CN101967200B - Acetylated hydroxypropyl potato starch, preparation method thereof and application thereof - Google Patents
Acetylated hydroxypropyl potato starch, preparation method thereof and application thereof Download PDFInfo
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- CN101967200B CN101967200B CN2010101192617A CN201010119261A CN101967200B CN 101967200 B CN101967200 B CN 101967200B CN 2010101192617 A CN2010101192617 A CN 2010101192617A CN 201010119261 A CN201010119261 A CN 201010119261A CN 101967200 B CN101967200 B CN 101967200B
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Abstract
The invention provides acetylated hydroxypropyl potato starch, a preparation method thereof and application thereof. The preparation method comprises the steps of: performing an etherification reaction of potato starch by adopting epoxypropane to obtain hydroxypropyl potato starch; and performing an etherification reaction by adopting acetic anhydride. The acetylated hydroxypropyl potato starch prepared according to the preparation method has the advantages of good hydrophily, vicidity and emulsibility, low pasting temperature, transparent paste liquid, weak retrogradation, high stability, high temperature resistance, acidic environment resistance, high freeze thawing stability and the like.
Description
Technical field
The application relates to a kind of preparation method of acetylated hydroxypropyl potato starch, reaches the acetylated hydroxypropyl potato starch and the purposes that prepare according to the method.
Background technology
The proportion that accounts for gross national product along with foodstuffs industry increases, and needs a large amount of foodstuff additive.Starch is as the basic material of foodstuffs industry, because the catabiosis that its structure and performance produce, and can not satisfy the quality stability of Food storage and processing, therefore need to be with its sex change processing.From the forties in 20th century, west economy developed country begins the large-scale production modified starch, and U.S. food reaches more than 500 kinds with modified starch, and consumption is more than 500,000 tons.The development and production of China's modified starch is started late, but development is very fast, begins to take shape through the development in more than 20 years.In recent years, along with the Economic development of China, every profession and trade increases year by year to the demand of modified starch.
Hydroxypropylated starch is that starch and propylene oxide react a class non-ionic type modified starch that makes, because etherification reaction has changed the character of starch, hydroxypropylated starch is widely used in many industrial circles, such as in field of food, being used as additive (thickening material, suspension agent emulsifying agent etc.), in daily-use chemical industry, be used as tackiness agent etc.But find in long-term application, the hydroxypropylated starch viscosity is poor, emulsifying property is low, the heavy property of its anti-freezing is poor and the problem such as stable deficiency, also have when in acidic food, using hydroxypropylated starch due Heterosis insufficient.
The inventor is for overcoming the existing shortcoming of hydroxypropylated starch; carried out a large amount of research; unexpectedly find; select the yam starch of abundant raw material to make raw material; the preparation hydroxypropyl potato starch; and it is carried out acetylize process, the composite modified starch for preparing has solved the existing problem of hydroxypropylated starch in the prior art.
Summary of the invention
The invention provides a kind of preparation method of acetylated hydroxypropyl potato starch; it comprises yam starch, expansion inhibitor and catalyzer soluble in water; regulate pH value to alkalescence; add propylene oxide and carry out etherification reaction, obtain hydroxypropyl potato starch, then regulate pH value to pH=8.20-8.40; add again acetic anhydride and carry out esterification; in after reaction finishes and PH to slightly acidic, washing, dry, pulverize and sieve, obtain acetylated hydroxypropyl potato starch.
In above-mentioned preparation method, described expansion inhibitor is selected from anhydrous sodium sulphate, sodium-chlor; Described catalyzer is selected from sodium hydroxide, potassium hydroxide, calcium hydroxide, quaternary ammonium hydroxide; Described propylene oxide preferably adopts 6-9% weight, the propylene oxide of preferred 7.0% weight; Described acetic anhydride preferably adopts the acetic anhydride of 2.5-3.5%; Regulate pH value can adopt 3.8%-4.2% to alkalescence alkali lye, preferred 4.0% sodium hydroxide lye carries out, and preferably is adjusted to pH=10.90-11.30, such as pH=11.10-11.20; The degree Beaume of emulsion is at 24.0-27.5Be; In and PH can adopt the hydrochloric acid of 9-11% to carry out to slightly acidic, preferably be neutralized to pH=8.20-8.40, such as pH=8.30; The sieve aperture that sieves is the 80-100 order, such as 90 orders.
