CN1962696A - Process for producing starch octenylsucciniate - Google Patents
Process for producing starch octenylsucciniate Download PDFInfo
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- CN1962696A CN1962696A CNA2006101546189A CN200610154618A CN1962696A CN 1962696 A CN1962696 A CN 1962696A CN A2006101546189 A CNA2006101546189 A CN A2006101546189A CN 200610154618 A CN200610154618 A CN 200610154618A CN 1962696 A CN1962696 A CN 1962696A
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- 229920002472 Starch Polymers 0.000 title claims abstract description 87
- 239000008107 starch Substances 0.000 title claims abstract description 87
- 235000019698 starch Nutrition 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title description 11
- 230000008569 process Effects 0.000 title description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 45
- 239000000839 emulsion Substances 0.000 claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 6
- KCYQMQGPYWZZNJ-BQYQJAHWSA-N hydron;2-[(e)-oct-1-enyl]butanedioate Chemical compound CCCCCC\C=C\C(C(O)=O)CC(O)=O KCYQMQGPYWZZNJ-BQYQJAHWSA-N 0.000 claims description 39
- 238000006243 chemical reaction Methods 0.000 claims description 38
- -1 octenyl succinate anhydride Chemical class 0.000 claims description 32
- 238000010790 dilution Methods 0.000 claims description 15
- 239000012895 dilution Substances 0.000 claims description 15
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 13
- 230000035484 reaction time Effects 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 230000000694 effects Effects 0.000 claims description 8
- 229960004756 ethanol Drugs 0.000 claims description 5
- 238000010298 pulverizing process Methods 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 238000012546 transfer Methods 0.000 claims description 5
- 150000002148 esters Chemical class 0.000 abstract description 7
- 229920001592 potato starch Polymers 0.000 abstract description 4
- 238000002156 mixing Methods 0.000 abstract 2
- 229940014800 succinic anhydride Drugs 0.000 abstract 2
- KCLANYCVBBTKTO-UHFFFAOYSA-N Proparacaine Chemical compound CCCOC1=CC=C(C(=O)OCCN(CC)CC)C=C1N KCLANYCVBBTKTO-UHFFFAOYSA-N 0.000 abstract 1
- 229940087458 alcaine Drugs 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 17
- 238000006467 substitution reaction Methods 0.000 description 14
- 230000032050 esterification Effects 0.000 description 12
- 238000005886 esterification reaction Methods 0.000 description 12
- 239000008186 active pharmaceutical agent Substances 0.000 description 10
- 235000013305 food Nutrition 0.000 description 10
- 244000061456 Solanum tuberosum Species 0.000 description 8
- 235000002595 Solanum tuberosum Nutrition 0.000 description 8
- 235000013826 starch sodium octenyl succinate Nutrition 0.000 description 8
- 239000001334 starch sodium octenyl succinate Substances 0.000 description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000000654 additive Substances 0.000 description 6
- 230000000996 additive effect Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 229920000881 Modified starch Polymers 0.000 description 5
- 239000004368 Modified starch Substances 0.000 description 5
- 235000019426 modified starch Nutrition 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000006386 neutralization reaction Methods 0.000 description 4
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 4
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 4
- 206010013786 Dry skin Diseases 0.000 description 3
- 150000008065 acid anhydrides Chemical class 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 235000013373 food additive Nutrition 0.000 description 3
- 239000002778 food additive Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- GUOCOOQWZHQBJI-UHFFFAOYSA-N 4-oct-7-enoxy-4-oxobutanoic acid Chemical compound OC(=O)CCC(=O)OCCCCCCC=C GUOCOOQWZHQBJI-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229910001961 silver nitrate Inorganic materials 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 229920000856 Amylose Polymers 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 244000017020 Ipomoea batatas Species 0.000 description 1
- 235000002678 Ipomoea batatas Nutrition 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- FLISWPFVWWWNNP-BQYQJAHWSA-N dihydro-3-(1-octenyl)-2,5-furandione Chemical compound CCCCCC\C=C\C1CC(=O)OC1=O FLISWPFVWWWNNP-BQYQJAHWSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- HZVOZRGWRWCICA-UHFFFAOYSA-N methanediyl Chemical compound [CH2] HZVOZRGWRWCICA-UHFFFAOYSA-N 0.000 description 1
- 239000003094 microcapsule Substances 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 125000004365 octenyl group Chemical group C(=CCCCCCC)* 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000001384 succinic acid Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a manufacturing method of octal-olefin succinic starch ester, which comprises the following steps: 1) blending potato starch and water in the thermostatic magnetic stirrer into emulsion; 2) adopting 3% sodium hydroxide to adjust the pH value of emulsion to 7.5-8.0; 3) adopting anhydrous alcohol to dilute octal-olefin succinic anhydride; 4) blending the diluted octal-olefin succinic anhydride and emulsion phase in the step 2) to form reacting system; adding 3% NaOH solution to maintain the pH value of reacting system; reacting 2-4h; 5) using 2mol/L alcaine to adjust the pH value to 6.4-6.6; washing through water and 70% alcohol separately; drying; grinding.
