CN114751999A - Green preparation method of acidolysis polysaccharide - Google Patents
Green preparation method of acidolysis polysaccharide Download PDFInfo
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- CN114751999A CN114751999A CN202210541173.9A CN202210541173A CN114751999A CN 114751999 A CN114751999 A CN 114751999A CN 202210541173 A CN202210541173 A CN 202210541173A CN 114751999 A CN114751999 A CN 114751999A
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 76
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 76
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 230000005684 electric field Effects 0.000 claims abstract description 30
- 239000002253 acid Substances 0.000 claims abstract description 25
- 230000006698 induction Effects 0.000 claims abstract description 25
- 229920002907 Guar gum Polymers 0.000 claims abstract description 22
- 229960002154 guar gum Drugs 0.000 claims abstract description 22
- 235000010417 guar gum Nutrition 0.000 claims abstract description 22
- 239000000665 guar gum Substances 0.000 claims abstract description 22
- 150000007522 mineralic acids Chemical class 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 229920001661 Chitosan Polymers 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 18
- 239000011541 reaction mixture Substances 0.000 claims description 16
- 238000005903 acid hydrolysis reaction Methods 0.000 claims description 15
- 230000005284 excitation Effects 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 238000001556 precipitation Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000009826 distribution Methods 0.000 abstract description 10
- 230000000694 effects Effects 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 239000012429 reaction media Substances 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 36
- 239000000047 product Substances 0.000 description 10
- 239000000706 filtrate Substances 0.000 description 8
- 230000003472 neutralizing effect Effects 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 101710134784 Agnoprotein Proteins 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000002715 modification method Methods 0.000 description 4
- 229910052573 porcelain Inorganic materials 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000005086 pumping Methods 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 238000003892 spreading Methods 0.000 description 4
- 230000007480 spreading Effects 0.000 description 4
- 238000013021 overheating Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000000967 suction filtration Methods 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 244000007835 Cyamopsis tetragonoloba Species 0.000 description 1
- 239000012445 acidic reagent Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0087—Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof
- C08B37/0096—Guar, guar gum, guar flour, guaran, i.e. (beta-1,4) linked D-mannose units in the main chain branched with D-galactose units in (alpha-1,6), e.g. from Cyamopsis Tetragonolobus; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- 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
-
- C—CHEMISTRY; METALLURGY
- 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
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Molecular Biology (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Emergency Medicine (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The application discloses a green preparation method of acidolysis polysaccharide, which comprises the following steps: placing the polysaccharide acid solution in an induction electric field for acidolysis treatment to prepare acidolysis polysaccharide; the polysaccharide acid solution comprises a polysaccharide-based material and an inorganic acid. This application utilizes induction electric field as the auxiliary means, regard as reaction medium with inorganic acid solution, to guar gum, polysaccharide such as chitosan carries out the acidolysis and modifies, wherein utilize non-contact's induction electric field joule heating effect and non-heat effect, polysaccharide preparation efficiency is higher than current acidolysis polysaccharide method, the resultant product molecular weight distribution interval is narrow, the acidolysis is more thorough, the polysaccharide molecule is more even unanimous, non-contact's electric field acidolysis is safe green, reaction conditions is mild, the product quality is high, has fine industrialization application prospect.
Description
Technical Field
The application particularly relates to a green preparation method of acidolysis polysaccharide.
Background
Acid hydrolysis can increase the utilization rate of polysaccharide and improve its physicochemical properties, and is generally used as a pretreatment means for enzymatic and chemical modification. However, the complex structure of the polysaccharide and the poor water solubility of part of the polysaccharide lead to the phenomena of low acidolysis efficiency, long reaction time, low product degradation degree and the like. Although it has been discovered in recent years that the acid hydrolysis efficiency of polysaccharides can be improved by using high-voltage pulsed electric field, ohmic heating and medium auxiliary techniques, these techniques have some drawbacks that are difficult to overcome, for example, they require a metal electrode to be in contact with a reaction system, and since the reaction system is acidic, metal ions and the like in the metal electrode are liable to be eluted and enter the final product, and the final product is contaminated, resulting in serious degradation of quality.
Disclosure of Invention
The main purpose of the present application is to provide a green preparation method of acidolysis polysaccharide to overcome the disadvantages of the prior art.
