CN104086662B - Acid-heat degradation and enzymolysis preparation method of low-viscosity octenyl succinic anhydride modified starch - Google Patents
Acid-heat degradation and enzymolysis preparation method of low-viscosity octenyl succinic anhydride modified starch Download PDFInfo
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Abstract
The invention discloses an acid-heat degradation and enzymolysis preparation method of low-viscosity octenyl succinic anhydride modified starch. The method comprises the following steps: raw starch is prepared into a slurry; alkaline liquid is added; octenyl succinic anhydride is fed; an esterification reaction is allowed; neutralization and liquid-removal are carried out; washing refining is carried out; a filter cake is prepared into a slurry; the pH value is regulated; an acid hydrolysis reaction is carried out; a continuous-ejection high-temperature acid-heat treatment is carried out; laminar-flow thermal insulation is carried out; cooling is carried out; a saturated calcium hydroxide solution is added; the mixture is stirred such that neutralization is carried out; pullulanase is added for carrying out debranching enzymolysis; active carbon is added; temperature is increased and decolorization is carried out; pressure filtration is carried out; the filtrate is concentrated under vacuum; fine filtration is carried out; spray drying is carried out; and cooling and packaging are carried out, such that a product is obtained. The product is suitable to be used as an emulsifier of foods and daily chemicals, or as a microencapsulation material. With the method, the low-viscosity water-soluble octenyl succinic anhydride modified starch product can be produced, and good economical benefit can be achieved. With a pullulanase debranching effect upon modified starch molecules, more products with linear or low-branch-degree molecular structures can be produced, such that product emulsifying and film-forming properties can be improved.
Description
Technical field
The present invention relates to the process of a kind of degraded of employing acid heat and enzymatic degradation is and in particular to a kind of low viscosity octenyl
The acid heat degraded of succinic acid starch ester and enzymolysis preparation.
Background technology
Starch alkenyl succinate ester is with ative starch or starch derivatives as raw material, in the basic conditions with containing different length
The alkenyl succinic anhydride of carbochain, through kind of starch ester products obtained from esterification, mainly has octenyl succinic acid anhydride decene
Base succinic anhydrides, dodecenylsuccinic anhydride and hexadecylene base succinic anhydrides, are allowed for food starch degenerative treatments at present
Be only octenyl succinic acid anhydride.
Starch octenyl succinate anhydride (octenyl succinic anhydride modified starch, referred to as
Osa- starch) it is the modified starch product developed by U.S. caldwell and wurzburg company, in nineteen fifty-three application
Patent.Osa starch is classified as the product of generally accepted safety (gras) by Food and Drug Administration (fda), and 1972 beautiful
This product has been shown on the food chemicals handbook that state publishes.China is used this modified starch can conduct in approval in 1997
Food additive, calendar year 2001 is ratified to expand this product scope used in food again, and consumption can add according to demand, need not
Control.
Starch octenyl succinate anhydride is different from other traditional modified starches, has surface activity and emulsifying thickening
Agent, molecular weight is again larger, especially in oil-in-water emulsion, can play important and efficient effect.Had due to it
Specific function, using effect is good, is widely used in varieties of food items and daily chemical products, such as emulsifying essence, microscapsule powder system
Product, powdered oil, soft drink, yogurt and cheese, tinned food and cosmetics, apply in weaving, papermaking and medicine, latex in addition
Also there is use in material, be the modified starch product of high-end high market price.Starch octenyl succinate anhydride product, mainly has two big
Classification:
(1) one class is the modified starch product prepared for raw material with ative starch, is mainly used as thickening agent, has certain simultaneously
Surface activity, be suitable for gluing in highly concentrated food or chemical products in some height and use.The modified starch product of this kind of high concentration
Generally monotropy, of less types, the manufacturing is relatively easy to, and technical requirements are not relatively high, the quality of domestic and international product
No obvious difference.
(2) another kind of is ocentyl succinic (former) starch ester through appropriateness degraded, prepared low viscous octenyl
Succinic acid starch ester, typically has cold water soluble, it is possible to have cold water is insoluble, is mainly used as emulsion stabilizer or micro-
Capsule wall material.The low viscous starch octenyl succinate anhydride product of cold water not property, typically also needs to gelatinizing during use.This kind of pungent
Starch alkenyl succinate ester is composite modified starch product, and different biodegrading process and degree can obtain the series of different qualities
Product, kind is more, and it manufactures step and technique is complex, and the requirement of production technology is higher, the quality of home products
Quality is larger with external gap.
Starch octenyl succinic acid anhydride carries out, after esterification, introducing long carbochain, improve esterification starch
Paste viscosity, the starch viscosity after degeneration is very high, limits its application.In order to solve this problem generally using the side of degraded
Method, reduces the relative molecular weight of starch, such as makes its dextrin, can reach the low viscous purpose of fall.It is obtained through appropriateness degraded
Low-viscosity octenyl succinic anhydride modified starch, can as microcapsule wall timber-used in embed water-insoluble nonvolatile component thing
Matter, compared with the wall material traditional with arabic gum, dextrin, maltodextrin etc., from the aspect of many, resultant effect will be got well.