Description
Technical field
The present invention relates to belong to the food chemistry field, be specifically related to manufacturing method of octal-olefin succinic.
Background technology
Starch octenyl succinate anhydride (Starch Octenyl Succinate), claim again starch Sodium Octenyl Succinate (StarchSodium Octenyl Succinates, SSOS), octenyl succinate starch, octenyl Succinic Acid esterification starch, pure glue.It is the esterified prod that is generated under alkalescence or weak basic condition by starch or derivatives thereof and octenyl succinic acid anhydride (Octenyl Succinic Anhydride is called for short OSA), during production often the form with sodium salt prepare.
The raw material that the preparation starch octenyl succinate anhydride uses can be different types of ative starch, denaturated starch by acid, dextrin and other derivative.In numerous starch alkenyl succinate ester products, have only now with the modified starch of octenyl succinic acid anhydride process for producing and listed in the foodstuff additive category in approval in 1972 by U.S. food and FAD (FDA).
Starch octenyl succinate anhydride is a kind of safe emulsifing thickener, is used by the approval of the major country of the U.S., Europe and the Asian-Pacific area.When its quality index was production food grade starch octenyl succinate anhydride, it was 3% that the maximum of octenyl succinic acid anhydride allows treatment capacity, and substitution value is about 0.02, and the residual quantity of octenyl succinic is less than 0.3%.The Food and Argriculture OrganizationFAO and the World Health Organization (FAO/WHO) estimate: the amount of being permitted day need not special stipulation and can be used for food, and use range without limits.The Chinese government ratified this modified starch as foodstuff additive in 1997, and calendar year 2001 has ratified to enlarge the use range of this product in food again, and consumption can add according to demand, need not control.
Nineteen fifty-three Caldwell and Wurzburg find that its preparation principle is based on esterification and can carries out under the alkaline condition of gentleness.This product was put into U.S. food additive category in 1997.People such as Shogren have studied octenyl succinic acid anhydride in the inside and outside distribution situation of the starch granules of octenyl succinic acid starch (waxy corn) ester in 2000, provide foundation for further explaining the relation between starch octenyl succinate anhydride structure and the physical property.Wherein starch octenyl succinate anhydride has dropped into suitability for industrialized production abroad, the produce market promise well, and as the chemical company limited of the national starch of the U.S., the Song Gu Chemical Co., Ltd of Japan etc. all has multiple starch octenyl succinate anhydride product to come out.With national starch company limited is example, and the food that this enterprise produces has 60 to 70 kind more than with modified starch, and wherein starch octenyl succinate anhydride has twenties kinds.
