CN102363118B - Method for removing heavy metal lead in aquatic product flavoring - Google Patents
Method for removing heavy metal lead in aquatic product flavoring Download PDFInfo
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- CN102363118B CN102363118B CN2011101276462A CN201110127646A CN102363118B CN 102363118 B CN102363118 B CN 102363118B CN 2011101276462 A CN2011101276462 A CN 2011101276462A CN 201110127646 A CN201110127646 A CN 201110127646A CN 102363118 B CN102363118 B CN 102363118B
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- 229910001385 heavy metal Inorganic materials 0.000 title claims abstract description 16
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- 150000001413 amino acids Chemical class 0.000 claims abstract description 8
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000001179 sorption measurement Methods 0.000 claims abstract description 6
- 239000007787 solid Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 33
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 33
- 239000008367 deionised water Substances 0.000 claims description 33
- 229910021641 deionized water Inorganic materials 0.000 claims description 33
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- 238000001914 filtration Methods 0.000 claims description 18
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- 238000007654 immersion Methods 0.000 claims description 12
- 239000003480 eluent Substances 0.000 claims description 11
- 239000000796 flavoring agent Substances 0.000 claims description 11
- 235000019634 flavors Nutrition 0.000 claims description 11
- 238000011010 flushing procedure Methods 0.000 claims description 11
- 230000007935 neutral effect Effects 0.000 claims description 11
- 238000010521 absorption reaction Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 3
- 241000238366 Cephalopoda Species 0.000 claims description 2
- 241000238557 Decapoda Species 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 241000218645 Cedrus Species 0.000 claims 3
- 239000003463 adsorbent Substances 0.000 abstract description 8
- 238000011084 recovery Methods 0.000 abstract description 5
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 239000003513 alkali Substances 0.000 abstract 2
- 239000000047 product Substances 0.000 description 28
- 239000000706 filtrate Substances 0.000 description 9
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- 238000001514 detection method Methods 0.000 description 5
- 238000010298 pulverizing process Methods 0.000 description 5
- 238000005342 ion exchange Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 108090000790 Enzymes Proteins 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- RVPVRDXYQKGNMQ-UHFFFAOYSA-N lead(2+) Chemical compound [Pb+2] RVPVRDXYQKGNMQ-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
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- 235000014653 Carica parviflora Nutrition 0.000 description 1
- 241000243321 Cnidaria Species 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000005842 biochemical reaction Methods 0.000 description 1
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- 239000003245 coal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
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- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
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- 239000011347 resin Substances 0.000 description 1
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- 210000002345 respiratory system Anatomy 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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- 125000004646 sulfenyl group Chemical group S(*)* 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- Seasonings (AREA)
- Meat, Egg Or Seafood Products (AREA)
Abstract
The invention relates to a method and an adsorbent for removing heavy metal lead in an aquatic product flavoring. The method is characterized by comprising the following steps of: adding lignocellulose after acid and alkali treatment into aquatic product flavoring aqueous solution with amino acid concentration of 0.02-0.1g/ml; and performing shaking adsorption for 1-5 times, wherein the shaking rate is 50-500r/min, liquid-solid ratio range is 10-150:1, the temperature range is 20-60 DEG C, and the adsorption time is 0.5-24 hours; and the lignocellulose after acid and alkali treatment is used as the adsorbent, so that the contact area of reaction is increased. The method and the adsorbent have the advantages of quick adsorption, no pollution, easiness in recovery and the like.
Description
Technical field
The present invention relates to a kind of method of heavy metal lead in the aquatic products flavouring and relevant adsorbent field of removing.
