EP1613575A2 - Procede d elimination d un solvant contenu dans l' acetylene. installation pour la mise en oeuvre du procede - Google Patents

Procede d elimination d un solvant contenu dans l' acetylene. installation pour la mise en oeuvre du procede

Info

Publication number
EP1613575A2
EP1613575A2 EP04721218A EP04721218A EP1613575A2 EP 1613575 A2 EP1613575 A2 EP 1613575A2 EP 04721218 A EP04721218 A EP 04721218A EP 04721218 A EP04721218 A EP 04721218A EP 1613575 A2 EP1613575 A2 EP 1613575A2
Authority
EP
European Patent Office
Prior art keywords
acetylene
gas
solvent
bed
liquid impurities
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Withdrawn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
EP04721218A
Other languages
German (de)
English (en)
French (fr)
Inventor
Fabrice Delcorso
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.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA a Directoire et Conseil de Surveillance pour lEtude et lExploitation des Procedes Georges Claude
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 Air Liquide SA, LAir Liquide SA a Directoire et Conseil de Surveillance pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP1613575A2 publication Critical patent/EP1613575A2/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers

Definitions

  • the subject of the invention is a process for the purification of acetylene.
  • Acetylene is industrially stored under pressure in containers in the form of a solute in a solvent or in a mixture of solvents such as acetone or dimethylformamide (DMF), fixed by a porous material.
  • the pressure in the container is between approximately 15.10 5 Pa and 20.10 5 Pa.
  • acetylene When stored in solution in a solvent, acetylene contains at the outlet of the container, in addition to conventional impurities, oxygen, nitrogen, water or phosphine, a non-negligible amount of solvent in a content essentially dependent on storage pressure and temperature.
  • acetylene When it comes to acetone, acetylene generally contains between 1% v / v and 10% v / v. Sometimes the solvent is entrained in liquid form with acetylene which hinders the user in the application in which he uses it.
  • Another solution is to produce acetylene on the user's site to avoid this storage in solvent.
  • This solution is not always industrially possible because the process by cracking hydrocarbons involves large investments which can only be made profitable by a high consumption of acetylene by the user. The same applies to the process by hydrolysis of calcium carbide.
  • the subject of the invention is a process for the purification of acetylene stored under pressure in a container dissolved in a solvent, characterized in that it comprises: At least one step (a) of expansion of the acetylene at the outlet of the container, to produce a stream of acetylene gas comprising a non-zero quantity of liquid impurities,
  • the acetylene obtained at the end of step (a) must be at a temperature sufficient to prevent its liquefaction and lower than the temperature Tdec, causing the decomposition of said gas. This temperature depends in particular on the working pressure of the gas.
  • the process as defined above is generally implemented for a pressure of use of the acetylene gas greater than atmospheric pressure (approximately 10 5 Pa) and generally less than 10.10 5 Pa (10 bars) and more particularly less than or equal to 5.10 5 Pa (5 bars).
  • atmospheric pressure approximately 10 5 Pa
  • 10.10 5 Pa 10.10 5 Pa
  • 5.10 5 Pa 5.10 5 Pa
  • the process may include one or more separation steps.
  • separation step (b) there is for example a step of condensing the solvent by cooling the gas stream from step (a) to a temperature lower than or equal to the liquefaction temperature of the solvent or of the mixture of solvents. .
  • the stream of acetylene gas is more particularly made to circulate through a bed of activated carbon.
  • the activated carbon used in the process which is the subject of the present invention has the following properties:
  • the speed of circulation of the flow in the activated carbon bed is between 1 cm / s and 1 m / s and preferably between 5 cm / s and 50 cm / s.
  • the acetylene leaving the container is expanded to a pressure less than or equal to 2.5 ⁇ 10 5 Pa (2.5 bars) and it is cooled to a temperature less than or equal to -15 ° C. .
