CN115448988A - Method for efficiently preparing acetate high-amylose corn starch - Google Patents
Method for efficiently preparing acetate high-amylose corn starch Download PDFInfo
- Publication number
- CN115448988A CN115448988A CN202211080874.3A CN202211080874A CN115448988A CN 115448988 A CN115448988 A CN 115448988A CN 202211080874 A CN202211080874 A CN 202211080874A CN 115448988 A CN115448988 A CN 115448988A
- Authority
- CN
- China
- Prior art keywords
- corn starch
- stirring
- amylose corn
- ethanol
- starch
- 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
- 229920000856 Amylose Polymers 0.000 title claims abstract description 61
- 229920002261 Corn starch Polymers 0.000 title claims abstract description 57
- 239000008120 corn starch Substances 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 32
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 title claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 93
- 238000003756 stirring Methods 0.000 claims abstract description 38
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 27
- WETWJCDKMRHUPV-UHFFFAOYSA-N acetyl chloride Chemical compound CC(Cl)=O WETWJCDKMRHUPV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000012346 acetyl chloride Substances 0.000 claims abstract description 15
- 150000007530 organic bases Chemical class 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002244 precipitate Substances 0.000 claims abstract description 7
- 238000000967 suction filtration Methods 0.000 claims abstract description 7
- 239000006228 supernatant Substances 0.000 claims abstract description 7
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical group C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 20
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 10
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- 238000006467 substitution reaction Methods 0.000 abstract description 10
- 239000003513 alkali Substances 0.000 abstract description 6
- 238000001035 drying Methods 0.000 abstract description 6
- 239000000047 product Substances 0.000 abstract description 4
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 230000036632 reaction speed Effects 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 229920002472 Starch Polymers 0.000 description 25
- 239000008107 starch Substances 0.000 description 25
- 235000019698 starch Nutrition 0.000 description 24
- 239000012065 filter cake Substances 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- 230000032050 esterification Effects 0.000 description 7
- 238000005886 esterification reaction Methods 0.000 description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 238000002386 leaching Methods 0.000 description 5
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 4
- 239000005457 ice water Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 125000004185 ester group Chemical group 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 150000001263 acyl chlorides Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 2
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- RZWZRACFZGVKFM-UHFFFAOYSA-N propanoyl chloride Chemical compound CCC(Cl)=O RZWZRACFZGVKFM-UHFFFAOYSA-N 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229920001685 Amylomaize Polymers 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 125000000218 acetic acid group Chemical group C(C)(=O)* 0.000 description 1
- 238000006640 acetylation reaction Methods 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- PASDCCFISLVPSO-UHFFFAOYSA-N benzoyl chloride Chemical compound ClC(=O)C1=CC=CC=C1 PASDCCFISLVPSO-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000113 differential scanning calorimetry Methods 0.000 description 1
- 235000019439 ethyl acetate Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B33/00—Preparation of derivatives of amylose
- C08B33/02—Esters
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The application relates to a method for efficiently preparing acetate high-amylose corn starch, which comprises the following steps: (1) Adding acetonitrile and organic base into high amylose corn starch, and stirring in a water bath for 0.5-1 h; (2) Slowly adding acetyl chloride, stirring for 1-12 h, then adding ethanol, stirring for 0.5-5 h, standing for 0.5-5 h, and removing supernatant; (3) Adding ethanol into the precipitate, stirring for 0.5-1 h, performing suction filtration, and washing with ethanol until no organic base taste exists. The high-amylose corn starch obtained by the method has low degree of substitution, but the viscosity and the gelatinization characteristics are obviously changed. The method uses a waterless environment, and because the organic alkali is used, no water is generated, namely no water is added or generated, the system viscosity is low, the filtration is convenient, the solvent removal is simple and quick, the industrial operation and the drying are convenient, and the product storage is facilitated. The reaction speed is high, the treatment is simple, and the operation energy consumption is low.
