USH943H - Organic liner for thermoset composite tank - Google Patents

Organic liner for thermoset composite tank Download PDF

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Publication number
USH943H
USH943H US07/449,175 US44917589A USH943H US H943 H USH943 H US H943H US 44917589 A US44917589 A US 44917589A US H943 H USH943 H US H943H
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sup
astm
layer
thick
shell
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US07/449,175
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Raymond E. Garvey
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US Department of Energy
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US Department of Energy
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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
    • F17C3/00—Vessels not under pressure
    • F17C3/12—Vessels not under pressure with provision for protection against corrosion, e.g. due to gaseous acid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
    • B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
    • B65D90/00—Component parts, details or accessories for large containers
    • B65D90/02—Wall construction
    • B65D90/04—Linings
    • B65D90/046—Flexible liners, e.g. loosely positioned in the container
    • 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
    • F17C2203/0658—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
    • 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
    • F17C2203/0675—Synthetics with details of composition
    • 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

Definitions

  • This invention relates to a coating for sealing surfaces having complex geometry, particularly to a coating of epoxy layers that forms a surface impermeable in harsh cryogenic and chemically corrosive environments.
  • cryotanks that were impervious to deterioration caused by the contained material and environmental factors.
  • One is a metal lined tank with the metal usually in the form of a foil.
  • the other is an organically coated tank where the coating is a film. Both the foil and the film are theoretically impermeable; however, the bond to the substrate and the integrity of the final surface have proven to be unsatisfactory in both applications.
  • Cryotanks are generally fabricated from composites of either graphite fiber reinforced fiberglass or a glass reinforced polymer matrix. These tanks have been lined with either the metal foils or organic films. Metal coatings have also been utilized but the coating process, usually some form of deposition, has resulted in a porous surface that does not satisfactorily bond to the substrate.
  • the article of manufacture of this invention may comprise a tank configuration of suitable material to withstand cryogenic conditions.
  • the interior of the tank is lined with consecutive layers of organic coatings.
  • the first layer is of minimum thickness to establish a continuous coating for bonding; the next layer is of suitable thickness to establish bonding reliability; the next layer is of suitable thickness to insure molecular impermeability; the next layer is of suitable thickness to guarantee integrity at cryogenic temperatures; the final layer is of suitable thickness to insure a smooth defect-free surface.
  • the coating is an epoxy.
  • the first layer is from about 0.0001 to 0.001 in. thick; the second layer is also about 0.0001 to 0.001 in. thick.
  • the third layer is about 0.001 to 0.010 in. thick and so is the forth layer.
  • the final layer is from about 0.0001 to 0.001 in. thick.
  • the invention is an improvement over past line cryotanks since the integrity of the lining has a longer life under cryogenic conditions than prior art methods.
  • the invention relates generally to a leak-proof seal for structural composites in extremely harsh cryogenic and chemically corrosive environments.
  • Such seals have particular applicability for sealing surfaces having complex geometry as may be encountered on hypervelocity transport vehicles.
  • the method of the invention comprises the application, successively, of layers of epoxy resin formulations. First, two very thin layers, from about 0.0001 to 0.001 in. thick, are applied. This is followed by two thicker layers, about 0.001 to 0.010 in. thick. A final layer, from about 0.0001 to 0.001 in. thick, is added for a smooth defect-free surface.
  • the thin and thick epoxy resin formulations are each comprised of an A-component and a B-component.
  • the application of each layer is followed by a curing step.
  • a thin A-component composition is shown is Table 1, with thin A-component properties given in Table 2.
  • the ingredients and solvents of thin B-component are shown in Table 3.
  • Thin B-component properties are given in Table 4.
  • the amido-amine and diethylenetriamine are mixed at room temperature until homogeneous.
  • the epoxy resin solution EPON 1001CX 75
  • the epoxy resin solution is preheated to 75° C. ⁇ 5°, then gradually added to the amido amine diethylenetriamine mixture. Constant stirring is provided during the addition to provide for a complete reaction, while the temperature is maintained at 52° C. ⁇ 3°. Mixing is discontinued when the brown solution becomes clear, after which the reaction mixture is allowed to cool to 37° C. ⁇ 3°.
  • the solvent mixture (Table 4) is added slowly with constant stirring until the solution is homogeneous and meets non-volatile requirements.
  • the thin coating is applied to the interior of a cryotank made of fiberglass reinforced with graphite fiber or of a polymer matrix reinforced with glass fiber.
  • Application can be made with a dry lint-free and oil-free cloth or with a Teflon applicator such as a paddle, scraper or roller.
  • the thin layers are allowed to dry for 30 minutes after which they are cured at 230° F. ⁇ 5° for 2 hours.
  • the combined components must be used within 8 hours of mixing and should be stored, if necessary, in a closed container at room temperature.
  • a thick A-component is shown in Table 5 with thick A-component properties given in Table 6.
  • the ingredient and solvents of thick B-component are shown in Table 7.
  • Thick B-component properties are given in Table 8.
  • the thick A+B composition comprises a 50:50 mixture ( ⁇ 1%) of the two solutions.
  • the combined mixture has a maximum work life of 12 minutes at 75° F. ⁇ 10° and must, therefore, be quickly applied using a dry lint-free and oil-free cloth or with a Teflon applicator such as a paddle, scraper or roller.
  • the applied thick layers are cured at 150° F. for about 90 minutes, or at 165° F. for 60 minutes, or at 205° F. for at least 45 minutes. It is not recommended that the article be subjected to a temperature of more than 215° F. until curing is completed.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Laminated Bodies (AREA)

