Water Epoxy PDF

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Background Two piece cans are used throughout the world to distribute beer and soft drinks. Against the threats of glass and polyester containers, two piece cans have the advantage of fitting the requirements and also being cheaper overall, hence it holds the greater part of a growing market. Currently the developed market in the west is growing at 2-3%, however the newer developing markets in the east are growing at a projected rate of 11-12%. The organic coating is an integral part of the two piece can. Without the thin organic film, the product packed in the can would spoil or at the very least become contaminated, certainly the can would suffer from corrosion problems. Therefore it is necessary to use organic coatings to protect both the products, the can and the packed beverage. The standard organic solvent based coating within the two piece can industry was the epoxy-phenolic, or epoxy-urea interior spray coating. This type of coating has now been almost completely superseded by waterborne systems. Environmental legislation passed in the early 1970's (eg. California's Rule 66) prohibited the use of specific organic solvents and restricted the use of others, and demanded that higher solids coatings be developed. In the late 70's, and early 80's ecological pressure demanded that manufacturers cease using organic solvents within their products. This has led to a reduction in the VOC of polymeric coatings within the industry, especially in the high volume consumer markets like the can coatings industry. The result has been the development and expansion of waterborne coatings technology including of course waterborne epoxy resins. The original waterborne two piece can coating lacquers were based on water dispersible acrylic resins, similar to emulsion polymerisation types. Although simple and flexible in their ease of use within formulations, they quickly proved to be inferior with respect to chemical resistance and flavour impairment problems. Epoxy based films however meet the above requirements, extremely well. They are in general non toxic, exhibit relative chemical inertness, give excellent chemical resistance, and can be formulated to give good adhesion and flexibility. Waterborne epoxies have been available to the coatings industry since the early 1960's and have found extensive use as primers for the automotive and the structural coatings industries. Nevertheless food contact legislation (FDA(1) in the US, BGA in Germany etc....) lists materials approved for food contact, and prohibits the use of nonapproved materials. This has restricted the use of waterborne epoxy technology of the automotive industry from being used in can coatings. In order to overcome legislative restrictions, coating technologists have been forced to develop legislation approved waterborne systems.
Waterborne epoxies for two piece interior can coatings By A.C. Hoggan LRSC
BBA Associates Limited Registered in England and Wales No: 4177437 VAT Registration No: 702718945
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Epoxy chemistry Originally developed commercially in the late 30's by Castan, and early 40's by Ciba A.G., then taken up for use in aircraft manufacture, epoxy (polyglycidyl ether) technology was introduced to the coatings industry in the late 1940's. The excellent chemical and physical properties exhibited by epoxies has meant a sustained and continued growth in importance within the coatings industry to a level such that over 500,000 tonnes/year of epoxy resins were consumed by the industry in 1990. Each major manufacturer (eg. Ciba Geigy, Dow, Shell, Du Pont) of epoxy resins has an extensive range of products based on the glycidation of epichlorohydrin (EPC) and polyhydroxy phenols (or polybasic acids). The most significant series of resins for the can coatings industry is based on the condensation reaction of EPC and diphenylolpropane (4,4-isopropylidenediphenol, Bisphenol A) as illustrated below (see figure 1).
Figure 1.
CH3 HO CH3 Diphenolpropane (Bisphenol A) Epichlorohydrin OH
Cl
CH3 HO CH3 O O
Na Cl
O O
CH3 O CH3 Diphenolpropane digycidyl ether (epoxy) O
The variations produced by the above reaction are almost unlimited. Practically however, the range of resins offered by the manufacturers are restricted to those most commercially viable. Although each manufacturer will have their own commercial names or codes for their products, in order to differentiate between the variants possible, most coatings technologists generally refer to the (2)`Epikote' series of epoxy resins when discussing resin types. A brief example of the resins and their epoxy functionality are listed in Table 1.
