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1. (WO2018121042) PRODUCTION METHOD FOR HIGH-QUALITY PURE HEXANEDIAMINE
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Pub. No.: WO/2018/121042 International Application No.: PCT/CN2017/108867
Publication Date: 05.07.2018 International Filing Date: 06.11.2017
IPC:
C07C 211/12 (2006.01) ,C07C 209/48 (2006.01) ,C07C 209/84 (2006.01)
C CHEMISTRY; METALLURGY
07
ORGANIC CHEMISTRY
C
ACYCLIC OR CARBOCYCLIC COMPOUNDS
211
Compounds containing amino groups bound to a carbon skeleton
01
having amino groups bound to acyclic carbon atoms
02
of an acyclic saturated carbon skeleton
09
Diamines
12
1,6-Diaminohexanes
C CHEMISTRY; METALLURGY
07
ORGANIC CHEMISTRY
C
ACYCLIC OR CARBOCYCLIC COMPOUNDS
209
Preparation of compounds containing amino groups bound to a carbon skeleton
44
by reduction of carboxylic acids or esters thereof in presence of ammonia or amines, or by reduction of nitriles, carboxylic acid amides, imines or imino-ethers
48
by reduction of nitriles
C CHEMISTRY; METALLURGY
07
ORGANIC CHEMISTRY
C
ACYCLIC OR CARBOCYCLIC COMPOUNDS
209
Preparation of compounds containing amino groups bound to a carbon skeleton
82
Purification; Separation; Stabilisation; Use of additives
84
Purification
Applicants:
河南神马尼龙化工有限责任公司 HENAN SHENMA NYLON CHEMICAL CO., LTD. [CN/CN]; 中国河南省平顶山市 建设路高新技术开发区711号 No. 711, High-tech Development District, Jianshe Road Pingdingshan, Henan 467013, CN
Inventors:
乔思怀 QIAO, Sihuai; CN
赵铎 ZHAO, Duo; CN
陈聚良 CHEN, Juliang; CN
高先明 GAO, Xianming; CN
王海营 WANG, Haiying; CN
王红专 WANG, Hongzhuan; CN
郭卫东 GUO, Weidong; CN
欧玲 OU, Ling; CN
黄敏 HUANG, Min; CN
白湘涛 BAI, Xiangtao; CN
刘水侠 LIU, Shuixia; CN
赵时超 ZHAO, Shichao; CN
刘耀文 LIU, Yaowen; CN
李振锋 LI, Zhenfeng; CN
霍美菊 HUO, Meiju; CN
刘永 LIU, Yong; CN
张军伟 ZHANG, Junwei; CN
Agent:
郑州联科专利事务所(普通合伙) ZHENGZHOU LIANKE PATENT AGENCY (COMMON PARTNERSHIP); 中国河南省郑州市 郑东新区黄河南路宏图街西100米璞居大厦5楼 Floor 5, Puju Building, 100 meters West Hongtu Street South Huanghe Road, Zhengdong New District Zhengzhou, Henan 450046, CN
Priority Data:
201611224721.627.12.2016CN
Title (EN) PRODUCTION METHOD FOR HIGH-QUALITY PURE HEXANEDIAMINE
(FR) PROCÉDÉ DE PRODUCTION D'HEXANEDIAMINE PURE DE HAUTE QUALITÉ
(ZH) 一种高品质精己二胺的生产方法
Abstract:
(EN) Disclosed is a production method for high-quality pure hexanediamine, comprising: preparing a half-finished hexanediamine and purifying high-quality pure hexanediamine, specifically, uniformly mixing adiponitrile, ethanol, and sodium hydroxide according to a certain mass ratio, and adding a nickel-based catalyst for hydrogenation reaction to obtain the half-finished hexanediamine; subjecting the half-finished hexanediamine to distillation and purification for several times to obtain high-quality pure hexanediamine. The present invention adopts ethanol as a diluent, facilitating recycling, and adopts the nickel-based catalyst as a cocatalyst, guaranteeing the conversion rate of hexanediamine; vacuum rectification technology is adopted to dewater, remove light components and heavy components under a vacuum condition according to different boiling points of impurities in the half-finished hexanediamine to finally obtain high-quality pure hexanediamine with the purity≥99.9% (mass percentage), polarogram value≤100 mmolIB/T-HMD and total volatile alkali≤4 mL/100 g.
