CN103833862A - Oxidized glutinous rice starch as well as preparation method and application thereof - Google Patents
Oxidized glutinous rice starch as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of modified starch, and particularly discloses oxidized glutinous rice starch as well as a preparation method and an application thereof. The preparation method disclosed by the invention comprises the steps of mechanical activation, milk adjustment, catalyzing, oxidation, termination reaction and product purification. The oxidized glutinous rice starch obtained by using the method can be applied to surface sizing agents, coating adhesive, wet end additives, corrugated board adhesives and the like in papermaking industries. The preparation method disclosed by the invention is reasonable in process, short in preparation cycle and high in product yield; and compared with native starch, the prepared oxidized glutinous rice starch has the advantages of light color, low gelatinization temperature, good mobility, low paste viscosity, high stability, high transparency, good film-forming property, strong adhesive force and the like.
Description
Technical field
The invention belongs to modified starch field, be specifically related to a kind of oxidation glutinous rice starch and preparation method thereof and application.
Background technology
Because native starch kind is limited, and exist cold water poor heat stability, anti-shear performance insoluble, that stick with paste low, cooling rear easy dehydration, easily aging, film-forming properties is poor and lack the shortcoming such as water-resistant capacity, in modern industry, extensively adopt new technology simultaneously, being of limited application in the situation such as new installation, new technology, growing modern crafts and the needs of equipment can not be met, therefore, need to carry out denaturing treatment to starch.Starch denaturalization is exactly to adopt physics, chemistry or biological means to change the character of native starch, cut off, reset, be oxidized or introduce substituting group by molecule in starch molecule and can make the starch derivative that character changes, it is modified starch, in order to increase its performance or to introduce new features, defect while overcoming application, the needs of producing to adapt to modern industry.
Mechanical activation starch belongs to physically denatured starch, refers to starch effect due to mechanical forces such as friction, collision, impact, shearings in mechanical activation process, and its crystalline texture is damaged, and degree of crystallinity reduces, and is finally transformed into non-crystalline state by polycrystalline state.Under the effect of mechanical force, the crystalline texture of starch has been subject to destruction, and the double-spiral structure of the starch that dissociated, has greatly promoted the combination of water molecules and starch molecule radical.The granular of starch is mainly to carry out wet ball-milling taking organic solvents such as ethanol as ball milling liquid, make the normal-temperature dissolution degree of starch reach more than 80% and higher reactive behavior, and milling time needs more than 50 hours.And the preparation method of mechanical activation starch uses dry method, through the ball milling activation of short period to starch, just can make it have good cold-water solution performance and higher chemical reactivity, can strengthen from inside the chemical reaction process of starch.
Sumstar 190 is by the hydroxyl in oxygenant Sumstar 190 molecule, converts it into carbonyl and carboxyl, destroys the glycosidic link in partial starch molecule simultaneously, causes a certain amount of degraded of molecule.It is a kind of extremely important and at industrial application treated starch very widely.Sumstar 190 is compared with ative starch in nature, and Sumstar 190 has the advantages such as look shallow, gelatinization point is low, good fluidity, reaction control is low and stability is high, transparency is high, film forming properties is good, adhesive power is strong.
Sumstar 190 can adopt dry method or wet method manufacture to form.Abroad to the research of modified starch early, China aspect modified starch further investigation with also there is certain gap abroad.External in recent years to the research of Sumstar 190 mainly the selecting of oxygenant and catalyzer, to improve reaction efficiency and to reduce production costs.Synthetic Sumstar 190 can be used the oxidant production such as clorox, potassium permanganate, potassium bichromate.In industrial production, adopting at present clorox is that the wet process technique of oxygenant is more, but that this technique produces waste water is many, contaminate environment.If employing hydrogen peroxide is oxygenant, hydrogen peroxide is finally decomposed into water, can not affect environment, is a comparatively desirable friendly process.