Preparing low-viscosity octenyl succinic anhydride modified starch technology path mainly has synthetic starch ester to be degraded again, or former
Starch is esterified after degraded again.The method of degraded includes thermal degradation, hypochlorite oxidation, acid hydrolysis and enzymolysis, sour water
Solution and enzymolysis are most common methods.Acidolysis is acid hydrolysis starch milk at high temperature, and the de value typically smaller than 10 of product, than former
Starch has more linear side chain.Enzyme used by enzymolysis is α-amylase or beta amylase.Using during α-amylase it is desirable to product
De value is less than 20, and needs Heat Gelatinization in advance before digesting.Molecular structure and β-restriction using beta amylase products obtained therefrom
Dextrin is similar to, and has good emulsifiability.Sun unit pretty young woman etc. is degraded using i.e. α-amylase and saccharifying enzyme, and de value has been obtained
For 30, mobility is 80 low-viscosity octenyl succinic anhydride modified starch.Richards of the U.S. etc., trzasko etc., Japan plus rattan
Deng personage, all the degraded of starch octenyl succinate anhydride is carried out with systematic study, result shows using ferment treatment octenyl succinic
Acid-starch ester, can forming part branched oligosaccharides, can effectively reduce the viscosity of modified starch, also improve other performances simultaneously,
Strengthen as pasted transparency, freeze thawing resistance stability improves, dissolubility increases, the stability in water strengthens etc., expand it and use model
Enclose.Blue etc., with different starch enzymatic degradation starch octenyl succinate anhydrides, obtains the product of different dextrose equivalents (19.8～45),
Its application in microcapsule wall material is studied, is found that there is preferable embedding effect.
Using different biodegrading process and process conditions, different low viscosities or the ocentyl succinic of de value can be prepared
Starch ester product, disclosure satisfy that different application requirements.
Content of the invention
The present invention is according to existing production method and technology, there is provided a kind of acid of low-viscosity octenyl succinic anhydride modified starch
Thermal degradation and enzymolysis preparation, prepare low viscosity water miscible starch octenyl succinate anhydride product.
A kind of employing acid heat degraded and the process meanses of enzymolysis that the present invention provides, prepare the water miscible octenyl of low viscosity
Succinic acid starch ester method, size mixing including starch, esterification, neutralization, de- liquid washing, acid adjustment of sizing mixing, acidolysis reaction, continuous spray
Penetrate high-temperature process, isothermal holding, neutralization, debranching enzyme enzymolysis, decolouring, concentrated in vacuo, filter, be spray-dried, cooling and packaging etc.
Step, specifically comprises the following steps that
(1) size mixing, esterification, neutralization: starch stirring be added to the water, obtain starch emulsion, the solid amount of substance of serosity
Concentration be 40%～45%(w/w), heat up 40 DEG C ~ 50 DEG C, use concentration 10%(w/w) sodium carbonate liquor adjust starch milk ph be
8.5 ~ 9.5, keep temperature and the ph of starch milk, the octenyl succinic acid anhydride of stream plus relative starch quality 1% ~ 8% is reacted, ester
6 ~ 24 hours change time, then use concentration 10%(v/v) hydrochloric acid solution in and starch milk ph to 6.0 ~ 6.5；
Starch described in above-mentioned steps includes common corn starch, waxy corn starch, Maninot esculenta crantz., Semen Tritici aestivi or the former shallow lake of Rhizoma Solani tuber osi
Powder；When low viscous starch octenyl succinate anhydride products application is in field of food, the usage ratio of octenyl succinic acid anhydride
Not can exceed that relative starch quality 3.0%, optimal 2.8% ~ 3.0%.Auxiliary agent as pesticide, daily use chemicals is used, ocentyl succinic
The usage ratio of acid anhydride is high, and application effect can be more preferably.
(2) liquid washing, acid adjustment of sizing mixing, acidification reaction are taken off: the emulsion filter pressing after neutralization or the method removing waste liquid of centrifugation,
Wash with water, more de- liquid.Filter cake adds water and sizes mixing, and uses concentration 10%(w/w) oxalic acid solution adjust starch emulsion ph be 2.0 ~ 2.8,
The dry substance mass concentration of emulsion is 15%～25%(w/w), it is warming up to 45 DEG C ~ 50 DEG C, it is little that stirring carries out acidolysis reaction 2.0 ~ 4.0
When.
In above-mentioned steps, preferably ph scope is 2.0 ~ 2.4, acidolysis reaction 3.5 ~ 4.0 hours, and the ph of system is lower, acidolysis
Temperature is higher, and the time is longer, and the palliating degradation degree of starch is bigger.