In order to achieve the above purpose, the present application adopts a technical solution comprising:
some embodiments of the present application provide a green preparation method of acid hydrolysis polysaccharide, comprising: placing the polysaccharide acid solution in an induction electric field with the excitation voltage of 25-150V and the frequency of 400-700Hz for acidolysis treatment to prepare acidolysis polysaccharide; wherein the polysaccharide acid solution comprises a polysaccharide-based material and an inorganic acid. According to the electromagnetic induction principle, if the excitation voltage is too high, a local overheating phenomenon can occur, so that the acidic medium is burnt and blocked, and if the excitation voltage is too low, the induced electric field strength induced in the medium is insufficient, so that the acidolysis efficiency is low. And according to the ohmic heating raw material, if the frequency is too high, the effective migration distance of the charged solute is small, the acidolysis efficiency is low due to insufficient thermal effect, and if the frequency is too low, the effective migration distance of the charged solute is large, but the loss of the excitation loop is high at low frequency, so that the strength of an effective induction electric field induced in the extraction of the acidolysis medium is low, and the acidolysis efficiency is also low.
In one embodiment, the green preparation method specifically includes:
Mixing inorganic acid and water uniformly to form an inorganic acid solution with the concentration of 0.1-1.5mol/L, wherein if the concentration of the inorganic acid is too high, a local overheating phenomenon can occur, so that an acidolysis medium is burnt and blocked; if the concentration of the inorganic acid is too low, the system impedance is high, the induced electric field intensity in the medium is not enough, and the acidolysis efficiency is low;
adding a polysaccharide-based material into the inorganic acid solution and uniformly mixing to form a polysaccharide acid solution, wherein the polysaccharide acid solution contains 0.5-5 wt% of the polysaccharide-based material, and if the content of the polysaccharide-based material is too high, the viscosity is high, the impedance is low, so that the local overheating phenomenon is easy to occur, and the medium is burnt and blocked; if the polysaccharide matrix content is too low, the system impedance is high, which results in insufficient induced electric field strength inside the medium and low acidolysis efficiency.
In one embodiment, the green preparation method specifically includes: and (3) placing the polysaccharide acid solution in the induction electric field, and continuously stirring at a stirring speed of 200-300rpm until the acid hydrolysis treatment is completed.
In one embodiment, the polysaccharide based material is selected from pure polysaccharides or agricultural byproducts having a major component of polysaccharides.
In one embodiment, the polysaccharide includes any one or combination of guar gum, chitosan, but is not limited thereto.
In one embodiment, the inorganic acid includes any one or a combination of more of hydrochloric acid, sulfuric acid, and nitric acid, but is not limited thereto.
In one embodiment, the green preparation method specifically includes: and during the acidolysis treatment, the temperature of the polysaccharide acid solution is controlled to be 20-50 ℃, and the acidolysis treatment time is 4-6 h.
In one embodiment, the green color preparation method further comprises: after the acid hydrolysis treatment is completed, the obtained reaction mixture is subjected to post-treatment to obtain acid-hydrolyzed polysaccharide.
In one embodiment, the post-processing comprises: adjusting the pH value of the reaction mixture to 7 by using an alkaline substance, adding ethanol for precipitation, filtering, washing and drying to obtain the acidolysis polysaccharide.
In one embodiment, the post-processing specifically includes: and fully washing the filtered solid with 70 v/v% ethanol water solution until no chloride ions are separated out, freeze-drying, and sieving with a 100-mesh sieve to obtain the acid hydrolysis polysaccharide.
Compared with the prior art, the technical scheme provided by the embodiment of the application is that an induction electric field is used as an auxiliary means, an inorganic acid solution is used as a reaction medium, and acidolysis modification is carried out on polysaccharides such as guar gum and chitosan, so that non-contact electric field processing is realized, the joule heat effect and the non-heat effect of the induction electric field are utilized, the polysaccharide production efficiency is remarkably improved, the molecular weight distribution interval of the obtained product is narrow, and the obtained acidolysis polysaccharide molecules are more uniform and consistent and have high quality; on the contrary, the product has a large molecular weight distribution interval, which indicates that the acidolysis is not thorough, the molecular size is not uniform, i.e. the quality is poor, the method is safe and green, the reaction condition is mild, the product quality is high, and the method has a good industrial application prospect.
Detailed Description
This application is when the acidolysis polysaccharide, through assisting with appropriate induction electric field, can realize the modification of quick, high efficiency, high yield of polysaccharide acidolysis under the condition of not introducing exogenous material, and the quality of the modified polysaccharide product that obtains is higher, mainly shows that its molecular weight distribution interval is narrow, shows that the polysaccharide molecule of acidolysis is more even unanimous, otherwise the molecular weight distribution interval is big, shows that the acidolysis is not thorough, and the molecular size is inhomogeneous promptly the quality is poor. The principle of the application mainly lies in that: the induction electric field that the magnetic field induction produced can produce the electric current in mixing feed liquid system, and they have the synergism of non-heat effect and heat effect separately, can improve reaction efficiency for the ion after the acid dissociation in the raw materials and the collision of polysaccharide molecule, and efficiency is higher, and is more obvious with acid reagent combined action effect, makes follow-up separation labour saving and time saving, thereby can save time and the energy.
