AU706258B2 - Process and apparatus for performing a polymerisation in a tube reactor - Google Patents

Process and apparatus for performing a polymerisation in a tube reactor Download PDF

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Publication number
AU706258B2
AU706258B2 AU60666/96A AU6066696A AU706258B2 AU 706258 B2 AU706258 B2 AU 706258B2 AU 60666/96 A AU60666/96 A AU 60666/96A AU 6066696 A AU6066696 A AU 6066696A AU 706258 B2 AU706258 B2 AU 706258B2
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AU
Australia
Prior art keywords
tube reactor
mixture
polymerisation
heat exchanger
monomer
Prior art date
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Ceased
Application number
AU60666/96A
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AU6066696A (en
Inventor
Jacques Juvet
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Sulzer Chemtech AG
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Sulzer Chemtech AG
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24Stationary reactors without moving elements inside
    • B01J19/2415Tubular reactors
    • B01J19/2435Loop-type reactors
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F2/00Processes of polymerisation
    • C08F2/02Polymerisation in bulk

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Polymerisation Methods In General (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Description

P.6691 Ehph Sulzer Chemtech AG, Winterthur, Switzerland Process and apparatus for performing a polymerisation in a tube reactor The invention relates to a process for carrying out a polymerisation in a tube reactor. It also refers to an apparatus for carrying out the process as well as to corresponding uses.
Polystyrenes and copolymers, polyacrylates such as PMMA and other products can be polymerised by means of ionic initiation. This initiation is brought about by anionic or cationic starter substances which are mixed into the monomer.
Such starter substances, called starters for short, are temperature sensitive and decompose if the temperature exceeds, for example, 150 0
C.
Metal-organic compounds known as starter substances are: sec butyl-lithium
(C
4 HgLi) and cumyl-potassium (CgHnK) for the manufacture of polystyrene, diphenylmethyl-potassium
(C
13
H
11 fluorenyl-potassium
(C
13
H
9 K) and lithium chloride (LiCI) for the manufacture of polymethylmethylacrylate (PMMA) 2 The ionic polymerisation is rapid and highly exothermic. Due to the heat liberated the temperature can increase to beyond the decomposition temperature of the starter, whereupon the reaction ceases.
In order to carry out a continuous reaction, it is proposed to use a tube reactor in which the static mixer elements are arranged to be cross section filling (cf. EP 0 096 201).
Since, however, the polymerisation is associated with a strong increase in viscosity, problems arise which can lead to non-uniform product quality. As a result of the axial viscosity gradient a segregation can develop in which strongly polymerised, highly viscous phases can separate out from the less polymerised phases of lower viscosity in the mixture. Furthermore, the formation of a deposit on the reactor walls can also contribute to insufficiency of the product quality.
oo It is thus the object of the invention to provide a continuous process for the ionic polymerisation which leads to an improved product quality. This object is satisfied by the features of claim 1. In this process the axial viscosity gradient in a tube reactor is compensated for by a returned reaction product which still consists of unreacted monomers to a considerable extent. In order to prevent polymerisation from occurring in the return line, which would have a disturbing influence on the carrying out of the process, the starter is thermally annihilated at the outlet of the reactor.
The dependent claims 2 to 4 relate to advantageous embodiments of the process in accordance with the invention.
Claims 5 to 7 relate to apparatuses for carrying out the 3 process in accordance with the invention, and claim 8 relates to corresponding uses.
In the following the invention will be explained on the basis of the drawings. Shown are: Fig. 1 a schematic representation of the installation for carrying out the process in accordance with the invention, and Fig. 2 a diagram with the schematically represented plot of the temperature and the viscosity in the installation of Fig. 1 e* -The scheme of Fig. 1 shows: a tube reactor 1, a mixer-heat exchanger 2 for heating the product, a pump 3, a mixer-heat exchanger 4 for cooling the mixture to be fed into the reactor 1, a supply point 5 for a monomer M, a supply point 6 for a starter S and a removal point 7 for the product produced in accordance with the invention. The temperature and viscosity values are shown in the drawing of Fig. 2 for two embodiments for the points A, B, C and D.
