CN103755819A - Microwave-assisted method for synthesis of oxidized corn starch from composite oxidant and composition - Google Patents
Microwave-assisted method for synthesis of oxidized corn starch from composite oxidant and composition Download PDFInfo
- Publication number
- CN103755819A CN103755819A CN201310697319.XA CN201310697319A CN103755819A CN 103755819 A CN103755819 A CN 103755819A CN 201310697319 A CN201310697319 A CN 201310697319A CN 103755819 A CN103755819 A CN 103755819A
- Authority
- CN
- China
- Prior art keywords
- starch
- microwave
- composite oxidant
- value
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention relates to a microwave-assisted method for synthesis of oxidized corn starch from a composite oxidant and a composition. The method includes the steps of: preparing corn starch into a starch emulsion, using hydrochloric acid to adjust the pH value to a set value; then transferring the starch emulsion into a three-neck flask, adding an FeSO4 catalyst, and slowly adding the composite oxidant dropwise under a constant pressure to undergo constant temperature reaction under microwave irradiation, then adding a sodium sulfite aqueous solution to terminate reaction; conducting washing with distilled water and ultra-pure water in order several times, and carrying out suction filtration after each washing, subjecting the filtrate to detection by KSCN, HNO3, BaCl2 and AgNO3 in order until the system is free of Fe<2+>, SO3<2->, SO4<2-> and Cl<->; and carrying out pressure reduced drying and crushing. The method is employed to synthesize the oxidized corn starch, by means of microwave-assisted synthesis, the shortest reaction time can be 21min, the needed starch emulsion has a higher concentration, and less wastewater is generated.
Description
Technical field
The present invention relates to a kind of synthetic method and synthetics of oxidised maize starch, particularly method and the synthetics of the synthetic oxidised maize starch of a kind of microwave-assisted composite oxidant.
Background technology
Starch is most important carbohydrate in human diet, is also the main source of needed by human body energy.But due to ative starch, to have cold water insoluble, the poor heat stability of starch paste, anti-shear performance is poor, and cooling rear easy dehydration, the shortcoming such as aging and film-forming properties is poor, lack water tolerance and emulsifying capacity is poor, therefore can not farthest meet the requirement of each field to starch property.The synthetic great majority of Sumstar 190 are under alkaline condition at present, and adopt single-oxidizer more.This method reaction system viscosity is large, stirs difficulty, and reaction mass should not mix, and reaction effect is poor.Therefore, how to provide the synthetic method that a kind of reaction system viscosity is little, stir the oxidised maize starch light, reaction mass easily mixes, reaction effect is good, just become the problem of worth solution.
Summary of the invention
In order to address the above problem, the present invention proposes the technical scheme of the method for the synthetic oxidised maize starch of a kind of microwave-assisted composite oxidant.The present invention is achieved through the following technical solutions.
Method and the synthetics of the synthetic oxidised maize starch of microwave-assisted composite oxidant of the present invention comprise the following steps: W-Gum is mixed with to starch emulsion, uses salt acid for adjusting pH value to set(ting)value; Proceed in there-necked flask, add FeSO
4catalyzer, and constant voltage slowly drips composite oxidant, adds sodium sulfite aqueous solution termination reaction under microwave radiation after isothermal reaction; With distilled water, ultrapure water washing, wash rear suction filtration successively, after washing for several times, filtrate is used KSCN, HNO successively at every turn
3, BaCl
2, AgNO
3detect, until in system without Fe
2+, SO
3 2-, SO
4 2-, Cl
-till; Decompression drying, pulverizes.
The present invention can also further improve by the following technical programs: preferred, the concentration of described starch milk is 35%～45%; The set(ting)value of described pH value is 3.0～5.0; The temperature setting of described isothermal reaction is set to 45 ℃～55 ℃, and the reaction times is 15min～30min; Described FeSO
4the massfraction of catalyzer is 0.2%～0.4%, and the massfraction of described composite oxidant is 6%～10%; Described sodium sulfite aqueous solution is the sodium sulfite aqueous solution that 8mL～15mL massfraction is 10%; The temperature of described decompression drying step is 55 ℃.
Further preferred, the concentration of described starch milk is 45%; The set(ting)value of described pH value is 4; The temperature setting of described isothermal reaction is set to 55 ℃, and the reaction times is 21min; Described FeSO
4the massfraction of catalyzer is 0.3%, and the massfraction of described composite oxidant is 8%.
Further preferred, the power of described microwave radiation is 400W.
