公开(公告)号：KR100993009B1

公开(公告)日：2010-11-09

申请号：KR1020080026571

申请日：2008-03-21

Applicant: 한국화학연구원

Inventor： 장태선 ,  이혁희 ,  우항수 ,  최동언

IPC: C02F1/40 ,  C02F101/10

CPC classification number: Y02W10/37

Abstract: 본 발명은 수중에 발생된 조류(algae) 및 폐수 중의 부유물질을 수면 위로 고속으로 제거하면서 부영양화 원인인 인산염을 연속적으로 동시에 제거하는 방법에 관한 것으로서, 더욱 상세하게는 양전하를 제공하는 무기염과 고분자로 개질화된 자성분말체를 조류가 발생된 수역 또는 폐수 중에 주입하여 진탕(shaking)하면 음전하를 띠고 있는 녹조 및 부유물질은 전위차법에 의해 양전하를 띠고 있는 자성분말체 표면에 흡착되고, 수중에 이온상태로 존재하는 인산염은 무기염과 반응하여 부유물질인 불용성의 인산염이 형성되며, 이곳에 외부자력을 공급하여 수중에 발생된 녹조 및 부유물질은 물론 부영양화 원인인 인산염을 동시에 수면 위로 고속제거하는 방법에 관한 것이다.
전위차법, 조류(algae), 부유물질, 인산염

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

Inventor： 이정호 ,  김형록 ,  한요한 ,  정석종 ,  최낙모 ,  우항수 ,  김인기

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。

公开(公告)号：KR1020040079236A

公开(公告)日：2004-09-14

申请号：KR1020030014263

申请日：2003-03-07

Applicant: 한국화학연구원 ,  에이케이홀딩스 주식회사

Inventor： 이정호 ,  김형록 ,  한요한 ,  정석종 ,  최낙모 ,  우항수 ,  김인기 ,  이태경

IPC: C07C29/149

CPC classification number: Y02P20/584

Abstract: PURPOSE: A method for preparing 1,4-butanediol from an maleic acid ester is provided to produce 1,4-butanediol stably with high selectivity, high yield and high productivity without the treatment for reactivating a catalyst. CONSTITUTION: The method comprises the step of hydrogenating an maleic acid ester in the presence of a catalyst represented by CuO(a)MnO2(b)M(c)SiO2(d), wherein a, b, c and d are a percentage based on weight, a is 40-90, b is 0.15-5, c is 0.001-5 and d is 5-50; and M is at least one oxide of metal selected from the group consisting of Zn, Pt, Pd, Re, Ru and Rh. Preferably the catalyst is used in the hydrogenation after activated by using hydrogen or a hydrogen-containing gas at a temperature of 100-250 deg.C for 1-60 hours. Preferably the hydrogenation is carried out at a temperature of 140-260 deg.C and a pressure of 30-120 atm with a weight hourly space velocity of a maleic acid ester of 0.1-2.0/hr. Preferably the maleic acid ester is selected from dimethyl malate, diethyl malate, dipropyl malate, diisopropyl malate and dibutyl malate.

Abstract translation: 目的：提供从马来酸酯制备1,4-丁二醇的方法，以高选择性，高产率和高生产率稳定地生产1,4-丁二醇，而不用催化剂再活化。 构成：该方法包括在由CuO（a）MnO 2（b）M（c）SiO 2（d）表示的催化剂存在下氢化马来酸酯的步骤，其中a，b，c和d是基于 重量，a为40-90，b为0.15-5，c为0.001-5，d为5-50; M是选自Zn，Pt，Pd，Re，Ru和Rh中的至少一种金属氧化物。 优选地，在100-250℃的温度下使用氢气或含氢气体活化1〜60小时后，催化剂用于氢化。 优选氢化在140-260℃的温度和30-120大气压的压力下进行，马来酸酯的重时空速为0.1-2.0 /小时。 优选马来酸酯选自苹果酸二甲酯，苹果酸二乙酯，苹果酸二丙酯，苹果酸二异丙酯和苹果酸二丁酯。

公开(公告)号：KR1020030012738A

公开(公告)日：2003-02-12

申请号：KR1020010047151

申请日：2001-08-04

Applicant: 한국화학연구원 ,  에이케이홀딩스 주식회사

Inventor： 이정호 ,  김형록 ,  한요한 ,  신현관 ,  최낙모 ,  우항수 ,  김인기 ,  김성재 ,  주동균

IPC: B01J23/72 ,  B01J21/08 ,  B82Y30/00

CPC classification number: B01J23/72 ,  B01J37/038 ,  B01J37/06 ,  B01J37/08 ,  C07C29/149 ,  C07C45/002

