CN101773819A - Resin preparation process for removing residual heavy metal arsenic in laminaria seaweed extract - Google Patents
Resin preparation process for removing residual heavy metal arsenic in laminaria seaweed extract Download PDFInfo
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- CN101773819A CN101773819A CN201010119859A CN201010119859A CN101773819A CN 101773819 A CN101773819 A CN 101773819A CN 201010119859 A CN201010119859 A CN 201010119859A CN 201010119859 A CN201010119859 A CN 201010119859A CN 101773819 A CN101773819 A CN 101773819A
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Abstract
The invention relates to a resin preparation process for removing residual heavy metal arsenic in larminaria seaweed extract. Chitosan is adopted as the raw material, arsenic standard solution is used as template ion, and the chitonsan arsenic template resin is prepared through the procedures such as absorption, dispersion, emulsion, pre-crosslink, crosslink, washing and the like. The chitonsan template resin has the advantages of short production period, simple preparation process, uniform product specification, low cost and the like, and is applicable to the industrial production. The product is white or faint yellow, has good quality, is safe and non-toxic, can be used for the fields such as the medical healthcare product, cosmetics, food and the like, provides a new thought for the high value application of the agriculture product and the aquatic product, effectively solves the overstandard heavy metal problem in the agriculture product and the aquatic product, and has promising application prospect.
Description
Technical field:
The present invention relates to a kind of preparation technology who is used for sea-tangle juice heavy-metal residual deresinate.To heavy metal removing rate height in the agricultural product, production technology is simple, and is with low cost, and safety with the resin of the present invention preparation.Can be used as a kind of novel heavy metal removing material, be widely used in fields such as food, medicine and health products.
Background technology:
(arsenic As) is a kind of poisonous chemical element to arsenic.It mainly exists with atom arsenic, trivalent arsenic or pentavalent arsenic form, and generally speaking, inorganic arsenic is than organo-arsenic poison, and trivalent arsenic is than pentavalent arsenic strong toxicity.Arsenic is usually used in pesticide, anticorrisive agent, feed addictive (arsanilic acid) and some industrial materials.Therefore the arsenic that uses in the industrial and agricultural production finally will enter environment, and wherein most arsenic finally all will flow into the sea, and causes that arsenic content exceeds standard in the sea-tangle far away.It is reported that arsenic content is higher in the marine product, especially total arsenic amount is the highest in the marine alga.
Sea-tangle is the important kind of China natural algae field and sea-farming, in China resource distribution is widely arranged, poly complexs such as the polysaccharide on the sea-tangle cell membrane, protein, phosphatide provide the functional group that can combine with heavy metal ion in a large number, can fully contact with heavy metal ion, easy Adsorption of Heavy Metal Ions is arsenic especially.Total arsenic content per kilogram in the general sea-tangle can be up to the arsenic of dozens or even hundreds of milligram, far above the drinking water safety standard of 0.01 μ g/g.Sea-tangle is except that direct human consumption, and is most all as food additives, chemical industry and medical raw material.Because arsenic content is higher in the sea-tangle, bring higher arsenic content residue problem for the finely processed product of sea-tangle, had a strong impact on the deep processing development of sea-tangle, yet Shang Weijian there is the residual removal methods of arsenic in pair sea-tangle deep processed product.Therefore how to remove in sea-tangle juice and the relevant agricultural product that arsenic is residual to be very necessary and to be extremely urgent.
Summary of the invention:
The present invention provides a kind of residual resin of sea-tangle juice arsenic that is used for removing, preparation technology's technology of its resin is: with polysaccharide powder join carry out adsorption reaction in the arsenic solution after, 1. wash the shitosan powder with reagent, to remove unnecessary arsenic, to be dissolved in reagent after the shitosan powder oven dry after the washing 2. in the solution, adopt crosslinking agent to carry out crosslinked preparation polysaccharide arsenic resin respectively, use earlier benzinum, acetone and ethanol cyclic washing, adopt the 3. solution arsenic in the desorb polysaccharide resins repeatedly of reagent at last, till vulcanized sodium detects less than arsenic, dry about 60 ℃, must remove the resin of residual heavy metal arsenic in the sea-tangle juice.
