CN102276741A - Method for utilizing octenyl succinic anhydride to produce starch ester in circulation - Google Patents
Method for utilizing octenyl succinic anhydride to produce starch ester in circulation Download PDFInfo
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Abstract
The invention discloses a method for utilizing octenyl succinic anhydride to produce starch ester in circulation. The method comprises steps that: water is added to 100 parts of dry basis starch; the starch is homogenized and emulsified; the pH value of the starch is regulated to 8 to 10; the starch is added to an octenyl succinic anhydride solution containing 3 parts of octenyl succinic anhydride, and is subject to a reaction; when the reaction is finished, the pH value of a reaction liquid is regulated to 5.5 to 6.5; the reaction liquid is filtered, and is processed from processes of washing, drying, crushing and sieving three times, such that white starch sodium octenyl succinate is obtained; a residual from the filtering process is mixed with the filtered washing solution, such that an octenyl succinic anhydride mixed solution is obtained; the solution is distilled, octenyl succinic anhydride is supplemented, and a solvent is added for dissolving, such that an octenyl succinic anhydride solution is obtained; water and ethanol obtained from distillation are fractionated, ethanol concentration is adjusted, and the materials can be repeatedly used. The method provided by the invention is advantaged in that: the technology is simple and is easy to control; recycling of octenyl succinic anhydride and recycling of the solvent can both be realized.
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 is generally with starch Sodium Octenyl Succinate (Starch Sodium Octenyl Succinates, SSOS) form exists, be a kind of safe emulsifing thickener, its preparation principle is based on esterification can carry out under the alkaline condition of gentleness.This product was listed in U.S. food additive category in 1972 by U.S. food and FAD (FDA), also was present unique starch alkenyl succinate ester product that is allowed to be used for foodstuff additive by FDA.
Starch octenyl succinate anhydride has now been comprised the world major country approval use of China, when its quality index is production food grade starch octenyl succinate anhydride, it is 3% that the maximum of octenyl succinic acid anhydride allows treatment capacity, substitution value is not more than 0.02, and the residual quantity of octenyl succinic is less than 0.3%.
Substitution value generally uses titration measuring, and measuring method is as follows:
Claim the 5.0g sample to place the 100mL beaker, wetting with dehydrated alcohol, add and add 100mL95% ethanol behind the 25mL2.5mol/L ethanol solution hydrochloride magnetic agitation 30min and continue to stir 10min.Pour sample into the sand core funnel suction filtration, with 90% washing with alcohol to there not being Cl-ion (checking) with Silver Nitrate.With the sample oven dry, take by weighing pure samples 0.5g, add 150mL distilled water in the 250mL Erlenmeyer flask, boiling water bath is heated to the solution clarification, adds 2 phenolphthalein (1%), uses 0.05mol/L NaOH titration while hot to terminal, and calculates substitution value according to following formula.
Substitution value
162.4: glucosyl residue molar mass, g/mol;
210: octenyl succinic acid anhydride molar mass, g/mol;
C:NaOH standardized solution volumetric molar concentration, mol/L;
V: the sample titration consumes NaOH standardized solution volume, mL;
W: sample quality, g.
At present the production technology of starch octenyl succinate anhydride is only grasped by several companies such as national of the United States's starch chemistry company limited, Japanese Song Gu Chemical Co., Ltd, the domestic progress that obtains in this respect is very limited, even there is enterprise of several family can produce this product, but its product performance are far apart with external like product.Major cause is: 1) starch octenyl succinate anhydride complex manufacturing, and the control of sex change condition requires high; 2) a large amount of dependence on import of octenyl succinic acid anhydride raw material, thereby raise cost.
Except technical reason, the control of " three wastes " is increasingly serious in the industrial production at present, and when producing starch octenyl succinate anhydride, can produce a large amount of waste water because of washing, the reaction efficiency of octenyl succinic acid anhydride is very low simultaneously, a large amount of unreacted octenyl succinic acid anhydrides as waste by flush away, if the undesirable application performance that also can influence starch octenyl succinate anhydride of washing effect.Although existing at present, do not relate to substantially and simplify technology and improve raw material availability much about starch octenyl succinate anhydride preparation method's report.About starch octenyl succinate anhydride preparation method's report, mainly contain following several:
Nineteen fifty-three Caldwell and Wurzburg have at first disclosed the preparation method of starch octenyl succinate anhydride in US2661349A, its basic procedure comprises: starch is made into certain density starch milk, slowly add the octenyl succinic acid anhydride through alcohol dilution then, controlling the pH value simultaneously is 8～9; Add sour adjust pH to slightly acidic after reaction finishes, again through repeatedly washing, dry, obtain product after pulverizing, sieving.This is classical wet method preparation process, continued to use by most people in decades always, but this method long reaction time and octenyl succinic acid anhydride reaction efficiency are low, and a large amount of unreacted octenyl succinic acid anhydrides are washed off, and washing process also can produce a large amount of waste water simultaneously.
