CN104387479A - Cationic starch with conditioning and setting effects and preparation method of cationic starch - Google Patents
Cationic starch with conditioning and setting effects and preparation method of cationic starch Download PDFInfo
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- CN104387479A CN104387479A CN201410710071.0A CN201410710071A CN104387479A CN 104387479 A CN104387479 A CN 104387479A CN 201410710071 A CN201410710071 A CN 201410710071A CN 104387479 A CN104387479 A CN 104387479A
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Abstract
The invention discloses a preparation method of cationic starch with conditioning and setting effects. The preparation method comprises the following steps: alkalifying the starch by use of alkali liquor, and then injecting a cationic modifier and stirring thoroughly to obtain a starch mixed pulp; dispersing the starch mixed pulp into the aqueous solution of an organic solvent to obtain a starch suspension; increasing the temperature to the range of 40-80 DEG C, reacting for 1.5-3 hours, next, adding an acid, stirring for neutralizing until the pH is within the range of 5-8, and finally, performing centrifugal drying, thereby obtaining the cationic starch with the conditioning and setting effects. The cationic starch is prepared from the starch raw material of a specific structure, and is enabled to have a strong setting effect and a good conditioning effect, namely the double effects of setting and conditioning, after being etherified by use of the special cationic modifier.
Description
Technical field
The present invention relates to macromolecular compound technical field, particularly relate to a kind of cationic starch and preparation method thereof with conditioning styling.
Background technology
Hair fixing principle is to combine closely with hair, and forms a kind of film outside, and its film need have snappiness, intensity and elasticity, and enemy delivers now good affinity and adhesivity, difficult drop-off.At present, as membrane-forming agent mainly polyvinylpyrrolidone or its multipolymer of hairspray, model has K30, K90 etc.The acclimatization ability of polyvinylpyrrolidone film is poor, in a humid environment can the moisture absorption, and the hardness of film reduces, and loses style-ability; Become fragile in dry environment easily crisp.The polymkeric substance of vinyl pyrrolidine ketone and the poor compatibility of alkanes propelling agent are only good with the consistency of freonll-11 propelling agent.Fluorine Lyons makes one of destroyed reason of atmospheric ozone layer, pollutes global environment.Compared with the natural high molecular substance of starch, Mierocrystalline cellulose, guar gum plant origin, the biological degradability of polyvinylpyrrolidone film and lower with Environmental compatibility.Because hair styling product is resident type product, require that setting agent must safety non-toxic.
Starch has the outstanding advantages of cheapness, renewable, never exhaustion, biodegradable, environmental protection compared with industrial chemicals.
The hair conditioning cation type water-soluble polymer compound of daily use chemicals industry widespread use is the cationic polysaccharides such as cation guar gum, cationic hydroxyethyl cellulose material.It has flexibility, hair conditioning, moisture-keeping functions, and easily rinsing, with the dual-use function of polyose and cats product, comparatively fast colloid can be formed when itself and the anion binding in filling a prescription, silicone oil, the material fast deposition such as anti-dandruff of parcel formula on hair, thus reach opsonization.Cationic starch, because it has polysaccharide and the cation group of long-chain, so its with the guar gum extensively adopted, Mierocrystalline cellulose cationic derivative is the same has good conditioning performance, again because starch can form the just right polymeric membrane with certain toughness, thus reach conditioning sizing effect.Meanwhile, the guar gum of its Starches ratio and Natvosol then have extremely significantly wide material sources, the advantage that cost is low.Cationic starch has antistatic, suspension, thickening, the effect such as qualitative equally, and have good affinity with the Keratin sulfate of hair and skin, and gentle, the pungency of washing composition to skin can be reduced, under lower consumption, namely there is good suspension, thickening capabilities.
Therefore cationic starch is applied in makeup as amendment and is favored very much, but because of its gelatinization point high, could be water-soluble more than 95 DEG C, bring very large difficulty to operating procedure in cosmetics production, limit its application in makeup.Based on this point, the cationic starch composition of the aqueous solution type of some modifications enters market, can be used for of having process containing keratic substrate can in medium used for cosmetic.This based composition is containing Multiple components, and great majority belong to emulsion or suspended substance, not easily preserve, transport, and need add sanitas, are adjust the bad control of consumption in use to bring certain trouble to cosmetic formulations.
Summary of the invention
Based on this, the object of this invention is to provide a kind of can low temperature gelatinization have conditioning styling cationic starch.