  • the solvent condensed during step (b) is recovered to be reused.
  • it comprises a step of regenerating the bed of adsorbents.
  • the regeneration of the adsorbent bed is carried out for example, with a hot gas such as nitrogen or acetylene, within pressure and temperature limits which do not induce acetylene instability. whether it is regenerating gas or whether it is the fraction of adsorbed gas.
  • a hot gas such as nitrogen or acetylene
  • the latter is preferably again subjected to steps (b) then (c) of the process as defined above.
  • the invention finally relates to an acetylene production installation capable of implementing the method as defined above, comprising: an expansion means capable of delivering, at its outlet, acetylene at a pressure below 10.10 5 Pa (10 bars) and more particularly less than or equal to 5.10 5 Pa (5 bars), a means of exchanging frigories able to deliver downstream, a stream of gas cooled to a temperature between -70 ° C and 15 ° C, a means of purification by adsorption on a bed of particles and more particularly on a bed of activated carbon, capable of separating the residual liquid impurities from the cooled gas flow, a first connection pipe adapted so that the expanded gas s '' flows there from the outlet of said expansion means to the inlet of said refrigerant exchange means, and a second connecting pipe adapted so that the cooled gas flows there from the outlet of said refrigerant exchange means until the entry of said purification means by adsorption on a bed of particles.
  • an expansion means capable of delivering, at its
  • the refrigeration exchange means will consist of one or more exchangers connected to each other in series or in parallel, supplied with a refrigerant having a temperature lower than the gas flowing against the flow of the gas to be cooled.
  • it comprises means for recovering the droplets of condensed solvent.
  • a capacity containing packing rings provided with a drain in its lower part, to allow the evacuation of the condensate.
  • the means for recovering droplets is integrated by means of exchange of fiigories.
  • the means of separation by adsorption will consist of one or more beds of particles.
  • the installation is insulated as a whole so as to limit the transfers of heat energy with the external environment with the exception of said first connecting pipe.
  • Said first connecting line is long enough to prevent the acetylene from cooling downstream of the regulator
  • the installation comprises a third non-insulated pipe adapted so that the hot gases serving for the regeneration of the adsorbent bed flow therein at the outlet of said bed and having a length large enough to not create hot spots in the residual acetylene .
  • the process and the installation which are the subject of the present invention have the following advantages: They make it possible to easily make available to the user acetylene with a very low residual solvent content, often less than 500 ppm. When the process involves passing over a bed of adsorbents, they make it possible to obtain the gas with an impurity content of less than 100 ppb.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Separation Of Gases By Adsorption (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
EP04721218A 2003-04-04 2004-03-17 Procede d elimination d un solvant contenu dans l' acetylene. installation pour la mise en oeuvre du procede Withdrawn EP1613575A2 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR0304192A FR2853313B1 (fr) 2003-04-04 2003-04-04 Procede d'elimination d'un solvant contenu dans l'acetylene, installation pour la mise en oeuvre du procede
PCT/FR2004/050112 WO2004089859A2 (fr) 2003-04-04 2004-03-17 Procede d'elimination d'un solvant contenu dans l'acetylene. installation pour la mise en oeuvre du procede

Publications (1)

Publication Number Publication Date
EP1613575A2 true EP1613575A2 (fr) 2006-01-11

Family

ID=32982233

Family Applications (1)

Application Number Title Priority Date Filing Date
EP04721218A Withdrawn EP1613575A2 (fr) 2003-04-04 2004-03-17 Procede d elimination d un solvant contenu dans l' acetylene. installation pour la mise en oeuvre du procede

Country Status (4)

Country Link
EP (1) EP1613575A2 (https=)
JP (2) JP2006522079A (https=)
FR (1) FR2853313B1 (https=)
WO (1) WO2004089859A2 (https=)

Families Citing this family (19)

