CN104888717A - Modified vermiculite mercury removal adsorbent, preparation method and application thereof - Google Patents
Modified vermiculite mercury removal adsorbent, preparation method and application thereof Download PDFInfo
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- CN104888717A CN104888717A CN201410074037.9A CN201410074037A CN104888717A CN 104888717 A CN104888717 A CN 104888717A CN 201410074037 A CN201410074037 A CN 201410074037A CN 104888717 A CN104888717 A CN 104888717A
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Abstract
Belonging to the technical field of wastewater treatment, the invention in particular relates to a modified vermiculite mercury removal adsorbent, a preparation method and application thereof. The method includes: taking vermiculite as the main raw material, soaking vermiculite with thickness of 0.6-1mm and a particle size of 7-8mm with 25% hydrogen peroxide, performing heating, then placing the vermiculite in certain power microwave to perform heating, thus obtaining expanded vermiculite, grinding the expanded vermiculite to less than 100 meshes, then conducting further modification with a certain amount of chitosan to obtain the modified vermiculite adsorbent with a chitosan loading capacity of 0.01g/g-0.05g/g, and applying the adsorbent for treatment of mercury-containing wastewater. The modified vermiculite mercury removal adsorbent prepared by the method provided by the invention has the advantages of low price, simple operation and the like, and mercury removal examples prove that the adsorbent has fast adsorption speed and strong adsorption capacity to mercury ions, and can be used for treatment of mercury-containing wastewater with a wide concentration range.
Description
Denomination of invention
A kind of PERFORMANCE OF MODIFIED VERMICULITE mercury-removing adsorbent and preparation method thereof and application
1 technical field
The invention belongs to technical field of waste water processing, be specifically related to a kind of PERFORMANCE OF MODIFIED VERMICULITE mercury-removing adsorbent and preparation method thereof and application.
2 background technologies
China is mercury consumption and big producing country, there is a variety of approach in the source of mercury pollution, wherein the industry such as fire coal, chlor-alkali manufacture, non-ferrous metal metallurgy, electronic waste process, manufacture of cement, battery, electrolysis all can be discharged a large amount of containing mercury contaminants in environment, mercury pollution is day by day serious, causes great threat to environment and the mankind.Mercury and derivative organic mercury thereof, because having the characteristics such as the bioconcentration of easy animal migration, persistence, high bio-toxicity and height, receive the very big concern in the whole world as a kind of very serious toxic pollutant.Mercury can exist lastingly in food chain and air, huge to the murder by poisoning of human body, and its effect comprises Toxicity of Kidney, neurotoxicity, genotoxicity, Cardiovascular Toxicity and immune system toxicity etc., so mercury pollution must strictly control.Removal of mercury method for waste water common at present has chemical precipitation method, reducing process, ion-exchange-resin process, absorption method etc., wherein absorption method is because it is easy and simple to handle, cheap, efficiency advantages of higher is widely used, so it is crucial for finding a kind of adsorbent of good performance.
Nonmetallic mineral, as one of the adsorbent of practical application, is progressively applied, and becomes one of focus of current research and exploitation.Some clay minerals have feature that is cheap, rich reserves as bentonite, diatomite, zeolite etc., have been used to the process of waste water.Vermiculite adsorbing research report is also more.Vermiculite is the special moisture layer silicate mineral of a class, have that specific area is large, absorption property good, ion-exchange capacity is strong, rich reserves, the feature such as with low cost, so be widely used in the aspects such as heavy metal containing wastewater treatment, edible oil refinery decolorization, petroleum cleanup, sewage disposal.The nonmetal mineral of advantage of vermiculite mineral Ye Shi China, its ore deposit reserve is normally large-scale and superhuge, its mineral are also relatively pure, the ore dressing of vermiculite and purification are all than being easier to, therefore in view of it, there is the features such as specific area is large, ion-exchange capacity is strong, absorption property is good, rich reserves, wide material sources, with low cost, treatment process is relatively simple, carry out the research that vermiculite mineral makes adsorbent and have broad application prospects.
