US3104984A - Containers for liquefied gases - Google Patents

Containers for liquefied gases Download PDF

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Publication number
US3104984A
US3104984A US792759A US79275959A US3104984A US 3104984 A US3104984 A US 3104984A US 792759 A US792759 A US 792759A US 79275959 A US79275959 A US 79275959A US 3104984 A US3104984 A US 3104984A
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composition
coating
parts
curing
containers
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US792759A
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Richard A Reck
Charles S Wilhelmy
Benveniste Jacques
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Conch International Methane Ltd
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Conch International Methane Ltd
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    • 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
    • F17C3/00—Vessels not under pressure
    • F17C3/02—Vessels not under pressure with provision for thermal insulation
    • F17C3/04—Vessels not under pressure with provision for thermal insulation by insulating layers
    • F17C3/06—Vessels not under pressure with provision for thermal insulation by insulating layers on the inner surface, i.e. in contact with the stored fluid
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50—Amines
    • C08G59/5006—Amines aliphatic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • 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
    • F17C2203/00—Vessel construction, in particular walls or details thereof
    • F17C2203/03—Thermal insulations
    • F17C2203/0304—Thermal insulations by solid means
    • F17C2203/0354—Wood
    • 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
    • F17C2203/00—Vessel construction, in particular walls or details thereof
    • F17C2203/06—Materials for walls or layers thereof; Properties or structures of walls or their materials
    • F17C2203/0602—Wall structures; Special features thereof
    • F17C2203/0604—Liners
    • 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
    • F17C2203/00—Vessel construction, in particular walls or details thereof
    • F17C2203/06—Materials for walls or layers thereof; Properties or structures of walls or their materials
    • F17C2203/0602—Wall structures; Special features thereof
    • F17C2203/0607—Coatings
    • 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
    • F17C2203/00—Vessel construction, in particular walls or details thereof
    • F17C2203/06—Materials for walls or layers thereof; Properties or structures of walls or their materials
    • F17C2203/0634—Materials for walls or layers thereof
    • F17C2203/0636—Metals
    • F17C2203/0646—Aluminium
    • 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
    • F17C2203/00—Vessel construction, in particular walls or details thereof
    • F17C2203/06—Materials for walls or layers thereof; Properties or structures of walls or their materials
    • F17C2203/0634—Materials for walls or layers thereof
    • F17C2203/0636—Metals
    • F17C2203/0648—Alloys or compositions of metals
    • 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
    • F17C2203/00—Vessel construction, in particular walls or details thereof
    • F17C2203/06—Materials for walls or layers thereof; Properties or structures of walls or their materials
    • F17C2203/0634—Materials for walls or layers thereof
    • F17C2203/0658—Synthetics
    • F17C2203/0663—Synthetics in form of fibers or filaments
    • F17C2203/0673—Polymers
    • 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
    • F17C2209/00—Vessel construction, in particular methods of manufacturing
    • F17C2209/22—Assembling processes
    • F17C2209/225—Spraying
    • 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
    • F17C2209/00—Vessel construction, in particular methods of manufacturing
    • F17C2209/22—Assembling processes
    • F17C2209/227—Assembling processes by adhesive means
    • 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
    • F17C2209/00—Vessel construction, in particular methods of manufacturing
    • F17C2209/22—Assembling processes
    • F17C2209/228—Assembling processes by screws, bolts or rivets
    • 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
    • F17C2221/00—Handled fluid, in particular type of fluid
    • F17C2221/01—Pure fluids
    • F17C2221/014—Nitrogen
    • 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
    • F17C2221/00—Handled fluid, in particular type of fluid
    • F17C2221/03—Mixtures
    • F17C2221/032—Hydrocarbons
    • F17C2221/033—Methane, e.g. natural gas, CNG, LNG, GNL, GNC, PLNG
    • 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
    • F17C2223/00—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel
    • F17C2223/01—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel characterised by the phase
    • F17C2223/0146—Two-phase
    • F17C2223/0153—Liquefied gas, e.g. LPG, GPL
    • F17C2223/0161—Liquefied gas, e.g. LPG, GPL cryogenic, e.g. LNG, GNL, PLNG
    • 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
    • F17C2223/00—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel
    • F17C2223/03—Handled fluid before transfer, i.e. state of fluid when stored in the vessel or before transfer from the vessel characterised by the pressure level
    • F17C2223/033—Small pressure, e.g. for liquefied gas

Definitions

  • balsa wood In attempting to solve the problem, containers have been built which have an inner lining of laminated balsa wood.