Abstract

A cryogenic tank that is made leak-proof under cryogenic conditions by successive layers of epoxy lining the interior of the tank.

Description

This invention was developed pursuant to a contract with the U.S. Department of Energy.
This invention relates to a coating for sealing surfaces having complex geometry, particularly to a coating of epoxy layers that forms a surface impermeable in harsh cryogenic and chemically corrosive environments.
BACKGROUND OF THE INVENTION
Previously, scientists have followed two approaches in the development of cryotanks that were impervious to deterioration caused by the contained material and environmental factors. One is a metal lined tank with the metal usually in the form of a foil. The other is an organically coated tank where the coating is a film. Both the foil and the film are theoretically impermeable; however, the bond to the substrate and the integrity of the final surface have proven to be unsatisfactory in both applications.
Cryotanks are generally fabricated from composites of either graphite fiber reinforced fiberglass or a glass reinforced polymer matrix. These tanks have been lined with either the metal foils or organic films. Metal coatings have also been utilized but the coating process, usually some form of deposition, has resulted in a porous surface that does not satisfactorily bond to the substrate.
In the case of metal foils, application is suitable for cone, cylinder or flat surface geometry; however the surfaces that need to be covered are not limited to these configurations making foils an unsuitable approach. With organic coatings, as with foils, the adhesion between the liner and the tank has not been satisfactory when exposed to cryotank temperatures. Therefore, there is a need to develop a containment tank that is impermeable to liquids and gases in harsh cryogenic and chemically corrosive environments.
SUMMARY OF THE INVENTION
In view of the above needs, it is an object of this invention to provide a cryotank that is impermeable to molecular intrusion at fluctuating temperatures.
It is another object of this invention to provide a molecularly impermeable coating that can adhere to a surface and maintain integrity at cryogenic temperatures.
It is another object of this invention to provide a molecularly impermeable coating that can adhere to a surface of irregular configuration.
Additional objects, advantages and novel features of the invention will be set forth in part in the description which follows, and in part will become apparent to those skilled in the art upon examination of the following or may be learned by practice of the invention. The objects and advantages of the invention may be realized and attained by means of the instrumentalities and combinations particularly pointed out in the appended claims.
To achieve the foregoing and other objects and in accordance with the purpose of the present invention, as embodied and broadly described herein, the article of manufacture of this invention may comprise a tank configuration of suitable material to withstand cryogenic conditions. The interior of the tank is lined with consecutive layers of organic coatings. The first layer is of minimum thickness to establish a continuous coating for bonding; the next layer is of suitable thickness to establish bonding reliability; the next layer is of suitable thickness to insure molecular impermeability; the next layer is of suitable thickness to guarantee integrity at cryogenic temperatures; the final layer is of suitable thickness to insure a smooth defect-free surface. In the preferred embodiment the coating is an epoxy. The first layer is from about 0.0001 to 0.001 in. thick; the second layer is also about 0.0001 to 0.001 in. thick. The third layer is about 0.001 to 0.010 in. thick and so is the forth layer. The final layer is from about 0.0001 to 0.001 in. thick.
The invention is an improvement over past line cryotanks since the integrity of the lining has a longer life under cryogenic conditions than prior art methods.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENT
The invention relates generally to a leak-proof seal for structural composites in extremely harsh cryogenic and chemically corrosive environments. Such seals have particular applicability for sealing surfaces having complex geometry as may be encountered on hypervelocity transport vehicles.