It is a kind of by the synthetic oxidised maize starch of above-mentioned method that the present invention also provides.Oxidised maize starch of the present invention, is white powder, and water content is 8.57%; Acidity is 4.78mL; Oxidisability is 0.140%; The transmittance of sticking with paste is 49.0%; The bleed rate of sticking with paste is 51.3%.Gelatinization starting temperature is 84.9 ℃, and the highest gelatinization point is 91.6 ℃, and limiting viscosity is 0.04128Pas, and elasticity is greater than viscosity.
Compared with prior art, the present invention has following beneficial effect:
(1) method of the synthetic oxidised maize starch of microwave-assisted composite oxidant of the present invention, the microwave assisted synthesizing method reaction times can foreshorten to 21mi n; The concentration of its required starch milk is larger, and waste water is few.
(2) oxidised maize starch of the present invention is compared with former W-Gum, and moisture content reduction, acidity, solubleness and turgidity increase; The transparency of sticking with paste and freeze-thaw stability reduce, and the heavy property of anti-freezing raises; Gelatinization point raises, and visco-elasticity and plasticity are better.
Accompanying drawing explanation
Fig. 1 is the starch granules structure iron of the oxidised maize starch of the present invention of scanning electronic microscope demonstration.
As seen from the figure, median size 52.86 μ m; X-ray diffraction determines that it is A N-type waferN; Gelatinization starting temperature is 84.9 ℃, and the highest gelatinization point is 91.6 ℃, and limiting viscosity is 0.04128Pas, and elasticity is greater than viscosity; Infrared spectrum is at 1600cm
-1and 1400cm
-1near have the characteristic absorbance of carboxyl, C-O-C (1200-1000cm
-1) locate intensity of absorption bands and weaken, there is Partial digestion in starch molecule.
Embodiment
Measurement index using carboxyl-content as oxidisability, with starch concentration, temperature of reaction, the synthesize/power of abstraction instrument of microwave catalysis, catalyst quality mark, composite oxidant massfraction, pH value of reaction system, reaction times seven factors, carry out single factor experiment, find that starch concentration, composite oxidant massfraction, catalyst quality mark, reaction times are the principal element that affects oxidisability, in conjunction with the scope of four factor impacts, designed the synthesis technique that carries out optimization of orthogonal test.
Below in conjunction with specific embodiment, the method for the synthetic oxidised maize starch of microwave-assisted composite oxidant of the present invention is described in further detail.
Embodiment mono-:
The method of the synthetic oxidised maize starch of this routine microwave-assisted composite oxidant comprises the following steps:
A, W-Gum is mixed with to starch emulsion, the concentration of starch milk is 35%;
B, regulate the pH value of reaction system with hydrochloric acid, pH value is 3.0～5.0;
C, will proceed in there-necked flask through the starch emulsion of step a and b, adding massfraction is 0.2% FeSO
4catalyzer, and constant voltage slowly drips composite oxidant 6%;
D, by the isothermal reaction 15min under microwave radiation of the starch emulsion through above-mentioned reaction, temperature of reaction is set to 45 ℃～55 ℃; Add sodium sulfite aqueous solution 8mL～15mL termination reaction of 10%;
E, by through the Sumstar 190 emulsion of steps d successively with distilled water, ultrapure water washing, suction filtration after each washing, after washing for several times, filtrate is used KSCN, HNO successively
3, BaCl
2, AgNO
3detect, until in system without Fe
2+, SO
3 2-, SO
4 2-, Cl
-till, 55 ℃ of decompression dryings of product, Universalpulverizer are pulverized, and obtain oxidised maize starch.
Embodiment bis-:
The method of the synthetic oxidised maize starch of this routine microwave-assisted composite oxidant comprises the following steps:
A, W-Gum is mixed with to starch emulsion, the concentration of starch milk is 40%;
B, regulate the pH value of reaction system with hydrochloric acid, pH value is 3.0～5.0.
C, the starch emulsion through step a and b is proceeded in there-necked flask, add FeSO
4catalyzer 0.3%, and constant voltage slowly drips composite oxidant 8%.
D, by the isothermal reaction 18min under microwave radiation of the starch emulsion through above-mentioned reaction, temperature of reaction is set to 45 ℃～55 ℃; Add sodium sulfite aqueous solution 8mL～15mL termination reaction of 10%;
E, by through the Sumstar 190 emulsion of steps d successively with distilled water, ultrapure water washing, suction filtration after each washing, after washing for several times, filtrate is used KSCN, HNO successively
3, BaCl
2, AgNO
3detect, until in system without Fe
2+, SO
3 2-, SO
4 2-, Cl
-till, 55 ℃ of decompression dryings of product, Universalpulverizer are pulverized, and obtain oxidised maize starch.