  • the balsa wood is strong enough to provide structural strength and is light in weight, but there is the disadvantage that the liquids soak into the wood.
  • linings such as balsa wood which are coated with special compositions.
  • the special compositions utilized in this invention involve certain epoxy resins in combination with certain llers and bonding agents which are catalyzed with a curing agent. These compositions when applied to the balsa wood or other such lining material are converted to a substantially solid coating which is found to be resistant to the very low temperatures involved and also substantially impermeable to the liquefied gases.
  • the coating is utilized in a thickness of about 1A; inch, although other thicknesses may be employed satisfactorily.
  • the epoxy resin is combined with certain fillers and binders.
  • these lillers and binders may be aluminum ⁇ oxide (alumina) and asbestos.
  • this coating composition can also be employed as an adhesive in laminating the strips of insulating material making up the lining.
  • HG. l is a perspective View of one embodiment of the present invention showing a container having a removable top section or cover, and
  • FG. 2 is a cross-sectional view showing the specialcoating composition used as an adhesive between the laminations of the container hner.
  • Section A designates generally the bottom part of the container and the letter B designates generally the cover or lid for the container.
  • Section A is provided with a shell ⁇ or outer supporting framework 12 made up of upper horizontal members 13 and 14, lower horizontal members 15 and 16, and vertical members 17, 18, 19 and 20. The horizontal and vertical supporting members are held together by screw bolts 21.
  • Patented Sept. 24, 1963 ICC Disposed within the framework 12, are pieces of insulating material 22 of varying Width but of substantially the same thickness.
  • the pieces of insulating material 22 can be laminated together by means of an adhesive 23, shown in FIG. 2, preferably the coating composition of the present invention.
  • the cavity 25, into which the liquid gas is placed, is lined on all sides 26 and the bottom (not shown) with the coating composition of the present invention.
  • the cover B of the container, is provided with a plug 30 formed from the coating composition of the present invention.
  • the dimensions of plug 30 are such that it will completely cover the opening to cavity 25 and prevent the escape of the liquid gas stored in the cavity.
  • Cover B is also provided with parallel grooves 31 and 32. The dimensions of these grooves are such that when cover B is placed ⁇ on bottom section A of the container so that surfaces 33 and 134 are in contact with each other, upper horizontal supporting members 13 and 14 will 4lill the space left by grooves 3'1 and 32, respectively.
  • balsa wood 22 in constructing the container of the present invention, pieces of balsa wood 22 of varying width but of substantially the same thickness were employed. These pieces of balsa wood are cut to the desired lengths and laminated together to form the bottom section A of the container and the cover or lid B. If desired, the pieces 22 may be so arranged that succeeding layers ⁇ are at right angles to each other for increased strength and rigidity. This type of construction is shown in lower section 24 of the container and also in cover A.
  • the pieces of insulating material 22, preferably balsa wood, can be laminated together by an adhesive 23 shown in FIG. 2, preferably the special coating composition of the present invention. No clamping of the pieces is required, since the application of a small amount of hand pressure ⁇ such as to reduce the thickness of the adhesive layer 23 to about l/l inch is su'icient to obtain a strong bond.
  • the bottom section A is provided with -a suitable framework 12.
  • the purpose of this framework is to provide additional support and rigidity to the container.
  • Various materials may be employed in the construction of the framework such as Wood, steel or like materials.
  • the vertical and horizontal members may be bolted together by means of screw bolts 21 or welded together if steel stock is used.
  • the cavity 25, into which the liquid gas is placed is ready to be lined on all sides and bottom with the special coating composition of the present invention.
  • This coating composition is produced through the combination of an epoxy resin with aluminum oxide, asbestos, and a curing agent capable of converting lthe resin, aluminum oxide, and asbestos into a hard, thermoset solid.
