CN110684129A - Sodium alginate green preparation method based on choline eutectic solvent - Google Patents
Sodium alginate green preparation method based on choline eutectic solvent Download PDFInfo
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- CN110684129A CN110684129A CN201910850548.8A CN201910850548A CN110684129A CN 110684129 A CN110684129 A CN 110684129A CN 201910850548 A CN201910850548 A CN 201910850548A CN 110684129 A CN110684129 A CN 110684129A
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- 239000002904 solvent Substances 0.000 title claims abstract description 64
- 230000005496 eutectics Effects 0.000 title claims abstract description 56
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 235000010413 sodium alginate Nutrition 0.000 title claims abstract description 30
- 239000000661 sodium alginate Substances 0.000 title claims abstract description 30
- 229940005550 sodium alginate Drugs 0.000 title claims abstract description 30
- 229960001231 choline Drugs 0.000 title claims abstract description 13
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000000843 powder Substances 0.000 claims abstract description 47
- 239000002244 precipitate Substances 0.000 claims abstract description 29
- 241000512259 Ascophyllum nodosum Species 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 15
- 241001474374 Blennius Species 0.000 claims abstract description 14
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 239000000047 product Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 3
- 238000007873 sieving Methods 0.000 claims abstract description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 62
- 239000006228 supernatant Substances 0.000 claims description 43
- 239000011780 sodium chloride Substances 0.000 claims description 31
- HMBHAQMOBKLWRX-UHFFFAOYSA-N 2,3-dihydro-1,4-benzodioxine-3-carboxylic acid Chemical compound C1=CC=C2OC(C(=O)O)COC2=C1 HMBHAQMOBKLWRX-UHFFFAOYSA-N 0.000 claims description 18
- 229940075419 choline hydroxide Drugs 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims description 14
- 238000002390 rotary evaporation Methods 0.000 claims description 14
- 239000000126 substance Substances 0.000 claims description 14
- KWIUHFFTVRNATP-UHFFFAOYSA-N Betaine Natural products C[N+](C)(C)CC([O-])=O KWIUHFFTVRNATP-UHFFFAOYSA-N 0.000 claims description 11
- 238000000643 oven drying Methods 0.000 claims description 10
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 6
- 235000019743 Choline chloride Nutrition 0.000 claims description 6
- 229960003237 betaine Drugs 0.000 claims description 6
- 229960003178 choline chloride Drugs 0.000 claims description 6
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 241000195474 Sargassum Species 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- KWIUHFFTVRNATP-UHFFFAOYSA-O N,N,N-trimethylglycinium Chemical compound C[N+](C)(C)CC(O)=O KWIUHFFTVRNATP-UHFFFAOYSA-O 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 4
- 238000001556 precipitation Methods 0.000 abstract description 2
- 239000002028 Biomass Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 238000000926 separation method Methods 0.000 description 12
- 238000003756 stirring Methods 0.000 description 12
- 238000005303 weighing Methods 0.000 description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000029087 digestion Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 230000020477 pH reduction Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 241000195493 Cryptophyta Species 0.000 description 1
- 241000199919 Phaeophyceae Species 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001079 digestive effect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- -1 polysaccharide salts Chemical class 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
- C08B37/0084—Guluromannuronans, e.g. alginic acid, i.e. D-mannuronic acid and D-guluronic acid units linked with alternating alpha- and beta-1,4-glycosidic bonds; Derivatives thereof, e.g. alginates
-
- 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
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Sustainable Development (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention provides a choline eutectic solvent-based green preparation method of sodium alginate, which belongs to the field of marine biomass extraction and specifically comprises the following steps of drying, crushing and sieving kelp or seaweed to obtain kelp powder or seaweed powder, mixing the kelp powder or seaweed powder with a choline eutectic solvent aqueous solution, heating at 100-130 ℃ for 1-5 hours, adding ethanol for precipitation, washing the precipitate with ethanol, and drying to obtain white powder, namely a sodium alginate product. The invention provides a simple, green and efficient preparation method of sodium alginate. Meanwhile, the choline eutectic solvent used is degradable, can be recycled and has low cost.
Description
Technical Field
The invention belongs to the technical field of marine biological resource extraction, and relates to green preparation of sodium alginate based on choline eutectic solvent.
Background
Sodium alginate is mainly derived from natural polysaccharide salts of algae of Phaeophyta such as kelp, kelp and gulfweed, has good biocompatibility, hygroscopicity and adsorbability, and can be widely applied to the fields of medicine, food, water treatment and the like.