CN1823617 discloses a kind of preparation method of emulsifying agent of stabilizing food product opaque system, and this patent proposes to prepare starch octenyl succinate anhydride with early rice starch, but preparation process and above-mentioned patent are similar.
CN1985622 has introduced a kind of method of controlling the starch sodium octenyl succinate of early rice viscosity, by with previously prepared starch sodium octenyl succinate of early rice enzymolysis, acidifying with add alkali neutralization, make the product of different viscositys, the preparation technology in not mentioned early stage.
CN1903883A discloses a kind of preparation method of pre-gelatinization octenyl succinic acid starch, by will early stage the octenyl succinic waxy starch that prepare 100～200 ℃ down pre-gelatinizations obtain the products of high viscosity, highly water-soluble, but its preparation technology not have to innovate substantially.
CN1962696A discloses a kind of preparation method of starch octenyl succinate anhydride, and this patent just proposes to replace waxy corn starch commonly used to prepare starch ester with yam starch, and whole preparation process does not have substantial breakthrough.
CN101407552A has introduced the technology that a kind of oxidation style is produced the low-viscosity starch octenyl succinate anhydride, and the wax Starch rice carries out esterification with octenyl succinic acid anhydride again behind process hypochlorite oxidation, pyrosulphite sodium reduction, make product at last.This technology is being done the pre-treatment improvement in early stage, but esterification remains by octenyl succinic acid anhydride is slowly joined in the starch milk and is achieved.
More than report all belongs to wet method preparation process, is widely adopted because of it is environmentally friendly.The report that in addition some other technologies are also arranged:
[oil and foodstuffs science and technology, 2004,12 such as Chen Junzhi, 16-18] and [Carbohydrate Polymers, 2006,64 such as Atanu, 484-487] all mention in the microwave oven reactor of backflow is arranged and prepare starch octenyl succinate anhydride, can shorten the reaction times to a certain extent.
KR100857290 has introduced the method that a kind of dry heating method prepares starch octenyl succinate anhydride, this method is at first with the octenyl succinic acid anhydride hydrolysis, mix with starch then and mixture is dried to water content less than 10%, then heating at high temperature causes the replacement of starch hydrolysis and octenyl succinic.This method has certain difference with the wet processing of classics, but has the difficult control of esterification process, the inhomogeneous and residual high drawback of free sodium octenyl succinate of replacement.
The report that also prepares starch octenyl succinate anhydride in addition relevant for organic solvent method, starch and octenyl succinic acid anhydride are finished reaction in organic solvents such as benzene, acetone, dimethyl alum, but this method is used to prepare the starch octenyl succinate anhydride product that is applied to field of food because of the existence significant discomfort of organic solvent.
Summary of the invention
The objective of the invention is problem, provide a kind of recycle octenyl succinic acid anhydride to prepare the method for starch ester at above-mentioned existence.May further comprise the steps, following umber all by weight:
1) 100 parts of butt starch mix under 30 ℃～60 ℃ with 100～150 parts of water, and homogenizing emulsifying 5～30 minutes obtains finely divided emulsion, add pH value to 8～10 that sodium hydroxide or yellow soda ash are regulated above-mentioned emulsion then;
2) 3 parts of octenyl succinic acid anhydrides being dissolved in 100～150 parts of mass concentrations is not less than 80% ethanol and obtains octenyl succinic acid anhydride solution;
3) step 1) gained emulsion is joined the step 2 of 1000～2000r/min under stirring with Sprayable) in the described octenyl succinic acid anhydride solution, control reaction temperature is 30 ℃～60 ℃, reacted 0.5～1 hour, reaction finishes with pH value to 5.5～6.5 of hydrochloric acid conditioned reaction liquid;
4) filtering reacting liquid obtains product and octenyl succinic acid anhydride raffinate rapidly, water, ethanol, mass concentration are not less than 80% ethanol and respectively wash product one time respectively then, and washings mixes with the octenyl succinic acid anhydride raffinate after filtering and obtains the octenyl succinic acid anhydride mixed solution; Product again drying, pulverize, sieve can obtain white starch octenyl succinate anhydride;
5) in the step 4) gained octenyl succinic acid anhydride mixed solution after distillation, replenishing octenyl succinic acid anhydride and solubilizing agent dissolving, can become step 2) described octenyl succinic acid anhydride solution, unreacted octenyl succinic acid anhydride is realized recycle, and water that distillation obtains and ethanol can be used as mass concentration and is not less than 80% ethanol use behind fractionation, adjustment alcohol concn.