Based on the above unexpected findings, the applicant has proposed the technical solution of the present application, and the technical solution, the implementation process and the principle thereof, etc. will be further explained with reference to several embodiments as follows. It should be understood, however, that within the scope of the present application, the above-described features of the present application and those specifically described below (examples) may be combined with one another to form new or preferred embodiments. Not to be repeated herein, depending on the space.
In the following examples, unless otherwise specified, various raw materials, reagents, reaction equipment, test equipment and methods used were commercially available.
Embodiment 1 a modification method for preparing acid-hydrolyzed guar gum with the assistance of an induction electric field, comprising the following steps:
(1) preparing an inorganic acid solution: a hydrochloric acid solution with the concentration of about 0.15mol/L is prepared by concentrated hydrochloric acid and deionized water, and the total volume is about 400 mL.
(2) Acid hydrolysis: adding guar gum into the hydrochloric acid solution prepared in the step (1), and stirring for about 5min to fully mix the guar gum and the hydrochloric acid solution to obtain guar gum acid solution with polysaccharide concentration of about 0.8 wt%.
(3) Acidolysis in an induction electric field: pumping the guar gum acid solution prepared in the step (2) into an induction electric field system, controlling the excitation condition to be about 75V of excitation voltage, about 400Hz of frequency, about 50 ℃ of constant-temperature water bath temperature, treating for about 4h, and stirring at the speed of about 200 rpm.
(4) Neutralizing: and (3) neutralizing the reaction mixture finally obtained in the step (3) by using an NaOH solution with the concentration of about 8mol/L, adding the NaOH solution while stirring so as to uniformly neutralize the reaction mixture until the pH value reaches 7.0, and stopping adding the NaOH solution.
(5) And (3) precipitation: adding three times of ethanol into the reaction mixture treated in the step (4), precipitating, filtering by suction, and using about 7 Washing the filtrate with 0% (v/v) ethanol until the eluate is free of chloride ions (with AgNO)3No white precipitate was detected from the solution).
(6) And (3) drying: and (5) spreading the filtered substance treated in the step (5) in a white porcelain plate, and drying in a freeze dryer.
(7) Screening: and (4) sieving powder with the fineness of about 100 meshes from the filtrate treated in the step (6), namely the prepared acid hydrolysis guar gum, wherein the molecular weight distribution interval of the product is about 9000-10000 Da.
Comparative example 1 a method for the modification of acid-split guar comprising the steps of:
steps (1) to (2): same as in steps (1) to (2) of example 1.
And (3): putting the beaker into a constant-temperature water bath kettle which is adjusted to about 50 ℃, stirring for about 20h, and taking out.
Steps (4) - (7): same as in steps (4) to (7) of example 1.
The molecular weight distribution range of the finally obtained product of the comparative example 1 is about 11000-14000Da, and the treatment time of the comparative example 1 is obviously higher than that of the example 1.
Embodiment 2 a modification method for preparing acidolysis chitosan by induction electric field assistance, comprising the following steps:
(1) preparing an inorganic acid solution: a hydrochloric acid solution with the concentration of about 0.15mol/L is prepared by concentrated hydrochloric acid and deionized water, and the total volume is about 400 mL.
(2) Acid hydrolysis: adding chitosan into the hydrochloric acid solution prepared in the step (1), and stirring for 5min to fully and uniformly mix the chitosan and the hydrochloric acid solution to obtain chitosan acid solution with the polysaccharide concentration of about 0.8 wt%.
(3) Acidolysis in an induction electric field: pumping the chitosan acid solution prepared in the step (2) into an induction electric field system, controlling the excitation condition to be about 75V of excitation voltage, about 400Hz of frequency, about 50 ℃ of constant-temperature water bath temperature, treating for about 5h, and stirring at the speed of about 200 rpm.
(4) Neutralizing: and (3) neutralizing the reaction mixture finally obtained in the step (3) by using an NaOH solution with the concentration of about 8mol/L, adding the NaOH solution while stirring so as to uniformly neutralize the reaction mixture until the pH value reaches 7.0, and stopping adding the NaOH solution.
(5) And (3) precipitation: step towards the channelsAdding ethanol with three times volume into the reaction mixture treated in the step (4) for precipitation, performing suction filtration, and washing the filtrate by using about 70% (v/v) ethanol until the eluate is free of chloride ions (by using AgNO)3No white precipitate was detectable in the solution).
