CN102500332A - Composite decoloration adsorbent for shellfish products and preparation method of composite decoloration adsorbent - Google Patents
Composite decoloration adsorbent for shellfish products and preparation method of composite decoloration adsorbent Download PDFInfo
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- CN102500332A CN102500332A CN2011103336754A CN201110333675A CN102500332A CN 102500332 A CN102500332 A CN 102500332A CN 2011103336754 A CN2011103336754 A CN 2011103336754A CN 201110333675 A CN201110333675 A CN 201110333675A CN 102500332 A CN102500332 A CN 102500332A
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- composite decoloration
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Abstract
The invention provides a safer, high-efficiency and multifunctional preparation method of composite decoloration adsorbent for shellfishes, which is used for realizing decoloration of shellfish products and heavy metal adsorption so as to reduce heavy metal content and color of shellfish cooking liquid, mussel cooking liquid can be sufficiently developed and utilized by the aid of the method, and injury to human bodies due to excessive heavy metal is avoided.
Description
Technical field
The present invention relates to a kind of composite decoloration adsorbent, particularly a kind of composite decoloration adsorbent that is used for seashell products decolouring, heavy metal absorption and preparation method thereof.
Background technology
The delicious nutrition of seashells animal be loved by the people, but mostly it is filter food that heavy metal is had very high accumulation capability, and the river receives heavy metal pollution in recent years in addition, and the harmful heavy metal in the shellfish body is also accumulated increase.Some is the area seriously, and the heavy metals exceeding standard rate of shellfish reaches more than 90% unexpectedly.
Mussel boiling liquid is to be processed into the accessory substance that produces in the process of freezing article or dried product mussel; Contain a large amount of soluble proteins, polysaccharide, lipid etc.; Nutriment is very abundant; Along with further developing of mussel processing, a large amount of cooking liquors enters marine, and is very serious to the pollution of environment.Therefore develop mussel boiling liquid, resource was fully utilized, can reduce the pollution of environment again.And mussel self can accumulate heavy metal as filter food in a large number, thereby causes some heavy metals exceeding standard in the mussel boiling liquid.Therefore, the prerequisite of development and use cooking liquor is the content of beary metal that effectively reduces wherein.
Cadmium element is big to fish and hydrobiological toxicity, also can cause infringement in various degree to the mankind, can cause the infringement of organs and tissues, and is wherein obvious with kidney damage, and can cause osteoporosis and osteomalacia.Cadmium can suppress the liver cell mitochondria oxidative phosphorylation process simultaneously, makes tissue metabolism that obstacle take place, and the people is had teratogenesis, carcinogenic, mutagenesis.
Trivalent chromium is big to the murder by poisoning of animal, and Cr VI is big to the harm of human body.Comprise that skin is had stimulation and irritated effect, respiratory system, internal organ are had infringement.The census of population and the experimental study of chromium show that all liver, kidney are the vitals that chromium distributes and drains, and also are the main target organs of toxic action simultaneously.International cancer research institution (IARC) and industrial hygienist association of U.S. government (ACGIH) have confirmed that all 6 valency chromium compounds have carcinogenic at present.
Lead is a kind of height noxious material, the heavy metal of serious harm health.The maximum characteristics of lead poisoning are non-specific, are difficult for causing people's attention.After human body sucks or eats; Finally can locate to form Pb accumulation at bone, hair, tooth etc., when run up to a certain amount of after, will cause that health is weak, headache, sleep-disorder, stomachache; Also can cause blood and urine uric acid concentration to increase, cause joint and kidney damage.Plumbous nervous system and the heart and the respiratory system that can damage the people makes people's decreased attention, and can produce bigger influence to people's hematopoiesis function, digestive function, reproductive function.
Shitosan is the deacetylation product of natural biological macromolecular compound chitin, can be used as the pregnant solution of heavy metal ion, can effectively remove heavy metal ion poisonous in the industrial wastewater.And it is advantageous that nontoxic, pollution-free, biodegradable.Japan is used for the about 500t of shitosan of water treatment every year, and EPA's approved is used to drink water purification with shitosan at present.The domestic content of beary metal that has research shitosan to be used for reducing Chinese traditional medicine water extract.Zhang Tongs etc. are used for shitosan Chinese traditional medicine water extracts such as Radix Angelicae Sinensis, RADIX POLYGONI MULTIFLORI PREPARATA, find that it can reduce plumbous content effectively.Huang Bingnan etc. have proved that also shitosan can reduce lead and the arsenic content in the Chinese medicine extract.Though shitosan has the single-minded enrichment performance to heavy metal; And do not receive the influence of a great number of elements (K, Na etc.) and adsorb heavy metal effectively, thereby obviously reduce content of beary metal in the nutrient solution and do not reduce its inorganic nutrients composition, but shitosan has solubility in acid, matter is soft; Settleability is poor in water; Be prone to shortcomings such as diffusing shape through the water long period of soaking, make troubles, must it be carried out the chemical modification processing and could effectively bring into play its strong point to concrete operations and activating and regenerating.