  • this special coating composition 45 to 53 parts of an epoxy resin having a viscosity of from to 195 poises at 25 C., and an epoxide equivalent of from to 205 (grams of resin containing 1 gram-equivalent of epoxide) is combined with 7 to 10 pants aluminum oxide, 35 to 45 par-ts of asbestos, and from 3 to 4.5 parts of a curing agent for converting the thermoplastic epoxy resins into a hard, thermoset composition.
  • Two types of materials are generally employed as curing agents, [these materials are amines and acid anhydrides. Examples of amines which can be used are diethylenetriamine, triethylenetetramine, and diethylaminopropylamine. Acid anhydrides such as phthalic anhydride and dodecenylsuccinic anhydride may also be employed.
  • the fillers for example, aluminum oxide and asbestos are mixed together being careful that the aluminum oxide is well dispersed in the asbestos fiber. Then thecatalyst or curing agent is added to the epoxy resin and welldispersed therein. Thereafter the fillers and the Iresin containing the curing Iagent are introduced into a mixer and thoroughly agitated together. After thorough mixing has taken place, the composition is ready to be applied to a surface or to an article.
  • the cavity 25 is lined on all sides.
  • the bottom is also lined (not shown).
  • This composition may be suitably ftroweled or sprayed on the insulating material to a thickness of about Ms inch. If it is desired that the composition be applied by means of a spray, it is preferred that successive coats -or layers of the composition be applied, allowing time between applications for the layers to harden.
  • the plug 30 is likewise formed from Ithe coating composition of .the present invention.
  • the coating composition may be applied directly to surface 33 so that the outer dimensions of the plug are such that it will completely seal fthe opening to cavity 25. It is preferred that the thickness of plug 30 be greater than the lining of cavity 2S to insure that the plug ts Well down into vthe cavity. A plug thickness of .about 1/2 inch has proven to be very satisfactory.
  • EXAMPLE I Aluminum oxide and asbestos tiber were thoroughly mixed, making certain that the aluminum oxide was thoroughly dispersed in the asbestos, and then set aside 'to .await the mixing of the resin and curing agent.
  • An epoxy resin (Epon 828, Shell Chemical Corporation) (epichlorohydrin/ bisphenol A-type, a glycidyl polyether of dihydric alcohol) having a viscosity of from 135 to 195 poises at 25 C. and an epoxide equivalent of from 185 to 205 was Well dispersed with diethylaminopropylamine. Thereafter the mixture of alumina and asbestos was added slowly to -the resin mixture, taking care to insure thorough mixing in au internal type mixer.
  • Balsa wood specimens of 1 x 1 x 2 inch dimension were coated on all sides tto a thickness of l/s" and cured one hour at 200 F.
  • the coated specimens were then immersed into liquid nitrogen for 24 hours (-325 F.) and inspected for cracks and permeability. Coatings that developed cracks, checks or that proved to be permeable to the liquid gas were rejected.
  • the following compositions (in parts by weight) exhibited no surface cracks or flaws.
  • EXAMPLE III Tests were conducted to determine the suitability of replacing the alumina and asbestos fillers with other fillers such as wood ilour and finely ground leather.
  • four parts of the epoxy resin (Epon 828) and one part Wood flour were intimately mixed.
  • Diethylaminopropylamine catalyst was added to the epoxy in the amount of 1.25 parts before the addition of the filler.
  • Example No. 1 was rejected due to excessive expansion of the coating probably caused by gas formation.
  • specimens 2 and 3 were left standing at room temperature for 72 hours. The coatings did not harden, whereupon the specimens were cured for one and one-half hours at 200 F. in an air circulating oven. The coatings displayed tackiness, but developed no foamy swelling. An additional cure of one hour at 250 F. did not eliminate the tackiness.
  • Samples 2 and 3 were also subjected to a 250 F./1 hour cure without room temperature cure. There was no swelling but the cure was incomplete as evidenced by tackiness and softness at the surface of the coatings.
  • Sample No. 4 was prepared to determine Whether lthe inclusion of Igepal 630, a non-ionic wetting agent, would facilitate the mixing and application of the composition. These conditions were slightly improved. However, no foamy swelling developed.
  • Sample No. 5 was prepared to determine the eifect of a comparatively large amount (11% on the basis of epoxy resin) of catalyst. Application of the coating was somewhat easier. In compounding, the epoxy resin and ground leather were roller milled andthe catalyst was added subsequently. Specimens required a longer curing cycle, 2 hours at 200 F. No foamy swelling developed. Two specimens of specimen No. 5 were immersed inV liquid nitrogen for 24 hours. They developed cracks and the specimens were rejected.
