Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/0005—Other compounding ingredients characterised by their effect
  • C11D3/0084—Antioxidants; Free-radical scavengers
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/38—Cationic compounds
  • C11D1/62—Quaternary ammonium compounds
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/40—Dyes ; Pigments
  • C11D3/42—Brightening agents ; Blueing agents
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
  • D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
  • D06L4/60—Optical bleaching or brightening
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
  • D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
  • D06L4/60—Optical bleaching or brightening
  • D06L4/614—Optical bleaching or brightening in aqueous solvents
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06L—DRY-CLEANING, WASHING OR BLEACHING FIBRES, FILAMENTS, THREADS, YARNS, FABRICS, FEATHERS OR MADE-UP FIBROUS GOODS; BLEACHING LEATHER OR FURS
  • D06L4/00—Bleaching fibres, filaments, threads, yarns, fabrics, feathers or made-up fibrous goods; Bleaching leather or furs
  • D06L4/60—Optical bleaching or brightening
  • D06L4/657—Optical bleaching or brightening combined with other treatments, e.g. finishing, bleaching, softening, dyeing or pigment printing
• • D—TEXTILES; PAPER
  • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
  • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
  • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
  • D06M2200/25—Resistance to light or sun, i.e. protection of the textile itself as well as UV shielding materials or treatment compositions therefor; Anti-yellowing treatments

Definitions

• the present invention relates to a method of improving the sun protection factor (SPF) of textile fibre material comprising treating the textile fibre material with a composition comprising at least one fluorescent whitening agent which absorbs radiation in the wavelength range 280-400 nm.
• SPF sun protection factor
• wavelengths 280-400 nm permits tanning of the epidermis.
• rays of wavelengths 280-320 nm (termed UV-B radiation), cause erythemas and skin burning which can inhibit skin tanning.
• UV-A radiation Radiation of wavelengths 320-400 nm (termed UV-A radiation) is known to induce skin tanning but can also cause skin damage, especially to sensitive skin which is exposed to sunlight for long periods. Examples of such damage include loss of skin elasticity and the appearance of wrinkles, promotion of the onset of erythemal reaction and the inducement of phototoxic or photoallergic reactions.
• Any effective protection of the skin from the damaging effects of undue exposure to sunlight clearly needs to include means for absorbing both UV-A and UV-B components of sunlight before they reach the skin surface.
• One aspect of the desire to increase the level of skin protection against sunlight has been the consideration of additional measures, over and above the direct protection of the skin. For example, consideration has been given to the provision of protection to skin covered by clothing and thus not directly exposed to sunlight.
• Such lightweight summer clothing normally has a density of of less than 200 g/m2 and has a sun protection factor rating between 1.5 and 20, depending on the type of fibre from which the clothing is manufactured.
• the SPF rating of a sun protectant may be defined as the multiple of the time taken for the average person wearing the sun protectant to suffer sun burning under average exposure to sun. For example, if an average person would normally suffer sun burn after 30 minutes under standard exposure conditions, a sun protectant having an SPF rating of 5 would extend the period of protection from 30 minutes to 2 hours and 30 minutes. For people living in especially sunny climates, where mean sun burn times are minimal, e.g. only 15 minutes for an average fair-skinned person at the hottest time of the day, SPF ratings of at least 20 are desired for lightweight clothing.
• the present invention provides a method of improving the sun protection factor (SPF) of textile fibre material, comprising treating the textile fibre material with a composition comprising at least one fluorescent whitening agent which absorbs radiation in the wavelength range 280-400 nm.
• SPF sun protection factor
• the textile fibre material treated according to the method of the present invention may be composed of a wide variety of natural or synthetic fibres, e.g., wool, polyamide, cotton, polyester, polyacrylic, silk, polypropylene or mixtures thereof, preferably cotton.
• the textile fibre material may be in the form of endless filaments (stretched or unstretched), staple fibres, flocks, hanks, textile filament yarns, threads, nonwovens, felts, waddings, flocked structures or woven textile or bonded textile fabrics or knitted fabrics.
• the method according to the present invention may be effected by various techniques.
• the method may be conducted by contacting the textile fibre material with one of the following treatment compositions comprising at least one fluorescent whitening agent which absorbs radiation in the wavelength range 280-400 nm.:
• the amount of fluorescent whitening agent present in the composition used according to the method of the present invention may vary within a wide range, e.g. from 0.005 to 20 %, based on the weight of the textile fibre material, depending on the particular composition used in the method of the present invention.
• the amount of fluorescent whitening agent present in the composition preferably ranges from 0.01 to 3%, especially from 0.05 to 1%, based on the weight of the textile fibre material.
• the amount of fluorescent whitening agent present in the composition preferably ranges from 0.005 to 2%, especially from 0.01 to 1%, based on the weight of the textile fibre material.
• the amount of fluorescent whitening agent present in the composition preferably ranges from 0.1 to 20%, especially from 1 to 10%, based on the weight of the textile fibre material.
• the fluorescent whitening agent used may be selected from a wide range of chemical types such as 4,4'-bis-(triazinylamino)-stilbene-2,2'-disulfonic acids, 4,4'-bis-(triazol-2-yl)stilbene-2,2'-disulfonic acids, 4,4'-(diphenyl)-stilbenes, 4,4'-distyryl-biphenyls, 4-phenyl-4'-benzoxazolyl-stilbenes, stilbenyl-naphthotriazoles, 4-styryl-stilbenes, bis-(benzoxazol-2-yl) derivatives, bis-(benzimidazol-2-yl) derivatives, coumarines, pyrazolines, naphthalimides, triazinyl-pyrenes, 2-styryl-benzoxazole- or -naphthoxazole derivatives, benz
• preferred 4,4'-bis-(triazinylamino)-stilbene-2,2'-disulfonic acids are those having the formula: in which R1 and R2, independently, are phenyl, mono- or disulfonated phenyl, phenylamino, mono- or disulfonated phenylamino, morpholino, -N(CH2CH2OH)2, -N(CH3)(CH2CH2OH), -NH2, -N(C1-C4alkyl)2, -OCH3, -Cl, -NH-CH2CH2SO3H or -NH-CH2CH2OH; and M is H, Na, K, Ca, Mg, ammonium, mono-, di-, tri- or tetra-C1-C4-alkylammonium, mono-, di- or tri-C1-C4-hydroxyalkylammonium or ammoni
• each R1 is 2,5-disulfophenyl and each R2 is morpholino; or each R1 is 2,5-disulfophenyl and each R2 is N(C2H5)2; or each R1 is 3-sulfophenyl and each R2 is NH(CH2CH2OH) or N(CH2CH2OH)2; or each R1 is 4-sulfophenyl and each R2 is N(CH2CH2OH)2; and, in each case, the sulfo group is SO3M in which M is sodium.
