CN106279450A - A kind of preparation method of porous starch octenyl succinate anhydride - Google Patents
A kind of preparation method of porous starch octenyl succinate anhydride Download PDFInfo
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- CN106279450A CN106279450A CN201610760246.8A CN201610760246A CN106279450A CN 106279450 A CN106279450 A CN 106279450A CN 201610760246 A CN201610760246 A CN 201610760246A CN 106279450 A CN106279450 A CN 106279450A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B31/00—Preparation of derivatives of starch
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- C08B31/04—Esters of organic acids, e.g. alkenyl-succinated starch
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
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- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/04—Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
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- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
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Abstract
The invention discloses the preparation method of a kind of porous starch octenyl succinate anhydride, mainly comprise the steps that and obtain starch milk by soluble in water for starch, regulation pH, add uncooked amylum enzyme, react a period of time at a certain temperature, further regulation pH and temperature, it is slowly added to the octenyl succinic acid anhydride after dehydrated alcohol dilutes and reacts a period of time, absolute ethanol washing reactant liquor is used in reaction after terminating, collect solid content and be dried pulverizing, obtain porous starch octenyl succinate anhydride.The porous starch octenyl succinate anhydride that the present invention prepares combines the double properties of porous-starch and starch octenyl succinate anhydride, both there is good adsorptivity and inclusion, there is again good emulsibility, substantially increase the surcharge of starch, expand the range of application of starch, there is preferable promotion potential.
Description
Technical field
The present invention relates to the preparation method of a kind of porous starch octenyl succinate anhydride, belong to modified starch preparation field.
Background technology
Porous-starch has another name called micropore starch, is a kind of novel modified starch.Natural uncooked amylum after hydrolysis process, its
Particle surface forms aperture, and extends to inside granule, is the hollow particle of a kind of similar hornet's nest shape, can contain each
Kind material, in wherein, has good adsorptivity.Therefore, porous-starch is a kind of novel organic adsorption with high-tech content
Agent and embedded material, be widely used in medicine, pesticide, printing, sewage disposal, daily-use chemical industry, cosmetics and food service industry.
Uncooked amylum enzyme refers to the direct enzymolysis enzyme without gelatinized starch granule, have certain economic worth and energy-conservation far
Scape, the present invention uses uncooked amylum enzyme treated starch to obtain porous-starch, then reacts with octenyl succinic acid anhydride, obtain porous pungent
Starch alkenyl succinate ester.Porous starch octenyl succinate anhydride not only has a good adsorptivity and inclusion, and due to
Which increase the octenyl succinic acid groups with hydrophilic and oleophilic character so that it is there is the strongest emulsifying property, expand starch
Range.
Summary of the invention
The present invention provides the preparation method of a kind of porous starch octenyl succinate anhydride, acts on initially with uncooked amylum enzyme
Starch obtains porous-starch, then carries out esterification with octenyl succinic acid anhydride, obtains porous starch octenyl succinate anhydride.
Preparation method of the present invention mainly comprises the steps that
(1) enzyme digestion reaction: weigh a certain amount of starch, adds appropriate water and obtains starch milk, uses salt acid for adjusting pH, adds uncooked amylum
Enzyme, reacts a period of time at a certain temperature；
(2) esterification: in the range of the pH value of starch milk of step (1) gained being adjusted to 8.0-9.0 with NaOH, the most slowly add
Entering the octenyl succinic acid anhydride reagent through dehydrated alcohol dilution, temperature controls at 30 DEG C-50 DEG C；
(3) remove impurity is dried: reaction uses absolute ethanol washing three times after terminating, and washes away unreacted octenyl succinic acid anhydride reagent,
Dry, pulverize in vacuum drying oven after centrifuge dehydration, cross 120 mesh sieves, i.e. obtain porous starch octenyl succinate anhydride.
Wherein, the preparation method of described porous starch octenyl succinate anhydride, it is characterised in that described starch is big
One or more in rice starch, wheaten starch, tapioca, sweet potato starch, pea starch or sago starch.
The preparation method of described porous starch octenyl succinate anhydride, it is characterised in that described starch concentration exists
20%-50%。
The preparation method of described porous starch octenyl succinate anhydride, it is characterised in that described regulation starch milk pH is
3.0-6.0。
The preparation method of described porous starch octenyl succinate anhydride, it is characterised in that described uncooked amylum enzyme addition
It is that 30-100 U/g(is in terms of starch on dry basis).