Table 1.
(3)
`Epikote' code 1001 1002 1004 1007 1009 1010 2007
Mw 880 1150 1480 2870 4000 4300 3000
EEW (g/mol 500 600 900 1800 3600 4500 1500
EEW (mmol/kg) 2000 1600 1200 600 300 300 700
Using the above codes the technologist can discuss their general requirements without having to refer to specific technical data. As previously stated the range of epoxies available off the shelf, although suitable for most applications, can be restrictive to the coatings technologist. However a process has been developed whereby chemists can produce epoxy resins tailored to their individual requirements. The process uses a low molecular weight liquid epoxy reacted with DPP with a catalyst under dry nitrogen to produce a chain extended high molecular weight solid epoxy. The reaction is as follows (see figure 2).
Figure 2 O O CH3 Diphenolpropane digycidyl ether CH3 O O CH3 + HO CH3 Diphenolpropane (Bisphenol A) OH
+ organo-phosphonium salt O CH3 O CH3 O OH O n CH3 CH3 O CH3 OH
Higher molecure weight chain extended epoxy The molecular weight and EEW can be controlled and optomised by varying the ratio of liquid resin to DPP. The molecular weight (MW), and epoxy equivalent weight (EEW, or WPE, weight per epoxy) can be calculated and manufactured to individual requirements using the following calculation; Equation 1 100 = X - Y EEW1 EEW2 HEW Where: EEW1 = desired epoxy equivalent weight of extended epoxy. EEW2 = epoxy equivalent weight of liquid epoxy to be extended. HEW = hydroxyl equivalent weight of Bisphenol A, (or alternative polyhydroxyl phenol) X = % diglycidyl ether of Bisphenol A Y = % Bisphenol A The coatings have a number of criteria to meet in order to satisfy the can manufacturers requirements. Particularly in the two piece beer can market as the flavour of beer is easily impaired. A 5-10ppm iron contamination of a beer packed in a two piece electro tin plated steel can will impart a metallic flavour to the product.
It is therefore very important the internal coating provides a protective dry film of high integrity. The following criteria are general requirements which must be met by the coating formulator; 1. 2. 3. 4. The dry film must be non toxic, and meet food contact legislation. The dry film must have the chemical resistance to provide a protective barrier between the packaged product and the packaging. The dry film must have the physical properties to impart excellent flexibility and of course adhesion to the substrate. The dry film must not impart any flavours to the packaged product.
Waterborne resin chemistry In order to produce a waterborne epoxy coating the resin must be made compatible with water. There are many methods used in achieving this; emulsify the resin directly in water using an emulsifying surfactant or a water soluble polymer to stabilise the system; use either an acid or a base functionality on the epoxy to produce an ion compatible resin that can then be dispersed in water. However, waterborne polymers used in interior can coating lacquers over the past fifteen years, have generally been established upon base neutralised, acid modified epoxies, in conjunction with an acrylic functionality. The neutralisation of the epoxy generates a water compatible resin, the acrylic portion tends to lend adaptability to the resin. Changing the monomers in the acrylic component can produce significant changes in the lacquer properties, eg. additional reaction with the epoxy component, greater film flexibility, better substrate compatibility. Typically a solid epoxy of 3000 to 4000 EEW ((4)Epikote 1007 or 1009 types or an analog material manufactured by the chain extension of a lower Mw liquid epoxy resin) is modified to provide an acid functional epoxy. In general, the acid functionality can be conferred by two methods, acid capping (see resin 1, and resin 2) of the oxirane groups or by the graft polymersisation of an epoxy with a carboxyl functional co-polymer (see resin 3). The co-polymer can consist of the reaction product of a free radical polymerisation of any approved ethylenic unsaturated monomers containing carbon-carbon unsaturation, eg. carboxyl functional acrylic monomers, (acrylic acid, methacrylic acid etc....), the lower alkyl esters, vinyl monomers (acrylamides), vinyl esters (vinyl acetate, vinyl butyrate), vinyl aromatic monomers (styrene, methylstyrene) etc.... The following is an example of a typical formula and procedure used in manufacturing a (5)phosphatised epoxy resin for use in waterborne can coating lacquer.
Resin 1 Raw Material Butyl diglycol Phosphoric acid 85% Butyl diglycol D.I.Water Acrylic co-polymer N-ethylmorpholine D.I. Water
Wgt 445.9 11.9 24.7 21.1 337.2 18.7 1165.5
% 14.40% 00.38% 00.79% 00.68% 10.89% 00.60% 37.64% 100%
