EP1781634A1 - Procede pour la separation par distillation de trioxane pur - Google Patents

Procede pour la separation par distillation de trioxane pur

Info

Publication number
EP1781634A1
EP1781634A1 EP05775120A EP05775120A EP1781634A1 EP 1781634 A1 EP1781634 A1 EP 1781634A1 EP 05775120 A EP05775120 A EP 05775120A EP 05775120 A EP05775120 A EP 05775120A EP 1781634 A1 EP1781634 A1 EP 1781634A1
Authority
EP
European Patent Office
Prior art keywords
dividing wall
column
wall column
stream
twk1
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.)
Withdrawn
Application number
EP05775120A
Other languages
German (de)
English (en)
Inventor
Markus Siegert
Neven Lang
Eckhard Stroefer
Achim Stammer
Thorsten Friese
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
Publication of EP1781634A1 publication Critical patent/EP1781634A1/fr
Withdrawn legal-status Critical Current

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
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B01D3/146—Multiple effect distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D323/00—Heterocyclic compounds containing more than two oxygen atoms as the only ring hetero atoms
    • C07D323/04—Six-membered rings
    • C07D323/06—Trioxane
    • 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
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • 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
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/141—Fractional distillation or use of a fractionation or rectification column where at least one distillation column contains at least one dividing wall