Description
Technical Field
The invention relates to a method for efficiently preparing acetate high-amylose corn starch, belonging to the technical field of chemical industry.
Background
High amylose corn starch refers to a corn variety with an amylose content of more than 50% in the corn starch. The high amylose starch has good film forming property and strength compared with common starch, and therefore has unique application value. However, the amylose content has a significant effect on the granular morphology, structure and properties of high amylose corn starch. The high amylose granules show a slight expansion at 100 ℃ and a marked expansion at about 120 ℃ and the double helix structure of amylose starts to unwind at 130 ℃ which is much higher than the gelatinization temperature of ordinary starch (50-70 ℃). The gelatinization temperature of the high-amylose corn starch is significantly delayed, and the gelatinization temperature range is significantly increased. Starch gelatinization is a prerequisite for starch gel formation, and the tight double helical structure in high amylose corn starch limits its widespread use. Therefore, there is a need for modifying high amylose corn starch to reduce the difficulty of processing, particularly gelatinizing, the high amylose corn starch and to expand the range of applications for high amylose corn starch.
At present, the research on starch esterification modification is mainly carried out on common starch, the research on the esterification degree and efficiency of the high amylose corn starch is less, the common starch does not have the specific film forming property and gel property of the high amylose corn starch, the existing acetic acid esterification preparation operation is complex, and the efficiency is low and the cost is high particularly for the preparation of the high substitution degree acetic ester high amylose corn starch. Therefore, further research on the modification of high amylose corn starch is needed to provide new application materials for the food industry and the chemical industry.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for efficiently preparing acetate high-amylose corn starch.
In order to achieve the purpose, the invention adopts the technical scheme that:
a method for efficiently preparing acetate high-amylose corn starch comprises the following steps:
(1) Adding acetonitrile and organic base into high amylose corn starch, and stirring for 0.5-1 h in a water bath at 0-30 ℃;
(2) Slowly adding acetyl chloride, stirring for 1-12 h, then adding ethanol, stirring for 0.5-5 h, standing for 0.5-5 h, and removing supernatant;
(3) Adding ethanol into the precipitate, stirring for 0.5-1 h, performing suction filtration, and washing with ethanol until no organic base taste exists, thus obtaining the product.
The organic base is pyridine or triethylamine.
The dosage relation ratio of the high amylose corn starch, the acetonitrile and the organic alkali is 5-10 g: 10-60 mL:3 to 30mL.
Acetyl chloride was added slowly over 1-30 min.
The dosage ratio of the acetyl chloride to the organic alkali is 1-4 mL:3 to 30mL.
The dosage relation ratio of the ethanol and the high amylose corn starch in the step (2) is 15-50 mL:10g.
The dosage relation ratio of the ethanol added in the stirring step (3) to the high amylose corn starch is 10-30 mL:10g.
And (4) stirring and washing with ethanol when washing in the step (3), and then leaching with ethanol.
The reaction principle of the invention is as follows:
starch is considered as an alcohol (ROH) and an acid chloride (RCOCl) to form an ester (RCOOR). Glucose unit C of a starch molecule 2 、C 3 、C 6 (FIG. 1) has a hydroxyl group, and may be substituted with an acid chloride under an alkaline condition, and the produced HCl is captured by an organic base to produce a salt. The esterification process greatly alters the hydrophobicity of starch by replacing the hydroxyl group on each glucose residue, thereby converting it to an ester group with the corresponding acyl chloride (acetyl chloride, propionyl chloride, phosphoryl chloride, etc.). During esterification, the reaction occurs either on the starch chains, forming the traditional starch ester, or on the outer surface of the starch granule, leaving the internal crystalline structure intact.
FIG. 2 illustrates the acetyl chloride-starch esterification mechanism, wherein acetyl chloride undergoes a substitution reaction by its acyl group with any free hydroxyl moiety of the available glucose monomer.
