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WO2001051159A1 - Procede de nettoyage de colonnes de separation - Google Patents

Procede de nettoyage de colonnes de separation Download PDF

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Publication number
WO2001051159A1
WO2001051159A1 PCT/EP2001/000154 EP0100154W WO0151159A1 WO 2001051159 A1 WO2001051159 A1 WO 2001051159A1 EP 0100154 W EP0100154 W EP 0100154W WO 0151159 A1 WO0151159 A1 WO 0151159A1
Authority
WO
WIPO (PCT)
Prior art keywords
cleaning
column
aqueous
weight
basic compound
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.)
Ceased
Application number
PCT/EP2001/000154
Other languages
German (de)
English (en)
Inventor
Josef Neutzner
Wolfgang HÜBINGER
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.)
BASF SE
Original Assignee
BASF SE
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 BASF SE filed Critical BASF SE
Priority to AU2001240500A priority Critical patent/AU2001240500A1/en
Publication of WO2001051159A1 publication Critical patent/WO2001051159A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
    • C11D7/02—Inorganic compounds
    • C11D7/04—Water-soluble compounds
    • C11D7/06—Hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D19/00—Degasification of liquids
    • B01D19/0005—Degasification of liquids with one or more auxiliary substances
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B9/00—Cleaning hollow articles by methods or apparatus specially adapted thereto
    • B08B9/08—Cleaning containers, e.g. tanks
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
    • C11D2111/10—Objects to be cleaned
    • C11D2111/14—Hard surfaces
    • C11D2111/20—Industrial or commercial equipment, e.g. reactors, tubes or engines