At home, the research work of this respect just began in recent years.Acquired achievement mostly is about laurylene base succinic acid starch ester, research to the starch octenyl succinate anhydride that uses as foodstuff additive also rests on the starting stage, the main dependence on import of product, this mainly contains the reason of three aspects: at first, this modified starch is with high content of technology, the operational path complexity relates to twice sex change of ative starch and the mobility control of finished product, and general enterprise can't be competent at; Next is domestic shortage octenyl succinic acid anhydride raw material, does not still have the chemical plant can produce this acid anhydrides at present, thereby has restricted the production of starch octenyl succinate anhydride; Another reason is that Application Areas lags behind, and people also lack enough understanding to this starch product, and the exploitation in market needs the regular hour.The secretary general Liu Lianfang of Food Additives Used in China TIA showed literary composition in " foodstuffs industry science and technology " third phase in 1999 and points out: starch octenyl succinate anhydride is widespread use abroad, China does not still have production, owing to have the high-performance (as viscosity and emulsifying property) that other products can't replace, so be worth exploitation, this can play positive pushing effect surely to the development of starch industry and foodstuff additive." Food Additives Used in China " first phase calendar year 2001 and the third phase have the people that starch octenyl succinate anhydride is classified as the short kind that state's inner additive is badly in need of exploitation again.At present, the domestic Supreme Being of having only reaches enterprises of several family such as modified starch company limited and auspicious continuous heavy rain chemical industry company limited and can produce starch octenyl succinate anhydride.But the internal and international great majority of going up adopt W-Gum to produce as raw material, and the viscosity of product is not high, can't satisfy the demand of practical application.
Although also there are above many unfavorable factors in the present popularization at home of SSOS, its advantage also clearly.The first, product technology content improves, and has increased substantially the added value of cheap ative starch, and its competitive power is improved greatly; The second, because product is not also really realized industrialization at present at home, technology is abroad monopolized fully, and profit is very big, so this product has wide development space in China.
Potato is as a kind of abundant starch raw material, and it is originated widely and can reduce production costs greatly; Simultaneously potato starch particle is big, and the amylose starch polymerization degree is big, and characteristic such as have that gelatinization point is low, viscosity is high, good springiness, protein content are low is that other starch are irreplaceable.Therefore the contriver to consider to adopt yam starch be that raw material prepares and produces the high starch octenyl succinate anhydride of substitution value.
Summary of the invention
The technical problem to be solved in the present invention provides the high starch octenyl succinate anhydride production method of a kind of substitution value, and starch octenyl succinate anhydride viscosity height, the security of adopting the inventive method to produce are good.
In order to solve the problems of the technologies described above, the invention provides a kind of manufacturing method of octal-olefin succinic, may further comprise the steps:
1), yam starch and water are blended into emulsion under the effect of constant temperature blender with magnetic force, yam starch accounts for 30%～40% of emulsion gross weight; Temperature of reaction is 30～40 ℃, stirring velocity 90～110r/min;
2), adopting weight concentration is that 3% sodium hydroxide is regulated pH value to 7.5～8.0 of above-mentioned emulsion;
3), adopt dehydrated alcohol dilution octenyl succinic acid anhydride, the volume ratio of dehydrated alcohol and octenyl succinic acid anhydride is 3～7 times;
4), with octenyl succinic acid anhydride and step 2 after the dilution of step 3) gained) the mixed mutually reaction system that forms of the emulsion of gained, the weight ratio of yam starch is 3% in octenyl succinic acid anhydride after the described dilution and the emulsion; Add weight concentration and be pH value to 7.5～8.0 that 3% NaOH solution is kept reaction system, the reaction times is 2～4 hours;
5), transfer to pH value to 6.4～6.6 of step 4) products therefrom earlier with hydrochloric acid (HCl) solution of 2mol/L; Again respectively water, weight concentration be each washing of 70% ethanol once; Then carry out drying and pulverizing successively, promptly obtain the starch octenyl succinate anhydride of white.
The present invention is taking all factors into consideration under the situation of various factors, selects the water legal system to be equipped with starch octenyl succinate anhydride.Its reaction mechanism is as follows:
Wherein R is the front three subunit, and R ' is 8 carbene bases.
Specific as follows: under the effect of alkali, the ring of acid anhydrides is opened, one end combines with the hydroxyl of starch molecule with the form of ester bond, the other end then produces a carboxyl, the pH value of whole reaction system descends along with the carrying out of reaction, so another effect of alkali is the carboxylic acid that neutralization dissociates and in esterification, to keep the weakly alkaline of reaction system, reaction is carried out to the esterification direction.