The invention has the beneficial effects that:
according to the method, reagents such as organic alkali, acetyl chloride and the like are selected for treatment, and under an alkaline condition, hydroxyl on the high-amylose corn starch is replaced by acyl chloride, so that the high-amylose corn starch is converted into an ester group, and the hydrophobicity of the high-amylose corn starch is changed. During the esterification process, conventional starch esters are formed on the starch chains.
The high-amylose corn starch obtained by the method has low degree of substitution, but the viscosity and the gelatinization characteristics are obviously changed. Wherein, the viscosity of the esterified high-amylose corn starch is remarkably reduced to 26-55% of that of untreated starch; the gelatinization temperature and gelatinization enthalpy are significantly reduced compared to untreated starch. Therefore, the method does not change the molecular structure of the starch greatly, but obtains a high-efficiency modification result with better characteristics.
The method of the invention uses an anhydrous environment, and no water is generated due to the use of the organic base, namely no water is added or generated, the viscosity of the system is small, the filtration is convenient, the solvent removal is simple and rapid, the industrial operation and drying are convenient, and the product storage is facilitated. The reaction speed is high, the treatment is simple, and the operation energy consumption is low.
The method is convenient to expand, and can convert acetyl chloride into propionyl chloride, benzoyl chloride and the like to obtain the corresponding esterified starch.
Drawings
FIG. 1 is a schematic representation of the hydroxyl position of a high amylose corn starch glucose unit.
FIG. 2 is a schematic diagram of the acetylation reaction of the present invention.
Detailed Description
The following examples further illustrate the embodiments of the present invention in detail.
Example 1
A method for efficiently preparing acetate high-amylose corn starch comprises the following steps: the method comprises the following steps:
adding 30mL of acetonitrile and 30mL of pyridine into 10g of high amylose corn starch (the amylose content is 73.67 percent), and stirring in an ice water bath at 0-4 ℃ for 0.5h; slowly adding 1mL of acetyl chloride within 4min, stirring for 2h, adding 25mL of ethanol, stirring for 1h, standing for 1h, and removing a supernatant; adding 30mL of ethanol into the precipitate, stirring for 1h, and performing suction filtration; stirring and washing with 25mL of ethanol, leaching with 25mL of ethanol, and repeating for three times until no pyridine smell exists; and (5) drying the filter cake to obtain the filter cake.
Example 2
A method for efficiently preparing acetate high-amylose corn starch comprises the following steps: the method comprises the following steps:
adding 30mL of acetonitrile and 30mL of pyridine into 10g of high amylose corn starch, and stirring for 0.5h in an ice water bath at the temperature of 0-4 ℃; slowly adding 2mL of acetyl chloride within 4min, stirring for 2h, adding 25mL of ethanol, stirring for 1h, standing for 1h, and removing a supernatant; adding 30mL of ethanol into the precipitate, stirring for 1h, and performing suction filtration; stirring and washing with 25mL of ethanol, leaching with 25mL of ethanol, and repeating for three times until no pyridine smell exists; and (5) drying the filter cake to obtain the filter cake.
Example 3
A method for efficiently preparing acetate high-amylose corn starch comprises the following steps: the method comprises the following steps:
adding 30mL of acetonitrile and 30mL of pyridine into 10g of high amylose corn starch, and stirring in an ice water bath at 0-4 ℃ for 0.5h; slowly adding 3mL of acetyl chloride within 4min, stirring for 2h, adding 25mL of ethanol, stirring for 1h, standing for 1h, and removing a supernatant; adding 30mL of ethanol into the precipitate, stirring for 1h, and performing suction filtration; stirring and washing with 25mL of ethanol, leaching with 25mL of ethanol, and repeating for three times until no pyridine smell exists; and (5) drying the filter cake to obtain the filter cake.