The method of the invention comprises the application, successively, of layers of epoxy resin formulations. First, two very thin layers, from about 0.0001 to 0.001 in. thick, are applied. This is followed by two thicker layers, about 0.001 to 0.010 in. thick. A final layer, from about 0.0001 to 0.001 in. thick, is added for a smooth defect-free surface.
EXAMPLE
In the preferred embodiment, the thin and thick epoxy resin formulations are each comprised of an A-component and a B-component. The application of each layer is followed by a curing step. A thin A-component composition is shown is Table 1, with thin A-component properties given in Table 2. The ingredients and solvents of thin B-component are shown in Table 3. Thin B-component properties are given in Table 4.
              TABLE 1                                                     
______________________________________                                    
THIN A-COMPONENT COMPOSITION                                              
                         Percent by Wt                                    
Ingredient               (±0.010%)                                     
______________________________________                                    
Epon 1002 or 1002F.sup.1 54.9                                             
Dye, Oil Red PD15344.sup.2                                                
                         0.20                                             
Isopropyl Alcohol (ASTM D770)                                             
                         1.30                                             
Xylene (ASTM D846)       2.80                                             
Methyl Isobutyl Ketone (ASTM D1153)                                       
                         5.60                                             
Cyclohexanone, Tech. Grade                                                
                         2.60                                             
Methyl Ethyl Ketone (ASTM D740)                                           
                         8.20                                             
Normal Butyl Alcohol (ASTM D304)                                          
                         2.60                                             
1-Methoxy-2-Propanol     Remainder                                        
______________________________________                                    
 .sup.1 Shell Chemical Co., Polymer Division #1 Shell Plaza, Houston, Texa
 77002                                                                    
 .sup.2 Eaton Chemical Division, Western Eaton Solvents & Chemical Co.,   
 13395 Huron Dr., Romulus, Michigan, 48174                                

              TABLE 2                                                     
______________________________________                                    
THIN A-COMPONENT PROPERTIES                                               
Property       Requirement                                                
                          Method                                          
______________________________________                                    
Color          Red        Visual                                          
Specific gravity at 25° C.                                         
               1.03-1.05  ASTM D1963                                      
Resin Wt/Epoxide Equiv-                                                   
               600-730    Dry 5-10 ml sample at                           
alent (gm/eq)             65° C.; D1652; crst.                     
                          vio. indicator                                  
Viscosity Seconds                                                         
               25-40      ASTM D3794                                      
                          Zahn-Cup No. 3                                  
Solids, percent                                                           
               54-56      ASTM D1944                                      
Clarity        Clear      ASTM D2090                                      
______________________________________                                    