• Preferred 4,4'-bis-(triazol-2-yl)stilbene-2,2'-disulfonic acids are those having the formula: in which R3 and R4, independently, are H, C1-C4-alkyl, phenyl or monosulfonated phenyl; and M has its previous significance.
• Especially preferred compounds of formula (2) are those in which R3 is phenyl, R4 is H and M is sodium.
• 4,4'-(diphenyl)-stilbene is that having the formula:
• 4,4'-distyryl-biphenyls used are those of formula: in which R5 and R6, independently, are H, SO3M, SO2N(C1-C4-alkyl)2, O-(C1-C4-alkyl), CN, Cl, COO(C1-C4-alkyl), CON(C1-C4-alkyl)2 or O(CH2)3N ⁇ (CH3)2An ⁇ in which An ⁇ is an anion of an organic or inorganic acid, in particular a formate, acetate, propionate, glycolate, lactate, acrylate, methanephosphonate, phosphite, dimethyl or diethyl phosphite anion , or a mixture thereof; and n is 0 or 1.
• Especially preferred compounds of formula (4) are those in which n is 1 and each R5 is a 2-SO3M group in which M is sodium and each R6 is H, or each R5 is O(CH2)3N ⁇ (CH3)2An ⁇ in which An ⁇ is acetate.
• Preferred 4-phenyl-4'-benzoxazolyl-stilbenes have the formula: in which R7 and R8, independently, are H, Cl, C1-C4-alkyl or SO2-C1-C4-alkyl.
• An especially preferred compound of formula (5) is that in which R7 is 4-CH3 and R8 is 2-CH3.
• stilbenyl-naphthotriazoles used are those of formula: in which R9 is H or Cl; R10 is SO3M, SO2N(C1-C4-alkyl)2, SO2O-phenyl or CN; R11 is H or SO3M; and M has its previous significance.
• Especially preferred compounds of formula (6) are those in which R9 and R11 are H and R10 is 2-SO3M in which M is Na.
• 4-styryl-stilbenes used are those of formula: in which R12 and R13, independently, are H, SO3M, SO2N(C1-C4-alkyl)2, O-(C1-C4-alkyl), CN, Cl, COO(C1-C4-alkyl), CON(C1-C4-alkyl)2 or O(CH2)3N ⁇ (CH3)2An ⁇ in which An ⁇ is an anion of an organic or inorganic acid, in particular a formate, acetate, propionate, glcolate, lactate, acrylate, methanephosphonate, phosphite, dimethyl or diethyl phosphite anion , or a mixture thereof.
• Especially preferred compounds of formula (7) are those in which each of R12 and R13 is 2-cyano, 2-SO3M in which M is sodium or O(CH2)3N ⁇ (CH3)2An ⁇ in which An ⁇ is acetate.
• Preferred coumarines are those of formula: in which R18 is H, Cl or CH2COOH, R19 is H, phenyl, COO-C1-C4-alkyl or a group of formula: and R20 is O-C1-C4-alkyl, N(C1-C4-alkyl)2, NH-CO-C1-C4-alkyl or a group of formula: in which R1, R2, R3 and R4 have their previous significance and R21 is H, C1-C4-alkyl or phenyl.
• pyrazolines used are those having the formula: in which R22 is H, Cl or N(C1-C4-alkyl)2, R23 is H, Cl, SO3M, SO2NH2, SO2NH-(C1-C4-alkyl), COO-C1-C4-alkyl, SO2-C1-C4-alkyl, SO2NHCH2CH2CH2N ⁇ (CH3)3 or SO2CH2CH2N ⁇ H(C1-C4-alkyl)2
• An ⁇ , R24 and R25 are the same or different and each is H, C1-C4-alkyl or phenyl and R26 is H or Cl; and An ⁇ and M have their previous significance.
• Especially preferred compounds of formula (13) are those in which R22 is Cl, R23 is SO2CH2CH2N ⁇ H(C1-C4-alkyl)2 An ⁇ in which An ⁇ is phosphite and R24, R25 and R26 are each H; or those those having the formula:
• Preferred naphthalimides are those of formula: in which R27 is C1-C4-alkyl or CH2CH2CH2N ⁇ (CH3)3; R28 and R29, independently, are O-C1-C4-alkyl, SO3M or NH-CO-C1-C4-alkyl; and M has its previous significance.
• Especially preferred compounds of formula (16) are those having the formula:
• Preferred triazinyl-pyrenes used are those of formula: in which each R30, independently, is C1-C4-alkoxy.
• Especially preferred compounds of formula (19) are those in which each R30 is methoxy.
• Preferred 2-styryl-benzoxazole- or -naphthoxazole derivatives are those having the formula: in which R31 is CN, Cl, COO-C1-C4-alkyl or phenyl; R32 and R33 are the atoms required to form a fused benzene ring or R33 and R35, independently, are H or C1-C4-alkyl; and R34 is H, C1-C4-alkyl or phenyl.
• Especially preferred compounds of formula (20) are those in which R31 is a 4-phenyl group and each of R32 to R35 is H.
• Preferred benzimidazole-benzofuran derivatives are those having the formula: in which R36 is C1-C4-alkoxy; R37 and R38, independently, are C1-C4-alkyl; and An ⁇ has its previous significance.
• a particularly preferred compound of formula (21) is that in which R36 is methoxy, R37 and R38 are each methyl and An ⁇ is methane sulfonate.
• Preferred oxanilide derivatives include those having the formula: in which R39 is C1-C4alkoxy, R41 is C1-C4alkyl, C1-C4alkyl-SO3M or C1-C4alkoxy-SO3M in which M has its previous significance and R40 and R42 are the same and each is hydrogen, tert. butyl or SO3M in which M has its previous significance.
• the fluorescent whitening agent When applied in the present method in a composition which is a textile finishing bath, the fluorescent whitening agent may in used in various formulations such as:
• preferred fluorescent whitening agents for use in the present invention are those having one of the formulae: in which R43 and R44, independently, are OH, NH2, O-C1-C4-alkyl, O-aryl, NH-C1-C4-alkyl, N(C1-C4-alkyl)2, N(C1-C4-alkyl)(C1-C4-hydroxyalkyl), N(C1-C4-hydroxyalkyl)2, NH-aryl, morpholino, S-C1-C4-alkyl(aryl), Cl or OH; R45 and R46, independently, are H, C1-C4-alkyl, phenyl or a group of formula: R47 is H, Cl or SO3M; R48 is CN, SO3M, S(C1-C4-alkyl)2 or S(aryl)2;
• C1-C4-alkyl groups are, e.g., methyl, ethyl, n-propyl, isopropyl and n-butyl, especially methyl.
