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Indexed Report No. S-62-3 CC: C. W. Theobald, Wilm. F6F) In J. A. Kla.csmann, " n ) Turn W, D. Lawson, IMDEXED" " ") P. B. Cochran, " ") InTurn D. McBurney, " M) J. W. Nestor ") " ) In Turn ") m % 61 J. C. Richards, Newburgh L. G. Wise, Exp. Station 0. H. Bullitt, Jr., Exp. Sta. G. I. Mulholland, Flint ftEFOBfCE COPY NOT TO B TAKEN FROM UNUR? File: 1865 1IURI10 MARSHALL LABORATORY LIBRARY E. I. du Pont de Nemours & Company F. &F., Finishes Division Marshall Laboratory Sales Development Report PROGRESS REPORT ON CUSTOM COLOR UNIVERSAL COLORANTS Date Issued : Period Covered : Project No. : Previous Reports: Notebook Nos. : April 12, 1962 4/1/61 to 2/1/62 P-24102 M-696, M-746, SM-61-8, SM-61-9 7128, 7332, 7435, 7573 PREPARED BY: APPROVED BY: WTC :dk N41536 APPENDIX ABBREVIATIONS USED THROUGHOUT REPORT G-12 H-156 H-200 H-481 H-541 H-609 H-632 H-695 H-73 W-362 W-621 W-679 W-895 W-325 DCO HLB P.D.W. a,47 P'1 3 RL RC-601 Soya lecithin Dehydrated castor oil Aromatic hydrocarbon Non-ionic surfactant (HLB = 10-13) Polyoxyethylene (5) sorbitan mono-oleate (Tween 81) Non-ionic surfactant (HLB * 10-13) Polyoxyethylene ester of mixed fatty and rosin acids. (Renex 20) Non-ionic surfactant (HLB = 13+) Alkyl aryl polyether alcohol. (Triton X-100) Odorless mineral spirits Anionic surfactant (HLB = 10-13) Di-Octyl Sodium Sulfosuccinate. (Triton GR-5) A fine surface-treated calcium carbonate. A fine precipitated red iron oxide pigment. ''Dalamar"* Yellow YT-717-D-azo pigment dye-stuff C.F. Chrome Yellow Light Y-433-D 95% red iron oxide pigment Alizarne Type Maroon Lake RP-293-D Dehydrated Castor Oil Hydrophile/lipophile balance * water/oil miscibility. High Values = Good water misc. Paint Distribution Warehouse "47 Process" 3 Roll Mill 10% dimer a.cids/65% soya acids/P.E. alkyd resin *-Registered Du Pont Trademark DUP030C PROGRESS REPORT ON CUSTOM COLOR UNIVERSAL COLORANTS INTRODUCTION: The Custom Color System for Interior Trade Sales paints permit dealers to mix matching colors in "Flow-Koten*, nLucite3S*, Gloss Enamel, Semi-Gloss Enamel, and Flat Alkyd qualities to about 1000 colors now in the system. This is accomplished by dispensing a definite volume of colorant (632-Line Custom Color Universal Colorant) from the Color Master Mixing Machine or tubes into the Custom Color white bases. This permits the dealers to supply a variety of qualities and colors with a minimum amount of inventory. The present type 632-Line Custom Color Universal Color ants have been sold since 1958 and although they have been gener ally satisfactory, certain deficiencies either know initially or which developed as we sold the colorants, required correction. The purpose of this report is to record the work done during the past year to overcome some of the deficiencies of the line. OBJECTIVES: Although the overall objective has been to improve the compatibility of the 632-Line so that its use could be extended to other products, specific objectives requiring attention were as follows: 1. Violet. To improve the alkali resistance of #11 Bright Red 2. To improve the settling properties of #21 Venetian Red Oxide. 3. Develop lead-free colorants to replace #12 Orange Ver million, #13 Chrome Orange, #14 Chrome Yellow Light, and #15 Bright Chartruese. 4. To develop a bright purple colorant for interior use. *-Registered Du Pont Trademark DUP030005973 -2- SUMMARY AND CONCLUSIONS: 1. An improved settling resistant #21 Colorant has been developed. A 45 day field test in nine P.D.W.'s resulted in con siderably improved Color Master Mixing Machine performance. 2. Lead-free #14 and #15 Colorants have been developed; neither colorant has been field tested. One color step is lost with the proposed colorants. 3. A lead-free #12 Colorant has been developed with good cross quality color uniformity and a minimum of brush sensitivity. Scrubbability and stability tests have not been run. 4. A proposed bright purple colorant showed good initial cross quality color uniformity and brush sensitivity but upon aging lost compatibility with "Flow Kote"` and "Lucite" bases. 5. A proposed #11 Colorant resulted in good alkali resis tance and fair brush sensitivity but upon aging lost compatibility with "Flow Kote" and "Lucite" bases. 6. Practically no work was done on the overall long term objective of improving the comparability of the 632-Line color ants to expand its use. ACTION TAKEN OR PROPOSED: 1. Release Letter #1946 has been written for national re lease of #21 Colorant. Plant batch stabilities will continue to be followed. 2. A Release Letter will be written for field testing of #14 and #15 Colorants. 