              TABLE 3                                                     
______________________________________                                    
 THIN B-COMPONENT COMPOSITION                                             
______________________________________                                    
Ingredient      Percent by Wt (±0.05%)                                 
______________________________________                                    
Diethylenetriamine                                                        
                1.43 AEW = 34.4 to 37.0 g/eq                              
                Sp Grav = 0.945-0.955                                     
Amido-Amine     3.53 Celanese, #1 Riverfront Plaza                        
(Epi-Cure 855)  Louisville, KY 40202                                      
Epoxy Resin Solution                                                      
                3.25 Shell, #1 Shell Plaza                                
(Epon 1001 CX 75)                                                         
                Houston, TX 77002                                         
Solvent Mixture Remainder (See Below)                                     
______________________________________                                    
Solvent         Weight percent (±0.8%)                                 
______________________________________                                    
Toluene (ASTM D362)                                                       
                5.24                                                      
1-Methoxy-2-Propanol                                                      
                51.38                                                     
Isobutyl Alcohol                                                          
                23.75                                                     
(ASTM D1719)                                                              
Methyl Ethyl Ketone                                                       
                7.85                                                      
(ASTM D740)                                                               
Methyl Isobutyl Ketone                                                    
                10.16                                                     
(ASTM D1153)                                                              
Xylene (ASTM D846)                                                        
                1.62                                                      
______________________________________                                    

              TABLE 4                                                     
______________________________________                                    
THIN B-COMPONENT PROPERTIES                                               
Property       Requirement  Method                                        
______________________________________                                    
Amine equivalent weight                                                   
               1360-1608    N cmpds in gm                                 
(gm/eq)                     providing one                                 
                            titratable N.                                 
                            equiv.                                        
Specific gravity                                                          
               0.883-0.907  ASTM D1963                                    
Non-volatiles, wt %                                                       
               6.00-6.60    ASTM D1644                                    
Appearance     yellow to amber                                            
                            Visual                                        
               clear liquid                                               
______________________________________
To prepare the thin B-component composition, the amido-amine and diethylenetriamine are mixed at room temperature until homogeneous. The epoxy resin solution (EPON 1001CX 75) is preheated to 75° C.±5°, then gradually added to the amido amine diethylenetriamine mixture. Constant stirring is provided during the addition to provide for a complete reaction, while the temperature is maintained at 52° C.±3°. Mixing is discontinued when the brown solution becomes clear, after which the reaction mixture is allowed to cool to 37° C.±3°. The solvent mixture (Table 4) is added slowly with constant stirring until the solution is homogeneous and meets non-volatile requirements.
To prepare the thin coating, 45 volume % (±0.5%) quantities of A-component and B-component compositions are combined and thoroughly mixed. Methyl isobutyl ketone is gently stirred into a mixture of A-component and B-component to reach the 100% volume. The thin coating is then filtered through a Resco fine filter and allowed to stand for 45 minutes before using.
After degreasing the surface to be coated with one of several conventional degreasing solvents such as Freon TA or acetone, the thin coating is applied to the interior of a cryotank made of fiberglass reinforced with graphite fiber or of a polymer matrix reinforced with glass fiber. Application can be made with a dry lint-free and oil-free cloth or with a Teflon applicator such as a paddle, scraper or roller. The thin layers are allowed to dry for 30 minutes after which they are cured at 230° F.±5° for 2 hours. The combined components must be used within 8 hours of mixing and should be stored, if necessary, in a closed container at room temperature.
A thick A-component is shown in Table 5 with thick A-component properties given in Table 6. The ingredient and solvents of thick B-component are shown in Table 7. Thick B-component properties are given in Table 8.
              TABLE 5                                                     
______________________________________                                    
THICK A-COMPONENT COMPOSITION                                             
Ingredient          Percent by Weight                                     
______________________________________                                    
Dye, Oil Red, PD15344.sup.1                                               
                    0.1 ± 0.01                                         
Liquid Epoxy Resin  Remainder                                             
Shell Epon 828.sup.2                                                      
______________________________________                                    
 .sup.1 Eaton Chemical Division, Western Eaton Solvents & Chemical Co.,   
 13395 Huron Dr., Romulus, Michigan, 48174                                
 .sup.2 Shell Chemical Co., Polymer Division #1 Shell Plaza, Houston, Texa
 77002                                                                    

