CN106544176A - A kind of silver carboxymethyl chitosan antibacterial color fixative liquid detergent and preparation method thereof - Google Patents
A kind of silver carboxymethyl chitosan antibacterial color fixative liquid detergent and preparation method thereof Download PDFInfo
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- CN106544176A CN106544176A CN201610869652.8A CN201610869652A CN106544176A CN 106544176 A CN106544176 A CN 106544176A CN 201610869652 A CN201610869652 A CN 201610869652A CN 106544176 A CN106544176 A CN 106544176A
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- 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
- C11D1/88—Ampholytes; Electroneutral compounds
- C11D1/94—Mixtures with anionic, cationic or non-ionic 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
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2075—Carboxylic acids-salts thereof
- C11D3/2086—Hydroxy carboxylic acids-salts thereof
-
- 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
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/22—Carbohydrates or derivatives thereof
- C11D3/222—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin
- C11D3/227—Natural or synthetic polysaccharides, e.g. cellulose, starch, gum, alginic acid or cyclodextrin with nitrogen-containing groups
-
- 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
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/30—Amines; Substituted amines ; Quaternized amines
-
- 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
- C11D3/16—Organic compounds
- C11D3/34—Organic compounds containing sulfur
- C11D3/3418—Toluene -, xylene -, cumene -, benzene - or naphthalene sulfonates or sulfates
-
- 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
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/382—Vegetable products, e.g. soya meal, wood flour, sawdust
-
- 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
- C11D3/16—Organic compounds
- C11D3/38—Products with no well-defined composition, e.g. natural products
- C11D3/386—Preparations containing enzymes, e.g. protease or amylase
- C11D3/38618—Protease or amylase in liquid compositions only
-
- 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
- C11D3/48—Medical, disinfecting agents, disinfecting, antibacterial, germicidal or antimicrobial compositions
-
- 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
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic 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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/74—Carboxylates or sulfonates esters of polyoxyalkylene glycols
-
- 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
- C11D1/88—Ampholytes; Electroneutral compounds
- C11D1/90—Betaines
Abstract
The invention discloses a kind of silver carboxymethyl chitosan antibacterial color fixative liquid detergent and preparation method thereof, belongs to Field of Fine Chemicals, described shitosan silver antibacterial color fixative liquid detergent includes following raw material：Silver carboxymethyl chitosan, dodecylbenzene sodium sulfonate, ethoxylation methyl stearate, ethanolamine, cocamidopropyl betaine, HP66K, sodium citrate, amylase, quintessence oil, deionized water, described liquid detergent are made by the step of adopting preparation, heating, mixing, homogenizing.The present invention with the addition of the liquid detergent of silver carboxymethyl chitosan, the biocidal efficacies with silver carboxymethyl chitosan, can effectively kill the antibacterial of washing medicated clothing, has color fixative effect concurrently, and silver carboxymethyl chitosan can make liquid detergent preserve the longer time, and easily decompose, safety and environmental protection.
Description
Technical field
The invention belongs to household chemicalss manufacture field, and in particular to a kind of antibacterial color fixative liquid detergent and preparation method thereof.
Background technology
Liquid detergent is a kind of detergent compositions of liquid, and its operation principle is same with traditional detergent and soap kind, effectively into
It is all surfactant to divide.For, in the product of clothes washing, detergent accounts for main status always.But, liquid detergent master
Composition is wanted to be nonionic surfactant, dirt-removing power is strong, and can play cleaning function, decontamination inside deep enough clothes fiber
It is more thorough.Liquid detergent compares detergent, with more advantages.Detergent can not be completely dissolved in use, residue
Medicated clothing damage is easily caused, and is difficult rinsing；And liquid detergent can be completely dissolved and dissolution velocity fast, easily float washable, will not
Injure skin and medicated clothing.Detergent is generally alkaline, larger to skin irritation and injury；And liquid detergent pH value partial neutral,
Formula does not gently hurt hands.Liquid detergent is easy to add various effective ingredient, increases its feature, such as softness, gloss, brighten, it is degerming
With effect of lasting lasting.The waste liquid that detergent is produced is in difficult (the particularly branched alkyl benzene sulphonate of nature degraded
Sodium), water pollution is caused, very big destruction is caused to ecology；And liquid detergent then relative degraded relatively completely, environment cause it is bad compared with
It is little.As liquid detergent has many advantages, therefore, the growth of liquid detergent industry is also more swift and violent.The liquid detergent city of China
Increased with average annual 27.2% speed, 3 years compound has grown beyond 100%.Meanwhile, the average annual increasing in detergent market
Speed is only 2.2%.Domestic liquid detergent will reach the 19% of whole laundry detergents market in 2010, be reached in 2015 afterwards
30%.And in the U.S., the market share of liquid detergent has been over detergent, accounting reaches more than 80%, has greatly replacement laundry
The trend of powder.
