CN115975072A - Redispersible nano chitin and preparation method thereof - Google Patents
Redispersible nano chitin and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000006185 dispersion Substances 0.000 claims abstract description 37
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007864 aqueous solution Substances 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 15
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 14
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000007810 chemical reaction solvent Substances 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 8
- 239000002612 dispersion medium Substances 0.000 claims abstract description 7
- 238000007865 diluting Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 8
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 claims description 7
- 229940106681 chloroacetic acid Drugs 0.000 claims description 7
- OVYTZAASVAZITK-UHFFFAOYSA-M sodium;ethanol;hydroxide Chemical compound [OH-].[Na+].CCO OVYTZAASVAZITK-UHFFFAOYSA-M 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
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- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- GAWAYYRQGQZKCR-UHFFFAOYSA-N 2-chloropropionic acid Chemical compound CC(Cl)C(O)=O GAWAYYRQGQZKCR-UHFFFAOYSA-N 0.000 claims description 4
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 4
- QEYMMOKECZBKAC-UHFFFAOYSA-N 3-chloropropanoic acid Chemical compound OC(=O)CCCl QEYMMOKECZBKAC-UHFFFAOYSA-N 0.000 claims description 3
- 241000238366 Cephalopoda Species 0.000 claims description 3
- 241000238424 Crustacea Species 0.000 claims description 3
- 210000000988 bone and bone Anatomy 0.000 claims description 3
- 210000002421 cell wall Anatomy 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 230000002538 fungal effect Effects 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- FDRCDNZGSXJAFP-UHFFFAOYSA-M sodium chloroacetate Chemical compound [Na+].[O-]C(=O)CCl FDRCDNZGSXJAFP-UHFFFAOYSA-M 0.000 claims description 2
- 239000008367 deionised water Substances 0.000 abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 abstract description 9
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 5
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- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 4
- 241000238557 Decapoda Species 0.000 description 3
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 3
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Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention provides a re-dispersible nano chitin and a preparation method thereof, belonging to the technical field of preparation of chitin nano materials. The method comprises the steps of pretreating chitin powder, adding the pretreated chitin powder into a reaction solvent for alkalization, adding a carboxymethylation reaction reagent for carboxymethylation reaction, diluting with an ethanol aqueous solution to terminate the reaction, removing substances except chitin and water, performing ultrasonic treatment to obtain a nano chitin aqueous dispersion, and drying to remove a dispersion medium to obtain the re-dispersible nano chitin. The carboxyl content of the re-dispersible nano chitin prepared by the method is 10-40%, the re-dispersible nano chitin can be stably dispersed for more than two months within the pH value range of 3-11, the dispersion concentration in deionized water is up to 20mg/ml, the transportation cost of chitin products can be greatly reduced, and the method is very favorable for commercial application.
Description
Technical Field
The invention belongs to the technical field of preparation of chitin nano materials, and particularly relates to re-dispersible nano chitin and a preparation method thereof.
Background
In nature, chitin is widely present in shells of crustaceans such as lower plant fungi, shrimps, crabs and insects, and cell walls of fungi, and is the second largest natural biopolymer with the second best storage amount than cellulose. Chitin is odorless and tasteless, and is insoluble in water, dilute acid, alkali, ethanol or other organic solvents. The nano chitin inherits various excellent properties of the chitin, has high specific surface area, crystallinity and modulus, and is regarded as natural polymer fiber with excellent comprehensive performance for a long time. Compared with common inorganic nano materials, the nano chitin has the characteristics of reproducibility, wide sources, low energy consumption, low cost and the like, and the surface of the nano chitin has functional groups with certain reactivity and can participate in grafting reaction.