              TABLE 6                                                     
______________________________________                                    
THIN A-COMPONENT PROPERTIES                                               
Property          Requirements                                            
                              Method                                      
______________________________________                                    
Weight per Epoxide Equivalent                                             
                  180-196     ASTM D1652                                  
Refractive Index  1.5660-1.5760                                           
                              ASTM D1218                                  
Color             Red         Visual                                      
Specific Gravity at 25° C.                                         
                  1.15-1.18   ASTM D1963                                  
Water, wt %       0.25 max.   ASTM E203                                   
Viscosity at 25° C., CPS                                           
                  10,000-15,000                                           
                              ASTM D2393                                  
Workmanship       Free of visible                                         
                              Visual                                      
                  bubbles and                                             
                  contaminants                                            
______________________________________                                    

              TABLE 7                                                     
______________________________________                                    
THICK B-COMPONENT COMPOSITION                                             
Ingredient           Percent by Weight                                    
______________________________________                                    
P-Nonylphenol.sup.1  45 ± 0.5                                          
Versamid 125.sup.2   45 ± 0.5                                          
Mix well, then add                                                        
1-(2-Aminoethyl)piperazine.sup.3                                          
                     (Remainder)                                          
______________________________________                                    
 .sup.1 Eastman P7956 or equal, CAS Reg. No. 10440-5, Jan. 1979           
 .sup.2 Magnolia Plastics, Inc., Chamblee, CA; or Henkel Corp., Resin Div.
 4620 W 77th St., Minneapolis, MN 55435                                   
 .sup.3 Eastman 10643 or equal, CAS Reg. No. 14031-8                      

              TABLE 8                                                     
______________________________________                                    
THICK B-COMPONENT PROPERTIES                                              
Property   Requirement                                                    
                      Method                                              
______________________________________                                    
Amine equivalent                                                          
           190-210    N. compounds in gm providing                        
weight, gm/eq         one titratable N.sub.2 equivalent                   
Refractive Index                                                          
           1.5095-1.5195                                                  
                      ASTM D1218                                          
______________________________________
The thick A+B composition comprises a 50:50 mixture (±1%) of the two solutions. The combined mixture has a maximum work life of 12 minutes at 75° F.±10° and must, therefore, be quickly applied using a dry lint-free and oil-free cloth or with a Teflon applicator such as a paddle, scraper or roller. The applied thick layers are cured at 150° F. for about 90 minutes, or at 165° F. for 60 minutes, or at 205° F. for at least 45 minutes. It is not recommended that the article be subjected to a temperature of more than 215° F. until curing is completed.

Claims (3)