Glutinous rice, as one of main food of southern each province, is the important source material of producing Chinese traditional food.Glutinous rice starch is used for processing as food such as ice cream, meat soup juice and oyster sauce seasonings as food thickener.Glutinous rice starch is a kind of full amylopectin, its polymerization degree is more than 1,000,000, molecular weight is more than 200,000,000, for maximum in natural high moleculer eompound, it is a kind of three-dimensional polymer, side chain lengths approximately 20～25 AGUs, fork position alpha-1, the glucose unit quantity that 6 glycosidic links connect is approximately 5% of glucose unit sum.Glutinous rice starch molecule, because the relation of a fork structure is difficult for retrogradation occurs, weakens retrogradation.Due to the special chemical structure of glutinous rice starch, the most representative, but the research of it being carried out to sex change is both at home and abroad less, and therefore in order to improve its application performance, broaden application scope, is necessary glutinous rice starch to carry out study on the modification.
The raw material of at present common manufacture Sumstar 190 has W-Gum, tapioca (flour), wheat starch, yam starch and waxy corn starch etc., prepares Sumstar 190 be not seen in report taking glutinous rice starch as raw material.
Summary of the invention
In order to overcome prior art deficiency, primary and foremost purpose of the present invention is to provide a kind of preparation method who is oxidized glutinous rice starch, the present invention is first taking glutinous rice starch as raw material, the method preparation oxidation glutinous rice starch that adopts mechanical activation to be combined with oxidation modification, expand the use range of glutinous rice starch, enriched the kind of Sumstar 190;
The oxidation glutinous rice starch that provides above-mentioned preparation method to make is provided.
A further object of the present invention is to provide the application of above-mentioned oxidation glutinous rice starch.
Object of the present invention is achieved through the following technical solutions:
A preparation method who is oxidized glutinous rice starch, comprises the steps:
(1) mechanical activation: with ball mill by glutinous rice starch activation 50～60h;
(2) adjust breast: get the glutinous rice starch after step (1) activation, being mixed with massfraction with deionized water is 35%～40% starch milk;
(3) catalysis: add catalyzer in the described starch milk of step (2), be uniformly mixed, then with alkaline solution adjusting pH to 8～10, obtain the starch milk after catalysis;
(4) oxidation: add oxygenant in the starch milk after the described catalysis of step (3), isothermal reaction obtains the starch emulsion after oxidation;
(5) termination reaction: the starch emulsion pH value after the described oxidation of step (4) is neutralized to 6 with hydrochloric acid soln, then drips reductive agent termination reaction, obtain being oxidized the thick product of glutinous rice starch;
(6) product purifies: by the thick product of described oxidation glutinous rice starch after filtration, washing, dry, pulverize, screening, obtain being oxidized glutinous rice starch.
Preferably, the described activation condition of step (1) is: under room temperature condition, activate, ball mill revolution speed is 150r/min, and rotational velocity is 300r/min; The internal diameter of ball mill is 100mm, and volume is 500ml; In ball mill, the diameter of abrading-ball is 50mm, and Material quality of grinding balls is agate;
Preferably, the described catalyzer of step (3) is the cobalt chloride solution of massfraction 2%～4% or the ferrous sulfate aqueous solution of massfraction 2%～4%; The described alkaline solution of step (3) is that massfraction is the potassium hydroxide solution that 3%～5% sodium hydroxide solution or massfraction are 3%～5%.
Preferably, the consumption of the described catalyzer of step (3) is 1%～2.5% of glutinous rice starch quality after the described activation of step (2).
Preferably, the described oxygenant of step (4) is that massfraction is 30%～40% hydrogen peroxide; The described reductive agent of step (5) is that massfraction is the potassium sulfite solution that 5% sodium sulfite solution or massfraction are 5%; The concentration of the described hydrochloric acid soln of step (5) is 0.1mol/L.
Preferably, the consumption of the described oxygenant of step (4) is 1.5%～3% of glutinous rice starch quality after the described activation of step (2);
Preferably, the described isothermal reaction of step (4) is to react 1.5～3h under 40～45 DEG C of conditions of constant temperature;
Preferably, to continue to drop to the pH value of the starch emulsion after described oxidation be till 7～7.5 o'clock to the described interpolation reductive agent of step (5).