Example 4
A method for efficiently preparing acetate high-amylose corn starch comprises the following steps: the method comprises the following steps:
adding 30mL of acetonitrile and 30mL of pyridine into 10g of high amylose corn starch, and stirring for 0.5h in an ice water bath at the temperature of 0-4 ℃; slowly adding 4mL of acetyl chloride within 4min, stirring for 2h, adding 25mL of ethanol, stirring for 1h, standing for 1h, and removing a supernatant; adding 30mL of ethanol into the precipitate, stirring for 1h, and performing suction filtration; stirring and washing with 25mL of ethanol, leaching with 25mL of ethanol, and repeating for three times until no pyridine smell exists; and (5) drying the filter cake to obtain the filter cake.
Performance testing of the products of the invention
1. Gelatinization properties
The samples obtained in examples 1 to 4 were prepared into starch milk with a mass concentration of 8%, gelatinized for 30min at a temperature of 126 ℃ using a pressure cooker, and the viscosity of the paste at a temperature of 90 ℃ was measured using a DV-III rotational viscometer. The results are shown in table 1, using untreated high amylose corn starch as a control.
TABLE 1 viscosity of high amylose corn starch of the present invention
| Sample (I) | Example 1 | Example 2 | Example 3 | Example 4 | High amylose corn starch |
| Viscosity (cp) | 213.55±26.05 | 427.05±31.25 | 294.30±2.60 | 451.15±5.85 | 820.35±1.55 |
As can be seen from Table 1, the viscosity of the esterified high amylose corn starch is significantly reduced to 26-55% of the untreated starch.
2. Analysis of thermal Properties
The samples obtained in examples 1 to 4 and the untreated high amylose corn starch were analyzed by Differential Scanning Calorimetry (DSC) to determine thermal properties. Accurately weighing 2.5mg (on a dry basis) of the sample, wherein the ratio of the sample to water is 1:3, the scanning temperature range is 30-150 ℃, the heating rate is 10 ℃/min, and the nitrogen rate is 40mL/min. The results are shown in Table 2.
TABLE 2 thermal Properties of high amylose corn starch
| Sample name | T 0 /℃ | T p /℃ | T c /℃ | ΔH/(J·g -1 ) |
| Example 1 | 128.18±7.68 | 128.77±7.46 | 131.92±6.38 | 1.27±1.56 |
| Example 2 | 71.62±0.34 | 81.13±0.45 | 93.03±0.90 | 2.80±0.32 |
| Example 3 | 70.87±0.41 | 86.53±3.15 | 105.02±2.40 | 8.79±4.72 |
| Example 4 | 71.86±0.16 | 81.29±0.63 | 94.63±2.99 | 3.59±0.62 |
| High amylose corn starch | 121.62±3.44 | 121.98±3.78 | 126.92±1.10 | 77.02±76.48 |
Wherein, T 0 Represents the initial gelatinization temperature; t is p Represents the peak gelatinization temperature; t is c Indicating the end gelatinization temperature; Δ H represents the gelatinization enthalpy.
As can be seen from Table 2, the gelatinization temperature and enthalpy of the esterified high-amylose corn starch are significantly reduced, greatly improving the applicability of the high-amylose corn starch.
3. Degree of substitution
The samples obtained in examples 1 to 4 and untreated high amylose corn starch were analyzed for degree of substitution, and the results are shown in Table 3.
Putting 1.00g (calculated by dry basis) of a sample into the bottom of a 250mL conical flask (ensuring that no sticky starch particles exist on the wall of the conical flask), adding 50mL of 75% ethanol solution, magnetically stirring and wetting the sample for 2min, sealing, putting the sample into a magnetic constant-temperature water bath kettle at 50 ℃, heating and continuously stirring the sample for 30min, taking the sample out, cooling the sample to room temperature, slowly adding 40ml of 0.5mol/L NaOH solution, sealing, shaking the sample evenly, putting the sample into a constant-temperature oscillator, oscillating the sample for 72h at room temperature, taking the sample out, titrating the residual alkali by using 0.5mol/L hydrochloric acid standard solution, and taking phenolphthalein as an indicator. After standing for a period of time, titrating the separated alkali again, wherein the total amount of consumed hydrochloric acid is V 1 And simultaneously, taking untreated high amylose corn starch as a blank titration hydrochloric acid standard solution as V 2 . The above experiments were performed in triplicate and averaged. The calculation formula is as follows:
in the formula: 162 is the molar mass of one glucose unit; 43 is the molar mass of the ester groups.