It is the novel heavy metal absorbent and preparation method thereof of primary raw material with the shrimp shell that Chinese patent " a kind of is the novel heavy metal absorbent and preparation method thereof of primary raw material with the shrimp shell " (application number 201010574956.4) discloses a kind of; The preparation method comprises the steps: a, the shrimp shell is dehydrated after, carry out preliminary treatment after the pulverizing and process the shrimp shell meal that main component is a shitosan.B, the shrimp shell meal that contains shitosan that step a is made, washing, decolouring, drying.C, preparation adsorbent: by mass percentage, shrimp shell meal 57%～77%, pore creating material 20%～35% and the agglutinant 3%～8% of step b processing and preparing is joined in the acetum, heat calcination process at a certain temperature after, be cooled to room temperature.Advantages such as the novel heavy metal absorbent that makes has that method is simple, with low cost, environmental friendliness and adsorption effect excellence.
Chinese patent " a kind of novel tannic acid solidifies the preparation method of chitosan adsorbent for heavy metal " (application number 200910065915.X) has announced that a kind of novel tannic acid solidifies the method for chitosan adsorbent for heavy metal.It is soluble in water to take by weighing a certain amount of shitosan, adds a certain amount of high polymer monomer and is stirred to dissolving fully, adds initator, stir to make reaction muddy to occurring, and suction filtration, it is centrifugal on supercentrifuge to filtrate, and water is washed till neutrality with deposition, promptly gets chitosan particle.Take by weighing tannic acid in water, add chitosan particle, isothermal reaction.Product is changed in the epoxychloropropane solution, room temperature reaction, following stirring reaction spends the night in the water-bath, and suction filtration and water are washed till neutrality, promptly get novel solidified tannin acid chitosan particle.Novel tannic acid solidifies chitosan adsorbent for heavy metal Adsorption of Heavy Metal Ions from the aqueous solution fast; Acid with very in a small amount can elute the heavy metal ion that is adsorbed on the adsorbent rapidly.Novel tannic acid solidifies chitosan adsorbent for heavy metal and can recycle more than 200 time, and the life-span was 6 months.This adsorbent can be used for the processing of heavy metal ion sewage, the enrichment of trace heavy metal ion, the recovery of valuable heavy metal ion.
Chinese patent " method of synthesizing heavy metal adsorbent from silica gel and chitosan " (application number 01127897.8) discloses a kind of method of synthesizing heavy metal adsorbent from silica gel and chitosan; 1. 0.5～2.5mol/L acetic acid, 100～500 milliliters are added shitosan 10～40 grams; Constantly stir, filter; 2. in filtrating, add 60～100 order chromatogram body silica gel 20～80 gram, stirred 20～40 minutes, leave standstill 12～24 hours after, stir; 3. shitosan-silicone fluid is through vacuum dehydrating at lower temperature, and 0～15 ℃ of temperature adds 40～80 milliliters of sulfur-bearing organic solvents, ultrasonic dispersing 10～30 minutes; 4. add 3～15 milliliters of epoxychloropropane, the pH value transfers to 6～8, stirs 12～30 hours; 5. cross and filter to remove filtrating, 60～90 ℃ of oven dry with washing, get finished product with the ethanol cleaning, drying again.Mouldability of the present invention, good stability, easy to operate, adsorbent is removed heavy metal ion through column chromatography, also can be soaked in the spirulina breeding nutrient solution, makes it contact through the stirring nutrient solution and adsorbs heavy metal; High adsorption capacity; Regenerability is good, and the performance of the adsorbent after the regeneration is constant.
Above the whole bag of tricks all exists operation more numerous and diverse, and heating calcination process, vacuum dehydrating at lower temperature, equipment investment such as ultrasonic are bigger, and energy consumption is higher, organic solvent emission contaminated environment, the single problems such as (not having decolouring removal of impurities function) of product function.
