CN111171184A - Preparation method of instant agar - Google Patents
Preparation method of instant agar Download PDFInfo
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- CN111171184A CN111171184A CN202010119644.8A CN202010119644A CN111171184A CN 111171184 A CN111171184 A CN 111171184A CN 202010119644 A CN202010119644 A CN 202010119644A CN 111171184 A CN111171184 A CN 111171184A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0036—Galactans; Derivatives thereof
- C08B37/0039—Agar; Agarose, i.e. D-galactose, 3,6-anhydro-D-galactose, methylated, sulfated, e.g. from the red algae Gelidium and Gracilaria; Agaropectin; Derivatives thereof, e.g. Sepharose, i.e. crosslinked agarose
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Abstract
The invention discloses a preparation method of instant agar, which comprises the following steps: (1) pulverizing and sieving; (2) alkalization; (3) hydroxypropylation reaction; (4) neutralizing; (5) washing; (6) drying and pulverizing. The dissolution temperature of the prepared instant agar is 70-80 ℃, the dissolution time is less than or equal to 5min, and the gel strength is 200-750g/cm2(1.5％)。
Description
Technical Field
The invention belongs to the technical field of food processing, and particularly relates to a preparation method of instant agar.
Background
agar, or agar is a kind of functional polysaccharide extracted from red algae, which is a macromolecular polysaccharide formed by repeated β -D-galactose and α -3, 6-lacton-L-galactose through crosslinking, agar is white yellowish powder, which is insoluble in cold water and soluble in hot water, can swell in cold water, absorbs about 20 times of water in volume, and can be completely dissolved only in hot water above 95 deg.C, agar is different from carrageenan and other ionic gels, the former can form gel with high transparency and strong stability without adding ions, agar also has thickening and suspending functions, and is widely used in the fields of food processing, medicine and biological engineering, but the solubility in water is poor due to the long molecular chain length and large degree of polymerization.
In order to improve the water solubility of the agar, at present, there are two main methods, namely a physical modification method and a chemical modification method, wherein the physical modification method comprises the steps of adding sugar as a cosolvent, carrying out high-pressure homogenization or ultrasonic treatment and the like to treat the agar, the method is simple, but the problems that the action of the sugar and the agar is insufficient or the agar structure is damaged to a certain extent after the ultrasonic treatment and the like are possible, the gel strength of the obtained agar product is not easy to control, and the effect of the physical modification method is limited. The chemical modification method is mainly a carboxymethyl method, the purpose of improving the water-soluble performance of the agar is achieved by introducing a carboxymethyl group with strong hydrophilicity into an agar molecular chain, the agar which can be quickly dissolved at room temperature can be obtained even according to different substitution degrees after the carboxymethyl, but the hydrogen bond action among the carbonyl groups on the carboxymethyl is weak, the strength of the modified agar gel is obviously reduced, and the method is not suitable for preparing the high-strength quickly dissolved agar.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of instant agar.
The technical scheme of the invention is as follows:
a preparation method of instant agar comprises the following steps:
(1) crushing and sieving: placing the agar into a universal pulverizer to pulverize, and sieving to obtain powdery agar;
(2) alkalization: adding the powdery agar into an ethanol solution, adding sodium hydroxide while stirring, and performing alkalization treatment at 30-50 ℃ to obtain a suspension;
(3) hydroxypropylation reaction: adding 1, 2-epoxypropane into the suspension obtained in the step (2), and reacting for 3-9h at 40-70 ℃;
(4) neutralizing: after the hydroxypropylation reaction is finished, after the system is cooled, adding acetic acid solution to adjust the pH value to 7.0-7.2;
(5) washing: filtering the material obtained in the step (4) and fully washing the material with an ethanol solution;
(6) drying and crushing: and (5) drying, crushing and sieving the materials obtained in the step (5) in sequence to obtain the instant agar, wherein the dissolving temperature of the instant agar is 70-80 ℃, and the dissolving time is less than or equal to 5 min.
