CN102218301A - Chitosan cross-linked adsorbent preparation method - Google Patents
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 30
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000007787 solid Substances 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000001556 precipitation Methods 0.000 claims abstract description 8
- 235000019441 ethanol Nutrition 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims description 16
- ZLXPLDLEBORRPT-UHFFFAOYSA-M [NH4+].[Fe+].[O-]S([O-])(=O)=O Chemical compound [NH4+].[Fe+].[O-]S([O-])(=O)=O ZLXPLDLEBORRPT-UHFFFAOYSA-M 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000000247 postprecipitation Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 3
- 239000003153 chemical reaction reagent Substances 0.000 claims description 2
- 230000006196 deacetylation Effects 0.000 claims description 2
- 238000003381 deacetylation reaction Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 16
- 239000003814 drug Substances 0.000 abstract description 15
- 230000000694 effects Effects 0.000 abstract description 6
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- 229910052793 cadmium Inorganic materials 0.000 abstract description 5
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052802 copper Inorganic materials 0.000 abstract description 4
- 239000010949 copper Substances 0.000 abstract description 4
- 150000002500 ions Chemical class 0.000 abstract description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052753 mercury Inorganic materials 0.000 abstract description 3
- IMBKASBLAKCLEM-UHFFFAOYSA-L ferrous ammonium sulfate (anhydrous) Chemical compound [NH4+].[NH4+].[Fe+2].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O IMBKASBLAKCLEM-UHFFFAOYSA-L 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 229940010514 ammonium ferrous sulfate Drugs 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- FINHMKGKINIASC-UHFFFAOYSA-N Tetramethylpyrazine Chemical compound CC1=NC(C)=C(C)N=C1C FINHMKGKINIASC-UHFFFAOYSA-N 0.000 description 12
- 238000001179 sorption measurement Methods 0.000 description 11
- 238000004132 cross linking Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 6
- 239000004480 active ingredient Substances 0.000 description 6
- 241000196324 Embryophyta Species 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 241000112528 Ligusticum striatum Species 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- VRYALKFFQXWPIH-PBXRRBTRSA-N (3r,4s,5r)-3,4,5,6-tetrahydroxyhexanal Chemical group OC[C@@H](O)[C@@H](O)[C@H](O)CC=O VRYALKFFQXWPIH-PBXRRBTRSA-N 0.000 description 1
- MSWZFWKMSRAUBD-IVMDWMLBSA-N 2-amino-2-deoxy-D-glucopyranose Chemical compound N[C@H]1C(O)O[C@H](CO)[C@@H](O)[C@@H]1O MSWZFWKMSRAUBD-IVMDWMLBSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 235000004237 Crocus Nutrition 0.000 description 1
- 241000596148 Crocus Species 0.000 description 1
- 241000238557 Decapoda Species 0.000 description 1
- 229920002527 Glycogen Polymers 0.000 description 1
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- MSWZFWKMSRAUBD-UHFFFAOYSA-N beta-D-galactosamine Natural products NC1C(O)OC(CO)C(O)C1O MSWZFWKMSRAUBD-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 229910052956 cinnabar Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011790 ferrous sulphate Substances 0.000 description 1
- 235000003891 ferrous sulphate Nutrition 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 229960002442 glucosamine Drugs 0.000 description 1
- 229940096919 glycogen Drugs 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- RQKFOGXUTRDQPB-UHFFFAOYSA-N hydron;2,3,5,6-tetramethylpyrazine;chloride Chemical compound Cl.CC1=NC(C)=C(C)N=C1C RQKFOGXUTRDQPB-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 229910052957 realgar Inorganic materials 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229940032021 tetramune Drugs 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a chitosan cross-linked adsorbent preparation method, which comprises the steps as follows: firstly, ammonium ferrous sulfate solid is taken and dissolved into boiled de-ionized water; the pH value is adjusted to 2-3 by 1.0mol/L hydrochloric acid; secondarily, chitosan is added for stirring for reaction for 3h and then filtered; thirdly, absolute ethyl alcohol with equal size is added into a filtration liquid and stewed for 12h and then is filtered after product precipitation; and fourthly, 50 percent of ethanol in size is used for washing the product to obtain flaxen bulk solid and then is stewed into a 40-DEG C dry box for drying, thus obtaining the chitosan cross-linked adsorbent product. The novel cross-linked adsorbent manufactured by adopting the method has excellent absorption effects on heavy metals like lead, mercury, cadmium and copper during the Chinese medicine production process; moreover, the reservation effect of the effective Chinese medicine components is also very high. The chitosan cross-linked adsorbent preparation method has very important significances for improving Chinese medicine preparation quality and controlling heavy metal ion pollution.
Description
Technical field
The invention belongs to the shitosan applied technical field, more specifically, relate to a kind of preparation method of novel chitosan crosslinking adsorbent.
Background technology
The source of heavy metal mainly contains two kinds in the Chinese medicine: a kind of is to be purpose with the treatment, has added the mineral drug that contains heavy metal in prescription, as cinnabar and realgar etc.; The 2nd, by raw medicinal material bring into or in its processing, hide the exogenous pollution in storage, transportation and the preparation production process.These two kinds of sources have caused that content of beary metal exceeds standard in the Chinese medicine, become international community to one of focal issue of Chinese medicine safety concerns, have hindered the internationalization of tcm process.For OTC heavy metal pollution, should in addition strict control, to avoid heavy metal composition in the Chinese medicine to the damage of the health that weakens and medication person is caused of drug effect.Content of beary metal in the medicinal material is relevant with planting type, and content of beary metal is relevant with heavy metal in soil content in the medicinal herbs.For example plumbous very wide in distributed in nature, plant can absorb the lead of dissolved state in the soil by root, and the plant equipment of Chinese medicine processing, pipeline etc. also can contain lead.And the heavy metal of health toxicity mainly is distributed in kidney, spleen, lung, the brain, especially liver is the highest.
Present most of Chinese herbal product all needs to carry out the green authentication, " the green industry standard of medicinal plant and preparation foreign trade " of Department of Commerce's promulgation stipulated the foreign trade industry standard quality of medicinal plant and preparation, comprise medicinal plant raw material medicine materical crude slice, the requirement of limiting the quantity of of heavy metal in extract and the preparation.Concrete data such as table 1:
The requirement of limiting the quantity of of table 1 heavy metal
Shitosan (CTS) is the product of natural polymer de-acetyl chitin, claims chitosan again, is a kind of poly glucosamine linear polymeric material.Be generally white or pale yellow powder.Extensively be present in the shrimp and crab shells.In recent ten years, shitosan is in food industry, medicine, printing and dyeing, papermaking, immobilization material, and fields such as membrane material have obtained using widely, are one that research is comparatively concentrated in the current natural macromolecular material.It is the EVA of being made up of β-(1,4)-2-amino-2-deoxy-D-glucose unit and β-(1,4)-2-acetylaminohydroxyphenylarsonic acid 2-deoxy-D-glucose unit, and 2 of glycogen are-NHCOCH
3Or free-NH
2, 3 is the second month in a season-OH, 6 is primary-OH, can be by hydrogen bond and the similar cancellated cage type molecule of salt key travel, thereby shitosan has fabulous mating capability to many metal ions.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of novel chitosan crosslinking adsorbent, can be used for the absorption of heavy metal ion lead, mercury, cadmium, copper etc. in the Chinese medicine preparation, this preparation method relates to the preparation of different molecular weight shitosan and ferrous sulfate crosslinking adsorbent, to the absorption of heavy metal ion in the Chinese medicine preparation, can keep well Effective Components of Chinese Herb and useful metal ion simultaneously.
Technical scheme of the present invention is as follows:
A kind of chitosan crosslinked preparation of adsorbent method, the step of described method is:
A. get the iron ammonium sulfate solid, be dissolved in the deionized water that boiled, with hydrochloric acid adjust pH to 2 ~ 3 of 1.0mol/L;
B. stir after adding shitosan, filter behind the reaction 3h;
C. add isopyknic absolute ethyl alcohol in the filtrate, leave standstill 12h, treat that the product post precipitation filters;
D. use the product of 50 volume % ethanol washing precipitations, obtain flaxen blocks of solid, place 40 ℃ of drying boxes dry, promptly obtain chitosan crosslinked adsorbent product.
Aforesaid method, wherein, the ratio of described each raw material and reagent is: every 23.5g iron ammonium sulfate adds 0.5g shitosan and 250mL deionized water.
Aforesaid method, wherein, the deacetylation of described shitosan (DAG) between 85～95%, molecular weight between 12～130,000, particle diameter 80 orders.
Aforesaid method, wherein, it is pure that described iron ammonium sulfate, absolute ethyl alcohol and hydrochloric acid are top grade.
The chitosan crosslinked adsorbent that aforesaid method is made.
Beneficial effect of the present invention is:
Shitosan is a kind of natural cationic flocculant, and many materials are had the chelating suction-operated, and amino and hydroxyl and the many metal ion adjacent with amino in its molecule can form stable chelate.The novel chitosan crosslinking adsorbent that the present invention obtains all reaches more than 90% the adsorption efficiency of heavy metal lead, mercury, cadmium, copper, simultaneously in pharmaceutically active ingredient, can reach more than 70% as the retention rate of the ligustrazine in the Ligusticum wallichii.
The specific embodiment
Embodiment 1
Get iron ammonium sulfate 23.5g, be dissolved in the deionized water that 250mL boiled, put into the 500mL round-bottomed flask, with 1.0mol/L hydrochloric acid adjust pH to 2 ~ 3; Add shitosan (DAG 〉=85%, marine biotechnology Co., Ltd must be seen in the sea, Jinan) 0.5g, stir with agitator, filter behind the reaction 3h, add the equal-volume absolute ethyl alcohol in the filtrate and leave standstill 12h, treat that the product post precipitation filters, with the product of 50 volume % ethanol washing precipitations, obtain flaxen blocks of solid, place 40 ℃ of drying boxes dry.The yield of the crosslinking adsorbent that present embodiment makes is 73%.
Embodiment 2
Get iron ammonium sulfate 23.5g, be dissolved in the deionized water that 250mL boiled, put into the 500mL round-bottomed flask, with 1.0mol/L hydrochloric acid adjust pH to 2 ~ 3; Add shitosan (DAG 〉=92%, sea, Laizhou City, Shandong Lik-Sang Tetramune Co., Ltd) 0.5g, stir with agitator, filter behind the reaction 3h, filtrate adds the equal-volume absolute ethyl alcohol and leaves standstill 12h, treats that the product post precipitation filters, with the product of 50 volume % ethanol washing precipitations, obtain flaxen blocks of solid, place 40 ℃ of drying boxes dry.The yield of the crosslinking adsorbent that present embodiment makes is 85%.
Embodiment 3
Get iron ammonium sulfate 23.5g, be dissolved in the deionized water that 250mL boiled, put into the 500mL round-bottomed flask, transfer pH value to 2 ~ 3 with 1.0mol/L hydrochloric acid; Add shitosan (DAG 〉=90%, Jinan Haidebei Marine Organism Engineering Co., Ltd.) 0.5g, stir with agitator, filter behind the reaction 3h, filtrate adds the equal-volume absolute ethyl alcohol and leaves standstill 12h, treats that the product post precipitation filters, with the product of 50 volume % ethanol washing precipitations, obtain flaxen blocks of solid, place 40 ℃ of drying boxes dry.The yield of the crosslinking adsorbent that present embodiment makes is 76%.
The chitosan crosslinked adsorbent that adopts the inventive method to make, for heavy metal lead, cadmium, copper, the adsorbent consumption is that 0.36g, adsorption time are 120min, are optimum condition when temperature is 37 ℃ that its adsorption rate all can reach more than 90%; For active ingredient ligustrazine in the Ligusticum wallichii, above-mentioned condition can reach more than 84.8% the retention rate of ligustrazine.
The adsorption effect of the prepared chitosan crosslinked ABSORBENTS ABSORPTION metallic element palladium of the foregoing description 1-3, cadmium and centering pharmaceutically active ingredient ligustrazine is as shown in table 2.
Each embodiment of table 2 makes the adsorption effect of crosslinking adsorbent
| The adsorbent kind | Pb adsorption rate % | Cd adsorption rate % | Ligustrazine content |
| Embodiment 1(shitosan DAG85%) | 57.69 | 93.00 | 14.6224 |
| Embodiment 2(shitosan DAG92%) | 90.00 | 87.65 | 14.6633 |
| Embodiment 3(shitosan DAG90%) | 61.16 | 68.84 | 16.9286 |
| Do not add adsorbent | —— | —— | 17.2448 |
Comparative Examples 1
Take by weighing the 2.0g shitosan, be dissolved in 400 mL 5wt% acetic acid aqueous solutions, transfer pH to 2.5 with weak aqua ammonia, stir, with ultrasonic cleaning machine at 200 Hz, ultrasonic 5 min under 30 ℃, after making it become equal colloid, constant speed dropping initial concentration is the l ferrous ammonium sulfate solution of the hydrochloric azanol of 16mg/mL under the magnetic stirrer stirring, this moment, reaction system reached 800mL, and successive reaction 1h leaves standstill 10h then, centrifugal, (1:1 V:V) is precipitated out product, examines less than SO with barium chloride solution in cleaning solution with hydrous ethanol cyclic washing precipitation with acetone-ethanolic solution
4 2+, use the absolute ethanol washing post precipitation again, 40 ℃ of following oven dryings obtain crocus powder CTS-Fe (II) adsorbent to constant weight.
In boiling flask, CTS-Fe (II) is dissolved in the 33wt% NaOH solution of 30mL, stirs, at room temperature fully after the swelling being lower than under 4 ℃ the temperature more than the freezing 24h, make alkalization CTS-Fe (II).After taking-up was thawed, superfluous alkali lye was removed in extruding, added isopropyl alcohol, stirred 30 min under the room temperature.Add an amount of 10wt% tetramethyl ammonium hydroxide solution again, add the 20mL expoxy propane under the room temperature while stirring, stir 1h again.The constant temperature backflow adds thermal response 6h then, and cooling is filtered, and filter cake is dried the back for several times with washed with isopropyl alcohol.Add appropriate amount of deionized water, dissolving is at room temperature filtered, and filtrate transfers the pH value to neutrality with hydrochloric acid solution.Earlier separate out precipitation, use absolute ethanol washing again with a large amount of acetone.Under 60 ℃, be drying to obtain flaxen blocks of solid.This method building-up process complexity, the product crystallization is more tiny, and the yield of adsorbent is very low, only is 13.0-13.5%.
Comparative Examples 2
Get 20g flyash, add the shitosan of 1.6g, mix, add the acetic acid solution 12mL of 4wt% again, fully stir, be modulated into pasty state, make it moistening fully, make the granule that diameter is 1 ~ 3mm, be drying to obtain the CTS-acticarbon.This crosslinking adsorbent yield is more than 97%, yet its adsorption rate to heavy metal and middle pharmaceutically active ingredient is all very high, therefore is difficult to be applied to field of traditional Chinese.
The adsorption effect of the adsorbent CTS-active carbon centering pharmaceutically active ingredient that adsorbent that comparing embodiment 1-3 makes and Comparative Examples 2 make, the result is as shown in table 2.
Table 3 crosslinking adsorbent is to the Ligustrazine Hydrochloride adsorption effect
By table 3 as seen, the adsorption rate of the CTS-acticarbon centering pharmaceutically active ingredient ligustrazine that Comparative Examples 2 makes is too high, can't be applied to the heavy metal absorption of Chinese medicine preparation.
Claims (5)
1. chitosan crosslinked preparation of adsorbent method is characterized in that the step of described method is:
A. get the iron ammonium sulfate solid, be dissolved in the deionized water that boiled, with hydrochloric acid adjust pH to 2 ~ 3 of 1.0mol/L;
B. stir after adding shitosan, filter behind the reaction 3h;
C. add isopyknic absolute ethyl alcohol in the filtrate, leave standstill 12h, treat that the product post precipitation filters;
D. use the product of 50 volume % ethanol washing precipitations, obtain flaxen blocks of solid, place 40 ℃ of drying boxes dry, promptly obtain chitosan crosslinked adsorbent product.
2. the method for claim 1 is characterized in that, the ratio of described each raw material and reagent is: every 23.5g iron ammonium sulfate adds 0.5g shitosan and 250mL deionized water.
3. method as claimed in claim 1 or 2 is characterized in that, the deacetylation of described shitosan between 85～95%, molecular weight between 12～130,000, particle diameter 80 orders.
4. method as claimed in claim 1 or 2 is characterized in that it is pure that described iron ammonium sulfate, absolute ethyl alcohol and hydrochloric acid are top grade.
5. the chitosan crosslinked adsorbent that method as claimed in claim 1 or 2 is made.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107486166A (en) * | 2017-08-30 | 2017-12-19 | 北京联合大学 | A kind of compound adsorbent and preparation method thereof |
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|---|---|---|---|---|
| US5021561A (en) * | 1989-04-10 | 1991-06-04 | Etablissement Texcontor | Complexes of iron or other metals with sulphonated derivatives of chitosan |
| CN101200747A (en) * | 2007-12-14 | 2008-06-18 | 华南理工大学 | A physical field-enhanced metal-coordinated chitosan localized enzymatic hydrolysis method |
| CN101637709A (en) * | 2009-07-10 | 2010-02-03 | 广东海洋大学 | Methods for preparing carboxymethyl chitosan magnetic microspheres and adsorbing cadmium in oyster meat by using carboxymethyl chitosan magnetic microspheres |
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2011
- 2011-06-16 CN CN2011101616750A patent/CN102218301A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5021561A (en) * | 1989-04-10 | 1991-06-04 | Etablissement Texcontor | Complexes of iron or other metals with sulphonated derivatives of chitosan |
| CN101200747A (en) * | 2007-12-14 | 2008-06-18 | 华南理工大学 | A physical field-enhanced metal-coordinated chitosan localized enzymatic hydrolysis method |
| CN101637709A (en) * | 2009-07-10 | 2010-02-03 | 广东海洋大学 | Methods for preparing carboxymethyl chitosan magnetic microspheres and adsorbing cadmium in oyster meat by using carboxymethyl chitosan magnetic microspheres |
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| Title |
|---|
| 《应用化学》 20030831 张秀军等 "壳聚糖亚铁螯合物的合成及吸附动力学" 第749-750页1实验部分，2结果与讨论 1-5 第20卷, 第8期 * |
| 张秀军等: ""壳聚糖亚铁螯合物的合成及吸附动力学"", 《应用化学》, vol. 20, no. 8, 31 August 2003 (2003-08-31) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107486166A (en) * | 2017-08-30 | 2017-12-19 | 北京联合大学 | A kind of compound adsorbent and preparation method thereof |
| CN107486166B (en) * | 2017-08-30 | 2020-06-05 | 北京联合大学 | A kind of composite adsorbent and preparation method thereof |
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Application publication date: 20111019 |