At present, the traditional methods for preparing sodium alginate mainly comprise a calcium coagulation acidification method, an acid coagulation acidification method, a calcium coagulation ion exchange method, an enzymolysis method and the like. These methods all involve pretreatment, digestion and product purification of kelp or seaweed. Wherein, the pretreatment is usually carried out by methanol, hydrochloric acid, cellulose and the like, and is used for destroying the cell wall of the kelp or seaweed and improving the extraction rate of the sodium alginate. The digestion is usually carried out by adopting a sodium carbonate aqueous solution, and the concentration, the digestion time and the digestion temperature of the sodium carbonate aqueous solution all influence the extraction rate of the sodium alginate. The product purification is carried out by solidifying digestive juice with acid or calcium salt, ion exchanging for decalcifying with hydrochloric acid or sodium chloride solution, dissolving sodium carbonate, filtering to obtain supernatant, adding ethanol for precipitation, and oven drying to obtain sodium alginate. The acid-base solution, organic reagent and the like used in the methods have great pollution to the environment, and the preparation process is long and the water consumption is large.
Disclosure of Invention
The invention aims to provide a choline eutectic solvent-based green preparation method of sodium alginate, which is realized by the following steps:
a sodium alginate green preparation method based on choline eutectic solvent specifically comprises the following steps; drying herba Zosterae Marinae or Sargassum, pulverizing, and sieving to obtain herba Zosterae Marinae powder or Sargassum powder; mixing kelp powder or seaweed powder with choline eutectic solvent aqueous solution, heating for reaction, and centrifuging to obtain insoluble substance and supernatant; adding absolute ethyl alcohol into the supernatant to obtain a precipitate; washing the precipitate with ethanol, and oven drying to obtain white powder, which is sodium alginate product; and removing the ethanol in the supernatant by using a rotary evaporation method to obtain the eutectic solvent for recycling.
Preferably, the kelp powder or the seaweed powder has the particle size of 60-120 meshes.
Preferably, it is characterized in that said choline-based eutectic solvent is one of the following: the low-melting-point solvent comprises a choline hydroxide/sodium chloride low-melting-point solvent with a molar ratio of 1: 0.5-1: 2, a choline chloride/sodium chloride low-melting-point solvent with a molar ratio of 1: 0.5-1: 2, and a betaine/sodium chloride low-melting-point solvent with a molar ratio of 1: 0.5-1: 2.
Preferably, the eutectic solvent aqueous solution is characterized by comprising 10-30% of the eutectic solvent aqueous solution by mass.
Preferably, the kelp powder or the seaweed powder is mixed with the eutectic solvent solution according to the mass ratio of 1: 20-1: 100.
Preferably, the method is characterized in that the reaction temperature is 80-130 ℃, and the reaction time is 1-24 h.
Preferably, the sodium alginate product with the purity of 90-99% can be obtained.
Detailed Description
The technical solutions of the present invention are further illustrated by the following specific embodiments, but the present invention is not limited to these examples.
Example 1:
weighing 0.5g of kelp powder with the particle size of 60 meshes, mixing with 10g of 10% choline hydroxide/sodium chloride eutectic solvent (1:0.5, n: n) water solution, stirring at 80 ℃ for 24 hours after uniform mixing, and performing centrifugal separation to obtain insoluble substances and supernatant; adding anhydrous ethanol into the supernatant to obtain precipitate, washing the precipitate with anhydrous ethanol until no eutectic solvent remains, and oven drying to obtain white powder, i.e. sodium alginate, with purity of 90%; and removing absolute ethyl alcohol in the supernatant by rotary evaporation to obtain the choline hydroxide/sodium chloride eutectic solvent.
Example 2:
weighing 0.5g of kelp powder with the particle size of 120 meshes, mixing with 10g of 10% choline hydroxide/sodium chloride eutectic solvent (1:0.5, n: n) water solution, stirring for 24 hours at 80 ℃, and performing centrifugal separation to obtain insoluble substances and supernatant; adding anhydrous ethanol into the supernatant to obtain precipitate, washing the precipitate with anhydrous ethanol until no eutectic solvent remains, and oven drying to obtain white powder, i.e. sodium alginate, with purity of 90%; and removing absolute ethyl alcohol in the supernatant by rotary evaporation to obtain the choline hydroxide/sodium chloride eutectic solvent.
