EP0974026B1 - Asbestfreie poröse masse für azetylenbehälter - Google Patents

Asbestfreie poröse masse für azetylenbehälter Download PDF

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Publication number
EP0974026B1
EP0974026B1 EP97921510A EP97921510A EP0974026B1 EP 0974026 B1 EP0974026 B1 EP 0974026B1 EP 97921510 A EP97921510 A EP 97921510A EP 97921510 A EP97921510 A EP 97921510A EP 0974026 B1 EP0974026 B1 EP 0974026B1
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EP
European Patent Office
Prior art keywords
mass
per cent
acetylene
contents
mass per
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.)
Expired - Lifetime
Application number
EP97921510A
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English (en)
French (fr)
Other versions
EP0974026A1 (de
Inventor
Rados Radicevic
Jovan Gojkovic
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"Tehnogas" DD
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"Tehnogas" DD
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Publication of EP0974026A1 publication Critical patent/EP0974026A1/de
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Publication of EP0974026B1 publication Critical patent/EP0974026B1/de
Anticipated expiration legal-status Critical
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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
    • F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
    • F17C11/00—Use of gas-solvents or gas-sorbents in vessels
    • F17C11/002—Use of gas-solvents or gas-sorbents in vessels for acetylene
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
    • C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
    • C10L3/02—Compositions containing acetylene
    • C10L3/04—Absorbing compositions, e.g. solvents