3. Scrubbability tests, colorant and letdown stability, and Color Master Mixing Machine performance will be run with the lead-free #12 Colorant. 4. Laboratory work will continue to develop an alkali-resis tant #11 Colorant with little or no brush sensitivity and good com patibility with latex bases upon aging. DUP030005974 5. A lead-free #13 Colorant will be formulated from the lead-free #12 and #14 Colorants. 6. No further work will be done with the bright purple colorant until a. management decision is made concerning its desirability at the present time. PATENT SITUATION; No further patent action is currently contemplated with the color bases described in this report. U. S. Patent 2,996,397, assigned to Du Pont, embraces the Custom Color Universal Colorants having a vehicle consisting essentially of dehydrated castor oil and soya lecithin in combination with a non-ionic polyethanoxyethanol derivative surfactant. Several of the newer colorant for mulations are embraced by pending Patent Application FFD-1163, filed June 29, 1961, for which there has been no Office Action from the Patent Office to date. This invention embraces colorants based on synergistic combinations of certain non-ionic surfactants with an anionic soluble dialkyl sulfosuccinate salt and an oleagin ous vehicle consisting essentially of dehydrated castor oil. PUBLICATIONS PROPOSED: No publications are proposed at this time. ACKNOWLEDGEMENTS: The author wishes to express his gratitude to F. T. Stevenson, Jr., and J. J. Kilkeary for their valuable informa tion in this area. DUP030005975 -4- DISCUSSION: The Custom Color System permits dealers to mix about 1000 matching colors in "Flow Kote", ''Lucite", Semi-Gloss Enamel, Gloss Enamel, and Flat Enamel qualities by dispensing 632-Line Universal Colorants from the Color Master Mixing Machine or tubes into white bases. The original Custom Color Tube System was established in 1954-1955.3 The colorants involved were essentially pigments dis persed in RC-601, H-S32, and surfactants.7 Since these colorants were not stable in ,5Flow Rote51 bases, new colorants were developed in 1956-1958 on a H-156, G-12, H-632 and/or H-202, surfactant basis^>8, in 1960 the Custom Color white bases were revised to improve cross quality color uniformity .5 The Color Master Mixing Machine was introduced during 1959-1960 as a more accurate method of dispensing the Universal Colorants^. Since that time, the following deficiencies have been discovered in the Universal Colorants: 1. #21 Colorant (Venetian Red Iron Oxide) settles badly and is too viscous for good Color Master Mixing Machine dispensing. 2. tance . #11 Colorant (Bright Red Violet) has poor alkali resis 3. #12 (Orange Vermilion), #13 (Chrome Orange), #14 (Chrome Yellow Light), and #15 (Bright Chartreuse) colorants are prepared from lead-containing pigments. Removal of lead is desirable to avoid precautionary labeling under the Federal Hazardous Substances Labeling Act and to meet requirements of New York City and Baltimore. 4. The system does not contain a bright purple colorant. EXPERIMENTAL DETAILS: #21 Venetian Red Oxide 632-W-24456 Venetian Red Iron Oxide has been developed with settling and Color Master Mixing Machine dispensibillty im provement over 631-788 (#21 Colorant) although it is slightly more brush sensitive and shows considerable vehicle separation. However, the brush sensitivity is at an acceptable level and the vehicle se paration is readily reincorporated in the Color Mister Mixing Mach ine. The improved properties were achieved by replacing a calcined red iron oxide by a precipitated red iron oxide and by adding an DUP030005976 anionic surfactant (triton GR-5) to the Triton X-100/Soya Lecithin system. Fourteen months stability samples show no loss of compati bility in "Flow Kote:* and "Lucite" bases. A comparison of these two coslorants follows: #21 Venetian Red Oxide: Raw Current Materials Formula New Formula Reason for Change H-156 H-609 H-695 G-12 H-200 W-73 W-895 W-362 8.5 7.5 - 9.0 19.1 12.9 43.0 - 9.0 7.8 13.1 7.2 20.4 *" 42.5 Synergistic effect needed. Extender not needed to prevent flocculation. Produces less settling 100.0 100.0 Mill 3 RL Gallon Wt. 13.46 Raw Material Cost/Gal. $2.53 Milling Cost/ Gal. .83 Settling V. Poor Separation Considerable Ease of Re- incorporation V. Diff. S crubbability Satisfactory Gloss Reduc tion in Gloss Enamel 21 Gloss Increase in Flat Enamel " Brush Sensiti vity None "47 Process'* 11.93 $2.50 .39 Good Considerable Good Satisfactory it V. Slight DUP030005977 -6- Raw Materials Current Formula Mew ' Formula Reason for Changes Cross Quality Color Unifor mity. Good Aging on Color Master Mixing Machine Poor Color Master Mixing Mach ine Dispen sing Rase Poor Good Satisfactory Good #14 Chrome Yellow Light 632-W-18395 was developed as a lead-free #14 Colorant with ''Dalamar" Yellow replacing chrome yellow and by replacing Tween 81 and Soya Lecithin with Triton GR-5 and Renex 20 surfac tants.