DK147423B - PROCEDURE FOR SUSPENSION POLYMERIZATION OF VINYL CHLORIDE - Google Patents

PROCEDURE FOR SUSPENSION POLYMERIZATION OF VINYL CHLORIDE Download PDF

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Publication number
DK147423B
DK147423B DK355276AA DK355276A DK147423B DK 147423 B DK147423 B DK 147423B DK 355276A A DK355276A A DK 355276AA DK 355276 A DK355276 A DK 355276A DK 147423 B DK147423 B DK 147423B
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vinyl chloride
water
reactor
procedure
suspension polymerization
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DK355276AA
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Danish (da)
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DK147423C (en
DK355276A (en
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Dionigi Baldini
Francesco Carlin
Giancarlo Montanari
Enzo Bandini
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Anic Spa
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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
    • B01J19/0053Details of the reactor
    • B01J19/0073Sealings
    • 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
    • B01J19/0053Details of the reactor
    • 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
    • B01J19/0053Details of the reactor
    • B01J19/0066Stirrers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B9/00Cleaning hollow articles by methods or apparatus specially adapted thereto 
    • B08B9/08Cleaning containers, e.g. tanks
    • 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
    • C08F14/00Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
    • C08F14/02Monomers containing chlorine
    • C08F14/04Monomers containing two carbon atoms
    • C08F14/06Vinyl chloride
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00162Controlling or regulating processes controlling the pressure
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/141Feedstock

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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)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Polymerisation Methods In General (AREA)

Description

i 147423in 147423

Opfindelsen angår en fremgangsmåde til suspen-sionspolymerisering af vinylchlorid enten alene eller i blanding med op til 20 vægt% copolymeriserbare monomere, ved hvilken der under polymerisationen gennemføres en af-5 skylning af reaktorens loft med vand.The invention relates to a process for suspending polymerization of vinyl chloride either alone or in admixture with up to 20% by weight of copolymerizable monomers, during which a flushing of the reactor ceiling with water is carried out.

Det er velkendt, at et af de største problemer ved suspensionspolymerisering af vinylchlorid, enten alene eller i blandinger med andre monomere, skyldes de belægninger af polymere, som af lejres på reaktorens vaeg-10 ge og som, dersom de ikke fjernes, forurener produktet fra de følgende polymerisationer. Under alle omstændigheder kræver fjernelsen, enten manuelt eller mekanisk, med vand under højt tryk, at reaktoren åbnes, hvorved man spilder en eller flere timer.It is well known that one of the major problems in suspension polymerization of vinyl chloride, either alone or in mixtures with other monomers, is due to the coatings of polymers which are deposited on the walls of the reactor and which, if not removed, contaminate the product from the following polymerizations. In any case, the removal, either manually or mechanically, of high pressure water requires opening the reactor, wasting one or more hours.

15 I den senere tid er udtaget en række patenter, der gør fordring på at have løst problemet med belægninger på de reaktorvægge, som er i kontakt med den flydende fase.Recently, a number of patents have been issued claiming to have solved the problem of coatings on the reactor walls in contact with the liquid phase.

Generelt sagt gøres der brug af særlige præpara-20 ter, som forhindrer aflejringen, og som gør det nødvendigt, at man renser efter blot ca. 10 polymerisationer.Generally speaking, special preparations are used which prevent the deposition and which make it necessary to purify after just approx. 10 polymerizations.