As liquid detergent is more convenient for increasing functional components compared to detergent so that liquid detergent possesses work(more in all directions
Effect.The liquid detergent such as existing antibacterial, net white, soft, color drift, low alveolitoid on the market, species are various, and the rinsing of suitable difference medicated clothings need to
Ask.The liquid detergent demand that liquid detergent with antibiotic property becomes in recent years is popular.With the continuous lifting of people's living standard, more
Come more consumers for the demand of laundry, be not only embodied on higher detergency ability, for the removal of pathogenic bacterium
Pay attention to further.Existing patent and Patent Application Publication also relates to the formula and processing technology of antimicrobial laundry liquid at present.As sent out
Bright Patent Application Publication " antibiotic property liquid detergent " (number of patent application：201510846429.7) disclose a kind of antibiotic property laundry
Liquid, is characterized in that and with the addition of the composite mesoporous antibacterial of high activity cerium silver, by mesoporous material and the group of antibacterial activity material
Close so that antibacterial activity material can be evenly dispersed in needing degerming environment, antibacterial on medicated clothing is killed so as to reach
Effect；A kind of application for a patent for invention document " antimicrobial laundry liquid " (number of patent application：201410451184.3) disclose a kind of anti-
Bacterium liquid detergent, includes nano-TiO2High effect nontoxic antibacterial, good anti-bacterial effect；Application for a patent for invention document " receive by a kind of addition
Strong disinfecting and durable antibiotic liquid detergent of meter Yin and preparation method thereof " (number of patent application：201510810227.7) disclose
A kind of strong disinfecting and durable antibiotic liquid detergent and preparation method thereof of addition nanometer silver, the liquid detergent by soapberry extract,
Carrying nano silver zeolite antibacterial agent, shitosan-nanometer silver solution and Kazon etc. are constituted, via series of steps systems such as stirring, heating
It is standby to form, with strong bactericidal and persistently antibacterial double effectses.
Carboxymethyl chitosan is a kind of water-solubility chitosan derivative, has numerous characteristics, and such as antibiotic property is strong, with fresh-keeping work
With being a kind of polyampholyte, have various applications at the aspect such as cosmetics, fresh-keeping, medical, and Recent study obtains more
One of chitosan derivatives.The silver carboxymethyl chitosan being prepared from silver-colored complexation using carboxymethyl chitosan, stability are strong,
And hydrophilic compares shitosan more preferably, can be used to prepare the cosmetics of everyday use for requiring that there are biocidal efficacies.
Medicated clothing be in the suds colour fading and colour contamination reason have several：Fabric controls process conditions in dyeing process, not,
Cause dye fixing loosely；In detergent, the emulsifying ability and penetration of surfactant causes the depigmentation of dye molecule；Daily life
In work, Jing Exposures to Sunlight or repeatedly washing cause dye molecule oxidation reaction to occur or weakens which to adsorb fastness with fabric；Dark color is knitted
The color that thing and light coloured fabrics are caused when washing simultaneously is transferred on light coloured fabrics by deep-colour fabric；Different colours on single fabric
Dyestuff is attached to the infection phenomenon on another kind of fabric again by fabric to solution under Action of Surfactant.How fabric is avoided
Occur to fade and colour contamination phenomenon in common washing process, and a research direction of current liquid detergent on the market.
The disclosure of background above technology contents is only used for inventive concept and the technical scheme for aiding in understanding the present invention, and which is not
The prior art of present patent application is necessarily belonged to, shows the applying date of the above in present patent application there is no tangible proof
In the case of disclosed, above-mentioned background technology should not be taken to the novelty and creativeness for evaluating the application.
The content of the invention
The technical problem to be solved in the present invention be to provide a kind of silver carboxymethyl chitosan antibacterial color fixative liquid detergent and its
Preparation method, to solve the technical problem on the market without silver carboxymethyl chitosan antibacterial color fixative liquid detergent.