The solid curves 10 (temperature) and 20 (viscosity) are associated with the first embodiment. The product P contains equal parts of polymer and monomer, namely 2.7 kg/h of each.
At point D, 26.4 kg/h of this polymer-monomer mixture leaves the heat exchanger 2. Of this, 21.6 kg/h is returned via the pump 3 to point A, where 5.4 kg/h of monomer M is admixed.
The temperature of this mixture is 124 0 C at A. The temperature is lowered to 100 0 C in the cooler 4 between A and B. Thereafter, starter S is admixed at B. In the reactor tube 1 the temperature rises due to the liberated reaction heat to 4 126 0 C (point By heating in the heat exchanger 2, the temperature of the product is finally raised to 150 0 C. At this temperature the starter S decomposes. As the curve shows, the viscosity increases in the reactor 2 between B and C from 0.78 to 2.37 Pa s (Ns/m 2 that is approximately threefold.
Whereas in the first exemplary embodiment the degree of transformation ratio of the amount of the monomer to the total amount) increases from 40 to 50 during the reaction, provision is made in the second example dashed curves 11 and 12 that the degree of transformation increases from to 50 Here the viscosity in the reactor 1 increases from 0.064 to 1.097 Pa s, i.e. by about a factor of 17. This ratio is disadvantageously high; it should preferably not be greater than As the curve 12 for the second exemplary embodiment shows, **9 the product would just have the decomposition temperature 9* (150 0 C) after the reactor if no cooling took place between A and B. In this case the cooler 4 and the heater 2 could be dispensed with. It is however not recommendable to provide this special execution of the process, since, on the one hand, a large increase in viscosity is present and, on the other hand, it would be difficult to carry out a control of the process.
For a given mixing ratio of returned product and freshly introduced monomer an initial temperature is preferably provided by the heat exchanger 4 in such a manner that the temperature of the mixture at the outlet of the tube reactor lies at least 5 K below the decomposition temperature.
5 The tube reactor 1 advantageously has mixer elements whose structure is built up of intermeshing arms which cross one another, with the arms forming two groups of structure elements aligned in parallel (cf. DE-PS 28 08 854).
For the mixer-heat exchangers 2 and 4 an apparatus is preferably chosen as known from DE-PS 28 39 564: This apparatus is a static mixer with arms which are executed as heat exchanger tubes.
6 THE CLAIMS DEFINING THE INVENTION ARE AS FOLLOWS: 1. Process for carrying out a polymerisation in a tube reactor comprising the following steps: mixing a freshly introduced monomer with a returned monomer-polymer mixture as well as cooling the mixture to a prescribed initial temperature, admixing an inactivatable polymerisation starter, the inactivation of which begins when heated above a decomposition temperature, as well as performing a partial polymerisation in the tube reactor, heating the mixture leaving the tube reactor to at least the said decomposition temperature, and finally returning a portion of the mixture and removal of the other portion as product.
2. Process in accordance with claim 1 characterised in that at least half of the mixture at the outlet of the tube reactor is present in polymerised form.
3. Process in accordance with claim 1 characterised in that the amount of the returned mixture is chosen in relation to the amount of monomer introduced in such a manner that the viscosity of the mixture in the tube reactor during polymerisation does not increase by more than approximately a factor of ten.
4. Process in accordance with claim 1 characterised in that for a given mixing ratio of returned mixture and freshly introduced monomer an initial temperature is prescribed so that the temperature of the mixture at the outlet of the tube reactor lies at least 5 K below the decomposition temperature.
5. Apparatus for carrying out the process in accordance with claim 1 comprising the following components: a tube reactor with static mixer elements arranged so as to be space filling, at least one mixer-heat exchanger 2) at each of the input side and the

