过使用钯化合物作为催化剂，作为电子给体的膦配体材料，作为反应促进剂的酸性材料和作为反应溶剂的超临界流体，从烯烃制备酯衍生物的步骤（参见 反应方案II），其中R是被官能团取代的烷基或芳基。 优选地，超临界流体是二氧化碳。 优选酸性物质是对甲苯磺酸; 钯化合物选自乙酸钯（Pd（OAc）2），三氟乙酸钯（Pd（tfOAc）2）和四（三苯基膦）钯（Pd（PPh 3）4））。 膦配体材料选自PPh 3，P（p-toly）3，P（p-ClC 6 H 4）3，P（p-FC 6 H 4）3和P（p-CF 3（C 6 H 4））3。

公开(公告)号：KR100398747B1

公开(公告)日：2003-09-19

申请号：KR1019990043232

申请日：1999-10-07

Applicant: 한국화학연구원

Inventor： 박대철 ,  백진욱 ,  박양진

IPC: H01M6/36

Abstract: PURPOSE: Provided is a thin-film photoelectrode made of ion-added titanium oxide compound which is used for converting light energy to electric energy. And a method for preparing the same and a method for generating photoelectrical current using the same are also provided. CONSTITUTION: The thin-film photoelectrode made of titanium oxide compound is represented by the formula (1) CG/TixMyO2: wherein, CG is a conducting glass, which collects photoelectrical current generated from a semiconductor, such as indium tin oxide glass or SnO2 glass; M is ionic materials added to synthesize the titanium oxide semiconductor compound and is selected from the group consisting of P, As, Sb, Cr, V, Mo, Mn, Re, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Al, Ga, Sn, Pb, S, Y, Rb, Na, Mg and Ca; x represents atom % of Ti/(Ti+M) and is 92.00-99.99; and y represents atom % of M/(Ti+M) and is 0.01-8.00. The method for preparing the thin-film photoelectrode of titanium oxide compound comprises steps of: (i) gradually adding Ti(OCH(CH3)2)4 mixed with isopropyl alcohol to distilled water to make atom % of Ti/(Ti+M) be 92.00-99.99 under nitrogen atmosphere and intensely stirring the solution for 5-20 minutes; (ii) after adding HNO3 to the obtained solution of the step (i) until the pH value gets 1-2 to accurately deposit titania, adding ionic materials to the solution to make atom % of M/(Ti+M) be 0.01-8.00; (iii) intensely mixing the solution at a temperature of 60-100 deg.C for 5-10 hours and then evaporating water to obtain sol having viscosity; (iv) after dropping fixed amount of the obtained sol on ITO plate to coat the plate with the sol in order to have uniform thickness, sintering the ITO plate at a temperature of 200-550 deg.C for 30-60 minutes.

Abstract translation: 用途：提供一种用于将光能转化为电能的离子加入氧化钛化合物制成的薄膜光电极。 还提供了一种用于制备其的方法以及使用该方法产生光电流的方法。 构成：由氧化钛化合物制成的薄膜光电极由式（1）CG / TixMyO2表示：其中，CG是导电玻璃，其收集由半导体产生的光电流，例如氧化铟锡玻璃或SnO2玻璃 ; M是为了合成氧化钛半导体化合物而添加的离子材料，并且选自由P，As，Sb，Cr，V，Mo，Mn，Re，Fe，Ru，Co，Rh，Ir，Ni，Pd， Pt，Cu，Ag，Al，Ga，Sn，Pb，S，Y，Rb，Na，Mg和Ca; x表示Ti /（Ti + M）的原子％，为92.00-99.99; y表示M /（Ti + M）的原子％，为0.01〜8.00。 制备氧化钛化合物薄膜光电极的方法包括以下步骤：（i）将与异丙醇混合的Ti（OCH（CH3）2）4逐渐加入到蒸馏水中以使Ti /（Ti + M）原子％ 在氮气氛下为92.00-99.99并剧烈搅拌溶液5-20分钟; （ii）向得到的步骤（i）的溶液中加入HNO3直至pH值达到1-2，准确沉积二氧化钛后，向溶液中加入离子材料使M /（Ti + M）的原子百分比为0.01- 8.00; （iii）在60-100℃的温度下剧烈混合该溶液5-10小时，然后蒸发水以获得具有粘度的溶胶; （iv）将固定量的所得溶胶滴在ITO板上以将溶胶涂覆到板上以具有均匀的厚度后，在200-550℃的温度下将ITO板烧结30-60分钟。