In order to solve above technical problem, the present invention is employed the following technical solutions：
A kind of silver carboxymethyl chitosan antibacterial color fixative liquid detergent, it is characterised in that in units of weight portion, comprising following original
Material：8～30 parts of silver carboxymethyl chitosan, 150～300 parts of dodecylbenzene sodium sulfonate, ethoxylation methyl stearate 210～
440 parts, 20～60 parts of ethanolamine, 30～75 parts of cocamidopropyl betaine, HP66K3～16 part, sodium citrate 90～
270 parts, 3～12 parts of amylase, 2～9 parts of quintessence oil, 1800～4000 parts of deionized water.
Preferably, described carboxymethyl chitosan antibacterial color fixative liquid detergent, in units of weight portion, comprising following raw material：
12～25 parts of silver carboxymethyl chitosan, 180～260 parts of dodecylbenzene sodium sulfonate, ethoxylation methyl stearate 275～405
Part, 24～52 parts of ethanolamine, 40～66 parts of cocamidopropyl betaine, HP66K6～12 part, sodium citrate 140～230
Part, 5～10 parts of amylase, 3～7 parts of quintessence oil, 2400～3600 parts of deionized water.
Preferably, described silver carboxymethyl chitosan antibacterial color fixative liquid detergent, the quintessence oil include Herba Lysimachiae foenum-graeci quintessence oil, Herba Cymbopogonis Citrari
Quintessence oil, Citrua paradiai quintessence oil.
Preferably, the preparation method of described silver carboxymethyl chitosan antibacterial color fixative liquid detergent, comprises the following steps：
a：By portions of de-ionized water add reactor in, be heated to 50～60 DEG C, be slowly added to dodecylbenzene sodium sulfonate,
Ethoxylation methyl stearate, cocamidopropyl betaine, 20～40min is to being completely dissolved for stirring；
b：After mixed material temperature is down to room temperature obtained by step a, ethanolamine, sodium citrate, HP66K, essence are slowly added to
Oil, 10～20min is to being completely dissolved for stirring；
c：After obtained by step b, mixed material temperature is down to room temperature, add amylase, silver carboxymethyl chitosan, stirring 5～
After 15min, 2～6min of homogenizing, it is 7～8.5 to be adjusted to mixed liquor pH value using acid-base modifier, stands froth breaking.
Preferably, described silver carboxymethyl chitosan antimicrobial laundry liquid, the preparation method of silver carboxymethyl chitosan include with
Lower step：
S1：40%NaOH solution and aqueous isopropanol are added in shitosan after purification, under room temperature, 50min is stirred；
S2：Chloroacetic aqueous isopropanol is added dropwise in mixture obtained by step S1, after completion of dropping, continues reaction
3h；
S3：Mixed material obtained by step S2 is neutralized to into pH=7 with dilute hydrochloric acid, with acetone precipitation, is filtered, is taken filtering residue；
S4：Washed to filtering residue without chloride ion with 85% methanol solution, then washed with absolute methanol；
S5：By 20%AgNO3During solution adds step S4 resulting material under stirring, stirring reaction 1h；
S6：After step S5 resulting material is crystallized with acetone, washed 1 time with 85% methanol solution, then washed with methanol solution
Wash 3 times；
S7：Step S4 resulting material is placed in vacuum drying oven, 1h is vacuum dried in 60 DEG C.
Preferably, the preparation method of described silver carboxymethyl chitosan, in step S4, the method for inspection of chloride ion is use
AgNO3Acid solution inspection.
The invention has the advantages that：
(1) present invention adopts carboxymethyl chitosan and antibacterial color fixative liquid detergent is prepared for raw material, and carboxymethyl chitosan is one kind
Natural environmental-protective product, it is low toxicity, harmless, make the antimicrobial laundry liquid of preparation more environmentally friendly；
(2) present invention prepares silver carboxymethyl chitosan, carboxymethyl chitosan by the way of carboxymethyl chitosan complex silver
Dissolubility is good, and stability is strong, used in being suitably added into liquid detergent as a kind of antimicrobial component；
(3) liquid detergent of the present invention includes multiple actives, makes the dirt-removing power of liquid detergent strong；The starch for being possessed
Enzyme can effectively decompose spot；Preparation method step of the present invention is simple, is suitable for standardization, industrialized production.