Definitions

  • the invention relates to a process for the distillative separation of pure trioxane from a feed stream containing trioxane, formaldehyde and water.
  • Trioxane is generally prepared by reactive distillation of aqueous formaldehyde solution in the presence of acidic catalysts. From the trioxane containing formaldehyde and water distillate then the trioxane with halogenated hydrocarbons, such as methylene chloride or 1, 2-dichloroethane, or other, water-immiscible solvents extracted.
  • halogenated hydrocarbons such as methylene chloride or 1, 2-dichloroethane, or other, water-immiscible solvents extracted.
  • DE-A 1 668 867 describes a process for the separation of trioxane from mixtures containing water, formaldehyde and trioxane by extraction with an organic solvent.
  • an extraction section consisting of two sections is fed at one end with a customary organic water-immiscible extractant for trioxane, at the other end with water.
  • the distillate to be separated is added to the trioxane synthesis.
  • An aqueous formaldehyde solution is then obtained on the side of the solvent feed and a virtually formaldehyde-free solution of trioxane in the solvent is obtained on the side of the water feed.
  • the distillate resulting from the trioxane synthesis from 40% by weight of water, 35% by weight of trioxane and 25% by weight of formaldehyde is metered into the middle part of a pulsation column, at the upper end of the column methylene chloride and at the lower end of the column Water supplied.
  • about 25% strength by weight solution of trioxane in methylene chloride is obtained at the lower end of the column and about 30% strength by weight aqueous formaldehyde solution is obtained at the upper end of the column.
  • DE-A 197 32 291 describes a process for the separation of trioxane from an aqueous mixture consisting essentially of trioxane, water and formaldehyde, in which trioxane is removed from the mixture by pervaporation and the trioxane-enriched permeate is purified by rectification Trioxane and an azeotropic mixture of trioxane, water and formaldehyde separates.
  • an aqueous mixture consisting of 40% by weight of trioxane, 40% by weight of water and 20% by weight is used.
  • the azeotropic mixture is passed into a pervaporation unit containing a membrane of polydimethylsiloxane with a hydrophobic zeolite.
  • the trioxane-enriched mixture is separated in a second distillation column under normal pressure in trioxane and again in an azeotropic mixture of trioxane, water and formaldehyde. This azeotropic mixture is recycled before the pervaporation stage.
  • the object is achieved by a process for the distillative separation of pure trioxane from a feed stream containing trioxane in a mass fraction of at least 50 wt .-%, based on the total weight of the feed stream and in addition formaldehyde and water, that is characterized in that the feed stream and a further water-containing stream which does not contain non-feedstock components comprise a first dividing wall column with a dividing wall arranged in the column longitudinal direction, which accommodates the column interior in a feed zone, a removal zone, an upper common column zone and a lower common column area divides, are supplied, and that from the first dividing wall column, a bottom stream containing pure trioxane and a side stream from the removal area, containing pure water, are withdrawn.
  • trioxane / formaldehyde / water feed mixture, provided it contains a relatively high weight fraction of at least 50% by weight, preferably from 60 to 80% by weight of trioxane, in a single column Separation of pure trioxane and pure water to separate.
  • pure trioxane is understood as meaning a stream which contains at least 97.5% by weight, preferably at least 99% by weight, or 99.9% by weight of trioxane, and as pure water a stream having a water content of at least 95.0 wt .-%, be ⁇ preferably from at least 99.0 wt .-%.
  • ultrapure trioxane refers to a stream which contains at least 99.95% by weight or 99.96% by weight or else 99.99% by weight of trioxane.
  • a dividing wall column i. a distillation column having a separation wall arranged in the longitudinal direction of the column, which prevents mixing of liquid and bromine streams in partial regions of the column and which separates the column interior into a feed region, a removal region, an upper common column region and a lower common column region.
  • Dividing wall columns are known and described, for example, in EP-A 0 122 367, EP-A 0 126 288 or EP-A 0 133 510.
  • the dividing wall is not welded into the column, but designed in the form of loosely inserted and adequately sealed partial segments.
  • the loose dividing wall advantageously has internal manholes or removable segments which allow the inside of the column to pass from one side of the dividing wall to the other side thereof.
  • the liquid distribution in the individual Operaberei ⁇ surfaces of the first and / or second dividing wall column can be set uniquely targeted.
  • the liquid in the reinforcing part of the feed region and / or the removal region can be more intensively applied in the wall region and in the stripping section of the feed region and / or the removal region in the wall region of the partition wall.
  • the feed stream is preferably composed as follows: 60 to 80% by weight of trioxane, 10 to 30% by weight of water, 3 to 20% by weight of formaldehyde and optionally also up to 15% by weight of low-boiling components selected from a or more of the following substances: methyl formate, methylal, dimethoxydimethyl ether, methanol, formic acid and other hemiacetals and acetals.
  • the first dividing wall column is fed with an additional hydrous stream which contains no components foreign to the feed stream and whose water content preferably carries at least 10% by weight, in particular at least 50% by weight.
  • the feed stream by concentrating a crude trioxane stream obtained as a reactor effluent from a trioxane synthesis reactor, by separating low boilers and high boilers to a Trioxangehalt of at least 50 wt .-%, preferably of at least 60 wt .-%, on preferably at least 70% by weight.
  • the present process is not restricted with respect to the specific process management in the trioxane synthesis reactor.
  • the crude trioxane stream obtained in the trioxane synthesis generally has the following composition: 55 to 85% by weight of formaldehyde, 15 to 35% by weight of water, 1.0 to 30% by weight of trioxane and also low-boiling components and high boilers.
  • low-boiling substances are substances whose boiling point is lower than the boiling point of pure trioxane and, as high boilers, substances whose boiling point is higher than the boiling point of pure trioxane.
  • Low boilers are present in particular methylal, methanol and methyl formate and high boilers in particular dimethoxydimethyl ether and formic acid.
  • the crude trioxane stream is preferably fed to a dividing wall column in the feed region of the same and withdrawn from the removal region thereof a side stream concentrated to trioxane, which is conducted as feed stream into the first dividing wall column.
  • the bottom stream from the second dividing wall column generally contains less than 1% by weight, preferably less than 0.1% by weight, of trioxane, particularly preferably less than 0.01% by weight of trioxane.
  • the bottom stream is composed, for example, as follows: 65 to 85% by weight of formaldehyde, 15 to 35% by weight of water and 0 to 1% by weight of trioxane.
