Marketing Bulletin SILSOFT * AX SPECIALTY FLUIDS - PERSONAL CARE INCI Designation: Bis-Cetearyl Amodimethicone Silsoft AX, an alkyl modified amino fluid, can help consumers achieve thermal protection, superior smoothness and shine for dry hair. The combination of both pendant amino and terminal alkyl groups on the silicone structure help provide enhanced thermal protection, smoothness, softness and manageability. Key Features and Typical Benefits thermal protection outstanding smoothness not sticky or greasy shine without greasiness superior and manageability excellent for straight, sleek look color retention hair strengthening Typical Physical Properties (1) Appearance Translucent, pale yellow Active Content, % 100 Viscosity, mpa s 5,000-0,000 Amino Content Nwt % 0.1-0.3 (1) Typical data are average data. The actual data may vary. Product specifications for specific applications need to be agreed upon individually. Potential Applications Hair Care products to provide thermal protection products to smooth hair: leave-on conditioners shampoos rinse-off conditioners serum shine spray Other body wash liquid hand soap bar soap ethnic hair care products for color protection
Chemistry Silsoft AX is an alkyl modified amino silicone fluid. Alkyl Silicone Sensory Low Friction Alkyl Amino Anchoring to hair Electrostatic interaction Terminal Alkyl Group Interaction with hydrophobic materials (lipids, organic oils, etc.) Moisture barrier Anchoring to hair The combination of both pendant amino and terminal alkyl groups on the silicone structure help provide enhanced thermal protection, smoothness, softness and manageability. Performance Data Thermal Protection Performance Hair that is shiny and manageable is an indication that it is healthy. This is highly desirable by today s consumer. Everyday styling practices such as blow drying, hot curling and straightening with irons generate a great deal of heat. These styling appliances strip the hair of moisture leaving it brittle and dry and damage from heat is one of the main reasons why hair breaks. Most experts recommend limiting the use of flat irons on the hair to once a week, but this may be unrealistic for women who like to wear their hair straight. Using appropriate thermal protection may help protect hair from damage from flat irons. 1 - TGA (Thermal Gravimetric Analysis) Silicone fluids are unique materials and have a backbone of silicone-oxygen linkages similar to the linkages of high temperature inorganic materials such as quartz, glass and sand. This molecular backbone is much stronger than typical organic chains and more resistant to attack by temperature extremes. TGA was conducted to compare the thermal stability of Silsoft AX alkyl modified amino silicone, to other organic materials often found in thermal protection formulations. 100 90 80 Weight Loss (%) 70 60 50 0 30 0 10 0 0 100 00 300 00 500 Petrolatum Polyisobutene Isopropylmyristate Silsoft AX Temperature As shown by thermal gravimetric analysis, Silsoft AX was thermally stable over the temperature range for home-use hair irons (up to 180 C), as well as professional hair irons (up to 50 C). Page of 1
- Severe straightening test Damp Hair with Flat Iron. Daily styling practices can cause extensive damage to the cuticle, causing it to crack, buckle and lift. Damaged cuticles cause the hair to look dull, lifeless and frizzy. In a severe straightening test, heat was applied to damp hair with a flat iron until dry in order to distinguish differences between thermal protection ingredients. The photographs of the straightened tresses correlate with the SEM images in section 3 below and illustrate the film forming effects of Silsoft AX and the cuticle protection that it provided. Before Iron After Iron Initial Water Water Water + heat + Amodimethicone + Silsoft AX + heat + heat Protocol: 1. Frizziness process: Platinum bleached tress dipped for 1 min in 0.5% NaOH bath, rinsed, blown dry. Protection treatment: Dipped 1 min in 1% Si active* in water, prepared from a silicone emulsion. Squeeze excess liquid, iron 3. With iron at medium heat (130 C), pass hair through iron several times until dry (5-7 min) Silsoft AX helped protect hair from heat damage in the presence of water and reduced frizz. 3 - SEM imaging for bleached hair Water Water Water + Amodimethicone + Silsoft AX Initial + heat + heat + heat Silsoft AX helped prevent cuticle lift, by forming a protective film. Note: Test results. Actual results may vary. Page 3 of 1