1., 2. and 3. reagent described in the above-mentioned technological process be respectively water, acetate and watery hydrochloric acid; Crosslinking agent is formaldehyde and glutaraldehyde, or formaldehyde and epoxychloropropane; Polysaccharide is any in agarose, starch, shitosan or the chitosan oligosaccharide.
This product is that a kind of diameter is the spherical small porous particle of 20～500 μ m, and is white or yellow.This product is insoluble to conventional organic solvent, as acetone, ethyl acetate, chloroform, ether.The pH scope 2.0～12.0 that this product uses, 4～40 ℃ of the temperature ranges of use; This product not only has the effect that removes preferably to arsenic in the sea-tangle juice, also has the separating clarifying effect, can be applicable to aspects such as sea-tangle juice, fruit and vegetable juice processing, instant tea processing, the preparation of plant source active component.
The specific embodiment:
2～20g polysaccharide is joined in 50～300ml, 5～210mg/L arsenic solution, and 10～60 ℃ of condition lower magnetic forces stir 24h, the shitosan arsenic-adsorbing is reached capacity the polysaccharide arsenic-adsorbing is reached capacity.Adopt ultra-pure water with shitosan powder cyclic washing, suction filtration is till detecting less than arsenic with 0.5～5% vulcanized sodium.The shitosan powder that obtains is dissolved in after 60 ℃ of oven dry in 1%～5% acetate acid solution in the polysaccharide powder that will obtain.Adopt formaldehyde and glutaraldehyde or epoxychloropropane to do the precrosslink agent under 20～80 ℃ of conditions respectively and crosslinking agent prepares shitosan arsenic resin, benzinum, acetone and ethanol cyclic washing are adopted in the back; The hydrochloric acid solution that compound resin after the washing is adopted 0.1～2.0mol/L is the heavy metal arsenic of its absorption of desorb repeatedly, every washing in 2 hours once, and till vulcanized sodium can not detect arsenic.Eluted resins 60 ℃ of oven dry, is made and removes residual heavy metal arsenic resin finished product in the sea-tangle juice.
Example 1: get the 10g shitosan and join in the 200ml 10mg/L standard arsenic solution, 40 ℃ of condition lower magnetic forces stir 24h, and the shitosan arsenic-adsorbing is reached capacity.Adopt ultra-pure water cyclic washing shitosan powder, suction filtration is not till can detecting arsenic with 2% vulcanized sodium.The shitosan powder that obtains 50 ℃ of oven dry, is dissolved in 24h in 2% acetic acid solution.Under 50 ℃ and 60 ℃ of conditions, adopt formaldehyde and glutaraldehyde to prepare shitosan arsenic compound resin respectively, adopt benzinum, acetone and ethanol cyclic washing as precrosslink agent and crosslinking agent; The hydrochloric acid solution that compound resin after the washing is adopted 0.2mol/L is the heavy metal arsenic of its absorption of desorb repeatedly, every washing in 2 hours once, and till 2% vulcanized sodium can not detect arsenic.Eluted resins 60 ℃ of oven dry, is made the resin finished product that removes residual heavy metal arsenic in the sea-tangle juice.
Example 2: get the 10g agarose and join in the 200ml 10mg/L standard arsenic solution, 40 ℃ of condition lower magnetic forces stir 24h, and the agarose arsenic-adsorbing is reached capacity.Adopt ultra-pure water cyclic washing agarose powder, suction filtration is not till can detecting arsenic with 2% vulcanized sodium.The agarose powder that obtains 50 ℃ of oven dry, is dissolved in 24h in 2% acetic acid solution.Under 50 ℃ and 60 ℃ of conditions, adopt formaldehyde and epoxychloropropane to prepare the agar glycolipid respectively, adopt benzinum, acetone and ethanol cyclic washing as precrosslink agent and crosslinking agent; The hydrochloric acid solution that compound resin after the washing is adopted 0.2mol/L is the heavy metal arsenic of its absorption of desorb repeatedly, every washing in 2 hours once, and till 2% vulcanized sodium can not detect arsenic.Eluted resins 60 ℃ of oven dry, is made cross-linked chitosan arsenic template resin finished product.
