CZ308473B6 - Způsob izolace ɛ-kaprolaktamu z horní laktamové fáze - Google Patents

Způsob izolace ɛ-kaprolaktamu z horní laktamové fáze

Info

Publication number
CZ308473B6
CZ308473B6 CZ2018-651A CZ2018651A CZ308473B6 CZ 308473 B6 CZ308473 B6 CZ 308473B6 CZ 2018651 A CZ2018651 A CZ 2018651A CZ 308473 B6 CZ308473 B6 CZ 308473B6
Authority
CZ
Czechia
Prior art keywords
caprolactam
phase
mixture
pressure
kpa
Prior art date
Application number
CZ2018-651A
Other languages
English (en)
Other versions
CZ2018651A3 (cs
Inventor
Jiří Trejbal
Martin ZAPLETAL
Original Assignee
Vysoká škola chemicko-technologická v Praze
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Vysoká škola chemicko-technologická v Praze filed Critical Vysoká škola chemicko-technologická v Praze
Priority to CZ2018-651A priority Critical patent/CZ308473B6/cs
Priority to PL19211707T priority patent/PL3660002T3/pl
Priority to EP19211707.5A priority patent/EP3660002B1/en
Publication of CZ2018651A3 publication Critical patent/CZ2018651A3/cs
Publication of CZ308473B6 publication Critical patent/CZ308473B6/cs

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/42—Platinum
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/44—Palladium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/46—Ruthenium, rhodium, osmium or iridium
    • B01J23/462—Ruthenium
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D201/00—Preparation, separation, purification or stabilisation of unsubstituted lactams
    • C07D201/02—Preparation of lactams
    • C07D201/04—Preparation of lactams from or via oximes by Beckmann rearrangement
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D201/00—Preparation, separation, purification or stabilisation of unsubstituted lactams
    • C07D201/16—Separation or purification
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D223/00—Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom
    • C07D223/02—Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom not condensed with other rings
    • C07D223/06—Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D223/08—Oxygen atoms
    • C07D223/10—Oxygen atoms attached in position 2

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Other In-Based Heterocyclic Compounds (AREA)
  • Polyamides (AREA)

Abstract

Řešení se týká způsobu izolace ε-kaprolaktamu z horní laktamové fáze získané oddělením od síranové fáze po neutralizaci reakční směsi získané z Beckmanova přesmyku cyklohexyloximu amoniakem, při kterém se tato horní laktamová fáze nejprve destiluje za sníženého nebo atmosférického tlaku, čímž se sníží obsah vody v ní na 5 až 10 % hmotn., poté se z ní mechanicky odstraní pevná fáze, která vzniká při destilaci, a takto získaná zkoncentrovaná směs se destiluje při tlaku 0,1 až 4 kPa, přičemž se z ní odstraňují netěkavé složky. V takto získaném destilátu přídavkem rozpouštědla ze skupiny voda, methanol, ethanol, propanol, iso-propylalkohol nebo směs alespoň dvou z nich se upraví koncentrace ε-kaprolaktamu na 30 až 70 % hmotn. a takto vytvořená směs se hydrogenuje při teplotě 100 až 150 °C a tlaku vodíku 1 až 10 MPa v přítomnosti heterogenního nosičového katalyzátoru, který obsahuje alespoň jeden vzácný kov ze skupiny Pd, Pt, Ru, přičemž dochází k redukci násobných vazeb přítomných nečistot. Takto vytvořený rafinát se rektifikuje v sérii alespoň dvou rektifikačních kolon, které pracují při tlaku 0,05 až 4 kPa se souhrnnou minimální účinností soustavy kolon 10 teoretických pater, přičemž se z něj rektifikací oddělují lehké podíly a těžké zbytky, čím se z něj současně izoluje ε-kaprolaktam.
CZ2018-651A 2018-11-27 2018-11-27 Způsob izolace ɛ-kaprolaktamu z horní laktamové fáze CZ308473B6 (cs)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CZ2018-651A CZ308473B6 (cs) 2018-11-27 2018-11-27 Způsob izolace ɛ-kaprolaktamu z horní laktamové fáze
PL19211707T PL3660002T3 (pl) 2018-11-27 2019-11-27 Sposób wyodrębniania kaprolaktamu z górnej fazy laktamowej obejmujący etapy 1) destylacji, 2) rafinacji wodorem w obecności katalizatora z metalu szlachetnego, i 3) rektyfikacji
EP19211707.5A EP3660002B1 (en) 2018-11-27 2019-11-27 Method for isolating caprolactam from the upper lactam phase comprising the steps of 1) distillation, 2) refining with hydrogen in the presence of a nobel metal catalyst and 3) rectification

