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公开(公告)号：KR1020010028430A
公开(公告)日：2001-04-06
申请号：KR1019990040680
申请日：1999-09-21
Applicant: 한국과학기술연구원
IPC: B01J23/20 , B01J35/10 , C07D223/10 , C07B61/00
CPC classification number: B01J29/049 , C07D201/04 , Y02P20/52
Abstract: PURPOSE: Disclosed are a porous catalyst composed of pillard silica and metal oxide and a preparation method of ε-caprolactam from cyclohexanone oxime. CONSTITUTION: The porous catalyst is mainly composed of a pillard silica and a metal oxide. The sodium ion (Na+) on pillard silica is substituted with hydrogen ion (H+) of inorganic acid solution and a spacing width of pillard silica expands to 20 - 30 Å by using a long chained amine compound. And then metal oxide compounds are added in the spacing interval of the pillared silica. The added content of metal oxide is optimally 2 - 10 wt% and the surface area is 100 - 300 m2/g. The pillared silica is precipitated from kanemite, kenyaite, magadite, illite, octosilicate and Ta2O5, Nb2O5, TiO2 or SiO2 are used as metal oxides.
Abstract translation: 目的：公开了由二氧化硅和金属氧化物组成的多孔催化剂和由环己酮肟制备的ε-己内酰胺的制备方法。 构成：多孔催化剂主要由二氧化硅和金属氧化物组成。 使用长链胺化合物，将二氧化硅上的钠离子（Na +）用无机酸溶液的氢离子（H +）代替，并将二氧化硅的间隔宽度扩大至20〜30。 然后在柱状二氧化硅的间隔间隔中加入金属氧化物。 金属氧化物的添加量最好为2〜10重量％，表面积为100〜300m2 / g。 柱状二氧化硅从可卡因，肯尼亚，magadite，伊利石，八硅酸盐和Ta 2 O 5，Nb 2 O 5，TiO 2或SiO 2中析出用作金属氧化物。
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公开(公告)号：KR1020010004825A
公开(公告)日：2001-01-15
申请号：KR1019990025559
申请日：1999-06-30
Applicant: 한국과학기술연구원
IPC: B01J29/70
CPC classification number: B01J37/0009 , B01J29/70 , C07D201/04
Abstract: PURPOSE: Provided are a process for preparing a zeolite catalyst and a process for preparing ε-caprolactam from cyclohexanone oxime in the presence of the zeolite catalyst by Beckmann conversion reaction. CONSTITUTION: The MFI and MEL type zeolite catalysts having a molar ratio of Si/Al being more than 500 is treated at 20-150 °C with 0.01-0.5 N by concentration of an acid selected from the group consisting of hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, and acetic acid. The ε-caprolactam is prepared from cyclohexanone oxime by Beckman conversion reaction at 250-400 °C in the presence of the acid treated zeolite catalyst.
Abstract translation: 目的：提供一种沸石催化剂的制备方法以及通过Beckmann转化反应在沸石催化剂存在下由环己酮肟制备ε-己内酰胺的方法。 构成：将Si / Al的摩尔比大于500的MFI和MEL型沸石催化剂在20-150℃下通过浓度为0.01-0.5N的酸处理，所述酸选自盐酸，硝酸 ，硫酸，磷酸和乙酸。 通过Beckman转化反应在250-400℃，在酸处理的沸石催化剂的存在下，由环己酮肟制备ε-己内酰胺。
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公开(公告)号：KR1020040042720A
公开(公告)日：2004-05-20
申请号：KR1020020071308
申请日：2002-11-15
IPC: B01J21/08
CPC classification number: B01J21/08 , B01J35/1019 , B01J37/08 , B01J37/30 , C07D201/04
Abstract: PURPOSE: Provided are a metal ion impregnated porous catalyst and a method for preparing thereof, which is able to increase the yield of a conversion rate of cyclohexanone oxime and ε-caprolactam and provides safe, economical, environmental-friendly and life span extended metal ion, and a method for preparing ε-caprolactam from cyclohexanone oxime using the catalyst. CONSTITUTION: The metal ion impregnated porous catalyst has pores formed by metal oxide pillar introduced between layers of layered silica compound, wherein the metal ion is impregnated in pores. The method comprises steps of (a) synthesizing a layered silica compound; (b) acid-ion exchanging the synthesized layered silica compound by acid titration; (c) forming pores between layers of layered silica compound by adding organic metal to the acid-ion exchanged layered silica compound and sintering; and (d) supporting the surface of the pores in metal ion by adding an aqueous solution of the metal ion thereto and sintering. The ε-caprolactam is prepared by gaseous beckmann conversion of cyclohexanone oxime solution using the metal ion impregnated porous catalyst.