Background technology
Because factors such as marine pollution and natural origin, exist heavy metal lead to pollute in the marine and aquatic product processing fent tissue, lead ion in the waste protein hydrolysate used dried aquatic products flavouring exceeds standard, therefore enzymolysis liquid must remove lead ion, could realize the recycling of marine and aquatic product processing fent.Heavy metal lead is pollutant in the environment, pass through the oral cavity, approach such as skin and respiratory tract enters in the body, because the metal active of itself, very easily be combined with the sulfenyl of some enzyme, thereby the activity of the enzyme that the conformation that has changed zymophore makes reduces even inactivation, and metabolic half life in vivo is long, the serious human body health that threatens, caused the concern of more and more scholars, its primary pollution source is the tail gas of motor vehicle emission, the waste gas that coal combustion and paint produce, environment is caused great pollution, and organism by bio-absorbable from water body, soil, absorb plumbous in the air, cause the lead content of organism in the worldwide constantly to raise, the ocean accounts for 71% of ground sphere area again, living marine resources are extremely abundant, and therefore, studying a kind of method that removes lead in the aquatic products fast has important use to be worth.
Remove plumbous method at present both at home and abroad and mainly contain the precipitation method, absorption method, oxidizing process, ion-exchange, biological deleading method.Precipitation method deleading mainly is to form the post precipitation filtration by physical-chemical reaction takes place, but precipitating reagent commonly used refers to form with lead the sulphate of vulcanized lead or plumbite, and the new functional group that introduces can cause pollution again, is not suitable for the aquatic products flavouring.Therefore, oxidizing process is to point to wherein to add strong oxidizer, but the use of shortcoming chemicals can pollute equally.Ion-exchange refers to porous resin or ion-exchange fibre are adsorbed lead, this method can effectively reach removes plumbous effect, but in the operation of reality, because strong adsorption capacity makes the problems such as regeneration, recovery of adsorbent have certain difficulty, it is cumbersome to make its processing go up technology, use cost is not suitable for large-scale use also than higher.The method of biological deleading is introduced organism, and the biochemical reaction by itself methylates lead, but this method is fit to high concentration lead.Absorption method refers to select for use that itself to have a surface area big, water-insoluble solid material (coral, zeolite, lignocellulosic etc.), under the mechanism of physics, chemisorbed, lead is absorbed and fixed at the surface and plays and remove plumbous effect and can not increase water salinity again, be well suited in the aquatic products flavouring, using.
Summary of the invention is
First technical problem to be solved by this invention provide a kind ofly adsorb fast, the removing heavy metal lead in the aquatic products flavouring, guarantee the method that removes heavy metal lead in the aquatic products flavouring of product quality safety of pollution-free substantially, easy recovery.
Second technical problem to be solved by this invention provide a kind ofly adsorb fast, the adsorbent that removes heavy metal lead in the aquatic products flavouring of pollution-free substantially, easy recovery.
The present invention solves the technical scheme that above-mentioned first technical problem adopts: a kind of method that removes heavy metal lead in the aquatic products flavouring is characterized in that step is:
Be the lignocellulosic that adds in the aquatic products flavouring aqueous solution of 0.02～0.10g/ml after soda acid is handled at amino acid concentration, vibration absorption 1～5 time, oscillation rate is 50～500r/min (preferred 150r/min), the liquid-solid ratio scope is 10～150: 1 (preferred 30～120: 1), temperature range is 20～60 ℃, and adsorption time is 0.5～24 hour (preferred 12 hours).
Preferably, it is that lignocellulosic is placed 80～120 ℃ of baking oven bakings 1～10 hour that the soda acid of lignocellulosic is handled, pulverize then, adding concentration is NaOH solution immersion filtration after 2～10 days of 0.1～5mol/L, filter residue is colourless to eluent with deionized water rinsing, adding concentration again is HCl solution immersion filtration after 2～24 hours of 0.02～0.5mol/L, filter residue is washed till pH with deionized water and is neutral, (v) the % alcohol flushing is to colourless to be 90～98 with concentration again, be washed till no ethanol flavor back with deionized water at last and filter, the filter residue oven dry obtains lignocellulosic.
Be more preferably, it is that lignocellulosic is placed 105 ℃ of baking oven bakings 4 hours that soda acid is handled, wear into 60～80 order powderies then, adding concentration is NaOH solution immersion filtration after 5 days of 0.1～5mol/L, filter residue is colourless to eluent with deionized water rinsing, adding concentration again is HCl solution immersion filtration after 12 hours of 0.1mol/L, filter residue is washed till pH with deionized water and is neutral, (v) the % alcohol flushing is to colourless to be 95 with concentration again, be washed till no ethanol flavor back with deionized water at last and filter, the filter residue oven dry obtains lignocellulosic.