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Publication number Priority date Publication date Assignee Title
US7915166B1 (en) 2007-02-22 2011-03-29 Novellus Systems, Inc. Diffusion barrier and etch stop films
US20080242912A1 (en) * 2007-03-29 2008-10-02 Olivier Letessier Methods and Apparatus for Providing a High Purity Acetylene Product
FR2912401A1 (fr) * 2007-07-17 2008-08-15 Air Liquide Nouveau procede d'elimination d'un solvant contenu dans de l'acetylene sous pression. installation pour la mise en oeuvre du procede
FR2915991A1 (fr) * 2007-07-17 2008-11-14 Air Liquide Nouveau procede d'elimination d'un solvant contenu dans de l'acetylene detendu. installation pour la mise en oeuvre du procede
US8962101B2 (en) 2007-08-31 2015-02-24 Novellus Systems, Inc. Methods and apparatus for plasma-based deposition
US7820556B2 (en) * 2008-06-04 2010-10-26 Novellus Systems, Inc. Method for purifying acetylene gas for use in semiconductor processes
US8435608B1 (en) 2008-06-27 2013-05-07 Novellus Systems, Inc. Methods of depositing smooth and conformal ashable hard mask films
US8129577B2 (en) 2008-09-16 2012-03-06 Air Products And Chemicals, Inc. Process and system for providing acetylene
KR101493756B1 (ko) * 2008-09-16 2015-02-17 에어 프로덕츠 앤드 케미칼스, 인코오포레이티드 아세틸렌을 제공하기 위한 방법 및 시스템
US8398747B2 (en) 2009-06-23 2013-03-19 Praxair Technology, Inc. Processes for purification of acetylene
US8563414B1 (en) 2010-04-23 2013-10-22 Novellus Systems, Inc. Methods for forming conductive carbon films by PECVD
SG195494A1 (en) 2012-05-18 2013-12-30 Novellus Systems Inc Carbon deposition-etch-ash gap fill process
US9362133B2 (en) 2012-12-14 2016-06-07 Lam Research Corporation Method for forming a mask by etching conformal film on patterned ashable hardmask
US9304396B2 (en) 2013-02-25 2016-04-05 Lam Research Corporation PECVD films for EUV lithography
US9320387B2 (en) 2013-09-30 2016-04-26 Lam Research Corporation Sulfur doped carbon hard masks
US9589799B2 (en) 2013-09-30 2017-03-07 Lam Research Corporation High selectivity and low stress carbon hardmask by pulsed low frequency RF power
JP6975625B2 (ja) * 2017-11-29 2021-12-01 大陽日酸株式会社 真空浸炭炉用アセチレンガス供給装置及びその供給方法
US11837441B2 (en) 2019-05-29 2023-12-05 Lam Research Corporation Depositing a carbon hardmask by high power pulsed low frequency RF
CN114342043A (zh) 2019-08-30 2022-04-12 朗姆研究公司 低压下的高密度、模量和硬度的非晶碳膜

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ES344914A1 (es) * 1967-09-09 1969-02-01 Flix Electro Quimica Procedimiento e instalacion para secado de gases de poca solubilidad inertes frente a salmueras inorganicas y a baja presion.
JPH062682B2 (ja) * 1985-07-18 1994-01-12 日合アセチレン株式会社 アセチレンの精製法およびそれに用いる装置
JPS62285988A (ja) * 1986-06-04 1987-12-11 Nichigou Asechiren Kk 高純度アセチレンガスの提供方法およびそれに用いる精製装置
JPS6446098A (en) * 1987-08-07 1989-02-20 Nichigo Acetylen Method for cleaning inside of container of dissolved acetylene
JP4314015B2 (ja) * 2002-10-31 2009-08-12 ニチゴー日興株式会社 可搬式超高純度アセチレン供給装置

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2004089859A2 *

Also Published As

Publication number Publication date
WO2004089859A2 (fr) 2004-10-21
WO2004089859A3 (fr) 2004-11-25
FR2853313B1 (fr) 2005-05-06
FR2853313A1 (fr) 2004-10-08
JP2011021017A (ja) 2011-02-03
JP2006522079A (ja) 2006-09-28

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