In a preferred embodiment of the present invention, the step (1) is: and (3) placing the agar into a universal pulverizer to pulverize, and sieving the pulverized agar through a standard sieve of 200-300 meshes to obtain powdery agar with the particle size of less than or equal to 75 microns.
In a preferred embodiment of the present invention, the ethanol solution in the step (2) has a volume concentration of 60 to 95%.
Further preferably, in the step (2), the mass ratio of the powdered agar to the ethanol solution is 1: 4-1: 10.
In a preferred embodiment of the present invention, in the step (2), the mass ratio of the sodium hydroxide used for the alkalization treatment to the powdery agar is 1: 10 to 1: 20.
Further preferably, the time of the alkalization treatment is 1-2 h.
In a preferred embodiment of the present invention, in the step (3), 1, 2-propylene oxide is added in an amount of 1 to 3 times the mass of the powdered agar.
In a preferred embodiment of the present invention, in the step (4), the concentration of the acetic acid solution is 20 to 40% by volume.
In a preferred embodiment of the present invention, the ethanol solution in the step (5) has a volume concentration of 60 to 80%.
In a preferred embodiment of the present invention, the step (6) is: and (5) drying the material obtained in the step (5) by using a freeze dryer or a vacuum dryer, crushing and sieving to obtain the instant agar.
The invention has the beneficial effects that: dissolving the prepared instant agarThe dissolution temperature is 70-80 ℃, the dissolution time is less than or equal to 5min, and the gel strength is 200-750g/cm2(1.5％)。
Detailed Description
The technical solution of the present invention is further illustrated and described by the following detailed description.
Example 1
(1) Crushing raw material agar by a crusher, and sieving by a 250-mesh sieve to obtain powdery agar which is sieved by a 250-mesh sieve;
(2) adding 70L of 80% ethanol solution into a 150L reaction kettle, adding 10kg of powdery agar obtained by sieving in the step (1) into the reaction kettle, adding 0.7kg of sodium hydroxide solid, and stirring and alkalizing for 1.5h at the constant temperature of 40 ℃;
(3) heating the reaction system to 55 ℃, introducing 12L of 1, 2-epoxypropane, and stirring and reacting for 6 hours at constant temperature;
(4) after the reaction is finished, cooling the reaction system to 45 ℃, slowly introducing an acetic acid solution with the volume concentration of 20%, stirring for 10min after the introduction is finished, and adjusting the pH to 7.0;
(5) the obtained reaction suspension is subjected to pressure filtration by a plate-and-frame filter press and washed twice by ethanol solution with volume concentration of 70%, the obtained wet sample is subjected to freeze drying, crushing and sieving to obtain the instant agar which is quickly dissolved in hot water at 78 ℃, the dissolving time is 3min, and the gel strength is 377g/cm2(1.5％)。
Example 2
(1) Crushing raw material agar by a crusher, and sieving by a 300-mesh sieve to obtain powdery agar which is sieved by the 300-mesh sieve;
(2) adding 80L of 95 vol% ethanol solution into a 150L reaction kettle, adding 10kg of powdery agar obtained by sieving in the step (1) into the reaction kettle, adding 1kg of sodium hydroxide solid, and stirring and alkalizing for 2h at a constant temperature of 50 ℃;
(3) heating the reaction system to 70 ℃, introducing 18L of 1, 2-epoxypropane, and stirring at constant temperature for reaction for 9 hours;
(4) after the reaction is finished, cooling the reaction system to 40 ℃, slowly introducing an acetic acid solution with the volume concentration of 40%, stirring for 15min after the introduction is finished, and adjusting the pH to 7.0;
(5) filter-pressing the obtained reaction suspension by a plate-and-frame filter press, washing twice by using an ethanol solution with the volume concentration of 80%, freeze-drying the obtained wet sample, crushing and sieving to obtain the instant agar which is quickly dissolved in hot water at 72 ℃, wherein the dissolving time is 1min, and the gel strength is 205g/cm2(1.5％)。