(3) continuously injection high-temperature process, isothermal holding, neutralization, debranching enzyme digest: right at 125 DEG C ~ 130 DEG C with water heater
The modified starch breast of acidolysis carries out the continuous injection high-temperature process of 3 ~ 5 minutes, is incubated 1.0 ~ 2.5 in 90 DEG C ~ 99 DEG C underflows little
When；In different temperature retention time samplings, measure dextrose equivalent de value or the fluidity value of hydrolyzed solution, to control the hydrolysis obtaining needs
The product of degree.While adding the calcium hydroxide saturated solution ground with colloid mill, stirring neutralization system to ph is 4.9 ~ 5.1,
While being cooled to 55 DEG C ~ 57 DEG C, adding the debranching enzyme of relative starch quality 0.15 ~ 0.25% to carry out the de- of modified starch molecule and propping up
Effect, 2 ~ 4 hours time, produces the product more having wire or propping up the low molecular structure of fork degree.
In said method, the optional Novi of debranching enzyme believes the Pullulan such as promozyme d2 or Jie Neng section optimax l-1000
Enzyme.
(4) decolouring, filtration: add the activated carbon of relative starch quality 1.5% ~ 2.0%, heat up, stirring decolouring at 80 DEG C
0.5 hour, filter pressing obtained cleaner liquid, and, preferably more than 60 DEG C, the viscosity of filtrate is relatively low for temperature during filtration, was easier to filter.
(5) concentrate, be spray-dried, cool down, pack: filter vacuum is concentrated into concentration 40% ~ 50%(w/w), fine straining, remove
Possible granule.Cleaner liquid spray dryer is dried with typically conventional process conditions (such as preparing the maltodextrin of solid),
Through the cooling of 20 DEG C ~ 25 DEG C, the air of relative humidity about 50%, to 38 DEG C or less, packaging, obtain low viscous octenyl
Succinic acid starch ester product, has water solublity.
In said method, the catalyst that hydrolyzed as modified starch acidolysis using oxalic acid, using the degeneration to acidolysis for the water heater
Starch milk is continuously sprayed the process of high temperature.
In said method, material after continuous injection high-temperature process, it is incubated 1.0 ~ 2.5 in 90 DEG C ~ 99 DEG C underflows
Hour, continue further degraded.
In said method, the catalyst that hydrolyzed as modified starch acidolysis using oxalic acid, with the ground hydroxide of colloid mill
Calcium saturated solution neutralizes, and can form the indissoluble thing such as calcium oxalate.
In said method, cleaner liquid is dried with spray dryer, obtains low viscous starch octenyl succinate anhydride product.
The present invention compared with prior art, has the advantage that
(1) present invention on the basis of original solid maltodextrin production line, can add the reactor of part, stream adds
The production equipments such as tank, material-compound tank and storage tank, carry out certain technological transformation such as equipment, pipeline it becomes possible to production preparation low viscosity is water-soluble
The starch octenyl succinate anhydride product of property, realizes preferable economic benefit.
(2) ocentyl succinic (former) starch ester that the present invention obtains in preceding step, first in starch gelatinization temperature and acid
Property under the conditions of carry out a certain degree of acidolysis, can be next step continuous injection high temperature acid heat process, the viscosity reduction of plant process
Make certain contribution.
(3) present invention using starch liquefacation with water heater continuously sprayed high-temperature acid heat treatment so that system can be fast
The high-viscosity stage that speed is led to by starch or modified starch gelatinization process, then pass through 90 DEG C ~ 99 DEG C of laminar flow insulation effect,
Modified starch is little by little degraded.Certain de value or mobility can be obtained according to the time of the ph of acid heat effect and laminar flow insulation, regulation and control
Scope low viscous starch octenyl succinate anhydride product (de be dextrose equivalent, the de value of starch is 0, glucose be 100,
De is 1 or more starch or the hydrolyzate of modified starch, and its viscosity number will greatly reduce than ative starch).
(4) present invention adopts oxalic acid as the catalyst of acid heat high-temperature process and hydrolysis, with calcium hydroxide or Calcium Carbonate
Neutralization can form the calcium oxalate material of indissoluble, together can remove with activated carbon after decolorization filtering.
(5) present invention adopt the de- Zhi Zuoyong to modified starch molecule for the pullulanase, can produce more have wire or
Prop up the product of the low molecular structure of fork degree, improve the emulsifying filming performance of product.
Specific embodiment
The present invention is implemented through the following steps:
Tune ph → stream is sized mixing → heated up to ative starch → add water plus octenyl succinic acid anhydride carries out esterification → neutralization → take off
Liquid → wash → add water oxalic acid of sizing mixing → add adjusts ph continuously to spray high-temperature acid heat treatment to 2.0 ~ 2.8 → acidolysis reaction → water heater
→ laminar flow insulation → cooling → interpolation calcium hydroxide saturated solution neutralization → debranching enzyme enzymolysis → activated carbon decolorizing → filter pressing → true
Empty concentration → spray drying → cooling → packaging → low viscous starch octenyl succinate anhydride product.