公开(公告)号：KR1020020044889A

公开(公告)日：2002-06-19

申请号：KR1020000074137

申请日：2000-12-07

Applicant: 한국화학연구원

Inventor： 박대철 ,  백진욱 ,  박양진

IPC: C07C49/786

Abstract: PURPOSE: A method for preparing 2-hydroxy-4-octyloxybenzophenone of a benzophenone-based photostabilizer is provided, to improve the selectivity of the product(a yield of 95% without the generation of isomers). CONSTITUTION: The method comprises the step of mixing 2,4-dihydroxybenzophenone and octyl halide with a molar ratio of 2.0:1.8 to 2.0:3.0 (See the reaction scheme 1). In the reaction scheme 1, X is Cl, Br or I. Preferably the reaction temperature is 120-160 deg.C and the reaction time is 5-12 hours. Preferably an acid neutralizer(Na2CO3), a reaction catalyst(KI) and a reaction solvent(PEG400 : poly(ethylene glycol), a mean molecular weight 400) are employed. The molar ratio of Na2CO3 to 2,4-dihydroxybenzophenone is 2.0:0.5 to 1:1, and the molar ratio of KI is 0.05-0.10 mol% based on the weight of 2,4-dihydroxybenzophenone.

Abstract translation: 目的：提供二苯甲酮类光稳定剂的2-羟基-4-辛氧基二苯甲酮的制备方法，提高产物的选择性（产率95％，不产生异构体）。 方案：该方法包括以摩尔比2.0：1.8至2.0：3.0混合2,4-二羟基二苯甲酮和辛基卤化物的步骤（参见反应方案1）。 在反应方案1中，X为Cl，Br或I.优选反应温度为120-160℃，反应时间为5-12小时。 优选使用酸中和剂（Na 2 CO 3），反应催化剂（KI）和反应溶剂（PEG400：聚（乙二醇），平均分子量400）。 Na 2 CO 3与2,4-二羟基二苯甲酮的摩尔比为2.0:0.5:1:1，基于2,4-二羟基二苯甲酮的重量，KI的摩尔比为0.05-0.10mol％。

公开(公告)号：KR1020040021074A

公开(公告)日：2004-03-10

申请号：KR1020020052515

申请日：2002-09-02

Applicant: 한국화학연구원

Inventor： 박대철 ,  백진욱 ,  박양진

IPC: B01J27/04

CPC classification number: B01J27/04 ,  B01J27/043 ,  B01J27/051 ,  B01J35/004 ,  B01J37/031 ,  B01J37/08 ,  B01J37/12 ,  B01J37/16 ,  C01B3/042

Abstract: PURPOSE: A mixed metal sulfide based photocatalyst used in manufacturing hydrogen from water by photoreaction is provided, a method for manufacturing the same is provided, and a method for manufacturing hydrogen using the same is provided. CONSTITUTION: The mixed metal sulfide based photocatalyst for generating hydrogen is characterized in that it has the following general formula 1: MxM1yS, where M is a metal selected from Al, Cu, Ag, Sn and Zn, M1 is a metal selected from Pb, Fe, Mo, Ag, Cu, Ni and Al, x for showing a mixing ratio represented in an atom% of M/(M+M1) has a value of 5.0 to 95.0, and y for showing a mixing ratio represented in an atom% of M1/(M+M1) has a value of 5.0 to 95.0.