  • the second dividing wall column for concentrating the crude trioxane stream is preferably operated at a top pressure in the range from 0.10 to 5.0 bar absolute, in particular at a top pressure in the range from 0.50 to 2.50 bar absolute.
  • the first dividing wall column from which pure trioxane and pure water is separated, is advantageous at a higher top pressure than the second dividing wall column, namely at a pressure of 0.1 to 15.0 bar higher than the head pressure of the second dividing wall column, operated.
  • the first and / or the second dividing wall column are preferably laid out in such a way that the number of theoretical separation stages is in each case between 4 and 90, preferably between 15 and 60.
  • the sum of the number of theoretical plates in the feed is preferably 80 to 120%, more preferably 90 to 100% of the sum of the number of Trenn ⁇ stages in the removal region of the first and / or the second dividing wall column.
  • the theoretical separation stages in the first dividing wall column and / or in the second dividing wall column are preferably divided into the individual column regions as follows:
  • the feed points for the respective feed stream or the tapping points for the respective side draw stream can preferably be positioned as follows:
  • the feed point for the feed stream into the feed region of the first dividing wall column or for the reactor effluent from a trioxane synthesis reactor into the feed zone of the second dividing wall column are each from the soabzugs ⁇ point from the removal region of the first dividing wall column or the Soabzugsstelle from the removal region of the second dividing wall column at different heights in the dividing wall column, in particular by 1 to 20, preferably by 1 to 10 theoretical plates spaced apart arranged.
  • the feed region and / or the removal region of the first dividing wall column and / or the second dividing wall column are preferably completely or partially filled with ordered packings or random packings.
  • the dividing wall is designed to be heat-insulating in the regions equipped with geord ⁇ Neten packings or packing.
  • the side draw stream can be withdrawn both liquid and gaseous in the first and in the second dividing wall column.
  • the distribution of the vapor stream at the lower end of the dividing wall in the first and / or the second dividing wall column may be subject to a natural distribution.
  • the vapor stream at the lower end of the dividing wall of the first and / or the second dividing wall column can be adjusted by the choice and / or dimensioning of the separating internals and / or by the installation of pressure loss generating devices, in particular diaphragms, such that the Ratio of the vapor stream in the inlet region to the vapor stream in the removal region 0.5 to 1, 5, preferably 0.9 to 1, 1, is.
  • the liquid draining out of the upper common column region of the first and / or the second dividing wall column can preferably be collected in a collecting chamber arranged inside or outside the dividing wall column and split up by a fixed setting or regulation at the upper end of the dividing wall such that the ratio of the liquid flow to the inlet region to the liquid flow to the removal region 0.1 to 1, 0, preferably 0.25 to 0.8, is.
  • the liquid can be conveyed to the inlet region via a pump or fed volume-controlled via a static inlet height of at least 1 m, preferably via a cascade control in conjunction with the liquid level control of the collecting space, wherein the control is adjusted so that the the amount of liquid introduced into the inlet can not fall below 30% of its normal value.
  • the amount of liquid removed via the side take-off of the removal region can advantageously be regulated so that the amount of liquid applied to the enrichment part of the removal region can not fall below 30% of its normal value.
  • sampling possibilities can be provided in the first and / or second dividing wall column at the upper and at the upper end of the dividing wall, which make it possible to withdraw samples from the dividing wall column continuously or at regular intervals in liquid or gaseous form and with regard to their composition , preferably by gas chromatography, to examine.
  • the division ratio of the liquid at the upper end of the dividing wall in the first and / or second dividing wall column can be advantageously adjusted so that the concentration of those high-boiling components for which a certain limit value for the concentration is not to be exceeded in the side draw, in the liquid 5 to 75%, preferably 5 to 50% of the limit value in the side take-off and that the liquid distribution at the upper end of the partition is adjusted so that at higher levels of high-boiling components more liquid and lower levels of high-boiling components less liquid is directed to the inlet area.
  • the concentration of low-boiling components for which a specific limit value is not to be exceeded in the side stream is advantageously set at 10 to 99%, preferably 25 to 97.5%, of the limit value prescribed for the side stream at the lower end of the dividing wall and regulated the heat output of the bottom evaporator in such a way that at a higher content of low-boiling components, the heating power increases and th with a lower content of low-boiling Komponen ⁇ the heating power is reduced.
  • the removal of the top stream from the first and / or the second Trennwandkolon ⁇ ne can advantageously be temperature controlled, being used as the measuring temperature a Mess ⁇ point in the upper common column area of the first and / or second Trenn ⁇ wall column, which by 1 to 25, preferably is arranged by 1 to 10 theoretical plates below the upper end of the first and / or second Trennwandko- lonne.
  • the removal of the bottom product from the first and / or second Trennwandkolon ⁇ ne can advantageously be temperature-controlled, being used as the control temperature Mess ⁇ a site in the lower common column area of the first and / or second separation wall column, by 1 to 25, preferably in order 2 to 15 theoretical Separating stages above the lower end of the first and / or second Trennwandko ⁇ lonne is arranged.
  • the removal of the side stream from the removal region of the first and / or second dividing wall column can preferably be controlled in a controlled manner, and the liquid state can be used in the bottom evaporator.
  • each of the thermally coupled columns is each equipped with its own evaporator and its own condenser.
  • the thermally coupled columns can be operated at different pressures.
  • the bottom stream from the first of the thermally coupled columns can be partially or completely evaporated in an additional evaporator and then the second of the thermally coupled columns two-phase or supplied in the form of a gförmi- and a liquid stream.
  • the feed stream can be partially or completely pre-evaporated and fed to the first separation wall column or the first of the thermally coupled columns in two-phase or in the form of a gaseous and a liquid stream.
  • a single dividing wall column which corresponds to the above-described first dividing wall column and which thus the feed stream described above, containing at least 50 wt .-% of trioxane, based on the total weight of the feed stream, preferably in the middle Area, is supplied.
  • the reaction effluent from the trioxane synthesis reactor is fed to a first distillation column containing at least 2, preferably from 2 to 50, theoretical separating substances which absorb at a head pressure between 0.1 and 2 bar absolute, preferably 0.5 to 2 bar abso ⁇ lut, for example, 1 bar absolute, is operated.