Embodiment 1
(1) size mixing, esterification: the corn starch of 1000 dry weight parts, sized mixing with water, newborn concentration 40.0%(w/w),
Be warming up to 50 DEG C, concentration 10%(w/w) sodium carbonate liquor to adjust the ph of starch milk be 9.5, keep the temperature of starch milk and ph,
Stream plus 1%(relative starch quality) octenyl succinic acid anhydride esterification 6 hours, concentration 10%(v/v) hydrochloric acid solution neutralization
The ph of starch milk to 6.0.
(2) liquid washing, acid adjustment of sizing mixing, acidification reaction are taken off: the starch emulsion pressure filter after neutralization removes waste liquid, washes with water
Wash to washing liquid electrical conductivity be not more than 100 μ s/cm, filter cake adds water and sizes mixing, and uses concentration 10%(w/w) oxalic acid solution adjust emulsion
Ph is 2.0, and the dry substance mass concentration of emulsion is 25%(w/w), it is warming up to 50 DEG C, stirring carries out acidolysis reaction 4.0 hours.
(3) continuously injection high-temperature process, isothermal holding, neutralization, debranching enzyme digest: acidolysis is formed sediment at 130 DEG C with water heater
Powder breast carries out the continuous injection high-temperature process of 5 minutes, is incubated 2.5 hours in 97 DEG C ~ 99 DEG C underflows, interpolation colloid mill
Ground calcium hydroxide saturated solution, stirring neutralization system is 5.1 to ph, is cooled to 57 DEG C, adds 0.15%(relatively
Starch quality) Novi believe that promozyme d2 pullulanase carries out the de- Zhi Zuoyong of modified starch molecule, time 2 h.
(4) decolouring, filter: add 2.0%(relative starch quality) activated carbon, heat up, at 80 DEG C stir decolouring 0.5
Hour, filter pressing obtains cleaner liquid.
(5) concentrate, be spray-dried, cool down, pack: solution is concentrated in vacuo to concentration 50%(w/w), fine straining, cleaner liquid is used
Spray dryer is dried；Material through 20 DEG C, the cold air of relative humidity about 50% be cooled to 35 DEG C, packaging, obtain de
The starch octenyl succinate anhydride product of value 31.9.
Embodiment 2
(1) size mixing, esterification: the corn starch of 1000 dry weight parts, sized mixing with water, newborn concentration 42.0%(w/w),
Be warming up to 45 DEG C, concentration 10%(w/w) sodium carbonate liquor to adjust the ph of starch milk be 9.0, keep the temperature of starch milk and ph,
Stream plus 3%(relative starch quality) octenyl succinic acid anhydride esterification 14 hours, concentration 10%(v/v) hydrochloric acid solution neutralization
The ph of starch milk to 6.0.
(2) liquid washing, acid adjustment of sizing mixing, acidification reaction are taken off: the starch emulsion pressure filter after neutralization removes waste liquid, washes with water
Wash to washing liquid electrical conductivity be not more than 100 μ s/cm, filter cake adds water and sizes mixing, and uses concentration 10%(w/w) oxalic acid solution adjust emulsion
Ph is 2.5, and the dry substance mass concentration of emulsion is 20%(w/w), it is warming up to 45 DEG C, stirring carries out acidolysis reaction 2.0 hours.
(3) continuously injection high-temperature process, isothermal holding, neutralization, debranching enzyme digest: acidolysis is formed sediment at 125 DEG C with water heater
Powder breast carries out the continuous injection high-temperature process of 3 minutes, is incubated 1.0 hours in 90 DEG C ~ 94 DEG C underflows, interpolation colloid mill
Ground calcium hydroxide saturated solution, stirring neutralization system is 4.9 to ph, is cooled to 57 DEG C, adds 0.25%(relatively
Starch quality) Novi believe that promozyme d2 pullulanase carries out the de- Zhi Zuoyong of modified starch molecule, 4 hours time.
(4) decolouring, filter: add 1.5%(relative starch quality) activated carbon, heat up, at 80 DEG C stir decolouring 0.5
Hour, filter pressing obtains cleaner liquid.
(5) concentrate, be spray-dried, cool down, pack: solution is concentrated in vacuo to concentration 43%(w/w), fine straining, cleaner liquid is used
Spray dryer is dried；Material through 25 DEG C, the cold air of relative humidity about 50% be cooled to 38 DEG C, packaging, obtain de
The starch octenyl succinate anhydride product of value 9.5.
Embodiment 3
(1) size mixing, esterification: the corn starch of 1000 dry weight parts, sized mixing with water, newborn concentration 42.0%(w/w),
Be warming up to 45 DEG C, concentration 10%(w/w) sodium carbonate liquor to adjust the ph of starch milk be 9.0, keep the temperature of starch milk and ph,
Stream plus 3%(relative starch quality) octenyl succinic acid anhydride esterification 14 hours, concentration 10%(v/v) hydrochloric acid solution neutralization
The ph of starch milk to 6.0.