  • the method of producing a lining on the surface of a porous thermal insulating layer adapted to retain a liquid at low temperature When in surface contact therewith comprising coat-ing the surface with a coating composition formed of 45 to 53 parts by weight of an epoxy resin in the form of a glycidyl polyether of dihydric phenol, and a mixture of 7 to 10 parts by Weight of aluminum oxide and 35 to 45 parts by Weight of asbestos and a curing agent capable of converting the composition to a solid, and curing the coating at a temperature of 20 to 260 C.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Polymers & Plastics (AREA)
  • Medicinal Chemistry (AREA)
  • Health & Medical Sciences (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
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Description

Sept' 24, 1933 R. A. REcK ETAL 3,104,984
CONTAINERS FOR LIQUEFIED GASES Filed Feb. l2, 1959 E? mcg@ United States Patent O 3,104,984 CNTAINERS FOR LlQUEFEB GASES Richard A. Reck and Charles S. Wiihelmy, Chicago, El., and Jacques Benveniste, Union, NJ., assigner-s, by rnesne msignments, to Coach International Methane Limited, a Bahama corporation Filed Feb. 12, 1959, Ser. No. 792,759 4 Claims. (Cl. 117-148) The present invention relates to containers for liquefied gases such as liquid nitrogen `or liquid methane and deals especially with such containers having special linings which adapt the containers for use in connection with liquefied gases. The invention deals also with special coating compositions useful in this connection.
Since many of these gases must be stored and transported at low temperatures such as m250" C., the conventional gas storage tanks which are made of steel or other metals are not satisfactory. At these low temperatures the metal tanks become brittle and tend to crack, and the excessive expansion and contraction is also troublesome.
In attempting to solve the problem, containers have been built which have an inner lining of laminated balsa wood. The balsa wood is strong enough to provide structural strength and is light in weight, but there is the disadvantage that the liquids soak into the wood.
Applicants have discovered that satisfactory containers can be provided by using linings such as balsa wood which are coated with special compositions. The special compositions utilized in this invention involve certain epoxy resins in combination with certain llers and bonding agents which are catalyzed with a curing agent. These compositions when applied to the balsa wood or other such lining material are converted to a substantially solid coating which is found to be resistant to the very low temperatures involved and also substantially impermeable to the liquefied gases. Preferably the coating is utilized in a thickness of about 1A; inch, although other thicknesses may be employed satisfactorily.
In preparing the coating composition the epoxy resin is combined with certain fillers and binders. These lillers and binders may be aluminum `oxide (alumina) and asbestos. We have further discovered that this coating composition can also be employed as an adhesive in laminating the strips of insulating material making up the lining.
It is an object of the present invention to provide a container for the storage and transportation of low temperature iluids, the container hav-ing an outer structure which provides strength to the container and an inner insulating liner which is coated to make it resistant to the low temperatures and also impermeable to the iluids.
It is another object of the present invention to provide a coating composition especially suited for the construction of containers for liquefied gases.
In the accompanying drawings HG. l is a perspective View of one embodiment of the present invention showing a container having a removable top section or cover, and
FG. 2 is a cross-sectional view showing the specialcoating composition used as an adhesive between the laminations of the container hner.
Invthe drawings, the letter A designates generally the bottom part of the container and the letter B designates generally the cover or lid for the container. Section A is provided with a shell `or outer supporting framework 12 made up of upper horizontal members 13 and 14, lower horizontal members 15 and 16, and vertical members 17, 18, 19 and 20. The horizontal and vertical supporting members are held together by screw bolts 21.
Patented Sept. 24, 1963 ICC Disposed within the framework 12, are pieces of insulating material 22 of varying Width but of substantially the same thickness. The pieces of insulating material 22 can be laminated together by means of an adhesive 23, shown in FIG. 2, preferably the coating composition of the present invention.
The cavity 25, into which the liquid gas is placed, is lined on all sides 26 and the bottom (not shown) with the coating composition of the present invention.