Claims (3)

  1. 6. Apparatus in accordance with claim 5 characterised in that the tube reactor has mixer elements with a structure which is built up of arms crossing and intermeshing with one another, where the arms form two groups of structure elements directed parallel to one another.
  2. 7. Apparatus in accordance with claim 5 characterised in that the mixer-heat exchangers 4) are static mixers with arms which are formed as heat exchanger tubes.
  3. 8. The apparatus according to claim 5 for the manufacture of polystyrene or PMMA, where sec-butyl-lithium or LiCI respectively is used as an ionic starter. DATED this 28th day of August 1998 SULZER CHEMTECH AG WATERMARK PATENT TRADEMARK ATTORNEYS 290 BURWOOD ROAD HAWTHORN VICTORIA 3122 AUSTRALIA DOC 23 AU6066696.WPC IAS/CLR/CC P.6691 Ehph Abstract of Disclosure The process for carrying out a polymerisation in a tube reactor comprises the following steps: Freshly introduced monomer is mixed with a returned monomer-polymer mixture. The mixture is cooled to a prescribed initial temperature (heat exchanger A polymerisation starter which is inactivatable upon heating above a decomposition temperature is admixed. A partial polymerisation takes place in the tube reactor. The mixture leaving the tube reactor is heated up to at least the said decomposition temperature (heat exchanger Finally, a portion of the mixture is returned (pump 3) and the other portion removed as product (Fig. 1) 0 «n.
AU60666/96A 1995-07-26 1996-07-24 Process and apparatus for performing a polymerisation in a tube reactor Ceased AU706258B2 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
EP95810486 1995-07-26
EP95810486A EP0755945B1 (en) 1995-07-26 1995-07-26 Process and device for carrying out a polymerisation in a tube reactor

Publications (2)

Publication Number Publication Date
AU6066696A AU6066696A (en) 1997-01-30
AU706258B2 true AU706258B2 (en) 1999-06-10

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
AU60666/96A Ceased AU706258B2 (en) 1995-07-26 1996-07-24 Process and apparatus for performing a polymerisation in a tube reactor

Country Status (6)

Country Link
US (1) US5602216A (en)
EP (1) EP0755945B1 (en)
JP (1) JPH0940704A (en)
AU (1) AU706258B2 (en)
CA (1) CA2181633C (en)
DE (1) DE59504339D1 (en)