(2) liquid washing, acid adjustment of sizing mixing, acidification reaction are taken off: the starch emulsion pressure filter after neutralization removes waste liquid, washes with water
Wash to washing liquid electrical conductivity be not more than 100 μ s/cm, filter cake adds water and sizes mixing, and uses concentration 10%(w/w) oxalic acid solution adjust emulsion
Ph is 2.5, and the dry substance mass concentration of emulsion is 20%(w/w), it is warming up to 45 DEG C, stirring carries out acidolysis reaction 2.0 hours.
(3) continuously injection high-temperature process, isothermal holding, neutralization, debranching enzyme digest: acidolysis is formed sediment at 125 DEG C with water heater
Powder breast carries out the continuous injection high-temperature process of 3 minutes, is incubated 2.5 hours in 90 DEG C ~ 94 DEG C underflows, interpolation colloid mill
Ground calcium hydroxide saturated solution, stirring neutralization system is 4.9 to ph, is cooled to 57 DEG C, adds 0.20%(relatively
Starch quality) Novi believe that promozyme d2 pullulanase carries out the de- Zhi Zuoyong of modified starch molecule, 3 hours time.
(4) decolouring, filter: add 1.5%(relative starch quality) activated carbon, heat up, at 80 DEG C stir decolouring 0.5
Hour, filter pressing obtains cleaner liquid.
(5) concentrate, be spray-dried, cool down, pack: solution is concentrated in vacuo to concentration 45%(w/w), fine straining, cleaner liquid is used
Spray dryer is dried；Material through 25 DEG C, the cold air of relative humidity about 50% be cooled to 37 DEG C, packaging, obtain de
The starch octenyl succinate anhydride product of value 11.8.
Embodiment 4
(1) size mixing, esterification: the corn starch of 1000 dry weight parts, sized mixing with water, newborn concentration 42.0%(w/w),
Be warming up to 45 DEG C, concentration 10%(w/w) sodium carbonate liquor to adjust the ph of starch milk be 9.0, keep the temperature of starch milk and ph,
Stream plus 3%(relative starch quality) octenyl succinic acid anhydride esterification 14 hours, concentration 10%(v/v) hydrochloric acid solution neutralization
The ph of starch milk to 6.0.
(2) liquid washing, acid adjustment of sizing mixing, acidification reaction are taken off: the starch emulsion pressure filter after neutralization removes waste liquid, washes with water
Wash to washing liquid electrical conductivity be not more than 100 μ s/cm, filter cake adds water and sizes mixing, and uses concentration 10%(w/w) oxalic acid solution adjust emulsion
Ph is 2.2, and the dry substance mass concentration of emulsion is 20%(w/w), it is warming up to 45 DEG C, stirring carries out acidolysis reaction 2.0 hours.
(3) continuously injection high-temperature process, isothermal holding, neutralization, debranching enzyme digest: acidolysis is formed sediment at 125 DEG C with water heater
Powder breast carries out the continuous injection high-temperature process of 5 minutes, is incubated 2.5 hours in 90 DEG C ~ 94 DEG C underflows, interpolation colloid mill
Ground calcium hydroxide saturated solution, stirring neutralization system is 4.9 to ph, is cooled to 57 DEG C, adds 0.20%(relatively
Starch quality) Novi believe that promozyme d2 pullulanase carries out the de- Zhi Zuoyong of modified starch molecule, 4 hours time.
(4) decolouring, filter: add 1.5%(relative starch quality) activated carbon, at 80 DEG C stirring decolouring 0.5 hour,
Filter pressing obtains cleaner liquid.
(5) concentrate, be spray-dried, cool down, pack: solution is concentrated in vacuo to concentration 48%(w/w), fine straining, cleaner liquid is used
Spray dryer is dried；Material through 20 DEG C, the cold air of relative humidity about 50% be cooled to 38 DEG C, packaging, obtain de
The starch octenyl succinate anhydride product of value 19.6.
Embodiment 5
(1) size mixing, esterification: the corn starch of 1000 dry weight parts, sized mixing with water, newborn concentration 42.0%(w/w),
Be warming up to 45 DEG C, concentration 10%(w/w) sodium carbonate liquor to adjust the ph of starch milk be 9.0, keep the temperature of starch milk and ph,
Stream plus 3%(relative starch quality) octenyl succinic acid anhydride esterification 14 hours, concentration 10%(v/v) hydrochloric acid solution neutralization
The ph of starch milk to 6.0.
(2) liquid washing, acid adjustment of sizing mixing, acidification reaction are taken off: the starch emulsion pressure filter after neutralization removes waste liquid, washes with water
Wash to washing liquid electrical conductivity be not more than 100 μ s/cm, filter cake adds water and sizes mixing, and uses concentration 10%(w/w) oxalic acid solution adjust emulsion
Ph is 2.0, and the dry substance mass concentration of emulsion is 25%(w/w), it is warming up to 50 DEG C, stirring carries out acidolysis reaction 3.5 hours.