- Tensile test on damaged hair The by product of hair damage includes the loss of elasticity; the degree to which hair is damaged correlates to the force needed to break the hair fiber. The tensile property of hair is used to measure the extent of thermal damage. The same overworked tresses that were exposed to the severe hair straightening protocol detailed in section above were evaluated to determine if there was any loss of strength and if a treatment could prevent the damage from occurring. These graphs demonstrated trending that indicated that Silsoft AX reduced premature breaking and break strength loss generated by the ironing process. Break Strength (gmf/sq micron) 0.016 0.0155 0.015 0.015 0.01 0.0135 0.013 0.015 ADM = amodimethicone Initial Water+heat Water+ADM Water+ +heat Silsoft AX +heat % Premature Break 0 18 16 1 1 10 8 6 0 Initial Water+heat Water+ADM Water+ +heat Silsoft AX +heat 5 - Breakage test Simple brushing and combing can cause significant breakage of damaged hair. Used prior to heat styling, Silosft AX helped protect the hair from heat damage and reduced the force required to comb the hair. Tress Damage: g Platinum bleached tresses were treated with 0.5% NaOH for 1 minute, rinsed and blown dry. Treatment: Tresses were dipped for 1 minute in 1% active silicone bath, and excess liquid was squeezed out. Iron: Tresses were ironed at constant speed and constant pressure at temperature 15 C until almost dry. Breakage Test: After ironing, tresses were left at room temperature overnight. Tress was held vertically and combed manually with a coarse comb 5 times each side. Broken fibers were collected on an aluminum foil below the tress. Total weight of broken fibers was recorded on a precision balance. Hair Breakage (weight gms) 0.0 0.035 0.03 0.05 0.0 0.015 0.01 0.005 0 Water 1% Amodimethicone 1% Silsoft AX Reduction of hair breakage observed with Silsoft AX treatment was likely due to the protected cuticle layer and lowered friction. Note: Test data. Actual results may vary. 6 - Hydrophobicity test Healthy undamaged hair is hydrophobic. When it is damaged it becomes hydrophilic. If a product can restore hair to a more hydrophobic state, it is often concluded that hair is healthier. A simple wicking test was used to measure hydrophobicity before and after treatments and the change in wicking time is represented in the figure below. The surface hyrdophobicity of the bleached hair fibers was improved after treatment with Silsoft AX, restoring damaged bleached hair to what appears to be a more natural or healthy state. Protocol: Hydrophobicity test: 1) A bleached hair tress was dipped in a silicone dispersion prepared from an emulsion. The tress was dried, washed with a 10% SLES solution and dried again. ) Several deionized water droplets were deposited on a bleached hair tress held flat and taut in a clamp. 3) A record was kept of the time required for the droplets to wick into the hair tress. Treatment Wicking concentration time after of silicone 1 wash (s) No silicone 0 <10 Amodimethicone 0.3% 10 Silsoft AX 0.3% >300 The excellent thermal performance effect of Silsoft AX could be due to its very good spreading and lubricating properties, and also to its ability to form a very hydrophobic film. Page of 1