However, chitin is a highly crystalline polysaccharide, and has strong intramolecular and intermolecular hydrogen bond interactions, and thus it is difficult to produce chitin into a state of nanofibers or nanocrystals by a simple method. The existing technology for preparing the nano chitin is mainly to extract and separate the nano chitin from shrimp and crab shells by a mechanical method, a chemical method, an enzymatic hydrolysis method, a dissolution regeneration method and the like, and the obtained nano chitin is easy to form strong hydrogen bonds during drying, so that nano fibers are mutually entangled and are difficult to be redispersed into a nano-size state. Therefore, the redispersion effect of the nano chitin prepared by the method is not ideal. You et al extracted redispersible chitin nanofibrils (chem. Eng.j.2018,344, 498) from crab shells by deprotonation assisted liquid phase stripping using DMSO/KOH "pseudo-solvent", unfortunately, this method produced nanofibrils at low concentrations, only up to 0.5mg/mL, which greatly limited their commercial application.
At present, the nano chitin generally exists in a water phase form in the preparation and transportation processes, so the storage and transportation cost of the nano chitin is greatly increased. Therefore, the development of the re-dispersible nano chitin is particularly important.
Disclosure of Invention
In order to solve the technical problems, the invention provides a re-dispersible nano chitin and a preparation method thereof. The method comprises the steps of pretreating chitin powder, adding the pretreated chitin powder into a reaction solvent for alkalization, adding a carboxymethylation reaction reagent for carboxymethylation reaction, diluting with an ethanol aqueous solution to terminate the reaction, removing substances except chitin and water, performing ultrasonic treatment to obtain a nano chitin aqueous dispersion, and drying to remove a dispersion medium to obtain the re-dispersible nano chitin. The carboxyl content of the re-dispersible nano chitin prepared by the method is 10-40%, the re-dispersible nano chitin can be stably dispersed for more than two months within the pH value range of 3-11, the dispersion concentration in deionized water is up to 20mg/ml, the transportation cost of chitin products can be greatly reduced, and the method is very favorable for commercial application.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of re-dispersible nano chitin, which comprises the following steps: (1) Mixing chitin powder and NaOH ethanol aqueous solution, heating, filtering to remove alkali, washing with water to neutrality, and drying to obtain pretreated chitin; (2) Adding pretreated chitin into a reaction solvent, performing alkalization treatment by using a NaOH aqueous solution, then adding a carboxymethylation reaction reagent for carboxymethylation reaction, then diluting by using an ethanol aqueous solution to terminate the reaction, removing substances except the chitin and water, and performing ultrasonic treatment to obtain a nano chitin aqueous dispersion; (3) Drying the obtained nano chitin water dispersion liquid to remove a dispersion medium to obtain the re-dispersible nano chitin.
Preferably, the concentration of NaOH in the NaOH ethanol water solution in the step (1) is 10-30 wt%, and the concentration of ethanol is 1-20 wt%; the concentration of the chitin powder is 1-20 wt% after the chitin powder is mixed with NaOH ethanol aqueous solution; the temperature of the heating treatment is 55-65 ℃, and the time is 4.5-5.5 h; the deacetylation degree of the obtained pretreated chitin is 2-20%.
The pretreatment method can be used for pretreating chitin to introduce amino, and the amino can be ionized to provide positive charge under an acidic condition, so that the nano chitin can be stably dispersed under the acidic condition.
Preferably, the reaction solvent in the step (2) is one or more of water and isopropanol, acetone, dimethyl ether and tert-butyl alcohol; the mass fraction of the NaOH aqueous solution is 2-20 wt%, and the dosage is 0.5-5 ml; the temperature of the alkalization treatment is 45-55 ℃, and the time is 0.5-1.5 h.
Preferably, the carboxymethylation reaction reagent in the step (2) is any one or more of chloroacetic acid, sodium chloroacetate, 2-chloropropionic acid and 3-chloropropionic acid; the concentration of the chitin is 0.1-5 wt% during the carboxymethylation reaction; the temperature of the carboxymethylation reaction is 45-55 ℃, and the time is 3.5-4.5 h.