A kind of oxidation glutinous rice starch preparing according to above-mentioned preparation method.
The application of above-mentioned oxidation glutinous rice starch in paper industry; Preferred version is: the application of above-mentioned oxidation glutinous rice starch in preparation table surface sizing agent, coating binder, wet end additive or adhesive for corrugated paperboard.
Principle of the present invention:
By the ball milling activation through the short period to glutinous rice starch, make glutinous rice starch there is good cold-water solution performance and higher chemical reactivity, and strengthen the chemical reaction process of glutinous rice starch from inside.The reactive behavior of the glutinous rice starch after activation is improved, thereby the reaction efficiency of itself and oxygenant is further promoted, and has saved time and the cost of oxidation reaction process.
The present invention has following advantage and effect with respect to prior art:
(1) preparation technology of oxidation glutinous rice starch of the present invention is reasonable, through mechanical activation, adjust breast, catalysis, oxidation, termination reaction, filtration, washing, be dried, the accurate control of pulverizing, sieving technology system, make common glutinous rice starch there is Sumstar 190 characteristic, reduced gelatinization point and the retrogradation of starch simultaneously.
(2) the present invention adopts and first carries out mechanical activation processing, has greatly improved the speed of reaction, has strengthened the chemical reactivity of starch.
(3) the invention provides the preparation method who is oxidized glutinous rice starch, can make full use of southern superior resources glutinous rice starch, be conducive to the deep processing increment of southern area renewable resources.
(4) product oxidation glutinous rice starch of the present invention and preparation method thereof has vast potential for future development, and its further popularization also can, for the food enterprises reduces production costs, be increased economic efficiency and play promoter action.
Brief description of the drawings
Fig. 1 is the infrared spectrogram of oxidation glutinous rice starch.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited to this.
This patent balls grinding machine originates from Nanjing and speeds along development in science and technology company limited, PM series planetary ball mill.
Embodiment 1
A kind of oxidation glutinous rice starch, its preparation method is as follows:
(1) mechanical activation: be 150r/min with ball mill at ball milling revolution speed under room temperature, glutinous rice starch is activated 50h by the condition that rotational velocity is 300r/min; The internal diameter of ball mill is 100mm, and volume is 500ml; In ball mill, the diameter of abrading-ball is 50mm, and Material quality of grinding balls is agate;
(2) adjust breast: accurately take the glutinous rice starch after 30g activation, being mixed with massfraction with deionized water is 35% starch milk;
(3) catalysis: while stirring to the cobalt chloride solution that adds 6ml massfraction 2% in starch milk, starch milk pH is adjusted to 8 with the sodium hydroxide solution of massfraction 3%;
(4) oxidation: be 30% hydrogen peroxide to slowly adding 1ml massfraction in the starch milk after step (3) catalysis, 40 DEG C of reaction 1.0h of constant temperature, obtain the starch emulsion after oxidation;
(5) termination reaction: the pH value of starch emulsion after oxidation is neutralized to 6 with 0.1mol/L hydrochloric acid, continuing dropping massfraction is that 5% sodium sulfite aqueous solution to pH value of solution is 7.0 o'clock reaction terminatings, obtains being oxidized the thick product of glutinous rice starch;
(6) product purifies: will be oxidized the thick product of glutinous rice starch after filtration, washing, dry, pulverize, screening, obtain product and be oxidized glutinous rice starch;
(7) measure the carboxyl-content that is oxidized glutinous rice starch, the content of measuring carboxyl is 0.75.
Product oxidation glutinous rice starch is carried out to Infrared spectroscopy, and infrared spectrogram as shown in Figure 1.As can be seen from Figure 1, remove at 3435.9cm
-1, 2930.8cm
-1, 1424.0cm
-1, 1338.8cm
-1, 1159.8cm
-1, 1081.3cm
-1, 860.8cm
-1, 756.0cm
-1, 576.2cm
-1occurring beyond the charateristic avsorption band of starch at place, also there is the charateristic avsorption band of stronger carboxylate salt-COO-in oxidation glutinous rice starch at 1644.0cm-1; Illustrate on glutinous rice starch molecule and introduced carboxylic group, complete modification.