Specific embodiment
The present invention is described in further detail with reference to specific embodiment.It is emphasized that the description below is only
Only it is exemplary, rather than in order to limit the scope of the present invention and its application.
Embodiment 1：
A kind of silver carboxymethyl chitosan antibacterial color fixative liquid detergent, in units of weight portion, comprising following raw material：Carboxymethyl shell
8 parts of polysaccharide silver, 150 parts of dodecylbenzene sodium sulfonate, 210 parts of ethoxylation methyl stearate, 20 parts of ethanolamine, cocamidopropyl
30 parts of CAB, HP66K4.5 parts, 90 parts of sodium citrate, 3 parts of amylase, 2 parts of Herba Lysimachiae foenum-graeci quintessence oil, deionized water 1800
Part.
Wherein, silver carboxymethyl chitosan is prepared by following steps：
S1：40%NaOH solution and aqueous isopropanol are added in shitosan after purification, under room temperature, 50min is stirred；
S2：Chloroacetic aqueous isopropanol is added dropwise in mixture obtained by step S1, after completion of dropping, continues reaction
3h；
S3：Mixed material obtained by step S2 is neutralized to into pH=7 with dilute hydrochloric acid, with acetone precipitation, is filtered, is taken filtering residue；
S4：Washed with 85% methanol solution to filtering residue AgNO3Acid solution check without chloride ion, then washed with absolute methanol
Wash；
S5：By 20%AgNO3During solution adds step S4 resulting material under stirring, stirring reaction 1h；
S6：After step S5 resulting material is crystallized with acetone, washed 1 time with 85% methanol solution, then washed with methanol solution
Wash 3 times；
S7：Step S4 resulting material is placed in vacuum drying oven, 1h is vacuum dried in 60 DEG C.
The preparation method of described silver carboxymethyl chitosan antibacterial color fixative liquid detergent, comprises the following steps：
a：Portions of de-ionized water is added in reactor, 50 DEG C is heated to, is slowly added to dodecylbenzene sodium sulfonate, ethoxy
Base methyl stearate, cocamidopropyl betaine, 20min is to being completely dissolved for stirring；
b：After mixed material temperature is down to room temperature obtained by step a, it is slowly added to ethanolamine, sodium citrate, HP66K, smokes
Clothing grass quintessence oil, 10min is to being completely dissolved for stirring；
c：After mixed material temperature is down to room temperature obtained by step b, amylase, silver carboxymethyl chitosan, stirring are added
After 5min, homogenizing 2min, it is 7 to be adjusted to mixed liquor pH value using acid-base modifier, stands froth breaking.
Embodiment 2
A kind of silver carboxymethyl chitosan antibacterial color fixative liquid detergent, in units of weight portion, comprising following raw material：Carboxymethyl shell
30 parts of polysaccharide silver, 300 parts of dodecylbenzene sodium sulfonate, 440 parts of ethoxylation methyl stearate, 60 parts of ethanolamine, coconut oleoyl amine
75 parts of base CAB, HP66K17.5 parts, 270 parts of sodium citrate, 12 parts of amylase, 9 parts of oil of Cymbopogon winterianus, deionized water
4000 parts.
Wherein, silver carboxymethyl chitosan is prepared by following steps：
S1：40%NaOH solution and aqueous isopropanol are added in shitosan after purification, under room temperature, 50min is stirred；
S2：Chloroacetic aqueous isopropanol is added dropwise in mixture obtained by step S1, after completion of dropping, continues reaction
3h；
S3：Mixed material obtained by step S2 is neutralized to into pH=7 with dilute hydrochloric acid, with acetone precipitation, is filtered, is taken filtering residue；
S4：Washed with 85% methanol solution to filtering residue AgNO3Acid solution check without chloride ion, then washed with absolute methanol
Wash；
S5：By 20%AgNO3During solution adds step S4 resulting material under stirring, stirring reaction 1h；
S6：After step S5 resulting material is crystallized with acetone, washed 1 time with 85% methanol solution, then washed with methanol solution
Wash 3 times；
S7：Step S4 resulting material is placed in vacuum drying oven, 1h is vacuum dried in 60 DEG C.
