CN104387479B - Cationic starch with conditioning styling and preparation method thereof - Google Patents
Cationic starch with conditioning styling and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of the cationic starch with conditioning styling, comprise the following steps：Alkalinization is carried out to starch with alkali lye, cation modifier is then sprayed into, is sufficiently stirred for obtaining starch mixing slurry；Starch mixing slurry is distributed in aqueous solutions of organic solvent again, obtains starch suspension slurries；40 80 DEG C are warming up to, 1.5 3h are reacted, acid is subsequently adding, it is 58 that stirring is neutralized to pH, last centrifugal drying, obtains final product the cationic starch with conditioning styling.Cationic starch of the present invention, starch material of the selection with ad hoc structure, is etherified by special cation modifier, makes it have stronger sizing effect, and with preferable opsonic action, with sizing and the double action of conditioning.
Description
Technical field
The present invention relates to macromolecular compound technical field, more particularly to a kind of cation with conditioning styling
Starch and preparation method thereof.
Background technology
Hair fixing principle is that can be combined closely with hair, and forms a kind of film outside, and its film need to have soft
Toughness, intensity and elasticity, and enemy delivers now good compatibility and adhesiveness, it is difficult for drop-off.At present, as hairspray
Film forming agent is mainly polyvinylpyrrolidone or its copolymer, and model has K30, K90 etc..The gas of polyvinylpyrrolidone film
Wait adaptability poor, in a humid environment can the moisture absorption, the hardness reduction of film, forfeiture style-ability；Become in dry environment
It is crisp brittle.The polymer of vinyl pyrrolidine ketone and the poor compatibility of alkanes propellant, it is only compatible with freon propellant
Property is good.Freon is to make one of destroyed reason of atmospheric ozone layer, and earth environment is polluted.With starch, cellulose, melon
You compare the natural high molecular substance of glue plant origin, the biological degradability and being compatible with the environment property of polyvinylpyrrolidone film
It is than relatively low.Because hair styling product is resident product, it is desirable to which setting agent must safety non-toxic.
Starch has cheap, renewable, never exhaustion, biodegradable, environmental protection protrusion compared with industrial chemicals
Advantage.
The wide variety of hair conditioning cation type water-soluble polymer compound of daily use chemicals industry be cation guar gum, sun from
The cationic polysaccharides material such as sub- hydroxyethyl cellulose.It has flexibility, hair conditioning, moisture-keeping functions, and easily rinses, and
Dual-use function with polysaccharide and cationic surfactant, can comparatively fast form when the anion binding during it is with formula
Colloid, wraps up silicone oil, the material fast deposition such as anti-dandruff of formula on hair, so as to reach opsonic action.Cationic starch, because
It has the polysaccharide and cation group of long-chain, so it is as widely used guar gum, cellulose cationic derivative
With good conditioning performance, and because starch can form the just right polymeric membrane with certain toughness, so as to reach
Conditioning sizing effect.Meanwhile, its Starches than guar gum and hydroxyethyl cellulose then have extremely obvious wide material sources,
The advantage of low cost.Cationic starch equally have it is antistatic, suspend, thickening, the effect such as qualitative, and with hair and the angle of skin
Albumen has good compatibility, gently, excitant of the detergent to skin can be reduced, under relatively low consumption, i.e., with fine
Suspension, thickening capabilities.
Therefore cationic starch is applied as conditioner and is favored very much in cosmetics, but because of its gelatinization point
Height, can just be dissolved in water more than 95 DEG C, and very big difficulty is brought to operating procedure in Cosmetic Manufacture, limit it in cosmetics
In application.Based on this point, the cationic starch composition of some modified aqueous solution types enters market, and can be used for of having is processed
Substrate containing keratin can be in medium used for cosmetic.This based composition contains Multiple components, most of to belong to emulsion or outstanding
Float, not easy to maintain, transport, and preservative need to be added, it is that the bad control of adjustment consumption brings when in use to cosmetic formulations
Certain trouble.
The content of the invention
Based on this, it is an object of the invention to provide a kind of cation shallow lake with conditioning styling for being capable of low temperature gelatinization
Powder.