Abstract translation: 目的：提供一种用于通过光反应从水中制造氢的混合金属硫化物基光催化剂，其制造方法，并提供使用其制造氢的方法。 构成：用于产生氢的混合金属硫化物基光催化剂的特征在于其具有以下通式1：MxM1yS，其中M是选自Al，Cu，Ag，Sn和Zn的金属，M1是选自Pb， 表示以M /（M + M1）的原子％表示的混合比的Fe，Mo，Ag，Cu，Ni和Al的x的值为5.0〜95.0，y表示以原子表示的混合比 M1 /（M + M1）的％的值为5.0〜95.0。

公开(公告)号：KR1020040050999A

公开(公告)日：2004-06-18

申请号：KR1020020078816

申请日：2002-12-11

Applicant: 한국화학연구원

Inventor： 박대철 ,  백진욱 ,  박양진

IPC: B01J31/18

CPC classification number: B01J31/1885 ,  B01J2531/822 ,  C07C45/50

Abstract: PURPOSE: Provided are a rhodium (I) phosphite complex catalyst for a hydroformylation reaction, a method for preparing thereof and a method for selectively preparing an aldehyde by using the same. CONSTITUTION: The method for preparing a rhodium (I) phosphite complex catalyst for a hydroformylation reaction by using supercritical carbon dioxide having an excellent selectivity comprises a step of the following reaction II. The method for selectively preparing an aldehyde through the following reaction III, which selectively prepares the aldehyde by hydroformylating 1-octene under synthesized gas of CO/H2 by using a metal catalyst, is characterized in that the rhodium phosphite complex catalyst for the hydroformylation reaction is used as the catalyst and a supercritical fluid is used as a reaction solvent.

Abstract translation: 目的：提供用于加氢甲酰化反应的铑（I）亚磷酸酯配合物催化剂，其制备方法和使用它们选择性制备醛的方法。 构成：通过使用具有优异选择性的超临界二氧化碳制备用于加氢甲酰基化反应的铑（I）亚磷酸酯配合物催化剂的方法包括以下反应II的步骤。 通过以下反应III选择性制备醛的方法，其通过使用金属催化剂在CO / H 2的合成气体下加氢甲酰化1-辛烯来选择性地制备醛，其特征在于用于加氢甲酰化反应的铑亚磷酸酯络合物催化剂为 用作催化剂，使用超临界流体作为反应溶剂。

公开(公告)号：KR1020040021075A

公开(公告)日：2004-03-10

申请号：KR1020020052516

申请日：2002-09-02

Applicant: 한국화학연구원

Inventor： 박대철 ,  백진욱 ,  박양진

IPC: B01J27/04

CPC classification number: B01J27/04 ,  B01J27/043 ,  B01J27/045 ,  B01J37/0236 ,  B01J37/031 ,  B01J37/08 ,  B01J37/16 ,  C01B3/042

Abstract: PURPOSE: A semiconductor particle supported metal sulfide based photocatalyst used in manufacturing hydrogen from water by photoreaction is provided, a method for manufacturing the same is provided, and a method for manufacturing hydrogen using the same is provided. CONSTITUTION: The semiconductor particle supported metal sulfide based photocatalyst is characterized in that it has the following general formula 1: Ax/MyM1zS, where A is a supported semiconductor particle selected from Si, SiC and TiO2, x for representing a mole ratio £Ax/(MyM1zS)| of A to MyM1zS has a value of 0.5 to 2.0, M is a metal selected from Sn and Zn, M1 is a metal selected from Co, Mn, Fe, Cu and Ru, y for showing a mixing ratio represented in an atom% of M/(M+M1) has a value of 50.0 to 95.0, and z for showing a mixing ratio represented in an atom% of M1/(M+M1) has a value of 5.0 to 80.0.