Definitions

  • This invention falls into the technology of materials production scope based on calcium hydrosilicates having the intention to serve as a filler material in the steel vessels, thus enabling a safe storaging, transportation and the consumption of solved acetylene.
  • Acetylene is usually kept in gaseous state solved in some of the solvents such as acetone soaked by a porous mass, in this particular situation the calcium silicate.
  • Asbestos used to be taken for reinforcement of calcium silicates which was added into the mixture of various materials whose basis is calcium oxide, silica and water.
  • Such mixed suspension was introduced into the vessels equipped with special regulation valves, where, under the influence of a raised temperature and pressure in the autoclaves conditions, there came to stiffening of the suspension into a crystalline calcium silicate structure.
  • the stiff mass, together with the steel vessel without a pressure gauge, was then exposed to a raised temperature with the aim of releasing of nearly whole amount of free water quantity, aside from the bound water in crystal structure of calcium silicate.
  • the role of asbestos was, beside reinforcing calcium silicate, to enable a uniform fill-up of the vessel with raw mass, without an increased slackening of the input components in the raw mass.
  • porous mass as a filler material is to uniformly fill the vessel's volume intended for storaging, thus enabling the inlet of the acetylene solvent (mostly acetone or dimethylformamide), as well as the inlet of the gas which is solved in it.
  • This is enabled by exceptionally high porosity of the material provided - the calcium silicate which is characterised by very fine and uniformly distributed pores whose dimensions are up to about 25 ⁇ m, which make an effective contact possible of the gas and solvent as well as a proper filling and discharging of the acetylene vessels.
  • the stiffening and drying processes of the mass is performed in such a way that the distance between the steel vessel's shell and monolithic mass should not exceed 3 mm.
  • the porosity of calcium silicate mass reinforced by means of asbestos fibres amounts to 85 % up to about 92 % in voL
  • calcium silicate mass has the task of preventing a progressive disintegration of acetylene in the vessel, and when it comes to sparkling inside it, caused by the possible dragging in of the back fire from the burner, in the conditions of regular consumption of acetylene in practice.
  • the new product whose basis is the monolithic calcium silicate without asbestos contents, reinforced by uniformly distributed mixture of synthetic fibres on the basis of carbon and glass fibres resistant to alkali, with the addition of boric acid and carboxymethylcellulose, representing a good variant of the filler for the vessels in which the gaseous acetylene solved in the solvent, for example acetone, is safely storaged, kept and transported.
  • Calcium silicate monolithic filler obtained by the new procedure, contains a mixture of crystal phase Tobermorite and Xonotlite, having the porosity 86 - 93 % and the equally distributed fine pores.
  • Calcium silicate monolithic filling without asbestos contains an equally dispersed mixture of glass fibres resistant to alkali and synthetic fibres based on carbon, to which boric acid is added, secure a satisfactory mechanical strength of material, at the same time retaining a high porosity, which obtains optimum characteristics bound to the gas quantity which is possible to be storaged in the vessels, providing a high degree safeness, when used.
  • the biggest importance for the monolithic crystal filling is to be formed in such a way so that the initial components should be homogeneously mixed according to the following mass ratios.
  • carboxymethylcellulose does not exceed 0.5 %. It is added with the aim of preventing of settling of components in the raw mass, before the stiffening phase in autoclave. During baking procedure there occurs to its disintegration - pyrolisys, so favourably affecting the final porosity of the silicate mass.
  • boric acid which favourably affects onto the ratio of obtained crystals phases during autoclaving procedure, which has a positive influence on the shrinkage during baking process.
  • Production of the new calcium silicate filler material together with the raw materials within the said mass ratios is performed the following way.
  • the soft water whose total contents depends on the aimed porosity, approximately in the range of 3 : 1 up to 4 : 1 related to dry substance, is added the CaO in order to obtain, by means of agitating, the Ca(OH) 2 , the lime suspension.
  • Such homogeneous, well agitated suspension of all components is poured into the vessels for keeping the acetylene which are vacuumised at the same time.
  • the suspension must be previously cooled to 20 - 35°C, having in mind it was, in the exothermic process of "slaking" the quick lime, heated up to about 50°C.
  • the suspension is equally distributed in the whole volume of the vessel so as to avoid the possible cavities and bubbles of air in the mass.
  • the decisive part is on the dispersed components of the carboxymethylcellulose solution and the mixture of glass and synthetic fibres based on carbon.
  • the so filled vessel is equipped with a special shutting device having a pressure regulating unit which is screwed onto the vessel opening provided with a valve.
  • the so prepared vessel is exposed to autoclaving process in the furnace with residing temperature from 180 to 220°C.
  • the autoclaving process lasts about 20 to 50 hours, depending on the vessel volume, during which time it comes to the stiffening of suspension into a monolithic mass in the vessel itself
  • the vessel On elapsing the necessary time, the vessel is taken out of the furnace and is left to be completely cooled.
  • the shutting device together with pressure regulator is dismantled from the vessel and the opened vessel with calcium silicate filler material is taken into the furnace where the drying process takes place.
  • the drying process takes as long as nearly the whole quantity of free water is removed out from the calcium silicate mass.
  • the regime of drying process is adjusted so as not to cause an abrupt water evaporation out of the mass itself, which could imply to building up of major cavities and canals within the mass. For that reason, the increase of temperature up to 180°C lasts for 4 hours, and then it is gradually raised to 230 and up to 350°C at which it is maintained to the end of the drying process. Total time of drying process amounts to about 80 hours.
  • Figure 1/1 shows the example of vessel outlook intended for storaging, keeping and transportation of solved acetylene gas, which contains the metal shell with accompanying valve (2), metal support (3), calcium silicate monolithic filling without asbestos contents (4), a bored hole in monolithic mass filled with quartz sand (5), felt (6), steel net (7), and a free space up to 3 mm (8) between the steel cylinder body and the filling.
  • the so prepared mass is poured into the acetylene vessels which are at the same time vacuumized with the purpose of removal of the remained air.
  • the vessels are taken into the furnace where the process of autoclaving is performed at the temperature of 190°C.
  • the obtained calcium silicate filling has the volumetric mass of 255 g/l. Porosity is 91,9 %, and the compression strength is around 240 N/cm 2 .
  • the mass obtained after autoclaving and drying has the porosity 91,2 % and compression strength of 270 N/cm 2 .
  • Volumetric mass is 253 g/l.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Processing Of Solid Wastes (AREA)
  • Aftertreatments Of Artificial And Natural Stones (AREA)
  • Carbon And Carbon Compounds (AREA)

Claims (5)