7 - Frizz test Non-aqueous spray Treatment (A).5% Silsoft AX in cyclomethicone. Control= spray with cyclomethicone. Iron: temperature 05 ºC, 5 passes After 1 wash w 10% SLES and blow dry With With Control Silsoft AX Control Silsoft AX 1 wash w 10% SLES, blow dry And 30 min in humidity chamber at 90% RH With With Control Silsoft AX Control Silsoft AX Silsoft AX helps reducing frizz at high humidity. 8 - Conditioning Evaluations were conducted on undamaged and damaged hair. Preparation of Damaged Hair: Undamaged hair was immersed twice in a 6% hydrogen peroxide solution at ph 9.5 (ph adjusted with ammonia) for hours each time, followed by washing and drying. Products Tested Modification Viscosity % Active Silsoft AX Alkyl and amino 5,000-0,000 mpas 100% XF-B1989 Low vis. high amino 600-1,00 mpas 100% Silicone Wax A (1) C18 Alkyl dimethicone (Softening point: 0 C) 100% SME 53 silicone High amino 150-500 mpas 0% () (1) Silicone Wax A: MD500DR500M where M = (CH 3 ) 3 Si-O1/, D = (CH 3 ) Si-O-, DR = (CH 3 ) (C 18 H 37 )Si-O- () Micro-emulsion in water Note: Test results. Actual results may vary. Page 5 of 1
1. Controlled Deposition Dry Combing Test Method (1) Prepared D 5 solution containing 0.5 wt% of tested product. Used Isoparaffin for Silicone Wax A () Washed damaged hair tresses with non-silicone shampoo and dried (3) Uniformly treated the 9 gram-hair tress with 1.5 gram of solution and dried Control: Damaged hair treated with D 5 Sensory at Dosage Levels Test Method (1) Prepared D 5 solutions containing 0.5 wt% and 1.0 wt% of tested product. Used Isoparaffin for Silicone Wax A () Washed hair tress with non-silicone shampoo and dried (3) Uniformly treated the 9 gram-hair tress with 1.5 gram of solution and dried () Evaluated sensory of each hair tress Dosage Results 5 Dosage 0.5 wt% () Measured dry combing force of hair tress with combing tester Dry Combing Results Reduction of Dry Combing Force (%) 80.0 70.0 60.0 50.0 0.0 30.0 0.0 10.0 0.0 Silsoft AX XF-B1989 Silicone Wax A Undamaged Damaged Score 3 5 Silsoft AX XF-B1989 Wax A Smoothness Softness Dosage 1 wt% Sensory Panelists evaluated the sensory of each hair tress. The 3.0 sensory score of XF-B1989 was fixed as the standard; the other products were scored accordingly. Score 3 Sensory Results Not Greasy Smoothness 6 0 Less Fly Away Softness Silsoft AX XF-B1989 Wax A Smoothness Softness As a specialty product, Silsoft AX provided superior smoothness and softness. Comparatively, the aminosilicones resulted in a greasier, heavier sensory when dosage was increased. Silsoft AX XF-B1989 Silicone Wax A Note: Test data. Actual results may vary. Silsoft AX provided excellent hair manageability, softness and smoothness, without greasiness. Page 6 of 1
1. Rinse-Off Conditioner Dry Combing Test Method (1) Dry combing Techno Hashimoto combing tester. Measurement was an average of 10 comb passes. Ingredient Wt/wt% Steartrimonium (8% active) 7.1 Stearyl Alcohol Silicone Water qsp. 100 Dry Combing Results 70.0 Dry Combing Force Reduction (%) 60.0 50.0 0.0 30.0 0.0 10.0 0.0 Wet Friction Test Method 1) After application of conditioner and rinsing (standard protocol) excess water was squeezed between fingers ) Tresses mounted flat on the friction apparatus (TMI) 3) Normal load was 00g. Data are an average of 6 measurements (tress duplicate with 3 slider passes) Wet Friction Results 0.7 Coefficient of Wet Friction 0.6 0.5 0. 0.3 0. 0.1 0.0 Silsoft AX XF-B1989 Silicone Wax A Undamaged Damaged Control Silsoft AX Silicone Wax A XF-B1989 Undamaged Damaged Silsoft AX, when used in a rinse-off conditioner, significantly improved wet and dry combing of undamaged and damaged hair. Control: Conditioner without silicone Note: Test data. Actual results may vary. Sensory Test Method 1) Prepared conditioner containing % active silicone ) Uniformly applied g of conditioner after immersing 10g (30cm length) into 0 C bath 3) Rinsed hair tress in 0 C warm bath for 10 seconds. Repeated 3 times ) Dried the hair tress 5) Evaluated sensory of each hair tress Ingredient Wt/wt% Silsoft AX Mineral Oil 1 Cetearyl Alcohol 1 Stearyl Alcohol 1 Streartrimonium Chloride, 8% Glycerin 3 Preservative Per manufacturer s label Water q.s. Sensory Results Score Score 5 3 5 3 Damaged Hair Silsoft AX XF-B1989 Wax A Smoothness Softness Damaged Hair Silsoft AX XF-B1989 Wax A Smoothness Softness Silsoft AX significantly improved smoothness and softness of undamaged and damaged hair. Product formulations are included as illustrative examples only. Momentive makes no representation or warranty of any kind with respect to any such formulations, including, without limitation, concerning the efficacy or safety of any product manufactured using such formulations. Page 7 of 1
