EP0000463A1 - Verfahren zur Trennung von Toluoldiisocyanat aus Herstellungsgemischen - Google Patents
Verfahren zur Trennung von Toluoldiisocyanat aus Herstellungsgemischen Download PDFInfo
- 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
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
- 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)
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR7721436 | 1977-07-12 | ||
FR7721436A FR2397396A1 (fr) | 1977-07-12 | 1977-07-12 | Procede de recuperation du toluene diisocyanate a partir des residus de fabrication |
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)
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)
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 |
US9061971B2 (en) * | 2005-09-29 | 2015-06-23 | Basf Aktiengesellschaft | Method for purifying residues containing isocyanates |
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)
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)
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 |
-
1977
- 1977-07-12 FR FR7721436A patent/FR2397396A1/fr active Granted
-
1978
- 1978-06-15 PT PT68171A patent/PT68171A/pt unknown
- 1978-06-20 IN IN453/DEL/78A patent/IN148484B/en unknown
- 1978-06-23 US US05/918,581 patent/US4216063A/en not_active Expired - Lifetime
- 1978-06-23 IT IT68483/78A patent/IT1111627B/it active
- 1978-06-30 AR AR272793A patent/AR214462A1/es active
- 1978-07-03 EP EP78400051A patent/EP0000463B1/de not_active Expired
- 1978-07-03 DE DE7878400051T patent/DE2861504D1/de not_active Expired
- 1978-07-07 IE IE1366/78A patent/IE47024B1/en not_active IP Right Cessation
- 1978-07-10 DD DD78206629A patent/DD138314A5/de unknown
- 1978-07-10 AU AU37902/78A patent/AU522377B2/en not_active Expired
- 1978-07-11 BR BR7804465A patent/BR7804465A/pt unknown
- 1978-07-11 CA CA307,196A patent/CA1094090A/fr not_active Expired
- 1978-07-11 DK DK310578A patent/DK154426C/da not_active IP Right Cessation
- 1978-07-11 ES ES471637A patent/ES471637A1/es not_active Expired
- 1978-07-12 JP JP8412978A patent/JPS5419938A/ja active Granted
- 1978-07-12 SU SU782634047A patent/SU1264840A3/ru active
Patent Citations (3)
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)
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 |
---|---|
FR2397396A1 (fr) | 1979-02-09 |
DE2861504D1 (en) | 1982-02-25 |
IE781366L (en) | 1979-01-12 |
AU522377B2 (en) | 1982-06-03 |
CA1094090A (fr) | 1981-01-20 |
IN148484B (de) | 1981-03-07 |
FR2397396B1 (de) | 1980-01-18 |
EP0000463B1 (de) | 1982-01-06 |
BR7804465A (pt) | 1979-03-20 |
AU3790278A (en) | 1980-01-17 |
SU1264840A3 (ru) | 1986-10-15 |
AR214462A1 (es) | 1979-06-15 |
US4216063A (en) | 1980-08-05 |
DK154426B (da) | 1988-11-14 |
PT68171A (fr) | 1978-07-01 |
ES471637A1 (es) | 1979-02-01 |
JPS5419938A (en) | 1979-02-15 |
DD138314A5 (de) | 1979-10-24 |
JPS612057B2 (de) | 1986-01-22 |
DK310578A (da) | 1979-01-13 |
IT1111627B (it) | 1986-01-13 |
DK154426C (da) | 1989-04-10 |
IE47024B1 (en) | 1983-11-30 |
IT7868483A0 (it) | 1978-06-23 |
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