Abstract translation: 目的：提供一种用于通过光反应从水中制造氢的半导体颗粒负载的金属硫化物基光催化剂，其制造方法，并且提供了使用其制造氢的方法。 构成：半导体颗粒负载的金属硫化物基光催化剂的特征在于其具有以下通式1：Ax / MyM1zS，其中A是选自Si，SiC和TiO 2的负载型半导体颗粒，x表示摩尔比£Ax / （MyM1zS）| 的A至MyM 1 zS的值为0.5〜2.0，M为选自Sn，Zn的金属，M1为选自Co，Mn，Fe，Cu，Ru，y的金属，表示以原子％表示的混合比 M /（M + M1）的值为50.0〜95.0，用于表示M1 /（M + M1）的原子％表示的混合比的z的值为5.0〜80.0。

公开(公告)号：KR1020010036280A

公开(公告)日：2001-05-07

申请号：KR1019990043232

申请日：1999-10-07

Applicant: 한국화학연구원

Inventor： 박대철 ,  백진욱 ,  박양진

IPC: H01M6/36

CPC classification number: H01L31/022425 ,  H01L31/022466 ,  H01L31/0264

Abstract: PURPOSE: Provided is a thin-film photoelectrode made of ion-added titanium oxide compound which is used for converting light energy to electric energy. And a method for preparing the same and a method for generating photoelectrical current using the same are also provided. CONSTITUTION: The thin-film photoelectrode made of titanium oxide compound is represented by the formula (1) CG/TixMyO2: wherein, CG is a conducting glass, which collects photoelectrical current generated from a semiconductor, such as indium tin oxide glass or SnO2 glass; M is ionic materials added to synthesize the titanium oxide semiconductor compound and is selected from the group consisting of P, As, Sb, Cr, V, Mo, Mn, Re, Fe, Ru, Co, Rh, Ir, Ni, Pd, Pt, Cu, Ag, Al, Ga, Sn, Pb, S, Y, Rb, Na, Mg and Ca; x represents atom % of Ti/(Ti+M) and is 92.00-99.99; and y represents atom % of M/(Ti+M) and is 0.01-8.00. The method for preparing the thin-film photoelectrode of titanium oxide compound comprises steps of: (i) gradually adding Ti(OCH(CH3)2)4 mixed with isopropyl alcohol to distilled water to make atom % of Ti/(Ti+M) be 92.00-99.99 under nitrogen atmosphere and intensely stirring the solution for 5-20 minutes; (ii) after adding HNO3 to the obtained solution of the step (i) until the pH value gets 1-2 to accurately deposit titania, adding ionic materials to the solution to make atom % of M/(Ti+M) be 0.01-8.00; (iii) intensely mixing the solution at a temperature of 60-100 deg.C for 5-10 hours and then evaporating water to obtain sol having viscosity; (iv) after dropping fixed amount of the obtained sol on ITO plate to coat the plate with the sol in order to have uniform thickness, sintering the ITO plate at a temperature of 200-550 deg.C for 30-60 minutes.

Abstract translation: 目的：提供一种用于将光能转换成电能的离子加成氧化钛化合物制成的薄膜光电极。 还提供了制备该方法和使用该方法产生光电流的方法。 构成：由氧化钛化合物制成的薄膜光电极由式（1）CG / TixMyO2表示：其中，CG是导电玻璃，其收集由半导体产生的光电流，例如氧化铟锡玻璃或SnO 2玻璃 ; M是合成氧化钛半导体化合物的离子材料，选自P，As，Sb，Cr，V，Mo，Mn，Re，Fe，Ru，Co，Rh，Ir，Ni，Pd， Pt，Cu，Ag，Al，Ga，Sn，Pb，S，Y，Rb，Na，Mg和Ca; x表示Ti /（Ti + M）的原子％，为92.00-99.99; y表示M /（Ti + M）的原子％，为0.01-8.00。 制备氧化钛化合物的薄膜光电极的方法包括以下步骤：（i）逐渐加入与异丙醇混合的Ti（OCH（CH 3）2）4蒸馏水，使原子％的Ti /（Ti + M） 在氮气氛下为92.00-99.99，剧烈搅拌溶液5-20分钟; （ii）在所得到的步骤（i）的溶液中加入HNO 3直到pH值达到1-2以精确地沉积二氧化钛，向溶液中加入离子物质使M /（Ti + M）的原子％为0.01〜 8.00; （iii）将溶液在60-100℃的温度下强烈混合5-10小时，然后蒸发水以获得具有粘度的溶胶; （iv）在ITO板上固定量的所得溶胶放置后，用溶胶涂布以均匀的厚度，将ITO板在200-550℃的温度下烧结30-60分钟。

