CN1749279A - Process for preparing modified composite denatured starch by microwave acidiolysis and esterification - Google Patents
Process for preparing modified composite denatured starch by microwave acidiolysis and esterification Download PDFInfo
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- CN1749279A CN1749279A CN 200510094853 CN200510094853A CN1749279A CN 1749279 A CN1749279 A CN 1749279A CN 200510094853 CN200510094853 CN 200510094853 CN 200510094853 A CN200510094853 A CN 200510094853A CN 1749279 A CN1749279 A CN 1749279A
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Abstract
The present invention belongs to the field of denatured starch technology. Under normal pressure or vacuum microwave condition, starch is acidolyzed and esterified simultaneously to prepare compositely denatured starch product. The compositely denatured starch product has the properties of both esterified starch and acidolyzed starch, and may be used as fat substituent in producing low fat butter, ice cream, salad paste, and as Arabic gum substituent as microcapsule material. The present invention combines acidolysis, esterification and microwave treatment, and has the advantages of short reaction time, high reaction efficiency, less environmental pollution and excellent product performance.
Description
Technical field
Under the microwave radiation condition, a kind of preparation method and application of carrying out acidolysis and esterification modification composite modified starch simultaneously belongs to technical field of modified starch.
Technical background
Fatty acid starch ester is the esterified prod that is obtained by starch and derivative thereof and lipid acid, fatty acid methyl ester, lipid acid acyl chlorides or fatty acid anhydride reaction.Because the introducing of the organic carbochain of hydrophobicity, the hydrophobicity of starch increases, and makes it to have possessed hydrophilic and lipophilic parents' character, has emulsifying property, can be used on fields such as food, medicine, household chemicals.The fatty acid starch ester of high substitution value can be used for the micro encapsulation product and obtains high embedding rate because of having higher emulsifying capacity, replaces expensive gum arabic; The fatty acid starch ester of low degree of substitution can be used for fat-replacer.Relevant organic solvent method prepares fatty acid starch ester, external existing many reports.Have only Saiyavit Varavinit etc. to synthesize the starch stearate of sago and cassava with dry method.About microwave method starch is carried out the technology that acidolysis and esterification prepare composite modified starch simultaneously and yet there are no report so far.
Summary of the invention
The objective of the invention is: provide a kind of under the microwave radiation condition, the preparation method of lipid acid and starch direct esterification synthetic fatty acid starch ester.Owing to adopt in this reaction sourly can make the starch acidolysis as catalyzer in the reaction process, so acidolysis and esterification are carried out simultaneously among the preparation technology, product has numerous excellent specific properties.Hot anhydrous alcohol solution lipid acid and starch thorough mixing are adopted in this reaction, and ethanol can volatilize fully in the reaction process, so the invention belongs to dried preparation.
Technical scheme of the present invention: a kind of acidolysis and esterification composite modified starch are to adopt microwave (normal pressure or vacuum) method that the preparation method that starch carries out acidolysis and esterification sex change is simultaneously made, and make product have the characteristic of acidolysis and esterification modified starch simultaneously.
The described preparation method who carries out acidolysis and esterification modification composite modified starch simultaneously, be to be raw material with starch, esterifying agent is dissolved in the hot anhydrous ethanol solvent, add a certain amount of acid, and add suitable quantity of water conditioned reaction system moisture content, and slowly join in the starch, constantly stir, the slurry that obtains carries out acidolysis and esterification simultaneously under microwave radiation (normal pressure or vacuum), make acidolysis and esterification composite modified starch.
Starch material can be W-Gum, wheat starch, potato starch etc.
The used esterifying agent of esterification sex change can be a higher fatty acid, and as stearic acid, lauric acid, tetradecanoic acid, palmitinic acid, oleic acid, linolic acid, eicosanoic acid etc., the used solvent of dissolving esterifying agent can be a dehydrated alcohol.
The used acidolysis reagent of acidolysis sex change is easy volatile acid such as hydrochloric acid, acid or glacial acetic acid.
Microwave reaction can be to carry out under the conditions such as normal pressure, vacuum.