Specific technical scheme is as follows：
A kind of preparation method of the cationic starch with conditioning styling, comprises the following steps：
(1) by 100 weight starch addition batch mixer, it is then sprayed into the hydrogen that 4-20 weight portions concentration is 28-32wt%
Aqueous solution of sodium oxide, is well mixed, and fully sprays into cation modifier after alkalization, is sufficiently stirred for obtaining starch mixing slurry；
The straight chain and side chain ratio of the starch are 60:40-85:15；
(2) starch mixing slurry is distributed in the aqueous solutions of organic solvent of 400-600 weight portions, obtains starch suspension
Slurries；
(3) starch suspension slurries are warming up to 40-80 DEG C, react 1.5-3h, be subsequently adding acid, stirring is neutralized to pH for 5-
8, regulation viscosity to 20-8000mpa.s (1% aqueous solution, 25 DEG C), centrifugal drying, obtaining final product described has conditioning styling
Cationic starch.
Wherein in one embodiment, the straight chain and side chain ratio of the starch are 70:30-80：20.
Wherein in one embodiment, the starch be selected from cornstarch, tapioca, farina, wheaten starch,
One or more in starch from sweet potato or waxy starch.
Wherein in one embodiment, reaction temperature is 50-70 DEG C in step (3).
Wherein in one embodiment, the cation modifier is 2.3- epoxypropyltrimethylchloride chlorides, the chloro- 2- of 3-
The chloro- 2- hydroxypropyl dimethyls-lauryl ammonium chloride of hydroxypropyl-trimethyl ammonium chloride, 3-.
Wherein in one embodiment, the aqueous solutions of organic solvent is selected from methyl alcohol, isopropanol, ethanol or acetone
Plant or several and water combination, volumetric concentration is 50-80%.
Wherein in one embodiment, the acid is selected from：It is a kind of in acetic acid, hydrochloric acid, sulfuric acid.
It is a further object of the present invention to provide a kind of cationic starch with conditioning styling.
Specific technical scheme is as follows：
The cationic starch with conditioning styling that above-mentioned preparation method is prepared.
Principle of the invention and have the beneficial effect that：
A kind of cationic starch that the present invention is prepared, its hair to user has the effect of conditioning sizing, is
A kind of modified degree ofacationic substitution starch ether, dissolves in cold water (25 DEG C), and light transmittance is high, and aqueous solution viscosity range is wide, viscosity
With characteristics such as adjustabilitys.During described cationic starch is used to nurse one's health approved product, product conditioning sizing work(can be effectively improved
Can, improve properties of product；Can be cold with operation in products configuration technique, it is easy to use；While enhancing product performance, reduce
Cost, usage amount is 0.3-1.5%.
Preparation method of the invention carries out premix treatment using semidry method, the concentration of alkali used when improving alkalization starch, from
And the consumption of alkali is drastically reduce the area, and the full and uniform of alkalization is ensure that, the salt content in later stage is reduced, so as to improve
Product quality, its saliferous ash content is≤1%.There is less salinity just because of it, the salinity for making it bring into formula
Greatly decline, because hair care product is formulated cationic component (such as cationic starch, cation guar gum) meeting and anion group
Divide to combine and can produce wadding glue under certain condition, and increasing for salinity, wadding glue generation is exacerbated, so how many pairs of salinity are saturating
Bright formula has larger meaning.Therefore the present invention obtained by cationic starch, its low salt content be more beneficial for formula
Stabilization and the transparency.
The raw starch that the cationic starch is prepared in the present invention is derived from specific natural plants, and its species can be jade
One kind in the starch such as rice starch, tapioca, farina, wheaten starch, starch from sweet potato, waxy starch, or it is several multiple
Match somebody with somebody, but finally by the ratio control of the straight chain of raw starch and side chain 60:40-85:15, wherein more preferably 70:30-80:
20.The film produced after being gelatinized mainly due to amylose is hard crisp with more rigidly, showing as, so it is main component；
And film produced after amylopectin gelatinization is more soft, sizing effect is not notable, but its film produced by adjustable final product
Performance, it is not ruptured and become fragile.
