CN105694902A - Passivator for heavy-metal polluted soil, and preparation method and application thereof - Google Patents
Passivator for heavy-metal polluted soil, and preparation method and application thereof Download PDFInfo
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- CN105694902A CN105694902A CN201610064068.5A CN201610064068A CN105694902A CN 105694902 A CN105694902 A CN 105694902A CN 201610064068 A CN201610064068 A CN 201610064068A CN 105694902 A CN105694902 A CN 105694902A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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Abstract
The invention discloses a passivator for heavy-metal polluted soil, and a preparation method and application thereof. The passivator is mainly composed of modified zeolite and modified chitosan carried on the modified zeolite. The chemical structure general formula of the modified chitosan is disclosed as Formula I, wherein R is disclosed in the specification. The preparation method comprises the steps of preparation of the modified chitosan, preparation of the modified zeolite and preparation of the passivator. The passivator has the advantages of favorable adsorbability and low cost, can effectively enhance the passivation effects of heavy metals in soil, is suitable for treating soil heavy metals, and is especially suitable for treating heavy metals in polluted agricultural land.
Description
Technical field
The invention belongs to heavy metal-polluted soil passivating technique field, be specifically related to a kind of passivator for heavy-metal contaminated soil and its preparation method and application。
Background technology
Soil is important natural resources, and it is the material base of agricultural development, is the source of the base stock that people depend on for existence。Soil once contaminated, hardly results in reparation after being especially subject to heavy metal pollution。Heavy metal pollution of soil become instantly widest in area, endanger one of maximum environmental problem。Heavy metal pollution brings many adverse influences to proportion of crop planting, for instance the reduction of the yield and quality of soil fertility and crop, the threat etc. that the life and health of the mankind is subject to due to food chain。
Heavy metal pollution of soil has become as the environmental problem received significant attention in the world, and relative recovery technique is always up the focus studied in the world, simultaneously also because the complexity polluted also becomes the difficult point of environmental improvement。The approach administering heavy-metal contaminated soil mainly has two kinds: one to be change heavy metal existing forms in soil, reduce its animal migration in the environment and biological effectiveness, make it be become stable state from activated state, there are some researches show that reducing heavy metal available state activity can play the effect of heavy metal-passivated its toxicity of minimizing；Two is removal heavy metal from soil, so that it retains concentration close to or up background value。Specifically include engineering measure, chemical, agricultural measures and biological control measure etc.。
In the various technology administering heavy metal pollution of soil, passivation recovery technique is subject to people more and more payes attention to the advantage such as easy, quick, effective and economical and practical。But it is clearly disadvantageous in actual use to there are some in existing passivator。At present, conventional passivator has alkaline matter, clay mineral, organic materials, synthetic material etc., all has problems to a certain extent。
In alkaline matter the most commonly used with Calx, its heavy metal fixing mainly through improving soil pH value, make heavy metal generate oxide or precipitate with the form of carbonate and work, hence it is evident that reduce the bio-available Zn concentration of heavy metal-polluted soil。Liming can suppress plant absorption heavy metal, the content that can be effectively reduced in soil water-soluble state and exchange adsorption state heavy metal。But excessive interpolation Calx can cause the change of soil physico-chemical property, thus inhibiting the yield of crop, limit its practical application。
Clay mineral is a class rich reserves, eco-friendly natural material, has good absorption property, and becomes widely used inorganic carrier material because of the layer structure of its uniqueness, the most general with graft process in carrying method。Graft process realizes functionalization load by ion exchange in solution, and its preparation method is relatively easy。But there is the problems such as specific surface area is low, load is uneven, grafting key is more weak in the material modified of gained by this method。As modifiied with modal cetyl trimethylammonium bromide, the specific surface area of the modified clays such as zeolite, bentonite, montmorillonite, Vermiculitum is all relatively low, lacks enough pore passage structures, causes that its practicality is substantially reduced。