  • the stripping section generally comprises at least 25% of the total number of theoretical stripping agents of the column, preferably 50 to 90%.
  • the feed stream to the first distillation column which is the reactor from an upstream trioxane synthesis reactor, generally contains from 35 to 80% by weight of formaldehyde, from 25 to 45% by weight of water and from 1 to 30% by weight of trioxane.
  • This mixture is separated in the first distillation column into a stream from the lower region of the first distillation column, in particular a bottom stream and a stream from the upper region of the first distillation column, in particular a top stream.
  • the stream from the lower region of the first distillation column generally contains from 51 to 80% by weight of formaldehyde, from 20 to 49% by weight of water and from 0 to 1% by weight of trioxane and is preferably recycled to the trioxane synthesis reactor.
  • the stream from the upper region of the first distillation column generally contains from 1 to 15% by weight of formaldehyde, from 15 to 35% by weight of water and from 60 to 80% by weight of trioxane and is fed to a second distillation column for the removal of low-boiling components ,
  • the trioxane synthesis reactor can also be combined with the first distillation column in a reactive distillation column. In the stripping section, this can contain a catalyst fixed bed of a heterogeneous catalyst. Alternatively, the reactive distillation can also be carried out in the presence of a homogeneous catalyst.
  • the top stream from the first distillation column is preferably fed to a second distillation column for the separation of low boilers.
  • Conventional low-boiling components which can be formed in the trioxane synthesis and the subsequent distillative separation are methyl formate, methylal, dimethoxydimethyl ether, trimethoxydimethyl ether, methanol, formic acid and further hemiacetals and full acetals.
  • the low-boiling components are preferably separated off via the top of the second distillation column, which is preferably operated at a pressure of 1 to 2 bar.
  • the low boiler separation column has at least 5 theoretical plates, preferably 15 to 50 theoretical plates.
  • the Ab ⁇ drive part of this column comprises 25 to 90% of the theoretical plates of this column.
  • trioxane with a degree of purity corresponding to the minimum contents for ultrapure trioxane defined at the outset, it is possible to feed the pure trioxane stream to a further third distillation column which has the function of a high-purity column and in which high-boiling components are separated off from trioxane.
  • the trioxane-pure column can be designed with 5 to 20 theoretical plates and can be operated at atmospheric pressure or under atmospheric or superatmospheric pressure.
  • the trioxane ultra-pure column is particularly equipped with stripping and reinforcing part, but it may also be a pure stripping column without reinforcing part.
  • an ultrapure trioxane-containing stream is withdrawn from the upper region thereof, condensed in a condenser at the top of the column, partly returned to the column as reflux, and otherwise withdrawn as a product stream.
  • the bottom stream from the trioxane-pure column which still contains high-boiling components compared to trioxane, is preferably recycled to the trioxane synthesis reactor.
  • the pure trioxane or pure trioxane obtained is preferably used for the preparation of polyoxymethylene, polyoxymethylene derivatives such as polyoxymethylene dimethyl ether and diaminodiphenylmethane.
  • FIG. 1 shows the schematic representation of a plant for carrying out a preferred embodiment of the method according to the invention
  • Figure 2 is a schematic representation of a system for carrying out a further preferred embodiment of the method according to the invention.
  • the plant shown in Figure 1 has two dividing wall columns, TWK 1 and TWK2, each with a arranged in the column longitudinal partition, TW 1 and TW 2, the column interior in each case in a feed, A1, A2, a removal range, B1, B2 , an upper common column area C1, C2 and ei ⁇ nen lower common column area D1, D2, split.
  • the dividing wall columns TWK1 and TWK2 each have bottom evaporators and condensers on the bottom of the column.
  • the second dividing wall column TWK 2 is preceded by a trioxane synthesis reactor R.
  • a formaldehyde-rich aqueous solution is fed to the trioxane synthesis reactor, which is designed as an evaporator, stirred tank, fixed or fluidized bed reactor.
  • a trioxane / formaldehyde / water mixture VI is withdrawn, combined with the recycle stream VII, which is obtained as top stream from the first dividing wall column TWK1, and fed to the feed region A2 of the second dividing wall column TWK2.
  • a formaldehyde-rich bottom draw stream V which is recycled to the trioxane synthesis reactor R, and a side stream, which is fed as feed stream I to the feed zone A1 of the first dividing wall column TWK1.
  • first dividing wall column TWK1 is supplied with another hydrous stream II at a suitable point thereof.
  • a formaldehyde-rich, aqueous stream 1, with a formaldehyde content of usually 50 to 80% by weight, is fed to the trioxane synthesis reactor R, which forms an evaporator, stirred tank, fixed or fluidized bed reactor is.
  • the trioxane / formaldehyde / water mixture 2 leaving the trioxane synthesis reactor R is fed to the first distillation column K1 and separated into a bottom stream 3 containing formaldehyde and water and an overhead stream 4 containing formaldehyde, water and trioxane.
  • the bottom stream 3 is recycled to the trioxane synthesis reactor R.
  • the top stream 4 is condensed in a condenser at the top of the column, partly fed back to the column K1 as reflux, and otherwise fed to a second column K2 for the removal of low-boiling components.
  • a second column K2 for the removal of low-boiling components.
  • an overhead stream 5 containing low-boiling components inter alia methyl formate, methylal, dimethoxydimethyl ether and methanol, is withdrawn, condensed in a condenser at the top of the column, partly returned to the column as reflux, and otherwise discharged.
  • the bottom stream 6 from the low boiler separation column K2 is fed to a first dividing wall column TWK1, which is constructed as described for Figure 1, and from which a top stream 7 is withdrawn, which condenses in a condenser at the top of the column, partly as return to the first partition ⁇ TWK1 column abandoned and recycled in the rest in the first distillation column K1.
  • a side draw stream 8 corresponding to the side draw stream IV of the process variant shown in FIG.
  • a bottom stream 9 containing pure trioxane which corresponds to the bottom stream III from the process variant shown in FIG
  • the bottom stream 9 from the dividing wall column TWK1 is fed to a third distillation column K3, and is separated therein into a top stream 10 containing ultrapure trioxane and a bottom stream 11 which is recycled to the trioxane synthesis reactor R.
  • a water-rich stream 12 is fed to the dividing wall column TWK1 and to the distillation column K1, in each case at a suitable point thereof.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Heterocyclic Compounds That Contain Two Or More Ring Oxygen Atoms (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