The preparation method of described porous starch octenyl succinate anhydride, it is characterised in that described enzyme digestion reaction temperature is
30℃-70℃。
The preparation method of described porous starch octenyl succinate anhydride, it is characterised in that the described enzyme digestion reaction time is
1-6 h。
The preparation method of described porous starch octenyl succinate anhydride, it is characterised in that described esterification reaction temperature is
30℃-50℃。
The preparation method of described porous starch octenyl succinate anhydride, it is characterised in that described octenyl succinic acid anhydride
Addition is the 0.5%-5% of starch on dry basis.
The preparation method of described porous starch octenyl succinate anhydride, it is characterised in that described reaction time of esterification is
2-8 h。
By the present invention in that, with uncooked amylum enzyme, common starch reaction is become porous-starch, starch material surface is formed a lot
Aperture so that in follow-up esterification, reaction reagent can enter in space and react, improve reaction efficiency and
The utilization rate of reagent.The porous starch octenyl succinate anhydride obtained has good adsorptivity, inclusion and emulsibility.This
Bright simple to operate, reaction efficiency is high, and range is wide, has wide market prospect.
Detailed description of the invention
Below in conjunction with instantiation, technical scheme is described further.
The analysis method that uncooked amylum enzyme enzyme is lived
Soluble starch suspension using 2% is as substrate (the acetic acid-sodium acetate buffer solution preparation with pH is 4.6), reactant
System: 20 mL substrates, 0.5 mL enzyme liquid, reacts 60 min in 40 DEG C, adds 0.5 mL 0.1 mol/L NaOH immediately and terminate anti-
Should, compare as enzyme liquid after inactivation, reactant liquor 8000 r/min is centrifuged 5 min after terminating by reaction, and supernatant DNS method measures also
Raw sugar concentration (with glucose meter), thus converse corresponding uncooked amylum enzyme enzyme and live.Raw starch enzyme enzyme activity defines: at pH
4.6, the enzyme amount that under 40 DEG C of reaction conditions, 1 h hydrolyzes needed for 2% soluble starch suspension produces 1 mg reducing sugar is defined as one
Enzyme activity unit.
Embodiment 1
Weigh 30 g rice starchs, add appropriate water and obtain the starch milk of 20%, be 6.0 with salt acid for adjusting pH, add uncooked amylum
Enzyme 50 U/g, reacts 1 h at 30 DEG C.In the range of pH value of starch milk being adjusted to 8.0-9.0 with NaOH, it is then slowly added into through nothing
The octenyl succinic acid anhydride reagent of water-ethanol dilution, addition is the 5% of rice starch butt, and temperature controls at 50 DEG C, reacts 4
h.Reaction uses absolute ethanol washing three times after terminating, and washes away unreacted octenyl succinic acid anhydride reagent, very after centrifuge dehydration
Empty drying baker dry, pulverize, cross 120 mesh sieves, obtain porous ocentyl succinic rice starch ester.
Embodiment 2
Weigh 30 g wheaten starches, add appropriate water and obtain the starch milk of 30%, be 5.0 with salt acid for adjusting pH, add uncooked amylum
Enzyme 30 U/g, reacts 6 h at 70 DEG C.In the range of pH value of starch milk being adjusted to 8.0-9.0 with NaOH, it is then slowly added into through nothing
The octenyl succinic acid anhydride reagent of water-ethanol dilution, addition is the 0.5% of wheaten starch butt, and temperature controls at 50 DEG C, reaction
7 h.Reaction terminate after with absolute ethanol washing three times, wash away unreacted octenyl succinic acid anhydride reagent, after centrifuge dehydration
Vacuum drying oven dry, pulverize, cross 120 mesh sieves, obtain porous ocentyl succinic wheaten starch ester.