(3) continuously injection high-temperature process, isothermal holding, neutralization, debranching enzyme digest: acidolysis is formed sediment at 130 DEG C with water heater
Powder breast carries out the continuous injection high-temperature process of 5 minutes, is incubated 2.5 hours in 97 DEG C ~ 99 DEG C underflows, interpolation colloid mill
Ground calcium hydroxide saturated solution, stirring neutralization system is 5.1 to ph, is cooled to 55 DEG C, adds 0.15%(relatively
Starch quality) Novi believe that promozyme d2 pullulanase carries out the de- Zhi Zuoyong of modified starch molecule, 2.5 hours time.
(4) decolouring, filter: add 2.0%(relative starch quality) activated carbon, heat up, at 80 DEG C stir decolouring 0.5
Hour, filter pressing obtains cleaner liquid.
(5) concentrate, be spray-dried, cool down, pack: solution is concentrated in vacuo to concentration 50%(w/w), fine straining, cleaner liquid is used
Spray dryer is dried；Material through 20 DEG C, the cold air of relative humidity about 50% be cooled to 38 DEG C, packaging, obtain de
The starch octenyl succinate anhydride product of value 29.4.
Embodiment 6
(1) size mixing, esterification: the corn starch of 1000 dry weight parts, sized mixing with water, newborn concentration 45.0%(w/w),
Be warming up to 40 DEG C, concentration 10%(w/w) sodium carbonate liquor to adjust the ph of starch milk be 8.5, keep the temperature of starch milk and ph,
Stream plus 8%(relative starch quality) octenyl succinic acid anhydride esterification 24 hours, concentration 10%(v/v) hydrochloric acid solution neutralization
The ph of starch milk to 6.5.
(2) liquid washing, acid adjustment of sizing mixing, acidification reaction are taken off: the starch emulsion centrifuge after neutralization removes waste liquid, washes with water
Wash to washing liquid electrical conductivity be not more than 100 μ s/cm, filter cake adds water and sizes mixing, and uses concentration 10%(w/w) oxalic acid solution adjust emulsion
Ph is 2.8, and the dry substance mass concentration of emulsion is 15%(w/w), it is warming up to 48 DEG C, stirring carries out acidolysis reaction 2.0 hours.
(3) continuously injection high-temperature process, isothermal holding, neutralization, debranching enzyme digest: acidolysis is formed sediment at 130 DEG C with water heater
Powder breast carries out the continuous injection high-temperature process of 5 minutes, is incubated 1.5 hours in 97 DEG C ~ 99 DEG C underflows, interpolation colloid mill
Ground calcium hydroxide saturated solution, stirring neutralization system is 4.9 to ph, is cooled to 55 DEG C, adds 0.25%(relatively
Starch quality) Novi believe that promozyme d2 pullulanase carries out the de- Zhi Zuoyong of modified starch molecule, 4 hours time.
(4) decolouring, filter: add 1.5%(relative starch quality) activated carbon, heat up, at 80 DEG C stir decolouring 0.5
Hour, filter pressing obtains cleaner liquid.
(5) concentrate, be spray-dried, cool down, pack: filtrate liquid is concentrated in vacuo to concentration 40%(w/w), fine straining, cleaner liquid
It is dried with spray dryer；Material through 20 DEG C, the cold air of relative humidity about 50% be cooled to 38 DEG C, packaging, obtain
The starch octenyl succinate anhydride product of de value 5.1.
Embodiment 7
(1) size mixing, esterification: the corn starch of 1000 dry weight parts, sized mixing with water, newborn concentration 45.0%(w/w),
Be warming up to 40 DEG C, concentration 10%(w/w) sodium carbonate liquor to adjust the ph of starch milk be 8.5, keep the temperature of starch milk and ph,
Stream plus 8%(relative starch quality) octenyl succinic acid anhydride esterification 24 hours, concentration 10%(v/v) hydrochloric acid solution neutralization
The ph of starch milk to 6.5.
(2) liquid washing, acid adjustment of sizing mixing, acidification reaction are taken off: the starch emulsion centrifuge after neutralization removes waste liquid, washes with water
Wash to washing liquid electrical conductivity be not more than 100 μ s/cm, filter cake adds water and sizes mixing, and uses concentration 10%(w/w) oxalic acid solution adjust emulsion
Ph is 2.4, and the dry substance mass concentration of emulsion is 15%(w/w), it is warming up to 48 DEG C, stirring carries out acidolysis reaction 2.0 hours.