The limited sorption capacity of former vermiculite, so researchers are devoted to the modification of vermiculite, to improve the absorption property of vermiculite.The common method of modifying of vermiculite has sour modification, chemical modification, heat modification, organically-modified etc.Conventional heat modification method has Muffle furnace calcining, heating using microwave etc., and wherein more difficult control temperature calcined by Muffle furnace, inconvenient operation, is paid close attention to gradually so heating using microwave has the advantages such as heat time short, efficiency is high, easy control due to it.In chemical modifier, hydrogen peroxide can make vermiculite reach good expansion effect, and its mechanism of intumescence to produce oxygen in decomposable process pressure when hydrogen peroxide molecule in vermiculite crystal layer interlamination region, and vermiculite structure sheaf is dissociated expansion.
Shitosan is the main component of shellfish shell, and is one of the abundantest biopolymer of occurring in nature.Because shitosan has high amino group, can with heavy metal ion generation chelation, so heavy metal has superior adsorption capacity, be widely used in heavy metal containing wastewater treatment.Although shitosan is very effective to the removal of metal ion, shitosan has many shortcomings equally, and such as density is little, sinking speed is slow, cause solid and fluid separation applications difficulty, easily losing in acid solution, therefore, is very expensive with shitosan process waste water merely.
The present invention adopts microwave heating method easy and simple to handle and the combined modified technology of hydrogen peroxide to carry out expansion-modifying to former vermiculite.First, hydrogen peroxide molecule in the vermiculite crystal layer interlamination region pressure that produces oxygen in decomposable process makes vermiculite structure sheaf dissociate expansion, by heating using microwave, the vapour pressure formed between vermiculite layers is increased again, and then cause the further increase of expansion multiple, so under hydrogen peroxide and microwave double action, expanding vermiculite multiple is larger, to increase vermiculite specific area and cation exchange capacity, improves adsorption capacity.On this basis, chitin modified dose that Selection effect is good is carried out further modification to expanded vermiculite, shitosan is adsorbed onto on vermiculite, the shortcomings such as shitosan density is little can be overcome, play simultaneously its amino can with the advantage of mercury ion generation chelation, thus more strengthen PERFORMANCE OF MODIFIED VERMICULITE to the removal of mercury ion.So have broad application prospects as mercury-removing adsorbent by PERFORMANCE OF MODIFIED VERMICULITE of the present invention.
3 summary of the invention
The object of the invention is to cause significant damage for mercury-containing waste water to human body and environment, and the shortcomings such as active carbon class mercury-removing adsorbent is expensive, provide a kind of preparation method of cheap, preparation technology is simple, absorption property is excellent PERFORMANCE OF MODIFIED VERMICULITE mercury-removing adsorbent.
Another object of the present invention is to provide a kind of PERFORMANCE OF MODIFIED VERMICULITE mercury-removing adsorbent removing the application in mercury-containing waste water.
The former vermiculite filtered out first carries out expansion-modifying by the present invention, it is made to reach maximum swelling effect by hydrogen peroxide modification and microwave modification, to increase vermiculite specific area and absorption property, then expanded vermiculite shitosan is carried out further modification, further improve the mercury removal performance of vermiculite.Adsorbent of the present invention is owing to having the ion-exchange performance of expanded vermiculite itself, reach the absorption to mercury ion, add the amino further chelation to mercury ion on shitosan, can reach mercury ion under double action and remove well, and speed of removing is fast, efficiency is high, the removal of mercury is in extensive range, no matter effectively can be removed the mercury-containing waste water of high concentration or trace, Trace mercury waste water, be reached discharging standards.Mercury-removing adsorbent of the present invention has the features such as cheap, preparation technology is simple, absorption property is excellent, has great application prospect.