NVM: 43% @ 193 C/10 minutes The epoxy is dissolved in the BDG at 122 C to produce an epoxy solution, the concentrated (85%) phosphoric acid is then added under agitation, then a further addition of BDG is added. The mixture is agitated and held at 123 C over a period of 30 minutes, cooled to 121 C, and DIW added over a period of 10 minutes. The mixture is held under agitation at 124 C for two hours, then the acrylic copolymer(s) are mixed in over a period of 30 minutes at a temperature of ~124 C. Finally the mixture is reduced in viscosity and a water compatible dispersion produced, with the addition of the amine mixture. It should be noted the co-polymer should be added in the correct order otherwise the dispersion will prove to be unstable. Below is an example of a typical formula and procedure used in manufacturing a (7)benzoic acid capped epoxy resin for use in a waterborne can coating lacquer. Resin 2 Raw Material Diphenylolpropane Benzoic acid Butyl glycol n-butanol Acrylic co-polymer D.I. Water Wgt 915 52 156.3 680 2388 6137.7 % 07.59% 00.43% 01.30% 05.64% 19.81% 50.93% 100%
NVM: 28% 193 C/10 minutes The liquid epoxy, diphenylolpropane, benzoic acid and butyl glycol are mixed together, heated to ~130 C, allowed to exotherm to 200 C, then held at 165 C for two hours after the peak exotherm. The resulting reaction product is then cooled, with the addition of n-butanol to ~100 C. The acrylic co-polymer and DIW is mixed
together and held under reflux at ~95 C for twenty five minutes. The resulting acrylic solution is added to the acid capped epoxy under agitation at ~70 -80 C over a period of approximately one hour. The resulting aqueous dispersion can be neutralised with a tertiary amine and used to formulate can coating lacquers. The following is a typical example of an (9)epoxy-acrylic graft co-polymer used in waterborne epoxy can coating lacquers. Resin 3 Raw Material (10) DER 333 Diphenylolpropane n-butanol Butyl glycol Styrene Methacrylic Acid Ethyl acrylate Benzoyl peroxide D.I. Water Triethanolamine D.I. Water Wgt 231 117 203 135 40 64 44 10 795 57 300 % 11.57% 05.86% 10.17% 06.76% 02.00% 03.21% 02.20% 00.50% 39.83% 02.86% 15.04% 100%
NVM: 25% 193 C/10 minutes The epoxy chain extension reaction is normally carried out under an inert, dry, nitrogen blanket. The liquid epoxy is heated to 82 C, then diphenylolpropane is added and mixed in. The mixture is heated to ~191 C over two hours and held at that temperature under agitation for a further two hours until an epoxy of EEW 3500 - 4000 is produced, then n-butanol and butyl glycol is added. The acrylic monomers are then mixed together, and added gradually added over a period of two hours to the epoxy solution held at a temperature of 118 C. The resulting resin is then cooled to 85 C, and dropped into a mixture of DIW, and TEA under agitation. The monomers are added to the solution of epoxy in order that a free radical initiated polymerisation can take place in the presence of the epoxy. The grafting of the addition polymer onto the aliphatic carbons of the epoxy, takes place during this polymerisation stage. The free carboxyl groups on the acrylic graft co-polymer can be neutralised with a tertiary amine which can activate an esterification reaction between the acrylic carboxyl moieties and the epoxy reactive sites. On the addition of de-ionised water, the free carboxyl moieties of the acrylic co-polymer react with the amine to produce a water soluble or dispersable quaternary ammonium hydrogel of the modified epoxy. The quaternary reaction takes the following form;
Figure 3
O CH3 O CH3 O OH O n CH3 CH3 O CH3 OH
Diphenolpropane digycidyl ether (epoxy) 3 Tertiary amine + NR
O
+
O R 1N R 3 R2 CH3 H3C O O OH n + R4 C R5 n O C C R4 C O OH Acrylic monomer H3C CH3 O
R2 R 3N
-
R1
R5
O O CH3 H3C O O HO n n H3C CH3
R1 N R3 R2
R2 + R3 N R 1 O O C C O R4
R5
Can coating lacquers A waterborne interior two piece can coating lacquer would be formulated using resins similar to those described above. However, the lacquer, no matter which type of resin chemistry is available, must meet certain criteria.
1. 2. 3. 4. 5. 7. 8.
The coating must be formulated to a suitable viscosity for the chosen application method. The rheology (thixotropy, ie. pseudo-plastic, or dilatant flow) must be considered and adjusted or the coating will not apply well. The dynamic surface and interfacial tension of the coating must be made compatible with the substrate or substrate wetting problems will occur. The adhesion and flexibility of the dry film must be compatible with subsequent processing conditions. The resin solids content of the formulation must be sufficient that the coating will provide the dry film weight required for protection within the can. The coating must meet the requirements of the customers local and federal environmental legislation. Finally but not least all formulated interior two piece can coatings must be non-toxic, chemically inert, meet organoleptic requirements, and be approved within the current food contact legislation.