TABLE 3 degree of substitution of high amylose corn starch
| Sample name | Degree of substitution |
| Example 1 | 0.05±0.01 |
| Example 2 | 0.06±0.02 |
| Example 3 | 0.02±0.01 |
| Example 4 | 0.04±0.02 |
| High amylose corn starch | - |
Among them, high amylose corn starch is untreated high amylose corn starch and thus has no degree of substitution.
As can be seen from Table 3, the degree of substitution in examples 1 to 4 is not particularly high, but the viscosity and the gelatinization behavior of the starch are significantly changed according to the above experiments. Therefore, the method has no great change on the molecular structure of the starch, but obtains better modification effect.
Claims (8)
1. The method for efficiently preparing the acetate high-amylose corn starch is characterized by comprising the following steps of:
(1) Adding acetonitrile and organic base into high amylose corn starch, and stirring in a water bath at 0-30 ℃ for 0.5-1 h;
(2) Slowly adding acetyl chloride, stirring for 1-12 h, adding ethanol, stirring for 0.5-5 h, standing for 0.5-5 h, and removing supernatant;
(3) Adding ethanol into the precipitate, stirring for 0.5-1 h, performing suction filtration, and washing with ethanol until no organic base taste exists.
2. The process of claim 1, wherein the organic base is pyridine or triethylamine.
3. The method of claim 1, wherein the high amylose corn starch, the acetonitrile, and the organic base are present in an amount ranging from 5 to 10g: 10-60 mL:3 to 30mL.
4. The method of claim 1, wherein acetyl chloride is added slowly over 1-30 min.
5. The method of claim 1, wherein the acetyl chloride is present in an amount of 1 to 4mL:3 to 30mL.
6. The method of claim 1, wherein the ethanol and the high amylose corn starch in step (2) are used in a ratio of 15 to 50mL:10g.
7. The method according to claim 1, wherein the ethanol added during the stirring in step (3) is used in an amount of 10 to 30mL:10g.
8. The method of claim 1, wherein the washing in step (3) is performed by stirring with ethanol and then rinsing with ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211080874.3A CN115448988A (en) | 2022-09-05 | 2022-09-05 | Method for efficiently preparing acetate high-amylose corn starch |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211080874.3A CN115448988A (en) | 2022-09-05 | 2022-09-05 | Method for efficiently preparing acetate high-amylose corn starch |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115448988A true CN115448988A (en) | 2022-12-09 |
Family
ID=84303242
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211080874.3A Pending CN115448988A (en) | 2022-09-05 | 2022-09-05 | Method for efficiently preparing acetate high-amylose corn starch |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115448988A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6454001A (en) * | 1987-08-24 | 1989-03-01 | Sugiyama Sangyo Kagaku Kenk | Production of water-soluble starch fatty acid ester |
| US5703226A (en) * | 1993-11-19 | 1997-12-30 | Parrish & Heimbecker, Limited | Method for acylation of starch |
| CN103570838A (en) * | 2013-10-17 | 2014-02-12 | 广州大学 | Preparation method of composite modified high amylose starch |
| CN104892779A (en) * | 2015-06-26 | 2015-09-09 | 江南大学 | Esterified starch and preparation method and application thereof |
| CN104893009A (en) * | 2015-06-26 | 2015-09-09 | 江南大学 | Starch-based composite and preparation method thereof |
| CN106832014A (en) * | 2017-02-27 | 2017-06-13 | 南京福科帝生物科技有限公司 | The method that solvent method prepares esterification porous-starch |
| CN114805619A (en) * | 2022-06-15 | 2022-07-29 | 河南工业大学 | Preparation method of acetylated modified high-amylose corn starch |