(6) And (3) drying: and (5) spreading the filtered substance processed in the step (5) in a white porcelain plate, and drying in a freeze dryer.
(7) Screening: sieving the filtrate from step (6) to obtain powder with fineness of about 100 meshes, i.e. the prepared acid hydrolyzed chitosan with molecular weight of about 1.18 × 105g/mol。
Comparative example 2 a method for modification by acid hydrolysis of chitosan comprising the steps of:
steps (1) to (2): same as in steps (1) to (2) of example 1.
And (3): putting the beaker into a constant-temperature water bath kettle adjusted to about 50 ℃, stirring for 20h, and taking out.
Steps (4) - (7): same as in steps (4) to (7) of example 1.
The molecular weight distribution of the finally obtained product of comparative example 2 is within the range of about 12000-16000Da, and the treatment time of comparative example 2 is significantly higher than that of example 2.
Embodiment 3 a modification method for preparing acid-hydrolyzed guar gum with the assistance of an induction electric field, comprising the following steps:
(1) preparing an inorganic acid solution: a hydrochloric acid solution with the concentration of about 1.5mol/L is prepared by concentrated hydrochloric acid and deionized water, and the total volume is about 400 mL.
(2) Acid hydrolysis: adding guar gum into the hydrochloric acid solution prepared in the step (1), and stirring for about 5min to fully mix the guar gum and the hydrochloric acid solution to obtain guar gum acid solution with polysaccharide concentration of about 0.5 wt%.
(3) Acidolysis in an induction electric field: pumping the guar gum acid solution prepared in the step (2) into an induction electric field system, and controlling the excitation conditions to be about 25V of excitation voltage, about 700Hz of frequency, about 30 ℃ of constant-temperature water bath temperature, about 6h of treatment and about 200rpm of stirring speed.
(4) Neutralizing: and (3) neutralizing the reaction mixture finally obtained in the step (3) by using an NaOH solution with the concentration of about 8mol/L, adding the NaOH solution while stirring so as to uniformly neutralize the reaction mixture until the pH value reaches 7.0, and stopping adding the NaOH solution.
(5) And (3) precipitation: adding three times volume of ethanol into the reaction mixture treated in the step (4) for precipitation, performing suction filtration, and washing the filtrate with about 70% (v/v) ethanol until the eluate is free of chloride ions (by AgNO) 3No white precipitate was detectable in the solution).
(6) And (3) drying: and (5) spreading the filtered substance treated in the step (5) in a white porcelain plate, and drying in a freeze dryer.
(7) Screening: and (4) sieving powder with the fineness of about 100 meshes from the filtrate treated in the step (6), namely the prepared acidolysis guar gum, wherein the molecular weight distribution interval of the product is about 8000-8500 Da.
Embodiment 4 a modification method for preparing acid hydrolyzed guar gum with the assistance of an induction electric field, comprising the following steps:
(1) preparing an inorganic acid solution: a hydrochloric acid solution with the concentration of about 1.5mol/L is prepared by concentrated hydrochloric acid and deionized water, and the total volume is about 400 mL.
(2) Acid hydrolysis: adding guar gum into the hydrochloric acid solution prepared in the step (1), and stirring for about 5min to fully and uniformly mix the guar gum and the hydrochloric acid solution to obtain guar gum acid solution with polysaccharide concentration of about 5 wt%.
(3) Acidolysis in an induction electric field: pumping the guar gum acid solution prepared in the step (2) into an induction electric field system, controlling the excitation condition to be about 150V of excitation voltage, about 400Hz of frequency, about 20 ℃ of constant temperature water bath temperature, treating for about 5.5h, and stirring at the speed of about 200 rpm.
(4) Neutralizing: and (3) neutralizing the reaction mixture finally obtained in the step (3) by using an NaOH solution with the concentration of about 8mol/L, adding the NaOH solution while stirring so as to uniformly neutralize the reaction mixture until the pH value reaches 7.0, and stopping adding the NaOH solution.
(5) And (3) precipitation: adding three times volume of ethanol into the reaction mixture treated in the step (4) for precipitation, performing suction filtration, and washing the filtrate with about 70% (v/v) ethanol until the eluate is free of chloride ions (by AgNO)3No white precipitate was detected from the solution).
(6) And (3) drying: and (5) spreading the filtered substance treated in the step (5) in a white porcelain plate, and drying in a freeze dryer.
(7) Screening: and (4) sieving powder with the fineness of about 100 meshes from the filtrate treated by the step (6), namely the prepared acidolysis guar gum, wherein the molecular weight distribution interval of the product is about 7000-8000 Da.