Problemet med belægningerne på de dele af reaktoren, der er i kontakt med gasfasen, er imidlertid stadigvæk ikke løst med disse præparater, og den tendens, 25 der er til at udnytte reaktoren til det yderste (høj fyldningsgrad, kraftig omrøring, høj destillationshastighed og restmonomeren og andet), har forværret problemet, fordi der dannes et kraftigere skum og sprøjt, hvorved der aflejres polymer på reaktorens loft. Efter 30 nogle få polymerisationer, begynder dyserne at blive tilstoppet med fare for, at store klumper polymer af-rives og forhindrer udtømningen, hvilket har uheldig indvirkning på bundventilernes tæthed. På denne måde påvirkes fyldnings- og tømningsoperationerne, og reak-35 torens sikkerhed under polymeriseringen bliver problematisk.However, the problem of the coatings on the parts of the reactor in contact with the gas phase is still not solved with these preparations and the tendency to utilize the reactor to the extreme (high degree of filling, vigorous stirring, high distillation rate and the residual monomer and other), has exacerbated the problem because a stronger foam and syringe is formed, thereby depositing polymer in the ceiling of the reactor. After a few polymerizations, the nozzles begin to become clogged with the risk of large chunks of polymer being torn off and preventing the discharge, which adversely affects the density of the bottom valves. In this way, the filling and emptying operations are affected and the safety of the reactor during the polymerization becomes problematic.

Alt i alt gør belægningerne på reaktorens loft den eventuelle brug af et antitilsmudsningspræparat ir 2 147423 relevant i henseende til det ønskemål: at reaktoren åbnes så sjældent som muligt.All in all, the coatings in the ceiling of the reactor make the possible use of an anti-soiling preparation ir 2 147423 relevant for the purpose: to open the reactor as rarely as possible.

Fra tysk offentliggørelsesskrift nr. 2.239.942 kendes en fremgangsmåde til polymerisation af vinyl-5 chlorid, ved hvilken der under polymerisationen gennemføres en afskylning af reaktorens loft med vand for at modvirke afsætning af belægninger. Denne afskylning udføres under anvendelse af forholdsvis ringe tryk, 2 nemlig 2-3 kg/cm ,og i hele polymerisationsperioden, 10 også når vandtilførslen sker pulserende. En sådan afskylning med vand, udført under hele reaktionstiden, er kun i stand til permanent at forhindre aflejringen af polymeren ved batcher med lav fyldnings koefficient, langsom omrøring og lignende, dvs. i poly-15 meriseringsforløb, der har ringe industriel interesse.German Patent Publication No. 2,239,942 discloses a method for polymerizing vinyl chloride, during which, during the polymerization, a flushing of the reactor ceiling with water is carried out to counteract deposition of coatings. This flushing is carried out using relatively low pressures, 2 namely 2-3 kg / cm, and throughout the polymerization period, 10 even when the water supply is pulsed. Such rinsing with water, carried out throughout the reaction time, is only capable of permanently preventing the deposition of the polymer by batches with low filling coefficient, slow stirring and the like, i.e. in polymerization processes having little industrial interest.

I øvrigt har de i det tyske offentliggørelsesskrift anvendte dyser den ulempe, at de i høj grad er udsat for tilsmudsning og tilstopning.Moreover, the nozzles used in the German publication publication have the disadvantage that they are highly prone to dirt and clogging.

Det har nu vist sig, at de nævnte ulemper kan 20 undgås ved fremgangsmåden ifølge den foreliggende opfindelse, så at det ikke er nødvendigt ved hver polymerisation at åbne reaktoren for at undersøge loftet og for muligvis at fjerne belægningerne. Fremgangsmåden ifølge opfindelsen er ejendommelig ved, at afskylningen 25 med vand påbegyndes, når omdannelsesgraden har nået 15-25%, og at denne afskylning fortsættes under anven-delse af vand med et tryk på mindst 15 kg/cm og i en mængde på mindst 1000 liter vand pr. time indtil opnåelsen af en omdannelsesgrad på mindst 40%, hvorefter der, 30 når polymerisationen er afsluttet, gennemføres en vask- o ning med vand under et tryk på mindst 100 kg/cm . Sidstnævnte vaskning gennemføres f.eks. når batchen udtømmes eller under alle omstændigheder, når autoklaven lukkes.It has now been found that the disadvantages mentioned can be avoided by the process of the present invention, so that it is not necessary to open the reactor with each polymerization to examine the ceiling and possibly to remove the coatings. The process according to the invention is characterized in that the rinsing 25 is started with water when the conversion rate has reached 15-25% and that this rinsing is continued using water with a pressure of at least 15 kg / cm and in an amount of at least 1000 liters of water per at least 40%, after which, when the polymerization is complete, a wash with water under a pressure of at least 100 kg / cm is carried out. The latter washing is carried out e.g. when the batch is depleted or in any case when the autoclave is closed.