(3) continuously injection high-temperature process, isothermal holding, neutralization, debranching enzyme digest: acidolysis is formed sediment at 125 DEG C with water heater
Powder breast carries out the continuous injection high-temperature process of 5 minutes, is incubated 1.5 hours in 97 DEG C ~ 99 DEG C underflows, interpolation colloid mill
Ground calcium hydroxide saturated solution, stirring neutralization system is 5.0 to ph, is cooled to 56 DEG C, adds 0.16%(relatively
Starch quality) Jie Neng section optimax l-1000 pullulanase carry out the de- Zhi Zuoyong of modified starch molecule, 3 hours time.
(4) decolouring, filter: add 1.6%(relative starch quality) activated carbon, heat up, at 80 DEG C stir decolouring 0.5
Hour, filter pressing obtains cleaner liquid.
(5) concentrate, be spray-dried, cool down, pack: solution is concentrated in vacuo to concentration 43%(w/w), fine straining, cleaner liquid is used
Spray dryer is dried；Material through 20 DEG C, the cold air of relative humidity about 50% be cooled to 38 DEG C, packaging, obtain de
The starch octenyl succinate anhydride product of value 10.3.
Embodiment 8
(1) size mixing, esterification: the corn starch of 1000 dry weight parts, sized mixing with water, newborn concentration 45.0%(w/w),
Be warming up to 40 DEG C, concentration 10%(w/w) sodium carbonate liquor to adjust the ph of starch milk be 8.5, keep the temperature of starch milk and ph,
Stream plus 8%(relative starch quality) octenyl succinic acid anhydride esterification 24 hours, concentration 10%(v/v) hydrochloric acid solution neutralization
The ph of starch milk to 6.5.
(2) liquid washing, acid adjustment of sizing mixing, acidification reaction are taken off: the starch emulsion centrifuge after neutralization removes waste liquid, washes with water
Wash to washing liquid electrical conductivity be not more than 100 μ s/cm, filter cake adds water and sizes mixing, and uses concentration 10%(w/w) oxalic acid solution adjust emulsion
Ph is 2.2, and the dry substance mass concentration of emulsion is 15%(w/w), it is warming up to 48 DEG C, stirring carries out acidolysis reaction 2.0 hours.
(3) continuously injection high-temperature process, isothermal holding, neutralization, debranching enzyme digest: acidolysis is formed sediment at 125 DEG C with water heater
Powder breast carries out the continuous injection high-temperature process of 3 minutes, is incubated 1.0 hours in 95 DEG C ~ 99 DEG C underflows, interpolation colloid mill
Ground calcium hydroxide saturated solution, stirring neutralization system is 5.0 to ph, is cooled to 56 DEG C, adds 0.16%(relatively
Starch quality) Jie Neng section optimax l-1000 pullulanase carry out the de- Zhi Zuoyong of modified starch molecule, 4 hours time.
(4) decolouring, filter: add 1.6%(relative starch quality) activated carbon, heat up, at 80 DEG C stir decolouring 0.5
Hour, filter pressing obtains cleaner liquid.
(5) concentrate, be spray-dried, cool down, pack: solution is concentrated in vacuo to concentration 45%(w/w), fine straining, cleaner liquid is used
Spray dryer is dried；Material through 20 DEG C, the cold air of relative humidity about 50% be cooled to 38 DEG C, packaging, obtain de
The starch octenyl succinate anhydride product of value 16.5.
Using the technical process of the ative starch raw material such as Maninot esculenta crantz., Semen Tritici aestivi preparation, identical with the method for corn starch raw material, therefore
Slightly.Above-mentioned example is the present invention preferably embodiment, but embodiments of the present invention being not restricted to the described embodiments, its
His any spirit without departing from the present invention and the change made under principle, modification, replacement, combine or simplify, all should be
Equivalent substitute mode, is included within protection scope of the present invention.