Preparation technology's prescription:
Starch, butt quality meter 100
Esterifying agent, in mass 2～4
Dehydrated alcohol, by volume 80～120
Acid, in mass 0.05～0.20
Water, by volume 0～40
At breadboard concrete prescription be:
Starch (butt meter) 100g
Esterifying agent 2～4g
Dehydrated alcohol 80～120ml
Acid 0.05～0.20g
Water 0～40ml
Reaction process condition: after esterifying agent is dissolved in hot dehydrated alcohol earlier, add catalyst acid, adding or do not add water conditioned reaction system to moisture massfraction is 14%～42%, slowly joins the esterifying agent solvent in the starch then, and constantly stir the thing that is uniformly mixed reaction slurry.The power of microwave reaction is 700～1200W, and the reaction times is 3～10min, and normal pressure adopts the heating of 30s intermittent type, and stirs fast, or vacuum adopts heating continuously, vacuum tightness 0.08～0.1Mpa.The slow adding of esterifying agent solvent is to carry out under constantly stirring.The moisture massfraction of reaction paste is controlled at 14%～30% for better during microwave reaction.
The described application of under microwave condition, carrying out acidolysis and esterification modification composite modified starch simultaneously, be mainly used in the emulsifying agent in the foodstuffs industry, be used for numerous products such as present Emulsion flavour, micro encapsulation product, also can be used as the fat substitute in the milk fat spread.
Beneficial effect of the present invention: the present invention is directed to the microwave new technology in modified starch application and food-processing to the singularity requirement of modified starch, developed a kind of novel process and product innovation of modified starch targetedly.Utilize the dry microwave reactor that starch is carried out acidolysis and esterification sex change simultaneously, particularly prepared a kind of fatty acid starch ester with food fibre function, the acidolysis of starch and esterification are carried out simultaneously in preparation technology of the present invention.Product has numerous excellent specific properties, because the introducing of fatty acid group makes it to have hydrophilic and oleophylic parents group, thereby certain emulsifying property is arranged, adds the high temperature acidolysis effect in the starch, has reduced the viscosity of starch.Because change of molecular structure has formed heavy dextrin (food fibre function), has certain health-care effect.The product of gained can be applied to Emulsion flavour, be used for numerous products such as micro encapsulation product as microcapsule wall material, the higher gum arabic of alternative present price, Protanal Ester SD-LB etc., also can be used for replacing the part grease in the plant butter, production low fat plant butter, ice-creams, salad dressing etc.The adding of fatty acid starch ester has reduced the emulsifying agent in the prescription, the consumption of stablizer, thereby has reduced cost, and good economic benefit is arranged.This technology combines acidolysis and two kinds of denaturation methods of esterification, and utilizes the dry microwave reactor to react, and the reaction times is starkly lower than common dry process reaction, and reaction efficiency obviously improves, and is easy to implement, and environmental pollution is little.
Description of drawings
Under Fig. 1 microwave condition, carry out acidolysis and esterification modification composite modified starch preparation technology synoptic diagram simultaneously.
Embodiment
Embodiment 1
Take by weighing the 2g stearic acid, be dissolved in 70 ℃ of dehydrated alcohols of 80ml, add hydrochloric acid 0.05g again, do not add water, 70 ℃ of holding temperatures slowly add in the 100g starch (butt) then, and constantly stir, the thing that is uniformly mixed places the microwave oven of 700W to react in this mixture container of packing into, adopt the heating of 30s intermittent type, and stir fast, microwave irradiation time is 3min, cooling, pulverize, hard ester acid-starch ester gets product.Microwave oven is the NJL07-3 type experiment microwave oven that the full microwave equipment company limited of Nanjing outstanding person produces, down together.
Prepare the stearyl ester starch ester with stearic acid and starch reaction, adopt common normal pressure dry method, three kinds of different methods of microwave normal pressure dry method and microwave vacuum dry method are as shown in table 1 with the product performance of preparation starch stearate.Reaction efficiency is actual substitution value and the ratio of theoretical substitution value, and the reaction times of microwave method preparing product is starkly lower than common dry process reaction as can be seen from the table, and reaction efficiency obviously improves, and emulsifying property makes moderate progress.