Starch octenyl succinate anhydride is divided into two big series products: a class is that the starch octenyl succinate anhydride of feedstock production mainly glues the thickening stabilizer of system as height with the ative starch, another kind of is that the starch octenyl succinate anhydride of raw material production can obtain lower viscosity with the starch decomposition products, in microcapsule industry important use is arranged.It is the processing condition and the method for feedstock production starch octenyl succinate anhydride that this patent adopts wet processing to inquire into the potato ative starch, the added value that greatly promotes China's potato processing and utilize is developed the modified potato starch product that can satisfy multiple demand.
In order to check the present invention, can realize by following method:
Set up the measuring method of sample substitution value and reaction efficiency, this measuring method is not only simple, economical.Accurately take by weighing the 2.0g sample and place the 250mL beaker, wetting with the Virahol of 10mL90%, stir 10min, add hydrochloric acid-aqueous isopropanol of 15mL 2.5mol/L, magnetic agitation 30min adds the aqueous isopropanol of 50mL 90% then, continues to stir 10min.Sample is moved into B, and the washed with isopropyl alcohol with 90% is to there not being Cl
-(with the check of 0.1 mol/L Silver Nitrate).Sample is moved in the beaker of 500mL, adding distil water is to 300mL again, and boiling water bath 20min adds 2 phenolphthalein, uses the 0.1mol/LNaOH titration to pink while hot.
Substitution value (DS) calculation formula is as follows:
In the formula: A: by every gram starch Sodium Octenyl Succinate (SSOS) the amount of substance of consumption 0.1mol/LNaOH standardized solution, mmol;
V: the titration starch paste consumes the volume of NaOH standardized solution, mL;
The concentration of C:NaOH standardized solution, mol/L;
W: the quality of starch octenyl succinate anhydride sample (butt), g;
0.1624: the molar mass of glucose is 162.4, g/moL;
0.21: the molar mass of octenyl succinic acid anhydride is 210, g/moL;
W
1: the quality of octenyl succinic acid anhydride, g;
W
2: starch quality (butt), g.
The present invention is in production process, at first relatively and screened of the influence of differential responses condition, also investigated the influence of extension rate, reaction times, temperature of reaction, reaction PH and the reaction conditionss such as starch milk starting point concentration, OSA add-on of acid anhydrides to esterification to esterification.Found that the security of considering food, this experimental selection dehydrated alcohol is as thinner, and the substitution value of starch octenyl succinate anhydride is the highest when diluting 5 times, so dilute 5 times before OSA uses in this patent.At preceding 3 hours of reaction, substitution value DS and reaction efficiency RE prolonged in time and increase sharply, and prolong the reaction times again, and substitution value begins to descend, so the reaction times was advisable with 3 hours.From result of study as can be known, DS and RE reach the highest along with the rising of temperature slowly increases at 35 ℃, continue to heat up then to begin to descend again, and therefore select 35 ℃ of temperature as esterification.In esterification, pH also is an important factors, and it plays dual function in esterification.PH was at 8.0 o'clock, and DS and RE reach the highest, the pH that raises again, and DS and RE begin rapid decline.Starch is as reaction substrate, and its concentration directly has influence on the efficient of reaction itself.DS and DE raise along with the increase of starch concentration, reach the highest time 35%, increase concentration again and then begin slow reduction.OSA is as the reaction substrate that plays a decisive role, and its add-on has very big influence to final DS.But in foodstuffs industry, be conditional to the maximum addition of the octenyl succinic acid anhydride of food grade, its add-on was no more than for 3% (DS is about 0.02), so OSA can not unconfinedly add.The present invention has also carried out orthogonal optimization to the main factor that influences esterification at last, to obtain maximized esterification condition.
On the experiment of single factor basis, to temperature of reaction, reaction pH, in the reaction times, four factor designs of starch concentration orthogonal experiment is established four factors, three water-glasses, is optimized test.Can draw by range analysis, four factors to the primary and secondary that influences of reacting DS are in proper order: starch concentration＞reaction times＞temperature of reaction＞reaction pH.The esterification best of breed is reaction times 3h, 35 ℃ of temperature of reaction, starch concentration 35%, reaction pH8.0.