Definitions

  • the present invention relates to a process for cleaning separation columns through which aqueous polymer dispersions or polymer suspensions were passed following the polymerization reactions in order to remove volatile constituents.
  • aqueous polymer dispersions and polymer suspensions by so-called radically initiated aqueous emulsion or suspension polymerizations.
  • the products often also contain volatile constituents, such as residual monomers resulting from incomplete monomer conversion, impurities from the feedstocks, decomposition products of the initiators or low molecular weight products from side reactions.
  • aqueous polymer dispersions and polymer suspensions are used before or after an optional radical postpolymerization to remove these volatile components of a so-called inert gas - and / or steam stripping supplied (deodorization).
  • inert gas - and / or steam stripping supplied deodorization
  • Separation columns are frequently used for deodorization of large amounts of aqueous polymer dispersions and polymer suspensions, in which the aqueous polymer systems flow continuously from top to bottom and an inert gas and / or water vapor stream is directed towards them from bottom to top.
  • the volatile constituents are removed from the aqueous polymer systems and continuously discharged from the separation column via the inert gas and / or water vapor.
  • the separation columns In order to enable the volatile constituents from the aqueous polymer systems to transition as quickly and completely as possible into the inert gas and / or water vapor flow during the deodorization, the separation columns must have internals which ensure a large surface area of the aqueous polymer systems.
  • aqueous polymer systems form polymer films on the inner surfaces of the separation columns, which can also grow to form larger caking. These lead to a drop in performance and, in extreme cases, to complete blockage of the separation column. These caking can also partially detach again and lead to undesired particles in the product of value, which would interfere with the formation of the desired homogeneous polymer films in the corresponding end uses.
  • the aqueous polymer systems are therefore usually subjected to filtration.
  • these separation columns are regularly cleaned manually with a high-pressure water jet in complex work steps.
  • the resulting downtimes of the separation columns are up to two weeks.
  • a process for cleaning separation columns by which aqueous polymer dispersions or polymer suspensions were passed following the polymerization reactions to remove volatile constituents was found, which is characterized in that the cleaning comprises contacting the inner surfaces of the separation columns with an aqueous solution of a includes basic compound.
  • Suitable separation columns to be cleaned are generally customary columns, such as, for example, tray columns, packed columns and packed columns.
  • Commercially available shelves, packing elements or packings such as bell bottoms, tunnel bottoms, valve bottoms, sieve bottoms, dual flow bottoms and mesh shelves, Pall-Rings ® , Berl ® saddle bodies, mesh wire rings, Raschig-Rings ® , Intalox ® saddles, Interpak ® fillers can be installed and Intos ® rings, but also ordered packings such as Sulzer-Mellapak ® or Sulzer-Optiflow ® , kuhni-Rombopak ® and Montz-Pak ® as well as tissue packs are used.
  • the inner surfaces of the separation columns are understood to mean all surfaces within the separation columns, such as, for example, the inner surfaces of the separation columns themselves and all surfaces of the internals located in the separation columns.
  • the inner surfaces of a separation column are brought into contact with an aqueous solution of a basic compound (basic washing solution).
  • the contacting of the inner surfaces with the basic washing solution can be carried out, for example, in such a way that the separation column is completely filled with this solution.
  • the basic washing solution of the separation column can either be via feed lines in the column head or in the
  • Suitable basic compounds are alkali metal and alkaline earth metal hydroxides, such as sodium hydroxide, potassium hydroxide, lithium hydroxide, magnesium hydroxide and calcium hydroxide, ammonium hydroxide, alkali metal and alkaline earth metal salts of weak acids, such as carbonic acid, organic carboxylic acids or phosphoric acids, such as sodium carbonate, potassium carbonate and their hydrogen carbonates - Carbonate and potassium bicarbonate, sodium acetate, potassium acetate, calcium acetate, magnesium acetate, sodium propionate, potassium propionate, calcium propionate, magnesium propionate, trisodium phosphate, tripotassium phosphate and organic nitrogen compounds, such as C ⁇ ⁇ to C -alkylamine, such as methylamine, ethylamine, n-propylamine iso-propylamine, n-butylamine, 2-butylamine, tert.