Described starch comprises the starch of Glutinous Semen Maydis, corn, wheat, potato, early rice, wax rice and cassava; Described alcohol concn gas Chromatographic Determination, octenyl succinic acid anhydride content high-performance liquid chromatogram determination.
Advantage of the present invention is: 1) directly join in the octenyl succinic acid anhydride solution of high-speed stirring with Sprayable by starch emulsion being mixed up pH value back, save the troublesome operation of real-time control reacting liquid pH value, and significantly promoted reaction efficiency, make whole technology simple and easy to control; 2) by adjusting the concentration and the solvent composition of octenyl succinic acid anhydride, directly make unreacted octenyl succinic acid anhydride and solvent obtain recycle, in the conservation cost, more realized green production.
Embodiment
The present invention reacts by 100 parts of butt starch are joined in the octenyl succinic acid anhydride solution that contains 3 parts of octenyl succinic acid anhydrides with Sprayable after adding water homogenisation emulsification, regulating pH value to 8～10, reacts pH value to 5.5～6.5 of the conditioned reaction liquid that finishes; Filtering reacting liquid, to product carry out three washings, dry, pulverize and sieve and can obtain the starch octenyl succinate anhydride of white; Raffinate behind the reacting liquid filtering with filter after washings mix and obtain the octenyl succinic acid anhydride mixed solution, after distillation, replenishing octenyl succinic acid anhydride and solubilizing agent dissolving, can become octenyl succinic acid anhydride solution, water that distillation obtains and ethanol are reusable behind fractionation, adjustment alcohol concn.The present invention is described in detail below in conjunction with embodiment.The present invention is all drawing typical curve with standard specimen with gas Chromatographic Determination ethanol with before with the high-performance liquid chromatogram determination octenyl succinic acid anhydride, detects the peak area that obtains can calculate actual ethanol and octenyl succinic acid anhydride by the typical curve equation quality
Embodiment 1
1) 100kg butt waxy corn starch mixes also homogenizing emulsifying 5 minutes with 100kg water at 30 ℃, obtains finely divided emulsion, adds the pH value to 8 that 3% sodium hydroxide is regulated above-mentioned emulsion then;
2) the 3kg octenyl succinic acid anhydride being dissolved in the 100kg mass concentration is that 80% ethanol obtains octenyl succinic acid anhydride solution;
3) step 1) gained emulsion being joined 1000r/min with Sprayable and stirs step 2 down) in the described octenyl succinic acid anhydride solution, control reaction temperature is 60 ℃, react 0.5 hour, reacts the pH value to 5.5 of the usefulness hydrochloric acid conditioned reaction liquid that finishes;
4) filtering reacting liquid obtains product and octenyl succinic acid anhydride raffinate rapidly, be that 80% ethanol respectively washs product one time with 30kg water, 30kg ethanol, 30kg mass concentration respectively then, washings mixes with the octenyl succinic acid anhydride raffinate after filtering and obtains the octenyl succinic acid anhydride mixed solution; Product drying, pulverizing, mistake 100 mesh sieves again can obtain white octenyl succinic waxy corn starch ester, and substitution value is 0.018 after measured;
5) underpressure distillation of gained octenyl succinic acid anhydride mixed solution is to 1kg in the step 4), and octenyl succinic acid anhydride accounts for 0.67kg after testing, adds the 2.33kg octenyl succinic acid anhydride; Slipping out liquid, to obtain the 130kg mass concentration through multiple fractionation be 85.2% ethanol, gets wherein 100kg and be used to dissolve octenyl succinic acid anhydride and get octenyl succinic acid anhydride solution, and residue 30kg is used for washing; The about 100kg low-concentration ethanol of residue is used for cleaning reaction still and pipeline after slipping out the liquid fractionation.