The resin manufactured for use in can coatings may be the ideal formulation for the processing of the resin, however the dispersion produced will probably be totally unsuitable for use as a coating lacquer. In the unlikely event the resin dispersion is suitable for use directly as a coating lacquer, one customers' application technique and equipment specifications will almost certainly be different from another's. Therefore the coating formulator will either be required to formulate a single, standard coating to meet all conditions, or a different lacquer for each situation encountered. The first considerations for the formulator must be the application technique to be used, and the substrate to be applied. This will determine the resin chemistry, and the physical specifications of the formulation. All two piece beverage can fabricators currently use airless spray techniques of application, the two piece food can industry uses roller coated sheet or coil to fabricate food cans. The substrates available to the fabricators are of two metals, representing three substrate types, aluminium, electro-tin plated steel (ETP), and tin free steel (TFS), tin free steel is used exclusively in the two piece food can industry. There are many different grades of substrate, and equally, different surface treatments on the metal. The coating must perform no matter the type of substrate is chosen by the customer. Lacquer chemistry In general the coating viscosity can be adjusted by the addition of a water soluble tertiary amine, hydrophobic solvents, and of course water. The addition of the tertiary amine will further neutralise a base neutralised epoxy resin (up to 100% neutral-acetin) and produce an increase in viscosity. The effect of the addition of hydrophobic organic solvents will be to migrate into the dispersed resin, causing a
change in the particle size and the size distribution, resulting in a rheological change (increased pseudo-plastic behaviour) in the dispersion. The addition of water reduces the viscosity. Further, the addition of small quantities of hydroxyl functional cross-linking resins eg. cresol and phenol resoles, alkyl melamine and benzoguanamine aminoplast resins, can be used to modify the hardness, adhesion, and flexibility of the original waterborne epoxy. The coalescence and drying function of a waterborne coating is critical to its final performance. The evaporation rate of the mobile phase can be modified, and film given a longer open time avoiding water entrapment and blistering during drying. The careful selection and addition of organic solvents (hydrophilic, hydrophobic, resin compatible and resin incompatible) to the coatings will improve the substrate wetting and modify the coalescence of the applied coating during high temperature curing. The use of water soluble polymers will modify the application characteristics of the wet coating over the substrate towards that of a solvent system. Surfactants of the type eg, polyethylene oxide-polypropylene oxide, alkyl phenol ethoxylates, sorbitol modified dioctyl sulfosuccinates, alkylated alkynols, can be used to modify the dynamic surface tension towards that of the substrate, and the interfacial tension between the stationary and mobile phases of the dispersion. The reduction in surface tension can dramatically improve the application, wetting, and dry film appearance of the coating, however unless the surfactant is bonded within the coating, or is driven off during high temperature curing, the material can remain free within the dry film, generating organoleptic and chemical resistance problems. Lacquer formulations Typically the organic solvents employed in the formulation of the epoxy resin into a workable lacquer are generally of the following type; alkyl alcohols, aliphatic and aromatic ketones, glycol ethers, aliphatic and aromatic solvents. The solvent choice must be based upon the solvent properties and on consideration of the lacquer application technique. The more commonly preferred solvents of the past twenty years have been based around the lower homologues of ethylene glycol ether. Unfortunately, from the formulators viewpoint, this type of solvent is being phased out of coatings formulations by pressure from environmental and HSE legislation eg. US federal HAP's legislation. The alternatives available exploit the higher homologues of ethylene