The cover B, of the container, is provided with a plug 30 formed from the coating composition of the present invention. The dimensions of plug 30 are such that it will completely cover the opening to cavity 25 and prevent the escape of the liquid gas stored in the cavity. Cover B is also provided with parallel grooves 31 and 32. The dimensions of these grooves are such that when cover B is placed `on bottom section A of the container so that surfaces 33 and 134 are in contact with each other, upper horizontal supporting members 13 and 14 will 4lill the space left by grooves 3'1 and 32, respectively.
in constructing the container of the present invention, pieces of balsa wood 22 of varying width but of substantially the same thickness were employed. These pieces of balsa wood are cut to the desired lengths and laminated together to form the bottom section A of the container and the cover or lid B. If desired, the pieces 22 may be so arranged that succeeding layers `are at right angles to each other for increased strength and rigidity. This type of construction is shown in lower section 24 of the container and also in cover A.
The pieces of insulating material 22, preferably balsa wood, can be laminated together by an adhesive 23 shown in FIG. 2, preferably the special coating composition of the present invention. No clamping of the pieces is required, since the application of a small amount of hand pressure `such as to reduce the thickness of the adhesive layer 23 to about l/l inch is su'icient to obtain a strong bond.
Having constructed the bottom section A and cover B from laminated pieces of insulating material, .the bottom section A is provided with -a suitable framework 12. The purpose of this framework is to provide additional support and rigidity to the container. Various materials may be employed in the construction of the framework such as Wood, steel or like materials. The vertical and horizontal members may be bolted together by means of screw bolts 21 or welded together if steel stock is used.
After the construction of sections A and B, the cavity 25, into which the liquid gas is placed, is ready to be lined on all sides and bottom with the special coating composition of the present invention. This coating composition is produced through the combination of an epoxy resin with aluminum oxide, asbestos, and a curing agent capable of converting lthe resin, aluminum oxide, and asbestos into a hard, thermoset solid.
ln preparing this special coating composition, 45 to 53 parts of an epoxy resin having a viscosity of from to 195 poises at 25 C., and an epoxide equivalent of from to 205 (grams of resin containing 1 gram-equivalent of epoxide) is combined with 7 to 10 pants aluminum oxide, 35 to 45 par-ts of asbestos, and from 3 to 4.5 parts of a curing agent for converting the thermoplastic epoxy resins into a hard, thermoset composition. Two types of materials are generally employed as curing agents, [these materials are amines and acid anhydrides. Examples of amines which can be used are diethylenetriamine, triethylenetetramine, and diethylaminopropylamine. Acid anhydrides such as phthalic anhydride and dodecenylsuccinic anhydride may also be employed.
Best results are obtained when the fillers, for example, aluminum oxide and asbestos are mixed together being careful that the aluminum oxide is well dispersed in the asbestos fiber. Then thecatalyst or curing agent is added to the epoxy resin and welldispersed therein. Thereafter the fillers and the Iresin containing the curing Iagent are introduced into a mixer and thoroughly agitated together. After thorough mixing has taken place, the composition is ready to be applied to a surface or to an article.
The cavity 25 is lined on all sides. The bottom is also lined (not shown). This composition may be suitably ftroweled or sprayed on the insulating material to a thickness of about Ms inch. If it is desired that the composition be applied by means of a spray, it is preferred that successive coats -or layers of the composition be applied, allowing time between applications for the layers to harden.
After the resinous coating composition has been applied, it is necessary to allow the composition to cure or to harden into a solid coating. Curing will take place at room temperature and up to 260 C. As has been previously pointed out, a whole range .of curing agents can be utilized. Diethylaminopropylamine works very well as a curing agent at a temperature of about 93 C. When using diethylaminopropylamine, as a catalyst, a curing time of about 1 hour at 93 C. has proved to be satisfactory. A curing time of from 24 to 48 hours is necessary when the composition is cured at room temperature.
The plug 30 is likewise formed from Ithe coating composition of .the present invention. The coating composition may be applied directly to surface 33 so that the outer dimensions of the plug are such that it will completely seal fthe opening to cavity 25. It is preferred that the thickness of plug 30 be greater than the lining of cavity 2S to insure that the plug ts Well down into vthe cavity. A plug thickness of .about 1/2 inch has proven to be very satisfactory.
