EP0000463A1 - Verfahren zur Trennung von Toluoldiisocyanat aus Herstellungsgemischen - Google Patents

Verfahren zur Trennung von Toluoldiisocyanat aus Herstellungsgemischen Download PDF

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Publication number
EP0000463A1
EP0000463A1 EP78400051A EP78400051A EP0000463A1 EP 0000463 A1 EP0000463 A1 EP 0000463A1 EP 78400051 A EP78400051 A EP 78400051A EP 78400051 A EP78400051 A EP 78400051A EP 0000463 A1 EP0000463 A1 EP 0000463A1
Authority
EP
European Patent Office
Prior art keywords
tdi
residues
temperature
pressure
evaporator
Prior art date
Legal status (The legal status 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 status listed.)
Granted
Application number
EP78400051A
Other languages
English (en)
French (fr)
Other versions
EP0000463B1 (de
Inventor
Pierre Ailloud
Philippe D'haussy
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Rhone Poulenc Chimie de Base SA
Original Assignee
Produits Chimiques Ugine Kuhlmann
Ugine Kuhlmann SA
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 Produits Chimiques Ugine Kuhlmann, Ugine Kuhlmann SA filed Critical Produits Chimiques Ugine Kuhlmann
Publication of EP0000463A1 publication Critical patent/EP0000463A1/de
Application granted granted Critical
Publication of EP0000463B1 publication Critical patent/EP0000463B1/de
Expired legal-status Critical Current

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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
    • B01D3/10—Vacuum distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C263/00—Preparation of derivatives of isocyanic acid
    • C07C263/18—Separation; Purification; Stabilisation; Use of additives
    • C07C263/20—Separation; Purification
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S159/00—Concentrating evaporators
    • Y10S159/10—Organic

Definitions

  • the present invention relates to a process for the separation of toluene diisocyanate (TDI) from manufacturing residues.
  • TDI toluene diisocyanate
  • the Applicant has developed an entirely continuous process for separating TDI from heavy materials, and for extracting these residues in the form of a solid, which has the advantage of being simple, easy to use and reliable. , without foaming or decomposition, the residues containing only low TDI contents.
  • the separation takes place in a stirred and scraped type evaporator, such as that described in BF 2,039,628.
  • the Applicant has provided a solution to this problem which consists in continuously heating the TDI / heavy product mixture on a wall at a maximum temperature of 250 ° C., in evaporating the TDI at a fairly low temperature (100 to 130 ° C. under a pressure of 5 to 20 torr), stirring the mixture for a time sufficient to promote mass transfer.
  • the mixture is gradually brought throughout the apparatus to a temperature of approximately 220 to 260 ° C., while it passes from the viscous state to the pasty state then to the solid state.
  • the agitation must be sufficient to ensure the heat exchange, the progression of the products in the evaporator, the scraping of the solids and the breaking of the foams possibly formed.
  • the volume of the device must be such that it allows sufficient residence time to ensure the exchange of materials (from 15 to 45 minutes).
  • the outgoing solids contain less than 3% TDI. Their temperature can then be without risk of foaming brought to a higher temperature (280 ° C) at the end of the device to evacuate the last traces of TDI.
  • Solid residues in the form of powder or compact granules are taken up by pneumatic transport and sent to an incinerator, while the TDI is condensed in a conventional manner.
  • the process of the invention has the advantages of being able to operate continuously in an entirely automatic and to guarantee all non-pollution conditions. In addition, it requires little thermal or mechanical energy and is therefore very economical.
  • a device of 20 to 25 m2 and 1,600 liters, followed by an extruder, is sufficient to ensure the continuous separation of heavy and TDI from a unit of 30,000 tonnes / year of TDI.
  • a mixture composed of 43% TDI and 57% heavy compounds from the bottom of the concentration column is introduced into the apparatus at a rate of 60 kg / h m2.
  • the device has a heated surface of 0.86 m2 and a total volume of 20 liters and has 2 self-cleaning stirring screws rotating at different speeds. Under a pressure of 12 mm Hg, the mixture is gradually brought to 215 ° C., and is transformed into a powder containing 2.8% of TDI after a residence time of 15 min.
  • the TDI is condensed and collected, and the solid residues are extruded by pressure through a die in the form of granules of 6 mm in diameter and 15 mm in length, at a rate of 30 kg / h.
  • Example 3 shows that a minimum residence time, which we have set at 15 min, is required if we want to obtain a low TDI content in the residues.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
EP78400051A 1977-07-12 1978-07-03 Verfahren zur Trennung von Toluoldiisocyanat aus Herstellungsgemischen Expired EP0000463B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR7721436A FR2397396A1 (fr) 1977-07-12 1977-07-12 Procede de recuperation du toluene diisocyanate a partir des residus de fabrication
FR7721436 1977-07-12

Publications (2)

Publication Number Publication Date
EP0000463A1 true EP0000463A1 (de) 1979-01-24
EP0000463B1 EP0000463B1 (de) 1982-01-06

Family

ID=9193273

Family Applications (1)

Application Number Title Priority Date Filing Date
EP78400051A Expired EP0000463B1 (de) 1977-07-12 1978-07-03 Verfahren zur Trennung von Toluoldiisocyanat aus Herstellungsgemischen

Country Status (17)