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CZ2018-651A CZ308473B6 (cs) 2018-11-27 2018-11-27 Způsob izolace ɛ-kaprolaktamu z horní laktamové fáze

Publications (2)

Publication Number Publication Date
CZ2018651A3 CZ2018651A3 (cs) 2020-06-03
CZ308473B6 true CZ308473B6 (cs) 2020-09-09

Family

ID=69156142

Family Applications (1)

Application Number Title Priority Date Filing Date
CZ2018-651A CZ308473B6 (cs) 2018-11-27 2018-11-27 Způsob izolace ɛ-kaprolaktamu z horní laktamové fáze

Country Status (3)

Country Link
EP (1) EP3660002B1 (cs)
CZ (1) CZ308473B6 (cs)
PL (1) PL3660002T3 (cs)

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0065168A1 (en) * 1981-05-09 1982-11-24 Stamicarbon B.V. Process for the purification of epsilon caprolactam
JPH05230015A (ja) * 1992-02-19 1993-09-07 Mitsubishi Kasei Corp カプロラクタムの精製法
CN104072419A (zh) * 2013-10-28 2014-10-01 中国石油化工股份有限公司 一种己内酰胺的纯化方法和纯化装置
CN104557707A (zh) * 2013-10-28 2015-04-29 中国石油化工股份有限公司 一种己内酰胺加氢精制方法
CN107551598A (zh) * 2017-09-28 2018-01-09 神马实业股份有限公司 一种己内酰胺的结晶装置及使用方法
CN108409658A (zh) * 2018-04-24 2018-08-17 河北美邦工程科技股份有限公司 一种己内酰胺的高效精制方法

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
NL277685A (cs) 1961-04-27
PL120112B3 (en) 1978-10-10 1982-02-27 Akad Gorniczo Hutnicza Large-diameter rotary stabilizer for a dril pipe string ril'nojj kolonny
DE3925575A1 (de) 1989-08-02 1991-02-07 Basf Ag Verfahren zur kontinuierlichen reinigung von caprolactam
PL210210B1 (pl) 2007-01-31 2011-12-30 Inst Chemii Przemysłowej Im Prof Ignacego Mościckiego Sposób wytwarzania ε-kaprolaktamu
TWI520944B (zh) * 2015-02-13 2016-02-11 中國石油化學工業開發股份有限公司 己內醯胺之製造方法及其系統

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0065168A1 (en) * 1981-05-09 1982-11-24 Stamicarbon B.V. Process for the purification of epsilon caprolactam
JPH05230015A (ja) * 1992-02-19 1993-09-07 Mitsubishi Kasei Corp カプロラクタムの精製法
CN104072419A (zh) * 2013-10-28 2014-10-01 中国石油化工股份有限公司 一种己内酰胺的纯化方法和纯化装置
CN104557707A (zh) * 2013-10-28 2015-04-29 中国石油化工股份有限公司 一种己内酰胺加氢精制方法
CN107551598A (zh) * 2017-09-28 2018-01-09 神马实业股份有限公司 一种己内酰胺的结晶装置及使用方法
CN108409658A (zh) * 2018-04-24 2018-08-17 河北美邦工程科技股份有限公司 一种己内酰胺的高效精制方法

Also Published As

Publication number Publication date
EP3660002A1 (en) 2020-06-03
PL3660002T3 (pl) 2021-09-27
EP3660002B1 (en) 2021-02-17
CZ2018651A3 (cs) 2020-06-03

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