Solvent used can be ethanol, isopropanol, methyl alcohol one or more combinations with water, and the volumetric concentration of solvent can
Think 50%-80%.Solvent can play suppression cationic starch gelatinization, suppress the stretching, extension of starch chain, but because hydrogen-oxygen
Change that the alkali lye such as sodium and cationic reagent are dissolved in water and dissolubility is bad in a solvent, so as to need certain moisture to dissolve it
Fully with starch haptoreaction.Therefore solvent-water the ratio for needing control certain, so as to control starch chain spread length, water
Part is crossed and can be at most gelatinized, and cannot get solid product.Therefore it is 50%-80% to choose solvent strength.
Cation modifier used is 2.3- epoxypropyltrimethylchloride chlorides, the chloro- 2- Hydroxyproyl Trimethyls chlorinations of 3-
One kind in the substitution nitrification material of the different length alkyl chains such as the chloro- 2- hydroxypropyl dimethyls-lauryl ammonium chloride of ammonium, 3-
Or several cationic reagents compounded by different proportion, the substitution base of the cationic starch for so obtaining has specific chain length
With structure, different characteristics can be shown when being acted on from water.
Preferred starch, is allowed to carry out etherification reaction and follow-up process for refining with cation modifier, so as to generate one kind
Containing ammonium, the macromolecule starch ether derivative with positive charge on nitrogen-atoms.
Resulting cationic starch in the present invention, substitution value is in 0.08-0.15.The sun obtained under the specific substitution value
Ionic starch has (25 DEG C) gelatinization performances of cold water, while will not excessively be cationized again, makes hair cationic charge excessive, leads
Cause counter productive.
Heretofore described cationic starch, is white powder.Under normal temperature, water can be within a short period of time dissolved in, and easily
Dispersion not conglomeration.Described cationic starch has cationic degree higher and is prepared by extraordinary, crystallizes its starch granules
Region can just absorb water at relatively low temperature (25 DEG C) and be changed into rarefaction from arranging close state originally, and hydrogen bond fracture is broken
The associated state of molecule is broken, the double-spiral structure of the starch molecule after water suction stretches to form released state, so as to reach cold water
Solvable performance.And because smaller amylose oozes out from particle, viscosity is greatly increased, and transparency is improved
Light rate is up to 70-95%.It is special that described cationic starch has that quaternary ammonium salt side chain is more, strand unfolds the micro molecules such as degree is high
Property, it is easier its active group close with hair fiber, and foam is finer and smoother, can be formed in skin or hair surface
The film of gas, with excellent protective effect, gives hair and skin a kind of good smooth, moist sensation.Produced for having one's hair wash
In product, make that there is good antistatic and hair conditioning, the dry of hair, wet cardability can be improved, make the submissive easy comb of hair, make hair
Keep gloss, high resilience；In for bath product, the moisture feeling of skin can be strengthened, the guarantor for strengthening skin in face cream
Wet, silk smooth felling.
And do not need 95 DEG C of pastes of high temperature due to (25 DEG C) of dissolving with relatively low gelatinization point, can be gelatinized in cold water
Change, so as to avoid high temperature its molecular structure, reduce molecular weight, drop low viscous influence.Cationic starch 1% can be made
Solution viscosity selectable range 20-8000mpa.s (1% aqueous solution, 25 DEG C).
Cationic starch of the present invention, due to starch material of the selection with ad hoc structure, by special cation
Modifying agent is etherified, and makes it have stronger sizing effect, and with preferable opsonic action, with the double of sizing and conditioning
Recast is used.Can apply to be applied to qualitative dose of shampoo, hair, mildy wash, shower cream, setting lotion, moisture-retention gel water (cream),
Elastin, hair conditioner, treatment waxes, hand cleanser, skin care item etc..Micro- sizing shampoo of man can be more satisfied with, made so as to reach
It is that can reach the two-in-one effect of conditioning sizing with a kind of material.
Specific embodiment
The application is further elaborated by the following examples.
Embodiment 1
(ratio of straight chain and side chain is 75 to take 100g tapiocas:25) reactor is added, it is uniform to spray into 4g potassium hydroxide
Solution (concentration is 30wt%) is well mixed, and is alkalized, afterwards, by the chloro- 2- hydroxypropyls diformazans of 25g cation modifiers 3-
Base-lauryl ammonium chloride is sprayed into reactor, carries out being sufficiently stirred for obtaining starch mixing slurry.Added in reactor
In the ethanol water of 500g (volumetric concentration is 50%), the starch suspension slurries by alkalizing are obtained.Limit temperature is in 80 DEG C.