^- Although brush sensitivity is slightly greater than with the regular #14 Colorant (632-776) it is at an acceptable level and does not become worse with aging. One color step is lost in this substitution due to the high oil requirements of the ''Dalamar" Yellow. A comparison of the present colorant and the proposed colorant follows: Raw Materials Current Formula Proposed Formula Reason for Change H-156 H-481 H-609 G-12 H-695 H-541 H-200 H-632 W-679 W-621 4.7 7.9 1.1 3.0 - -- 6.8 3.2 73.3 * 100.0 25.0 5.0 - 5.0 5.0 45.0 15.0 100.0 Better wetting of W-621 II II II SI It If II II 1) It II It 11 II II 11 Lower consistency for "47 P" Reduce flocculation and also H-200 not required for new surfactant system. Lead-free DUP030005978 Raw Materials Current Formula Proposed Formula Reason for Change Mill Gal. Wt. Cost (Raw Mat.) per gal. Milling Cost per gal. Color Color Strength 3 RL 19.57 $6.41 $1.21 Red Toned Yellow Control "47 Process" 7.45 $5.97 .24 Clean-Green Yellow One-HaIf of control Cross Quality Color Uniformity Brush Sensitivity Stability on Color Master Mixing Machine Colorant & Let down Stability Settling Gloss Reduction in Gloss Enamel Gloss Increase in Flat Enamel Scrubbability Good None Satisfactory Satisfactory Fair Satisfactory Satisfactory Satisfactory Good Slight Satisfactory Satisfactory Good Satisfactory Satisfactory Satisfactory #15 Bright Chartreuse The proposed #15 Bright Chartreuse -is a blend Of approxi mately 97% "Balamar" Colorant and 3% #16 Colorant and has the same characteristics as the proposed lead-free #14 Colorant. #12 Orange Vermillion A lead-free #12 Colorant has been developed using Harmon's Signal Orange dispersed in Renex 20, Triton X-100, Triton GR-5, DCO, and solvents. Brush sensitivity and color development uni formity are satisfactory. Compatability with ''Flow KoteTC and 'Lucite" bases is satisfactory after three months. Scrubbability and water sensitivity tests have not been run. DUP030005979 -8- Peep Purple Colorant A deep purple colorant was developed by dispersing -325 (a Pigments Department Maroon Lake) in the above vehicle system. Although the initial color development and brush sensitivity were good, after three months aging, the compatibility with ""Flow Koten and "Lucite" bases deteriorated. Since this pigment is too hard to grind by "47 Process"5 it must be pebble milled or roller milled. #11 Bright Red Violet 332--18382, improved alkali resistant #11 Bright Red Violet Colorant, showed good color development initially with brush sensitivity slightly poorer than 632-773 (the current #11 Colorant). However, upon aging its compatibility with '"Flow Kote" and "Lucite" bases is very poor. This colorant is a dispersion of American Cyanamid Naphthol Red 20-7515 in Triton X-100, Triton GR-5, D.C.O,, and solvent. Although the Triton X-100 and Triton GR-5 produce a synergistic effect to give excellent cross quality color uniformity at a low surfactant level, they are apparently not stable in the presence of this pigment. The surfactant sys tem will be reviewed using both high and low HLB surfactants to replace medium range HLB surfactants and to determine in general whether a non-ionic or anionic/non-ionic system is more effective for color development and stability. Misc. In general, the organic pigments, being hydrophobic, are much more difficult to disperse in a water system than in organics which are hydrophilic. In addition, each organic pigment usually requires its own unique vehicle system. TC:dk DUP030005980 BIBLIOGRAPHY Release Letter 1513-B, National Marketing of Custom Color White Alkyd Bases", 1-10-55. Release Letter #1514, '`Trial Marketing of Custom Color Bases", F. T. Johnson, 12-28-53. Release Letter #1524 A & B, "National Marketing of Custom Color 'Flow Kote" Light Base", 1-10-55. Release letter #1673, "Trial Marketing of 10 Universal Color ants in Dallas and San Francisco", H.R. Heickel, 6-25-56. Release Letter #1882, "Proposal for Sale of New Custom Color Bases", B. L. Mansi, Sr. Memorandum Report No. SM-60-3, "Du Pont Color Master Mixing Machine", 0. R. Volk, 2-29-60. Memorandum Report No. M-696, "Custom Color Mix System for Trade Sales", C. W. Seeker, 4-9-54. Memorandum Report No. M-746, "Universal Tinting Bases", C. W. Seeker and H. R. Heickel, 12-10-54. Memorandum Report No. SM-61-8, 'Recent Technology Related to Pigment Dispersions, Color Development, and Surface Active Agents", J. J. Kilkeary, 3-21-61. Memorandum Report No. SM-61-9, 'Formulating Techniques Used in Universal Pigment Dispersions", J. J. Kilkeary, 4-4-61. DUP030005981