Organic materials such as chitosan is a kind of natural organic high-molecular flocculant, containing reactive group-NH in strand2With-OH, metal ion had stronger combination。Chitosan can form the cationic polyelectrolyte of high charge density in an acidic solution, good complex performance and flocculating property can be demonstrated in an acidic solution, have nontoxic, do not produce the advantages such as secondary pollution, biological degradability be good, thus be a kind of very good heavy metal absorbent。But, chitosan exists that relative molecular mass is little, bridge formation ability, degree of crystallinity are higher simultaneously, fragility is relatively big, the shortcoming that particularly cost is high。And chitosan can dissolve in acid condition, the adsorption effect of heavy metal ion is easily affected by the external environment so that the application of chitosan is very restricted。
Therefore, seek the novel passivator being conducive to improving heavy metal passivation effect and agricultural land soil repairing effect and become the task of top priority。
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, it is provided that a kind of absorption property is good, with low cost, the passivator for heavy-metal contaminated soil that can be effectively improved heavy metal in soil passivation effect and its preparation method and application。
For solving above-mentioned technical problem, the present invention by the following technical solutions:
A kind of passivator for heavy-metal contaminated soil, described passivator is mainly made up of modified zeolite and the modification of chitosan being carried on modified zeolite；The chemical structure of general formula of described modification of chitosan is lower formula I:
Wherein, R is
In the above-mentioned passivator for heavy-metal contaminated soil, it is preferred that the dynamic viscosity of described modification of chitosan is 50mPa s～800mPa s。
Conceive as a total technology, the preparation method that the present invention also provides for a kind of passivator for heavy-metal contaminated soil, comprise the following steps:
(1) preparation of modification of chitosan: dissolve the chitosan in acetic acid solution, adds modifying agent, and described modifying agent is phosphorous acid and formalin or is hypophosphorous acid and formalin, after agitated reaction, cools down, precipitates and dry, obtains modification of chitosan；
The preparation of modified zeolite: added in aqueous slkali by zeolite and boil, is washed out, dries and pulverizes, obtain modified zeolite；
(2) preparation of passivator: weigh step (1) gained modified zeolite and modification of chitosan, adds in the acetic acid solution of modification of chitosan by modified zeolite, after being sufficiently stirred for, dry, obtains the passivator for heavy-metal contaminated soil。
In the preparation method of the above-mentioned passivator being used for heavy-metal contaminated soil, preferably, in the preparation of the modification of chitosan of described step (1), described chitosan: phosphorous acid or hypophosphorous acid: the amount ratio of formalin is 1g: 0.2g～2g: 0.1mL～1.2mL, the mass concentration of described formalin is 20%～40%。When adopting hypophosphorous acid, generally adding with the form of hypophosphorous acid solution in the acetic acid solution of chitosan, the mass concentration of hypophosphorous acid solution is preferably 50%。
The preparation method of the above-mentioned passivator for heavy-metal contaminated soil, it is preferred that in described step (2), the mass ratio of described modification of chitosan and modified zeolite is 1: 5～50。
The preparation method of the above-mentioned passivator for heavy-metal contaminated soil, it is furthermore preferred that in described step (2), the mass ratio of described modification of chitosan and modified zeolite is 1: 15～30。
The preparation method of the above-mentioned passivator for heavy-metal contaminated soil, it is preferred that in the preparation of the modified zeolite of described step (1): described aqueous slkali is sodium hydroxide solution, the mass concentration of described sodium hydroxide solution is 3%～6%；The solid-to-liquid ratio of described zeolite and aqueous slkali is 1g: 1mL～10mL；Described boil after keep 1h～3h；10 order～200 mesh sieves are crossed after described pulverizing。
The preparation method of the above-mentioned passivator for heavy-metal contaminated soil, it is preferred that in the preparation of the modified zeolite of described step (1): described aqueous slkali is sodium hydroxide solution, the mass concentration of described sodium hydroxide solution is 3%～6%；The solid-to-liquid ratio of described zeolite and aqueous slkali is 1g: 1mL～10mL；Described boil after keep 1h～3h；10 order～200 mesh sieves are crossed after described pulverizing。