The present invention compared with prior art, its major advantage is as follows:
1, potato wide material sources, cheap can reduce production costs, and product is easy to preparation;
2, adopt the starch octenyl succinate anhydride substitution value of this method and explained hereafter higher, be up to 0.0177, also have some advantageous characteristics of former yam starch;
3, adopted the thinner of dehydrated alcohol in the starch octenyl succinate anhydride that adopts method of the present invention to produce as octenyl succinic acid anhydride, changed that to adopt Virahol (potential safety problem is arranged) in the traditional method be thinner, be a kind of safe foodstuff additive, reduced food safety risk.
Embodiment
Embodiment 1, a kind of potato octenyl succinic acid starch ester substitution value measuring method:
Accurately take by weighing the 2.0g sample and place the 250mL beaker, wetting with the Virahol of 10mL 90%, stir 10min, hydrochloric acid-the aqueous isopropanol that adds 15mL 2.5mol/L, magnetic agitation 30min adds the aqueous isopropanol of 50mL 90% then, continues to stir 10min.Sample is moved into B, and the washed with isopropyl alcohol with 90% is to there not being Cl-(with the check of 0.1mol/L Silver Nitrate).Sample is moved in the beaker of 500mL, adding distil water is to 300mL again, and boiling water bath 20min adds 2 phenolphthalein, uses the 0.1mol/LNaOH titration to pink while hot.
Substitution value (DS) calculation formula is as follows:
A: by every gram starch Sodium Octenyl Succinate (SSOS) the amount of substance of consumption 0.1mol/L NaOH standardized solution, mmol;
The production method of embodiment 2, a kind of potato octenyl succinic acid starch ester, carry out following steps successively:
1, yam starch and water are blended into emulsion under the effect of constant temperature blender with magnetic force, and yam starch accounts for 30% of emulsion gross weight; Temperature of reaction is 30 ℃, stirring velocity 100r/min;
2, adopting weight concentration is the pH value to 7.5 that 3% sodium hydroxide is regulated above-mentioned emulsion;
3, adopt dehydrated alcohol dilution octenyl succinic acid anhydride, the volume ratio of dehydrated alcohol and octenyl succinic acid anhydride is 5 times;
4, with octenyl succinic acid anhydride and step 2 after the dilution of step 3) gained) the mixed mutually reaction system that forms of the emulsion of gained, the weight ratio of yam starch is 3% in octenyl succinic acid anhydride after the described dilution and the emulsion; Add weight concentration and be 3% NaOH solution and keep the pH value to 7.5 of reaction system, the reaction times is 2 hours;
5, transfer to the pH value to 6.5 of step 4) products therefrom earlier with the hydrochloric acid soln of 2mol/L; Again respectively water, weight concentration be each washing of 70% ethanol once, NaCl and responseless octenyl succinic acid anhydride that the flush away neutralization reaction produces; Then gains are placed 45 ℃ of baking oven inner dryings, the product of pulverizing after drying is crossed 120 mesh sieves, promptly obtains the starch octenyl succinate anhydride of white.
The starch octenyl succinate anhydride of gained, its substitution value is 0.0127 after testing.Detection method such as embodiment 1.
The production method of embodiment 3, a kind of potato octenyl succinic acid starch ester, carry out following steps successively:
1, yam starch and water are blended into emulsion under the effect of constant temperature blender with magnetic force, and yam starch accounts for 35% of emulsion gross weight; Temperature of reaction is 35 ℃, stirring velocity 100r/min;
2, adopting weight concentration is the pH value to 8.0 that 3% sodium hydroxide is regulated above-mentioned emulsion;
3, adopt dehydrated alcohol dilution octenyl succinic acid anhydride, the volume ratio of dehydrated alcohol and octenyl succinic acid anhydride is 5 times;
4, with octenyl succinic acid anhydride and step 2 after the dilution of step 3) gained) the mixed mutually reaction system that forms of the emulsion of gained, the weight ratio of yam starch is 3% in octenyl succinic acid anhydride after the described dilution and the emulsion; Add weight concentration and be 3% NaOH solution and keep the pH value to 8.0 of reaction system, the reaction times is 3 hours;
5, transfer to the pH value to 6.5 of step 4) products therefrom earlier with the hydrochloric acid soln of 2mol/L; Again respectively water, weight concentration be each washing of 70% ethanol once, NaCl and responseless octenyl succinic acid anhydride that the flush away neutralization reaction produces; Then gains are placed 45 ℃ of baking oven inner dryings, the product of pulverizing after drying is crossed 120 mesh sieves, promptly obtains the starch octenyl succinate anhydride of white.