As preferably, described lignocellulosic is from the shirt wood chip.
At last, the described method that removes heavy metal lead in the aquatic products flavouring is characterized in that the aquatic products flavouring refers to the dried product of enzymolysis liquid of squid, shrimp or/and crab ocean water product processing fent.
The present invention solves the technical scheme that above-mentioned second technical problem adopt: a kind of adsorbent that removes heavy metal lead in the aquatic products flavouring, it is characterized in that adopting the lignocellulosic after soda acid is handled, it is that lignocellulosic is placed 80～120 ℃ of baking oven bakings 1～10 hour, pulverize then, adding concentration is NaOH solution immersion filtration after 2～10 days of 0.1～5mol/L, filter residue is colourless to eluent with deionized water rinsing, adding concentration again is HCl solution immersion filtration after 2～24 hours of 0.02～0.5mol/L, filter residue is washed till pH with deionized water and is neutral, (v) the % alcohol flushing is to colourless to be 90～98 with concentration again, be washed till no ethanol flavor back with deionized water at last and filter, the filter residue oven dry obtains lignocellulosic.
Preferably, it is that lignocellulosic is placed 105 ℃ of baking oven bakings 4 hours that soda acid is handled, wear into 60～80 order powderies then, adding concentration is NaOH solution immersion filtration after 5 days of 0.1～5mol/L, filter residue is colourless to eluent with deionized water rinsing, adding concentration again is HCl solution immersion filtration after 12 hours of 0.1mol/L, filter residue is washed till pH with deionized water and is neutral, (v) the % alcohol flushing is to colourless to be 95 with concentration again, be washed till no ethanol flavor back with deionized water at last and filter, the filter residue oven dry obtains lignocellulosic.
Compared with prior art, the invention has the advantages that: contain a large amount of hydroxyls and carboxyl in the surface texture of lignocellulosic, can with heavy metal generation ion-exchange, complex reaction etc.; Compare with other chemical method, natural lignocellulosic can not cause secondary pollution, more is conducive to be applied on the food; Because a large amount of hole in its surface is particularly handled the simple soda acid that carries out of lignocellulosic itself, change the lignocellulosic surface texture again, make the contact area of reaction increase, have advantages such as absorption is quick, pollution-free, easy recovery; The present invention selects for use lignocellulosic as sorbing material, lead in the aquatic products removed to reach good removal efficiency, adsorbing and removing can reach more than 97%, make the requirement (GB/T 5009.11) that can be up to state standards of aquatic products flavouring lead content, the employing lignocellulosic is adsorbent, and cost is low, the source is wide, is a kind of sorbing material of green safety, be conducive to use of large-scale production, can effectively guarantee the product quality of aquatic products flavouring.
The specific embodiment
Describe in further detail below in conjunction with the present invention of embodiment.
Embodiment 1
Get the conical flask of 250ml, adding amino acid concentration is the aquatic products flavouring aqueous solution 100ml of 0.05g/ml and the lead solution 100ml of 200 μ g/L, is settled to 250ml; With the shirt wood chip after pulverizing, in 0.1mol/L NaOH solution, soak after 5 days and filter, filter residue is colourless to eluent with deionized water rinsing, add 0.1mol/L HCl again and soak filtration after 12 hours, filter residue is washed till pH with deionized water and is neutral, use 95% alcohol flushing to colourless again, be washed till no ethanol flavor back with deionized water at last and filter, the filter residue oven dry obtains the lignocellulosic after soda acid is handled.The lignocellulosic 2g that got 60 mesh sieves adds in the conical flask, after 25 ℃ of following 150r/min vibrations are adsorbed 12h, left standstill 12h, filter, added the lignocellulosic 2g absorption of 60 mesh sieves in the filtrate more once, get filtrate detection, lignocellulosic reaches 97.35% to the removal efficiency of lead.