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FR2768740B1 (en) * 1997-09-19 2001-07-06 Bp Chem Int Ltd CONTINUOUS POLYMERIZATION PROCESS OF A VINYL MONOMER
ATE219701T1 (en) 1998-04-28 2002-07-15 Univ Heriot Watt METHOD AND DEVICE FOR PHASE-SEPARATED SYNTHESIS
DE19915916A1 (en) * 1999-04-09 2000-10-12 Basf Ag Process for the continuous production of polymers
CN1555387A (en) 2000-07-28 2004-12-15 古德里奇公司 Polymer composition for producing an optical waveguide, optical waveguide produced therefrom and method for producing the waveguide
US6906164B2 (en) 2000-12-07 2005-06-14 Eastman Chemical Company Polyester process using a pipe reactor
WO2002046266A2 (en) * 2000-12-07 2002-06-13 Eastman Chemical Company Low cost polyester process using a pipe reactor
US6979717B2 (en) * 2001-08-13 2005-12-27 Moore Eugene R Anionic process design for rapid polymerization of polystyrene without gel formation and product produced there from
PT1542793E (en) 2002-09-23 2007-09-17 Total Petrochemicals Res Feluy Slurry loop polyolefin reactor
EP1410843A1 (en) * 2002-10-17 2004-04-21 ATOFINA Research Slurry loop polyolefin reactor
DE10322830A1 (en) 2003-05-19 2004-12-09 Tesa Ag Process for the continuous production of polymers from vinyl compounds by bulk or solvent polymerization
US7135541B2 (en) 2003-06-06 2006-11-14 Eastman Chemical Company Polyester process using a pipe reactor
US7074879B2 (en) * 2003-06-06 2006-07-11 Eastman Chemical Company Polyester process using a pipe reactor
US7332548B2 (en) * 2004-03-04 2008-02-19 Eastman Chemical Company Process for production of a polyester product from alkylene oxide and carboxylic acid
JP4068108B2 (en) * 2005-11-04 2008-03-26 大陽日酸株式会社 Heating medium heating and cooling device
US20100105847A1 (en) 2006-01-24 2010-04-29 Intertape Polymer Corp. Plug flow bulk polymerization of vinyl monomers
US7906598B2 (en) * 2006-08-30 2011-03-15 Intertape Polymer Corp. Recirculation loop reactor bulk polymerization process
WO2008027858A1 (en) * 2006-08-30 2008-03-06 Intertape Polymer Corp. Recirculation loop reactor bulk polymerization process
US20080139780A1 (en) * 2006-12-07 2008-06-12 Debruin Bruce Roger Polyester production system employing short residence time esterification
US7649109B2 (en) * 2006-12-07 2010-01-19 Eastman Chemical Company Polyester production system employing recirculation of hot alcohol to esterification zone
US7943094B2 (en) 2006-12-07 2011-05-17 Grupo Petrotemex, S.A. De C.V. Polyester production system employing horizontally elongated esterification vessel
US7863477B2 (en) 2007-03-08 2011-01-04 Eastman Chemical Company Polyester production system employing hot paste to esterification zone
US7868129B2 (en) * 2007-07-12 2011-01-11 Eastman Chemical Company Sloped tubular reactor with spaced sequential trays
US7868130B2 (en) * 2007-07-12 2011-01-11 Eastman Chemical Company Multi-level tubular reactor with vertically spaced segments
US7847053B2 (en) * 2007-07-12 2010-12-07 Eastman Chemical Company Multi-level tubular reactor with oppositely extending segments
US7872090B2 (en) * 2007-07-12 2011-01-18 Eastman Chemical Company Reactor system with optimized heating and phase separation
US7858730B2 (en) 2007-07-12 2010-12-28 Eastman Chemical Company Multi-level tubular reactor with dual headers
US7842777B2 (en) * 2007-07-12 2010-11-30 Eastman Chemical Company Sloped tubular reactor with divided flow
US7829653B2 (en) * 2007-07-12 2010-11-09 Eastman Chemical Company Horizontal trayed reactor
US7872089B2 (en) 2007-07-12 2011-01-18 Eastman Chemical Company Multi-level tubular reactor with internal tray
DE102007040850A1 (en) 2007-08-29 2009-03-05 Wacker Chemie Ag Process for the preparation of protective colloid-stabilized polymers and apparatus for carrying out the process
JP2014012781A (en) * 2012-07-05 2014-01-23 Sumitomo Chemical Co Ltd Method for producing methacrylic polymer composition
CN103333278B (en) * 2013-01-30 2016-02-24 衢州市鼎盛化工科技有限公司 A kind of device and technique thereof preparing fluoropolymer and fluorinated copolymer
RU2607916C1 (en) * 2015-12-21 2017-01-11 Владимир Леонидович Письменный Heat exchanger

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DE2839564C2 (en) 1978-09-12 1982-10-21 Hoechst Ag, 6000 Frankfurt Device with supply and removal of heat and for mixing liquid media
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Also Published As

Publication number Publication date
CA2181633C (en) 1999-12-14
EP0755945B1 (en) 1998-11-25
CA2181633A1 (en) 1997-01-27
DE59504339D1 (en) 1999-01-07
US5602216A (en) 1997-02-11
EP0755945A1 (en) 1997-01-29
AU6066696A (en) 1997-01-30
JPH0940704A (en) 1997-02-10

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