Claims (7)
1. a kind of acid heat degraded of low-viscosity octenyl succinic anhydride modified starch and enzymolysis preparation are it is characterised in that include forming sediment
Powder is sized mixing, esterification, neutralization, de- liquid washing, acid adjustment of sizing mixing, acidolysis reaction, continuously spray high-temperature process, isothermal holding, in
With, debranching enzyme enzymolysis, decolouring, filter, concentrated in vacuo, be spray-dried, cooling and packaging step, specifically comprise the following steps that
(1) size mixing, esterification, neutralization: starch stirring be added to the water, obtain starch emulsion, the dry substance percent mass of serosity
Specific concentration is 40%～45%, is warming up to 40 DEG C ~ 50 DEG C, adjusts starch milk with the sodium carbonate liquor of mass percent concentration 10%
Ph is 8.5 ~ 9.5, keeps temperature and the ph of starch milk, and the octenyl succinic acid anhydride of stream plus relative starch quality 1% ~ 8% is carried out instead
Should, esterification time 6 ~ 24 hours, then use the ph to 6.0 ~ 6.5 with starch milk in the hydrochloric acid solution of concentration 10%；
(2) liquid washing, acid adjustment of sizing mixing, acidolysis reaction are taken off: the emulsion filter pressing after neutralization or the method removing waste liquid of centrifugation, use water
Washing takes off liquid again, and filter cake adds water and size mixing, and adjusts emulsion ph value with the oxalic acid solution of mass percent concentration 10%, emulsion solid
Amount of substance percent concentration is 15%～25%, is warming up to 45 DEG C ~ 50 DEG C, and stirring carries out acidolysis reaction, and the degeneration obtaining acidolysis is formed sediment
Powder breast；
(3) continuously injection high-temperature process, isothermal holding, neutralization, debranching enzyme digest: with water heater at 125 DEG C ~ 130 DEG C to acidolysis
Modified starch breast carry out the continuous injection high-temperature process of 3 ~ 5 minutes, be incubated 1.0 ~ 2.5 hours in 90 DEG C ~ 99 DEG C underflows；One
The calcium hydroxide saturated solution ground with colloid mill is added on side, and stirring neutralization system is 4.9 ~ 5.1 to ph, is cooled to 55
DEG C ~ 57 DEG C, add the debranching enzyme of relative starch quality 0.15% ~ 0.25% to be digested, 2 ~ 4 hours time, produce more tools
The product having wire or propping up the low molecular structure of fork degree；
(4) decolouring, filtration: add the activated carbon of relative starch quality 1.5% ~ 2.0%, heat up, stirring decolouring 0.5 is little at 80 DEG C
When, filter pressing obtains cleaner liquid, and temperature during filtration is more than 60 DEG C；
(5) concentrate, be spray-dried, cool down, pack: filter vacuum is concentrated into mass percent concentration 40% ~ 50%, fine straining, filter
Clear liquid is dried with spray dryer, and material, through the cooling of 20 DEG C ~ 25 DEG C, the air of relative humidity 50%, to less than 38 DEG C, wraps
Dress, obtains low-viscosity octenyl succinic anhydride modified starch product.
2. the acid heat degraded of low-viscosity octenyl succinic anhydride modified starch according to claim 1 and enzymolysis preparation, its
It is characterised by, described starch includes common corn starch, waxy corn starch, Maninot esculenta crantz., Semen Tritici aestivi or Rhizoma Solani tuber osi ative starch.
3. the acid heat degraded of low-viscosity octenyl succinic anhydride modified starch according to claim 1 and 2 and enzymolysis preparation,
It is characterized in that, when low-viscosity octenyl succinic anhydride modified starch products application is in field of food, the use of octenyl succinic acid anhydride
Amount ratio not can exceed that relative starch quality 3.0%.
4. the acid heat degraded of low-viscosity octenyl succinic anhydride modified starch according to claim 1 and 2 and enzymolysis preparation,
It is characterized in that, when low-viscosity octenyl succinic anhydride modified starch products application is in field of food, the use of octenyl succinic acid anhydride
Amount ratio is the 2.8% ~ 3.0% of relative starch quality.
5. the acid heat degraded of low-viscosity octenyl succinic anhydride modified starch according to claim 1 and enzymolysis preparation, its
It is characterised by, described in step (2), ph value is 2.0 ~ 2.8；The described acidolysis reaction time is 2.0 ~ 4.0 hours.
6. the acid heat degraded of low-viscosity octenyl succinic anhydride modified starch according to claim 1 and enzymolysis preparation, its
It is characterised by, described in step (2), ph value is 2.0 ~ 2.4；The described acidolysis reaction time is 3.5 ~ 4.0 hours.
7. the acid heat degraded of low-viscosity octenyl succinic anhydride modified starch according to claim 1 and enzymolysis preparation, its
It is characterised by, enzymolysis debranching enzyme used is pullulanase, believes promozyme d2 or Jie Neng section optimax l- including Novi
1000.
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| CN109355332B (en) * | 2018-11-01 | 2021-06-08 | 西南大学 | Method for preparing low-viscosity octenyl succinic acid konjac glucomannan ester by using beta-mannase and application |
| CN110003349A (en) * | 2019-04-04 | 2019-07-12 | 北京工商大学 | A kind of preparation method of ocentyl succinic dextrin ester |
| CN111035015B (en) * | 2019-12-27 | 2023-09-05 | 浙江新和成股份有限公司 | Non-water-soluble fat-soluble nutrient microcapsule and preparation method thereof |
| CN112262884A (en) * | 2020-10-22 | 2021-01-26 | 甘肃世邦星达生物科技有限公司 | Fruit and vegetable coating agent |
| CN112741247B (en) * | 2020-12-28 | 2023-05-05 | 浙江新和成股份有限公司 | Starch octenyl succinate and preparation method and application thereof |
| CN113024897B (en) * | 2021-03-10 | 2022-07-08 | 杭州纸友科技有限公司 | Preparation method of high-strength TPS starch for degradable material |
| CN113402623B (en) * | 2021-04-20 | 2022-03-29 | 佛山市南海华昊华丰淀粉有限公司 | Macromolecular starch-based emulsifier and preparation method and application thereof |
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