• Aryl groups are naphthyl or, especially, phenyl.
• preferred fluorescent whitening agents for use in the present invention have a spectrum covering a relatively low wavelength range, that is exhibiting rather reddish shades.
• fluorescent whitening agents include compounds of formula (23) in which R43 and R44 are each non-aromatic substituents, such as compounds of formula (23) in which R43 and R44, independently, are NH-C1-C4-alkyl, O-C1-C4-alkyl or morpholino; as well as compounds of formula (26) in which n is 1.
• Preferred compounds of formula (23) are those in which R43 and R44, independently, are O-methyl, O-phenyl, NH2, NH-methyl, N(methyl)2, N(methyl)(hydroxyethyl), NH-ethyl, N(hydroxyethyl)2, NH-phenyl, S-methyl(phenyl), Cl or OH.
• Specific examples of preferred compounds of formula (23) are those having the formulae:
• Specific preferred examples of compounds of formula (24) are those of formulae: in which n has its previous significance.
• Preferred examples of compounds of formula (26) are those having the formulae:
• Preferred examples of compounds of formula (27) are those of formulae:
• a preferred example of a compound of formula (30) is that having the formula:
• the compounds of formulae (23) to (30) are known and may be obtained by known methods.
• the cationic, amphoteric or anionic fluorescent whitening agent should preferably be compatible with the rinse cycle fabric care agent and should be capable of absorption on to the washed textile material during a rinse cycle fabric care treatment.
• the cationic fluorescent whitening agent is preferably of the bistyrylphenyl class or phosphinic acid salt class; the amphoteric fluorescent whitening agent is preferably of the styrene or amine oxide class; and the anionic fluorescent whitening agent is preferably of the aminostilbene, dibenzofuranylbiphenyl or bistyrylphenyl class.
• Y is arylene, preferably 1,4-phenylene or 4,4'-diphenylene, each optionally substituted by chloro, methyl or methoxy; q is 1 or 2;
• R55 is hydrogen, chloro, C1-C4-alkyl, C1-C4-alkoxy, cyano or C1-C4-alkoxycarbonyl;
• R56 and R57 are C1-C4-alkyl, chloroethyl, methoxyethyl, ⁇ -ethoxyethyl, ⁇ -acetoxyethyl or ⁇ -cyanoethyl, benzyl or phenylethyl;
• R58 is C1-C4-alkyl, C2-C3-hydroxyalkyl, ⁇ -hydroxy- ⁇ -chloropropyl, ⁇ -cyanoethyl or C1-C4-alkoxy-carbonyleth
• Preferred compounds of formula (48) are those in which Y is 1,4-phenylene or 4,4'-diphenylene; R55 is hydrogen, methyl or cyano; R56 and R57 are each methyl or cyano; and R58 and An ⁇ have their previously indicated preferred meanings.
• One particularly preferred compound of formula (48) is that having the formula:
• the compounds of formula (48) and their production are described in US-A-4 009 193.
• a further preferred class of cationic bistyrylphenyl fluorescent whitening agent is that having the formula: in which R55 and q have their previous significance; Y1 is C2-C4-alkylene or hydroxypropylene; R59 is C1-C4-alkyl or, together with R60 and the nitrogen to which they are each attached, R59 forms a pyrrolidine, piperidine, hexamethyleneimine or morpholine ring; R60 is C1-C4-alkyl or, together with R59 and the nitrogen to which they are each attached, R60 forms a pyrrolidine, piperidine, hexamethyleneimine or morpholine ring; R61 is hydrogen, C1-C4-alkyl, C3-C4-alkenyl, C1-C4-akoxycarbonylmethyl, benzyl, C2-C4-hydroxyalkyl, C2-C4-cyanoalkyl or, together with R59 and R60 and the nitrogen atom to which they are each attached,
• Preferred compounds of formula (50) are those in which q is 1; R55 is hydrogen, chlorine, C1-C4-alkyl or C1-C4-alkoxy; Y1 is (CH2)2; R59 and R60 are the same and each is methyl or ethyl; R61 is methyl or ethyl; p is 1; and An ⁇ is CH3OSO3 or C2H5OSO3.
• a further preferred class of cationic bistyrylphenyl fluorescent whitening agent is that having the formula: in which R55, Y1, An ⁇ , p and q have their previous significance; R62 and R63, independently, are C1-C4-alkyl or C2-C3-alkenyl or R62 and R63, together with the nitrogen atom to which they are attached, form a pyrrolidine, piperidine, hexamethyleneimine or morpholine ring; R64 is hydrogen, C1-C4-alkyl or C2-C3-alkenyl or R62, R63 and R64, together with the nitrogen atom to which they are attached, form a pyridine or picoline ring; and Z is sulfur, -SO2-, -SO2NH-, -O-C1-C4-alkylene-COO- or -OCO-.
• Preferred compounds of formula (51) are those in which R55 is hydrogen, chlorine, C1-C4-alkyl or C1-C4-alkoxy; R62 and R63, independently, are C1-C4-alkyl or, together with the nitrogen atom to which they are attached, form a pyrrolidine, piperidine or morpholine ring; R64 is hydrogen, C1-C4-alkyl or C3-C4-alkenyl or R62, R63 and R64, together with the nitrogen atom to which they are attached, form a pyridine ring; and Z is sulfur, -SO2- or -SO2NH-,.
• a further preferred class of cationic bistyrylphenyl fluorescent whitening agent is that having the formula: in which R55, R62, R63, R64, Y1, An ⁇ , p and q have their previous significance.
• Preferred compounds of formula (52) are those in which q is 1;
• R55 is hydrogen, chlorine, C1-C4-alkyl or C1-C4-alkoxy;
• R62 and R63 independently, are C1-C4-alkyl or, together with the nitrogen atom to which they are attached, form a pyrrolidine, piperidine or morpholine ring;
• R64 is hydrogen, C1-C4-alkyl or C3-C4-alkenyl or R62, R63 and R64, together with the nitrogen atom to which they are attached, form a pyridine ring.
• amphoteric styrene fluorescent whitening agent is that having the formula: in which R55, R62, R63, Y1 and q have their previous significance and Z1 is oxygen, sulfur, a direct bond, -COO-, -CON(R65)- or -SO2N(R65)- in which R65 is hydrogen, C1-C4-alkyl or cyanoethyl; and Q is -COO-or -SO3.