The preparation method of the above-mentioned passivator for heavy-metal contaminated soil, preferably, in the preparation of the modification of chitosan of described step (1), described modifying agent is to add when 70 DEG C～90 DEG C of waters bath with thermostatic control, the time of described stirring reaction is 1h～5h, and described precipitation is to adopt dehydrated alcohol to precipitate；In described step (2), described drying as lyophilization or drying, the temperature of described drying is 80 DEG C～120 DEG C, and the time of described drying is 1h～5h。
Conceive as total technology, the passivator for heavy-metal contaminated soil that the present invention also provides for a kind of above-mentioned passivator for heavy-metal contaminated soil or above-mentioned preparation method prepares application in heavy metal-polluted soil processes。
In above-mentioned application, it is preferred that described soil is heavy metal pollution farmland。
In the present invention, the dynamic viscosity of chitosan raw material is generally also selected in 50mPa s～800mPa s。
In the preparation method of the present invention, chitosan or modification of chitosan add in acetic acid solution and are all as the criterion with dissolving, and the mass concentration of acetic acid solution can be preferably 1%～5%, but is not limited to this。
In the preparation method of the present invention, step (1) includes the preparation of modification of chitosan and the preparation of modified zeolite, and the preparation order of the two can be exchanged, and is not construed as limiting。
Principles of the invention is as follows: zeolite is the aluminosilicate Ore that a class is natural, there is pore passage structure, stronger ion exchange and absorbability can be produced by heavy metal ion, and chitosan is the product after chitin deacetylase, there is wide material sources, the feature such as nontoxic, containing substantial amounts of hydroxyl and amino in its molecule, it is possible to carry out complexation with contents of many kinds of heavy metal ion, and adsorption occurs。The present invention passes through formaldehyde, is connected on the amino of chitosan by hypophosphorous acid or phosphorous acid, is prepared for the phosphonized chitosan of excellent adsorption, and by phosphonized chitosan is loaded on modified zeolite, reduce the amount of application of chitosan, improve passivation time, improve passivation effect。
The synthesis mechanism of the present invention is as follows:
Compared with prior art, it is an advantage of the current invention that:
(1) passivator of the present invention has zeolite and chitosan dual structure characteristic, absorption and inactivating performance well, can be effectively improved the repairing effect to heavy metal in soil。
(2) preparation method of the present invention is with modified zeolite for stock, load phosphonized chitosan, develops the new passivation agent for heavy metal pollution farmland, improves the passivation effect of heavy metal, improves the repairing effect to agricultural land soil。
Detailed description of the invention
Below in conjunction with concrete preferred embodiment, the invention will be further described, but protection domain not thereby limiting the invention。
The material adopted in following example and instrument are commercially available。
Embodiment 1:
A kind of passivator for heavy-metal contaminated soil of the present invention, this passivator is mainly made up of modified zeolite and the modification of chitosan (phosphorous acid chitosan) being carried on modified zeolite, and the chemical structure of general formula of modification of chitosan is lower formula I:
Wherein, R isThe dynamic viscosity of this modification of chitosan is 113mPa s。
The preparation method of the passivator for heavy-metal contaminated soil of a kind of above-mentioned the present embodiment, comprises the following steps:
(1) preparation of modification of chitosan and modified zeolite:
(1.1) preparation of modification of chitosan:
Weighing 1g chitosan and be dissolved in the acetic acid solution that 50mL mass concentration is 1%, water bath with thermostatic control 80 DEG C, adds 1g phosphorous acid and 0.3mL mass concentration is the formalin of 30%, stirring reaction 2h。Precipitate with dehydrated alcohol after cooling, dry, obtain phosphorous acid chitosan, i.e. modification of chitosan。
(1.2) preparation of modified zeolite:
Weigh 50 grams of zeolites and be placed in 500mL beaker, add the sodium hydroxide solution of 250mL mass concentration 4%, boil 1h。Remove solution, be then washed till neutrality with deionized water, dry, pulverize, cross 100 mesh sieves, obtain modified zeolite。
In the present embodiment, step (1.1) and step (1.2) can exchange sequences。
(2) preparation of passivator:
Weigh 1g modification of chitosan (phosphorous acid chitosan), it is dissolved in acetic acid solution, weigh in the acetic acid solution that 20g modified zeolite joins phosphorous acid chitosan, it is sufficiently stirred for, lyophilization or at 100 DEG C dry 2h, obtain the chitin modified zeolite of phosphorous acid, namely for the passivator of heavy-metal contaminated soil。
