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61.发明公开무수말레인산으로부터 감마-부티로락톤을 제조하는 기상수소화 촉매, 그 촉매의 제조 방법 및 그 촉매를 사용하여감마-부티로락톤의 제조 방법 失效用于从非水性马来酸生产丁酮的气相氢化催化剂，其制备方法和使用相同催化剂的丁酮的制备方法
公开(公告)号：KR1020020008600A
公开(公告)日：2002-01-31
申请号：KR1020000042410
申请日：2000-07-24
Applicant: 한국화학연구원 , 에이케이홀딩스 주식회사
IPC: B01J23/78 , C07D307/32 , B01J23/72
CPC classification number: B01J23/8926 , B01J23/78 , B01J23/835 , B01J23/8896 , B01J37/0009 , B01J37/08 , C07D307/33
Abstract: PURPOSE: A catalyst suitable for producing γ-butyrolactone from anhydrous maleic acid under mild reaction conditions with high selectivity and yield. γ-butyrolactone, used to prepare solvents such as pyrrolidone or N-methylpyrrolidone and also used as an intermediate to synthesize N-vinylpyrrolidone, polyvinylpyrrolidone, butanediol and tetrahydrofuran, is widely used over various industries, including pesticides, drugs, dyes, petrochemicals and electronic chemicals. CONSTITUTION: The catalyst is represented by the chemical formula 1, £CuO(a)· SiO2(b)|(100-x)M(x), where M is one or more oxides selected from Re, Ag, Sn, N, K, Mg and Ca; 'a' is an integer of 20 to 99; 'b' is an integer of 1 to 80; and 'x' ranging from 0.001 to 5 represents weight percentage. Further, CuO occupies preferably 50-95wt.% in total weight of CuO and SiO2. The catalyst is prepared by (i) addition of colloidal silica having a surface area of 100-300m¬2, a hydrogen-ion concentration of pH8-10 in a copper salt solution; (ii) coprecipitation of the mixture solution with an addition of an alkali solution followed by hydrothermal aging; (iii) washing the hydrothermally aged solution with deionized water after filtration, and then drying; (iv) supporting CuO catalyst with the precursor of M (referred in chemical formula I) in such a manner that M is supported into the CuO catalyst being dissolved in an organic solvent or water. According to the present invention, γ-butyrolactone is manufactured by after activating the present catalyst, supplying a gaseous mixture of anhydrous maleic acid and hydrogen in the presence of the activated catalyst, and then reacting at 220-350deg.C under a pressure of normal pressure to 20atm.
Abstract translation: 目的：一种适用于在温和反应条件下从无水马来酸生产γ-丁内酯的催化剂，具有高选择性和产率。 用于制备溶剂如吡咯烷酮或N-甲基吡咯烷酮的γ-丁内酯，也用作合成N-乙烯基吡咯烷酮，聚乙烯吡咯烷酮，丁二醇和四氢呋喃的中间体，广泛应用于各种行业，包括农药，药物，染料，石油化工和电子 化学品。 构成：催化剂由化学式1代表，CuO（a）·SiO2（b）|（100-x）M（x），其中M是一种或多种选自Re，Ag，Sn，N， K，Mg和Ca; 'a'是20到99的整数; 'b'为1〜80的整数。 而“x”的范围从0.001到5表示重量百分数。 此外，CuO优选占CuO和SiO 2总重量的50-95wt。％。 催化剂通过以下步骤制备：（i）在铜盐溶液中加入表面积为100-300m 2的胶体二氧化硅，pH8-10的氢离子浓度; （ii）通过加入碱溶液然后水热老化使混合溶液共沉淀; （iii）过滤后用去离子水洗涤水热老化溶液，然后干燥; （iv）以M的前体（化学式I所述）负载CuO催化剂，使得M被负载到溶解在有机溶剂或水中的CuO催化剂中。 根据本发明，通过活化本催化剂，在活化催化剂存在下，供给无水马来酸和氢气的气体混合物，然后在220-350℃，在正常压力下反应制备γ-丁内酯 压力为20atm。
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公开(公告)号：KR1020010103946A
公开(公告)日：2001-11-24
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 상~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.-
公开(公告)号：KR1020010103945A
公开(公告)日：2001-11-24
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 0.0001~1.0중량를 공급하여 반응시키는 것을 특징으로 하는 감마-부티로락톤의 제조방법에 관한 것이다.
본 발명의 방법은 무수말레인산이나 무수석신산을 수소화 반응시켜 감마-부티로락톤을 제조하는 방법에 있어서, 반응물에 0.1중량이하의 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：KR1019960010080B1
公开(公告)日：1996-07-25
申请号：KR1019930006150
申请日：1993-04-13
Applicant: 한국화학연구원
IPC: B01J21/16
Abstract: TtLl(SP)m-[M(II)1-xM(III)x(OH)2 X+(Ax/n)= yH2O) is one that anion phosphine metal complex(eqn 1: TtLl(SP)m) is coupled between layers of hydrotalcite compound (eqn 2: [M(II)1-xM(III)x(OH)2 X+(Ax/n)= yH2O), where T is Rh, Co, Ru, Ir, Pt, Ni, Cu, Mn, Fe, Pd, Ag or Au; L is Cl, CO, NO, COD, H, SR, OH, NH3 or alkylamine; SP is anion phosphine ligand, sulfonated or carbonated alkyl or anion allyl phosphine; t is 1-2; l is 0-8; m is 1-8; M(II) is Mg, Ni, Co, Fe, An, Cu or Li; M(III) is Al, Cr or Fe; A is organic or inorganic anion with quantity of electric charge of n; X is 0.2-0.4; n is the quantity of electric charge of A; y is the number of water molecule.