Når nævnte afskylning gennemføres under anven-35 delse af en strømningshastighed på mindst 1000 liter i timen, opnås der kun lette belægninger.When said rinsing is carried out using a flow rate of at least 1000 liters per hour, only light coatings are obtained.

3 167423 som let kan fjernes ved den sluttelige vaskning ved højt tryk, uden nogen vanskelighed med hensyn til tømning eller bundventilens tæthed.3 167423 which can be easily removed by the final washing at high pressure, without any difficulty in emptying or the density of the bottom valve.

Dersom afskylningen først påbegyndes, når omdan-5 nelsesgraden er over 25%, forhindrer den ikke afsætningen af belægninger i form af store klumper, og for tidlige operationer frembyder ingen fordel, da det reducerede fri volumen, der er tilgængelig ved de sædvanlige industrielle polymerisationer, ikke tillader, at den lo Ønskede strømningshastighed af vandet kan opretholdes.If rinsing is only started when the conversion rate is above 25%, it does not prevent the deposition of large lump coatings, and premature operations offer no advantage as the reduced free volume available in the usual industrial polymerizations. does not allow the desired flow rate of water to be maintained.

Vaskningen med vand under højt tryk er absolut nødvendig for at forhindre den lille restbelægning fra at blive tykkere, når de følgende batcher tilføres.The washing with high pressure water is absolutely necessary to prevent the small residual coating from becoming thicker when the following batches are applied.

Det følgende eksempel og sammenligningseksempel 15 tjener til nærmere at beskrive nødvendigheden af den samtidige anvendelse af de to nævnte foranstaltninger.The following example and Comparative Example 15 serve to further describe the necessity for the simultaneous application of the two mentioned measures.

Udførelseseksempel 3 2o En 25m autoklav udstyret med en omrører og enEXAMPLE 3 2o A 25m autoclave equipped with a stirrer and one

Pfandler-antiskvulpeanordning fyldtes op til 90% af dens volumen med lige volumendele vand og en 85/15 blanding af vinylchlorid og vinylacetat. Efter afskylning af lof- o tet med vand under et tryk på 25 kg/cm , når omdannelses- 25 graden var fra 2o% til 4o%, fjernedes der 3 kg skorper, der var ensartet fordelt over hele overfladen.The Pfandler anti-swelling device filled up to 90% of its volume with equal volumes of water and an 85/15 mixture of vinyl chloride and vinyl acetate. After rinsing the ceiling with water under a pressure of 25 kg / cm, when the conversion rate was from 20% to 40%, 3 kg of crusts which were uniformly distributed over the entire surface were removed.

Derefter anvendtes vaskning med vand under et tryk 2 på 3oo kg/cm , idet der anvendtes indstillelige dyser.Then, washing with water under a pressure 2 of 300 kg / cm was used, using adjustable nozzles.

Autoklaveloftet var fuldstændig rent, og der var 3o ingen problemer ved tømningen eller med bundventilens tæthed.The autoclave air was completely clean and there were no problems with the emptying or the tightness of the bottom valve.

Sammenligningseksempel I den samme autoklav som i det foregående eksempel var fyldningsgraden og forholdet mellem vand og vinyl-35 chlorid uændret som i udførelseseksemplet.Comparative Example In the same autoclave as in the previous example, the filling rate and the ratio of water to vinyl chloride were unchanged as in the embodiment.