Embodiment 2
A kind of oxidation glutinous rice starch, its preparation method is as follows:
(1) mechanical activation: with ball mill be 150r/min at ball milling revolution speed, rotational velocity is, under 300r/min condition, glutinous rice starch is activated to 55h;
(2) adjust breast: accurately take the glutinous rice starch after 30g activation, being mixed with massfraction with deionized water is 35% starch milk;
(3) catalysis: while stirring to the cobalt chloride solution that adds 9ml massfraction 3% in starch milk, starch milk pH is adjusted to 8 with the sodium hydroxide solution of massfraction 5%;
(4) oxidation: be 40% hydrogen peroxide to slowly adding 1.2ml massfraction in the starch milk after step (3) catalysis, 40 DEG C of reaction 1.5h of constant temperature, obtain the starch emulsion after oxidation;
(5) termination reaction: the pH value of starch emulsion after oxidation is neutralized to 6 with 0.1mol/L hydrochloric acid, continuing dropping massfraction is that 5% sodium sulfite aqueous solution to pH value of solution is 7.2 o'clock reaction terminatings, obtains being oxidized the thick product of glutinous rice starch;
(6) product purifies: will be oxidized the thick product of glutinous rice starch after filtration, washing, dry, pulverize, screening, obtain product and be oxidized glutinous rice starch;
(7) measure the carboxyl-content that is oxidized glutinous rice starch, the content of measuring carboxyl is 0.88.
Embodiment 3
A kind of oxidation glutinous rice starch, its preparation method is as follows:
(1) mechanical activation: with ball mill be 150r/min at ball milling revolution speed, rotational velocity is, under 300r/min condition, glutinous rice starch is activated to 60h;
(2) adjust breast: accurately take the glutinous rice starch after 30g activation, being mixed with massfraction with deionized water is 35% starch milk;
(3) catalysis: while stirring to the copperas solution that adds 9ml massfraction 4% in starch milk, starch milk pH is adjusted to 10 with the potassium hydroxide solution of massfraction 3%;
(4) oxidation: be 30% hydrogen peroxide to slowly adding 1.5ml massfraction in the starch milk after step (3) catalysis, 45 DEG C of reaction 2h of constant temperature, obtain the starch emulsion after oxidation;
(5) termination reaction: the pH value of starch emulsion after oxidation is neutralized to 6 with 0.1mol/L hydrochloric acid, continuing dropping massfraction is that 5% sodium sulfite aqueous solution to pH value of solution is 7.5 o'clock reaction terminatings, obtains being oxidized the thick product of glutinous rice starch;
(6) product purifies: will be oxidized the thick product of glutinous rice starch after filtration, washing, dry, pulverize, screening, obtain product and be oxidized glutinous rice starch;
Measure the carboxyl-content of oxidation glutinous rice starch, the content of measuring carboxyl is 0.81.
Embodiment 4
A kind of oxidation glutinous rice starch, its preparation method is as follows:
(1) mechanical activation: with ball mill be 150r/min at ball milling revolution speed, rotational velocity is, under 300r/min condition, glutinous rice starch is activated to 60h;
(2) adjust breast: accurately take the glutinous rice starch after 30g activation, being mixed with massfraction with deionized water is 40% starch milk;
(3) catalysis: while stirring to the copperas solution that adds 8ml massfraction 4% in starch milk, starch milk pH is adjusted to 10 with the potassium hydroxide solution of massfraction 3%;
(4) oxidation: be 40% hydrogen peroxide to slowly adding 1.2ml massfraction in the starch milk after step (3) catalysis, 45 DEG C of reaction 1.5h of constant temperature, obtain the starch emulsion after oxidation;
(5) termination reaction: the pH value of starch emulsion after oxidation is neutralized to 6 with 0.1mol/L hydrochloric acid, continuing dropping massfraction is that 5% sodium sulfite aqueous solution to pH value of solution is 7.0 o'clock reaction terminatings, obtains being oxidized the thick product of glutinous rice starch;
(6) product purifies: will be oxidized the thick product of glutinous rice starch after filtration, washing, dry, pulverize, screening, obtain product and be oxidized glutinous rice starch;
Measure the carboxyl-content of oxidation glutinous rice starch, the content of measuring carboxyl is 0.92.