The invention may be further illustrated by the following specic examples:
EXAMPLE I Aluminum oxide and asbestos tiber were thoroughly mixed, making certain that the aluminum oxide was thoroughly dispersed in the asbestos, and then set aside 'to .await the mixing of the resin and curing agent.
An epoxy resin (Epon 828, Shell Chemical Corporation) (epichlorohydrin/ bisphenol A-type, a glycidyl polyether of dihydric alcohol) having a viscosity of from 135 to 195 poises at 25 C. and an epoxide equivalent of from 185 to 205 was Well dispersed with diethylaminopropylamine. Thereafter the mixture of alumina and asbestos was added slowly to -the resin mixture, taking care to insure thorough mixing in au internal type mixer.
Balsa wood specimens of 1 x 1 x 2 inch dimension were coated on all sides tto a thickness of l/s" and cured one hour at 200 F. The coated specimens were then immersed into liquid nitrogen for 24 hours (-325 F.) and inspected for cracks and permeability. Coatings that developed cracks, checks or that proved to be permeable to the liquid gas were rejected. The following compositions (in parts by weight) exhibited no surface cracks or flaws.
Y 1 Epen 828 (Shell Chemical Corporation).
2 Dlethylaminopropylamine. All figures represent parts by Weight.
EXAMPLE II Inorder to test the suitability of the formulations set forth in Table I as adhesives to be used in laminating aroaese together pieces of insulating material, live samples were prepared of each of the tive formulations set forth in Table I. Laminates were prepared from pieces l x 1 x 2 inches and squeezed together with a layer of adhesive between them. No clamps were necessary. After curing one hour at 200 F., the laminated pieces were immersed in liquid nitrogen for 24 hours at 325 F. After the 24 hour period, the samples were removed and examined. The bond strength was such that delamination would not occur at the wood adhesive interface.
In the same manner, the preparation of one square foot panels, one inch thick, entailed no necessity of clamping the boards together, except for the application of a small amount of hand pressure such as to reduce the thickness of the adhesive layer to about G inch.
EXAMPLE III Tests were conducted to determine the suitability of replacing the alumina and asbestos fillers with other fillers such as wood ilour and finely ground leather. In this test, four parts of the epoxy resin (Epon 828) and one part Wood flour were intimately mixed. Diethylaminopropylamine catalyst was added to the epoxy in the amount of 1.25 parts before the addition of the filler.
Small balsa wood specimens (l x 1 x 2 inches) were prepared, coated with the above composition, cured for one hour at 200 F., and the specimens immersed in liquid nitrogen for 24 hours. All of the samples were rejected due to excessive expansion of the coating caused by gas formation. No cracks were apparent due to cooling.
The use of finely ground leather as a filler in the above formulation Was investigated. The following formulations Were used:
1 See Table I, footnote (l).
`Sample No. 1 was rejected due to excessive expansion of the coating probably caused by gas formation. In order to determine whether a slower curing cycle would eliminate the gas formation, specimens 2 and 3 were left standing at room temperature for 72 hours. The coatings did not harden, whereupon the specimens were cured for one and one-half hours at 200 F. in an air circulating oven. The coatings displayed tackiness, but developed no foamy swelling. An additional cure of one hour at 250 F. did not eliminate the tackiness.
Samples 2 and 3 were also subjected to a 250 F./1 hour cure without room temperature cure. There was no swelling but the cure was incomplete as evidenced by tackiness and softness at the surface of the coatings.
Sample No. 4 was prepared to determine Whether lthe inclusion of Igepal 630, a non-ionic wetting agent, Would facilitate the mixing and application of the composition. These conditions were slightly improved. However, no foamy swelling developed.
Sample No. 5 was prepared to determine the eifect of a comparatively large amount (11% on the basis of epoxy resin) of catalyst. Application of the coating was somewhat easier. In compounding, the epoxy resin and ground leather were roller milled andthe catalyst was added subsequently. Specimens required a longer curing cycle, 2 hours at 200 F. No foamy swelling developed. Two specimens of specimen No. 5 were immersed inV liquid nitrogen for 24 hours. They developed cracks and the specimens were rejected.
The foregoing detailed description has been given for clearness of understanding only and no unnecessary limitations are to be inferred therefrom.