I claim:
1. A cryogenic tank comprising:
a tank configuration of suitable material to withstand cryogenic conditions;
the interior of said tank configuration lined with consecutive layers of organic coatings, said layers comprising;
a first layer of minimum thickness, from about 0.0001 to 0.001 in. thick, to establish a continuous coating for bonding;
a layer subsequent to said first bonding layer of suitable thickness, from about 0.0001 to 0.001 in. thick, to establish bonding reliability;
a layer subsequent to said bonding reliability layer of suitable thickness, from about 0.001 to 0.010 in. thick, to insure molecular impermeability;
a layer subsequent to said molecular impermeability layer of suitable thickness, from about from 0.001 to 0.010 in. thick, to guarantee integrity at cryogenic temperatures;
a layer subsequent to said integrity layer of suitable thickness, from about 0.0001 to 0.001 in. thick, to insure a smooth defect-free surface.
2. The cryogenic tank of claim 1 wherein said organic coatings comprise epoxy resins.
3. The cryogenic tank of claim 2 wherein said first bonding layer comprises the epoxy mixture of Table 1 and Table 3, as follows:
              TABLE 1                                                     
______________________________________                                    
THIN A-COMPONENT COMPOSITION                                              
                         Percent by Wt                                    
Ingredient               (+0.010%)                                        
______________________________________                                    
Epon 1002 or 1002F.sup.1 54.9                                             
Dye, Oil Red PD15344.sup.2                                                
                         0.20                                             
Isopropyl Alcohol (ASTM D770)                                             
                         1.30                                             
Xylene (ASTM D846)       2.80                                             
Methyl Isobutyl Ketone (ASTM D1153)                                       
                         5.60                                             
Cyclohexanone, Tech. Grade                                                
                         2.60                                             
Methyl Ethyl Ketone (ASTM D740)                                           
                         8.20                                             
Normal Butyl Alcohol (ASTM D304)                                          
                         2.60                                             
1-Methoxy-2-Propanol     Remainder                                        
______________________________________                                    
 .sup.1 Shell Chemical Co., Polymer Division #1 Shell Plaza, Houston, Texa
 77002                                                                    
 .sup.2 Eaton Chemical Division, Western Eaton Solvents & Chemical Co.,   
 13395 Huron Dr., Romulus, Michigan, 48174                                

              TABLE 3                                                     
______________________________________                                    
 THIN B-COMPONENT COMPOSITION                                             
______________________________________                                    
Ingredient      Percent by Wt (+0.05%)                                    
______________________________________                                    
Diethylenetriamine                                                        
                1.43 AEW = 34.4 to 37.0 g/eq                              
                Sp Grav = 0.945-0.955                                     
Amido-Amine     3.53 Celanese, #1 Riverfront Plaza                        
(Epi-Cure 855)  Louisville, KY 40202                                      
Epoxy Resin Solution                                                      
                3.25 Shell, #1 Shell Plaza                                
(Epon 1001 CX 75)                                                         
                Houston, TX 77002                                         
Solvent Mixture Remainder (See Below)                                     
______________________________________                                    
Solvent           Weight percent (+0.8%)                                  
______________________________________                                    
Toluene (ASTM D362)                                                       
                  5.24                                                    
1-Methoxy-2-Propanol                                                      
                  51.38                                                   
Isobutyl Alcohol  23.75                                                   
(ASTM D1719)                                                              
Methyl Ethyl Ketone                                                       
                  7.85                                                    
(ASTM D740)                                                               
Methyl Isobutyl Ketone                                                    
                  10.16                                                   
(ASTM D1153)                                                              
Xylene (ASTM D846)                                                        
                  1.62                                                    
______________________________________
said bonding reliability layer comprises the epoxy mixture of Table 1 and Table 3, said molecular impermeability layer comprises the epoxy mixture of Table 5 and Table 7, as follows:
              TABLE 5                                                     
______________________________________                                    
THICK A-COMPONENT COMPOSITION                                             
Ingredient          Percent by Weight                                     
______________________________________                                    
Dye, Oil Red, PD15344.sup.1                                               
                    0.1 ± 0.01                                         
Liquid Epoxy Resin  Remainder                                             
Shell Epon 828.sup.2                                                      
______________________________________                                    
 .sup.1 Eaton Chemical Division, Western Eaton Solvents & Chemical Co.,   
 13395 Huron Dr., Romulus, Michigan, 48174                                
 .sup.2 Shell Chemical Co., Polymer Division #1 Shell Plaza, Houston, Texa
 77002                                                                    