After reaction 2h, by acetic acid addition reactor, it is 5-8 to be stirred neutralization to pH, obtains cationic starch suspension slurry.It
Afterwards, cationic starch suspension slurry is centrifuged, is dried to obtain the cationic starch for having and nursing one's health styling.
Embodiment 2
By 40g cassavas and 60g cornstarch, (ratio of straight chain and side chain is 81：19) reactor is added, hydrogen is uniformly sprayed into
Sodium hydroxide solution 4.5g (concentration is 30wt%) is well mixed, and is alkalized, afterwards, by the chloro- 2- hydroxyls of 22g cation modifiers 3-
Hydroxypropyltrimonium chloride is sprayed into reactor, carries out being sufficiently stirred for obtaining starch mixing slurry.Added in reactor
In the ethanol water of 300g (50% volume content), the starch suspension slurries by alkalizing are obtained.Limit temperature is in 70 DEG C.Instead
It is 5-8 by neutralization in hydrochloric acid addition reactor, is stirred to pH after answering 2.5h, adds excess acid to carry out viscosity regulation, obtains
Cationic starch suspension slurry.Afterwards, cationic starch suspension slurry is centrifuged, is dried to obtain with conditioning styling
Cationic starch.
Embodiment 3
By 10g tapiocas, 75g farinas, 15g waxy corn starch, (ratio of straight chain and side chain is 78:22)
Reactor, uniform potassium hydroxide solution 4g (concentration is 30wt%) that sprays into is added to be well mixed, alkalized, afterwards, by 18g sun
The epoxypropyltrimethylchloride chloride of ion modification agent 2,3 is sprayed into reactor, carries out being sufficiently stirred for obtaining starch mixing slurry.
In the ethanol water for adding 200g (50% volume content) in reactor, the starch suspension slurries by alkalizing are obtained.Instead
Limit temperature is answered in 70 DEG C.Reaction 1.5h after, will sulfuric acid add reactor in, be stirred neutralization to pH be 5-8, obtain sun from
Sub- starch suspension slurries.Afterwards, cationic starch suspension slurry is centrifuged, be dried to obtain can be used for nurse one's health sizing sun from
Sub- starch.
Embodiment 4-7, concrete technology is according to table 2.
Reactor, the uniform sodium hydroxide solution 4.5g that sprays into will be added to be well mixed according to starch consumption in table 1, carry out alkali
Change, afterwards, by the penetrating reactor of cation modifier described in table 1, carry out being sufficiently stirred for obtaining starch mixing slurry, press
According to solvent addition reactor in table 2, the starch suspension slurries by alkalizing are obtained.Reaction temperature is defined in 70 DEG C.Reaction 2h
Afterwards, it is 5-8 by neutralization in acetic acid addition reactor, is stirred to pH, adds excess acid to carry out viscosity regulation, obtains cation
Starch suspension slurries.Afterwards, cationic starch suspension slurry is centrifuged, is dried to obtain the cation that can be used for nursing one's health sizing
Starch.
The example 4-7 process conditions of table 1
The cationic starch physical index that the example 1-7 of table 2 is obtained
Style-ability is tested：
1st, topknot treatment：Big topknot is processed into growth L=24cm, the topknot of weight 1g.Hair is placed on mounted in 5g K12
Be heated to 80 DEG C in the 1000mL beakers of running water, soak two hours, repeat secondary, rinsed with running water, until non-foam,
Then dry naturally.
2nd, topknot gel water process：The gel water sample of 0.15g and 0.3g is weighed, is evenly coated on topknot, and roll up
On the curling iron of 1.2cm.
3rd, topknot is placed on drying 2 hours in 50 DEG C of electro-heating standing-temperature cultivators after gel water process, by topknot from curly hair
Removed on rod, hang over 30 DEG C, in the constant temperature and humidity incubator of 80%RH, carry out experiment of taking pictures, and once clap per doing every other hour
According to the facts test, the time is altogether 4 hours, detects the length change of hair.