  1. Poröse, asbestfreie Masse auf Basis von Calciumsilikaten zur Füllung des Inneren von Aufbewahrungsbehältern für Acetylen,
    dadurch gekennzeichnet, dass
    sie aus Kalk, Quarz und Borsäure erhalten wird, bezogen auf die Trockenmasse bis zu zehn Masse-Prozent einer fein dispergierten Mischung von Synthesefasern auf Basis von Kohlenstofffasern mit alkalibeständigen Glasfasern enthält und, falls erforderlich, einen Zusatz von bis zu 0,5 Masse-Prozent Carboxymethylzellulose, wobei die Masse feine, gleichmäßig verteilte Poren und im Wesentlichen keine Aushöhlungen enthält und eine Porosität von zumindest 88 % aufweist.
  2. Poröse, asbestfreie Masse nach Anspruch 1, dadurch gekennzeichnet, dass der Anteil von bis zu zehn Masse-Prozent der Mischung aus Synthesefasern auf Basis von Kohlenstofffasern und alkalibeständigen Glasfasern aus einem Anteil von Synthesefasern auf Basis von Kohlenstoff zwischen 0,5 und 5 Masse-Prozent, bezogen auf die Trockenmasse, besteht, wogegen der Rest auf alkalibeständigen Glasfasern besteht.
  3. Poröse, asbestfreie Masse nach Anspruch 1, dadurch gekennzeichnet, dass der Anteil an Borsäure bis zu drei Masse-Prozent beträgt.
  4. Poröse, asbestfreie Masse nach Anspruch 1, dadurch gekennzeichnet, dass der Anteil an feinen, gleichmäßig verteilten Poren 88 bis 93 Volumen-Prozent beträgt.
  5. Verfahren zur Herstellung einer porösen Masse gemäß den vorgehenden Ansprüchen für Aufbewahrungsbehälter von Azetylen,
    dadurch gekennzeichnet, dass
    eine wässrige Suspension hergestellt wird mit CaO und SiO2 im Verhältnis CaO: SiO2 = 0,8 - 1, dann mit bis zu drei Masse-Prozent Borsäure, bezogen auf die Trockenmasse, mit einer Mischung von bis zehn Masse-Prozent bezogen auf die Trockenmasse aus Synthesefasern auf Basis von Kohlenstofffasern und alkalibeständigen Glasfasern, und, falls erforderlich, mit bis zu 0,5 Masse-Prozent bezogen auf die Trockenmasse Carboxymethylzellulose, wobei die erhaltene Suspension in ein Metallgefäß eingebracht wird, zum Zwecke der Verfestigung in einem Autoklaven bei ca. 190° C behandelt und bei ca. 350° C getrocknet wird, so dass eine monolithische Calciumsilikat-Füllung erhalten wird, welche das Lösungsmittel und Azetylen sicher aufnehmen kann und bei der Verwendung das Gas leicht aus der Lösung freigibt.
EP97921510A 1996-12-26 1997-05-22 Asbestfreie poröse masse für azetylenbehälter Expired - Lifetime EP0974026B1 (de)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
YU69996A YU48898B (sh) 1996-12-26 1996-12-26 Porozna masa bez azbesta namenjena za ispunjavanje unutrašnjosti posuda za lagerovanje acetilena i postupak za njeno dobijanje
YU69996 1996-12-26
YU699966 1996-12-26
PCT/YU1997/000004 WO1998029682A1 (en) 1996-12-26 1997-05-22 Porous mass asbestos free for acetylene vessels

Publications (2)

Publication Number Publication Date
EP0974026A1 EP0974026A1 (de) 2000-01-26
EP0974026B1 true EP0974026B1 (de) 2001-08-16

Family

ID=25551040

Family Applications (1)

Application Number Title Priority Date Filing Date
EP97921510A Expired - Lifetime EP0974026B1 (de) 1996-12-26 1997-05-22 Asbestfreie poröse masse für azetylenbehälter

Country Status (5)

Country Link
EP (1) EP0974026B1 (de)
AT (1) ATE204368T1 (de)
DE (1) DE69706198D1 (de)
WO (1) WO1998029682A1 (de)
YU (1) YU48898B (de)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2904239B1 (fr) 2006-07-26 2008-12-05 Air Liquide Structure de garnissage a phase cristalline de recipients de gaz
FR2904240B1 (fr) 2006-07-26 2008-12-05 Air Liquide Structure de garnissage pour recipient de gaz a materiau cristallise sous forme d'aiguilles
FR2933396B1 (fr) 2008-07-02 2011-07-22 Air Liquide Procede de fabrication d'une structure de garnissage avec controle de l'etape de sechage.
FR2933689B1 (fr) * 2008-07-11 2011-03-18 Air Liquide Structure de garnissage a hautes performances avec jeux lateraux controles
FR2948884B1 (fr) 2009-08-05 2012-06-01 Air Liquide Matiere poreuse ceramique presentant une macroporosite controlee par empilement de porogenes
FR2948936B1 (fr) 2009-08-05 2011-10-28 Air Liquide Matiere poreuse ceramique presentant une architecture de type alveolaire et une macroporosite controlee

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4129450A (en) * 1977-11-09 1978-12-12 Union Carbide Corporation Acetylene vessel filler composition
US4765458A (en) * 1986-10-14 1988-08-23 Ni Industries, Inc. Asbestos free hardened monolithic filler mass
US5697990A (en) * 1995-01-31 1997-12-16 Worthington Acetylene Cylinder, Inc. High porosity calcium silicate mass for storing acetylene gas

Also Published As

Publication number Publication date
YU69996A (sh) 1998-11-05
WO1998029682A1 (en) 1998-07-09
EP0974026A1 (de) 2000-01-26
DE69706198D1 (de) 2001-09-20
YU48898B (sh) 2002-10-18
ATE204368T1 (de) 2001-09-15

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