In order fully to develop mussel boiling liquid, avoid excessive heavy metal that human body is brought harm, press for and find a kind of safer, efficient, multi-functional shellfish composite decoloration adsorbent, to reduce shellfish cooking liquor content of beary metal and colourity.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, a kind of safer, efficient, multi-functional composite decoloration adsorbent that is used for seashell products and preparation method thereof is provided, to reduce shellfish cooking liquor content of beary metal and colourity.
The composite decoloration adsorbent employing that is used for seashell products of the present invention is prepared as follows method and makes:
Step a: acid activation attapulgite: the HCl with 0.05～0.3mol/L soaks attapulgite, and centrifugation is dried to constant weight for 80～120 ℃ with solid content, and 250～450 ℃ of roasting 0.5～5h cross 100～300 mesh sieves, promptly get the acid activation attapulgite;
Step b: acid activation attapulgite and active carbon powder are mixed according to 1: 1～4 weight ratio;
Step c: modification is handled: with the shitosan of deacetylation＞80%, the acetum with 0.5%～5% slowly dissolves, and gets 1%～15% shitosan colloidal sol; In the mixture that step b makes, add 1%～10% shitosan colloidal sol, mix into paste thoroughly for 20～75 ℃, make acid activation attapulgite and active carbon powder mixture complete wetting, carry out modified-reaction;
Steps d: the mixture of step c is dried to constant weight under 80～120 ℃, ground 100～300 mesh sieves subsequently, promptly get the composite decoloration absorbent.
" % " related among the application is " weight % ".
The concrete application process of the application's composite decoloration absorbent: 20～75 ℃; Add above-mentioned 0.1%～5% composite decoloration absorbent in the pending mussel boiling liquid, under natural pH condition, stir absorption 0.2～1.5 hour; Centrifugation, diatomite filtration gets final product.After this method was handled, the clearance of the heavy metal cadmium in the mussel boiling liquid, chromium, lead, copper can reach 90%～95%, 25%～50%, 65%～80%, 90%～98% respectively.And keep retaining of main nutrient composition in the mussel boiling liquid basically.
The application's mussel boiling liquid is meant mussel carried out poach or boiling, treat that mussel opens shell after, wherein shellfish meat in addition packing water cooking liquid or cooking liquor are concentrated obtain subsequently to do its usefulness; And preferably handle at the composite decoloration absorbent that mussel boiling liquid is carried out enzymolysis or fermentation back application the application.
The present invention adopts the mechanism of heavy metal in the shitosan method reduction mussel boiling liquid following: chitosan molecule formula (C
6H
11NO
4)
n, the basic composition unit is the D-aminoglucose, contains a large amount of dissociating-NH in the molecule
2, and-NH
2The ortho position is a hydroxyl.So can borrow hydrogen bond, also can borrow ionic bond to form and have similar cancellated cage type molecule, thereby metal ion is had stable coordination.Shitosan is food additives, belongs to basic nontoxic type, and after interpolation was handled, the residual quantity in cooking liquor is the regulation of National standard also.But, shitosan is water insoluble have only the shitosan powder surface molecular can with the heavy metal ion chelating, thereby the shitosan addition is more.The swelling of shitosan in solution also makes difficulty of separation, and final flocculation and infall process are wayward.In addition, the corresponding valency of shitosan is high.
The present invention is carrier with the attapulgite, with chitosan loaded attapulgite and activated carbon surface in acid activation, again with the heavy metal ion chelating.This adsorbent both can be saved the shitosan addition, made lock out operation simple again, had that the rate of adsorption is fast, adsorption capacity is big, pollution-free a, advantage such as function is many.On the basis that as far as possible keeps original local flavor of mussel boiling liquid and nutritive value, can effectively reduce content of beary metal wherein, make mussel boiling liquid can supply human security edible, not discarded contaminated environment.
Major advantage of the present invention and effect:
(1) mouldability, good stability are easy to operate.This synthetic adsorbent is solid solid particle, can be used as the chromatographic column filler, removes heavy metal ion through column chromatography; Also can this adsorbent be soaked in the mussel boiling liquid; Make it fully to contact the purpose that reaches the absorption heavy metal through stirring mussel boiling liquid, and the heavy metal that is adsorbed is not as long as bigger variation (as becoming highly acid) takes place in the pH value of mussel boiling liquid with it, just can not be from desorption on this adsorbent; In addition, this adsorbent can bear broad pH value scope.