The following technology of preparation method of the PERFORMANCE OF MODIFIED VERMICULITE adsorbent of a kind of removal of mercury of the present invention is implemented:
1. be raw material with vermiculite in invention, the vermiculite size screened is: vermiculite thickness is 0.6-1mm, particle diameter is 7-8mm, washs post-drying with distilled water, for subsequent use.
2. be stir and evenly mix the vermiculite solid-to-liquid ratio in 1 after 25% hydrogen peroxide dipping of 1: 10, at 80 DEG C, heating and thermal insulation remains to no liquid, with microwave high fire heating 1-2min after taking out, then levigate for subsequent use to being less than 100 orders.
3. getting a certain amount of shitosan with solid-to-liquid ratio is that 1: 1000-1: 200 to be dissolved in volume fraction be in the acetum of 1%, makes it slowly fully dissolve, obtained chitosan solution.Be join in chitosan solution at 1: 10 by the vermiculite in 2 by solid-to-liquid ratio, fully infiltrate, at 50 DEG C, heat 2h, constantly stir in process.React complete, after being dried by mixture, grinding is opened, and obtained chitosan loaded amount is the PERFORMANCE OF MODIFIED VERMICULITE adsorbent of 0.01g/g-0.05g/g.
The mercury ion that PERFORMANCE OF MODIFIED VERMICULITE adsorbent of the present invention is mainly used in mercury-containing waste water is removed, and its application key step is as follows:
The chitin modified vermiculite absorbent prepared is joined in mercury-containing waste water in proportion, filters after stirring and adsorbing certain hour, the rear discharge up to standard of supernatant liquor mercury ion content.
In above-mentioned PERFORMANCE OF MODIFIED VERMICULITE removal of mercury application, in mercury-containing waste water, ion concentration of mercury is in extensive range, can be high concentration mercury waste water, also can be low mercury or Trace Hg waste water; In mercury-containing waste water, water body pH scope is at 6-7; In mercury-containing waste water, water temperature is room temperature.
The invention has the advantages that and first carry out expansion-modifying by hydrogen peroxide and microwave combined technology to vermiculite by vermiculite, make its maximum swelling multiple can reach 30-40 doubly, this result is higher than the report of current most of document.Then in order to improve vermiculite adsorption effect further, shitosan is carried out modification to expanded vermiculite again as modifier, under optimum adsorption conditions, the discharge standard (0.05mg/L) of country's permission can be reached by the mercury-containing waste water after chitin modified vermiculite absorbent absorption.Mercury-removing adsorbent of the present invention has the features such as cheap, preparation technology is simple, absorption property is excellent, and adsorption efficiency is high, particular/special requirement is not had to adsorption conditions, namely in room temperature, pH is neutral left and right, adsorption time 40min just can be removed mercury-containing waste water well, is suitable for practical application.
4 detailed description of the invention
Below by specific embodiment, a kind of PERFORMANCE OF MODIFIED VERMICULITE mercury-removing adsorbent of the present invention and preparation method thereof is described in detail with application.But the present invention is not limited to the example enumerated.
Embodiment 1
1. former vermiculite is filtered out the vermiculite sample that thickness is 0.6-1mm, particle diameter is 7-8mm, wash post-drying with distilled water, for subsequent use.
2. be stir and evenly mix the vermiculite solid-to-liquid ratio in 1 after 25% hydrogen peroxide dipping of 1: 10, at 80 DEG C, heating and thermal insulation remains to no liquid, with microwave high fire heating 1min after taking out, then levigate for subsequent use to being less than 100 orders.
3. shitosan being dissolved in volume fraction with the ratio that solid-to-liquid ratio is 1: 1000-1: 200 is in the acetum of 1%, makes it slowly fully dissolve, obtained chitosan solution.Be join in chitosan solution at 1: 10 by the vermiculite in 2 by solid-to-liquid ratio, fully infiltrate, at 50 DEG C, heat 2h, constantly stir in process.React complete, mixture is dried grinding and opens, obtained chitosan loaded amount is the chitin modified vermiculite absorbent of 0.01g/g-0.05g/g.