Example 3:
weighing 0.5g of kelp powder with the particle size of 120 meshes, mixing with 10g of 10% choline hydroxide/sodium chloride eutectic solvent (1:2, n: n) water solution, stirring for 24 hours at 80 ℃, and performing centrifugal separation to obtain insoluble substances and supernatant; adding absolute ethyl alcohol into the supernatant to obtain a precipitate, washing the precipitate with absolute ethyl alcohol until no eutectic solvent remains, and drying to obtain white powder, namely sodium alginate with the purity of 93%; and removing absolute ethyl alcohol in the supernatant by rotary evaporation to obtain the choline hydroxide/sodium chloride eutectic solvent.
Example 4:
weighing 0.5g of kelp powder with the particle size of 120 meshes, mixing with 50g of 10% choline hydroxide/sodium chloride eutectic solvent (1:2, n: n) water solution, stirring for 24 hours at 80 ℃, and performing centrifugal separation to obtain insoluble substances and supernatant; adding anhydrous ethanol into the supernatant to obtain precipitate, washing the precipitate with anhydrous ethanol until no eutectic solvent remains, and oven drying to obtain white powder, i.e. sodium alginate, with purity of 95%; and removing absolute ethyl alcohol in the supernatant by rotary evaporation to obtain the choline hydroxide/sodium chloride eutectic solvent.
Example 5:
weighing 0.5g of kelp powder with the particle size of 120 meshes, mixing with 50g of 30% choline hydroxide/sodium chloride eutectic solvent (1:2, n: n) water solution, stirring for 24 hours at 80 ℃, and performing centrifugal separation to obtain insoluble substances and supernatant; adding absolute ethyl alcohol into the supernatant to obtain a precipitate, washing the precipitate with absolute ethyl alcohol until no eutectic solvent remains, and drying to obtain white powder, namely sodium alginate with the purity of 97%; and removing absolute ethyl alcohol in the supernatant by rotary evaporation to obtain the choline hydroxide/sodium chloride eutectic solvent.
Example 6:
weighing 0.5g of kelp powder with the particle size of 120 meshes, mixing with 50g of 30% choline hydroxide/sodium chloride eutectic solvent (1:2, n: n) water solution, uniformly mixing, stirring for 1 hour at 130 ℃, and performing centrifugal separation to obtain insoluble substances and a supernatant; adding anhydrous ethanol into the supernatant to obtain precipitate, washing the precipitate with anhydrous ethanol until no eutectic solvent remains, and oven drying to obtain white powder, i.e. sodium alginate, with purity of 95%; and removing absolute ethyl alcohol in the supernatant by rotary evaporation to obtain the choline hydroxide/sodium chloride eutectic solvent.
Example 7:
weighing 0.5g of kelp powder with the particle size of 120 meshes, mixing with 50g of 30% choline hydroxide/sodium chloride eutectic solvent (1:2, n: n) water solution, uniformly mixing, stirring for 24 hours at 130 ℃, and performing centrifugal separation to obtain insoluble substances and a supernatant; adding absolute ethyl alcohol into the supernatant to obtain a precipitate, washing the precipitate with absolute ethyl alcohol until no eutectic solvent remains, and drying to obtain white powder, namely sodium alginate with the purity of 99%; and removing absolute ethyl alcohol in the supernatant by rotary evaporation to obtain the choline hydroxide/sodium chloride eutectic solvent.
Example 8:
weighing 0.5g of kelp powder with the particle size of 120 meshes, mixing with 50g of 30% choline chloride/sodium chloride eutectic solvent (1:2, n: n) water solution, uniformly mixing, stirring for 24 hours at 130 ℃, and performing centrifugal separation to obtain insoluble substances and a supernatant; adding absolute ethyl alcohol into the supernatant to obtain a precipitate, washing the precipitate with absolute ethyl alcohol until no eutectic solvent remains, and drying to obtain white powder, namely sodium alginate with the purity of 93%; and removing absolute ethyl alcohol in the supernatant by rotary evaporation to obtain the choline chloride/sodium chloride eutectic solvent.
Example 9:
weighing 0.5g of kelp powder with the particle size of 120 meshes, mixing with 50g of 30% betaine/sodium chloride eutectic solvent (1:2, n: n) water solution, uniformly mixing, stirring for 24 hours at 130 ℃, and performing centrifugal separation to obtain insoluble substances and a supernatant; adding absolute ethyl alcohol into the supernatant to obtain a precipitate, washing the precipitate with absolute ethyl alcohol until no eutectic solvent remains, and drying to obtain white powder, namely sodium alginate with the purity of 97%; and removing absolute ethyl alcohol in the supernatant by rotary evaporation to obtain the betaine/sodium chloride eutectic solvent.