Table 1: dry microwave (normal pressure or vacuum) compares with common dry process reaction
| Method | Reaction times/min | Substitution value | Reaction efficiency/% | Retrogradation | Emulsifying property/% | Solubleness/% (30 ℃) | Viscosity/mpa.s (20%, 30 ℃) |
| 1 | 240 | 0.0034 | 20 | Retrogradation is bigger than ative starch | 10 | 9 | 190 |
| 2 | 5 | 0.0060 | 35 | A little precipitation of bottom, the top clear | 25 | 35 | 160 |
| 3 | 10 | 0.0101 | 59 | Clear | 35 | 94 | 90 |
Annotate: method 1 is dried preparation under the normal pressure.Reaction conditions is: initial moisture massfraction 22%, 150 ℃ of temperature, stearic acid massfraction 3% (in the starch butt), reaction times 4h, HCl 0.08% (in the starch butt)
Method 2 is dry microwave preparation under the normal pressure.Reaction conditions is: moisture content is 28% before the reaction, stearic acid massfraction 3% (in the starch butt), microwave reaction power 800W, reaction times 5min, HCl0.12% (in the starch butt)
Method 3 is dry microwave preparation under the vacuum.Reaction conditions is: moisture content is 28% before the reaction, stearic acid massfraction 3% (in the starch butt), microwave reaction power 700W, reaction times 10min, HCl 0.12% (in the starch butt)
Embodiment 2
Take by weighing the 4g lauric acid, be dissolved in 70 ℃ of dehydrated alcohols of 120ml, add acetic acid 0.2g again, add 70 ℃ of 40ml water holding temperatures simultaneously, slowly join then in the 100g starch (butt), and constantly stir, the thing that is uniformly mixed places the microwave oven of 1200W to vacuumize reaction in this mixture container of packing into, microwave irradiation time is 10min, the lauric acid that gets product starch ester is pulverized in cooling.
Embodiment 3
Linolic acid is as esterifying agent, and all the other prescriptions and operational condition make finished product linolic acid starch ester with embodiment 1 or embodiment 2.
Embodiment 4
Tetradecanoic acid is as esterifying agent, and all the other prescriptions and operational condition make finished product tetradecanoic acid starch ester with embodiment 1 or embodiment 2.
Embodiment 5
Palmitinic acid is as esterifying agent, and all the other prescriptions and operational condition make finished product palmitinic acid starch ester with embodiment 1 or embodiment 2.
Embodiment 6
Oleic acid is as esterifying agent, and all the other prescriptions and operational condition make processed oil acid-starch ester with embodiment 1 or embodiment 2.
Embodiment 7
Eicosanoic acid is as esterifying agent, and all the other prescriptions and operational condition make finished product eicosanoic acid starch ester with embodiment 1 or embodiment 2.
Embodiment 8
Suitability for industrialized production, starch charging capacity 18～400kg/h, microwave oven is the NJ series tunnel type micro wave stove of the outstanding full microwave equipment company limited in Nanjing, or NJZ series vacuum microwave, all the other recipe ratio row and operational condition are with embodiment 1 or embodiment 2, make the finished product fatty acid starch ester, raw starch is W-Gum, wheat starch or potato starch.
Claims (6)
1, the preparation method of a kind of acidolysis and esterification modification composite modified starch, it is characterized in that with starch being raw material, esterifying agent is dissolved in the hot anhydrous ethanol solvent, and add a certain amount of acid and water, the esterifying agent that will be dissolved in hot ethanol slowly joins in the starch, constantly stir, the slurry that obtains carries out acidolysis and esterification simultaneously and is prepared under microwave condition
(1) prescription is:
Starch, butt quality meter 100
Esterifying agent, in mass 2～4
Dehydrated alcohol, by volume 80～120
Acid, in mass 0.05～0.20
Water, by volume 0～40
(2) preparation reaction slurry:
After esterifying agent is dissolved in hot dehydrated alcohol earlier, add catalyst acid, adding or do not add water conditioned reaction system to moisture massfraction is 14%-42%, then the esterifying agent solvent is slowly joined in the starch, and constantly stirs, the thing that is uniformly mixed reaction slurry;
(3) microwave reaction:
To react slurry and pack in the container, and place microwave oven to react, adopt the heating of atmosphere intermission formula, and stir fast; Or adopt vacuum to heat continuously.
2, preparation method according to claim 1 is characterized in that prescription is:
Starch, butt meter 100g
Esterifying agent 2～4g
Dehydrated alcohol 80～120ml
Acid 0.05～0.20g
Water 0～40ml
Microwave reaction power is 700～1200W, and the reaction times is 3～10min; Adopt normal pressure intermittent type heating in 30 seconds, and stir fast, or adopt vacuum to heat vacuum tightness 0.08-0.1Mpa continuously.
3, preparation method according to claim 1 is characterized in that starch is is raw material with W-Gum, wheat starch or potato starch.
4, preparation method according to claim 1 is characterized in that the employed catalyst acid of acidolysis sex change is hydrochloric acid, acid or glacial acetic acid.
5, preparation method according to claim 1 is characterized in that the esterification sex change, and employed esterifying agent is: stearic acid, lauric acid, tetradecanoic acid, palmitinic acid, oleic acid, linolic acid or eicosanoic acid; The solvent that uses is dehydrated alcohol.
6, preparation method according to claim 1, the moisture content massfraction of reaction slurry is controlled at 14%～30% when it is characterized in that microwave reaction.
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|---|---|---|---|
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