Embodiment 3
Weigh 30 g tapiocas, add appropriate water and obtain the starch milk of 40%, be 4.5 with salt acid for adjusting pH, add uncooked amylum
Enzyme 100 U/g, reacts 5 h at 40 DEG C.In the range of pH value of starch milk being adjusted to 8.0-9.0 with NaOH, be then slowly added into through
The octenyl succinic acid anhydride reagent of dehydrated alcohol dilution, addition is the 1% of tapioca butt, and temperature controls at 30 DEG C, reaction
8 h.Reaction terminate after with absolute ethanol washing three times, wash away unreacted octenyl succinic acid anhydride reagent, after centrifuge dehydration
Vacuum drying oven dry, pulverize, cross 120 mesh sieves, obtain porous tapioca starch sodium octenyl succinate.
Embodiment 4
Weigh 30 g sweet potato starchs, add appropriate water and obtain the starch milk of 45%, be 4.0 with salt acid for adjusting pH, add uncooked amylum
Enzyme 60 U/g, reacts 3 h at 50 DEG C.In the range of pH value of starch milk being adjusted to 8.0-9.0 with NaOH, it is then slowly added into through nothing
The octenyl succinic acid anhydride reagent of water-ethanol dilution, addition is the 2% of sweet potato starch butt, and temperature controls at 40 DEG C, reacts 2
h.Reaction uses absolute ethanol washing three times after terminating, and washes away unreacted octenyl succinic acid anhydride reagent, very after centrifuge dehydration
Empty drying baker dry, pulverize, cross 120 mesh sieves, obtain porous ocentyl succinic sweet potato starch ester.
Embodiment 5
Weigh 30 g pea starches, add appropriate water and obtain the starch milk of 50%, be 3.5 with salt acid for adjusting pH, add uncooked amylum
Enzyme 40 U/g, reacts 4 h at 60 DEG C.In the range of pH value of starch milk being adjusted to 8.0-9.0 with NaOH, it is then slowly added into through nothing
The octenyl succinic acid anhydride reagent of water-ethanol dilution, addition is the 3% of pea starch butt, and temperature controls at 35 DEG C, reacts 5
h.Reaction uses absolute ethanol washing three times after terminating, and washes away unreacted octenyl succinic acid anhydride reagent, very after centrifuge dehydration
Empty drying baker dry, pulverize, cross 120 mesh sieves, obtain porous ocentyl succinic pea starch ester.
Embodiment 6
Weigh 30 g sago starches, add appropriate water and obtain the starch milk of 35%, be 3.0 with salt acid for adjusting pH, add uncooked amylum
Enzyme 70 U/g, reacts 2 h at 55 DEG C.In the range of pH value of starch milk being adjusted to 8.0-9.0 with NaOH, it is then slowly added into through nothing
The octenyl succinic acid anhydride reagent of water-ethanol dilution, addition is the 4% of sago starch butt, and temperature controls at 45 DEG C, reacts 3
h.Reaction uses absolute ethanol washing three times after terminating, and washes away unreacted octenyl succinic acid anhydride reagent, very after centrifuge dehydration
Empty drying baker dry, pulverize, cross 120 mesh sieves, obtain porous ocentyl succinic sago starch ester.
Claims (10)
1. the preparation method of a porous starch octenyl succinate anhydride, it is characterised in that mainly comprise the steps that starch
The starch milk that obtains soluble in water, regulates pH, adds uncooked amylum enzyme, reacts a period of time at a certain temperature, regulate pH further
And temperature, it is slowly added to the octenyl succinic acid anhydride after dehydrated alcohol dilutes and reacts a period of time, react after terminating with anhydrous
Washing with alcohol reactant liquor, collects solid content and is dried pulverizing, obtain porous starch octenyl succinate anhydride.
The preparation method of porous starch octenyl succinate anhydride the most according to claim 1, it is characterised in that described shallow lake
Powder is one or more in rice starch, wheaten starch, tapioca, sweet potato starch, pea starch or sago starch.
The preparation method of porous starch octenyl succinate anhydride the most according to claim 1, it is characterised in that described shallow lake
Powder breast concentration is at 20%-50%.
The preparation method of porous starch octenyl succinate anhydride the most according to claim 1, it is characterised in that described tune
Joint starch milk pH is 3.0-6.0.
The preparation method of porous starch octenyl succinate anhydride the most according to claim 1, it is characterised in that described life
Amylase addition is that 30-100 U/g(is in terms of starch on dry basis).
