Abstract:
The present invention relates to a composition, process for preparation and use of a novel emulsion composition in the personal care industry. The composition when applied to hair provides outstanding lubrication, and delivers amino acids or proteins to the hair fiber. This aides in the manageability of the hair and remediates damage from treatment processes like permanent waving, dying and relaxing of the hair as well as environmental effects upon the hair.

Description:
DESCRIPTION OF THE ART AND PRACTICES 
     Silicone oils (dimethylpolysiloxane) have been known to be active at the surface of plastic, cellulosic and synthetic fibers as well as hair. Despite the fact that they are lubricants that are stable to oxidation, their high cost and lack of durability has made them cost prohibitive in most application areas. 
     The low efficiency of silicone oils is due to the fact that the oil is very water insoluble. Emulsions are generally prepared which contain silicone dispersed in micelles. While this method of application is easier for processing, much of the oil stays in the surfactant micelle and never gets deposited on the fiber. That which does deposit on the fiber surface remains there by hydrophobic binding, not ionic bonding. Since the polydimethylsiloxane is not in an ionic bonded the effect is very transient. The product is removed with one washing. 
     It is highly desirable to be able to deliver a silicone to the surface of the hair in a stable aqueous composition which will upon drying polymerize on the hair making a crosslinked network and one which will react an amino acid or protein to the hair&#39;s surface as part of the silicone matrix. It was not until the compounds of the present invention that this was possible. 
     THE INVENTION 
     The present invention relates to a composition, process for preparation and use of a novel emulsion composition in the personal care industry. The composition when applied to hair provides outstanding lubrication, and delivers amino acids or proteins to the hair fiber. This aides in the manageability of the hair and remediates damage from treatment processes like permanent waving, dying and relaxing of the hair as well as environmental effects upon the hair. 
     The compositions of the present invention are emulsions. These emulsions are applied to the hair surface preferably in a conditioner. The emulsion breaks causing the deposition of a uniform coating of composition of the current invention. 
     The emulsion composition is reactive after the water is removed. The composition is made up of a silanol, a alkoxy silicone and a nitrogen containing material, preferably an amino compound. The amino compound catalyses the reaction between the silanol hydroxyl group, the alkoxy group and the amino group. The result is a highly branched covalently bonded amino functional silicone polymer. 
     The compositions of the present invention are stable emulsions. These emulsions are applied to the hair surface whereupon they polymerize on the hair and provide conditioning and delivery of amino acids to the hair. 
     OBJECT OF THE INVENTION 
     It is the objective of the present invention to provide a composition which is a stable emulsion containing (a) a silanol, (b) an alkoxy silicone crosslinking agent, (c) a water soluble amino compound, preferably an amino acid or protein, (d) an emulsifier and (e) water. The composition polymerizes upon dry down. The silanol is the linear source of silicone, the alkoxy silicone compound provides crosslinking, the amino compound is the necessary catalyst for the reaction, the emulsifier is needed to provide a stable emulsion, and water is necessary as a diluting solvent, so that the polymerization does not occur before contact with the hair. 
     It is also another objective of the invention o provide a process for treating the hair which comprises the contacting of the hair with an effective conditioning amount of the above composition, allowing the contacted hair to dry and in a preferred embodiment, applying heat from a blow drier to accelerate the crosslinking. 
     SUMMARY OF THE INVENTION 
     The invention discloses a stable emulsion containing (a) a silanol, (b) an alkoxy silicone crosslinking agent, (c) a water soluble amino compound, preferably an amino acid or protein, (d) an emulsifier and (e) water. The composition polymerizes upon dry down. The silanol is the linear source of silicone, the alkoxy silicone provides crosslinking, the amino compound is the necessary catalyst for the reaction, the emulsifier is needed to provide a stable emulsion, and water is necessary as a diluting solvent, so that the polymerization does not occur before contact with the hair. 
    
    
     DETAILED DESCRIPTION OF THE INVENTION 
     The compositions of the present invention are made up of the following critical components: 
     a) an alkoxy silicone compound conforming to the following structure: ##STR1## Me is methyl; R is alkyl having one to ten carbon atoms; 
     R&#39; is methyl or ethyl; 
     a is an integer ranging from 1 to 12. 
     b) A silanol conforms to the following structure: ##STR2## Me is methyl and a ranges from 1 to 2,000. 
     3) An amino compound 
     The amino source of choice is an amino acid, or a protein. Proteins are materials which play a critical role in all biological processes. They are natural products and have enjoyed increasing use in personal care products as conditioners, humectants and softeners. Natural proteins, which are high molecular weight polymers, are generally hydrolyzed into lower molecular weight proteins to obtain water solubility. The water solubility results in easier formulating, but the soluble proteins are less substantive to hair and skin. Consequently, the water soluble proteins end up washed off the substrate being treated. The compounds of the present invention are far more substantive since they have silicone in the molecule. Not only is the silicone more substantive to the skin and hair, the presence of alkylene oxide in the silicone polymer in a preferred embodiment results in a protein with an inverse cloud point. The silicone protein becomes insoluble above this temperature and is more substantive to the hair and skin. This suggests the use of these materials in treatment products were heat is applied, like hot oil treatments. 
     Amino acids are the basic structural units of proteins. An amino acid has both an amino group and a carboxyl group. ##STR3## 
     The amino acids are well known to those skilled in the art. They are: 
     
         ______________________________________Amino Acids______________________________________Alanine        Arginine    AsparagineAspartic Acid  Glutamine   GlycineHistidine      Isoleucine  LeucineLysine         Methionine  PhenylalanineProline        Serine      ThreonineTryptophan     Tyrosine    Valine______________________________________ 
    
     In proteins the carboxyl group of one amino acid is joined to the carboxyl group of another amino acid in an amide bond. When this aide bond is in a protein it is called a peptide bond. Many amino acids are joined in peptide bonds to form a polypeptide chain. This polypeptide chain is what we commonly call a protein. The polypeptide has a free amino group and a free carboxyl group present. ##STR4## s is an integer from 0 to 5,000, giving the protein a molecular weight up to 500,000 EMWU (EMWU is equivalent molecular weight units) 
     The compounds of the present invention are dependant upon the reaction of the terminal amino group in the protein with a reactive silicone intermediate which results in functionalizing of the amino group. 
     It will be clearly understood that the &#34;polypeptide bonded amino acids can be any combination of the amino acids listed above in any order. 
     4) Emulsifying agent(s) 
     In a preferred embodiment composition contains a nonionic emulsifier which has a HLB ranging from 8 to 10. 
     Examples of emulsifiers which are useful are; 
     
         ______________________________________Trade name   HLB      Description______________________________________Neodol 23-3  8        C.sub.12 H.sub.24 O--(CH.sub.2 CH.sub.2 --O).sub.3                 H                 3 mole ethoxylateAlkasurf DA-3        9        C.sub.10 H.sub.22 O--(CH.sub.2 CH.sub.2 --O).sub.3                 H                 3 mole ethoxylateAlkasurf NP-5        10       Nonylphenol 5 mole ethoxylate50/50 blend of        9.5      Secondary Alcohol ethoxylatesTergitol 15-S-3       having three and five moles EOand Tergitol 15-S-5______________________________________ 
    
     NEODOL is a trademark of Shell chemical 
     ALKASURF is a trademark of Alkaril Chemicals Inc. 
     TERGITOL is a trademark of Union Carbide Chemical 
     and 
     5) Water 
     EXAMPLES 
     Raw Materials 
     The raw materials useful in the preparation of the compounds of the present invention are listed below and have been designated as RM-1 through RM-36. That stands for Raw Material Example 1 through Raw Material Example 36. 
     1) Alkoxy Silicone Compounds 
     The silicone compounds useful for the preparation of the compounds of the present invention were provided by Siltech Inc. and conform to the following structures: ##STR5## Me is methyl; R is alkyl having one to ten carbon atoms; 
     R&#39; is methyl or ethyl; 
     a is an integer ranging from 0 to 12. 
     The following compounds are commercially available from Siltech Inc. of Norcross, Ga.; 
     
         ______________________________________SiliconeExample      R         R&#39;       a______________________________________RM-1         CH.sub.3  CH.sub.3 0RM-2         CH.sub.3  CH.sub.2 CH.sub.3                           8RM-3         CH.sub.3  CH.sub.3 12RM-4         C.sub.4 H.sub.9                  CH.sub.3 4RM-5         C.sub.4 H.sub.9                  CH.sub.2 CH.sub.3                           12RM-6         C.sub.8 H.sub.17                  CH.sub.3 4RM-7         C.sub.8 H.sub.17                  CH.sub.2 CH.sub.3                           0RM-8         CH.sub.3  CH.sub.3 2RM-9         CH.sub.3  CH.sub.2 CH.sub.3                           0RM-10        CH.sub.3  CH.sub.3 2RM-11        C.sub.4 H.sub.9                  CH.sub.3 2RM-12        C.sub.4 H.sub.9                  CH.sub.2 CH.sub.3                           0RM-13        C.sub.4 H.sub.9                  CH.sub.3 0RM-14        C.sub.4 H.sub.9                  CH.sub.2 CH.sub.3                           0______________________________________ 
    
     2) Silanol Compounds 
     Silanol compounds are well known and are marketed in the trade under many names. The compounds conform to the following generic structure; ##STR6## Me is methyl and c ranges from 1 to 2,000. 
     Compounds conforming to the above structure are available from Siltech Inc. Norcross Ga. and are marketed under the Siltech S series tradename shown; 
     
         ______________________________________Example   Name       Molecular Weight                            Value of &#34;c&#34;______________________________________RM-15     Siltech S 700                  500        4RM-16     Siltech S 701                 1,000       11RM-17     Siltech S 706                 6,000       79RM-18     Siltech S 710                10,000      133RM-19     Siltech S 750                50,000      673RM-20     Siltech S 790                86,000      1160RM-21     Siltech S HV                150,000     2000______________________________________ 
    
     3) Amino Acids 
     Examples of Amino acids are: 
     
         ______________________________________Example             Amino Acid______________________________________RM-22               AlanineRM-23               ArginineRM-24               AsparagineRM-25               Aspartic AcidRM-26               GlutamineRM-27               GlycineRM-28               HistidineRM-29               IsoleucineRM-30               LeucineRM-31               LysineRM-32               MethionineRM-33               PhenylalanineRM-34               ProlineRM-35               SerineRM-36               ThreonineRM-37               TryptophanRM-38               TyrosineRM-39               Valine______________________________________ 
    
     Examples of proteins are: 
     Proteins useful in the preparation of the products of the present invention are derived from many sources. Many are prepared by the hydrolysis of native proteins. The hydrolysis results in cleavage of some of the polypeptide bonds and increases water solubility. The hydrolysis processes are either acid, alkaline or enzymatic and are well known to those skilled in the art. 
     Soya Protein (CAS number 68153-28-6); Milk Protein (CAS number 9000-71-9); Wheat Protein; Oat Protein; Vegetable Protein; Keratin Protein (CAS Number 68238-35-7); Placental Protein and Collagen are all sources from which protein is derived. 
     The proteins useful in the preparation of the compounds of the present invention, in a preferred embodiment range in molecular weight from 1,000 equivalent molecular weight units to 500,000 equivalent molecular weight units. The equivalent molecular weight units are determined by calculation of the free amino groups. An analysis called the &#34;amine value&#34; is run using a standardized acid titrant. The titrations are well known to the fatty chemist and are determined as follows; ##EQU1## 
     The amine value is expressed in mg KOH/gm. The amine value is then converted into equivalent molecular weight using the following formula; ##EQU2## 
     
         ______________________________________Example Number      Commercial Name  Equivalent weight______________________________________RM-40      Peptin 2,000     2,054 EMWURM-41      Peptin 5,000     5,010 EMWURM-42      Polypro 15,000   14,980 EMWURM-43      Peptin AH        1,500 EMWURM-44      Sollagen         275,000 EMWURM-45      Wheat Protein (Hydrolyzed)                         500 EMWURM-46      Wheat Protein    2,505 EMWURM-47      Oat Protein      5,560 EMWURM-48      Soya Protein     15,625 EMWURM-49      Collagen         500,120 EMWURM-50      Placental Protein                       50,450 EMWU______________________________________ (Peptin, Polupro, and Sollagen are Trademarks of Hormel) (Samples obtained from Phoenix Chemical Inc.) 
    
     4) Emulsifiers 
     Examples of emulsifiers which are useful are; 
     
         ______________________________________Example  Trade name   HLB    Description______________________________________RM-51  Neodol 23-3  8      C.sub.12 H.sub.24 O--(CH.sub.2 CH.sub.2                      --O).sub.3 H                      3 mole ethoxylateRM-52  Alkasurf DA-3               9      C.sub.10 H.sub.22 O--(CH.sub.2 CH.sub.2).sub.3                      H                      3 mole ethoxylateRM-53  Alkasurf NP-5               10     Nonylphenol 5 mole                      ethoxylateRM-54  50/50 blend of               9.5    Alcohol ethoxylates  Tergitol 15-S-3     having three and five moles EO  and Tergitol 15-S-5______________________________________ 
    
     COMPOUNDS OF THE PRESENT INVENTION 
     General Procedure 
     To enough water to adjust the solids to 60% by weight of the total formulation is added the specified amount of surfactants under agitation. Mix well about 15 minutes. Slowly add the specified amount of the specified silanol under good agitation over a one hour period. Slowly add the specified amount of alkoxy silicone over a one hour period. Add the specified amount of the specified amino acid or protein. Mix one hour after all ingredients have been added. Homogenize in a Matin Gaulin Homogenizer at 6,000 psi. Allow to cool under agitation. The resulting emulsion is used as prepared. 
     The calculation of the amount of water to add is: ##EQU3## So for example 1; A=250.0+70.0+5.0+89.0=414.0 
     Water to Add=(414.0/0.60)-414.0=276.0 gm 
     Emulsions were prepared using the above procedure and the following formulations; 
     EXAMPLES 1-29 
     
         __________________________________________________________________________      Alkoxy          AminoEx  Silanol  Silicone              Emulsifier                      Source# Type Grams      Ex. #          Grams              Ex. #                  Grams                      Ex. #                          Grams__________________________________________________________________________ 1  RM15 250.0      RM1 70.0              RM51                  5.0 RM22                          89.0 2  RM16 500.0      RM2 1320.0              RM52                  5.0 RM23                          174.2 3  RM17 3000.0      RM3 1892.0              RM53                  4.0 RM24                          132.1 4  RM18 5000.0      RM4 720.0              RM54                  3.0 RM25                          133.1 5  RM19 25000.0      RM5 1920.0              RM51                  5.0 RM26                          146.1 6  RM20 43000.0      RM6 786.0              RM52                  5.0 RM27                          75.0 7  RM21 7S000.0      RM7 186.0              RM53                  5.0 RM28                          155.2 8  RM15 250.0      RM8 120.0              RM54                  5.0 RM29                          131.2 9  RM16 500.0      RM9 100.0              RM51                  5.0 RM30                          131.210  RM17 3000.0      RM10          400.0              RM52                  5.0 RM31                          146.211  RM18 5000.0      RM11          420.0              RM53                  5.0 RM32                          149.212  RM19 25000.0      RM12          120.0              RM54                  5.0 RM33                          165.213  RM20 43000.0      RM13          120.0              RM54                  5.0 RM34                          115.114  RM21 75000.0      RM14          120.0              RM52                  5.0 RM35                          105.115  RM15 250.0      RM14          120.0              RM53                  5.0 RM36                          119.116  RM16 500.0      RM1 70.0              RM51                  3.0 RM37                          204.317  RM17 3000.0      RM13          120.0              RM51                  3.0.                      RM38                          181.918  RM18 5000.0      RM12          80.0              RM52                  3.0 RM39                          117.119  RM19 25000.0      RM11          280.0              RM53                  3.0 RM40                          2054.020  RM20 43000.0      RM10          290.0              RM54                  3.0 RM41                          5010.021  RM21 75000.0      RM9 50.0              RM51                  3.0 RM42                          14980.022  RM15 250.0      RM8 60.0              RM52                  4.0 RM43                          1500.023  RM16 500.0      RM7 100.0              RM53                  4.0 RM44                          275000.024  RM17 3000.0      RM6 395.0              RM54                  4.0 RM45                          500.025  RM18 5000.0      RM5 1000.0              RM51                  4.0 RM46                          2505.026  RM19 25000.0      RM4 360.0              RM52                  4.0 RM47                          5560.027  RM20 43000.0      RM3 946.0              RM53                  4.0 RM48                          15625.028  RM21 75000.0      RM2 660.0              RM54                  4.0 RM49                          500120.029  RM21 75000.0      RM2 660.0              RM54                  4.0 RM50                          50450.0__________________________________________________________________________ 
    