glycol ether and of course the homologues of propylene glycol ethers. Although the ester variation of the glycol ethers are available to the formulator, great care must be taken to ascertain the hydrolysis stability of the ester being considered. Careful study of the hydrophobic/hydrophilic tendency of the ester will indicate whether water compatibility would propagate an undesired (delayed) hydrolysis reaction to the carboxylic acid form of the alkyl ester. The hydrolysis reaction can take from a few days to a few weeks, however the reaction can be accelerated in the presence of other acid groups, and certain surfactants. It should also be noted that glycol ether esters are not the only solvents capable of hydrolysis, certain ketones will exhibit similar delayed hydrolysis, as will waterborne epoxies but over a period of up to six months as opposed to weeks.
Lacquer 1 The following formulation is typical of type used as a spray applied beverage can coating lacquer. Raw Material Epoxy resin 3 (11) Texanol (12) Dowanol PM (13) Be 3747 D.I. Water TEA % 78.89% 2.37% 1.48% 6.67% 16.76% 0.49% 100%
Viscosity: 24" Ford No 4 cup (25 C) NVM: 24% 200 C/3 minutes The (14)Texanol and (15)Dowanol PM are added slowly to the epoxy dispersion under agitation, and mixed together for 20 minutes. The cross-linker is then added to the dispersion under maximum agitation, so that it enters the dispersion at the center of the agitators vortex. the mixture is agitated continuously for a further 40 minutes. The dispersion is then adjusted to the final NVM, and viscosity by the careful addition of DIW, and tertiary amine to reach the NVM and viscosity required. The above formulation can be airless spray applied to a two piece beverage can giving a flexible, protective coating with excellent adhesion to aluminium or ETP. If required the coating viscosity/solids relationship can be modified by carefully balancing the DIW and tertiary amine (TEA) addition, to give a lower NVM, higher viscosity, or higher NVM, lower viscosity coating. Lacquer 2 Raw Material Epoxy resin 1 Butyl glycol n-butanol (16) Cymel 1156 D.I. Water n-ethylmorpholine % 78.89% 2.37% 1.48% 8.00% 16.76% 0.49% 100%
Viscosity: 165 cps NVM: 40% 193 C/10 minutes The above formulation can be used as a coating for roller coat in a sheet fed process for food can manufacture. The formulation exhibits excellent adhesion over TFS, plus good acid and alkali resistance. Again if required the coating viscosity/solids relationship can be modified by the DIW/tertiary amine balance. The coating rheology of this coating could also be modified by addition of water soluble polymers, or associative thickeners in order to produce a coil coating material. The
practical limits to the type and quantity of the solvents and additives used are created by legislative and commercial factors ie. toxicity, maximum VOC allowable and the price of the formulated lacquer. Two piece beverage can fabrication. As stated previously two piece beverage cans are coated using an airless spray technique. In general different spray techniques are used for aluminium cans than for steel cans, also there are differences between cans for beer and cans for soft drinks. The differences between the application techniques and conditions used are due to the fabrication techniques and problems associated with the substrates, and the differences in the beverages to be packed. Most high production units (1 - 2 billion cans/year) use the draw and wall iron (DWI) technique of fabricating two piece cans. DWI cans are fabricated as follows, a coil of substrate is lubricated and fed through a press where shallow cups are punched out. The cups are then thinned and formed by drawing through a series of progressively smaller dies (rings) until the can shape is formed. The can is then trimmed to the correct height, and passed through a series of washes (aluminium is acid etched at this stage) and rinsed before being dried, decorated externally, and spray coated internally. The main difference, but not exclusively so, is after the can has received the external decoration, at this point steel cans are generally (though not always) passed through a necking process before receiving the internal coating. Aluminium cans however are washed, decorated externally, and coated internally before the necking process. The slightly different fabrication route between the two substrates is due to the lack of lubrication in aluminium cans causing die wear. The necking process for aluminium cans relies on the external and internal coating to provide die protection. The tin coating of the ETP steel provides sufficient lubrication to prevent pronounced wear of the necking dies. Two piece can coating