• Preferred compounds of formula (53) are those in which Z1 is oxygen, a direct bond, -CONH-, -SO2NH- or -COO-, especially oxygen; q is 1; R62 is hydrogen, C1-C4-alkyl, methoxy or chlorine; and R63, R64, Y1 and Q have their previous significance.
• B is a brightener radical selected from a 4,4'-distyrylbiphenyl, 4,4'-divinyl-stilbene, and a 1,4'-distyrylbenzene, each optionally substituted by one to four substituents selected from halogen, C1-C4-alkyl, C1-C4-hydroxyalkyl, C1-C4-halogenoalkyl, C1-C4-cyanoalkyl, C1-C4-alkoxy-C1-C4-alkyl, phenyl-C1-C4-alkyl, carboxy-C1-C4-alkyl, carb-C1-C4-alkoxy-C1-C4-alkyl, C1-C4-alkenyl, C5-C8-cycloalkyl, C1-C4-alkoxy, C1-C4-alkenoxy
• Preferred brightener radicals B are those having the formula: in which q has its previous significance and the rings are optionally substituted as indicated above.
• Z2 is oxygen, -SO2- or -SO2N(R69)- in which R69 is hydrogen or C1-C4-alkyl optionally substituted by hydroxyl, halogen or cyano; and R66 and R67, independently, are C1-C4-alkyl optionally substituted by halogen, cyano, hydroxyl, C1-C4-alkoxy, phenyl, chlorophenyl, methylphenyl, methoxyphenyl or C2-C5-alkoxycarbonyl.
• Z2 is oxygen, sulfur, -SO2-, -CON(R69)- or -SO2N(R69)- in which R69 is hydrogen or C1-C4-alkyl optionally substituted by hydroxyl, halogen or cyano; and Y2 is C1-C4-alkylene.
• One preferred class of cationic phosphinic acid salt fluorescent whitening agent is that having the formula: in which q and Y2 have their previous significance; B1 is brightener radical; Z3 is a direct bond, -SO2-C2-C4-alkyleneoxy, -SO2-C2-C4-alkylene-COO-, -SO2-, -COO-, -SO2-C2-C4-alkylene-CON(R75)- or -SO2N(R75)- in which R75 is hydrogen or C1-C4-alkyl optionally substituted by hydroxyl, halogen or cyano; R70 is C1-C4-alkyl or C2-C4-alkenyl, each optionally substituted by halogen, cyano, hydroxy, C1-C4-alkoxycarbonyl or C1-C4-alkylcarbonyloxy, or R70 is benzyl, optionally substituted by halogen , C1-C4-alkyl or
• brightener radical B1 has the formula: or the formula: each optionally substituted by one to four substituents selected from halogen, C1-C4-alkyl, C1-C4-hydroxyalkyl, C1-C4-halogenoalkyl, C1-C4-cyanoalkyl, C1-C4-alkoxy-C1-C4-alkyl, phenyl-C1-C4-alkyl, carboxy-C1-C4-alkyl, carb-C1-C4-alkoxy-C1-C4-alkyl, C1-C4-alkenyl, C5-C8-cycloalkyl, C1-C4-alkoxy, C1-C4-alkenoxy, C1-C4-alkoxycarbonyl, carbamoyl, cyano, C1-C4-alkyl-sulfonyl, phenylsulfonyl, C1-C4-alkoxy
• Preferred bis(triazinyl)diaminostilbene anionic fluorescent whitening agents for use in the present invention are those having the formula:
• Preferred dibenzofuranylbiphenyl anionic fluorescent whitening agents for use in the present invention are those having the formula:
• Preferred anionic bistyrylphenyl fluorescent whitening agents for use in the present invention are those having the formula:
• R76 is phenyl optionally substituted by one or two SO3M groups and R77 is NH-C1-C4-alkyl, N(C1-C4-alkyl)2, NH-C1-C4-alkoxy, N(C1-C4-alkoxy)2, N(C1-C4-alkyl)(C1-C4-hydroxyalkyl), N(C1-C4-hydroxyalkyl)2;
• R70 is H, C1-C4-alkyl, CN, Cl or SO3M;
• R79 and R80 independently, are H, C1-C4
• C1-C4-alkyl groups are, e.g., methyl, ethyl, n-propyl, isopropyl and n-butyl, especially methyl.
• Aryl groups are naphthyl or, especially, phenyl.
• preferred compounds of formula (56) are those having the formula (31), (32) or (34), each as hereinbefore defined.
• Preferred examples of compounds of formula (57) are those of formula (43), (44), (45) or (46), each as hereinbefore defined.
• Preferred examples of compounds of formula (58) are those having the formula (40), (41) or (42), each as hereinbefore defined.
• the fluorescent whitening agent is applied from a textile finishing composition
• the co-use of the fluorescent whitening agent with a UV absorber is the co-use of the fluorescent whitening agent with a UV absorber.
• the UV absorber used may be, e.g., an oxalic anilide, an o-hydroxybenzophenone, an o-hydroxyaryl-1,3,5-triazine, a sulphonated-1,3,5-triazine, an o-hydroxyphenylbenzotriazole, a 2-aryl-2H-benzotriazole, a salicylic acid ester, a substituted acrylonitrile, a substituted arylaminoethylene or a nitrilohydrazone.
• UV absorbers for use in the present invention are described, for example, in the US patent specifications 2 777 828, 2 853 521, 3 118 887, 3 259 627, 3 293 247, 3 382 183, 3 403 183, 3 423 360, 4 127 586, 4 141 903, 4 230 867, 4 675 352 and 4 698 064.
• Preferred UV absorbers for use in the present invention include those of the benzo-triazine or benzo-triazole class.
• benzo-triazine UV absorbers having the formula: in which R82 and R83, independently, are hydrogen, hydroxy or C1-C5alkoxy.
• a second preferred class of triazine UV absorbers is that having the formula: in which at least one of R84, R85 and R86 is a radical of formula: in which M has its previous significance; m is 1 or 2; and the remaining substituent(s) R84, R85 and R86 are, independently, amino, C1-C12alkyl, C1-C12alkoxy, C1-C12alkylthio, mono- or di-C1-C12alkylamino, phenyl, phenylthio, anilino or N-phenyl-N-C1-C4alkylamino, preferably N-phenyl-N-methylamino or N-phenyl-N-ethylamino, the respective phenyl substituents being optionally substituted by C1-C12alkyl or -alkoxy, C5-C8cycloalkyl or halogen.