Concrete technical scheme is as follows:
There is a preparation method for the cationic starch of conditioning styling, comprise the steps:
(1) add in mixer by 100 weight starch, then spraying into 4-20 weight part concentration is the aqueous sodium hydroxide solution of 28-32wt%, mixes, and fully sprays into cation modifier after alkalization, fully stirs and obtains starch mixing soup compound; The straight chain of described starch and straight chain ratio are 60:40-85:15;
(2) starch mixing soup compound is distributed in the aqueous solutions of organic solvent of 400-600 weight part, obtains starch suspension slurries;
(3) starch suspension slurries are warming up to 40-80 DEG C, reaction 1.5-3h, then adds acid, it is 5-8 that stirring is neutralized to pH, and adjusting viscosity is to 20-8000mpa.s (1% aqueous solution, 25 DEG C), centrifugal drying, has the cationic starch of conditioning styling described in obtaining.
Wherein in an embodiment, the straight chain of described starch and straight chain ratio are 70:30-80:20.
Wherein in an embodiment, described starch is selected from one or more in W-Gum, tapioca (flour), yam starch, wheat starch, sweet potato starch or waxy starch.
Wherein in an embodiment, in step (3), temperature of reaction is 50-70 DEG C.
Wherein in an embodiment, described cation modifier is 2.3-epoxypropyltrimethylchloride chloride, the chloro-2-hydroxypropyl dimethyl-lauryl ammonium chloride of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, 3-.
Wherein in an embodiment, described aqueous solutions of organic solvent is selected from the combination of one or more and water in methyl alcohol, Virahol, ethanol or acetone, and volumetric concentration is 50-80%.
Wherein in an embodiment, described acid is selected from: a kind of in acetic acid, hydrochloric acid, sulfuric acid.
Another object of the present invention is to provide a kind of cationic starch with conditioning styling.
Concrete technical scheme is as follows:
What above-mentioned preparation method prepared has the cationic starch nursing one's health styling.
Principle of the present invention and beneficial effect as follows:
A kind of cationic starch that the present invention prepares, it has the effect of conditioning sizing to the hair of user, is a kind of degree ofacationic substitution starch ethers of modification, dissolve in cold water (25 DEG C), transmittance is high, and aqueous solution viscosity range is wide, and viscosity has the characteristics such as adjustability.Described cationic starch, for nursing one's health in standardized product, effectively can improve product conditioning shapping function, improve product performance; Coldly operation can be joined in products configuration technique, easy to use; While enhancing product performance, reduce cost, usage quantity is 0.3-1.5%.
Preparation method of the present invention adopts semidrying to carry out premix process, improves paper mill wastewater used when alkalizing starch, thus drastically reduce the area the consumption of alkali, and ensure that the full and uniform of alkalization, decrease the salt content in later stage, thus improve product quality, its saliferous ash content is≤1%.Just because of it, there is less salinity, its salinity brought in formula is also greatly declined, wadding glue can be produced under certain condition because hair care product formula cationic component (as cationic starch, cation guar gum etc.) can be combined with anionic group, increasing of salinity, exacerbate wadding glue generate, so salinity number to clear formula, there is larger meaning.Therefore the cationic starch that obtains of the present invention, it is stable and transparent that its low salt content is more conducive to filling a prescription.
The raw starch preparing described cationic starch in the present invention stems from specific natural phant, its kind can be the one in the starch such as W-Gum, tapioca (flour), yam starch, wheat starch, sweet potato starch, waxy starch, or it is several composite, but finally by the ratio control of the straight chain of raw starch and side chain at 60:40-85:15, wherein to be more preferred from 70:30-80:20.Film mainly owing to producing after the gelatinization of amylose starch institute has more rigidity, shows as firmly crisp, so it is main component; And the film produced after amylopectin gelatinization is more soft, sizing effect is remarkable, but its adjustable final product produce the performance of film, make it not break and become fragile.
Solvent used can be the combination of ethanol, Virahol, methyl alcohol one or more and water, and the volumetric concentration of solvent can be 50%-80%.Solvent can play and suppress cationic starch gelatinization, suppresses the stretching, extension of starch chain, but because the alkali lye such as sodium hydroxide are with cationic reagent is water-soluble and solvability is bad in a solvent, thus need certain moisture to make it dissolve abundant and starch contact reacts.Therefore need to control certain solvent-water ratio, thus control starch chain stretch length, moisture content is crossed and gelatinization can be occurred at most, can not get solid phase prod.Therefore choosing solvent strength is 50%-80%.