Embodiment tri-:
The method of the synthetic oxidised maize starch of this routine microwave-assisted composite oxidant comprises the following steps:
A, W-Gum is mixed with to starch emulsion, the concentration of starch milk is 45%;
B, regulate the pH value of reaction system with hydrochloric acid, pH value is 3.0～5.0;
C, will proceed in there-necked flask through the starch emulsion of step a and b, adding massfraction is 0.4% FeSO
4catalyzer, and constant voltage slowly drips composite oxidant 10%;
D, by the isothermal reaction 21min under microwave radiation of the starch emulsion through above-mentioned reaction, temperature of reaction is set to 45 ℃～55 ℃; Add sodium sulfite aqueous solution 8mL～15mL termination reaction of 10%;
E, by the Sumstar 190 emulsion in steps d successively with the washing of distilled water, ultrapure water, suction filtration after each washing, after washing for several times, filtrate is used KSCN, HNO successively
3, BaCl
2, AgNO
3detect, until in system without Fe
2+, SO
3 2-, SO
4 2-, Cl
-till, 55 ℃ of decompression dryings of product, Universalpulverizer are pulverized, and obtain oxidised maize starch.
The above embodiments have provided concrete experimental data, and its data are as shown in the table:
Embodiment is the method steps of the concrete preparation of Optimization Technology of the present invention, and the raw material of each embodiment and consumption are in Table 1 and table 2.
Table 1 orthogonal test factor and level
Table 2 orthogonal experiments and analysis
By table 2, can obtain optimised process is A
3b
2c
2d
3, i.e. starch concentration 45%, composite oxidant massfraction 8%, catalyst quality mark 0.3%, reaction times 21min.It is 0.140% that proof test obtains its oxidisability.
Method steps and parameter thereof in the concrete preparation process of optimised process: W-Gum is mixed with to 45% starch emulsion, regulates pH=4.00 with hydrochloric acid, proceed in there-necked flask, add 0.3%FeSO simultaneously
4catalyzer, and constant voltage slowly drips 8% composite oxidant, at 55 ℃ of microwave 400W and temperature of reaction, react after 21min, adding massfraction is 10% sodium sulfite aqueous solution termination reaction, suction filtration, product is successively with distilled water, ultrapure water washing, suction filtration after each washing, after washing for several times, filtrate is used KSCN, HNO successively
3, BaCl
2, AgNO
3detect, until in system without Fe
2+, SO
3 2-, SO
4 2-, Cl
-till, 55 ℃ of decompression dryings of product, Universalpulverizer are pulverized, and obtain oxidised maize starch.
The above embodiments be only for clearly illustrate that the present invention does for example; it is not the restriction that the specific embodiment of the invention is done; to those skilled in the art; on basis of the present invention, the thinkable various conversion of institute are all within invention which is intended to be protected, here without also giving exhaustive to all embodiments of the present invention.
Claims (5)
1. a method for the synthetic oxidised maize starch of microwave-assisted composite oxidant, is characterized in that, comprises the following steps: W-Gum is mixed with to starch emulsion, uses salt acid for adjusting pH value to set(ting)value; Proceed in there-necked flask, add FeSO
4catalyzer, and constant voltage slowly drips composite oxidant, adds sodium sulfite aqueous solution termination reaction under microwave radiation after isothermal reaction; With distilled water, ultrapure water washing, wash rear suction filtration successively, after washing for several times, filtrate is used KSCN, HNO successively at every turn
3, BaCl
2, A
gnO
3detect, until in system without Fe
2+, SO
3 2-, SO
4 2-, Cl
-till; Decompression drying, pulverizes.
2. according to the method for the synthetic oxidised maize starch of microwave-assisted composite oxidant claimed in claim 1, it is characterized in that: the concentration of described starch milk is 35%～45%; The set(ting)value of described pH value is 3.0～5.0; The temperature setting of described isothermal reaction is set to 45 ℃～55 ℃, and the reaction times is 15min～30min; Described FeSO
4the massfraction of catalyzer is 0.2%～0.4%, and the massfraction of described composite oxidant is 6%～10%; Described sodium sulfite aqueous solution is the sodium sulfite aqueous solution that 8mL～15mL massfraction is 10%; The temperature of described decompression drying step is 55 ℃.
3. according to the method for the synthetic oxidised maize starch of microwave-assisted composite oxidant claimed in claim 2, it is characterized in that: the concentration of described starch milk is 45%; The set(ting)value of described pH value is 4; The temperature setting of described isothermal reaction is set to 55 ℃, and the reaction times is 21min; Described FeSO
4the massfraction of catalyzer is 0.3%, and the massfraction of described composite oxidant is 8%.