(2) high adsorption capacity.After this law was handled, the clearance of heavy metal cadmium, chromium, lead, copper can reach 90%～95%, 25%～50%, 65%～80%, 90%～98% respectively.
(3) regenerability is good.The adsorbent that adsorbs heavy metal is resolved regeneration with 1mol/LNaCl, clean, dry promptly reusable with pure water.
(4) security is good.These article primary raw material is attapulgite, active carbon, shitosan, and all safety non-toxic can be made food additives or food adsorption filtration auxiliary agent, so these article are adsorption decolourisers of natural and safe.
Embodiment one
HCl with 0.2mol/L soaks attapulgite, and centrifugation is dried to constant weight for 90 ℃ with solid content, and 300 ℃ of roasting 3h cross 200 mesh sieves, promptly get the acid activation attapulgite; With the acid activation attapulgite: active carbon powder=mix at 1: 2.With the shitosan of deacetylation 92%, the acetum with 3.5% slowly dissolves, and gets 4% shitosan colloidal sol; With acid activation attapulgite and active carbon powder mixture, add 5% shitosan colloidal sol, mix into paste thoroughly for 30 ℃, make acid activation attapulgite and active carbon powder mixture complete wetting, carry out modified-reaction; Be dried to constant weight in 100 ℃ then; Cross 200 mesh sieves, promptly get the composite decoloration absorbent.
Absorption (uses) method: 25 ℃, add 2.5% composite decoloration absorbent in the pending mussel boiling liquid, under natural pH condition, stirring absorption 1 hour centrifugalizes, and diatomite filtration gets final product.
After this method was handled, the clearance of heavy metal cadmium, chromium, lead, copper can reach 91%, 30%, 75%, 95% respectively.
Embodiment two
HCl with 0.1mol/L soaks attapulgite, and centrifugation is dried to constant weight for 95 ℃ with solid content, and 350 ℃ of roasting 2.5h cross 200 mesh sieves, promptly get the acid activation attapulgite; With the acid activation attapulgite: active carbon powder=mix at 1: 3.With the shitosan of deacetylation 90%, the acetum with 4% slowly dissolves, and gets 3% shitosan colloidal sol; With acid activation attapulgite and active carbon powder mixture, add 4% shitosan colloidal sol, mix into paste thoroughly for 25 ℃, make acid activation attapulgite and active carbon powder mixture complete wetting, carry out modified-reaction; Be dried to constant weight in 95 ℃ then; Cross 200 mesh sieves, promptly get the composite decoloration absorbent.
Absorption (uses) method: 25 ℃, add 1% composite decoloration absorbent in the pending mussel boiling liquid, under natural pH condition, stirring absorption 1.5 hours centrifugalizes, and diatomite filtration gets final product.
After this method is handled, can effectively reduce the content of heavy metal in the mussel boiling liquid, keep the intact of nutritional labeling in the mussel boiling liquid simultaneously.Protein retention efficiency is more than 55%, and the total reducing sugar rate of retaining is higher than 60%.
Embodiment three
HCl with 0.15mol/L soaks attapulgite, and centrifugation is dried to constant weight for 85 ℃ with solid content, and 400 ℃ of roasting 2h cross 200 mesh sieves, promptly get the acid activation attapulgite; With the acid activation attapulgite: active carbon powder=mix at 1: 2.5.With the shitosan of deacetylation 85%, the acetum with 3.0% slowly dissolves, and gets 3.5% shitosan colloidal sol; With acid activation attapulgite and active carbon powder mixture, add 3.5% shitosan colloidal sol, mix into paste thoroughly for 20 ℃, make acid activation attapulgite and active carbon powder mixture complete wetting, carry out modified-reaction; Be dried to constant weight in 90 ℃ then; Cross 200 mesh sieves, promptly get the composite decoloration absorbent.
Absorption (uses) method: 20 ℃, add 2.0% composite decoloration absorbent in the pending mussel boiling liquid, under natural pH condition, stirring absorption 2 hours centrifugalizes, and diatomite filtration gets final product.
After this method was handled, the clearance of heavy metal cadmium, chromium, lead, copper can reach 90%, 30%, 70%, 92% respectively.