Embodiment 2
Get the conical flask of 250ml, adding amino acid concentration is the aquatic products flavouring aqueous solution 100ml of 0.1g/ml and the lead solution 100ml of 200 μ g/L, is settled to 250ml; With the shirt wood chip after pulverizing, in 1mol/L NaOH solution, soak after 5 days and filter, filter residue is colourless to eluent with deionized water rinsing, add 0.1mol/L HCl again and soak filtration after 12 hours, filter residue is washed till pH with deionized water and is neutral, use 95% alcohol flushing to colourless again, be washed till no ethanol flavor back with deionized water at last and filter, the filter residue oven dry obtains the lignocellulosic after soda acid is handled.The lignocellulosic 3g that got 80 mesh sieves adds in the conical flask, after 30 ℃ of following 150r/min vibrations are adsorbed 12h, left standstill 12h, filter, added the lignocellulosic 2g absorption secondary of 80 mesh sieves in the filtrate again, get filtrate detection, lignocellulosic reaches 98.76% to the removal efficiency of lead.
Embodiment 3
Get the conical flask of 250ml, adding amino acid concentration is the aquatic products flavouring aqueous solution 100ml of 0.1g/ml and the lead solution 100ml of 200 μ g/L, is settled to 250ml; With the shirt wood chip after pulverizing, in 2mol/L NaOH solution, soak after 5 days and filter, filter residue is colourless to eluent with deionized water rinsing, add 0.1mol/L HCl again and soak filtration after 12 hours, filter residue is washed till pH with deionized water and is neutral, use 95% alcohol flushing to colourless again, be washed till no ethanol flavor back with deionized water at last and filter, the filter residue oven dry obtains the lignocellulosic after soda acid is handled.The lignocellulosic 5g that got 60 mesh sieves adds in the conical flask, filter after 30 ℃ of following 150r/min vibrations are adsorbed 12h, left standstill 12h, the lignocellulosic 5g that added 60 mesh sieves in the filtrate again adsorbs three times, get filtrate detection, lignocellulosic reaches 99.48% to the removal efficiency of lead.
Embodiment 4
Get the conical flask of 250ml, adding amino acid concentration is the aquatic products flavouring aqueous solution 100ml of 0.25g/ml and the lead solution 100ml of 200ug/L, is settled to 250ml; With the shirt wood chip after pulverizing, in 4mol/L NaOH solution, soak after 5 days and filter, filter residue is colourless to eluent with deionized water rinsing, add 0.1mol/L HCl again and soak filtration after 12 hours, filter residue is washed till pH with deionized water and is neutral, use 95% alcohol flushing to colourless again, be washed till no ethanol flavor back with deionized water at last and filter, the filter residue oven dry obtains the lignocellulosic after soda acid is handled.The lignocellulosic 10g that got 80 mesh sieves adds in the conical flask, filters after 35 ℃ of following 150r/min vibrations are adsorbed 12h, left standstill 12h, gets filtrate detection, and lignocellulosic reaches 97.64% to the removal efficiency of lead.
Embodiment 5
Get the conical flask of 250ml, adding amino acid concentration is the aquatic products flavouring aqueous solution 100ml of 0.15g/ml and the lead solution 100ml of 200ug/L, is settled to 250ml; With the shirt wood chip after pulverizing, in 5mol/L NaOH solution, soak after 5 days and filter, filter residue is colourless to eluent with deionized water rinsing, add 0.1mol/L HCl again and soak filtration after 12 hours, filter residue is washed till pH with deionized water and is neutral, use 95% alcohol flushing to colourless again, be washed till no ethanol flavor back with deionized water at last and filter, the filter residue oven dry obtains the lignocellulosic after soda acid is handled.The lignocellulosic 8g that got 80 mesh sieves adds in the conical flask, at 40 ℃ of following 150r/min vibration absorption 12h, filter after leaving standstill 12h, the lignocellulosic 8g that added 80 mesh sieves in the filtrate again adsorbs four times, at 40 ℃ of following 150r/min vibration absorption 12h, filter after leaving standstill 12h, get filtrate detection, lignocellulosic reaches 99.96% to the removal efficiency of lead.