In above-mentioned preparation method, yam starch, the expansion inhibitor, catalyzer, the part by weight of water can be 42: 5.7: 0.3: 52-44: 5.7: 0.3: 50, be preferable over 43: 5.7: 0.3: 51, yam starch and propylene oxide are (herein, weighing scale with pure propylene oxide, such as for the propylene oxide of 98.7% (w/w) then take the weighing scale of the pure propylene oxide that wherein comprises) part by weight as 100: 6-100: 9, be preferable over 100: 7, yam starch and acetic anhydride are (herein, weighing scale with pure acetic anhydride, such as for the acetic anhydride of 99.6% (w/w) then take the weighing scale of the pure acetic anhydride that wherein comprises) part by weight as 200: 5-200: 7, be preferable over 200: 6.
In above-mentioned preparation method, in the etherification reaction, regulate pH value to alkalescence, preferably stirred 20-60 minute, such as 30-50 minute, 40 minutes, the churning time behind the adding propylene oxide was 1-3 hour, preferred 2 hours, be heated to afterwards 42-43 ℃ and react, the reaction times can be 20-24 hour, such as 22 hours; The reaction times of esterification was 1-3 hour, such as 2 hours.
In above-mentioned preparation method, washing can adopt any washing methods known in the art to use soft water or pure water to wash, such as adopting the eddy flow washer to wash; Dry and pulverize and also can adopt any drying known in the art and breaking method to carry out, can be first dewater minute to≤45% with the Centrifugal peeling blade machine such as drying, pass through again air stream drying moisture extremely≤15%.
In a preferred scheme, a kind of preparation method of acetylated hydroxypropyl potato starch is provided, it comprises the steps:
1) sizes mixing: will be based on the anhydrous Na of starch weight 13.26%
2SO
4In the water that is dissolved in based on starch weight 0.7% solid NaOH based on 1.18 times of starch weight, then with load weighted starch dissolution in mentioned solution, stir, obtain starch milk;
2) add alkali lye (preferred 3.8-4.2%, w/w) in starch milk etherificate: to step 1) to pH=10.90-11.30, such as pH=11.10-11.20, stir half an hour; Add based on starch weight 7.0% propylene oxide, sealing was stirred one hour again; Starch milk is warming up to 42 ℃-43 ℃, when being warming up to 40 ℃, the beginning clock reaction, whole reaction process is kept temperature of reaction 42-43 ℃; React and cool off after 20-24 hour, be neutralized between the pH=8.20-8.40;
3) esterification: the acetic anhydride that adds 2.5-3.5% carries out esterification, adds simultaneously alkali lye (preferred 3.8-4.2%, w/w) and keeps PH between 8.20-8.40;
4) neutralization: after reaction finishes, be neutralized to pH=5.0-6.5 with the hydrochloric acid of 9-11%;
5) washing, dry, pulverize and sieve, obtain finished product.
Preparation method's of the present invention technological operation is simple, constant product quality, and raw potatoes is abundant, is convenient to industrialized production, and with low cost, and economic benefit is high.
The invention provides a kind of acetylated hydroxypropyl potato starch; it prepares according to preparation method of the present invention; it has wetting ability; better toughness, emulsifying property; gelatinization point is low, paste liquid is transparent, and a little less than the retrogradation, stability is high; energy is high temperature resistant, the impact of anti-acid environment, the freeze-thaw stability advantages of higher.
Prepare after the acetylated hydroxypropyl potato starch according to preparation method of the present invention, it can be packed, for example adopt 20-25kg/ bag form packing.
The present invention also provides the purposes of described acetylated hydroxypropyl potato starch, is used for especially food-processing, as foodstuff additive, such as thickening material, stablizer, emulsifying agent or pore forming material etc.For example, the hydroxypropyl modified starch is stable high on ionogen and the impact of different pH value, is specially adapted in the high and acidic food of saltiness, as adds in the concentrated orange juice, can make good fluidity, places not stratifiedly, and nothing precipitates; Be applied in soup stock, the soy sauce, can obtain better suspending stabilized effect; As the base-material of chewing gum, can embody preferably elasticity and chewing; Be applied in the ice-creams can improve whipability and the rate of expansion of ice cream mix, and to play the effect of fat-replacer as emulsifying agent and pore forming material; Be applied in the food such as beverage, jam, ice-creams, jelly as thickening material or stablizer, can replace or the natural gum (comprising gum arabic, agar, gelatin, pectin etc.) of Partial Replacement costliness; Be applied in the noodles, can reduce the degree of bringing back to life of starch, the quality of noodles, solubility rate are improved.