Abstract translation: Ttll（SP）m- [M（II）1-xM（III）x（OH）2 X +（Ax / n）= yH2O）是阴离子膦金属络合物（等式1：TtL1（SP） 水滑石化合物层（方程2：[M（II）1-xM（III）x（OH）2 X +（Ax / n）= yH 2 O），其中T是Rh，Co，Ru，Ir，Pt，Ni， Cu，Mn，Fe，Pd，Ag或Au; L是Cl，CO，NO，COD，H，SR，OH，NH 3或烷基胺; SP是阴离子膦配体，磺化或碳酸化烷基或阴离子烯丙基膦; t是1-2; l为0-8; m为1-8; M（II）是Mg，Ni，Co，Fe，An，Cu或Li; M（III）为Al，Cr或Fe; A是电荷量为n的有机或无机阴离子; X为0.2-0.4; n是A的电荷量; y是水分子的数量。
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65.发明授权
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Patent Agency Ranking
公开(公告)号：KR1019960003795B1
公开(公告)日：1996-03-22
申请号：KR1019930006148
申请日：1993-04-13
Applicant: 한국화학연구원
IPC: B01J27/199
Abstract: This is new heteropolyacid-based catalyst of formula (I). The manufacturing method comprises :1)dissolving 12-molybdophosphoric acid in water followed by adding phosphoric acid and vanadium pentoxide; 2)refluxing the mixture for 12hrs at an elevated temp. to produce molybdovanadophosphoric acid solution(A); 3)dissolving one kind of Cu, Ce, Ru, Bi, Sb N-heterocyclic compd and above one of oxalic acid or its salts(B); 4)adding solution B to solution A with stirring at 30-80deg.C and maturing the stirred mixture; 5)cooling it to room temp and stirring for 30min, filtering and washing it; 6)drying the cake and molding; and 7)1st firing at 380-450deg.C for 2-10hrs, and 2nd firing at 260-420deg.C for 2-10hrs.
Abstract translation: 这是式（I）的新型杂多酸催化剂。 制造方法包括：1）将12-钼磷酸溶解在水中，然后加入磷酸和五氧化二钒; 2）在升高的温度下将混合物回流12小时。 生产钼钒磷酸溶液（A）; 3）溶解一种草酸或其盐（B）中的一种Cu，Ce，Ru，Bi，Sb N-杂环化合物; 4）将溶液B在30-80℃搅拌下加入到溶液A中，熟化搅拌的混合物; 5）将其冷却至室温并搅拌30分钟，过滤并洗涤; 6）干燥蛋糕和成型; 7）第一次烧制380-450℃2-10小时，第二次焙烧260-420℃2-10小时。
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公开(公告)号：KR1019940001849B1
公开(公告)日：1994-03-09
申请号：KR1019910007017
申请日：1991-05-01
Applicant: 한국화학연구원
IPC: C07C69/54
Abstract: The method producing methyl metacrylate or ethyl metacrylate continuosly and recovering non-reaction metacrylic acid and alcohols. Metacrylic acid is synthesized by gas-phase catalytic oxidizing at least one compound of isobutylene, t-butanol and metacrolein. In manufacturing metacrylic acid ester with metacrylic acid, alcohol and solid-acid catalyst, the reaction temp is 60-130 deg.C, and pressure is 0-30 psig. A fluidized bed catalyst reactor is used for continuous production. Mixing solvents selected from aromatics such as ethylbenzene, xylene and cumene and from aliphatic such as nonane, decane, decaline and tetraline are used as esterification solvent. The above solid-acid catalyst are porous polystyrene base cation exchange resin and fluorine base cation exchange resin.
Abstract translation: 连续制造甲基丙烯酸甲酯或甲基丙烯酸乙酯的方法，回收非反应的甲基丙烯酸和醇。 甲基丙烯酸通过气相催化氧化至少一种异丁烯，叔丁醇和甲基丙烯醛化合物合成。 在用甲基丙烯酸，醇和固体酸催化剂制备甲基丙烯酸酯时，反应温度为60-130℃，压力为0-30psig。 流化床催化反应器用于连续生产。 作为酯化溶剂，使用选自芳族化合物如乙苯，二甲苯和枯烯的混合溶剂和来自脂肪族如壬烷，癸烷，十氢萘和四氢萘的混合溶剂。 上述固体酸催化剂是多孔聚苯乙烯基阳离子交换树脂和氟碱阳离子交换树脂。
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