Country Link
US (1) US4216063A (de)
EP (1) EP0000463B1 (de)
JP (1) JPS5419938A (de)
AR (1) AR214462A1 (de)
AU (1) AU522377B2 (de)
BR (1) BR7804465A (de)
CA (1) CA1094090A (de)
DD (1) DD138314A5 (de)
DE (1) DE2861504D1 (de)
DK (1) DK154426C (de)
ES (1) ES471637A1 (de)
FR (1) FR2397396A1 (de)
IE (1) IE47024B1 (de)
IN (1) IN148484B (de)
IT (1) IT1111627B (de)
PT (1) PT68171A (de)
SU (1) SU1264840A3 (de)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0017972A1 (de) * 1979-04-19 1980-10-29 BASF Aktiengesellschaft Gewinnung von Toluylendiisocyanat und/oder höhersiedenden Lösungsmitteln im Wirbelbett aus Destillationsrückständen der Toluylendiisocyanat-Herstellung
EP0324701A1 (de) * 1988-01-13 1989-07-19 Rhone-Poulenc Chimie Verfahren zur Trennung von Toluoldiisocyanat aus seinen Herstellungsrückständen
EP0699659A3 (de) * 1994-08-31 1996-06-26 Bayer Ag Verfahren und Vorrichtung zur kontinuierlichen Abtrennung eines festen Rückstandes aus seiner Lösung im gerührten Gutbett
CN104411681A (zh) * 2012-07-11 2015-03-11 拜耳材料科技股份有限公司 后处理由制备异氰酸酯产生的蒸馏残渣的方法

Families Citing this family (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02138567U (de) * 1989-04-21 1990-11-19
US5051152A (en) * 1989-09-26 1991-09-24 Air Products And Chemicals, Inc. Preparation of urethane prepolymers having low levels of residual toluene diisocyanate
JP2504851Y2 (ja) * 1990-02-07 1996-07-24 株式会社シマノ 釣り用リ―ルのリ―ドスイッチ取り付け構造
DE4317669A1 (de) * 1993-05-27 1994-12-01 Bayer Ag Verfahren zur Herstellung von Isocyanaten und kontinuierlichen Aufarbeitung des Rückstandes
US5962728A (en) * 1997-10-31 1999-10-05 Arco Chemical Technology, L.P. Isocyanate residue purification
DE10260092A1 (de) * 2002-12-19 2004-07-01 Basf Ag Verfahren zur Reinigung von Isocyanaten
KR101287282B1 (ko) * 2005-09-29 2013-07-23 바스프 에스이 아이소시아네이트를 함유하는 잔류물의 정제 방법
CN102408354A (zh) * 2011-10-24 2012-04-11 天津大学 一种回收甲苯二异氰酸酯的方法及装置

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3405040A (en) 1965-08-31 1968-10-08 Mobay Chemical Corp Method for recovering tolylene diisocyanate
US3457291A (en) 1965-04-01 1969-07-22 Union Carbide Corp Production of isocyanates
FR2091813A5 (de) 1970-05-22 1972-01-14 Du Pont

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2706169A (en) * 1954-03-04 1955-04-12 Du Pont Flash distillation of 2,4-tolylene diisocyanate
US2974725A (en) * 1954-05-04 1961-03-14 Bayer Ag Process and apparatus for continuously obtaining dry materials
US3542112A (en) * 1968-06-05 1970-11-24 Artisan Ind Thin-film evaporator having multi-zone temperature control jacket
DD130143B1 (de) * 1975-08-15 1979-12-27 Guenter Muecke Verfahren zur kontinuierlichen thermischen abtrennung organischer isocyanate aus fluessigem destillationsrueckstand

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3457291A (en) 1965-04-01 1969-07-22 Union Carbide Corp Production of isocyanates
US3405040A (en) 1965-08-31 1968-10-08 Mobay Chemical Corp Method for recovering tolylene diisocyanate
FR2091813A5 (de) 1970-05-22 1972-01-14 Du Pont

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0017972A1 (de) * 1979-04-19 1980-10-29 BASF Aktiengesellschaft Gewinnung von Toluylendiisocyanat und/oder höhersiedenden Lösungsmitteln im Wirbelbett aus Destillationsrückständen der Toluylendiisocyanat-Herstellung
EP0324701A1 (de) * 1988-01-13 1989-07-19 Rhone-Poulenc Chimie Verfahren zur Trennung von Toluoldiisocyanat aus seinen Herstellungsrückständen
EP0699659A3 (de) * 1994-08-31 1996-06-26 Bayer Ag Verfahren und Vorrichtung zur kontinuierlichen Abtrennung eines festen Rückstandes aus seiner Lösung im gerührten Gutbett
CN104411681A (zh) * 2012-07-11 2015-03-11 拜耳材料科技股份有限公司 后处理由制备异氰酸酯产生的蒸馏残渣的方法
CN104411681B (zh) * 2012-07-11 2017-03-29 科思创德国股份有限公司 后处理由制备异氰酸酯产生的蒸馏残渣的方法

Also Published As

Publication number Publication date
CA1094090A (fr) 1981-01-20
BR7804465A (pt) 1979-03-20
AR214462A1 (es) 1979-06-15
ES471637A1 (es) 1979-02-01
FR2397396B1 (de) 1980-01-18
DK154426B (da) 1988-11-14
FR2397396A1 (fr) 1979-02-09
US4216063A (en) 1980-08-05
EP0000463B1 (de) 1982-01-06
PT68171A (fr) 1978-07-01
IT7868483A0 (it) 1978-06-23
AU3790278A (en) 1980-01-17
JPS612057B2 (de) 1986-01-22
JPS5419938A (en) 1979-02-15
IN148484B (de) 1981-03-07
IT1111627B (it) 1986-01-13
AU522377B2 (en) 1982-06-03
DK310578A (da) 1979-01-13
DK154426C (da) 1989-04-10
DE2861504D1 (en) 1982-02-25
IE47024B1 (en) 1983-11-30
IE781366L (en) 1979-01-12
SU1264840A3 (ru) 1986-10-15
DD138314A5 (de) 1979-10-24

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