Abstract translation: 目的：提供一种金属离子浸渍多孔催化剂及其制备方法，其能够提高环己酮肟和ε-己内酰胺的转化率的产率，并提供安全，经济，环保和寿命延长的金属离子 以及使用该催化剂从环己酮肟制备ε-己内酰胺的方法。 构成：金属离子浸渍多孔催化剂具有由层状二氧化硅化合物层之间引入的金属氧化物柱形成的孔，其中金属离子浸渍在孔中。 该方法包括以下步骤：（a）合成层状二氧化硅化合物; （b）通过酸滴定将合成的层状二氧化硅化合物进行酸离子交换; （c）通过向酸离子交换的层状二氧化硅化合物中加入有机金属并烧结而在层状二氧化硅化合物的层之间形成孔; 和（d）通过向其中加入金属离子的水溶液并进行烧结来支撑金属离子中的孔的表面。 使用金属离子浸渍的多孔催化剂，通过环己酮肟溶液的气态贝克曼转化制备ε-己内酰胺。
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Patent Agency Ranking
公开(公告)号：KR100333495B1
公开(公告)日：2002-04-25
申请号：KR1019990030397
申请日：1999-07-26
Applicant: 한국과학기술연구원
IPC: C01B39/00
Abstract: 본발명은분자체골격을이루고있는구성원소가갈륨과규소산화물로된 기스몬다인구조를갖는분자체및 이의제조방법을제공하여, 규소와알루미늄이외에다른원소를분자체에도입하여그 골격성분의몰비를자유롭게조절할수 있어촉매활성에필요한분자체의산성질을자유롭게조절할수 있을뿐만아니라새로도입한원소고유의촉매특성도이용가능하며또한몰비를낯추어분자체의이온교환능을상당히개선시킬시킬수 있다.
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公开(公告)号：KR100333494B1
公开(公告)日：2002-04-25
申请号：KR1019990030396
申请日：1999-07-26
Applicant: 한국과학기술연구원
IPC: C01B39/02
Abstract: 본발명은분자체골격을이루고있는구성원소가알루미늄과게르마늄산화물로된 기스몬다인구조를갖는분자체및 이의제조방법을제공하여, 규소와알루미늄이외에다른원소를분자체에도입하여그 골격성분의몰비를자유롭게조절할수 있어촉매활성에필요한분자체의산성질을자유롭게조절할수 있을뿐만아니라새로도입한원소고유의촉매특성도이용가능하며또한몰비를낯추어분자체의이온교환능을상당히개선시킬시킬수 있다.
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公开(公告)号：KR100327157B1
公开(公告)日：2002-03-13
申请号：KR1019990025559
申请日：1999-06-30
Applicant: 한국과학기술연구원
IPC: B01J29/70
Abstract: 본발명은제올라이트촉매의제조방법및 이촉매를이용하여베크만전환반응에의해시클로헥사논옥심으로부터ε-카프로락탐을제조하는방법에관한것으로, 제올라이트촉매의제조방법은, MFI, MEL형의제올라이트촉매의제조에있어서, Si/Al의몰비가 500 이상되도록제조된촉매를산으로더 처리해주는단계를포함하는것을특징으로하고, ε-카프로락탐의제조방법은, Si/Al의몰비가 500 이상이고산으로더 처리된제올라이트촉매를사용하여기상의베크만전환반응에의해시클로헥사논옥심으로부터ε-카프로락탐을제조하는것을특징으로한다. 본발명에따르면, 제올라이트촉매가시클로헥사논옥심의베크만전환반응에서시클로헥사논옥심의전환율과ε-카프로락탐의선택도를더욱높여줄 뿐만 아니라촉매의수명이연장되게되며, 이러한촉매를이용하여시클로헥사논옥심으로부터ε-카프로락탐을경제적이고효율적으로제조할수 있게된다.
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公开(公告)号：KR1020010011156A
公开(公告)日：2001-02-15
申请号：KR1019990030397
申请日：1999-07-26
Applicant: 한국과학기술연구원
IPC: C01B39/00
CPC classification number: C01B39/082
Abstract: PURPOSE: A preparation method of gallosilicate molecular sieve with a gismondine structure in K2O-Ga2O3-SiO2-H2O system is provided to control the molar ratio of structure components freely by substituting Ga and K for Al and Na of zeolite, respectively. The gallosilicate molecular sieve is applicable to catalysts, adsorbents and ion exchangers. CONSTITUTION: The gallosilicate molecular sieve is prepared by the following steps: mixing H2O, KOH, and a source of Ga such as gallium oxide or Ga2O3xH2O for 2-4hrs.; heating it for 12-24hrs. and cooling to room temperature; adding a source of Si such as colloid silica, sodium silicate and fumed silica, and stirring for 4-24hrs., resulting in a gel represented as vK2O : 1.0Ga2O3 : wSiO2 : zH2O (v=6.0-8.0, w=5.0-15.0, z=50-250); heating at 80-130deg.C for 1-10days; washing with H2O and drying.
Abstract translation: 目的：提供K2O-Ga2O3-SiO2-H2O体系中具有结晶组分的硅酸盐分子筛的制备方法，通过分别用Ga和K代替沸石的Al和Na来自由控制结构组分的摩尔比。 硅酸盐分子筛适用于催化剂，吸附剂和离子交换剂。 构成：通过以下步骤制备聚硅酸盐分子筛：将H 2 O，KOH和诸如氧化镓或Ga 2 O 3 xH 2 O的Ga源混合2-4小时。 加热12-24小时。 并冷却至室温; 加入Si胶体硅胶，硅酸钠和煅制二氧化硅等硅源，搅拌4〜24h，得到表示为vK2O的凝胶：1.0Ga 2 O 3 :WSiO 2 :zH 2 O（v = 6.0-8.0，w = 5.0〜15.0 ，z = 50-250）; 加热80-130℃，持续1-10天; 用H2O洗涤并干燥。
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