Embodiment 2
1) 100kg butt W-Gum mixes also homogenizing emulsifying 30 minutes with 150kg water at 60 ℃, obtains finely divided emulsion, adds the pH value to 10 that 3% yellow soda ash is regulated above-mentioned emulsion then;
2) the 3kg octenyl succinic acid anhydride being dissolved in the 150kg mass concentration is that 85% ethanol obtains octenyl succinic acid anhydride solution;
3) step 1) gained emulsion being joined 2000r/min with Sprayable and stirs step 2 down) in the described octenyl succinic acid anhydride solution, control reaction temperature is 30 ℃, react 1 hour, reacts the pH value to 6.5 of the usefulness hydrochloric acid conditioned reaction liquid that finishes;
4) filtering reacting liquid obtains product and octenyl succinic acid anhydride raffinate rapidly, be that 83% ethanol respectively washs product one time with 30kg water, 30kg ethanol, 30kg mass concentration respectively then, washings mixes with the octenyl succinic acid anhydride raffinate after filtering and obtains the octenyl succinic acid anhydride mixed solution; Product drying, pulverizing, mistake 100 mesh sieves again can obtain white octenyl succinic W-Gum ester, and substitution value is 0.012 after measured;
5) underpressure distillation of gained octenyl succinic acid anhydride mixed solution is to 2kg in the step 4), and octenyl succinic acid anhydride accounts for 1.42kg after testing, adds the 1.58kg octenyl succinic acid anhydride; Slipping out liquid, to obtain the 180kg mass concentration through multiple fractionation be 78.2% ethanol, adds 20kg ethanol, gets wherein 150kg and be used to dissolve octenyl succinic acid anhydride and get octenyl succinic acid anhydride solution, and residue 50kg is used for washing; The about 170kg low-concentration ethanol of residue is used for cleaning reaction still and pipeline after slipping out the liquid fractionation.
Embodiment 3
1) 100kg butt wheat starch mixes also homogenizing emulsifying 10 minutes with 120kg water at 40 ℃, obtains finely divided emulsion, adds the pH value to 9 that 3% sodium hydroxide is regulated above-mentioned emulsion then;
2) the 3kg octenyl succinic acid anhydride is dissolved in 120kg ethanol and obtains octenyl succinic acid anhydride solution;
3) step 1) gained emulsion being joined 1500r/min with Sprayable and stirs step 2 down) in the described octenyl succinic acid anhydride solution, control reaction temperature is 50 ℃, react 40 minutes, reacts the pH value to 6 of the usefulness hydrochloric acid conditioned reaction liquid that finishes;
4) filtering reacting liquid obtains product and octenyl succinic acid anhydride raffinate rapidly, be that 85% ethanol respectively washs product one time with 50kg water, 30kg ethanol, 30kg mass concentration respectively then, washings mixes with the octenyl succinic acid anhydride raffinate after filtering and obtains the octenyl succinic acid anhydride mixed solution; Product drying, pulverizing, mistake 100 mesh sieves again can obtain white octenyl succinic wheat starch ester, and substitution value is 0.019 after measured;
5) underpressure distillation of gained octenyl succinic acid anhydride mixed solution is to 1kg in the step 4), and octenyl succinic acid anhydride accounts for 0.48kg after testing, adds the 2.52kg octenyl succinic acid anhydride; Slipping out liquid, to obtain the 150kg mass concentration through multiple fractionation be 86.7% ethanol, gets wherein 120kg and be used to dissolve octenyl succinic acid anhydride and get octenyl succinic acid anhydride solution, and residue 30kg is used for washing; The about 150kg low-concentration ethanol of residue is used for cleaning reaction still and pipeline after slipping out the liquid fractionation.
Embodiment 4
1) 100kg butt yam starch mixes also homogenizing emulsifying 15 minutes with 130kg water at 50 ℃, obtains finely divided emulsion, adds the pH value to 8.5 that 3% yellow soda ash is regulated above-mentioned emulsion then;
2) the 3kg octenyl succinic acid anhydride being dissolved in the 110kg mass concentration is that 90% ethanol obtains octenyl succinic acid anhydride solution;
3) step 1) gained emulsion being joined 1200r/min with Sprayable and stirs step 2 down) in the described octenyl succinic acid anhydride solution, control reaction temperature is 55 ℃, react 45 minutes, reacts the pH value to 5.8 of the usefulness hydrochloric acid conditioned reaction liquid that finishes;
4) filtering reacting liquid obtains product and octenyl succinic acid anhydride raffinate rapidly, be that 90% ethanol respectively washs product one time with 30kg water, 30kg ethanol, 30kg mass concentration respectively then, washings mixes with the octenyl succinic acid anhydride raffinate after filtering and obtains the octenyl succinic acid anhydride mixed solution; Product drying, pulverizing, mistake 100 mesh sieves again can obtain white octenylsuccinate potato starch ester, and substitution value is 0.017 after measured;
5) underpressure distillation of gained octenyl succinic acid anhydride mixed solution is to 1kg in the step 4), and octenyl succinic acid anhydride accounts for 0.83kg after testing, adds the 2.17kg octenyl succinic acid anhydride; Slipping out liquid, to obtain the 140kg mass concentration through multiple fractionation be 83.8% ethanol, gets wherein 110kg and be used to dissolve octenyl succinic acid anhydride and get octenyl succinic acid anhydride solution, and residue 30kg is used for washing; The about 150kg low-concentration ethanol of residue is used for cleaning reaction still and pipeline after slipping out the liquid fractionation.