The carboxymethylation reaction reagent may be used in the form of a mixed solution in which the reagent is dissolved in a reaction solvent, in addition to 2-chloropropionic acid.
Preferably, the concentration of ethanol in the ethanol aqueous solution used for terminating the reaction in the step (2) is 10 to 90wt%.
Preferably, the power of the ultrasonic treatment in the step (2) is 100-800 w, and the time is 1-10 min.
Preferably, the reaction solvent used in the alkalization treatment in the step (2) is water and isopropanol, and the volume ratio of the water to the isopropanol is 1:1 to 1:10, the mass fraction of NaOH aqueous solution is 5-15%; the carboxymethylation reaction reagent is a mixed solution of chloroacetic acid and isopropanol, and the mass volume ratio of the two is 1:1 to 1:10.
preferably, the preparation raw material of the redispersible nano chitin is any one or more of fungal cell walls, shells of crustaceans and squid bones.
The invention also provides the re-dispersible nano chitin prepared by the preparation method.
The carboxyl content of the redispersible nano chitin is 10-40%, the redispersible nano chitin can be stably dispersed in the pH value range of 3-11, and the dispersion concentration in deionized water is up to 20mg/ml.
The redispersible nano chitin can be redispersed by adding into water through a simple ultrasonic treatment mode to obtain the chitin water dispersion, and the nano size can be still maintained. The method can obviously reduce the transportation cost of the liquid nano chitin, greatly improve the practicability of the liquid nano chitin in the fields of chemistry, chemical industry, agriculture and environmental engineering, and has higher commercial value.
Compared with the prior art, the invention has the following technical effects:
(1) The nano chitin prepared by the invention has redispersibility. The chitin in the invention is treated by concentrated alkali and carboxymethylation reagent, so that the hydrogen bond effect in molecules and among molecules is greatly weakened, the nano chitin aqueous dispersion in the invention can be redispersed in water after being dried, and the dispersible concentration in deionized water reaches 20mg/ml, thus obviously reducing the transportation cost of the liquid nano chitin and widening the application range of the nano chitin.
(2) The nano chitin prepared by the invention has wider pH tolerance. The invention uses NaOH ethanol water solution to pretreat chitin to introduce amino, then uses carboxymethylation reagent to treat the chitin to introduce carboxyl, thereby obtaining the nano chitin with amino and carboxyl and acid-base amphiprotic property, the nano chitin can be dispersed in a wider pH range of-3-11, and can be stably dispersed for more than two months under acidic condition and alkaline condition.
Detailed Description
The following examples are intended to illustrate the invention, but are not intended to limit the scope of the invention. It is intended that all modifications or alterations to the methods, procedures or conditions of the present invention be made without departing from the spirit or essential characteristics thereof.
The technical solution of the present invention is further illustrated in detail by the following examples.
Example 1
(1) Preparing 500ml of NaOH ethanol water solution, wherein the concentration of NaOH is 20wt%, the concentration of ethanol is 10wt%, adding 20g of purified crab shell powder (after being crushed, the crab shell powder is sieved by a 40-mesh sieve), and heating and stirring for 5 hours at the temperature of 60 ℃. Filtering alkali, washing with deionized water to neutrality, and drying to obtain pretreated chitin. The deacetylation degree of the obtained pretreated chitin was 12%. Wherein the purification of the crab shell powder means that protein, pigment and some impurities need to be removed after the crab shell is ground, and a common purification method in the field can be used.
(2) 10g of pretreated chitin was added to 100ml of a mixed solution of water and isopropanol mixed at a volume ratio of 1.
(3) Dissolving 15g of chloroacetic acid in 20ml of isopropanol, slowly and dropwise adding the solution into the chitin alkalization solution, keeping the reaction temperature for reacting for 4 hours, and then adding an ethanol water solution with the ethanol concentration of 70wt% for diluting to stop the reaction. Washing out substances except chitin and water in the obtained crude product by using ultrapure water, performing ultrasonic treatment for 5min under 500W ultrasonic power to obtain nano chitin water dispersion, and drying to remove a dispersion medium to obtain the nano chitin.