Claims (2)
1. composite decoloration adsorbent that is used for seashell products, it adopts the method for being prepared as follows to make:
Step a: acid activation attapulgite: the HCl with 0.05～0.3mol/L soaks attapulgite, and centrifugation is dried to constant weight for 80～120 ℃ with solid content, and 250～450 ℃ of roasting 0.5～5h cross 100～300 mesh sieves, promptly get the acid activation attapulgite;
Step b: acid activation attapulgite and active carbon powder are mixed according to 1: 1～4 weight ratio;
Step c: modification is handled: with the shitosan of deacetylation＞80%, the acetum with 0.5%～5% slowly dissolves, and gets 1%～15% shitosan colloidal sol; In the mixture that step b makes, add 1%～10% shitosan colloidal sol, mix into paste thoroughly for 20～75 ℃, make acid activation attapulgite and active carbon powder mixture complete wetting, carry out modified-reaction;
Steps d: the mixture of step c is dried to constant weight under 80～120 ℃, ground 100～300 mesh sieves subsequently, promptly get the composite decoloration absorbent; Described " % " is " weight % ".
2. the composite decoloration adsorbent of claim 1 is used for removing the method for the heavy metal of mussel boiling liquid; It is characterized in that, under 20～75 ℃, add 0.1%～5% composite decoloration absorbent in the pending mussel boiling liquid; Under natural pH condition; Stir absorption 0.2～1.5 hour, centrifugation, diatomite filtration.
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Cited By (7)
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| CN103012616A (en) * | 2013-01-14 | 2013-04-03 | 广东海洋大学 | Method for effectively removing cadmium from shellfish polysaccharide |
| CN103783332A (en) * | 2012-10-29 | 2014-05-14 | 浙江海洋学院 | Method of removing lead from squid viscera enzyme hydrolysate by attapulgite adsorption |
| CN105053755A (en) * | 2015-08-12 | 2015-11-18 | 广东环境保护工程职业学院 | Method for effectively removing heavy metals from shellfish protein enzymatic hydrolysate |
| CN105879844A (en) * | 2016-05-26 | 2016-08-24 | 青岛科技大学 | Method for preparing composite shellfish toxin adsorbent by coating porous shell particles with chitosan |
| CN106166479A (en) * | 2016-07-28 | 2016-11-30 | 安徽天港生物科技有限公司 | A kind of heavy metal removing efficient macromolecule pluralgel adsorbent and preparation method thereof |
| CN108371281A (en) * | 2018-02-01 | 2018-08-07 | 江南大学 | A method of cadmium in small Dried fish is removed using chitosan nano microballoon |
| CN109482154A (en) * | 2018-12-06 | 2019-03-19 | 武汉纺织大学 | A kind of preparation method of Dye Adsorption material |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103783332A (en) * | 2012-10-29 | 2014-05-14 | 浙江海洋学院 | Method of removing lead from squid viscera enzyme hydrolysate by attapulgite adsorption |
| CN103783332B (en) * | 2012-10-29 | 2016-03-30 | 浙江海洋学院 | A kind of method plumbous in attapulgite adsorbing and removing squid viscera enzymolysis liquid |
| CN103012616A (en) * | 2013-01-14 | 2013-04-03 | 广东海洋大学 | Method for effectively removing cadmium from shellfish polysaccharide |
| CN103012616B (en) * | 2013-01-14 | 2015-08-26 | 广东海洋大学 | A kind of method of cadmium in effective elimination Shellfish polysaccharide |
| CN105053755A (en) * | 2015-08-12 | 2015-11-18 | 广东环境保护工程职业学院 | Method for effectively removing heavy metals from shellfish protein enzymatic hydrolysate |
| CN105879844A (en) * | 2016-05-26 | 2016-08-24 | 青岛科技大学 | Method for preparing composite shellfish toxin adsorbent by coating porous shell particles with chitosan |
| CN106166479A (en) * | 2016-07-28 | 2016-11-30 | 安徽天港生物科技有限公司 | A kind of heavy metal removing efficient macromolecule pluralgel adsorbent and preparation method thereof |
| CN108371281A (en) * | 2018-02-01 | 2018-08-07 | 江南大学 | A method of cadmium in small Dried fish is removed using chitosan nano microballoon |
| CN109482154A (en) * | 2018-12-06 | 2019-03-19 | 武汉纺织大学 | A kind of preparation method of Dye Adsorption material |
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Application publication date: 20120620 |