The preparation method of porous starch octenyl succinate anhydride the most according to claim 1, it is characterised in that described enzyme
Solving reaction temperature is 30 DEG C-70 DEG C.
The preparation method of porous starch octenyl succinate anhydride the most according to claim 1, it is characterised in that described enzyme
The solution response time is 1-6 h.
The preparation method of porous starch octenyl succinate anhydride the most according to claim 1, it is characterised in that described ester
Changing reaction temperature is 30 DEG C-50 DEG C.
The preparation method of porous starch octenyl succinate anhydride the most according to claim 1, it is characterised in that described is pungent
Alkenyl succinic anhydride addition is the 0.5%-5% of starch on dry basis.
The preparation method of porous starch octenyl succinate anhydride the most according to claim 1, it is characterised in that described ester
The change response time is 2-8 h.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106967177A (en) * | 2017-04-20 | 2017-07-21 | 南昌大学 | Ocentyl succinic wheaten starch ester prepared by a kind of vacuum infrared collaboration processing |
| CN106977612A (en) * | 2017-04-20 | 2017-07-25 | 南昌大学 | A kind of porous tapioca starch sodium octenyl succinate |
| CN107011450A (en) * | 2017-04-20 | 2017-08-04 | 南昌大学 | A kind of production method of high-purity octenylsuccinate potato starch ester |
| CN107098983A (en) * | 2017-04-20 | 2017-08-29 | 南昌大学 | A kind of production method of high added value ocentyl succinic Lotus Root Starch ester |
| CN107141362A (en) * | 2017-04-20 | 2017-09-08 | 南昌大学 | Ocentyl succinic cornstarch ester prepared by a kind of synchronous concentration reaction method |
| CN107141361A (en) * | 2017-04-20 | 2017-09-08 | 南昌大学 | A kind of production method of high esterification ocentyl succinic water caltrop starch ester |
| CN107573534A (en) * | 2017-09-27 | 2018-01-12 | 山东神州翔宇科技集团有限公司 | A kind of preparation method of the porous-starch with emulsibility |
| CN113214532A (en) * | 2021-06-25 | 2021-08-06 | 江南大学 | Preparation method of high-load esterified porous starch-based material |
| CN114805618A (en) * | 2022-05-12 | 2022-07-29 | 甘肃农业大学 | Preparation method of 3-hydroxycinnamic acid porous starch ester with oxidation resistance |
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| CN1504485A (en) * | 2002-11-29 | 2004-06-16 | 四平市帝达变性淀粉有限公司 | Starch alkenyl succinic acid ester, preparing process and uses thereof |
| CN1546529A (en) * | 2003-12-01 | 2004-11-17 | 江南大学 | Method for producing porous starch and its application |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106967177A (en) * | 2017-04-20 | 2017-07-21 | 南昌大学 | Ocentyl succinic wheaten starch ester prepared by a kind of vacuum infrared collaboration processing |
| CN106977612A (en) * | 2017-04-20 | 2017-07-25 | 南昌大学 | A kind of porous tapioca starch sodium octenyl succinate |
| CN107011450A (en) * | 2017-04-20 | 2017-08-04 | 南昌大学 | A kind of production method of high-purity octenylsuccinate potato starch ester |
| CN107098983A (en) * | 2017-04-20 | 2017-08-29 | 南昌大学 | A kind of production method of high added value ocentyl succinic Lotus Root Starch ester |
| CN107141362A (en) * | 2017-04-20 | 2017-09-08 | 南昌大学 | Ocentyl succinic cornstarch ester prepared by a kind of synchronous concentration reaction method |
| CN107141361A (en) * | 2017-04-20 | 2017-09-08 | 南昌大学 | A kind of production method of high esterification ocentyl succinic water caltrop starch ester |
| CN107573534A (en) * | 2017-09-27 | 2018-01-12 | 山东神州翔宇科技集团有限公司 | A kind of preparation method of the porous-starch with emulsibility |
| CN113214532A (en) * | 2021-06-25 | 2021-08-06 | 江南大学 | Preparation method of high-load esterified porous starch-based material |
| CN114805618A (en) * | 2022-05-12 | 2022-07-29 | 甘肃农业大学 | Preparation method of 3-hydroxycinnamic acid porous starch ester with oxidation resistance |
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