Comparative example 1
A kind of oxidation glutinous rice starch, its preparation method is as follows:
(1) adjust breast: accurately take 30g glutinous rice starch, being mixed with massfraction with deionized water is 40% starch milk;
(2) catalysis: while stirring to the copperas solution that adds 8ml massfraction 4% in starch milk, starch milk pH is adjusted to 10 with the potassium hydroxide solution of massfraction 3%;
(3) oxidation: be 40% hydrogen peroxide to slowly adding 1.2ml massfraction in the starch milk after step (3) catalysis, 45 DEG C of reaction 3h of constant temperature, obtain the starch emulsion after oxidation;
(4) termination reaction: the pH value of starch emulsion after oxidation is neutralized to 6 with 0.1mol/L hydrochloric acid, continuing dropping massfraction is that 5% sodium sulfite aqueous solution to pH value of solution is 7.5 o'clock reaction terminatings, obtains being oxidized the thick product of glutinous rice starch;
(5) product purifies: will be oxidized the thick product of glutinous rice starch after filtration, washing, dry, pulverize, screening, obtain product and be oxidized glutinous rice starch;
Measure the carboxyl-content of oxidation glutinous rice starch, the content of measuring carboxyl is 0.63.
In conjunction with the embodiments and comparative example, can find out that the carboxyl-content of the oxidation glutinous rice starch of not preparing through mechanical activation is lower than the carboxyl-content of the oxidation glutinous rice starch of preparation method's gained of the present invention.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (10)
1. be oxidized a preparation method for glutinous rice starch, it is characterized in that comprising the steps:
(1) mechanical activation: with ball mill by glutinous rice starch activation 50～60h;
(2) adjust breast: get the glutinous rice starch after step (1) activation, being mixed with massfraction with deionized water is 35%～40% starch milk;
(3) catalysis: add catalyzer in the described starch milk of step (2), be uniformly mixed, then with alkaline solution adjusting pH to 8～10, obtain the starch milk after catalysis;
(4) oxidation: add oxygenant in the starch milk after the described catalysis of step (3), isothermal reaction obtains the starch emulsion after oxidation;
(5) termination reaction: the starch emulsion pH value after the described oxidation of step (4) is neutralized to 6 with hydrochloric acid soln, then drips reductive agent termination reaction, obtain being oxidized the thick product of glutinous rice starch;
(6) product purifies: by the thick product of described oxidation glutinous rice starch after filtration, washing, dry, pulverize, screening, obtain being oxidized glutinous rice starch.
2. a kind of preparation method who is oxidized glutinous rice starch according to claim 1, is characterized in that: the condition of the described activation of step (1) is: under room temperature condition, activate, ball mill revolution speed is 150r/min, and rotational velocity is 300r/min; The internal diameter of ball mill is 100mm, and volume is 500ml; In ball mill, the diameter of abrading-ball is 50mm, and Material quality of grinding balls is agate.
3. a kind of preparation method who is oxidized glutinous rice starch according to claim 1, is characterized in that: the described catalyzer of step (3) is the cobalt chloride solution of massfraction 2%～4% or the ferrous sulfate aqueous solution of massfraction 2%～4%; The described alkaline solution of step (3) is that massfraction is the potassium hydroxide solution that 3%～5% sodium hydroxide solution or massfraction are 3%～5%.