• a third preferred class of triazine UV absorbers is that having the formula: in which R87 is hydrogen or hydroxy; R88, independently, are hydrogen or C1-C4alkyl; n1 is 1 or 2; and B is a group of formula: in which n2 is an integer from 2 to 6 and is preferably 2 or 3; Y3 and Y4, independently, are C1-C4alkyl optionally substituted by halogen, cyano, hydroxy or C1-C4alkoxy or Y3 and Y4, together with the nitrogen atom to which they are each attached, form a 5-7 membered heterocyclic ring, preferably a morpholine, pyrrolidine, piperidine or hexamethyleneimine ring; Y5 is hydrogen, C3-C4alkenyl or C1-C4alkyl optionally substituted by cyano, hydroxy or C1-C4alkoxy or Y3, Y4 and Y5, together with the nitrogen atom to which they are each attached
• T1 is chlorine or, preferably, hydrogen
• T2 is a random statistical mixture of at least three isomeric branched sec. C8-C30, preferably C8-C16, especially C9-C12alkyl groups, each having the formula -CH(E1)(E2) in which E1 is a straight chain C1-C4alkyl group and E2 is a straight chain C4-C15alkyl group, the total number of carbon atoms in E1 and E2 being from 7 to 29.
• a second preferred class of triazole UV absorbers is that having the formula: in which M has its previous significance, but is preferably sodium, and T3 is hydrogen, C1-C12alkyl or benzyl.
• a third preferred class of triazole UV absorbers is that having the formula: in which B has its previous significance.
• C1-C12alkyl groups R84, R85, R86 and T3 may be methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, tert.-butyl,n-amyl, n-hexyl, n-heptyl, n-octyl, isooctyl, n-nonyl, n-decyl, n-undecyl and n-dodecyl, methyl and ethyl being preferred, except in the case of T3 for which isobutyl is preferred.
• C8-C30alkyl groups T2 include sec.octyl, decyl, dodecyl, tridecyl, tetradecyl, hexadecyl, octadecyl, eicosyl and triacontyl groups.
• C1-C5Alkoxy groups R82 or R83 may be, e.g., methoxy, ethoxy, n-propoxy, isopropoxy, n-butoxy, isobutoxy, tert.-butoxy or n-amyloxy, preferably methoxy or ethoxy, especially methoxy.
• C1-C12Alkoxy groups R84, R85 and R86 include those indicated for the C1-C5alkoxy groups R82 or R83 together with, e.g., n-hexoxy, n-heptoxy, n-octoxy, isooctoxy, n-nonoxy, n-decoxy, n-undecoxy and n-dodecoxy, methoxy and ethoxy being preferred.
• C1-C12Alkylthio groups R84, R85 and R86 may be, e.g., methylthio, ethylthio, n-propylthio, isopropylthio, n-butylthio, isobutylthio, tert.-butylthio, n-amylthio, hexylthio, n-heptylthio, n-octylthio, isooctylthio, n-nonylthio, n-decylthio, n-undecylthio and n-dodecylthio, methylthio and ethylthio being preferred.
• C1-C12Mono- or di-alkylamino groups R84, R85 and R86 include, e.g., mono- or di-methylamino, ethylamino, n-propylamino, isopropylamino, n-butylamino, isobutylamino, tert.-butylamino, n-amylamino, n-hexylamino, n-heptylamino, n-octylamino, isooctylamino, n-nonylamino, n-decylamino, n-undecylamino and n-dodecylamino, mono- or di-methylamino or ethylamino being preferred.
• the alkyl radicals in the mono-, di-, tri- or tetra-C1-C4alkylammonium groups M are preferably methyl.
• Mono-, di- or tri-C1-C4hydroxyalkylammonium groups M are preferably those derived from ethanolamine, di-ethanolamine or tri-ethanolamine.
• M is ammonium that is di- or tri-substituted by a mixture of C1-C4alkyl and C1-C4hydroxyalkyl groups, it is preferably N-methyl-N-ethanolamine or N,N-dimethyl-N-ethanolamine.
• M is preferably, however, hydrogen or sodium.
• Preferred compounds of formula (59) are those having the formulae:
• the compounds of formula (59) are known and may be prepared e.g. by the method described in U.S. Patent 3 118 887.
• Preferred compounds of formula (60) are those having the formula: in which R89 and R90, independently, are C1-C12alkyl, preferably methyl; m is 1 or 2; M1 is hydrogen, sodium, potassium, calcium, magnesium, ammonium or tetra-C1-C12alkylammonium, preferably hydrogen; and n3 and n4, independently, are 0, 1 or 2, preferably 1 or 2.
• Particularly preferred compounds of formula (73) are: 2,4-diphenyl-6-[2-hydroxy-4-(2-hydroxy-3-sulfopropoxy)-phenyl]-1,3,5-triazine; 2-phenyl-4,6-bis-[2-hydroxy-4-(2-hydroxy-3-sulfopropoxy)- phenyl] -1,3,5-triazine; 2,4-bis(2,4-dimethylphenyl)-6-[2-hydroxy-4-(2-hydroxy-3-sulfopropoxy)-phenyl] -1,3,5-triazine; and 2,4-bis(4-methylphenyl)-6-[2-hydroxy-4-(2-hydroxy-3-sulfo propoxy)-phenyl] -1,3,5-triazine.
• the compounds of formula (60) are known and may be prepared in the manner, e.g., described in US Patent 5 197 991.
• the compounds of formula (63) are known and may be prepared in the manner, e.g., described in US Patent 4 675 352.
• the compounds of formula (64) are known and may be prepared in the manner, e.g., described in EP-A-0 314 620.
• the compounds of formula (65) are known and may be prepared in the manner, e.g., described in EP-A-0 357 545.
• the method of the present invention is advantageously conducted in an aqueous medium in which the relevant fluorescent whitening agent is present in solution or as a fine dispersion.
• some of the fluorescent whitening agents or UV absorbers for use in the method according to the present invention may be only sparingly soluble in water and may need to be applied in dispersed or emulsified form. For this purpose, they may be milled with an appropriate dispersant, conveniently using quartz balls and an impeller, down to a particle size of 1-2 microns.
• the method of the present invention which is effected from a textile finishing composition, and depending on the type of fluorescent whitening agent used, it may be beneficial to carry out the treatment in a neutral, alkaline or acidic bath.
• the method is usually conducted in the temperature range of from 20 to 140°C.,for example at or near to the boiling point of the aqueous bath, e.g. at about 90°C.
• Solutions of the fluorescent whitening agent, or its emulsions in organic solvents may also be used in the method of the present invention.
• solvent dyeing pad thermofix application
• exhaust dyeing methods in dyeing machines may be used.
• the fluorescent whitening agent is made fully effective by an after-treatment.
• This may comprise a chemical treatment such as treatment with an acid, a thermal treatment or a combined thermal/chemical treatment.