Cation modifier used is 2.3-epoxypropyltrimethylchloride chloride, one or more in the replacement nitrification material of the different lengths alkyl chains such as the chloro-2-hydroxypropyl dimethyl-lauryl ammonium chloride of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, 3-press the composite cationic reagent of different ratios, the substituting group of the cationic starch obtained like this has specific chain length and structure, can show different characteristics from during water effect.
Preferred starch, makes it to carry out etherification reaction and follow-up process for refining with cation modifier, thus generates a kind of containing ammonium, with the polymer starch ether derivative of positive charge on nitrogen-atoms.
The cationic starch obtained in the present invention, substitution value is at 0.08-0.15.The cationic starch obtained under this specific substitution value has cold water (25 DEG C) gelatinization performance, simultaneously again can not excessive cationization, makes hair cationic charge too much, causes counter productive.
Cationic starch described in the present invention is white powder.Under normal temperature, can within a short period of time water-soluble, and easily disperse not conglomeration.Described cationic starch has higher cationic degree and prepares through extraordinary, its starch granules crystal region just can be absorbed water from originally arranging state closely at lower temperature (25 DEG C) and become rarefaction, hydrogen bond rupture destroys the associated state of molecule, the double-spiral structure of the starch molecule after water suction stretches formation separate stage, thus reaches the performance of cold water solubles.And because smaller amylose starch oozes out from particle, viscosity greatly increases, transparency is improved transmittance can reach 70-95%.Described cationic starch has that quaternary ammonium salt side chain is many, molecular chain unfolds the micro molecule characteristics such as degree is high; make its active group more easily and hair fiber close; and foam is finer and smoother; ventilative film can be formed at skin or hair surface; there is excellent provide protection, to hair and a kind of smooth, moist sensation well of skin.For in hair washing product, make to have well antistatic and hair conditioning, dry, the wet cardability of hair can be improved, make the submissive easy comb of hair, make hair keep gloss, high resilience; For in bath product, the moisture feeling of skin can be strengthened, for strengthening moisturizing, the silk smooth felling of skin in protective skin cream.
And owing to having lower gelatinization point, in cold water, gelatinization dissolving (25 DEG C) can not need high temperature 95 DEG C of gelatinizations, thus avoid its molecular structure of high temperature, reduce molecular weight, fall low viscous impact.Cationic starch 1% solution viscosity selectable range 20-8000mpa.s (1% aqueous solution, 25 DEG C) can be made.
Cationic starch of the present invention, owing to selecting the starch material with ad hoc structure, through special cation modifier etherificate, makes it have stronger sizing effect, and has good opsonization, with the dual function of shaping and nurse one's health.Shampoo, qualitative dose of hair, face cleaning milk, body wash, setting lotion, moisture-retention gel water (cream), elastin, hair conditioner, treatment wax, Liquid soap, skin care product etc. can be applied to.More can be satisfied with micro-sizing shampoo of man, thus reach and use a kind of material can reach the two-in-one effect of conditioning sizing.
Embodiment
By the following examples the application is further elaborated.
Embodiment 1
Get 100g tapioca (flour) (ratio of straight chain and side chain is 75:25) and add reactor, evenly spray into 4g potassium hydroxide solution (concentration is 30wt%) to mix, alkalize, afterwards, chloro-for 25g cation modifier 3-2-hydroxypropyl dimethyl-lauryl ammonium chloride is sprayed in reactor, carries out fully stirring obtaining starch mixing soup compound.Add in reactor in the aqueous ethanolic solution of 500g (volumetric concentration is 50%), obtain the starch suspension slurries through alkalization.Limit temperature is in 80 DEG C.After reaction 2h, added by acetic acid in reactor, carrying out stirring neutralization is 5-8 to pH, obtains cationic starch suspension slurry.Afterwards, cationic starch suspension slurry is carried out centrifugal, there is described in drying obtains the cationic starch of conditioning styling.