(FR) L'invention concerne un procédé de production d'hexanediamine pure de haute qualité, consistant à : préparer une hexanediamine semi-finie et purifier l'hexanediamine pure de haute qualité, plus particulièrement, mélanger uniformément de l'adiponitrile, de l'éthanol et de l'hydroxyde de sodium selon un certain rapport massique et ajouter un catalyseur à base de nickel pour une réaction d'hydrogénation afin d'obtenir l'hexanediamine semi-finie ; soumettre l'hexanediamine semi-finie à une distillation et à une purification à plusieurs reprises pour obtenir une hexanediamine pure de haute qualité. La présente invention adopte de l'éthanol en tant que diluant, facilitant le recyclage, et adopte le catalyseur à base de nickel en tant que cocatalyseur, garantissant le taux de conversion de l'hexanediamine ; une technologie de rectification sous vide est adoptée pour déshydrater, éliminer les constituants légers et les constituants lourds dans une condition de vide selon des points d'ébullition différents des impuretés dans l'hexanediamine semi-finie pour obtenir finalement une hexanediamine de haute qualité présentant une pureté ≥ 99,9 % (pourcentage en masse), une valeur de polarogrammes ≤ 100 mmoles IB/T-HMD et une teneur totale en alcali volatil ≤ 4 ml/100 g.
(ZH) 本发明公开了一种高品质精己二胺的生产方法,包括半成品己二胺的制备和高品质精己二胺的提纯,具体是将己二腈、乙醇、氢氧化钠按一定质量比混合均匀,再加入镍基催化剂,进行加氢反应,得到半成品己二胺;然后将半成品己二胺进行多次蒸馏提纯,即得高品质精己二胺。本发明采用乙醇作稀释剂,有利于回收、再利用,采用镍基催化剂作助催化剂,保证了己二胺的转化率;采用真空精馏技术,根据半成品己二胺中杂质的沸点不同,在真空条件下经过脱水、脱除轻组分、脱除重组分,最后得到纯度≥99.9%(质量百分比)、极谱值≤100mmolIB/T-HMD、总挥发碱≤4mL/100g的高品质精己二胺产品。
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Designated States: AE, AG, AL, AM, AO, AT, AU, AZ, BA, BB, BG, BH, BN, BR, BW, BY, BZ, CA, CH, CL, CN, CO, CR, CU, CZ, DE, DJ, DK, DM, DO, DZ, EC, EE, EG, ES, FI, GB, GD, GE, GH, GM, GT, HN, HR, HU, ID, IL, IN, IR, IS, JO, JP, KE, KG, KH, KN, KP, KR, KW, KZ, LA, LC, LK, LR, LS, LU, LY, MA, MD, ME, MG, MK, MN, MW, MX, MY, MZ, NA, NG, NI, NO, NZ, OM, PA, PE, PG, PH, PL, PT, QA, RO, RS, RU, RW, SA, SC, SD, SE, SG, SK, SL, SM, ST, SV, SY, TH, TJ, TM, TN, TR, TT, TZ, UA, UG, US, UZ, VC, VN, ZA, ZM, ZW
African Regional Intellectual Property Organization (ARIPO) (BW, GH, GM, KE, LR, LS, MW, MZ, NA, RW, SD, SL, ST, SZ, TZ, UG, ZM, ZW)
Eurasian Patent Office (AM, AZ, BY, KG, KZ, RU, TJ, TM)
European Patent Office (EPO) (AL, AT, BE, BG, CH, CY, CZ, DE, DK, EE, ES, FI, FR, GB, GR, HR, HU, IE, IS, IT, LT, LU, LV, MC, MK, MT, NL, NO, PL, PT, RO, RS, SE, SI, SK, SM, TR)
African Intellectual Property Organization (BF, BJ, CF, CG, CI, CM, GA, GN, GQ, GW, KM, ML, MR, NE, SN, TD, TG)
Publication Language: Chinese (ZH)
Filing Language: Chinese (ZH)