In the present invention, the measuring method of molar substitution and degree of substitution with acetyl group can adopt measuring method known in the art, also can adopt the following measuring method that provides.
1. the measuring method of molar substitution:
Take by weighing respectively 0.05-0.1g acetylated hydroxypropyl potato starch and untreated yam starch (potato ative starch) and place the 100ml volumetric flask, add 25ml 0.5mol/L sulfuric acid, be heated to sample in 100 ℃ of water-baths and dissolve fully.Be cooled to room temperature, with distilled water diluting to scale.Draw this solution of 1ml in the 25ml color-comparison tube, place frozen water, slowly add the 8ml vitriol oil, should avoid local superheating in the operation, in case the volatilization of anti-avulsion water rearrangement product is overflowed.In 100 ℃ of water-baths, heat 3min after mixing, put into immediately ice bath and cool off.Carefully add 0.6ml 3% ninhydrin solution along tube wall, shake up immediately, in 25 ℃ of water-baths, place 100min, arrive scale with diluting concentrated sulfuric acid again.Topple over mixing (noting not vibration).Leave standstill 5min, in the 595nm place, make reference with reagent blank with the 1cm cuvette, measure absorbancy, find the content of corresponding propylene glycol at typical curve, the deduction ative starch is blank, be multiplied by reduction factor 0.7763, namely get hydroxypropyl content, obtain molar substitution by following formula:
MS＝2.84wH/(100-w
H)
Reaction efficiency=W
H/ M
In the formula: MS-----is the molar substitution of hydroxypropylated starch
w
H-----is the content (%) of hydroxypropyl
2.84---massfraction changes into the reduction factor of MS
M------adds the percentage amounts of going back Ethylene Oxide
2. the measuring method of degree of substitution with acetyl group
5g (moisture free dry weight) starch sample of accurate weighing is changed in the 500ml iodine flask carefully, add 50ml water and shake up (hand), drip 3 phenolphthalein indicators, being titrated to pink with 0.1mol/LNaOH solution does not just disappear and is terminal point, move with the 25ml transfer pipet again and add 0.25mol/L NaOH solution 25ml in iodine flask, the limit edged rocks, with the good flask of stopper plug, after putting velocity-modulated oscillator middling speed jolting 30min, take off stopper, with a small amount of distilled water wash stopper and bottleneck, till just disappearing to pink with alkali lye excessive in the 0.25mol/L HCL standardized solution titration sample, write down the HCL standardized solution volume V that consumes this moment
1(ml).
Blank assay: accurately take by weighing 5g (moisture free dry weight) ative starch, determination step is the same, writes down and consumes HCL liquor capacity V
2(ml).
The result calculates
Ethanoyl (%)=[(V
1-V
2) * C * 0.043/m] * 100
DS=(162 * ethanoyl %)/(4300-42 * ethanoyl)
C titration hydrochloric acid standard solution concentration (mol/L)
V
1The volume number (mL) of sample quota of expenditure hydrochloric acid soln
V
2The volume number (mL) of the standard salt acid solution that blank assay consumes
The weight of M absolute dried sample (g)
Description of drawings
Fig. 1 is the viscosimetric analysis figure of the acetylated hydroxypropyl potato starch for preparing of embodiment 1.
Fig. 2 is the viscosimetric analysis figure of the acetylated hydroxypropyl potato starch for preparing of embodiment 2.
Fig. 3 is the viscosimetric analysis figure of the acetylated hydroxypropyl potato starch for preparing of embodiment 3.
Fig. 4 is the viscosimetric analysis figure of the acetylated hydroxypropyl potato starch for preparing of embodiment 4.
Annotate: 1 curve represents viscograph; 2 represent the actual temperature curve; 3 represent the design temperature curve.