Abstract: PURPOSE: A preparation method of silica stabilized copper catalyst used in hydrogenating or dehydrogenating organic compounds is provided, and the catalyst prepared by the method is provided. CONSTITUTION: The preparation method of Cu/SiO2 catalyst comprises the steps of (a) preparing a slurry solution of copper hydroxide by adding a precipitant solution to an aqueous copper salt solution; (b) preparing a copper hydroxide-silica slurry solution by stirring the mixed solution after adding a colloidal silica solution to the slurry solution; (c) separating sediments from the solution and cleaning the sediment after aging the copper hydroxide-silica slurry solution at a temperature of 50 to 100 deg.C; and (d) drying and baking the cleaned sediment, wherein the precipitant is carbonate or hydroxide of alkaline metal, a weight ratio of copper oxide (CuO) to silica (SiO2) of catalyst is 9:1 to 3:7, the colloidal silica is stabilized by ammonium (NH4¬+), Na¬+ or other alkali metal, has a particle size of 4 to 60 nm, surface area of 100 to 300 m¬2/g and concentration of 5 to 60 wt.% on the basis of silica, and the aging is performed at a temperature of 60 to 90 deg.C for 0.5 to 24 hours.

Abstract translation: 目的：提供用于氢化或脱氢有机化合物的二氧化硅稳定的铜催化剂的制备方法，并提供通过该方法制备的催化剂。 构成：Cu / SiO2催化剂的制备方法包括以下步骤：（a）通过向铜盐水溶液中加入沉淀剂溶液制备氢氧化铜浆液; （b）通过在将浆料溶液中加入胶体二氧化硅溶液之后搅拌混合溶液制备氢氧化铜 - 二氧化硅浆料溶液; （c）在50至100℃的温度下，将氢氧化硅 - 二氧化硅浆料溶液老化后，从溶液中分离出沉淀物并清洗沉淀物; 和（d）干燥和烘烤清洁的沉淀物，其中沉淀剂是碱金属的碳酸盐或氢氧化物，催化剂的氧化铜（CuO）与二氧化硅（SiO 2）的重量比为9:1至3:7，胶体二氧化硅 由铵（NH 4 +），Na +或其它碱金属稳定，粒径为4〜60nm，表面积为100〜300m2 / g，浓度为5〜60wt。％ 二氧化硅的基础，老化在60〜90℃的温度下进行0.5〜24小时。

公开(公告)号：KR1020090100990A

公开(公告)日：2009-09-24

申请号：KR1020080026571

申请日：2008-03-21

Applicant: 한국화학연구원

Inventor： 장태선 ,  이혁희 ,  우항수 ,  최동언

IPC: C02F1/40 ,  C02F101/10

CPC classification number: Y02W10/37 ,  C02F1/40 ,  C02F2101/105 ,  C02F2201/002

Abstract: PURPOSE: A method for removing algae, suspended materials, and nutritive salts in water with a potential difference method at high speed is provided to minimize economical damage by protecting contamination of a lake or sea. CONSTITUTION: A method for removing algae, suspended materials, and nutritive salts in water with a potential difference method at high speed through includes the following steps of: moving a device for continuous removal of algae and phosphate on the water surface; measuring concentration of the algae, the suspended materials, and hydrogen ion flowed to an inlet of a reaction tank(1); supplying a modified magnetic property composite, acid or alkali respectively; separating the algae and the nutritive salts attached on the magnetic property composite powder in the reaction tank; and discharging the water to an outlet of the reaction tank.

Abstract translation: 目的：提供一种以高速度以潜在差异法去除水中的藻类，悬浮物和营养盐的方法，以通过保护湖泊或海洋的污染来最大限度地减少经济损失。 构成：以高速通过电位差方法除去水中的藻类，悬浮物和营养盐的方法包括以下步骤：移动用于在水面上连续除去藻类和磷酸盐的装置; 测量藻类的浓度，悬浮物质和氢离子流入反应罐（1）的入口; 分别提供改性的磁性复合材料，酸或碱; 分离附着在反应罐中的磁性复合粉末上的藻类和营养盐; 并将水排出到反应罐的出口。

公开(公告)号：KR100457066B1

公开(公告)日：2004-11-12

申请号：KR1020020022029

申请日：2002-04-22

Applicant: 한국화학연구원 ,  에이케이홀딩스 주식회사

Inventor： 이정호 ,  김형록 ,  한요한 ,  정석종 ,  최낙모 ,  우항수 ,  김인기

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: The present invention relates to a hydrogenation catalyst represented by the following formula 1, a method for the preparation thereof, and a method for preparing gamma-butyrolactone using this catalyst. The method for preparing gamma-butyrolactone from maleic anhydride using the catalyst of the invention prepared by stabilizing the precursor particles of copper oxide, zinc oxide, and manganese oxide with a silica exhibits high selectivity, high yield, and high productivity under the operation conditions of a low molar ratio of hydrogen with regard to the reactants, and enables the preparation of gamma-butyrolactone from maleic anhydride with long-term stability without requiring frequent re-activation of the catalyst: Formula (I) CuO(a)ZnO(b)MnO 2 (c)SiO 2 (d) wherein a, b, c, and d are represented on the basis of weight, wherein a is 20 to 90, b is 0.01 to 10, c is 0.01 to 5, and d is 5 to 50.