Efter afskylning af loftet med vand under et tryk 4 147423 på 30 kg/cm^, når omdannelsesgraden var fra 40-65%, opsamledes der 10 kg skorper i form af grove klumper.After flushing the ceiling with water under a pressure of 30 kg / cm 2, when the conversion rate was from 40-65%, 10 kg of crust was collected in the form of coarse lumps.

Vaskning, under de følgende polymerisationer, med vand under et tryk på 350 kg/cm bevirkede, at man f jer-5 nede tilsmudsningen væsentligt, men den forlængede betydeligt tømningstiderne, således at det krævede en manuel operation at fjerne polymeren, der tilstoppede bundventilen.Washing, during the following polymerizations, with water under a pressure of 350 kg / cm, significantly reduced the soiling, but significantly prolonged the emptying times, requiring manual operation to remove the polymer clogging the bottom valve.

Den ovenfor beskrevne fremgangsmåde kan anvendes 10 uden begrænsninger på autoklaver af en hvilken som helst størrelse i industrien og til alle formuleringer, der kendes inden for indsutrien, også omfattende de i patenterede antitilsmudsningsfremgangsmåder anvendte.The above-described method can be used without limitation on autoclaves of any size in the industry and for all formulations known in the art, including those used in patented anti-fouling methods.

De polymerisationer, hvortil den foreliggende 15 fremgangsmåde kan anvendes, er polymerisationer af vinyl· chlorid enten alene eller i blandinger med andre monomere, .der indeholder 20% eller mindre comonomer. Comono-mererne er alle sådanne, om hvilke det er kendt af fagmanden, at de kan copolymeriseres med vinylchlorid.The polymerizations to which the present process can be used are polymerizations of vinyl chloride either alone or in mixtures with other monomers containing 20% or less comonomer. The comonomers are all such as are known to those skilled in the art that can be copolymerized with vinyl chloride.

20 Eksempelvis kan de være vinylidenchlorid, vinylacetat, vinylbutyrat, methylacrylater og metacrylater, butyl-acrylater og metacrylater, isooctylacrylater og metacrylater, diethyl- og dipropylmaleater og -fumarater, styren, ethylen, propylen, butylen, vinylethylether, allyl-25 acetat, diallylphthaiat, diallylmaleat, acrylonitril, metacrylonitril og andre.For example, they may be vinylidene chloride, vinyl acetate, vinyl butyrate, methyl acrylates and metacrylates, butyl acrylates and metacrylates, isooctyl acrylates and metacrylates, diethyl and dipropyl maleate and fumarates, styrene, ethylene, propylene, butylene, vinylethyl, vinyl ethyl, diallyl maleate, acrylonitrile, methacrylonitrile and others.

Når man i praksis skal anvende , hvad der er beskrevet ovenfor, er det nødvendigt at huske nogle få ting, der tilsigter at udnytte afskylningen og vaske-30 vandet til det yderste uden at gribe uheldigt ind i den korrekte gennemførsel af reaktionen.In practice, when applying what is described above, it is necessary to keep in mind a few things which aim to utilize the rinse and wash water to the utmost without interfering unduly with the proper conduct of the reaction.

F.eks. vil faste installationer, der rager ind i det indre af autoklaven, være foretrukne steder, hvor polymerbelægninger kan opbygges. Dette reducerer i 35 betydelig grad virkningen af afskylningen og vaskningen.Eg. For example, fixed installations projecting into the interior of the autoclave will be preferred locations where polymer coatings can be built up. This significantly reduces the effect of the rinse and wash.

Man bør således foretrække bevægelige installationer af den slags, som er afbildet på tegningen, og som er karakteristisk ved, at vand (under enten lavtMoving installations of the kind depicted in the drawing should therefore be preferred, characterized by water (below or low).