Embodiment
The below further elaborates the present invention with reference to embodiment, but it will be appreciated by those skilled in the art that but the present invention is not limited to the method for these embodiment and use.And those skilled in the art can carry out it is equal to replacement, combination, improvement or modification to the present invention according to description of the invention, but these all will comprise within the scope of the invention.
The preparation of embodiment 1 acetylated hydroxypropyl potato starch
Prepare in accordance with the following steps acetylated hydroxypropyl potato starch:
1) sizes mixing: with the 28.5Kg anhydrous Na
2SO
4Be dissolved in the 260kg water with 15kg solid NaOH, then the 210kg yam starch be dissolved in the solution, stir, obtain starch milk;
2) sodium hydroxide lye of adding 3.8% stirs half an hour to pH=10.90 in starch milk etherificate: to step 1); The propylene oxide that adds again 12.6Kg, sealing was stirred one hour, and starch milk is warming up to 42 ℃-43 ℃; React and cool off after 20 hours, be neutralized to pH=8.20;
3) esterification: add acetic anhydride 5.25Kg and carry out esterification, add simultaneously the 3.8-% sodium hydroxide lye and keep PH between 8.20-8.40;
4) neutralization: after reaction finished, the hydrochloric acid with 9% was neutralized to pH=5.5;
5) washing: adopt the eddy flow washer to wash; Dry: as to dewater minute to≤45% with the Centrifugal peeling blade machine first, pass through again air stream drying moisture extremely≤15%; Pulverize: pulverize with pulverizer; Sieve: cross 80 mesh sieves, obtain finished product;
6) packing (choosing wantonly): adopt 20-25kg/ bag form packing.
The molar substitution MS=0.015 of the acetylize hydroxypropylated starch that this embodiment prepares, DS=0.049, the viscosity of mensuration is referring to Fig. 1.
The preparation of embodiment 2 acetylated hydroxypropyl potato starchs
Prepare in accordance with the following steps acetylated hydroxypropyl potato starch:
1) sizes mixing: with the 28.5kg anhydrous Na
2SO
4Be dissolved in the 255kg water with 1.5kg solid NaOH, then the 215kg yam starch be dissolved in the solution, stir, obtain starch milk;
2) sodium hydroxide lye of adding 4.2% stirs half an hour to pH=11.30 in starch milk etherificate: to step 1); The propylene oxide that adds again 15.05Kg, sealing was stirred one hour, and starch milk is warming up to 42 ℃-43 ℃; React and cool off after 24 hours, be neutralized to pH=8.20;
3) esterification: add acetic anhydride 6.45Kg and carry out esterification, add simultaneously 4.2% sodium hydroxide alkali and keep PH 8.40;
4) neutralization: after reaction finished, the hydrochloric acid with 11% was neutralized to pH=6.0;
5) washing: adopt the eddy flow washer to wash; Dry: as to dewater minute to≤45% with the Centrifugal peeling blade machine first, pass through again air stream drying moisture extremely≤15%; Pulverize: pulverize with pulverizer; Sieve: cross 100 mesh sieves, obtain finished product;
6) packing (choosing wantonly): adopt 20-25kg/ bag form packing.
The molar substitution MS=0.211 of the acetylated hydroxypropyl potato starch that this embodiment prepares, DS=0.053, the viscosity of mensuration is referring to Fig. 2.
The preparation of embodiment 3 acetylated hydroxypropyl potato starchs
Prepare in accordance with the following steps acetylated hydroxypropyl potato starch:
1) sizes mixing: with the 28.5kg anhydrous Na
2SO
4Be dissolved in the 255kg water with 1.5kg solid NaOH, then the 215kg yam starch be dissolved in the solution, stir, obtain starch milk;
2) sodium hydroxide lye of adding 3.8% stirs half an hour to pH=11.10 in starch milk etherificate: to step 1); The propylene oxide that adds again 17.2kg, sealing was stirred one hour, and starch milk is warming up to 41 ℃-42 ℃; React and cool off after 22 hours, be neutralized to pH=8.30;
3) esterification: add acetic anhydride 6.45Kg and carry out esterification, add simultaneously 4.0% sodium hydroxide lye and keep PH 8.20;
4) neutralization: after reaction finished, the hydrochloric acid with 10% was neutralized to pH=6.5;
5) washing: adopt the eddy flow washer to wash; Dry: as to dewater minute to≤45% with the Centrifugal peeling blade machine first, pass through again air stream drying moisture extremely≤15%; Pulverize: pulverize with pulverizer; Sieve: cross 90 mesh sieves, obtain finished product;
6) packing (choosing wantonly): adopt 20-25KG/ bag form packing.