application Due to the taste contamination of beer by tiny concentrations of iron, it is necessary to protect beer cans against this form of spoilage. In order to guarantee protection of the packed product (beer, cola etc....) from iron contamination, the internal coating is applied twice, wet on wet, or wet on dry, to steel cans. The contamination problem is less pronounced with aluminium cans therefore the industry applies a single coat to aluminium cans. The type of products packed are split into two groups, beer, and soft beverages. Beer is considered to be less aggressive and corrosive than soft beverages. These factors manifest themselves in practice through the dry film weight required to protect the can (see Table 2, & 3).
Table 2. 33 cl cans Aluminium ETP steel Table 3. 50 cl cans Aluminium ETP steel
Beer 120 mg 2 x 160 mg
Soft drinks 140 mg 2 x 170 mg
Beer 180 mg 2 x 180 mg
Soft drinks 210 mg 2 x 200 mg
As stated previously the technique used to apply the lacquer to the cans is airless spray. Unlike air spray application, this technique allows a finely atomised spray to be produced and therefore greater control over the lacquer application. In order to successfully apply a can using this technique, three parameters must be considered before the lacquer is applied, can type, required coating weight, and finally the nozzle type to use. The first consideration has to be the can type, steel or aluminium, necked or unnecked, for beer or soft drinks. The category of can to be applied determines the coating weight, and dry film distribution required, which in turn determines the nozzle type(s) to be used. Nozzles are graded by the flowrate, and angle of the fan delivered. Each nozzle manufacturer (eg. Nordson, Delevan, Spraying Systems) has a range of flat spray nozzles which will deliver lacquer at a set flowrate, and a set angle to the fan pattern. The application technique applies the lacquer at very high pressures (50-70 bar, 800-1000 psi) through a tungsten tipped nozzle to the interior of the rotating can. The fan pattern can either be symmetric or asymmetric. The type of nozzle chosen will define the angle, distance, and the height of the spray gun (and hence the nozzle) in relation to the can. The nozzle is chosen on the amount of lacquer to be delivered to attain the correct dry film weight and distribution. The following table lists a sample of the typical specification for a `Spraying Systems' flat spray nozzle (see table 4).
Table 4 Nozzle Designation 650050 650033 650017 650008 500050 500033 500017 500008 400050 400033 400017 400008 150050 150033 150017 150008 Orifice Diameter 0.46 mm 0.38 mm 0.28 mm 0.18 mm 0.46 mm 0.38 mm 0.28 mm 0.18 mm 0.46 mm 0.38 mm 0.28 mm 0.18 mm 0.46 mm 0.38 mm 0.28 mm 0.18 mm Fan Angle 65 65 65 65 50 50 50 50 40 40 40 40 15 15 15 15 Flowrate(@ 60 bar) 1.13 l/min 0.72 l/min 0.36 l/min 0.18 l/min 1.13 l/min 0.72 l/min 0.36 l/min 0.18 l/min 1.13 l/min 0.72 l/min 0.36 l/min 0.18 l/min 1.13 l/min 0.72 l/min 0.36 l/min 0.18 l/min
The decision has to be made whether to apply using a single spray gun (ie. one nozzle), or a two gun (two nozzle) system. Generally aluminium cans are sprayed using a single gun setup, steel with a double gun system, however the system used will depend on the coating requirements. At a manufacturing rate of 1000 to >2000 cans per minute, the application window in front of the nozzle is limited (maximum 150 - 200 mS). The application time is selected so that the lacquer is applied within this window. Also within the application time selected the can should execute 2.5 rotations, this ensures complete coverage around the can. Care is required to select a nozzle with sufficient flowrate (ml/min.)to allow application of the required coating weight within the application window, and the can rotation required. The angle of the fan should permit the lacquer to be applied over the area of can requiring coating. Single gun application In a single gun application the nozzle is required to deliver the full coating weight to the can, the angle of the fan pattern must be capable of applying lacquer just above the can dome center, and along the length of the can, allowing for an overspray (minimum) in order to ensure coverage of the can edge.