Claims (3)
1. method that removes heavy metal lead in the aquatic products flavouring is characterized in that step is:
Be the lignocellulosic that adds in the aquatic products flavouring aqueous solution of 0.02～0.1g/mL after soda acid is handled at amino acid concentration, vibration absorption 1～5 time, oscillation rate is 50～500r/min, the liquid-solid ratio scope is 10～150: 1, temperature range is 20～60 ℃, and adsorption time is 0.5～24 hour;
Described lignocellulosic is from cedar sawdust, it is that cedar sawdust is placed 80～120 ℃ of baking oven bakings 1～10 hour that described soda acid is handled, pulverize then, adding concentration is NaOH solution immersion filtration after 2～10 days of 0.1～5mol/L, filter residue is colourless to eluent with deionized water rinsing, adding concentration again is HCl solution immersion filtration after 2～24 hours of 0.02～0.5mol/L, filter residue is washed till pH with deionized water and is neutral, (v) the % alcohol flushing is to colourless to be 90～98 with concentration again, be washed till no ethanol flavor back with deionized water at last and filter, the filter residue oven dry obtains lignocellulosic.
2. the method that removes heavy metal lead in the aquatic products flavouring according to claim 1, it is characterized in that it is that cedar sawdust is placed 105 ℃ of baking oven bakings 4 hours that soda acid is handled, wear into 60～80 order powderies then, adding concentration is NaOH solution immersion filtration after 5 days of 0.1～5mol/L, filter residue is colourless to eluent with deionized water rinsing, adding concentration again is HCl solution immersion filtration after 12 hours of 0.1mol/L, filter residue is washed till pH with deionized water and is neutral, (v) the % alcohol flushing is to colourless to be 95 with concentration again, be washed till no ethanol flavor back with deionized water at last and filter, the filter residue oven dry obtains lignocellulosic.
3. according to claim 1 or the described method that removes heavy metal lead in the aquatic products flavouring of 2 any claims, it is characterized in that the aquatic products flavouring refers to the dried product of enzymolysis liquid of squid, shrimp or/and crab ocean water product processing fent.
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| CN102783673A (en) * | 2012-07-12 | 2012-11-21 | 浙江海洋学院 | Method for removing heavy metals in squid enzymolysis liquid |
| CN102786162A (en) * | 2012-08-27 | 2012-11-21 | 杭州普丽美地生物科技有限公司 | Method for treating tea-leaf intensive processing industry sewage with sawdust |
| CN103506087B (en) * | 2013-09-27 | 2015-12-09 | 华南农业大学 | A kind of maleylation wood fibre room temperature prepares the method for adsorbent for heavy metal |
| CN105077382A (en) * | 2015-05-18 | 2015-11-25 | 浙江海洋学院 | Method for removing metal ions in shrimp products |
| CN107319499B (en) * | 2017-07-27 | 2020-10-16 | 浙江省海洋开发研究院 | Preparation method of deep-fermented shrimp head sauce |
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| CN101306347A (en) * | 2008-02-19 | 2008-11-19 | 浙江大学 | Preparation method and renovation method of treatment tea for absorbing heavy metal ion in waste water |
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| JPH05277467A (en) * | 1992-03-30 | 1993-10-26 | Nobuo Ogura | Adsorption removal of heavy metal salt by tannin-containing wood |
| JP3268657B2 (en) * | 1992-09-09 | 2002-03-25 | 睦 庄司 | How to remove heavy metals from amino acid solution of fish and shellfish |
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| JP特开平5-277467A 1993.10.26 |
| JP特开平6-106155A 1994.04.19 |
| 改性纤维素吸附剂的制备及其对重金属离子的吸附;陈丽华;《中国新技术新产品》;20091231(第12期);第6页 * |
| 陈丽华.改性纤维素吸附剂的制备及其对重金属离子的吸附.《中国新技术新产品》.2009,(第12期),第6页. |
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