The preparation method of described silver carboxymethyl chitosan antibacterial color fixative liquid detergent, comprises the following steps：
a：Portions of de-ionized water is added in reactor, 60 DEG C is heated to, is slowly added to dodecylbenzene sodium sulfonate, ethoxy
Base methyl stearate, cocamidopropyl betaine, 40min is to being completely dissolved for stirring；
b：After mixed material temperature is down to room temperature obtained by step a, ethanolamine, sodium citrate, HP66K, perfume (or spice) are slowly added to
Thatch quintessence oil, 20min is to being completely dissolved for stirring；
c：After mixed material temperature is down to room temperature obtained by step b, amylase, silver carboxymethyl chitosan, stirring are added
After 15min, homogenizing 6min, it is 8.5 to be adjusted to mixed liquor pH value using acid-base modifier, stands froth breaking.
Embodiment 3
A kind of silver carboxymethyl chitosan antibacterial color fixative liquid detergent, in units of weight portion, comprising following raw material：Carboxymethyl shell
12 parts of polysaccharide silver, 180 parts of dodecylbenzene sodium sulfonate, 275 parts of ethoxylation methyl stearate, 24 parts of ethanolamine, coconut oleoyl amine
40 parts of base CAB, HP66K7 parts, 140 parts of sodium citrate, 5 parts of amylase, 3 parts of Citrua paradiai quintessence oil, 2400 parts of deionized water.
Wherein, silver carboxymethyl chitosan is prepared by following steps：
S1：40%NaOH solution and aqueous isopropanol are added in shitosan after purification, under room temperature, 50min is stirred；
S2：Chloroacetic aqueous isopropanol is added dropwise in mixture obtained by step S1, after completion of dropping, continues reaction
3h；
S3：Mixed material obtained by step S2 is neutralized to into pH=7 with dilute hydrochloric acid, with acetone precipitation, is filtered, is taken filtering residue；
S4：Washed with 85% methanol solution to filtering residue AgNO3Acid solution check without chloride ion, then washed with absolute methanol
Wash；
S5：By 20%AgNO3During solution adds step S4 resulting material under stirring, stirring reaction 1h；
S6：After step S5 resulting material is crystallized with acetone, washed 1 time with 85% methanol solution, then washed with methanol solution
Wash 3 times；
S7：Step S4 resulting material is placed in vacuum drying oven, 1h is vacuum dried in 60 DEG C.
The preparation method of described silver carboxymethyl chitosan antibacterial color fixative liquid detergent, comprises the following steps：
a：Portions of de-ionized water is added in reactor, 50 DEG C is heated to, is slowly added to dodecylbenzene sodium sulfonate, ethoxy
Base methyl stearate, cocamidopropyl betaine, 20min is to being completely dissolved for stirring；
b：After mixed material temperature is down to room temperature obtained by step a, ethanolamine, sodium citrate, HP66K, west are slowly added to
Shaddock oil, 10min is to being completely dissolved for stirring；
c：After mixed material temperature is down to room temperature obtained by step b, amylase, silver carboxymethyl chitosan, stirring are added
After 5min, homogenizing 2min, it is 7 to be adjusted to mixed liquor pH value using acid-base modifier, stands froth breaking.
Embodiment 4
A kind of silver carboxymethyl chitosan antibacterial color fixative liquid detergent, in units of weight portion, comprising following raw material：Carboxymethyl shell
25 parts of polysaccharide silver, 260 parts of dodecylbenzene sodium sulfonate, 405 parts of ethoxylation methyl stearate, 52 parts of ethanolamine, coconut oleoyl amine
66 parts of base CAB, HP66K14 parts, 230 parts of sodium citrate, 10 parts of amylase, 7 parts of oil of Cymbopogon winterianus, deionized water 3600
Part.
Wherein, silver carboxymethyl chitosan is prepared by following steps：
S1：40%NaOH solution and aqueous isopropanol are added in shitosan after purification, under room temperature, 50min is stirred；
S2：Chloroacetic aqueous isopropanol is added dropwise in mixture obtained by step S1, after completion of dropping, continues reaction
3h；
S3：Mixed material obtained by step S2 is neutralized to into pH=7 with dilute hydrochloric acid, with acetone precipitation, is filtered, is taken filtering residue；
S4：Washed with 85% methanol solution to filtering residue AgNO3Acid solution check without chloride ion, then washed with absolute methanol
Wash；
S5：By 20%AgNO3During solution adds step S4 resulting material under stirring, stirring reaction 1h；
S6：After step S5 resulting material is crystallized with acetone, washed 1 time with 85% methanol solution, then washed with methanol solution
Wash 3 times；
S7：Step S4 resulting material is placed in vacuum drying oven, 1h is vacuum dried in 60 DEG C.