We claim:
1. The method of producing a lining on the surface of a porous thermal insulating layer adapted to retain a liquid at low temperature When in surface contact therewith comprising coat-ing the surface with a coating composition formed of 45 to 53 parts by weight of an epoxy resin in the form of a glycidyl polyether of dihydric phenol, and a mixture of 7 to 10 parts by Weight of aluminum oxide and 35 to 45 parts by Weight of asbestos and a curing agent capable of converting the composition to a solid, and curing the coating at a temperature of 20 to 260 C.
2. The method as claimed in claim 1 in Which the porous thermal insulating layer comprises balsa Wood.
3. The method as claimed in claim 1 in which the 5 curing agent is present in an amount within 4the range of 3.0 to 4.5 percent by weight.
4. The method of claim 1, wherein the curing agent is diethyl amino propylamine.
References Cited in the le of this patent UNITED STATES PATENTS 97,390 Goddard Nov. 30, 1869 2,494,920 Warrick Jan. 17, 1950 2,570,958 Lee Oct. 9, 1951 2,682,515 Naps June 29, 1954 2,895,936 Archer et al. July 21, 1959 2,934,452 Sternberg Apr. 26, 1960 2,943,953 Daniel July 5, 1960 FOREIGN PATENTS 516,107 Canada Aug. 30, 1955

Claims (1)

1. THE METHOD OF PRODUCING A LINING ON THE SURFACE OF A POROUS THERMAL INSULATING LAYER ADAPTED TO RETAIN A LIQUID AT LOW TEMPERATURE WHEN IN SURFACE CONTACT THEREWITH COMPRISING COATING THE SURFACE WITH A COOATING COMPOSITION FORMED OF 45 TO 53 PARTS BY WEIGHT OF AN EPOXY RESIN IN THE FORM OF A GLYCIDYL POLYETHER OF DIHYDRIC PHENOL, AND A MIXTURE OF 7 TO 10 PARTS BY WEIGHT OF ALUMINUM OXIDE AND 35 TO 45 PARTS BY WEIGHT OF ASBESTOS AND A CURING AGENT CAPABLE OF CONVERTING THE COMPOSITION TO A SOLID, AND CURING THE COATING AT A TEMPERATURE OF 20* TO 260*C.
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US2494920A (en) * 1945-07-25 1950-01-17 Corning Glass Works Method of coating with organopolysiloxanes
US2570958A (en) * 1948-09-18 1951-10-09 Francis E Lee Lined drawer
US2682515A (en) * 1952-07-05 1954-06-29 Shell Dev Adhesive composition containing polyepoxide materials
CA516107A (en) * 1955-08-30 General Mills Polyamide-epoxy resin reaction product
US2895936A (en) * 1956-12-20 1959-07-21 Dow Chemical Co Resinous compositions from coal acids and polyfunctional amines and method for making composite products thereof
US2934452A (en) * 1956-12-14 1960-04-26 Steelcote Mfg Company Resurfaced concrete structure
US2943953A (en) * 1957-07-05 1960-07-05 Frederick K Daniel Flooring composition and method of making the same

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US97390A (en) * 1869-11-30 Improved moss of cohstrttcting- water-pitchers and other vessels
CA516107A (en) * 1955-08-30 General Mills Polyamide-epoxy resin reaction product
US2494920A (en) * 1945-07-25 1950-01-17 Corning Glass Works Method of coating with organopolysiloxanes
US2570958A (en) * 1948-09-18 1951-10-09 Francis E Lee Lined drawer
US2682515A (en) * 1952-07-05 1954-06-29 Shell Dev Adhesive composition containing polyepoxide materials
US2934452A (en) * 1956-12-14 1960-04-26 Steelcote Mfg Company Resurfaced concrete structure
US2895936A (en) * 1956-12-20 1959-07-21 Dow Chemical Co Resinous compositions from coal acids and polyfunctional amines and method for making composite products thereof
US2943953A (en) * 1957-07-05 1960-07-05 Frederick K Daniel Flooring composition and method of making the same

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014144347A1 (en) * 2013-03-15 2014-09-18 Interface Solutions, Inc. Insulating container and methods of making an insulating container
US8955708B2 (en) 2013-03-15 2015-02-17 Interface Solutions, Inc. Insulating container and methods of making an insulating container

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