Curl retention formula is calculated：Curl retention %=(L-Lt)/(L-L0) × 100%
Wherein：L --- the topknot length before hai roll is done in expression
L0 --- represent curl length when being removed from curling iron
Lt --- the curl length after representing t hours
Cationic starch style-ability test data obtained by the example 1-7 of table 3
Lt represents the curl length after t hours
Xt represents the curl retention after t hours (its numeral is higher, represents fixed effect better)
Tested according to above example, it can be seen that prepared example 1-7 contrasts blank sample, be respectively provided with preferably sizing
Effect.When especially the straight chain ratio of example 2,4,5,6 is more than 80% when straight chain ratio is higher, work(of preferably shaping is shown
Effect, performance constancy is especially apparent especially when cereal starch is more.(cereal starch is for example：Wheaten starch, cornstarch etc.),
And can then have stronger counter productive to sizing when with the addition of waxy starch, such as 7 expression effects of example 3 and example.
Hair conditioning is tested
1st, by the cationic starch obtained by different instances allocate into shampoo formula in.
2nd, 4 beams topknot after treatment is taken, a branch of is blank, other three beams take same method in shampoo respectively
Cleaning.
3rd, carding force size is tested using combing tester, it is believed that carding force diminishes, and hair smoothness, hair conditioning is better.
The embodiment 1-7 of table 4 is obtained the cationic starch application dry combing test result of formula topknot
The embodiment 1-7 of table 5 is obtained the cationic starch application formula wet combing test result of topknot
Tested according to above example, it can be seen that prepared example 1-7 cationic starches, be respectively provided with it is certain it is dry,
Wet comb conditioning effect.Especially when amylopectin content is higher, (such as example 1, example 7) hair conditioning has obvious enhancing effect.
Degree ofacationic substitution example 1,2,7 high also shows to obtain product conditioning performance high than other embodiment.
Embodiment described above only expresses several embodiments of the invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention
Shield scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (7)
1. it is a kind of with conditioning styling cationic starch preparation method, it is characterised in that comprise the following steps：
(1) by 100 weight starch addition batch mixer, it is then sprayed into the hydroxide that 4-20 weight portions concentration is 28-32wt%
Sodium water solution, is well mixed, and fully sprays into cation modifier after alkalization, is uniformly mixing to obtain starch mixing slurry；It is described
The straight chain and side chain ratio of starch are 60:40-85:15；
The addition of the cation modifier is 16-25 with the weight part ratio of starch addition:100；
The cation modifier is 2,3- epoxypropyltrimethylchloride chlorides, 3- chloro-2-hydroxypropyl-trimethyl ammonium chlorides, 3-
Chloro- 2- hydroxypropyl dimethyls-lauryl ammonium chloride；
(2) starch mixing slurry is distributed in the aqueous solutions of organic solvent of 400-600 weight portions, obtains starch suspension slurry
Liquid；
(3) starch suspension slurries are warming up to 40-80 DEG C, react 1.5-3h, be subsequently adding acid, stirring is neutralized to pH for 5-8, from
The heart is dried, and obtains final product the cationic starch for having and nursing one's health styling.
2. preparation method according to claim 1, it is characterised in that the straight chain and side chain ratio of the starch are 70:30-
80:20。
3. preparation method according to claim 1 and 2, it is characterised in that the starch is selected from cornstarch, para arrowroot
One or more in powder, farina, wheaten starch, starch from sweet potato or waxy starch.
4. preparation method according to claim 1 and 2, it is characterised in that reaction temperature is 50-70 DEG C in step (3).
5. preparation method according to claim 1 and 2, it is characterised in that the aqueous solutions of organic solvent is selected from methyl alcohol, different
One or more combinations with water in propyl alcohol, ethanol or acetone, volumetric concentration is 50-80%.
6. preparation method according to claim 1 and 2, it is characterised in that the acid is selected from：In acetic acid, hydrochloric acid, sulfuric acid
It is a kind of.
7. the cationic starch with conditioning styling that preparation method described in any one of claim 1-6 is prepared.
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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 |
| CN108078796B (en) * | 2017-12-28 | 2019-12-31 | 珠海伊斯佳科技股份有限公司 | Silicone-oil-free moistening and smoothing hair mask 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 |
| 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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| JP2010180320A (en) * | 2009-02-05 | 2010-08-19 | Kao Corp | Method for producing cationized starch |
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