Claims (4)
1. resin preparation process that removes residual heavy metal arsenic in the sea-tangle juice is characterized in that step is as follows:
(1) the 2-20g shitosan is joined in the 50-300ml 5-20mg/L arsenic solution, 20-60 ℃ of condition lower magnetic force stirs 0.5-24h, and shitosan arsenic-adsorbing ion is reached capacity.
(2) adopt ultra-pure water with shitosan powder cyclic washing, suction filtration is till detecting less than arsenic with 0.5-5% vulcanized sodium.
(3) with the shitosan powder that obtains 20-60 ℃ of oven dry, after be dissolved in 8-36h in the 1%-5% acetic acid solution.Adopt formaldehyde and glutaraldehyde to prepare shitosan arsenic resin as precrosslink agent and crosslinking agent under 20-80 ℃ of condition respectively, benzinum, acetone and ethanol cyclic washing are adopted in the back.
(4) the hydrochloric acid solution heavy metal arsenic of its absorption of desorb repeatedly that adopts 0.1-2-0mol/L of the compound resin after will washing, every washing in 1-8 hour once, till vulcanized sodium can not detect.Eluted resins 30-60 ℃ of oven dry, is made shitosan arsenic template resin finished product.
2. according to the technology of claim 1 preparation chitosan resin, it is characterized in that: wash conditions is the concentration of control washing times and vulcanized sodium in described (2).
3. according to the technology of claim 1 preparation chitosan resin, it is characterized in that: dissolution time can be decided according to actual conditions in described (3).General 3-4 time of washing times.
4. according to the technology of claim 1 preparation chitosan resin, it is characterized in that: washing times is generally 6 times in described (4), and drying time is determined on a case-by-case basis.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010119859A CN101773819A (en) | 2010-03-04 | 2010-03-04 | Resin preparation process for removing residual heavy metal arsenic in laminaria seaweed extract |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010119859A CN101773819A (en) | 2010-03-04 | 2010-03-04 | Resin preparation process for removing residual heavy metal arsenic in laminaria seaweed extract |
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| CN101773819A true CN101773819A (en) | 2010-07-14 |
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| CN201010119859A Pending CN101773819A (en) | 2010-03-04 | 2010-03-04 | Resin preparation process for removing residual heavy metal arsenic in laminaria seaweed extract |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104012818A (en) * | 2014-05-18 | 2014-09-03 | 曹庸 | Method for reducing heavy metals in edible mushrooms and Chinese herbal medicines by solvent extraction |
| CN110845032A (en) * | 2019-11-01 | 2020-02-28 | 自然资源部第三海洋研究所 | Method for recycling kelp blanching liquid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020043496A1 (en) * | 2000-08-01 | 2002-04-18 | Boddu Veera M. | Composite biosorbent for treatment of waste aqueous system(s) containing heavy metals |
| CN1616505A (en) * | 2004-09-30 | 2005-05-18 | 北京理工大学 | Process for preparing chitosan base macroporous high water absorptive resin |
-
2010
- 2010-03-04 CN CN201010119859A patent/CN101773819A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20020043496A1 (en) * | 2000-08-01 | 2002-04-18 | Boddu Veera M. | Composite biosorbent for treatment of waste aqueous system(s) containing heavy metals |
| CN1616505A (en) * | 2004-09-30 | 2005-05-18 | 北京理工大学 | Process for preparing chitosan base macroporous high water absorptive resin |
Non-Patent Citations (1)
| Title |
|---|
| 《江西科学》 20080630 郑重等 交联壳聚糖的合成及其对重金属离子吸附的研究进展 第421-425页 1-4 第26卷, 第3期 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104012818A (en) * | 2014-05-18 | 2014-09-03 | 曹庸 | Method for reducing heavy metals in edible mushrooms and Chinese herbal medicines by solvent extraction |
| CN110845032A (en) * | 2019-11-01 | 2020-02-28 | 自然资源部第三海洋研究所 | Method for recycling kelp blanching liquid |
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Application publication date: 20100714 |