Example 3
(1) Crushing raw material agar by a crusher, and sieving by a 200-mesh sieve to obtain powdery agar which is sieved by the 200-mesh sieve;
(2) adding 100L of 80% ethanol solution into a 150L reaction kettle, adding 10kg of the powdery agar obtained by sieving in the step (1) into the reaction kettle, adding 0.5kg of sodium hydroxide solid, and stirring and alkalizing for 1h at constant temperature of 30 ℃;
(3) heating the reaction system to 40 ℃, introducing 10L of 1, 2-epoxypropane, and carrying out heat preservation and stirring reaction for 3 hours;
(4) after the reaction is finished, cooling the reaction system to 35 ℃, slowly introducing an acetic acid solution with the volume concentration of 30%, stirring for 5min after the introduction is finished, and adjusting the pH value to 7.0;
(5) filter-pressing the obtained reaction suspension by a plate-and-frame filter press, washing twice by using an ethanol solution with the volume concentration of 60%, freeze-drying the obtained wet sample, crushing and sieving to obtain the instant agar which is quickly dissolved in hot water at 80 ℃, wherein the dissolving time is 5min, and the gel strength is 746g/cm2(1.5％)。
Example 4
(1) Crushing raw material agar by a crusher, and sieving by a 270-mesh sieve to obtain powdery agar which is sieved by 270 meshes;
(2) adding 60L of 90% ethanol solution into a 150L reaction kettle, adding 10kg of powdery agar obtained by sieving in the step (1) into the reaction kettle, adding 0.6kg of sodium hydroxide solid, and stirring and alkalizing for 1.5h at the constant temperature of 45 ℃;
(3) heating the reaction system to 50 ℃, introducing 10L of 1, 2-epoxypropane, and stirring and reacting for 4 hours at constant temperature;
(4) after the reaction is finished, cooling the reaction system to 40 ℃, slowly introducing an acetic acid solution with the volume concentration of 20%, stirring for 8min after the introduction is finished, and adjusting the pH to 7.0;
(5) filter-pressing the obtained reaction suspension by a plate-and-frame filter press, washing twice by using an ethanol solution with the volume concentration of 80%, freeze-drying the obtained wet sample, crushing and sieving to obtain the instant agar which is quickly dissolved in hot water at 78 ℃, wherein the dissolving time is 4min, and the gel strength is 560g/cm2(1.5％)。
Example 5
(1) Crushing raw material agar by a crusher, and sieving by a 300-mesh sieve to obtain powdery agar which is sieved by the 300-mesh sieve;
(2) adding 40L of 90% ethanol solution into a 150L reaction kettle, adding 10kg of powdery agar obtained by sieving in the step (1) into the reaction kettle, adding 0.8kg of sodium hydroxide solid, and stirring and alkalizing for 1.8h at the constant temperature of 36 ℃;
(3) heating the reaction system to 60 ℃, introducing 14L of 1, 2-epoxypropane, and stirring and reacting for 5 hours at constant temperature;
(4) after the reaction is finished, cooling the reaction system to 50 ℃, slowly introducing an acetic acid solution with the volume concentration of 30%, stirring for 8min after the introduction is finished, and adjusting the pH to 7.0;
(5) filter-pressing the obtained reaction suspension by a plate-and-frame filter press, washing twice by using an ethanol solution with the volume concentration of 80%, freeze-drying the obtained wet sample, crushing and sieving to obtain the instant agar which is quickly dissolved in hot water with the temperature of 76 ℃, wherein the dissolving time is 2min, and the gel strength is 316g/cm2(1.5％)。
Comparative example
The results of comparing the instant agar prepared in the above examples with the solutions disclosed in CN102766224A, CN1793184A, CN108264584A and CN106977752A in sequence are shown in the following table:
the above description is only a preferred embodiment of the present invention, and therefore should not be taken as limiting the scope of the invention, which is defined by the appended claims.