  • weak acids such as carbonic acid, organic carboxylic acids or phosphoric acids, such
  • C ⁇ ⁇ to C 4 -dialkylamines such as dimethylamine, diethylamine, di-n-propylamine, di-iso-propylamine, di-n-butylamine, dibutylamine-2, di-tert.
  • -butylamine C ⁇ ⁇ to C 4 ⁇ trialkylamines, such as trimethylamine, triethylamine, tri-n-propylamine, tri-iso-propylamine, tri-n-butylamine, tributylamine-2, tri-tert-butylamine but also amino group-containing organic hydroxy - Compounds such as monoethanolamine, diethanolamine, triethanolamine, 2-aminopropanol, 3-aminopropanol, 2-aminobutanol, 3-aminobutanol, 4-aminobutanol, 2-amino-2-methylpropanol, 2-amino-2-hydroxymethyl-l, 3 propanediol and 2-amino-2-ethyl-l, 3-propanediol.
  • an aqueous solution which contains two or more of the aforementioned basic compounds.
  • Aqueous solutions of sodium hydroxide and / or potassium hydroxide are preferably used
  • basic washing solutions are used whose proportion by weight of the basic compound is generally> 0.1% by weight,> 1% by weight,> 2% by weight,> 3% by weight,> 5% by weight % and
  • Basic washing solutions are frequently used, the basic compounds of which have a proportion by weight of between 1 and 20% by weight, often between 1.5 and 15% by weight or between 2 and 10% by weight, in each case based on the total weight of the basic washing solution.
  • the basic washing solution has a temperature of> 0 to 150 ° C during cleaning. However, it is also possible to set even higher temperatures. For practical reasons, temperatures between 20 and 150 ° C are preferred.
  • the basic washing solution often has temperatures between 30 and 120 ° C or between 40 and 110 ° C.
  • the way in which the basic washing solution is heated is in principle irrelevant; for example, internal or external heat exchangers attached to the separating column or a separate electric heater can be used for this.
  • it has proven to be advantageous if the basic washing solution flowing down within the separating column is heated by steam which is introduced at the bottom of the column. This also leads to the basic washing solution being agitated vigorously within the separation column.
  • the steam temperature is usually> 100 ° C and can have values of> 110 ° C,> 120 ° C,> 130 ° C,> 140 ° C,> 150 ° C or> 160 ° C.
  • Water vapor is often fed in in the form of water vapor under pressure. The water vapor often has a pressure of 4 or 16 bar. The steam flow is adjusted so that on the one hand the desired cleaning temperature can be reached and maintained and on the other hand the basic washing solution can flow down and be pumped around.
  • cleaning takes place at an internal column pressure corresponding to the external atmospheric pressure (1 bar absolute), at negative pressure ( ⁇ 1 bar absolute) or at excess pressure (> 1 bar absolute), each measured in the column head.
  • cleaning can be carried out at pressures of ⁇ 950 mbar, ⁇ 900 mbar, ⁇ 850 bar, ⁇ 800 mbar or even lower pressures.
  • cleaning is often carried out at atmospheric pressure or at pressures> 1.5 bar,> 2 bar,> 3 bar,> 4 bar,> 5 bar (absolute values in each case) or even higher pressures, each measured in the column top.
  • volume quantities are used which are> 0.1 vol.%,> 1 vol.%,> 3 vol.%,> 5 vol.%,> 10 vol.%,> 20 vol.% ,> 30 vol.%,> 50 vol.%,> 70 vol.%,> 100 vol. -% or even higher values, based in each case on the total internal volume of the separation column.
  • volume quantities are used which are> 0.1 vol.%,> 1 vol.%,> 3 vol.%,> 5 vol.%,> 10 vol.%,> 20 vol.% ,> 30 vol.%,> 50 vol.%,> 70 vol.%,> 100 vol. -% or even higher values, based in each case on the total internal volume of the separation column.
  • the cleaning according to the invention can in principle take place in the case of polymer films or caking adhering to the inner surfaces, which were formed from polymer particles whose homo- or copolymers are composed of at least one of the following ethylenically unsaturated monomers: vinyl-aromatic monomers such as styrene, ⁇ -methylstyrene, o-chlorostyrene or vinyl toluenes, esters of vinyl alcohol and monocarboxylic acids containing 1 to 18 carbon atoms, such as vinyl acetate, vinyl propionate, vinyl n-butyrate, vinyl laurate and vinyl stearate, esters of ⁇ -, ß- preferably having 3 to 6 carbon atoms monoethylenically unsaturated mono- and dicarboxylic acids, such as, in particular, acrylic acid, methacrylic acid, maleic acid, fumaric acid and itaconic acid, with alkanols which generally have 1 to 12, preferably 1 to 8 and in
  • the monomers mentioned In the case of aqueous polymer systems produced by the free-radical aqueous emulsion or suspension polymerization method, the monomers mentioned generally form the main monomers, which, based on the total amount of the monomers to be polymerized by the free-radically initiated aqueous emulsion or suspension polymerization process, normally combine a share of more than 50 wt .-%.
  • the following monomers are usually used in free-radical aqueous emulsion or suspension polymerization only as modifying monomers in amounts, based on the total amount of the monomers to be polymerized, of less than 50% by weight, generally 0.5 to 20, preferably 1 to 10% by weight polymerized: ⁇ , ß-monoethylenically unsaturated mono- and dicarboxylic acids and their amides, such as acrylic acid, methacrylic acid, maleic acid, fumaric acid, itaconic acid, acrylamide and methacrylamide, furthermore monoethylenically unsaturated sulfonic acids and their water-soluble salts, such as vinylsulfonic acid and N vinylpyrrolidone.
  • ß-monoethylenically unsaturated mono- and dicarboxylic acids and their amides such as acrylic acid, methacrylic acid, maleic acid, fumaric acid, itaconic acid, acrylamide and methacrylamide, furthermore monoethy
  • Monomers which usually increase the internal strength of the films of the aqueous polymer dispersions or suspensions normally have at least one epoxy, hydroxyl, N-methylol or carbonyl group, or at least two non-conjugated ethylenically unsaturated double bonds.
  • these are N-alkylolamides of ⁇ , ⁇ -monoethylenically unsaturated carboxylic acids having 3 to 10 C atoms, among which the N-methylolacrylamide and the N-methylolmethacrylamide are very particularly preferred and their esters having 1 to 4 C atoms alkanols.
  • two monomers having vinyl radicals two monomers having vinylidene radicals and two monomers having alkenyl radicals are also suitable.
  • Particularly advantageous are the di-esters of dihydric alcohols with ⁇ , ⁇ -mono-ethylenically unsaturated monocarboxylic acids, among which acrylic and methacrylic acid are preferred.
  • alkylene glycol diacrylates and dimethacrylates such as ethylene glycol diacrylate, 1, 2-propylene glycol diacrylate, 1, 3-propylene glycol diacrylate, 1, 3-butylene glycol diacrylate and 1, 4-methylene diacrylate -Propylene glycol dimethacrylate, 1, 3-propylene glycol dimethacrylate, 1, 3-butylene glycol dimethacrylate, 1, 4-butylene glycol dimethacrylate as well as divinylbenzene, vinyl methacrylate, vinyl acrylate, allyl methacrylate, allyla acrylate, dially maleate, diallyl bisyl acrylate, diallyl bisacrylate, Of particular importance in this context are the methacrylic acid and acrylic acid Ci-Cs-hydroxyalkyl esters such as n-hydroxyethyl, n-hydroxypropyl or n-hydroxybutyl acrylate, Of particular importance in this context are the methacrylic acid and acrylic acid Ci-Cs-hydroxyal
  • the abovementioned monomers are generally polymerized in amounts of up to 10% by weight.
  • the cleaning method according to the invention can advantageously be used in the case of polymer filming or caking which have been formed from polymer systems whose homo- or copolymers are at least partially composed of an ethylenically unsaturated Monomers of the following monomer classes are constructed: esters of vinyl alcohol and monocarboxylic acids having 1 to 18 carbon atoms, such as vinyl acetate, vinyl propionate, vinyl n-butyrate, vinyl laurate and vinyl stearate, esters of ⁇ having preferably 3 to 6 carbon atoms , ß-monoethylenically unsaturated mono- and dicarboxylic acids, such as in particular acrylic acid, methacrylic acid, maleic acid, fumaric acid and itaconic acid, with alkanols generally having 1 to 12, preferably 1 to 8 and in particular 1 to 4 carbon atoms, such as, in particular, acrylic acid and Methacrylic acid methyl, ethyl, n-butyl, tert.
  • -butyl-, -iso-butyl and -2-ethylhexyl esters dimethyl maleate or di-n-butyl maleate, ⁇ , ß-monoethylenically unsaturated mono- and dicarboxylic acids and their amides such as acrylic acid, methacrylic acid, maleic acid, fumaric acid, itaconic acid , Acrylamide and methacrylamide, and also ethylenically unsaturated sulfonic acids, such as vinyl sulfonic acid.
  • the cleaning process according to the invention can be used for polymer films or caking formed from polymer systems whose homo- or copolymers are> 10% by weight,> 20% by weight,> 30% by weight,> 40 % By weight,> 50% by weight,> 60% by weight,> 70% by weight,> 80% by weight,> 90% by weight or even 100% by weight, in each case based based on the total amount of ethylenically unsaturated monomers used for the polymerization, composed of at least one ethylenically unsaturated monomer of the following monomer classes: esters of ⁇ , ⁇ -monoethylenically unsaturated mono- and dicarboxylic acids, preferably having 3 to 6 C atoms, such as in particular acrylic acid, Methacrylic acid, maleic acid, fumaric acid and itaconic acid, with alkanols generally having 1 to 12, preferably 1 to 8 and in particular 1 to 4 carbon atoms, such as, in particular, methyl, ethyl,
  • -butyl-, -isobutyl and -2-ethylhexyl ester maleic acid dimethyl ester or maleic acid di-n-butyl ester
  • ⁇ ß-monoethylenically unsaturated mono- and dicarboxylic acids and their amides such as e.g. Acrylic acid, methacrylic acid, maleic acid, fumaric acid, itaconic acid, acrylamide and methacrylamide, and also ethylenically unsaturated sulfonic acids, such as vinylsulfonic acid.
  • the mechanical detachment for example with a high-pressure water jet, facilitates and thus the cleaning time compared to the purely mechanical cleaning is significantly shortened.
  • the period of contacting is strongly dependent, for example, on the volume and type of internals of the separation column, the nature and thickness of the polymer films and caking, the type and amount of the basic compound used, their concentration in aqueous solution, and the one chosen for the cleaning process Temperature and the selected pressure.
  • the contact time can be from a few minutes to several hours. The optimal time period can easily be determined in routine tests that are easy to carry out.
  • the heat exchanger and / or filtration devices upstream or downstream of the separation column can also be cleaned of their adhering polymer films or caking. This is possible by simply contacting the inner surfaces of the separation column with basic washing solution in accordance with the invention by contacting the inner surfaces of the upstream or downstream heat exchangers and / or filtration devices, for example by integrating these apparatuses into the pumping line of the basic Wash solution, expands.
  • the basic washing solution is usually completely emptied from the separation column and any apparatuses connected upstream or downstream.
  • the separation column and any upstream or downstream apparatus are then rinsed with deionized water until the rinsing water has a pH ⁇ 8 or often ⁇ 7.5.
  • the devices After the devices have been completely emptied, they are again available for removing volatile constituents from aqueous polymer suspensions or polymer dispersions.
  • aqueous polymer dispersions In a 9.3 m high separation column with an inner diameter of approx. 50 cm and a total of 10 so-called rain sieve trays, aqueous polymer dispersions, the polymer particles of which were copolymers of tert. -Butyl acrylate, ethyl acrylate and methacrylic acid were built, freed of volatile constituents by introducing 4 bar water vapor. After treating a total of approx. 240 t of aqueous polymer dispersions, the column had heavy deposits, caking and coagulum precipitates with a thickness of up to 5 mm, so that they only had to a throughput reduced compared to the nominal power could be operated.
  • Caking can be determined more.
  • the separation column could again be operated at 100% of its performance.
  • the column had severe filming, deposits and coagulum precipitates with a thickness of up to 5 mm, so that they are only operated at significantly reduced throughputs, in each case based on the corresponding nominal outputs could.
  • aqueous sodium hydroxide solution About 4000 kg of a 2% strength by weight aqueous sodium hydroxide solution at about 25 ° C. were placed in a stirred tank serving as a template. With a volume flow of approx. 12 m 3 per hour, the aqueous sodium hydroxide solution was pumped through one in the feed line Bag filter and a feed device on the top of the column. The aqueous sodium hydroxide solution was heated to about 100 ° C. in the feed line using a steam injector. At the same time, approximately 500 kg of 4 bar water vapor were metered into the separation column at the bottom of the column. The feed of fresh aqueous sodium hydroxide solution was terminated after about 20 minutes.
  • the sodium hydroxide solution collected in the column sump was then pumped back through the feed pump to the top of the column, from where it continuously flowed down over all the trays.
  • the volume flow of the circulation was also approximately 12 m 3 per hour.
  • the amount of 4 bar steam fed in at the bottom of the column was gradually increased to about 1700 kg per hour within 6 hours. After a total of 6 hours, the steam supply and the pumping over of the aqueous sodium hydroxide solution were stopped.
  • the separation column was then completely emptied.
  • the separating column with its feed and discharge lines was then rinsed five times with 200 l of deionized water from the sodium hydroxide solution and in each case completely emptied. In the end, the rinse water had a pH of 7.5.
  • the separation column could again be operated at 100% of its performance.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Other Resins Obtained By Reactions Not Involving Carbon-To-Carbon Unsaturated Bonds (AREA)