     General Procedure 
     To enough water to adjust the solids to 35% by weight of the total formulation is added the specified amount of surfactants under agitation. Mix well about 15 minutes. Slowly add the specified amount of the specified silanol under good agitation over a one hour period. Slowly add the specified amount of alkoxy silicone over a one hour period. Add the specified amount of the specified amino acid or protein. Mix one hour after all ingredients have been added. Homogenize in a Matin Gaulin Homogenizer at 6,000 psi. Allow to cool under agitation. The resulting emulsion is used as prepared. 
     The calculation of the amount of water to add is: 
     A=Weight in grams of (silanol+Alkoxy Silane+Emulsifier+Amino) 
     Water to Add=(A/0.35)-A 
     So for example 30; 
     A=250.0+70.0+5.0+89.0=414.0 
     Water to Add=(414.0/0.35)-414.0=768.8 gm 
     Emulsions were prepared using the above procedure and the following formulations; 
     EXAMPLES 30-59 
     
         __________________________________________________________________________      Alkoxy          AminoEx  Silanol  Silicone              Emulsifier                      Source# Type Grams      Ex. #          Grams              Ex. #                  Grams                      Ex. #                          Grams__________________________________________________________________________30  RM15 250.0      RM1 70.0              RM51                  5.0 RM22                          89.031  RM16 500.0      RM2 1320.0              RM52                  5.0 RM23                          174.232  RM17 3000.0      RM3 1892.0              RM53                  4.0 RM24                          132.133  RM18 5000.0      RM4 720.0              RM54                  3.0 RM25                          133.134  RM19 25000.0      RM5 1920.0              RM51                  5.0 RM26                          146.135  RM20 43000.0      RM6 786.0              RM52                  5.0 RM27                          75.036  RM21 75000.0      RM7 186.0              RM53                  5.0 RM28                          155.238  RM15 250.0      RM8 120.0              RM54                  5.0 RM29                          131.239  RM16 500.0      RM9 100.0              RM51                  5.0 RM30                          131.240  RM17 3000.0      RM10          400.0              RM52                  5.0 RM31                          146.241  RM18 5000.0      RM11          420.0              RM53                  5.0 RM32                          149.242  RM19 25000.0      RM12          120.0              RM54                  5.0 RM33                          165.243  RM20 43000.0      RM13          120.0              RM54                  5.0 RM34                          115.144  RM21 75000.0      RM14          120.0              RM52                  5.0 RM35                          105.145  RM15 250.0      RM14          120.0              RM53                  5.0 RM36                          119.146  RM16 500.0      RM1 70.0              RM51                  3.0 RM37                          204.347  RM17 3000.0      RM13          120.0              RM51                  3.0 RM38                          181.948  RM18 5000.0      RM12          80.0              RM52                  3.0 RM39                          117.149  RM19 25000.0      RM11          280.0              RM53                  3.0 RM40                          2054.050  RM20 43000.0      RM10          290.0              RM54                  3.0 RM41                          5010.051  RM21 75000.0      RM9 50.0              RM51                  3.0 RM42                          14980.052  RM15 250.0      RM8 60.0              RM52                  4.0 RM43                          1500.053  RM16 500.0      RM7 100.0              RM53                  4.0 RM44                          275000.054  RM17 3000.0      RM6 395.0              RM54                  4.0 RM45                          500.055  RM18 5000.0      RM5 1000.0              RM51                  4.0 RM46                          2505.056  RM19 25000.0      RM4 360.0              RM52                  4.0 RM47                          5560.057  RM20 43000.0      RM3 946.0              RM53                  4.0 RM48                          15625.058  RM21 75000.0      RM2 660.0              RM54                  4.0 RM49                          500120.059  RM21 75000.0      RM2 660.0              RM54                  4.0 RM50                          50450.0__________________________________________________________________________ 
    
     Applications Results 
     The compounds of the present invention, when applied to the hair and allowed to dry, provide conditioning, softening and improvement to damaged hair.