Claims (10)
1. A preparation method of instant agar is characterized in that: the method comprises the following steps:
(1) crushing and sieving: placing the agar into a universal pulverizer to pulverize, and sieving to obtain powdery agar;
(2) alkalization: adding the powdery agar into an ethanol solution, adding sodium hydroxide while stirring, and performing alkalization treatment at 30-50 ℃ to obtain a suspension;
(3) hydroxypropylation reaction: adding 1, 2-epoxypropane into the suspension obtained in the step (2), and reacting for 3-9h at 40-70 ℃;
(4) neutralizing: after the hydroxypropylation reaction is finished, after the system is cooled, adding acetic acid solution into the system to adjust the pH value to 7.0-7.2;
(5) washing: filtering the material obtained in the step (4) and fully washing the material with an ethanol solution;
(6) drying and crushing: and (3) drying, crushing and sieving the material obtained in the step (5) in sequence to obtain the instant agar, wherein the dissolving temperature of the instant agar is 70-80 ℃, and the dissolving time is less than or equal to 5 min.
2. The method of claim 1, wherein: the step (1) is as follows: and (3) placing the agar into a universal pulverizer to pulverize, and sieving the pulverized agar through a standard sieve of 200-300 meshes to obtain powdery agar with the particle size of less than or equal to 75 microns.
3. The method of claim 1, wherein: the volume concentration of the ethanol solution in the step (2) is 80-95%.
4. The method of claim 3, wherein: in the step (2), the mass ratio of the powdery agar to the ethanol solution is 1: 4-1: 10.
5. The method of claim 1, wherein: in the step (2), the mass ratio of the sodium hydroxide used for the alkalization treatment to the powdery agar is 1: 10-1: 20.
6. The method of claim 5, wherein: the time of the alkalization treatment is 1-2 h.
7. The method of claim 1, wherein: in the step (3), the addition amount of the 1, 2-epoxypropane is 1-3 times of the mass of the powdery agar.
8. The method of claim 1, wherein: in the step (4), the volume concentration of the acetic acid solution is 20-40%.
9. The method of claim 1, wherein: the volume concentration of the ethanol solution in the step (5) is 60-80%.
10. The method of claim 1, wherein: the step (6) is as follows: and (5) drying the material obtained in the step (5) by using a freeze dryer or a vacuum dryer, crushing and sieving to obtain the instant agar.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864960A (en) * | 2014-04-03 | 2014-06-18 | 福建省水产研究所 | Preparation method for hydroxypropyl low-melting-point agarose |
| CN105175579A (en) * | 2015-10-20 | 2015-12-23 | 国家海洋局第三海洋研究所 | Preparation method of instant agar |
| CN105542035A (en) * | 2016-01-22 | 2016-05-04 | 华侨大学 | Preparation method of low-solidification-temperature agarose |
| CN107674132A (en) * | 2017-09-28 | 2018-02-09 | 福建农林大学 | A kind of processing method of the soft Agar Gel of low-temperature instant |
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2020
- 2020-02-26 CN CN202010119644.8A patent/CN111171184B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864960A (en) * | 2014-04-03 | 2014-06-18 | 福建省水产研究所 | Preparation method for hydroxypropyl low-melting-point agarose |
| CN105175579A (en) * | 2015-10-20 | 2015-12-23 | 国家海洋局第三海洋研究所 | Preparation method of instant agar |
| CN105542035A (en) * | 2016-01-22 | 2016-05-04 | 华侨大学 | Preparation method of low-solidification-temperature agarose |
| CN107674132A (en) * | 2017-09-28 | 2018-02-09 | 福建农林大学 | A kind of processing method of the soft Agar Gel of low-temperature instant |
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