Abstract

La présente invention concerne un procédé permettant de nettoyer des colonnes de séparation à travers lesquelles ont été dirigées des suspensions polymères ou dispersions polymères aqueuses après les réactions de polymérisation afin de supprimer les composantes légèrement volatiles. Le procédé se caractérise en ce que le nettoyage comprend une mise en contact des surfaces internes des colonnes de séparation avec une solution aqueuse d'un composé basique.
PCT/EP2001/000154 2000-01-12 2001-01-09 Procede de nettoyage de colonnes de separation Ceased WO2001051159A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU2001240500A AU2001240500A1 (en) 2000-01-12 2001-01-09 Method for cleaning stripping columns

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE10000854.2 2000-01-12
DE10000854A DE10000854A1 (de) 2000-01-12 2000-01-12 Verfahren zum Reinigen von Trennkolonnen

Publications (1)

Publication Number Publication Date
WO2001051159A1 true WO2001051159A1 (fr) 2001-07-19

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Application Number Title Priority Date Filing Date
PCT/EP2001/000154 Ceased WO2001051159A1 (fr) 2000-01-12 2001-01-09 Procede de nettoyage de colonnes de separation

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AR (1) AR026816A1 (fr)
AU (1) AU2001240500A1 (fr)
DE (1) DE10000854A1 (fr)
WO (1) WO2001051159A1 (fr)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003076385A1 (fr) * 2002-03-13 2003-09-18 Basf Aktiengesellschaft Procede de nettoyage de colonnes a plateaux utilisees pour le traitement rectificatif de liquides contenant de l'acide (meth)acrylique et/ou ses esters
WO2004020116A1 (fr) * 2002-08-09 2004-03-11 Basf Aktiengesellschaft Procede de nettoyage d'appareils dans lesquels ont ete traites et / ou produits des solvants organiques contenant de l'acide (meth)acrylique
EP1787972A3 (fr) * 2001-10-09 2007-12-26 Mitsubishi Chemical Corporation Procédé de lavage d'une colonne de distillation utilisée pour la purification d'acides (méth)acryliques.

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112325698A (zh) * 2020-09-27 2021-02-05 河南省科学院能源研究所有限公司 一种工业循环水冷却塔清洗装置及方法

Citations (5)

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Publication number Priority date Publication date Assignee Title
GB1368393A (en) * 1972-06-29 1974-09-25 Sumitomo Chemical Co Removal of deposits from surfaces of polymerization equipment
US3865628A (en) * 1973-02-26 1975-02-11 Cesco Inc Removal of polymer residue from surfaces of processing equipment
SU539065A1 (ru) * 1974-09-30 1976-12-15 Предприятие П/Я А-7827 Состав дл очистки поверхности от налипшего низкомолекул рного полимера
US4904309A (en) * 1986-06-06 1990-02-27 Kanegafuchi Chemical Industry Co., Ltd. Chemical cleaning method of the interior of polymerization reactor
US5728272A (en) * 1995-09-28 1998-03-17 Basf Aktiengesellschaft Separation by rectification of unsaturated carboxylic acids from solvents

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1368393A (en) * 1972-06-29 1974-09-25 Sumitomo Chemical Co Removal of deposits from surfaces of polymerization equipment
US3865628A (en) * 1973-02-26 1975-02-11 Cesco Inc Removal of polymer residue from surfaces of processing equipment
SU539065A1 (ru) * 1974-09-30 1976-12-15 Предприятие П/Я А-7827 Состав дл очистки поверхности от налипшего низкомолекул рного полимера
US4904309A (en) * 1986-06-06 1990-02-27 Kanegafuchi Chemical Industry Co., Ltd. Chemical cleaning method of the interior of polymerization reactor
US5728272A (en) * 1995-09-28 1998-03-17 Basf Aktiengesellschaft Separation by rectification of unsaturated carboxylic acids from solvents

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
DATABASE WPI Section Ch Week 17729, Derwent World Patents Index; Class A35, AN 1977-51661y, XP002167113 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1787972A3 (fr) * 2001-10-09 2007-12-26 Mitsubishi Chemical Corporation Procédé de lavage d'une colonne de distillation utilisée pour la purification d'acides (méth)acryliques.
WO2003076385A1 (fr) * 2002-03-13 2003-09-18 Basf Aktiengesellschaft Procede de nettoyage de colonnes a plateaux utilisees pour le traitement rectificatif de liquides contenant de l'acide (meth)acrylique et/ou ses esters
US7331354B2 (en) 2002-03-13 2008-02-19 Basf Aktiengesellschaft Cleaning of tray columns which have been used for rectificatively treating liquids comprising (meth)acrylic acid and/or esters thereof
WO2004020116A1 (fr) * 2002-08-09 2004-03-11 Basf Aktiengesellschaft Procede de nettoyage d'appareils dans lesquels ont ete traites et / ou produits des solvants organiques contenant de l'acide (meth)acrylique
CN100335184C (zh) * 2002-08-09 2007-09-05 巴斯福股份公司 其中已经处理和/或产生含(甲基)丙烯酸的有机溶剂的设备的清洁方法
US7287534B2 (en) 2002-08-09 2007-10-30 Basf Aktiengesellschaft Cleaning of apparatus in which meth(acrylic) acid-containing organic solvents have been treated and/or generated

Also Published As

Publication number Publication date
AU2001240500A1 (en) 2001-07-24
DE10000854A1 (de) 2001-07-19
AR026816A1 (es) 2003-02-26

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