L'invention concerne un procédé pour séparer par distillation du trioxane pur d'un flux d'alimentation (I) contenant du trioxane dans un pourcentage en masse d'au moins 50 % en poids par rapport au poids total du flux d'alimentation (I), et contenant en outre du formaldéhyde et de l'eau. Le procédé selon l'invention est caractérisé en ce que le flux d'alimentation (I), ainsi qu'un autre flux (II) contenant de l'eau et ne contenant aucun constituant étranger au flux d'alimentation, sont amenés à une colonne à paroi séparatrice (TWK1) comprenant une paroi séparatrice pratiquement perpendiculaire (TW) qui sépare l'espace intérieur de la colonne en une zone d'amenée (A1), en une zone de prélèvement (B1), en une zone de colonne commune supérieure (C1), ainsi qu'en une zone de colonne commune inférieure (D1). Une fraction de bas de colonne (III) contenant du trioxane pur et une fraction latérale (IV) contenant de l'eau pure sont prélevées de la première colonne à paroi séparatrice (TWK1), au niveau de la zone de prélèvement (B1).
EP05775120A 2004-08-19 2005-08-18 Procede pour la separation par distillation de trioxane pur Withdrawn EP1781634A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102004040284A DE102004040284A1 (de) 2004-08-19 2004-08-19 Verfahren zur destillativen Abtrennung von Rein-Trioxan
PCT/EP2005/008944 WO2006018302A1 (fr) 2004-08-19 2005-08-18 Procede pour la separation par distillation de trioxane pur