DK355276A 1975-08-08 1976-08-06 PROCEDURE FOR SUSPENSION POLYMERIZATION OF VINYL CHLORIDE DK147423C (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
IT2621975 1975-08-08
IT26219/75A IT1044367B (en) 1975-08-08 1975-08-08 PROCEDURE FOR THE REMOVAL OF STAINS FROM PARTS IN CONTACT WITH THE GASEOUS PHASE IN SUSPENSION VINYL CHLORIDE POLYMERIZERS

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DK355276A DK355276A (en) 1977-02-09
DK147423B true DK147423B (en) 1984-07-30
DK147423C DK147423C (en) 1985-02-18

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AR (1) AR211275A1 (en)
AT (1) AT351256B (en)
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BG (1) BG33298A3 (en)
CA (1) CA1083750A (en)
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CS (1) CS209874B2 (en)
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DE (1) DE2635487C3 (en)
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EG (1) EG12260A (en)
ES (1) ES450917A1 (en)
FR (1) FR2320314A1 (en)
GB (1) GB1519359A (en)
IE (1) IE44309B1 (en)
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IT (1) IT1044367B (en)
LU (1) LU75552A1 (en)
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NL (1) NL164869C (en)
NO (1) NO147030C (en)
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US4058652A (en) * 1976-02-10 1977-11-15 Exxon Research & Engineering Co. Autorefrigeration process and apparatus
DE3637060C2 (en) * 1986-10-31 1999-02-04 Wacker Chemie Gmbh Device for spraying or injecting liquid into a container and its use
DE60016112T2 (en) * 1999-08-27 2005-11-03 Rohm And Haas Co. Process for the purification of reactors
EP1471077A3 (en) * 1999-08-27 2005-02-02 Rohm And Haas Company Process for cleaning reactors
ES2551414T3 (en) 2010-12-14 2015-11-18 Sasol Technology (Proprietary) Limited Cleaning process equipment

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DE2239942B2 (en) * 1972-08-14 1979-08-30 Wacker-Chemie Gmbh, 8000 Muenchen Process for the polymerization of vinyl chloride

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GB1519359A (en) 1978-07-26
IN144224B (en) 1978-04-08
DE2635487C3 (en) 1985-07-18
IE44309B1 (en) 1981-10-21
BG33298A3 (en) 1983-01-14
NO147030C (en) 1984-09-07
DK147423C (en) 1985-02-18
PH13287A (en) 1980-03-04
AU1641176A (en) 1978-02-02
ES450917A1 (en) 1977-08-16
FR2320314B1 (en) 1979-08-17
NO762717L (en) 1977-02-09
ATA585376A (en) 1978-12-15
YU192376A (en) 1982-05-31
AU506993B2 (en) 1980-01-31
FR2320314A1 (en) 1977-03-04
TR19096A (en) 1978-05-16
NL164869B (en) 1980-09-15
IN144965B (en) 1978-10-05
CA1083750A (en) 1980-08-12
PT65447B (en) 1978-02-10
CS209874B2 (en) 1981-12-31
DD126262A5 (en) 1977-07-06
IL50152A (en) 1979-11-30
PT65447A (en) 1976-09-01
EG12260A (en) 1978-12-31
BE844978A (en) 1977-02-07
IT1044367B (en) 1980-03-20
NL7608848A (en) 1977-02-10
SE429554B (en) 1983-09-12
NO147030B (en) 1982-10-11
LU75552A1 (en) 1977-03-25
DK355276A (en) 1977-02-09
RO72240A (en) 1981-11-04
YU39217B (en) 1984-08-31
AT351256B (en) 1979-07-10
IE44309L (en) 1977-02-08
DE2635487A1 (en) 1977-06-30
MX3261E (en) 1980-08-12
IL50152A0 (en) 1976-09-30
DE2635487B2 (en) 1980-02-14
JPS5237990A (en) 1977-03-24
AR211275A1 (en) 1977-11-15
NL164869C (en) 1981-02-16
ZA764470B (en) 1977-07-27
SE7608867L (en) 1977-02-09
CH608507A5 (en) 1979-01-15

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