Embodiment 5
1) 100kg butt early rice starch mixes also homogenizing emulsifying 20 minutes with 125kg water at 45 ℃, obtains finely divided emulsion, adds the pH value to 9.5 that 3% yellow soda ash is regulated above-mentioned emulsion then;
2) the 3kg octenyl succinic acid anhydride being dissolved in the 100kg mass concentration is that 95% ethanol obtains octenyl succinic acid anhydride solution;
3) step 1) gained emulsion being joined 1600r/min with Sprayable and stirs step 2 down) in the described octenyl succinic acid anhydride solution, control reaction temperature is 55 ℃, react 0.5 hour, reacts the pH value to 5.8 of the usefulness hydrochloric acid conditioned reaction liquid that finishes;
4) filtering reacting liquid obtains product and octenyl succinic acid anhydride raffinate rapidly, be that 80% ethanol respectively washs product one time with 30kg water, 30kg ethanol, 30kg mass concentration respectively then, washings mixes with the octenyl succinic acid anhydride raffinate after filtering and obtains the octenyl succinic acid anhydride mixed solution; Product drying, pulverizing, mistake 100 mesh sieves again can obtain white octenyl succinic early rice starch ester, and substitution value is 0.014 after measured;
5) underpressure distillation of gained octenyl succinic acid anhydride mixed solution is to 2kg in the step 4), and octenyl succinic acid anhydride accounts for 1.18kg after testing, adds the 1.82kg octenyl succinic acid anhydride; Slipping out liquid, to obtain the 130kg mass concentration through multiple fractionation be 88.7% ethanol, gets wherein 100kg and be used to dissolve octenyl succinic acid anhydride and get octenyl succinic acid anhydride solution, and residue 30kg is used for washing; The about 110kg low-concentration ethanol of residue is used for cleaning reaction still and pipeline after slipping out the liquid fractionation.
Embodiment 6
1) 100kg butt wax Starch rice mixes also homogenizing emulsifying 8 minutes with 100kg water at 30 ℃, obtains finely divided emulsion, adds the pH value to 8.8 that 2% sodium hydroxide is regulated above-mentioned emulsion then;
2) the 3kg octenyl succinic acid anhydride being dissolved in the 110kg mass concentration is that 88% ethanol obtains octenyl succinic acid anhydride solution;
3) step 1) gained emulsion being joined 1700r/min with Sprayable and stirs step 2 down) in the described octenyl succinic acid anhydride solution, control reaction temperature is 50 ℃, react 0.5 hour, reacts the pH value to 5.7 of the usefulness hydrochloric acid conditioned reaction liquid that finishes;
4) filtering reacting liquid obtains product and octenyl succinic acid anhydride raffinate rapidly, be that 90% ethanol respectively washs product one time with 40kg water, 30kg ethanol, 40kg mass concentration respectively then, washings mixes with the octenyl succinic acid anhydride raffinate after filtering and obtains the octenyl succinic acid anhydride mixed solution; Product drying, pulverizing, mistake 100 mesh sieves again can obtain white octenyl succinic wax Starch rice ester, and substitution value is 0.015 after measured;
5) underpressure distillation of gained octenyl succinic acid anhydride mixed solution is to 1.5kg in the step 4), and octenyl succinic acid anhydride accounts for 1.04kg after testing, adds the 1.96kg octenyl succinic acid anhydride; Slipping out liquid, to obtain the 140kg mass concentration through multiple fractionation be 85.2% ethanol, gets wherein 110kg and be used to dissolve octenyl succinic acid anhydride and get octenyl succinic acid anhydride solution, and residue 30kg is used for washing; The about 150kg low-concentration ethanol of residue is used for cleaning reaction still and pipeline after slipping out the liquid fractionation.