Example 10:
weighing 0.5g of seaweed powder with the particle size of 120 meshes, mixing with 50g of 30% betaine/sodium chloride eutectic solvent (1:2, n: n) water solution, stirring for 24 hours at 130 ℃, and performing centrifugal separation to obtain insoluble substances and supernatant; adding anhydrous ethanol into the supernatant to obtain precipitate, washing the precipitate with anhydrous ethanol until no eutectic solvent remains, and oven drying to obtain white powder, i.e. sodium alginate, with purity of 92%; and removing absolute ethyl alcohol in the supernatant by rotary evaporation to obtain the betaine/sodium chloride eutectic solvent.
Example 11:
weighing 0.5g of seaweed powder with the particle size of 120 meshes, mixing with 50g of 30% choline hydroxide/sodium chloride eutectic solvent (1:2, n: n) water solution, uniformly mixing, stirring for 24 hours at 130 ℃, and performing centrifugal separation to obtain insoluble substances and a supernatant; adding anhydrous ethanol into the supernatant to obtain precipitate, washing the precipitate with anhydrous ethanol until no eutectic solvent remains, and oven drying to obtain white powder, i.e. sodium alginate, with purity of 95%; and removing absolute ethyl alcohol in the supernatant by rotary evaporation to obtain the choline hydroxide/sodium chloride eutectic solvent.
Example 12:
weighing 0.5g of seaweed powder with the particle size of 120 meshes, mixing with 50g of 30% choline chloride/sodium chloride eutectic solvent (1:2, n: n) water solution, stirring for 24 hours at 130 ℃, and performing centrifugal separation to obtain insoluble substances and supernatant; adding anhydrous ethanol into the supernatant to obtain precipitate, washing the precipitate with anhydrous ethanol until no eutectic solvent remains, and oven drying to obtain white powder, i.e. sodium alginate, with purity of 91%; and removing absolute ethyl alcohol in the supernatant by rotary evaporation to obtain the choline chloride/sodium chloride eutectic solvent.
Claims (7)
1. A sodium alginate green preparation method based on choline eutectic solvent specifically comprises the following steps; drying herba Zosterae Marinae or Sargassum, pulverizing, and sieving to obtain herba Zosterae Marinae powder or Sargassum powder; mixing kelp powder or seaweed powder with choline eutectic solvent aqueous solution, heating for reaction, and centrifuging to obtain insoluble substance and supernatant; adding absolute ethyl alcohol into the supernatant to obtain a precipitate; washing the precipitate with ethanol, and oven drying to obtain white powder, which is sodium alginate product; and removing the ethanol in the supernatant by using a rotary evaporation method to obtain the eutectic solvent for recycling.
2. The method according to claim 1, wherein the particle size of the kelp powder or the seaweed powder is 60 to 120 mesh.
3. The method according to claim 1, wherein the choline eutectic solvent is one of the following: the low-melting-point solvent comprises a choline hydroxide/sodium chloride low-melting-point solvent with a molar ratio of 1: 0.5-1: 2, a choline chloride/sodium chloride low-melting-point solvent with a molar ratio of 1: 0.5-1: 2, and a betaine/sodium chloride low-melting-point solvent with a molar ratio of 1: 0.5-1: 2.
4. The method according to claim 1, wherein the mass fraction of the eutectic solvent aqueous solution is 10 to 30%.
5. The method according to claim 1, wherein the mass ratio of the kelp powder or the seaweed powder to the eutectic solvent aqueous solution is 1:20 to 1: 100.
6. The method according to claim 1, wherein the reaction temperature is 80 to 130 ℃ and the reaction time is 1 to 24 hours.
7. The method of claim 1, wherein the sodium alginate product with purity of 90-99% can be obtained.
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| CN114014947A (en) * | 2022-01-10 | 2022-02-08 | 菏泽高新区优科生物科技有限公司 | Eutectic solvent for degrading algal polysaccharide and preparation method and application thereof |
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| CN113735802A (en) * | 2021-10-12 | 2021-12-03 | 自然资源部第三海洋研究所 | A method for preparing fucoxanthin extract with eutectic solvent |
| CN114014947A (en) * | 2022-01-10 | 2022-02-08 | 菏泽高新区优科生物科技有限公司 | Eutectic solvent for degrading algal polysaccharide and preparation method and application thereof |
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