The molar substitution MS=0.235 of the acetylize hydroxypropylated starch that this embodiment prepares, DS=0.053, the viscosity of mensuration is referring to Fig. 3.
The preparation of embodiment 4 acetylated hydroxypropyl potato starchs
Prepare in accordance with the following steps acetylated hydroxypropyl potato starch:
1) size mixing: 28.5Kg anhydrous Na 2SO4 and 1.5Kg solid NaOH are dissolved in the 250kg water, then with the 220Kg starch dissolution in solution, stir, obtain starch milk;
2) sodium hydroxide lye of adding 3.8% stirs half an hour to pH=11.20 in starch milk etherificate: to step 1); The propylene oxide that adds again 19.8kg, sealing was stirred one hour, and starch milk is warming up to 41 ℃-43 ℃; React and cool off after 22 hours, be neutralized to pH=8.20;
3) esterification: add acetic anhydride 7.7Kg and carry out esterification, add simultaneously 4.0% sodium hydroxide lye and keep PH 8.30;
4) neutralization: after reaction finished, the hydrochloric acid with 10.5% was neutralized to pH=5.5;
5) washing: adopt the eddy flow washer to wash; Dry: as to dewater minute to≤45% with the Centrifugal peeling blade machine first, pass through again air stream drying moisture extremely≤15%; Pulverize: pulverize with pulverizer; Sieve: cross the 80-100 mesh sieve, obtain finished product;
6) packing (choosing wantonly): adopt 20-25KG/ bag form packing.
The molar substitution MS=0.268 of the acetylize hydroxypropylated starch that this embodiment prepares, DS=0.059, the viscosity of mensuration is referring to Fig. 4.
The application example vanilla pudding
Component
Vanilla pudding compound 19.5g
Fresh milk 118.0ml
Starch 4.5g
Making processes: with fresh milk and starch together heated and stirred; After using the cold water cooling, add the vanilla pudding compound and mix thoroughly, fully after the dissolving, use screen filtration, pour model into, place refrigerator cold-storage to typing.
Starch adopts respectively acetylize hydroxypropylated starch and the potato ative starch (in contrast) of embodiment 1 preparation.
The application experiment result:
| Starches | Stability | Mouthfeel | Refrigeration property (20 days) |
| The acetylize hydroxypropylated starch of |
Good | Satiny, soft tender | Anhydrous separating out, mouthfeel are as before |
| The potato ative starch | Bad | Granular sensation is arranged, hard | There are a large amount of elutriations to go out |
Claims (7)
1. the preparation method of an acetylated hydroxypropyl potato starch, it comprises yam starch, expansion inhibitor and catalyzer soluble in water, regulate the pH value to alkaline pH=10.90-11.30, add propylene oxide and carry out etherification reaction, obtain hydroxypropyl potato starch, then regulate the pH value to pH=8.20-8.40, add again acetic anhydride and carry out esterification, in after reaction finishes and pH to slightly acidic, washing, dry, pulverize and sieve, obtain acetylated hydroxypropyl potato starch, wherein said expansion inhibitor is selected from sodium sulfate, sodium-chlor; Described catalyzer is selected from sodium hydroxide, potassium hydroxide, calcium hydroxide, quaternary ammonium hydroxide, and wherein the part by weight of yam starch and propylene oxide is 100: 6-100: 9, and the part by weight of yam starch and acetic anhydride is 200: 5-200: 7; Regulating pH value to alkalescence adopts the alkali lye of 3.8-4.2w/w to carry out; The degree Beaume 24.0-27.5Be of emulsion; In and pH adopt the hydrochloric acid of 9-11% to carry out to slightly acidic.
2. the preparation method of the acetylated hydroxypropyl potato starch of claim 1, wherein the part by weight of yam starch, expansion inhibitor, catalyzer, water is 42: 5.7: 0.3: 52-44: 5.7: 0.3: 50.
3. the preparation method of claim 1 acetylated hydroxypropyl potato starch; wherein the part by weight of yam starch, expansion inhibitor, catalyzer, water is 43: 5.7: 0.3: 51; the part by weight of yam starch and propylene oxide is 100: 7, and the part by weight of yam starch and acetic anhydride is 200: 6.