9 - Comparison to Silicone Quat on Undamaged Hair Sensory Test Procedure 10 - Comparison to Silicone Quat on Damaged Hair Sensory Test Procedure Conditioner: % active silicone Conditioner: % active silicone Hair Tresses: Undamaged hair, 10gram, 0cm length Hair Tresses: Undamaged hair, 10gram, 0cm length Sensory: 5 trained panelists Sensory: 5 trained panelists Silsoft Q quat silicone Silsoft AX Silsoft Q quat silicone Silsoft AX Silsoft AX delivered sleekness. Silsoft Q quat silicone provided volume without flyaway. Silsoft AX delivered sleekness. Silsoft Q quat silicone provided volume without flyaway. 11 - Shine Spray: Comparison to Silicone Benchmark Test Procedure 1) Single bleached hair was sprayed and spray amount recorded by weight ) Tresses blow dried 3) Measurement of diffuse reflectance used Murakami Spectrogoniophotometer ) Gloss Contrast = (S-D)*100/S with S specular reflectance (max value) and D diffusive reflectance at 0 viewing angle 80 70 Contrast Gloss (%) 60 50 0 30 0 0 0.0 0.0 0.06 0.08 0.1 0.1 Spray (g/ g hair) Commercial Benchmark Non-aqueous spray w/ Silsoft AX Aqueous tonic spray w/ Silsoft AX Note: Test results. Actual results may vary. Page 8 of 1
Untreated Treated with silicone benchmark Untreated Treated with Silsoft AX Shine level obtained with Silsoft AX was comparable to shine level of commercial benchmark at similar dose. In addition to comparable shine, the Silsoft AX tress had a better, non-greasy look and combed smoothly. Silsoft AX can be delivered from non-aqueous and aqueous sprays. 1 - Color Retention Test Method 1) 6 g single bleached tresses dyed with well-known commercial red hair dye; contact time 30 min ) Tresses rinsed, shampooed with the test shampoo (standard protocol), blow dried 3) L*, A*, b* measured with a spectrogoniophotometer (baseline value) ) Tresses washed 3 times with test shampoo, color measured 5) Tresses washed 3 more times with test shampoo, color measured 6) Control was the SLES/CAPB shampoo without silicone 7) Each result was an average of tresses 1% in a SLES/CAPB Shampoo Formulation Color Retention Results 8 Total Color Change (DE*) 7 6 5 3 1 0 3X Control 6X Silsoft AX About 0% improvement of color retention from the shampoo base. Note: Test results. Actual results may vary. Inc. Page 9 of 1
13 - Sample Formulae Cationic Conditioner Procedure 1. Heat water to 70 C and add Behenamidopropyl Dimethylamine while agitating at 600 rpm. Mix until melted and homogeneous.. Add the lactic acid while continuing to agitate. 3. Add the cetearyl alcohol, and mix until melted and homogeneous. Continue to mix for 30 minutes at 70 C.. Cool mixture, 10 C every 30 minutes. Increase agitation slowly as viscosity increases until temperature reaches 0 C. 5. Add Silsoft AX emulsion and mix at 1000 rpm until homogeneous. Continue to agitate until temperature reaches ambient. Ingredients Wt/wt% Behenamidopropyl Dimethylamine 1.7 Cetearyl Alcohol 3.3 Lactic Acid 0.5 Silsoft AX 1. Water q.s. 100 Non-Ionic Conditioner Procedure 1. Heat water to 70 C.. Add wax component while agitating at 00 rpm. Mix until homogeneous. 3. Cool to 0 C while mixing.. Add emulsion of Silsoft AX. 5. Increase agitation to 600 rpm and cool to room temperature. Ingredients Wt/wt% Glyceryl stearate (and) ceteareth-0 10 (and) ceteareth-1 and cetearyl alcohol and cetyl palmitate Silsoft AX 1. Water q.s. 100 Non-aqueous Hair Shine Spray ~ 6% non-volatile Ingredients Wt/wt% Silsoft AX.5 Light Mineral Oil 1.5 Cyclopentasiloxane 9 Non-aqueous Commercial Hair Shine Spray Benchmark ~ 7.% non-volatile Ingredients: alcohol denat., cyclopentasiloxane, bis-phenylpropyl dimethicone, dimethicone, C1-15 alkyl benzoate, benzophenone-3, fragrance. Product formulations are included as illustrative examples only. Momentive makes no representation or warranty of any kind with respect to any such formulations, including, without limitation, concerning the efficacy or safety of any product manufactured using such formulations. Inc. Page 10 of 1
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