• the fluorescent whitening agent in admixture with an assistant or extender such as anhydrous sodium sulfate, sodium sulfate decahydrate, sodium chloride, sodium carbonate, an alkali metal phosphate such as sodium or potassium orthophosphate, sodium or potassium pyrophosphate or sodium or potassium tripolyphosphate, or an alkali metal silicate such as sodium silicate.
• an assistant or extender such as anhydrous sodium sulfate, sodium sulfate decahydrate, sodium chloride, sodium carbonate, an alkali metal phosphate such as sodium or potassium orthophosphate, sodium or potassium pyrophosphate or sodium or potassium tripolyphosphate, or an alkali metal silicate such as sodium silicate.
• the preferred fluorescent whitening agent for use in the method according to the present invention will vary depending on the fibre from which the treated fabric is composed.
• a fluorescent whitening agent of formula (1), (2), (4), (6) or (9) is preferably used; for polyester fabrics, a fluorescent whitening agent of formula (4), (5), (6), (7), (8), (10), (12), (19) or (20) is preferably used; for the treatment of polyamide, a fluorescent whitening agent of formula (1), (2), (4), (5), (6), (7), (8), (10), (11) or (20) is preferably used; for the treatment of polyacrylonitrile, a fluorescent whitening agent of formula (6), (9), (10), (11), (12) or (21) is preferably used; for wool or silk, a fluorescent whitening agent of formula (1), (2), (4), (6), (9), (10) or (11) is preferably used; and for polypropylene, a fluorescent whitening agent of formula (8) is preferably used.
• the use according to the present invention is preferably effected by washing the textile fibre material at least once with the detergent composition, preferably at a temperature ranging from 10 to 100°C., especially from 15 to 60°C.
• the detergent composition used preferably comprises:
• the detergent may be formulated as a solid, as an aqueous liquid comprising 5-50, preferably 10-35% water or as a non-aqueous liquid detergent, containing not more than 5, preferably 0-1 wt.% of water, and based on a suspension of a builder in a non-ionic surfactant, as described, e.g., in GB-A-2158454.
• the anionic surfactant component may be, e.g., a sulphate, sulphonate or carboxylate surfactant, or a mixture of these.
• Preferred sulphates are alkyl sulphates having 12-22 carbon atoms in the alkyl radical, optionally in combination with alkyl ethoxy sulphates having 10-20 carbon atoms in the alkyl radical.
• Preferred sulphonates include alkyl benzene sulphonates having 9-15 carbon atoms in the alkyl radical.
• the cation is preferably an alkali metal, especially sodium.
• Preferred carboxylates are alkali metal sarcosinates of formula R-CO(R1)CH2COOM1 in which R is alkyl or alkenyl having 9-17 carbon atoms in the alkyl or alkenyl radical, R1 is C1-C4 alkyl and M1 is alkali metal.
• the nonionic surfactant component may be, e.g., a condensate of ethylene oxide with a C9-C15 primary alcohol having 3-8 moles of ethylene oxide per mole.
• the builder component may be an alkali metal phosphate, especially a tripolyphosphate; a carbonate or bicarbonate, especially the sodium salts thereof; a silicate; an aluminosilicate; a polycarboxylate; a polycarboxylic acid; an organic phosphonate; or an aminoalkylene poly (alkylene phosphonate); or a mixture of these.
• Preferred silicates are crystalline layered sodium silicates of the formula NaHSi m O 2m+1 .pH2O or Na2Si m O 2m+1 .pH2O in which m is a number from 1.9 to 4 and p is 0 to 20.
• aluminosilicates are the commercially-available synthetic materials designated as Zeolites A, B, X, and HS, or mixtures of these. Zeolite A is preferred.
• Preferred polycarboxylates include hydroxypolycarboxylates, in particular citrates, polyacrylates and their copolymers with maleic anhydride.
• Preferred polycarboxylic acids include nitrilotriacetic acid and ethylene diamine tetra-acetic acid.
• Preferred organic phosphonates or aminoalkylene poly (alkylene phosphonates) are alkali metal ethane 1-hydroxy diphosphonates, nitrilo trimethylene phosphonates, ethylene diamine tetra methylene phosphonates and diethylene triamine penta methylene phosphonates.
• any peroxide component may be any organic or inorganic peroxide compound, described in the literature or available on the market, which bleaches textiles at conventional washing temperatures, e.g. temperatures in the range of from 5°C. to 90°C.
• the organic peroxides are, for example, monoperoxides or polyperoxides having alkyl chains of at least 3, preferably 6 to 20, carbon atoms; in particular diperoxydicarboxylates having 6 to 12 C atoms, such as diperoxyperazelates, diperoxypersebacates, diperoxyphthalates and/or diperoxydodecanedioates, especially their corresponding free acids, are of interest.
• inorganic peroxides such as persulphate, perborate and/or percarbonate. It is, of course, also possible to employ mixtures of organic and/or inorganic peroxides.
• the peroxides, especially the inorganic peroxides are preferably activated by the inclusion of a activator such as tetraacetyl ethylenediamine or nonoyloxybenzene sulfonate.
• Bleaching catalysts which may be added include, e.g., enzymatic peroxide precursors and/or metal complexes.
• Preferred metal complexes are manganese or iron complexes such as manganese or iron phthalocyanines or the complexes described in EP-A-0 509 787.
• the detergents used will usually contain one or more auxiliaries such as soil suspending agents, for example sodium carboxymethylcellulose; salts for adjusting the pH, for example alkali or alkaline earth metal silicates; foam regulators, for example soap; salts for adjusting the spray drying and granulating properties, for example sodium sulphate; perfumes; and also, if appropriate, antistatic and softening agents; such as smectite clays; enzymes, such as amylases; photobleaching agents; pigments; and/or shading agents.
• auxiliaries such as soil suspending agents, for example sodium carboxymethylcellulose; salts for adjusting the pH, for example alkali or alkaline earth metal silicates; foam regulators, for example soap; salts for adjusting the spray drying and granulating properties, for example sodium sulphate; perfumes; and also, if appropriate, antistatic and softening agents; such as smectite clays; enzymes, such as amylases; photobleaching agents
• the preferred fluorescent whitening agent for use in the detergent used according to the present invention will vary depending on the fibre from which the treated fabric is composed.
• a fluorescent whitening agent of formula (28) is preferably used for the treatment of polyester fabrics from a detergent composition.
• a fluorescent whitening agent of formula (28) is preferably used for the treatment of polyester fabrics from a detergent composition.
• a fluorescent whitening agent of formula (29), (30) or (34) is preferably used for the treatment of polyamide.
• a fluorescent whitening agent of formula (29), (30) or (37) is preferably used for wool.