The starch octenyl succinate anhydride of gained, under optimum reaction condition, substitution value can reach 0.017.Detection method such as embodiment 1.
The production method of embodiment 4, a kind of potato octenyl succinic acid starch ester, carry out following steps successively:
1, bell sweet potato starch and water are blended into emulsion under the effect of constant temperature blender with magnetic force, and yam starch accounts for 40% of emulsion gross weight; Temperature of reaction is 35 ℃, stirring velocity 100r/min;
2, adopting weight concentration is the pH value to 7.5 that 3% sodium hydroxide is regulated above-mentioned emulsion;
3, adopt dehydrated alcohol dilution octenyl succinic acid anhydride, the volume ratio of dehydrated alcohol and octenyl succinic acid anhydride is 5 times;
4, with octenyl succinic acid anhydride and step 2 after the dilution of step 3) gained) the mixed mutually reaction system that forms of the emulsion of gained, the weight ratio of yam starch is 3% in octenyl succinic acid anhydride after the described dilution and the emulsion; Add weight concentration and be 3% NaOH solution and keep the pH value to 7.5 of reaction system, the reaction times is 4 hours;
5, transfer to the pH value to 6.5 of step 4) products therefrom earlier with the hydrochloric acid soln of 2mol/L; Again respectively water, weight concentration be each washing of 70% ethanol once, NaCl and responseless octenyl succinic acid anhydride that the flush away neutralization reaction produces; Then gains are placed 45 ℃ of baking oven inner dryings, the product of pulverizing after drying is crossed 120 mesh sieves, promptly obtains the starch octenyl succinate anhydride of white.
The starch octenyl succinate anhydride of gained, its substitution value is 0.015 after testing.Detection method such as embodiment 1.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (2)
1, a kind of manufacturing method of octal-olefin succinic may further comprise the steps:
1), yam starch and water are blended into emulsion under the effect of constant temperature blender with magnetic force, yam starch accounts for 30%～40% of emulsion gross weight; Temperature of reaction is 30～40 ℃, stirring velocity 90～110r/min;
2), adopting weight concentration is that 3% sodium hydroxide is regulated pH value to 7.5～8.0 of above-mentioned emulsion;
3), adopt dehydrated alcohol dilution octenyl succinic acid anhydride, the volume ratio of dehydrated alcohol and octenyl succinic acid anhydride is 3～7 times;
4), with octenyl succinic acid anhydride and step 2 after the dilution of step 3) gained) the mixed mutually reaction system that forms of the emulsion of gained, the weight ratio of yam starch is 3% in octenyl succinic acid anhydride after the described dilution and the emulsion; Add weight concentration and be pH value to 7.5～8.0 that 3% NaOH solution is kept reaction system, the reaction times is 2～4 hours;
5), transfer to pH value to 6.4～6.6 of step 4) products therefrom earlier with the hydrochloric acid soln of 2mol/L; Again respectively water, weight concentration be each washing of 70% ethanol once; Then carry out drying and pulverizing successively, promptly obtain the starch octenyl succinate anhydride of white.
2, manufacturing method of octal-olefin succinic according to claim 1 is characterized in that: yam starch accounts for 35% of emulsion gross weight in the step 1); Temperature of reaction is 35 ℃, stirring velocity 100r/min; The volume ratio of dehydrated alcohol and octenyl succinic acid anhydride is 5 times in the step 3); The pH value of reaction system is 8 in the step 4), and the reaction times is 3 hours.
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