Twin gun application For a twin gun application technique, the first nozzle applies lacquer to the dome and lower side wall of the can, the second nozzle applies lacquer over the dome, and along the length of the can, again the second gun is set up to overspray the can edge. The ratio of the applied film weight split between the first and second nozzle should reflect the area of the can each gun and nozzle covers. In both cases the distribution of the internal lacquer can be regulated by adjustment of the gun angle or more useful the choice of a nozzle with an asymmetric fan pattern. The standard symmetrical nozzle exhibits an even distribution of lacquer to the extent the direction of the nozzle in relation to the can is in effect unimportant as long as it is perpendicular to the open end of the can. The asymmetric nozzle as would be expected, exhibits an asymmetric lacquer distribution , where the fan pattern displays a higher flowrate end and a lower flowrate end. The asymmetric nozzle should be set to apply the higher flowrate end to the lower side wall area of the can, ie. should be uppermost to the can. Evaluation and testing A series of standard tests are undertaken to evaluate the quality of the application, and the dry film. Film thickness: A lacquer is applied to a can and cured, the coating thickness is tested using a Strand Gauge. The equipment is calibrated using panels applied with the coating at known film thicknesses. The Strand Gauge measures the insulation resistance of the coating with reference to the calibration standards used, and gives a relative value for the coating thickness. Porosity: This tests the successful application of the can and the dry film integrity. The can is filled to the rim with a salt solution (1% NaCL, or NaHSO4) an electrode is immersed in the solution, and a voltage is applied across the can, 6.3 V/4 seconds, then the insulation properties of the cured film measured. The conductance should be < 5 mA, preferably < 1 mA. Flavour: The coated can is filled with a bottled or draught lager beer, left to react, then compared against a standard. Points of reference are changes in acidity, bitterness, and any metallic flavour compared to the standard Adhesion: A standard test used on most organic coatings, in the case of two piece cans the coated can is pasteurised in a water bath at 82 C/30 minutes. The can is cooled, dried, then crosshatched and an adhesive tape applied to the crosshatched area to confirm the cured film adheres to the body, and base of the can.
Flexibility: Normally evaluated using a wedge bend or T-bend test, with reference to ASTM test methods D3281-84, or D4145-83. A sample of applied and cured coating is bent through 180 , and evaluated for fracture using acidic copper sulphate. The sample can be further evaluated through a second, third, and fourth 180 bend. This corresponds to bending the substrate and hence the coating over 1, 2, and 3 thicknesses of substrate, ie. 1T, 2T, 3T. Pack test: The applied cans are packed with product, eg. beer, cola, diet drinks, product simulants etc.... A series of cans are applied, cured, packed with product, sealed and stored for 6 months (12 months in the US). A representative sample of the cans on test are opened every month and tested for substrate contamination via the cured film, ie. iron, or aluminium pick-up. Generally this is the only specific evaluation accepted by two piece can manufacturers as conclusive proof of coating integrity.
1 2,4,6,8 5 7 9 10 11,14 12,15 13 16
Refers to food contact legislation wrt can coatings, FDA listing 175.300. 'Epikote' is a trademark of Shell Chemicals US Patent No 4,638,020; Christenson, Rosenberger, Tetenbaum, PPG Industries Inc. US Patent No 4,302,373; Steinmetz W.H., E.I. Du Pont de Nemours & Co. US Patent No 4,212,718; Ting & Evans, SCM Corporation. 'DER' is a trademark of The Dow Chemical Company 'Texanol' is a commercial name for 2,2,4-trimethyl-1,3pentanediolmonoisobutyrate 'Dowanol' is a trademark of Dow Solvents. Supplied by BIP. 'Cymel' is a trademark of Dyno Cytec.

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CH3 HO CH3 Diphenolpropane (Bisphenol A) Epichlorohydrin OH

CH3 O CH3 Diphenolpropane digycidyl ether (epoxy) O

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`Epikote' code 1001 1002 1004 1007 1009 1010 2007

Mw 880 1150 1480 2870 4000 4300 3000

EEW (g/mol 500 600 900 1800 3600 4500 1500

EEW (mmol/kg) 2000 1600 1200 600 300 300 700

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+ organo-phosphonium salt O CH3 O CH3 O OH O n CH3 CH3 O CH3 OH

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Wgt 445.9 11.9 24.7 21.1 337.2 18.7 1165.5

% 14.40% 00.38% 00.79% 00.68% 10.89% 00.60% 37.64% 100%

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Diphenolpropane digycidyl ether (epoxy) 3 Tertiary amine + NR

O R 1N R 3 R2 CH3 H3C O O OH n + R4 C R5 n O C C R4 C O OH Acrylic monomer H3C CH3 O

O O CH3 H3C O O HO n n H3C CH3

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Beer 120 mg 2 x 160 mg

Soft drinks 140 mg 2 x 170 mg

Beer 180 mg 2 x 180 mg

Soft drinks 210 mg 2 x 200 mg

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