• the use in the present invention of a fluorescent whitening agent which absorbs radiation in the wavelength range 280-400 nm from a detergent composition has the following advantages: easier application since it exhausts on to the fibre; coloured textile goods can be washed with a detergent composition according to the claimed use (previously it was generally believed that FWAs had no useful role to play in detergents for coloured goods - see, e.g., A.E.Lee "Technology developments in laundry products", Proc. of the 3 rd World Conference on Detergents, Montreux, Sept.
• the present invention provides, as a further aspect, a stable, concentrated fabric care composition
• a stable, concentrated fabric care composition comprising 0.3 to 10, preferably 0.3 to 3% by weight of a fluorescent whitening agent which is compatible with a fabric care ingredient, preferably a cationic, amphoteric or anionic fluorescent whitening agent, based on the total weight of the composition, and a fabric care ingredient, preferably a fabric softener, a stain release or stain repellant ingredient or a water-proofing agent, the remainder being substantially water.
• the fabric care ingredient is preferably present in an amount of from 2 to 25, preferably 5 to 20% by weight, based on the total weight of the composition.
• the present invention provides, as a still further aspect, a stable, concentrated rinse cycle fabric softener composition
• a fabric softening agent preferably a cationic fabric softening agent and 0.3 to 10, preferably 0.3 to 3% by weight of a fluorescent whitening agent which is compatible with the fabric softening agent, preferably a cationic, amphoteric or anionic fluorescent whitening agent, each based on the total weight of the composition, the remainder being substantially water.
• cationic fabric softening agents include imidazolines, quaternary ammonium compounds, ester amide amine salts, as well as mixtures thereof.
• R91 is hydrogen or methyl;
• R92 is C14-C18alkyl or C14-C18alkenyl; and
• R92 and An ⁇ have their previous significance
• R92 is C14-C18alkyl or C14-C18alkenyl
• R94 is C14-C18alkyl, C14-C18alkenyl, C1-C4alkyl, C1-C4halogenoalkyl or C1-C4hydroxyalkyl
• Preferred anions An ⁇ include chloride, bromide, iodide, fluoride, sulfate, methosulfate, nitrite, nitrate or phosphate anions, as well as carboxylate anions such as acetate, adipate, phthalate, benzoate, stearate or oleate anions.
• preferred compounds of formula (74) include: 2-tallow-1-(2-stearoyloxyethyl)-imidazoline chloride, 2-tallow-1-(2-stearoyloxyethyl)-imidazoline sulfate, 2-tallow-1-(2-stearoyloxyethyl)-imidazoline methosulfate, 2-tallow-1-methyl-3-(2-stearoylamidoethyl)-imidazoline chloride, 2-tallow-1-methyl-3-(2-stearoylamidoethyl)-imidazoline sulfate and 2-tallow-1-methyl-3-(2-stearoylamidoethyl)-imidazoline methosulfate.
• preferred compounds of formula (75) include: 2-heptadecyl-1-methyl-1-oleylamidoethyl-imidazolinium-metho-sulfate, 2-heptadecyl-1-methyl-1-(2-stearoylamido)ethyl-imidazolinium-sulfate, 2-heptadecyl-1-methyl-1-(2-stearoylamido)ethyl-imidazolinium- chloride 2-coco-1-(2-hydroxyethyl)-1-benzyl-imidazolinium-chloride 2-coco-1-(2-hydroxyethyl)-1-(4-chlorobutyl)-imidazolinium-chloride 2-cococo-1-(2-hydroxyethyl)-1-octadecenyl-imidazolinium-chloride 2-tallow-1-(2-hydroxyethyl)-1-benzyl-imidazolinium-chloride 2-tallow-1-(2-hydroxy
• Preferred compounds of formula (76) are those in which R98 is C12-C18alkyl and R99, R100, R101, R102 and R103, independently, are C1-C4alkyl, especially methyl.
• preferred compounds of formula (76) are: N-(tallow)-N,N,N',N'-tetramethyl-1,3-propanediammoniumdimethosulfate N-(tallow)-N,N',N'-trimethyl-1,3-propanediammoniumdimetho sulfate N-(tallow)-N,N,N',N',N'-pentamethyl-1,3-propanediammoniumdimethosulfate N-oleyl-N,N,N',N',N'-pentamethyl-1,3-propanediammoniumdime thosulfate N-stearyl-N,N,N',N',N'-pentamethyl-1,3-propanediammoniumdime thosulfate and N-stearyloxypropyl-N,N',N'-tris(3-hydroxypropyl)-1,3-propanediammoniumdiacetate.
• the remaining groups R104 are C1-C4alkyl, especially methyl or ethyl,
• preferred compounds of formula (77) are: distearyldimethylaminonium chloride dilauryldimethylammonium chloride dihexadecyldimethylammonium chloride distearyldimethylammonium bromide distearyldimethylammonium methosulfate and distearyldi-(isopropyl)-ammonium chloride distearoyl(hydroxyethyl)methylammonium methosulfate.
• the remaining groups R104 are C1-C4alkyl, especially methyl or ethyl, or C1-C4hydroxyalkyl, especially hydroxymethyl or hydroxyethyl.
• a preferred compound of formula (78) is: 3-stearoylamidopropyl-2-stearoyloxymethyl-methylamine hydrochloride.
• the fabric care composition according to the present invention may also contain a minor proportion of one or more adjuvants.
• adjuvants include emulsifiers, perfumes, colouring dyes, opacifiers, UV absorbers, bactericides, nonionic surfactants, anti-gelling agents such as nitrites or nitrates of alkali metals, especially sodium nitrate, and corrosion inhibitors such as sodium silicate.
• the amount of each of these optional adjuvants should not exceed 2% by weight of the composition.
• the present invention also provides, as a yet further aspect, a method for the treatment of a textile article, comprising applying, to a previously washed article, a fabric rinse composition comprising 0.3 to 10% by weight of a cationic, amphoteric or anionic fluorescent whitening agent, based on the total weight of the composition, and optionally a fabric care ingredient, the remainder being substantially water.
• the fabric care ingredient is a fabric softener, a stain release or stain repellant ingredient or a water-proofing agent, which is preferably present in an amount of from 5 to 25%, especially from 10 to 20% by weight, based on the total weight of the composition.
• a preferred method for the treatment of a textile article comprises applying, to the previously washed article, a rinse cycle fabric softener composition comprising 5 to 25, preferably 10 to 20% by weight of a cationic fabric softening agent and 0.3 to 10, preferably 0.3 to 3% by weight of a cationic, amphoteric or anionic fluorescent whitening agent, each based on the total weight of the composition, the remainder being substantially water.