4. the preparation method of claim 1 acetylated hydroxypropyl potato starch wherein in the etherification reaction, regulates the pH value to alkalescence, stirred 20-60 minute, churning time behind the adding propylene oxide is 1-3 hour, is heated to afterwards 42-43 ℃ and reacts, and the reaction times is 20-24 hour; The reaction times of esterification is 1-3 hour.
5. the preparation method of the acetylated hydroxypropyl potato starch of claim 1, it comprises the steps:
1) sizes mixing: will be based on the anhydrous Na of starch weight 13.26%
2SO
4In the water that is dissolved in based on starch weight 0.7% solid NaOH based on 1.18 times of starch weight, then with load weighted starch dissolution in mentioned solution, stir, obtain starch milk;
2) alkali lye that adds 3.8%-4.2w/w in starch milk etherificate: to step 1) is regulated pH=10.90-11.30, stirs half an hour; Add the propylene oxide based on starch weight 7.0%, sealing was stirred one hour again; Starch milk is warming up to 42 ℃-43 ℃, when being warming up to 40 ℃, the beginning clock reaction, whole reaction process is kept temperature of reaction 42-43 ℃; React and cool off after 20-24 hour, be neutralized between the pH=8.20-8.40;
3) esterification: add acetic anhydride and carry out esterification, the part by weight of yam starch and acetic anhydride is 200: 5-200: 7, and add simultaneously 3.8-4.2w/w alkali and keep pH between 8.20-8.40;
4) neutralization: after reaction finishes, be neutralized to pH=5.0-6.5 with the hydrochloric acid soln of 9-11%;
5) washing, dry, pulverize and sieve, obtain finished product.
6. acetylated hydroxypropyl potato starch, it is according to each preparation method preparation in the claim 1 to 5.
7. the acetylated hydroxypropyl potato starch of claim 6 is used for food-processing or is used for the purposes of daily-use chemical industry, is used for food-processing, and it is as thickening material, stablizer, emulsifying agent or pore forming material; Be used for daily-use chemical industry, it is as tackiness agent.
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| CN102408489B (en) * | 2011-07-28 | 2013-03-13 | 广西农垦明阳生化集团股份有限公司 | Preparation method of compound modified starch |
| CN102550896B (en) * | 2011-12-13 | 2014-06-18 | 江南大学 | Resistant starch-based emulsifier and application thereof |
| CN102603904A (en) * | 2012-03-14 | 2012-07-25 | 江苏宝宝宿迁国民生物科技有限公司 | Method for preparing hydroxypropyl acetylated adipate starch |
| CN104277125B (en) * | 2013-07-10 | 2016-12-28 | 江苏宝宝宿迁国民生物科技有限公司 | A kind of preparation method of high substituted degree acetylated rice starch |
| CN107467114A (en) * | 2017-07-25 | 2017-12-15 | 合肥台香食品有限公司 | A kind of bran bread quality modifying agent |
| CN107692001A (en) * | 2017-10-12 | 2018-02-16 | 汪彩平 | A kind of preparation method for telling the low and not easily broken rice stick of slurry rate |
| CN107974216A (en) * | 2017-12-07 | 2018-05-01 | 明光市永德包装有限公司 | A kind of water-fast adhesive of corrugated case |
| CN108191986A (en) * | 2017-12-26 | 2018-06-22 | 吉林中粮生化有限公司 | A kind of preparation method of hydroxypropul starch |
| CN108559004A (en) * | 2018-04-13 | 2018-09-21 | 周枫 | A kind of preparation method and application of multiple elements design converted starch |
| CN109400728A (en) * | 2018-11-18 | 2019-03-01 | 甘肃丰收农业科技有限公司 | A kind of converted starch and preparation method thereof applied in jam production |
| CN110343184A (en) * | 2019-08-08 | 2019-10-18 | 广西民族大学 | A kind of etherificate -ester starch based surfactants and preparation method thereof |
| CN113667026B (en) * | 2021-05-20 | 2022-11-18 | 华南理工大学 | High-viscosity instant carboxymethyl octenyl composite modified starch emulsion thickener and preparation method and application thereof |
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