Abstract translation: 本发明涉及由下式1表示的氢化催化剂，其制备方法以及使用该催化剂制备γ-丁内酯的方法。 使用通过用二氧化硅稳定氧化铜，氧化锌和氧化锰的前体颗粒制备的本发明的催化剂由马来酸酐制备γ-丁内酯的方法在操作条件下表现出高选择性，高收率和高生产率 氢气与反应物的低摩尔比，并且能够以长期稳定性从马来酸酐制备γ-丁内酯，而不需要频繁地重新活化催化剂：式（I）CuO（a）ZnO（b） （d）其中a，b，c和d以重量为基准表示，其中a为20-90，b为 0.01〜10，c为0.01〜5，d为5〜50。

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

Inventor： 이정호 ,  김형록 ,  한요한 ,  정석종 ,  최낙모 ,  우항수 ,  김인기

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。

公开(公告)号：KR100431898B1

公开(公告)日：2004-05-17

申请号：KR1020010047151

申请日：2001-08-04

Applicant: 한국화학연구원 ,  에이케이홀딩스 주식회사

Inventor： 이정호 ,  김형록 ,  한요한 ,  신현관 ,  최낙모 ,  우항수 ,  김인기 ,  김성재 ,  주동균

IPC: B01J23/72 ,  B01J21/08 ,  B82Y30/00

Abstract: PURPOSE: A preparation method of silica stabilized copper catalyst used in hydrogenating or dehydrogenating organic compounds is provided, and the catalyst prepared by the method is provided. CONSTITUTION: The preparation method of Cu/SiO2 catalyst comprises the steps of (a) preparing a slurry solution of copper hydroxide by adding a precipitant solution to an aqueous copper salt solution; (b) preparing a copper hydroxide-silica slurry solution by stirring the mixed solution after adding a colloidal silica solution to the slurry solution; (c) separating sediments from the solution and cleaning the sediment after aging the copper hydroxide-silica slurry solution at a temperature of 50 to 100 deg.C; and (d) drying and baking the cleaned sediment, wherein the precipitant is carbonate or hydroxide of alkaline metal, a weight ratio of copper oxide (CuO) to silica (SiO2) of catalyst is 9:1 to 3:7, the colloidal silica is stabilized by ammonium (NH4¬+), Na¬+ or other alkali metal, has a particle size of 4 to 60 nm, surface area of 100 to 300 m¬2/g and concentration of 5 to 60 wt.% on the basis of silica, and the aging is performed at a temperature of 60 to 90 deg.C for 0.5 to 24 hours.

Abstract translation: 目的：提供一种用于有机化合物加氢或脱氢的二氧化硅稳定的铜催化剂的制备方法，并提供该方法制备的催化剂。 构成：Cu / SiO2催化剂的制备方法包括以下步骤：（a）通过向铜盐水溶液中加入沉淀剂溶液制备氢氧化铜浆液; （b）在将所述胶体二氧化硅溶液加入到所述浆液中之后搅拌所述混合溶液来制备氢氧化铜 - 二氧化硅浆液; （c）在50-100℃的温度下老化氢氧化铜 - 二氧化硅浆液后，从溶液中分离沉淀物并清洗沉淀物; （d）将清洗过的沉淀物干燥并烘干，其中沉淀剂为碱金属碳酸盐或氢氧化物，氧化铜（CuO）与催化剂二氧化硅（SiO2）的重量比为9：1至3：7，胶体二氧化硅 由铵（NH 4 +; +）稳定，Na +或其它碱金属具有4-60nm的粒径，100-300m 2 / g的表面积和5-60重量％的浓度 以二氧化硅为基准，老化在60〜90℃的温度下进行0.5〜24小时。

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

Inventor： 이정호 ,  김형록 ,  한요한 ,  정석종 ,  최낙모 ,  우항수 ,  김인기

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。

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

Inventor： 이정호 ,  김형록 ,  한요한 ,  신현관 ,  김정곤 ,  우항수 ,  이정훈

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.