The preparation method of described silver carboxymethyl chitosan antibacterial color fixative liquid detergent, comprises the following steps：
a：Portions of de-ionized water is added in reactor, 60 DEG C is heated to, is slowly added to dodecylbenzene sodium sulfonate, ethoxy
Base methyl stearate, cocamidopropyl betaine, 40min is to being completely dissolved for stirring；
b：After mixed material temperature is down to room temperature obtained by step a, ethanolamine, sodium citrate, HP66K, perfume (or spice) are slowly added to
Thatch quintessence oil, 20min is to being completely dissolved for stirring；
c：After mixed material temperature is down to room temperature obtained by step b, amylase, silver carboxymethyl chitosan, stirring are added
After 15min, homogenizing 6min, it is 8.5 to be adjusted to mixed liquor pH value using acid-base modifier, stands froth breaking.
Embodiment 5
A kind of silver carboxymethyl chitosan antibacterial color fixative liquid detergent, in units of weight portion, comprising following raw material：Carboxymethyl shell
18 parts of polysaccharide silver, 205 parts of dodecylbenzene sodium sulfonate, 360 parts of ethoxylation methyl stearate, 42 parts of ethanolamine, coconut oleoyl amine
51 parts of base CAB, HP66K10 parts, 180 parts of sodium citrate, amylase 8 part, 5 parts of Herba Lysimachiae foenum-graeci quintessence oil, deionized water 3000
Part.
Wherein, silver carboxymethyl chitosan is prepared by following steps：
S1：40%NaOH solution and aqueous isopropanol are added in shitosan after purification, under room temperature, 50min is stirred；
S2：Chloroacetic aqueous isopropanol is added dropwise in mixture obtained by step S1, after completion of dropping, continues reaction
3h；
S3：Mixed material obtained by step S2 is neutralized to into pH=7 with dilute hydrochloric acid, with acetone precipitation, is filtered, is taken filtering residue；
S4：Washed with 85% methanol solution to filtering residue AgNO3Acid solution check without chloride ion, then washed with absolute methanol
Wash；
S5：By 20%AgNO3During solution adds step S4 resulting material under stirring, stirring reaction 1h；
S6：After step S5 resulting material is crystallized with acetone, washed 1 time with 85% methanol solution, then washed with methanol solution
Wash 3 times；
S7：Step S4 resulting material is placed in vacuum drying oven, 1h is vacuum dried in 60 DEG C.
The preparation method of described silver carboxymethyl chitosan antibacterial color fixative liquid detergent, comprises the following steps：
a：Portions of de-ionized water is added in reactor, 55 DEG C is heated to, is slowly added to dodecylbenzene sodium sulfonate, ethoxy
Base methyl stearate, cocamidopropyl betaine, 30min is to being completely dissolved for stirring；
b：After mixed material temperature is down to room temperature obtained by step a, ethanolamine, sodium citrate, HP66K, west are slowly added to
Shaddock oil, 15min is to being completely dissolved for stirring；
c：After mixed material temperature is down to room temperature obtained by step b, amylase, silver carboxymethyl chitosan, stirring are added
After 10min, homogenizing 4min, it is 8 to be adjusted to mixed liquor pH value using acid-base modifier, stands froth breaking.
For more detailed description beneficial effects of the present invention, selection do not add silver carboxymethyl chitosan, other there is phase
The liquid detergent of homogenous quantities part ratio compares test, the following provides specific result of the test.
The liquid detergent A being prepared into using component and preparation method described in the embodiment of the present invention 1 with except silver carboxymethyl chitosan
And the liquid detergent B being prepared into that HP66K is outer, other components component and preparation method are same as Example 1, it is added to same weight
Amount, cleans the medicated clothing of equal number using identical washing machine, identical program for washing, and two groups of medicated clothings that cleaning is obtained is compared in detection
In contained clump count (escherichia coli, staphylococcus aureuses) and medicated clothing color fastness.Test result indicate that, cleaned using A
The medicated clothing that the medicated clothing ratio for obtaining is cleaned using B, escherichia coli number reduce by 18%, and staphylococcus aureuses number reduces by 24%；
Color fastness lifts 8%.As can be seen here, the liquid detergent containing silver carboxymethyl chitosan of the invention has good antibacterial, color fixative
Effect.