Embodiment 2
40g cassava and 60g W-Gum (ratio of straight chain and side chain is 81:19) are added reactor, evenly spray into sodium hydroxide solution 4.5g (concentration is 30wt%) to mix, alkalize, afterwards, 22g cation modifier 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride is sprayed in reactor, carries out fully stirring obtaining starch mixing soup compound.Add in reactor in the aqueous ethanolic solution of 300g (50% volume content), obtain the starch suspension slurries through alkalization.Limit temperature is in 70 DEG C.After reaction 2.5h, added by hydrochloric acid in reactor, carrying out stirring neutralization is 5-8 to pH, adds excess acid and carries out viscosity adjustment, obtain cationic starch suspension slurry.Afterwards, undertaken centrifugal by cationic starch suspension slurry, drying obtains the cationic starch with conditioning styling.
Embodiment 3
10g tapioca (flour), 75g yam starch, 15g waxy corn starch (ratio of straight chain and side chain is 78:22) are added reactor, evenly spray into potassium hydroxide solution 4g (concentration is 30wt%) to mix, alkalize, afterwards, by 18g cation modifier 2,3 epoxypropyltrimethylchloride chlorides spray in reactor, carry out fully stirring obtaining starch mixing soup compound.Add in reactor in the aqueous ethanolic solution of 200g (50% volume content), obtain the starch suspension slurries through alkalization.Temperature of reaction is defined in 70 DEG C.After reaction 1.5h, added by sulfuric acid in reactor, carrying out stirring neutralization is 5-8 to pH, obtains cationic starch suspension slurry.Afterwards, undertaken centrifugal by cationic starch suspension slurry, drying obtains the cationic starch that can be used for nursing one's health sizing.
Embodiment 4-7, concrete technology is according to table 2.
Reactor will be added according to starch consumption in table 1, evenly spray into sodium hydroxide solution 4.5g to mix, alkalize, afterwards, cation modifier described in table 1 is sprayed in reactor, carry out fully stirring obtaining starch mixing soup compound, add in reactor according to solvent in table 2, obtain the starch suspension slurries through alkalization.Temperature of reaction is defined in 70 DEG C.After reaction 2h, added by acetic acid in reactor, carrying out stirring neutralization is 5-8 to pH, adds excess acid and carries out viscosity adjustment, obtain cationic starch suspension slurry.Afterwards, undertaken centrifugal by cationic starch suspension slurry, drying obtains the cationic starch that can be used for nursing one's health sizing.
Table 1 example 4-7 processing condition
The cationic starch physical index that table 2 example 1-7 obtains
Style-ability is tested:
1, topknot process: by large topknot process growth L=24cm, the topknot of heavy 1g.Hair is placed in the 1000mL beaker being contained in 5g K12 and tap water and is heated to 80 DEG C, soak two hours, repeat secondary, with tap water, until non-foam, then naturally dry.
2, topknot hair gel process: the hair gel sample taking 0.15g and 0.3g, is coated on topknot equably, and twists on the curling iron of 1.2cm.
3, after hair gel process, topknot is placed on 50 DEG C of electro-heating standing-temperature cultivator inner dryings 2 hours, topknot is taken off from curling iron, hang over 30 DEG C, in the fixed temperature and humidity incubator of 80%RH, carry out experiment of taking pictures, and once photo taking experiment was done every one hour, time is 4 hours altogether, detects the length variations of hair.
Curl retention formulae discovery: curl retention %=(L-Lt)/(L-L0) × 100%
Wherein: L---represent the topknot length before making hai roll
L0---represent curl length when taking off from curling iron
Lt---represent the curl length after t hour
Cationic starch style-ability test data obtained by table 3 example 1-7
Lt represents the curl length after t hour
Xt represents the curl retention after t hour (its numeral is higher, represents fixed effect better)
Test according to above example, can find out, prepared example 1-7, according to blank sample, all has good fixed effect.When the straight chain ratio of the special example 2,4,5,6 when straight chain ratio is higher is all more than 80%, show effect of shaping preferably, show constancy especially when cereal starch is more especially obvious.(cereal starch such as: wheat starch, W-Gum etc.), then can have stronger counter productive, such as example 3 and example 7 expression effects to sizing when with the addition of waxy starch.
Hair conditioning is tested
1, the cationic starch of different instances gained is allocated in shampoo formula.
2, get 4 bundles topknot after treatment, a branch of is blank, and other three beams take same method to clean in shampoo respectively.
3, adopt combing tester test carding force size, think that carding force diminishes, hair smoothness, hair conditioning is better.