• the use according the present invention in addition to providing an improvement in the SPF of the treated textile material, may also increase the useful life of the textile material so treated; for example by preserving its tear strength and/or its lightfastness.
• the present invention is further illustrated by the following Examples.
• An aqueous textile finishing bath is made up having the composition: 2 g/l acetic acid (40%); 40 g/l of an alkyl-modified dihydroxyethyleneurea/melamine-formaldehyde derivative; 12 g/l MgCl2; and 30 g/l of an emulsion of fatty acid amides.
• AS active substances
• the whiteness (GW) of the treated samples is measured with a DCI/SF 500 spectrophotometer according to the Ganz method.
• the Ganz method is described in detail in the Ciba-Geigy Review, 1973/1, and also in the article "Whiteness Measurement", ISCC Conference on Fluorescence and the Colorimetry of Fluorescent Materials, Williamsburg, February 1972, published in the Journal of Color and Appearance, 1, No.5 (1972).
• the Sun Protection Factor is determined by measurement of the UV light transmitted through the swatch, using a double grating spectrophotometer fitted with an Ulbricht bowl. Calculation of SPF is conducted as described by B.L.Diffey and J.Robson in J. Soc. Cosm. Chem. 40 (1989), pp. 130-131.
• samples of poplin (Supraluxe" ex Walser AG; density 0.62 g/cm3; thickness 0.17 mm) are foularded (70 % liquor uptake) with the various finishing baths, at pH 4-5. Drying of the samples of poplin is effected for 3 minutes at 110°C. followed by thermofixing for 4 minutes at 150°C.
• the whiteness (GW) and SPF of the respective treated samples are measured as before.
• the respective treated poplin samples are washed ten times and the whiteness (GW) and SPF values are determined after the first, fifth and tenth washes.
• the washing is conducted at 60°C. over 15 minutes.
• the swatches are then rinsed under cold running tap water for 30 seconds and dried.
• a 5 g. sample of poplin (“Supraluxe” ex Walser AG; density 0.62 g/cm3) is foularded (80% liquor uptake) with an aqueous bath containing: 4 g/l sodium bicarbonate and 12.5 g/l of a fluorescent whitening agent having the formula: to provide a concentration of 1% by weight of active substance on the poplin substrate.
• Foularding is conducted at alkaline pH.
• Drying of the treated sample is carried out at 80°C. for 2 minutes.
• the treated poplin has an SPF rating of above 40, whereas that of the untreated poplin is 4.
• a 5 g. sample of poplin (“Supraluxe” ex Walser AG; density 0.62 g/cm3) is foularded (80% liquor uptake) with an aqueous bath containing: 2 g/l acetic acid (40%) 40 g/l of an alkyl-modified dihydroxyethyleneurea/melamine-formaldehyde derivative; 12 g/l MgCl2; 30 g/l of an emulsion of fatty acid amides and 12.5 g/l of a fluorescent whitening agent having the formula: to provide a concentration of 1% by weight of active substance on the poplin substrate.
• Foularding is conducted at a pH of 6-7.
• Drying of the treated sample is carried out at 80°C. for 2 minutes, followed by thermofixing for 4 minutes at 150°C.
• the treated poplin has an SPF rating of above 30, whereas that of the untreated poplin is 4.
• a 5 g. sample of poplin (Supraluxe" ex Walser AG; density 0.62 g/cm3) is treated with an aqueous bath containing: 3 g/l anhydrous sodium sulfate 3 g/l caustic soda flake 1.5 g/l nonylphenol ethoxylate (7 mols EO) and 1% by weight of poplin fabric of a fluorescent whitening agent having the formula: the treatment is conducted at 95°C. over 30 minutes and at a liquor ratio of 40:1, using a laboratory dyeing machine.
• the treated poplin is rinsed successively with hot or cold water and dried.
• the treated poplin has an SPF rating of above 30, whereas that of the untreated poplin is 4.
• the washing is conducted at 40°C. over 15 minutes.
• the swatches are then rinsed under cold running tap water for 30 seconds and dried.
• the wash treatment is repeated three times. After the third wash, the swatches are ironed at 160°C.
• SPF values are the average of 3 measurements at various points on the swatches.
• the relative variation of the results lies within a range of from about plus or minus 10%.
• a bleached, mercerised cotton swatch is dyed by the exhaustion method using 0.95% by weight on the fabric of a commercial blue reactive dye.
• the dyeing is conducted at a liquor ratio of 20:1, the temperature is raised from 25° to 100°C. over 40 minutes, and then held for 1 hour at 100°C. with the addition of 15g/l of sodium sulphate, before applying a final cold rinse.
• the SPF of the dyed goods is then determined by the method described in Examples 24 to 29.
• the dyed goods are then washed in the manner described in Examples 24 to 29 using the same detergent composition.
• the FWA compound used in the detergent is the compound of formula (40), at a level of 0.1 weight % of active substance, based on the weight of the detergent.
• the SPF value of the washed goods and also of goods washed with the same detergent containing no FWA (for control purposes) is determined after 1, 3, 5 and 10 washes. The results are set out in the following Table 4.
• Table 4 Example number of washes SPF without fwa with fwa - control pre-wash 23.7 23.7 30 one 22.5 23.8 three 22.0 25.9 five 20.9 26.9 ten 19.8 28.7
• the following rinse cycle softener base composition is made up: 7.0g. distearyldimethylammonium chloride (72% active ingedient) 0.5g. fatty alcohol ethoxylate 92.5g. deionised water.
• amphoteric fluorescent whitening agent of formula:
• the following rinse cycle softener base composition is made up: 7.0g. distearyldimethylammonium chloride 0.5g. fatty alcohol ethoxylate 92.5g. deionised water.
• 5g. of cotton fabric are first washed with 4g/l of ECE standard detergent using a liquor ratio of 1:20 at 60°C.
• the washed goods are then rinsed and are subjected, while still wet, to a rinse softener treatment.
• the amount of the rinse cycle softener base composition of Example 1 or 2 used is 5g/l.
• the liquor ratio is 1:40 using tap water and the treatment is effected at 25°C. for 10 minutes.
• the softener-treated goods are then spin-dried at 60°C.
• the whiteness and SPF values of the dried softener-treated goods are measured.
• the dried softener-treated goods are then re-washed using the same detergent and washing conditions that are used for the initial wash except that, after the rinse, the re-washed goods are spin-dried at 60°C. without being subjected to a rinse softener treatment.
• the whiteness and SPF values of the re-washed, dried goods are measured.
• the concentration of FWA denotes the concentration of active FWA compound based on the total weight of the rinse formulation.

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