Publications (1)

Publication Number Publication Date
EP1781634A1 true EP1781634A1 (fr) 2007-05-09

Family

ID=35159685

Family Applications (1)

Application Number Title Priority Date Filing Date
EP05775120A Withdrawn EP1781634A1 (fr) 2004-08-19 2005-08-18 Procede pour la separation par distillation de trioxane pur

Country Status (8)

Country Link
US (1) US20070293688A1 (fr)
EP (1) EP1781634A1 (fr)
JP (1) JP2008509960A (fr)
KR (1) KR20070046870A (fr)
CN (1) CN101006073A (fr)
DE (1) DE102004040284A1 (fr)
MY (1) MY138442A (fr)
WO (1) WO2006018302A1 (fr)

Families Citing this family (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
MY153212A (en) * 2007-01-25 2015-01-29 Basf Se Method for separating trioxane from a triozane/formaldehyde/water mixture by means of pressure change rectification
CN101121709B (zh) * 2007-09-17 2010-08-11 浙江三博聚合物有限公司 三聚甲醛合成后的初步提浓、净化的方法
US8350063B2 (en) * 2007-10-09 2013-01-08 Basf Se Method for separating tioxane from a trioxane/formaldehyde/water mixture by means of pressure change rectification
JP5355587B2 (ja) * 2007-12-19 2013-11-27 ビーエーエスエフ ソシエタス・ヨーロピア 粗トリオキサンの製造法
BRPI1008753B1 (pt) * 2009-02-12 2020-01-28 Lg Chemical Ltd coluna de destilação com parede divisória
KR101236664B1 (ko) * 2009-07-20 2013-02-22 주식회사 엘지화학 에너지 절감형 증류탑 어셈블리
CN102631791B (zh) * 2012-03-31 2016-03-09 中国石油化工股份有限公司 一种分壁精馏塔的控制方法
CN102633770B (zh) * 2012-04-06 2013-12-18 邢台旭阳煤化工有限公司 一种三聚甲醛脱除轻组分的方法及装置
CN102702167B (zh) * 2012-05-11 2015-01-07 北京旭阳化工技术研究院有限公司 三聚甲醛合成过程中在线脱甲酸的方法
CN103664460B (zh) * 2012-09-18 2015-03-11 中国石油化工集团公司 一种制备间戊二烯和双环戊二烯的系统及方法
KR102091679B1 (ko) * 2013-02-21 2020-03-23 쥐티씨 테크놀로지 유에스,엘엘씨 분할된 증류탑을 사용하는 분리 공정
DE102013207282A1 (de) * 2013-04-22 2014-11-06 Wacker Chemie Ag Verfahren und Vorrichtung zur destillativen Trennung eines Drei- oder Mehrkomponentengemisches
US9504934B2 (en) 2013-10-27 2016-11-29 Purdue Research Foundation Multicomponent dividing wall columns
CN110559678B (zh) * 2019-10-21 2024-02-27 无锡赫利邦化工科技有限公司 一种聚甲氧基二甲醚合成与分离的精馏塔及其使用方法
WO2023140986A1 (fr) 2022-01-19 2023-07-27 Exxonmobil Chemical Patents Inc. Compositions contenant du tri-cyclopentadiène et leurs procédés de fabrication