Above content it cannot be assumed that the present invention be embodied as be confined to these explanation, for belonging to the present invention technology neck
For the those of ordinary skill in domain, without departing from the inventive concept of the premise, some simple deduction or replace can also be made,
The scope of patent protection that the present invention is determined by the claims submitted to should be all considered as belonging to.
Claims (6)
1. a kind of silver carboxymethyl chitosan antibacterial color fixative liquid detergent, it is characterised in that in units of weight portion, comprising following original
Material：8～30 parts of silver carboxymethyl chitosan, 150～300 parts of dodecylbenzene sodium sulfonate, ethoxylation methyl stearate 210～
440 parts, 20～60 parts of ethanolamine, 30～75 parts of cocamidopropyl betaine, HP66K4.5～17.5 part, sodium citrate 90
～270 parts, 3～12 parts of amylase, 2～9 parts of quintessence oil, 1800～4000 parts of deionized water.
2. silver carboxymethyl chitosan antibacterial color fixative liquid detergent according to claim 1, it is characterised in that with weight portion as list
Position, comprising following raw material：12～25 parts of silver carboxymethyl chitosan, 180～260 parts of dodecylbenzene sodium sulfonate, ethoxylation are hard
275～405 parts of fat acid methyl ester, 24～52 parts of ethanolamine, 40～66 parts of cocamidopropyl betaine, HP66K7～14 part,
140～230 parts of sodium citrate, 5～10 parts of amylase, 3～7 parts of quintessence oil, 2400～3600 parts of deionized water.
3. silver carboxymethyl chitosan antibacterial color fixative liquid detergent according to claims 1 to 2, it is characterised in that the quintessence oil
Including Herba Lysimachiae foenum-graeci quintessence oil, oil of Cymbopogon winterianus, Citrua paradiai quintessence oil.
4. the preparation method of the silver carboxymethyl chitosan antibacterial color fixative liquid detergent according to any one of claim 1～2, which is special
Levy and be, comprise the following steps：
a：Portions of de-ionized water is added in reactor, 50～60 DEG C is heated to, is slowly added to dodecylbenzene sodium sulfonate, ethoxy
Base methyl stearate, cocamidopropyl betaine, 20～40min is to being completely dissolved for stirring；
b：After mixed material temperature is down to room temperature obtained by step a, ethanolamine, sodium citrate, HP66K, quintessence oil is slowly added to, is stirred
10～20min is mixed to being completely dissolved；
c：After obtained by step b, mixed material temperature is down to room temperature, add amylase, silver carboxymethyl chitosan, stirring 5～
After 15min, 2～6min of homogenizing, it is 7～8.5 to be adjusted to mixed liquor pH value using acid-base modifier, stands froth breaking.
5. the silver carboxymethyl chitosan antibacterial color fixative liquid detergent according to any one of claim 1～2, it is characterised in that institute
The preparation method of the silver carboxymethyl chitosan stated is comprised the following steps：
S1：40%NaOH solution and aqueous isopropanol are added in shitosan after purification, under room temperature, 50min is stirred；
S2：Chloroacetic aqueous isopropanol is added dropwise in mixture obtained by step S1, after completion of dropping, continues reaction 3h；
S3：Mixed material obtained by step S2 is neutralized to into pH=7 with dilute hydrochloric acid, with acetone precipitation, is filtered, is taken filtering residue；
S4：Washed to filtering residue without chloride ion with 85% methanol solution, then washed with absolute methanol；
S5：By 20%AgNO3During solution adds step S4 resulting material under stirring, stirring reaction 1h；
S6：After step S5 resulting material is crystallized with acetone, washed 1 time with 85% methanol solution, then 3 are washed with methanol solution
It is secondary；
S7：Step S4 resulting material is placed in vacuum drying oven, 1h is vacuum dried in 60 DEG C.
6. the preparation method of silver carboxymethyl chitosan according to claim 5, it is characterised in that chloride ion in step S4
The method of inspection is to use AgNO3Acid solution inspection.
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| CN104560457A (en) * | 2014-12-19 | 2015-04-29 | 北京绿伞化学股份有限公司 | Infant laundry detergent and preparation method thereof |
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| CN106962199A (en) * | 2017-05-04 | 2017-07-21 | 南宁市辉雄中药材农民专业合作社 | A kind of beautiful millettia root antibacterial tissue culture medium (TCM) and preparation method thereof |
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Application publication date: 20170329 |