Table 4 embodiment 1-7 obtains cationic starch application formula topknot and does combing test result
Table 5 embodiment 1-7 obtains cationic starch application formula topknot and to wet combing test result
Test according to above example, can find out, prepared example 1-7 cationic starch, all there is certain dry, wet comb conditioning effect.When amylopection content is higher, (as example 1, example 7) hair conditioning has obvious reinforced effects especially.The example 1,2,7 that degree ofacationic substitution is high also shows and obtains the high conditioning performance of product than other embodiments.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (8)
1. there is a preparation method for the cationic starch of conditioning styling, it is characterized in that, comprise the steps:
(1) add in mixer by 100 weight starch, then spraying into 4-20 weight part concentration is the aqueous sodium hydroxide solution of 28-32wt%, mixes, and fully sprays into cation modifier after alkalization, stirs and obtain starch mixing soup compound; The straight chain of described starch and side chain ratio are 60:40-85:15;
(2) starch mixing soup compound is distributed in the aqueous solutions of organic solvent of 400-600 weight part, obtains starch suspension slurries;
(3) starch suspension slurries are warming up to 40-80 DEG C, reaction 1.5-3h, then adds acid, and stirring and being neutralized to pH is 5-8, centrifugal drying, has the cationic starch of conditioning styling described in obtaining.
2. preparation method according to claim 1, is characterized in that, the straight chain of described starch and side chain ratio are 70:30-80:20.
3. preparation method according to claim 1 and 2, is characterized in that, described starch is selected from one or more in W-Gum, tapioca (flour), yam starch, wheat starch, sweet potato starch or waxy starch.
4. preparation method according to claim 1 and 2, is characterized in that, in step (3), temperature of reaction is 50-70 DEG C.
5. preparation method according to claim 1 and 2, is characterized in that, described cation modifier is 2.3-epoxypropyltrimethylchloride chloride, the chloro-2-hydroxypropyl dimethyl-lauryl ammonium chloride of 3-chloro-2-hydroxypropyl-trimethyl ammonium chloride, 3-.
6. preparation method according to claim 1 and 2, is characterized in that, described aqueous solutions of organic solvent is selected from the combination of one or more and water in methyl alcohol, Virahol, ethanol or acetone, and volumetric concentration is 50-80%.
7. preparation method according to claim 1 and 2, is characterized in that, described acid is selected from: the one in acetic acid, hydrochloric acid, sulfuric acid.
8. what preparation method described in any one of claim 1-7 prepared has the cationic starch nursing one's health styling.
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Cited By (5)
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| CN106279451A (en) * | 2016-08-09 | 2017-01-04 | 广州天赐高新材料股份有限公司 | Cationic starch with high substitution degree and preparation method thereof |
| CN108078796A (en) * | 2017-12-28 | 2018-05-29 | 珠海伊斯佳科技股份有限公司 | A kind of no silicone oil moistens submissive hair film and preparation method thereof |
| CN108486182A (en) * | 2018-03-07 | 2018-09-04 | 四会市格鲁森润滑技术有限公司 | It is a kind of with cationic compatible phosphate microorganism method of modifying |
| CN109678979A (en) * | 2018-12-24 | 2019-04-26 | 江南大学 | A kind of complex denaturation cationic starch and preparation method thereof |
| CN115299435A (en) * | 2022-05-30 | 2022-11-08 | 振德医疗用品股份有限公司 | Disinfection spray with indication function and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106279451A (en) * | 2016-08-09 | 2017-01-04 | 广州天赐高新材料股份有限公司 | Cationic starch with high substitution degree and preparation method thereof |
| CN108078796A (en) * | 2017-12-28 | 2018-05-29 | 珠海伊斯佳科技股份有限公司 | A kind of no silicone oil moistens submissive hair film and preparation method thereof |
| CN108486182A (en) * | 2018-03-07 | 2018-09-04 | 四会市格鲁森润滑技术有限公司 | It is a kind of with cationic compatible phosphate microorganism method of modifying |
| CN109678979A (en) * | 2018-12-24 | 2019-04-26 | 江南大学 | A kind of complex denaturation cationic starch and preparation method thereof |
| CN109678979B (en) * | 2018-12-24 | 2020-11-06 | 江南大学 | Composite modified cationic starch and preparation method thereof |
| CN115299435A (en) * | 2022-05-30 | 2022-11-08 | 振德医疗用品股份有限公司 | Disinfection spray with indication function and preparation method and application thereof |
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