-
2022
- 2022-09-05 CN CN202211080874.3A patent/CN115448988A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6454001A (en) * | 1987-08-24 | 1989-03-01 | Sugiyama Sangyo Kagaku Kenk | Production of water-soluble starch fatty acid ester |
| US5703226A (en) * | 1993-11-19 | 1997-12-30 | Parrish & Heimbecker, Limited | Method for acylation of starch |
| CN103570838A (en) * | 2013-10-17 | 2014-02-12 | 广州大学 | Preparation method of composite modified high amylose starch |
| CN104892779A (en) * | 2015-06-26 | 2015-09-09 | 江南大学 | Esterified starch and preparation method and application thereof |
| CN104893009A (en) * | 2015-06-26 | 2015-09-09 | 江南大学 | Starch-based composite and preparation method thereof |
| CN106832014A (en) * | 2017-02-27 | 2017-06-13 | 南京福科帝生物科技有限公司 | The method that solvent method prepares esterification porous-starch |
| CN114805619A (en) * | 2022-06-15 | 2022-07-29 | 河南工业大学 | Preparation method of acetylated modified high-amylose corn starch |
Non-Patent Citations (1)
| Title |
|---|
| 尤新主编: "《淀粉衍生物》", vol. 1, 中国物资出版社, pages: 197 - 198 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Pushpamalar et al. | Optimization of reaction conditions for preparing carboxymethyl cellulose from sago waste | |
| Akpa et al. | Modification of cassava starch for industrial uses | |
| Singh et al. | Factors influencing the physico-chemical, morphological, thermal and rheological properties of some chemically modified starches for food applications—A review | |
| Ayucitra | Preparation and characterisation of acetylated corn starches | |
| Bhosale et al. | Effect of octenylsuccinylation on physicochemical and functional properties of waxy maize and amaranth starches | |
| Ren et al. | Two-step preparation and thermal characterization of cationic 2-hydroxypropyltrimethylammonium chloride hemicellulose polymers from sugarcane bagasse | |
| DE69829135T2 (en) | Modification of polysaccharide in compressed liquid | |
| Lin et al. | Study on physicochemical properties, digestive properties and application of acetylated starch in noodles | |
| Xiao et al. | Preparation and characterization of octenyl succinic anhydride modified agarose derivative | |
| Zhang et al. | Synthesis of long-chain fatty acid starch esters in aqueous medium and its characterization | |
| US3720663A (en) | Preparation of starch esters | |
| CN107663241B (en) | Cross-linked starch with high resistant starch content and preparation method thereof | |
| Trela et al. | Synthesis and characterization of acetylated cassava starch with different degrees of substitution | |
| Čížová et al. | Carboxymethyl starch octenylsuccinate: Microwave‐and ultrasound‐assisted synthesis and properties | |
| US3238193A (en) | Cross-linked starch esters and process of making same | |
| US3022289A (en) | Acylation of starch | |
| JPH07252302A (en) | Thermoplastic biodegradable polysaccharide derivatives, their production and their use | |
| Fashi et al. | Solid state malic acid esterification on fungal α-amylase treated corn starch: Design of a green dual treatment | |
| CN115448988A (en) | Method for efficiently preparing acetate high-amylose corn starch | |
| US2660577A (en) | Derivatization of starch witch lactones | |
| US3728332A (en) | Preparation of starch esters | |
| Qiu et al. | Synthesis and properties study of carboxymethyl cassava starch | |
| US9353193B2 (en) | Method for preparing acetylated derivatives of an amylaceous material | |
| US4992539A (en) | High-viscosity cold-water-swellable granular starch | |
| JP2010013549A (en) | Carboxylethyl cellulose |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |