CN105032367A - Heavy metal ions adsorbent formed by grafting thiocarbamide acetic acid on chitosan - Google Patents
Heavy metal ions adsorbent formed by grafting thiocarbamide acetic acid on chitosan Download PDFInfo
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- CN105032367A CN105032367A CN201510539571.7A CN201510539571A CN105032367A CN 105032367 A CN105032367 A CN 105032367A CN 201510539571 A CN201510539571 A CN 201510539571A CN 105032367 A CN105032367 A CN 105032367A
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Abstract
The invention relates to a heavy metal ions adsorbent formed by grafting thiocarbamide acetic acid on chitosan, belonging to the field of environmental protection. Aiming at the problems that the chitosan adsorbent has poor adsorption capacity and is easily corroded by acid and base solutions, the method for preparing the absorbent by grafting thiocarbamide acetic acid on chitosan is adopted, so that the stability of the chitosan adsorbent is effectively improved, and the heavy metal ions can be effectively adsorbed. The thiocarbamide acetic acid is grafted on chitosan for modification, the adsorption stability is improved by 50%, the prepared absorbent does not dissolve in acid or base, and can be directly used without crosslinking; and after adsorption, the adsorbent can be recycled after acid picking, so that the cost is saved. When in use, the adsorbent provided by the invention is loaded and fixed on a waste water filter screen, after waste water flows by the waste water filter screen with the absorbent, the content of the heavy metal ions is measured, and the removal rate of the heavy metal ions can achieve 95%.
Description
Technical field
The present invention relates to a kind of thiocarbamide acetic acid grafted chitosan heavy metal absorbent, belong to field of Environment Protection.
Background technology
Heavy metal refers to the about 45 kind elements of density more than 5.0.Arsenic, selenium are nonmetal, but its toxicity and some character similar to heavy metal, so listed in the scope of heavy metal contaminants.The heavy metal of environmental pollution aspect indication mainly refers to the significant mercury of bio-toxicity, cadmium, lead, chromium and metalloid arsenic, also comprises the pollutants such as the virose heavy metal copper of tool, cobalt, nickel, tin, vanadium.The pollution of heavy metal to environment such as air, water body, soil, biospheres caused due to production and the life activity of people is exactly heavy metal pollution.Heavy metal both can directly enter air, water body and soil, caused the direct pollution of all kinds of environmental key-element; Also mutually can move in air, water body and soil, cause the indirect pollution of all kinds of environmental key-element.Because heavy metal can not be degraded by microorganisms, the mutual conversion between various form can only occur in the environment, so the elimination of heavy metal pollution is often more difficult, the impact cause biology and harm are also the problems that people more pay close attention to.Along with the development of China's process of industrialization, the environment negative effect of generation can not be ignored.In recent years, about the report of heavy metal pollution agricultural land soil and water quality more and more causes the concern of people.
Shitosan is a kind of natural polymer, on the earth outside isolating protein, the nitrogenous natural organic matter that quantity is maximum, belong to the polysaccharide in carbohydrate, it is the product of chitin deacetylase, containing various active functional groups such as amino and hydroxyls in its molecule, it is made to have stronger with ability that is metallic ion coordination, energy and Cu
2+, Ni
2+, Hg
2+, Pb
2+, Cr
3+more stable chelate is formed Deng metal ion.Therefore, shitosan can be used as the heavy metal ion in sorbent treatment waste water.But the shortcomings such as shitosan easily runs off, mechanical strength is low, can not regenerate limit its application.
Summary of the invention
The technical problem that the present invention mainly solves: poor for chitosan absorbent adsorption capacity, easily by the problem of soda acid dissolved corrosion, provide a kind of method being prepared adsorbent by thiocarbamide acetic acid graft modification shitosan, effectively improve the stability of chitosan absorbent, can effectively adsorb by heavy metal ion.
In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:
(1) chitosan solid is carried out high pressure to mill, making it form granular size is 80 ~ 100 object chitosan solid particles, by mass percentage, choose the chitosan solid particle of 3 ~ 15%, benzaldehyde solution that the mass fraction of 65 ~ 67% is the methanol solution of 40% and the 0.8mol/L of 20 ~ 30% filters it carry out mix and blend 12 ~ 16h at temperature is 25 ~ 30 DEG C after, get its filter residue for subsequent use;
(2) to be mixed complete after, choosing mass fraction is after the filtrate of 30% methanol solution to above-mentioned preparation extracts 3 ~ 4h in cable type extractor according, place it in after cyclic washing being carried out to it with ether at temperature is 70 ~ 80 DEG C and dry, obtain shitosan alkali for subsequent use;
(3) by mass percentage, choose the epoxychloropropane of 30 ~ 65%, the hydrochloric acid of the 2mol/L of 2 ~ 10%, the mass fraction of 3 ~ 10% be that the ethanolic solution of 30% and the deionized water of 30 ~ 50% are prepared into mixed solution, and by solid-to-liquid ratio 1:10, the shitosan alkali of above-mentioned preparation is added in mixed solution, back flow reaction 3 ~ 4h at temperature 90 DEG C again after magnetic agitation 2h, after backflow completes, it is filtered, choose acetone wash it and dry at temperature 80 DEG C, obtained shitosan intermediate is for subsequent use simultaneously;
(4) by mass percentage, choose the deionized water of the shitosan intermediate of 20 ~ 45%, the thiocarbamide of 15 ~ 30% and the natrium carbonicum calcinatum of 20 ~ 25% and 20 ~ 25%, under temperature is 90 DEG C of water bath with thermostatic control conditions, reflux 1h in there-necked flask, after backflow completes, it is filtered, and extremely neutral with the washing of the NaOH solution of mass fraction 2%, the hydrochloric acid of mass fraction 1% and distilled water successively, dry for standby in 60 DEG C of baking ovens;
(5) by the modification of chitosan of step (4) dry for standby at temperature is 25 ~ 30 DEG C, be soak 48h in the hydrochloric acid solution of 4% at mass fraction, after removing benzaldehyde, 3 ~ 5min is soaked again by the NaOH solution of 0.5mol/L, after band pickling alkali soak, adopt deionized water cyclic washing to neutral and in 60 DEG C of baking ovens oven dry can obtain a kind of thiocarbamide acetic acid grafted chitosan heavy metal absorbent.
Application process of the present invention is: the load of thiocarbamide acetic acid grafted chitosan heavy metal absorbent is fixed on waste water filtering online, and surveying its water inlet content of chromium ion is 100ppm, and surveying its content of chromium ion after treating wastewater streams is 5ppm, and it is 95% that chromium ion clearance reaches.
The invention has the beneficial effects as follows:
(1) the present invention carries out modification by thiocarbamide acetic acid grafted chitosan, and its absorption stability improves 50%;
(2) be both insoluble to acid and be also insoluble to alkali, crosslinked can directly use can not have been needed;
(3) pickling and reusable, cost-saving after adsorbent.
detailed description of the invention:
Chitosan solid is carried out high pressure mill, making it form granular size is 80 ~ 100 object chitosan solid particles, by mass percentage, choose the chitosan solid particle of 3 ~ 15%, benzaldehyde solution that the mass fraction of 65 ~ 67% is the methanol solution of 40% and the 0.8mol/L of 20 ~ 30% filters it carry out mix and blend 12 ~ 16h at temperature is 25 ~ 30 DEG C after, get its filter residue for subsequent use; To be mixed complete after, choosing mass fraction is after the filtrate of 30% methanol solution to above-mentioned preparation extracts 3 ~ 4h in cable type extractor according, places it at temperature is 70 ~ 80 DEG C and dries, obtain shitosan alkali for subsequent use with ether to it after carrying out cyclic washing; By mass percentage, choose the epoxychloropropane of 30 ~ 65%, the hydrochloric acid of the 2mol/L of 2 ~ 10%, the mass fraction of 3 ~ 10% be that the ethanolic solution of 30% and the deionized water of 30 ~ 50% are prepared into mixed solution, and by solid-to-liquid ratio 1:10, the shitosan alkali of above-mentioned preparation is added in mixed solution, back flow reaction 3 ~ 4h at temperature 90 DEG C again after magnetic agitation 2h, after backflow completes, it is filtered, choose acetone wash it and dry at temperature 80 DEG C, obtained shitosan intermediate is for subsequent use simultaneously; By mass percentage, choose the deionized water of the shitosan intermediate of 20 ~ 45%, the thiocarbamide of 15 ~ 30% and the natrium carbonicum calcinatum of 20 ~ 25% and 20 ~ 25%, under temperature is 90 DEG C of water bath with thermostatic control conditions, reflux 1h in there-necked flask, after backflow completes, it is filtered, and extremely neutral with the washing of the NaOH solution of mass fraction 2%, the hydrochloric acid of mass fraction 1% and distilled water successively, dry for standby in 60 DEG C of baking ovens; By the modification of chitosan of dry for standby at temperature is 25 ~ 30 DEG C, be soak 48h in the hydrochloric acid solution of 4% at mass fraction, after removing benzaldehyde, 3 ~ 5min is soaked again by the NaOH solution of 0.5mol/L, after band pickling alkali soak, adopt deionized water cyclic washing to neutral and in 60 DEG C of baking ovens oven dry can obtain a kind of thiocarbamide acetic acid grafted chitosan heavy metal absorbent; The present invention carries out modification by thiocarbamide acetic acid grafted chitosan, and its absorption stability improves 50%; Both be insoluble to acid and be also insoluble to alkali, crosslinked can directly use can not have been needed; Pickling and reusable, cost-saving after adsorbent.
Chitosan solid is carried out high pressure mill, making it form granular size is 80 object chitosan solid particles, by gross mass 100g, choose the chitosan solid particle of 3g, benzaldehyde solution that the mass fraction of 67g is the methanol solution of 40g and the 0.8mol/L of 30g filters it carry out mix and blend 12h at temperature is 25 DEG C after, get its filter residue for subsequent use; To be mixed complete after, choosing mass fraction is after the filtrate of 30% methanol solution to above-mentioned preparation extracts 3h in cable type extractor according, places it at temperature is 70 DEG C and dries, obtain shitosan alkali for subsequent use with ether to it after carrying out cyclic washing; By gross mass 100g, choose the epoxychloropropane of 30g, the hydrochloric acid of the 2mol/L of 10g, the mass fraction of 10g be that the ethanolic solution of 30% and the deionized water of 50g are prepared into mixed solution, and by solid-to-liquid ratio 1:10, the 10g shitosan alkali of above-mentioned preparation is added in mixed solution, back flow reaction 3h at temperature 90 DEG C again after magnetic agitation 2h, after backflow completes, filter it, choose acetone simultaneously and wash it and dry at temperature 80 DEG C, obtained shitosan intermediate is for subsequent use; By gross mass 100g, choose the deionized water of the shitosan intermediate of 20g, the thiocarbamide of 30g and the natrium carbonicum calcinatum of 25g and 25g, under temperature is 90 DEG C of water bath with thermostatic control conditions, reflux 1h in there-necked flask, after backflow completes, it is filtered, and extremely neutral with the washing of the NaOH solution of mass fraction 2%, the hydrochloric acid of mass fraction 1% and distilled water successively, dry for standby in 60 DEG C of baking ovens; By the modification of chitosan of dry for standby at temperature is 25 DEG C, be soak 48h in the hydrochloric acid solution of 4% at mass fraction, after removing benzaldehyde, 3min is soaked again by the NaOH solution of 0.5mol/L, after band pickling alkali soak, adopt deionized water cyclic washing to neutral and in 60 DEG C of baking ovens oven dry can obtain a kind of thiocarbamide acetic acid grafted chitosan heavy metal absorbent; The present invention carries out modification by thiocarbamide acetic acid grafted chitosan, and its absorption stability improves 50%; Both be insoluble to acid and be also insoluble to alkali, crosslinked can directly use can not have been needed; Pickling and reusable, cost-saving after adsorbent.
Chitosan solid is carried out high pressure mill, making it form granular size is 90 object chitosan solid particles, by gross mass 200g, choose the chitosan solid particle of 26g, benzaldehyde solution that the mass fraction of 134g is the methanol solution of 80g and the 0.8mol/L of 40g filters it carry out mix and blend 14h at temperature is 28 DEG C after, get its filter residue for subsequent use; To be mixed complete after, choosing mass fraction is after the filtrate of 30% methanol solution to above-mentioned preparation extracts 3h in cable type extractor according, places it at temperature is 75 DEG C and dries, obtain shitosan alkali for subsequent use with ether to it after carrying out cyclic washing; By gross mass 200g, choose the epoxychloropropane of 80g, the hydrochloric acid of the 2mol/L of 10g, the mass fraction of 10g be that the ethanolic solution of 30% and the deionized water of 100g are prepared into mixed solution, and by solid-to-liquid ratio 1:10, the 20g shitosan alkali of above-mentioned preparation is added in mixed solution, back flow reaction 4h at temperature 90 DEG C again after magnetic agitation 2h, after backflow completes, filter it, choose acetone simultaneously and wash it and dry at temperature 80 DEG C, obtained shitosan intermediate is for subsequent use; By gross mass 200g, choose the deionized water of the shitosan intermediate of 60g, the thiocarbamide of 40g and the natrium carbonicum calcinatum of 50g and 50g, under temperature is 90 DEG C of water bath with thermostatic control conditions, reflux 1h in there-necked flask, after backflow completes, it is filtered, and extremely neutral with the washing of the NaOH solution of mass fraction 2%, the hydrochloric acid of mass fraction 1% and distilled water successively, dry for standby in 60 DEG C of baking ovens; By the modification of chitosan of dry for standby at temperature is 27 DEG C, be soak 48h in the hydrochloric acid solution of 4% at mass fraction, after removing benzaldehyde, 4min is soaked again by the NaOH solution of 0.5mol/L, after band pickling alkali soak, adopt deionized water cyclic washing to neutral and in 60 DEG C of baking ovens oven dry can obtain a kind of thiocarbamide acetic acid grafted chitosan heavy metal absorbent; The present invention carries out modification by thiocarbamide acetic acid grafted chitosan, and its absorption stability improves 50%; Both be insoluble to acid and be also insoluble to alkali, crosslinked can directly use can not have been needed; Pickling and reusable, cost-saving after adsorbent.
Chitosan solid is carried out high pressure mill, making it form granular size is 80 ~ 100 object chitosan solid particles, by gross mass 300g, choose the chitosan solid particle of 45g, benzaldehyde solution that the mass fraction of 195g is the methanol solution of 40% and the 0.8mol/L of 60g filters it carry out mix and blend 16h at temperature is 30 DEG C after, get its filter residue for subsequent use; To be mixed complete after, choosing mass fraction is after the filtrate of 30% methanol solution to above-mentioned preparation extracts 4h in cable type extractor according, places it at temperature is 80 DEG C and dries, obtain shitosan alkali for subsequent use with ether to it after carrying out cyclic washing; By gross mass 300g, choose the epoxychloropropane of 195g, the hydrochloric acid of the 2mol/L of 6g, the mass fraction of 9g be that the ethanolic solution of 30% and the deionized water of 90g are prepared into mixed solution, and by solid-to-liquid ratio 1:10, the 30g shitosan alkali of above-mentioned preparation is added in mixed solution, back flow reaction 4h at temperature 90 DEG C again after magnetic agitation 2h, after backflow completes, filter it, choose acetone simultaneously and wash it and dry at temperature 80 DEG C, obtained shitosan intermediate is for subsequent use; By gross mass 300g, choose the deionized water of the shitosan intermediate of 135g, the thiocarbamide of 45g and the natrium carbonicum calcinatum of 60g and 60g, under temperature is 90 DEG C of water bath with thermostatic control conditions, reflux 1h in there-necked flask, after backflow completes, it is filtered, and extremely neutral with the washing of the NaOH solution of mass fraction 2%, the hydrochloric acid of mass fraction 1% and distilled water successively, dry for standby in 60 DEG C of baking ovens; By the modification of chitosan of dry for standby at temperature is 30 DEG C, be soak 48h in the hydrochloric acid solution of 4% at mass fraction, after removing benzaldehyde, 5min is soaked again by the NaOH solution of 0.5mol/L, after band pickling alkali soak, adopt deionized water cyclic washing to neutral and in 60 DEG C of baking ovens oven dry can obtain a kind of thiocarbamide acetic acid grafted chitosan heavy metal absorbent; The present invention carries out modification by thiocarbamide acetic acid grafted chitosan, and its absorption stability improves 50%; Both be insoluble to acid and be also insoluble to alkali, crosslinked can directly use can not have been needed; Pickling and reusable, cost-saving after adsorbent.
Claims (1)
1. a thiocarbamide acetic acid grafted chitosan heavy metal absorbent, is characterized in that concrete preparation process is:
(1) chitosan solid is carried out high pressure to mill, making it form granular size is 80 ~ 100 object chitosan solid particles, by mass percentage, choose the chitosan solid particle of 3 ~ 15%, benzaldehyde solution that the mass fraction of 65 ~ 67% is the methanol solution of 40% and the 0.8mol/L of 20 ~ 30% filters it carry out mix and blend 12 ~ 16h at temperature is 25 ~ 30 DEG C after, get its filter residue for subsequent use;
(2) to be mixed complete after, choosing mass fraction is after the filtrate of 30% methanol solution to above-mentioned preparation extracts 3 ~ 4h in cable type extractor according, place it in after cyclic washing being carried out to it with ether at temperature is 70 ~ 80 DEG C and dry, obtain shitosan alkali for subsequent use;
(3) by mass percentage, choose the epoxychloropropane of 30 ~ 65%, the hydrochloric acid of the 2mol/L of 2 ~ 10%, the mass fraction of 3 ~ 10% be that the ethanolic solution of 30% and the deionized water of 30 ~ 50% are prepared into mixed solution, and by solid-to-liquid ratio 1:10, the shitosan alkali of above-mentioned preparation is added in mixed solution, back flow reaction 3 ~ 4h at temperature 90 DEG C again after magnetic agitation 2h, after backflow completes, it is filtered, choose acetone wash it and dry at temperature 80 DEG C, obtained shitosan intermediate is for subsequent use simultaneously;
(4) by mass percentage, choose the deionized water of the shitosan intermediate of 20 ~ 45%, the thiocarbamide of 15 ~ 30% and the natrium carbonicum calcinatum of 20 ~ 25% and 20 ~ 25%, under temperature is 90 DEG C of water bath with thermostatic control conditions, reflux 1h in there-necked flask, after backflow completes, it is filtered, and extremely neutral with the washing of the NaOH solution of mass fraction 2%, the hydrochloric acid of mass fraction 1% and distilled water successively, dry for standby in 60 DEG C of baking ovens;
(5) by the modification of chitosan of step (4) dry for standby at temperature is 25 ~ 30 DEG C, be soak 48h in the hydrochloric acid solution of 4% at mass fraction, after removing benzaldehyde, 3 ~ 5min is soaked again by the NaOH solution of 0.5mol/L, after band pickling alkali soak, adopt deionized water cyclic washing to neutral and in 60 DEG C of baking ovens oven dry can obtain a kind of thiocarbamide acetic acid grafted chitosan heavy metal absorbent.
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Cited By (7)
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| CN105712429A (en) * | 2016-04-08 | 2016-06-29 | 成都理工大学 | Method for adsorbing IV ions with salicylaldehyde modified chitosan |
| CN106831079A (en) * | 2015-12-07 | 2017-06-13 | 无锡南理工科技发展有限公司 | A kind of modification of chitosan peanut Special slow release fertilizer and preparation method thereof |
| CN107129543A (en) * | 2017-03-20 | 2017-09-05 | 浙江工商大学 | A kind of thiocarbamide modification of chitosan and its preparation method and application |
| CN108079964A (en) * | 2017-12-18 | 2018-05-29 | 安徽唯诗杨信息科技有限公司 | A kind of preparation process and its production equipment of sulfhydryl modified chitosan absorbent |
| CN110586045A (en) * | 2019-09-21 | 2019-12-20 | 天津大学 | Preparation method and application of amphoteric magnetic chitosan adsorbent |
| CN110833135A (en) * | 2019-11-04 | 2020-02-25 | 大连海洋大学 | Method for removing heavy metals in shellfish enzymolysis liquid |
| CN111530436A (en) * | 2020-04-28 | 2020-08-14 | 中国科学院海洋研究所 | Method for modifying shells |
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2015
- 2015-08-30 CN CN201510539571.7A patent/CN105032367A/en not_active Withdrawn
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106831079A (en) * | 2015-12-07 | 2017-06-13 | 无锡南理工科技发展有限公司 | A kind of modification of chitosan peanut Special slow release fertilizer and preparation method thereof |
| CN105712429A (en) * | 2016-04-08 | 2016-06-29 | 成都理工大学 | Method for adsorbing IV ions with salicylaldehyde modified chitosan |
| CN107129543A (en) * | 2017-03-20 | 2017-09-05 | 浙江工商大学 | A kind of thiocarbamide modification of chitosan and its preparation method and application |
| CN107129543B (en) * | 2017-03-20 | 2019-06-11 | 浙江工商大学 | A kind of thiocarbamide modification of chitosan and its preparation method and application |
| CN108079964A (en) * | 2017-12-18 | 2018-05-29 | 安徽唯诗杨信息科技有限公司 | A kind of preparation process and its production equipment of sulfhydryl modified chitosan absorbent |
| CN108079964B (en) * | 2017-12-18 | 2021-02-12 | 浙江丰润生物科技股份有限公司 | Preparation process and production equipment of sulfydryl modified chitosan adsorbent |
| CN110586045A (en) * | 2019-09-21 | 2019-12-20 | 天津大学 | Preparation method and application of amphoteric magnetic chitosan adsorbent |
| CN110833135A (en) * | 2019-11-04 | 2020-02-25 | 大连海洋大学 | Method for removing heavy metals in shellfish enzymolysis liquid |
| CN110833135B (en) * | 2019-11-04 | 2023-07-07 | 大连海洋大学 | Method for removing heavy metals in shellfish enzymolysis liquid |
| CN111530436A (en) * | 2020-04-28 | 2020-08-14 | 中国科学院海洋研究所 | Method for modifying shells |
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Application publication date: 20151111 |