Embodiment 7
1) 100kg butt tapioca (flour) mixes also homogenizing emulsifying 25 minutes with 140kg water at 45 ℃, obtains finely divided emulsion, adds the pH value to 9.2 that 1.5% yellow soda ash is regulated above-mentioned emulsion then;
2) the 3kg octenyl succinic acid anhydride being dissolved in the 150kg mass concentration is that 82% ethanol obtains octenyl succinic acid anhydride solution;
3) step 1) gained emulsion being joined 1000r/min with Sprayable and stirs step 2 down) in the described octenyl succinic acid anhydride solution, control reaction temperature is 40 ℃, react 0.5 hour, reacts the pH value to 6.3 of the usefulness hydrochloric acid conditioned reaction liquid that finishes;
4) filtering reacting liquid obtains product and octenyl succinic acid anhydride raffinate rapidly, be that 90% ethanol respectively washs product one time with 40kg water, 30kg ethanol, 50kg mass concentration respectively then, washings mixes with the octenyl succinic acid anhydride raffinate after filtering and obtains the octenyl succinic acid anhydride mixed solution; Product drying, pulverizing, mistake 100 mesh sieves again can obtain white tapioca starch sodium octenyl succinate, and substitution value is 0.013 after measured;
5) underpressure distillation of gained octenyl succinic acid anhydride mixed solution is to 1.5kg in the step 4), and octenyl succinic acid anhydride accounts for 1.27kg after testing, adds the 1.73kg octenyl succinic acid anhydride; Slipping out liquid, to obtain the 200kg mass concentration through multiple fractionation be 79.2% ethanol, adds 15kg ethanol, gets wherein 150kg and be used to dissolve octenyl succinic acid anhydride and get octenyl succinic acid anhydride solution, and residue 65kg is used for washing; The about 165kg low-concentration ethanol of residue is used for cleaning reaction still and pipeline after slipping out the liquid fractionation.
Claims (3)
1. a recycle octenyl succinic acid anhydride prepares the method for starch ester, it is characterized in that may further comprise the steps, following umber all by weight:
1) 100 parts of butt starch mix under 30 ℃～60 ℃ with 100～150 parts of water, and homogenizing emulsifying 5～30 minutes obtains finely divided emulsion, add pH value to 8～10 that sodium hydroxide or yellow soda ash are regulated above-mentioned emulsion then;
2) 3 parts of octenyl succinic acid anhydrides being dissolved in 100～150 parts of mass concentrations is not less than 80% ethanol and obtains octenyl succinic acid anhydride solution;
3) step 1) gained emulsion is joined the step 2 of 1000～2000r/min under stirring with Sprayable) in the described octenyl succinic acid anhydride solution, control reaction temperature is 30 ℃～60 ℃, reacted 0.5～1 hour, reaction finishes with pH value to 5.5～6.5 of hydrochloric acid conditioned reaction liquid;
4) filtering reacting liquid obtains product and octenyl succinic acid anhydride raffinate rapidly, water, ethanol, mass concentration are not less than 80% ethanol and respectively wash product one time respectively then, and washings mixes with the octenyl succinic acid anhydride raffinate after filtering and obtains the octenyl succinic acid anhydride mixed solution; Product again drying, pulverize, sieve can obtain white starch octenyl succinate anhydride;
5) in the step 4) gained octenyl succinic acid anhydride mixed solution after distillation, replenishing octenyl succinic acid anhydride and solubilizing agent dissolving, can become step 2) described octenyl succinic acid anhydride solution, unreacted octenyl succinic acid anhydride is realized recycle, and water that distillation obtains and ethanol can be used as mass concentration and is not less than 80% ethanol use behind fractionation, adjustment alcohol concn.
2. recycle octenyl succinic acid anhydride according to claim 1 prepares the method for starch ester, it is characterized in that described starch is the starch of Glutinous Semen Maydis, corn, wheat, potato, early rice, wax rice and cassava.
3. recycle octenyl succinic acid anhydride according to claim 1 prepares the method for starch ester, it is characterized in that described alcohol concn gas Chromatographic Determination, octenyl succinic acid anhydride content high-performance liquid chromatogram determination.
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| CN109485739A (en) * | 2018-11-06 | 2019-03-19 | 浙江新和成股份有限公司 | A kind of preparation method of starch octenyl succinate anhydride |
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