Embodiment 2
A kind of passivator for heavy-metal contaminated soil of the present invention, this passivator is mainly made up of modified zeolite and the modification of chitosan (hypophosphorous acid chitosan) being carried on modified zeolite, and the chemical structure of general formula of modification of chitosan is lower formula I:
Wherein, R isThe dynamic viscosity of this modification of chitosan is 115mPa s。
The preparation method of the passivator for heavy-metal contaminated soil of a kind of above-mentioned the present embodiment, comprises the following steps:
(1) preparation of modification of chitosan and modified zeolite:
(1.1) preparation of modified zeolite:
Weigh 50 grams of zeolites and be placed in 500mL beaker, add the sodium hydroxide solution of 250mL mass concentration 4%, boil 1h。Remove solution, be then washed till neutrality with deionized water, dry, pulverize, cross 100 mesh sieves, obtain modified zeolite。
(1.2) preparation of modification of chitosan:
Weigh 1g chitosan and be dissolved in the acetic acid solution that 50mL mass concentration is 1%, water bath with thermostatic control 80 DEG C, add hypophosphorous acid solution and the formalin of 0.3mL mass concentration 30%, stirring reaction 2h that 2g mass concentration is 50%。Precipitate with dehydrated alcohol after cooling, dry, obtain hypophosphorous acid chitosan, i.e. modification of chitosan。
In the present embodiment, step (1.1) and step (1.2) can exchange sequences。
(2) preparation of passivator:
Weigh 1g modification of chitosan (hypophosphorous acid chitosan), it is dissolved in acetic acid solution, weigh in the acetic acid solution that 20g modified zeolite joins hypophosphorous acid chitosan, it is sufficiently stirred for, lyophilization or at 100 DEG C dry 2h, obtain the chitin modified zeolite of hypophosphorous acid, namely for the passivator of heavy-metal contaminated soil。
Embodiment 3
A kind of application of the passivator for heavy-metal contaminated soil of the present invention, the passivator (the chitin modified zeolite of phosphorous acid) of Example 1 preparation, add in contaminated soil (preferred polluted agricultural land) according to the amount of soil weight 8 ‰, mixing。After testing, compared with the contaminated soil not adding passivator, soil pH maximum lift 1.71 after interpolation passivator, the heavy metal amount that water logging is leached can reduce by 87.2%, the heavy metal amount that TCLP leaches can reduce by 41.7%, and heavy metal in soil Acid extractable can reduce by 51.8%。
Embodiment 4
A kind of application of the passivator for heavy-metal contaminated soil of the present invention, the passivator (the chitin modified zeolite of hypophosphorous acid) of Example 2 preparation, add in contaminated soil (preferred polluted agricultural land) according to the amount of soil weight 8 ‰, mixing。After testing, compared with the contaminated soil not adding passivator, soil pH maximum lift 2.27 after interpolation passivator, the heavy metal amount that water logging is leached reduces by 87.2%, and the heavy metal amount that TCLP leaches reduces by 49.9%, heavy metal in soil Acid extractable reduction by 42.7%。
The above, be only presently preferred embodiments of the present invention, and the present invention not does any pro forma restriction。Although the present invention discloses as above with preferred embodiment, but is not limited to the present invention。Any those of ordinary skill in the art, when without departing from the spirit of the present invention and technical scheme, all may utilize the method for the disclosure above and technology contents and technical solution of the present invention is made many possible variations and modification, or be revised as the Equivalent embodiments of equivalent variations。Therefore, every content without departing from technical solution of the present invention, to any simple modification made for any of the above embodiments, equivalent replacement, equivalence change and modify according to the technical spirit of the present invention, all still fall within the scope of technical solution of the present invention protection。
Claims (10)
1. the passivator for heavy-metal contaminated soil, it is characterised in that described passivator is mainly made up of modified zeolite and the modification of chitosan being carried on modified zeolite；The chemical structure of general formula of described modification of chitosan is lower formula I:
Wherein, R is
2. the passivator for heavy-metal contaminated soil according to claim 1, it is characterised in that the dynamic viscosity of described modification of chitosan is 50mPa s～800mPa s。
3., for a preparation method for the passivator of heavy-metal contaminated soil, comprise the following steps:
(1) preparation of modification of chitosan: dissolve the chitosan in acetic acid solution, adds modifying agent, and described modifying agent is phosphorous acid and formalin or is hypophosphorous acid and formalin, after agitated reaction, cools down, precipitates and dry, obtains modification of chitosan；
The preparation of modified zeolite: added in aqueous slkali by zeolite and boil, is washed out, dries and pulverizes, obtain modified zeolite；
(2) preparation of passivator: weigh step (1) gained modified zeolite and modification of chitosan, adds in the acetic acid solution of modification of chitosan by modified zeolite, after being sufficiently stirred for, dry, obtains the passivator for heavy-metal contaminated soil。
4. the preparation method of the passivator for heavy-metal contaminated soil according to claim 3, it is characterized in that, in the preparation of the modification of chitosan of described step (1), described chitosan: phosphorous acid or hypophosphorous acid: the amount ratio of formalin is 1g: 0.2g～2g: 0.1mL～1.2mL, the mass concentration of described formalin is 20%～40%。
5. the mass ratio of the preparation method of the passivator for heavy-metal contaminated soil according to claim 3, it is characterised in that in described step (2), described modification of chitosan and modified zeolite is 1: 5～50。
6. the mass ratio of the preparation method of the passivator for heavy-metal contaminated soil according to claim 5, it is characterised in that in described step (2), described modification of chitosan and modified zeolite is 1: 15～30。
7. the preparation method of the passivator for heavy-metal contaminated soil according to any one of claim 2～6, it is characterized in that, in the preparation of the modified zeolite of described step (1): described aqueous slkali is sodium hydroxide solution, the mass concentration of described sodium hydroxide solution is 3%～6%；The solid-to-liquid ratio of described zeolite and aqueous slkali is 1g: 1mL～10mL；Described boil after keep 1h～3h；10 order～200 mesh sieves are crossed after described pulverizing。
8. the preparation method of the passivator for heavy-metal contaminated soil according to any one of claim 2～6, it is characterized in that, in the preparation of the modification of chitosan of described step (1), described modifying agent is to add when 70 DEG C～90 DEG C of waters bath with thermostatic control, the time of described stirring reaction is 1h～5h, and described precipitation is to adopt dehydrated alcohol to precipitate；In described step (2), described drying as lyophilization or drying, the temperature of described drying is 80 DEG C～120 DEG C, and the time of described drying is 1h～5h。
9. the passivator for heavy-metal contaminated soil that the passivator for heavy-metal contaminated soil as claimed in claim 1 or 2 or the preparation method as according to any one of claim 3～8 prepare application in heavy metal-polluted soil processes。
10. application according to claim 9, it is characterised in that described soil is heavy metal pollution farmland。
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| CN106380049A (en) * | 2016-09-23 | 2017-02-08 | 湖南大学 | Method for remediating heavy metal polluted sediment by use of modified zeolite molecular sieve and farmland soil improvement method |
| CN106544038A (en) * | 2016-10-26 | 2017-03-29 | 中国矿业大学(北京) | A kind of preparation method of environmentally friendly polymerization based high molecular heavy metal stabilizer |
| CN111040771A (en) * | 2019-12-07 | 2020-04-21 | 重庆市固体废物管理服务中心有限公司 | Site-contaminated soil ex-situ remediation agent and application method thereof |
| CN111073658A (en) * | 2019-11-21 | 2020-04-28 | 河北建设集团安装工程有限公司 | Heavy metal contaminated soil remediation agent and preparation method and application thereof |
| CN112646587A (en) * | 2020-11-25 | 2021-04-13 | 宁波城市阳光环境建设工程有限公司 | Soil remediation composition, preparation method thereof and soil bioremediation method |
| CN113289588A (en) * | 2021-05-24 | 2021-08-24 | 江苏乐尔环境科技股份有限公司 | Chitosan modified heavy metal chelating agent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106380049B (en) * | 2016-09-23 | 2019-08-23 | 湖南大学 | Utilize the method for modified zeolite molecular sieve repairing heavy metal pollution bed mud and the modification method of agricultural land soil |
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| CN111073658A (en) * | 2019-11-21 | 2020-04-28 | 河北建设集团安装工程有限公司 | Heavy metal contaminated soil remediation agent and preparation method and application thereof |
| CN111040771A (en) * | 2019-12-07 | 2020-04-21 | 重庆市固体废物管理服务中心有限公司 | Site-contaminated soil ex-situ remediation agent and application method thereof |
| CN112646587A (en) * | 2020-11-25 | 2021-04-13 | 宁波城市阳光环境建设工程有限公司 | Soil remediation composition, preparation method thereof and soil bioremediation method |
| CN113289588A (en) * | 2021-05-24 | 2021-08-24 | 江苏乐尔环境科技股份有限公司 | Chitosan modified heavy metal chelating agent |
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