4. a kind of preparation method who is oxidized glutinous rice starch according to claim 1, is characterized in that: the consumption of the described catalyzer of step (3) is 1%～2.5% of glutinous rice starch quality after the described activation of step (2).
5. a kind of preparation method who is oxidized glutinous rice starch according to claim 1, is characterized in that: the described oxygenant of step (4) is that massfraction is 30%～40% hydrogen peroxide; The described reductive agent of step (5) is that massfraction is the potassium sulfite solution that 5% sodium sulfite solution or massfraction are 5%; The concentration of the described hydrochloric acid soln of step (5) is 0.1mol/L.
6. a kind of preparation method who is oxidized glutinous rice starch according to claim 1, is characterized in that: the consumption of the described oxygenant of step (4) is 1.5%～3% of glutinous rice starch quality after the described activation of step (2); The pH value that the described interpolation reductive agent of step (5) continues to drop to the starch emulsion after described oxidation is till 7～7.5 o'clock.
7. a kind of preparation method who is oxidized glutinous rice starch according to claim 1, is characterized in that: the described isothermal reaction of step (4) is to react 1.0～3h under 40～45 DEG C of conditions of constant temperature.
8. the oxidation glutinous rice starch preparing according to preparation method described in claim 1 to 7 any one.
9. the application of oxidation glutinous rice starch according to claim 8 in paper industry.
10. the application of oxidation glutinous rice starch according to claim 8 in preparation table surface sizing agent, coating binder, wet end additive or adhesive for corrugated paperboard.
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| CN104782986A (en) * | 2015-04-28 | 2015-07-22 | 防城港市雅美好饲料有限公司 | Method for preparing special pre-gelatinized starch feed for aquaculture |
| CN106632706A (en) * | 2016-09-14 | 2017-05-10 | 重庆交通大学 | Method for preparing medium molecular branched-chain activator by using sticky rice |
| CN106986576A (en) * | 2017-05-02 | 2017-07-28 | 杨朝雄 | The preparation method of garden waste retaining soil |
| CN107254806A (en) * | 2017-06-12 | 2017-10-17 | 杭州特种纸业有限公司 | Label leather paper and its preparation method and application |
| CN107334141A (en) * | 2017-06-21 | 2017-11-10 | 许昌学院 | A kind of sweet potato oxidized starch and preparation method thereof |
| CN110331620A (en) * | 2019-07-09 | 2019-10-15 | 天津科技大学 | A kind of preparation method and applications of starch-based biological latex |
| CN115873139A (en) * | 2022-07-13 | 2023-03-31 | 上海交通大学 | Preparation method of dilute alkali hydrothermal modified starch |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104782986A (en) * | 2015-04-28 | 2015-07-22 | 防城港市雅美好饲料有限公司 | Method for preparing special pre-gelatinized starch feed for aquaculture |
| CN106632706A (en) * | 2016-09-14 | 2017-05-10 | 重庆交通大学 | Method for preparing medium molecular branched-chain activator by using sticky rice |
| CN106632706B (en) * | 2016-09-14 | 2019-06-28 | 重庆交通大学 | A method of with glutinous rice prepare in molecule branch activating agent |
| CN106986576A (en) * | 2017-05-02 | 2017-07-28 | 杨朝雄 | The preparation method of garden waste retaining soil |
| CN107254806A (en) * | 2017-06-12 | 2017-10-17 | 杭州特种纸业有限公司 | Label leather paper and its preparation method and application |
| CN107334141A (en) * | 2017-06-21 | 2017-11-10 | 许昌学院 | A kind of sweet potato oxidized starch and preparation method thereof |
| CN110331620A (en) * | 2019-07-09 | 2019-10-15 | 天津科技大学 | A kind of preparation method and applications of starch-based biological latex |
| CN115873139A (en) * | 2022-07-13 | 2023-03-31 | 上海交通大学 | Preparation method of dilute alkali hydrothermal modified starch |
| CN115873139B (en) * | 2022-07-13 | 2024-06-04 | 上海交通大学 | Preparation method of dilute alkali hydrothermal solution modified starch |
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