It should be understood that the above-mentioned embodiments are merely illustrative of the technical concepts and features of the present application, and are intended to enable those skilled in the art to understand the contents of the present application and implement the present application, and not to limit the scope of the present application. All equivalent changes and modifications made according to the spirit of the present application should be covered in the protection scope of the present application.
Claims (10)
1. A green preparation method of acidolysis polysaccharide is characterized by comprising the following steps: placing the polysaccharide acid solution in an induction electric field with the excitation voltage of 25-150V and the frequency of 400-700Hz for acidolysis treatment to prepare acidolysis polysaccharide; wherein the polysaccharide acid solution comprises a polysaccharide-based material and an inorganic acid.
2. The green process for producing acid-hydrolyzed polysaccharides as claimed in claim 1, wherein the process comprises:
mixing inorganic acid and water uniformly to form an inorganic acid solution with the concentration of 0.1-1.5 mol/L;
adding polysaccharide-based material into the inorganic acid solution and mixing uniformly to form polysaccharide acid solution, wherein the polysaccharide acid solution contains 0.5-5 wt% of polysaccharide-based material.
3. The green process for preparing acid-hydrolyzed polysaccharides of claim 1, wherein the process comprises: and (3) placing the polysaccharide acid solution in the induction electric field, and continuously stirring at a stirring speed of 200-300rpm until the acid hydrolysis treatment is completed.
4. The green process for producing acid-hydrolyzed polysaccharides according to claim 1 or 2, wherein: the polysaccharide-based material is selected from pure polysaccharide or agricultural and sideline products with polysaccharide as the main component.
5. The green process for producing acid-hydrolyzed polysaccharides according to claim 4, wherein: the polysaccharide comprises any one or more of guar gum and chitosan.
6. The green process for producing acid-hydrolyzed polysaccharides according to claim 2, wherein: the inorganic acid comprises any one or combination of hydrochloric acid, sulfuric acid and nitric acid.
7. The green process for producing acid-hydrolyzed polysaccharides according to claim 1 or 3, comprising: during the acidolysis treatment, the temperature of the polysaccharide acid solution is controlled to be 20-50 ℃, and the acidolysis treatment time is 4-6 h.
8. The green process for producing acid-hydrolyzed polysaccharides according to claim 1, wherein the process further comprises: after the acid hydrolysis treatment is completed, the obtained reaction mixture is subjected to post-treatment to obtain acid-hydrolyzed polysaccharide.
9. The green process for preparing acid-hydrolyzed polysaccharides of claim 8, wherein the post-treatment comprises: adjusting the pH value of the reaction mixture to 7 by using an alkaline substance, adding ethanol for precipitation, filtering, washing and drying to obtain the acidolysis polysaccharide.
10. The green process for preparing acid-hydrolyzed polysaccharides as claimed in claim 9, wherein the post-treatment comprises: and fully washing the filtered solid with 70 v/v% ethanol water solution until no chloride ions are separated out, freeze-drying, and sieving with a 100-mesh sieve to obtain the acid hydrolysis polysaccharide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210541173.9A CN114751999A (en) | 2022-05-17 | 2022-05-17 | Green preparation method of acidolysis polysaccharide |
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| CN202210541173.9A CN114751999A (en) | 2022-05-17 | 2022-05-17 | Green preparation method of acidolysis polysaccharide |
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| CN114751999A true CN114751999A (en) | 2022-07-15 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508790A (en) * | 2009-02-24 | 2009-08-19 | 华南理工大学 | Method for preparing low-molecular weight chitosan by using impulse electric field |
| CN102115501A (en) * | 2010-12-29 | 2011-07-06 | 哈尔滨商业大学 | Preparation method of acidolysis acetylated composite modified starch |
| CN107459585A (en) * | 2017-08-30 | 2017-12-12 | 华熙福瑞达生物医药有限公司 | A kind of production method of low molecule amount tremella polysaccharides |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508790A (en) * | 2009-02-24 | 2009-08-19 | 华南理工大学 | Method for preparing low-molecular weight chitosan by using impulse electric field |
| CN102115501A (en) * | 2010-12-29 | 2011-07-06 | 哈尔滨商业大学 | Preparation method of acidolysis acetylated composite modified starch |
| CN107459585A (en) * | 2017-08-30 | 2017-12-12 | 华熙福瑞达生物医药有限公司 | A kind of production method of low molecule amount tremella polysaccharides |
Non-Patent Citations (1)
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| 李丹丹: "感应电场辅助多糖酸解及其作用机制探究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
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