When the ultrasonic power of the obtained nano chitin is 100-800 w, the stable nano chitin aqueous dispersion can be prepared only by regulating and controlling the ultrasonic time. The obtained nano chitin can be completely dispersed in deionized water after ultrasonic treatment, and the dispersed nano chitin aqueous dispersion can be stably dispersed for more than two months in the range of pH 3-11, wherein the dispersion concentration of the chitin can also reach 20mg/ml.
Example 2
The material types and the process flow are the same as example 1, except that the pretreated chitin powder in the step (2) is alkalized in a mixed solution of water, isopropanol and NaOH at the water bath temperature of 50 ℃ for 1h, 15g of 2-chloropropionic acid is dissolved in 20ml of isopropanol in the step (3) to carry out carboxymethylation reaction, and other treatment conditions are kept unchanged.
The properties of the obtained nano chitin and the state of the aqueous dispersion prepared from the nano chitin are both close to those of the embodiment 1, wherein the dispersion concentration of the chitin can reach 16mg/ml.
Example 3
The material types and the process flow are the same as example 1, except that 15g of 3-chloropropionic acid is dissolved in 20ml of isopropanol in step (3), carboxymethylation reaction is continued, and other treatment conditions are kept unchanged.
The properties of the obtained nano chitin and the state of the aqueous dispersion prepared from the nano chitin are both close to those of the embodiment 1, wherein the dispersion concentration of the chitin can reach 15mg/ml.
Example 4
The process flow is the same as example 1, except that the chitin raw material is crawfish shell.
The deacetylation degree of the obtained pretreated chitin was 10%. The properties of the obtained nano chitin and the state of the aqueous dispersion prepared from the nano chitin are both close to those of the embodiment 1, wherein the dispersion concentration of the chitin can reach 18mg/ml.
Example 5
The process flow is the same as that of example 1, except that the chitin is squid bone.
The deacetylation degree of the obtained pretreated chitin was 15%. The properties of the obtained nano chitin and the state of the aqueous dispersion prepared from the nano chitin are both close to those of the embodiment 1, wherein the dispersion concentration of the chitin can reach 10mg/ml.
Comparative example 1
(1) 10g of purified crab shell powder was directly added to 100ml of a mixed solution of water and isopropyl alcohol mixed in a volume ratio of 1.
(2) Dissolving 15g of chloroacetic acid in 20ml of isopropanol, slowly and dropwise adding the solution into the chitin alkalization solution, keeping the reaction temperature for reaction for 4 hours, and then adding an ethanol water solution with the ethanol concentration of 70wt% to terminate the reaction. And washing out substances except chitin and water in the obtained crude product by using ultrapure water, setting different ultrasonic treatment powers and treatment times, and adjusting the pH value of the dispersion liquid for treatment.
The dispersion liquid obtained after treatment can be flocculated, so that a stably dispersible chitin nano-fiber water dispersion liquid can not be obtained, and the solid obtained after drying and removing a dispersion medium can not be dispersed in deionized water after ultrasonic treatment.
Comparative example 2
The material type and process flow were the same as in comparative example 1, except that the carboxymethylation time was extended to 10h.
The same as comparative example 1, no matter what ultrasonic power and ultrasonic treatment time are selected, no matter how the pH value of the dispersion is adjusted, the obtained dispersion after treatment is flocculated, and the chitin nanofiber aqueous dispersion with good dispersibility cannot be obtained, or the dispersion cannot be dispersed in deionized water.
Comparative example 3
The material types and process flow were the same as in comparative example 1, except that the alkalization time was extended to 4 hours.