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3328126A1 (de) * 1983-08-04 1985-02-21 Basf Ag, 6700 Ludwigshafen Verfahren zur herstellung von trioxan aus waessrigen, handelsueblichen formaldehydloesungen
DE19526307A1 (de) * 1995-07-19 1997-01-23 Hoechst Ag Verfahren zur Abtrennung von Trioxan aus einem wäßrigen Gemisch
DE19732291A1 (de) * 1997-07-26 1999-01-28 Basf Ag Verfahren zur Abtrennung von Trioxan
DE19851481A1 (de) * 1998-11-09 2000-05-11 Ticona Gmbh Destillative Trennung von flüssigen Gemischen enthaltend Formaldehyd, Trioxan, Alkohol und Hemiformal
DE10021703A1 (de) * 2000-05-04 2001-11-08 Basf Ag Verfahren zur destillativen Trennung von Tetrahydrofuran, gamma-Butyrolacton und/oder 1,4-Butandiol enthaltenden Gemischen

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2006018302A1 *

Also Published As

Publication number Publication date
WO2006018302A1 (fr) 2006-02-23
MY138442A (en) 2009-06-30
CN101006073A (zh) 2007-07-25
US20070293688A1 (en) 2007-12-20
JP2008509960A (ja) 2008-04-03
KR20070046870A (ko) 2007-05-03
DE102004040284A1 (de) 2006-02-23

Similar Documents

Publication Publication Date Title
EP1781634A1 (fr) Procede pour la separation par distillation de trioxane pur
EP1931650B1 (fr) Procede de production de dioxolane
EP1280787B1 (fr) Procede pour la separation par distillation de melanges contenant du tetrahydrofurane, de la gamma-butyrolactone et/ou du 1,4-butanediol
EP1351909B1 (fr) Procede de traitement par distillation de 1,6-hexandiol, de 1,5-pentandiol et de caprolactone
EP4093724A1 (fr) Procédé de production simultanée d'alcoolates de sodium et de potassium
EP1699776B1 (fr) Procede de separation de trioxane d'un melange trioxane/formaldehyde/eau a l'aide de la rectification par modification de pression
EP2114544B1 (fr) Procédé de séparation de trioxane d'un mélange trioxane/formaldéhyde/eau par rectification à échange de pression
EP2569274A1 (fr) Séparation par distillation d'acide acrylique par l'intermédiaire d'une conduite d'évacuation latérale
EP3323800A1 (fr) Procédé de fabrication des éthers diméthyliques de polyoxyméthylène à partir du formaldéhyde et du méthanol dans des solutions aqueuses
EP1699537B1 (fr) Procede pour separer le trioxane d'un melange de trioxane/formaldehyde/eau
EP1805162B1 (fr) Procede de fabrication de trioxane caracterise en ce qu'un courant secondaire aqueux est soutire a la premiere etape de distillation
EP1115682B1 (fr) Procede de production de monoethylene glycol de haute purete
EP1660426A1 (fr) Procede de traitement de compositions contenant du 1,1,2,2-tetramethoxyethane et du glyoxaldimethylacetal
EP1915358B1 (fr) Procede integre pour preparer du trioxane a partir de formaldehyde
WO2022167311A1 (fr) Procédé de préparation écoénergétique d'alcoolates de métal alcalin
EP1912965A1 (fr) Procede integre de production de trioxane a partir de formaldehyde
WO2007017479A1 (fr) Procede integre de production de trioxane a partir de formaldehyde
EP2032553B1 (fr) Procédé intégré de préparation de trioxanne à partir de formaldéhyde
DE102016211734A1 (de) Verfahren zur Aufreinigung von Acrylsäurederivaten
DD283041A7 (de) Verfahren zur herstellung von absolutalkohol ausgehend von gaerungsalkohol

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20070319

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HU IE IS IT LI LT LU LV MC NL PL PT RO SE SI SK TR

DAX Request for extension of the european patent (deleted)
RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: BASF SE

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN

18D Application deemed to be withdrawn

Effective date: 20080930