4. according to the method for the synthetic oxidised maize starch of microwave-assisted composite oxidant claimed in claim 3, it is characterized in that: the power of described microwave radiation is 400W.
5. a method for synthetic oxidised maize starch, is characterized in that: synthetic by the method described in claim 1～4 any one.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310697319.XA CN103755819A (en) | 2013-12-19 | 2013-12-19 | Microwave-assisted method for synthesis of oxidized corn starch from composite oxidant and composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310697319.XA CN103755819A (en) | 2013-12-19 | 2013-12-19 | Microwave-assisted method for synthesis of oxidized corn starch from composite oxidant and composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103755819A true CN103755819A (en) | 2014-04-30 |
Family
ID=50523162
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310697319.XA Pending CN103755819A (en) | 2013-12-19 | 2013-12-19 | Microwave-assisted method for synthesis of oxidized corn starch from composite oxidant and composition |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103755819A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3211564A (en) * | 1961-06-13 | 1965-10-12 | Kimberly Clark Co | Continuous high temperature process for oxidized starch for coating compositions |
| CN101863996A (en) * | 2010-06-18 | 2010-10-20 | 罗代洪 | Dry method for preparing oxidized starch by microwave |
-
2013
- 2013-12-19 CN CN201310697319.XA patent/CN103755819A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3211564A (en) * | 1961-06-13 | 1965-10-12 | Kimberly Clark Co | Continuous high temperature process for oxidized starch for coating compositions |
| CN101863996A (en) * | 2010-06-18 | 2010-10-20 | 罗代洪 | Dry method for preparing oxidized starch by microwave |
Non-Patent Citations (3)
| Title |
|---|
| 吴晓红等: "《化学教学论实验》", 30 September 2013 * |
| 李向高: "《中药材加工学》", 31 January 2004 * |
| 李玉秀等: ""微波辅助复合氧化法合成氧化玉米淀粉"", 《化学与生物工程》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103551201B (en) | A kind of preparation method of copper hydroxyphosphate catalyst | |
| CN104925867B (en) | A kind of nanometer wolframic acid caesium powder body and preparation method and application | |
| CN106268900A (en) | A kind of g C3n4quantum dot sensitized AgVO3the preparation method of nano wire | |
| CN105233845A (en) | ZnFe2O4/BiOBr magnetic photocatalyst and preparation method thereof | |
| CN107285376A (en) | A kind of two-dimentional TiO2Ultrathin nanometer piece and preparation method thereof | |
| CN107235506B (en) | A kind of preparation method of nano zine oxide heterojunction structure | |
| CN102702369A (en) | Starch octenyl succinate anhydride preparation process | |
| CN105399151B (en) | A kind of preparation method of cobalt acid nickel nano material | |
| Shi et al. | Preparation and characterization of carboxymethyl starch under ultrasound‐microwave synergistic interaction | |
| Liu et al. | Sensitive pH probe developed with water-soluble fluorescent carbon dots from chocolate by one-step hydrothermal method | |
| CN102616850A (en) | Preparation method for monodisperse vanadium pentoxide solid microspheres | |
| CN103694362A (en) | Method for synthesizing oxidized corn starch by assisting composite oxidant through ultrasonic waves and synthesized substance | |
| CN105668627A (en) | Nanometer NaBi(MoO4)2 and preparation method thereof | |
| Gao et al. | Preparation of nanoparticulate TmVO4 by sol-gel method and its visible-light photocatalytic activity | |
| CN103785425A (en) | Preparation method and application of flower-like Bi2O(OH)2SO4 photocatalyst | |
| CN103755819A (en) | Microwave-assisted method for synthesis of oxidized corn starch from composite oxidant and composition | |
| CN106749924A (en) | A kind of preparation method of degradable corn core biomass water-loss reducer | |
| CN103922402B (en) | Method for preparing NH4V3O8 nanoribbon | |
| CN107416899B (en) | A kind of nano wire α-Bi2O3The preparation method of dusty material | |
| CN104449615A (en) | Organic acid chromium crosslinking agent for oil production and preparation method thereof | |
| CN103709260A (en) | Method for synthesizing oxidized corn starch using water bath temperature control composite oxidant and composition | |
| CN109794232A (en) | A kind of preparation method of the spherical visible light catalyst of zinc doping pucherite | |
| CN103657732A (en) | Preparation method of SO4<2->/TiO2-ZnO mixed crystal solid acid carrier coordination catalyst | |
| Liu et al. | Photocatalytic degradation of oxytetracycline hydrochloride pollutants in marine aquaculture wastewater under visible light | |
| CN103224565A (en) | Method for preparing carboxymethyl cellulose used in printing paste by using straws |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20140430 |