              TABLE 7                                                     
______________________________________                                    
THICK B-COMPONENT COMPOSITION                                             
Ingredient           Percent by Weight                                    
______________________________________                                    
P-Nonylphenol.sup.1  45 ± 0.5                                          
Versamid 125.sup.2   45 ± 0.5                                          
Mix well, then add                                                        
1-(2-Aminoethyl)piperazine.sup.3                                          
                     (Remainder)                                          
______________________________________                                    
 .sup.1 Eastman P7956 or equal, CAS Reg. No. 10440-5, Jan. 1979           
 .sup.2 Magnolia Plastics, Inc., Chamblee, CA; or Henkel Corp., Resin Div.
 4620 W 77th St., Minneapolis, MN 55435                                   
 .sup.3 Eastman 10643 or equal, CAS Reg. No. 14031-8
said integrity layer comprises the epoxy mixture of Table 5 and Table 7, and said smooth defect-free layer comprises the epoxy mixture of Table 1 and Table 3.
US07/449,175 1989-12-13 1989-12-13 Organic liner for thermoset composite tank Abandoned USH943H (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5651474A (en) * 1994-12-22 1997-07-29 The United States Of America As Represented By The Secretary Of The Air Force Cryogenic structures
US6334589B1 (en) * 1998-05-11 2002-01-01 Lockheed Martin Corporation Cyanate ester composites for oxygen containment
US6494405B1 (en) * 1998-05-11 2002-12-17 Lockheed Martin Corporation PEAR composites for oxygen systems

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US3383004A (en) 1965-08-17 1968-05-14 Preload Co Inc Plastic storage tank
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US3814275A (en) 1972-04-03 1974-06-04 Mc Donnell Douglas Corp Cryogenic storage vessel
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US4366917A (en) 1975-03-04 1983-01-04 Technigaz Cryogenic tank
US4378403A (en) 1975-03-04 1983-03-29 Technigaz Laminated composite material usable in heat-insulating composite walls
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US4785955A (en) 1980-06-24 1988-11-22 Kabushiki Kaisha Toshiba Vacuum container for heat-vacuum test chamber

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Publication number Priority date Publication date Assignee Title
US2788306A (en) 1953-03-24 1957-04-09 Pittsburgh Plate Glass Co Surface treatment of halogenated fluoroethylenes and laminates thereof
US2927867A (en) 1954-06-23 1960-03-08 Donald L Hings Corrosion and abrasion resistant coating and method for making same
US3257265A (en) 1962-09-14 1966-06-21 Aerojet General Co Laminated cryogenic insulation
US3406857A (en) 1964-12-09 1968-10-22 Air Reduction Insulated plastic vessel
US3383004A (en) 1965-08-17 1968-05-14 Preload Co Inc Plastic storage tank
US3738527A (en) 1970-11-18 1973-06-12 J Townsend Method of manufacturing and liner for liquid storage tank
US3795573A (en) 1971-09-27 1974-03-05 E Smith Liner
US3814275A (en) 1972-04-03 1974-06-04 Mc Donnell Douglas Corp Cryogenic storage vessel
US4366917A (en) 1975-03-04 1983-01-04 Technigaz Cryogenic tank
US4378403A (en) 1975-03-04 1983-03-29 Technigaz Laminated composite material usable in heat-insulating composite walls
US4117947A (en) 1977-08-01 1978-10-03 Frigitemp Corporation Internal insulation for liquefied gas tank
US4785955A (en) 1980-06-24 1988-11-22 Kabushiki Kaisha Toshiba Vacuum container for heat-vacuum test chamber
US4452375A (en) 1981-04-02 1984-06-05 The Dow Chemical Company Manufacture of draw-redraw cans using steel sheet material film laminated or extrusion coated with a high density polyethylene graft copolymer

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5651474A (en) * 1994-12-22 1997-07-29 The United States Of America As Represented By The Secretary Of The Air Force Cryogenic structures
US6334589B1 (en) * 1998-05-11 2002-01-01 Lockheed Martin Corporation Cyanate ester composites for oxygen containment
US6494405B1 (en) * 1998-05-11 2002-12-17 Lockheed Martin Corporation PEAR composites for oxygen systems
US6837464B1 (en) * 1998-05-11 2005-01-04 Lockheed Martin Corporation Lox-compatible composite tank for aerospace applications

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