公开(公告)号：KR100486388B1

公开(公告)日：2005-04-29

申请号：KR1020020052516

申请日：2002-09-02

Applicant: 한국화학연구원

Inventor： 박대철 ,  백진욱 ,  박양진

IPC: B01J27/04

Abstract: 본 발명은 물을 광반응으로 분해하는 데에 사용되는 반도체입자가 담지된 금속 설파이드계 광촉매 및 그 제조방법, 그리고 이에 의한 물분해 수소 제조방법 관한 것으로, 이 광촉매는 하기의 일반식 I를 가지는 것을 특징으로 한다.
A
x /M
y M'
z S ------------------------------------------ 일반식 I
(상기 일반식에서 A는 담지된 반도체입자로서, Si, SiC, TiO
2 중 선택된 1종이며, x는 M
y M'
z S에 대한 A의 mole비[A
x /(M
y M'
z S)]를 나타낸 것으로 0.5 ∼ 2.0 의 값을 갖는다. M은 Sn, Zn 중 선택된 금속이고, M'은 Co, Mn, Fe, Cu, Ru 중 선택된 금속이다. y는 M/(M+M')의 atom %로 표시된 혼합비를 나타낸 것으로 50.0 ∼ 95.0의 값을 갖는다. z는 M'/(M+M')의 atom %로 표시된 혼합비를 나타낸 것으로 5.0 ∼ 80.0의 값을 갖는다.)
본 발명의 광촉매는 두 종류 이상의 상이한 반도체물질들과 혼합 금속 설파이드계 광촉매과의 접합으로 제조된 새로운 광촉매이며, 가시광선영역에서 물분해 광촉매로서 이상적인 band gap energy 와 band edge position을 가진 신규 반도체 광촉매이다.

公开(公告)号：KR1020040051000A

公开(公告)日：2004-06-18

申请号：KR1020020078817

申请日：2002-12-11

Applicant: 한국화학연구원

Inventor： 박대철 ,  백진욱 ,  박양진

IPC: B01J31/24

CPC classification number: B01J31/185 ,  B01J37/00 ,  B01J2231/321 ,  B01J2531/822 ,  C07C45/50

Abstract: PURPOSE: Provided are a rhodium (I) phosphite complex catalyst for a hydroformylation reaction, a method for preparing thereof and a method for selectively preparing an aldehyde by using the same. CONSTITUTION: The method for preparing a rhodium (I) phosphite complex catalyst for a hydroformylation reaction by using supercritical carbon dioxide having an excellent selectivity comprises a step of the following reaction III. The method for selectively preparing an aldehyde through the following reaction IV, which selectively prepares the aldehyde by hydroformylating 1-octene under synthesized gas of CO/H2 by using a metal catalyst, is characterized in that the rhodium phosphite complex catalyst for the hydroformylation reaction is used as the catalyst and a supercritical fluid is used as a reaction solvent.

Abstract translation: 目的：提供用于加氢甲酰化反应的铑（I）亚磷酸酯配合物催化剂，其制备方法和使用它们选择性制备醛的方法。 构成：通过使用具有优异选择性的超临界二氧化碳制备用于加氢甲酰化反应的铑（I）亚磷酸酯配合物催化剂的方法包括以下反应III的步骤。 通过以下反应IV选择性制备醛的方法，其通过使用金属催化剂在CO / H 2的合成气体下加氢甲酰化1-辛烯选择性地制备醛，其特征在于用于加氢甲酰化反应的铑亚磷酸酯配合物催化剂为 用作催化剂，使用超临界流体作为反应溶剂。