The same as in comparative example 1, no matter what ultrasonic power and ultrasonic treatment time were set, no matter how the pH of the dispersion was adjusted, the dispersion obtained after the treatment was flocculated, and a stably dispersible aqueous dispersion of chitin nanofibers could not be obtained, and the solid obtained after removal of the dispersion medium was subjected to ultrasonic treatment and pH adjustment, and could not be dispersed in deionized water.
Comparative example 4
The kind of material and the process flow were the same as in comparative example 1, except that the amount of NaOH used in the alkalization was adjusted to 4 times the amount used in example 1, and the other conditions were kept unchanged.
As a result, after adjusting the ultrasonic power, the ultrasonic time and the pH of the aqueous dispersion, the state of the aqueous dispersion obtained was the same as that of comparative example 1.
Comparative example 5
The material types and the process flow are the same as those of comparative example 1, except that the amount of chloroacetic acid used in carboxymethylation is adjusted to 4 times the amount used in example 1, and other conditions are kept unchanged.
After adjusting the ultrasonic power, ultrasonic time and pH of the dispersion, the state of the resulting aqueous dispersion was the same as that of comparative example 1.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (9)
1. A preparation method of re-dispersible nano chitin is characterized by comprising the following steps:
(1) Mixing chitin powder and NaOH ethanol aqueous solution, heating, filtering to remove alkali, washing with water to neutrality, and drying to obtain pretreated chitin;
(2) Adding pretreated chitin into a reaction solvent, performing alkalization treatment by using a NaOH aqueous solution, then adding a carboxymethylation reaction reagent for carboxymethylation reaction, then diluting by using an ethanol aqueous solution to terminate the reaction, removing substances except the chitin and water, and performing ultrasonic treatment to obtain a nano chitin aqueous dispersion;
(3) Drying the obtained nano chitin water dispersion liquid to remove a dispersion medium to obtain the re-dispersible nano chitin.
2. The method according to claim 1, wherein the concentration of NaOH in the aqueous solution of NaOH in step (1) is 10 to 30wt%, and the concentration of ethanol is 1 to 20wt%; the concentration of the chitin powder is 1-20 wt% after the chitin powder is mixed with NaOH ethanol aqueous solution; the temperature of the heating treatment is 55-65 ℃, and the time is 4.5-5.5 h; the deacetylation degree of the obtained pretreated chitin is 2-20%.
3. The method according to claim 2, wherein the reaction solvent in the step (2) is one or more of water and isopropyl alcohol, acetone, dimethyl ether, and t-butyl alcohol; the mass fraction of the NaOH aqueous solution is 2-20 wt%, and the dosage is 0.5-5 ml; the temperature of the alkalization treatment is 45-55 ℃, and the time is 0.5-1.5 h.
4. The preparation method according to claim 3, characterized in that the carboxymethylation reaction reagent in the step (2) is any one or more of chloroacetic acid, sodium chloroacetate, 2-chloropropionic acid and 3-chloropropionic acid; the concentration of the chitin is 0.1-5 wt% during the carboxymethylation reaction; the temperature of carboxymethylation reaction is 45-55 ℃, and the time is 3.5-4.5 h.
5. The method according to claim 4, wherein the concentration of ethanol in the aqueous ethanol solution used for terminating the reaction in the step (2) is 10 to 90wt%.
6. The preparation method according to claim 5, wherein the power of the ultrasonic treatment in the step (2) is 100-800 w, and the time is 1-10 min.
7. The method according to claim 6, wherein the reaction solvent used in the alkalization treatment in the step (2) is water and isopropyl alcohol at a volume ratio of 1:1 to 1:10, the mass fraction of NaOH aqueous solution is 5-15%; the carboxymethylation reaction reagent is a mixed solution of chloroacetic acid and isopropanol, and the mass volume ratio of the two is 1:1 to 1:10.
8. the method of claim 7, wherein the re-dispersible nano chitin is prepared from one or more of fungal cell wall, crustacean shell, and squid bone.
9. The re-dispersible nano chitin prepared by the preparation method of any one of claims 1-8.
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