4. be 1: 7.5 × 10 by chitin modified vermiculite according to quantity of sorbent and mercury ion amount
-3ratio join in mercury ion waste water, regulate pH value of solution to neutral, filter after stirred at ambient temperature 1h, measure mercury ion content in supernatant, obtaining removal effect when chitosan loaded amount is 0.05g/g best, is 93%.
Embodiment 2
1. former vermiculite is filtered out the vermiculite sample that thickness is 0.6-1mm, particle diameter is 7-8mm, wash post-drying with distilled water, for subsequent use.
2. be stir and evenly mix the vermiculite solid-to-liquid ratio in 1 after 25% hydrogen peroxide dipping of 1: 10, at 80 DEG C, heating and thermal insulation remains to no liquid, with microwave high fire heating min after taking out, then levigate for subsequent use to being less than 100 orders.
3. shitosan being dissolved in volume fraction with the ratio that solid-to-liquid ratio is 1: 200 is in the acetum of 1%, makes it slowly fully dissolve, obtained chitosan solution.Be join in chitosan solution at 1: 10 by the vermiculite in 2 by solid-to-liquid ratio, fully infiltrate, at 50 DEG C, heat 2h, constantly stir in process.React complete, after being dried by mixture, grinding is opened, and obtained chitosan loaded amount is the chitin modified vermiculite absorbent of 0.05g/g.
4. be 1: 7.5 × 10 by chitin modified vermiculite according to quantity of sorbent and mercury ion amount ratio
-3ratio join in mercury ion waste water, pH value of solution is transferred to 4-8, filters after stirred at ambient temperature 1h, and measure mercury ion content in supernatant, can obtain pH value of solution the highest at about 6-7 clearance, be 95%.
Embodiment 3
1. former vermiculite is filtered out the vermiculite sample that thickness is 0.6-1mm, particle diameter is 7-8mm, wash post-drying with distilled water, for subsequent use.
2. be stir and evenly mix the vermiculite solid-to-liquid ratio in 1 after 25% hydrogen peroxide dipping of 1: 10, at 80 DEG C, heating and thermal insulation remains to no liquid, with microwave high fire heating 1min after taking out, then levigate for subsequent use to being less than 100 orders.
3. shitosan being dissolved in volume fraction with the ratio that solid-to-liquid ratio is 1: 200 is in the acetum of 1%, makes it slowly fully dissolve, obtained chitosan solution.Be join in chitosan solution at 1: 10 by the vermiculite in 2 by solid-to-liquid ratio, fully infiltrate, at 50 DEG C, heat 2h, constantly stir in process.React complete, after being dried by mixture, grinding is opened, and obtained chitosan loaded amount is the chitin modified vermiculite absorbent of 0.05g/g.
4. be 1: 7.5 × 10 by chitin modified vermiculite according to adsorbent and mercury ion amount ratio
-3ratio join in mercury ion waste water, pH value of solution is transferred to 6-7, filters after stirred at ambient temperature 10-50min, measures mercury ion content in supernatant, reaches adsorption equilibrium after can obtaining absorption 30-40min.
Embodiment 4
1. former vermiculite is filtered out the vermiculite sample that thickness is 0.6-1mm, particle diameter is 7-8mm, wash post-drying with distilled water, for subsequent use.
2. be stir and evenly mix the vermiculite solid-to-liquid ratio in 1 after 25% hydrogen peroxide dipping of 1: 10, at 80 DEG C, heating and thermal insulation remains to no liquid, with microwave high fire heating 1min after taking out, then levigate for subsequent use to being less than 100 orders.
3. shitosan being dissolved in volume fraction with the ratio that solid-to-liquid ratio is 1: 200 is in the acetum of 1%, makes it slowly fully dissolve, obtained chitosan solution.Be join in chitosan solution at 1: 10 by the vermiculite in 2 by solid-to-liquid ratio, fully infiltrate, at 50 DEG C, heat 2h, constantly stir in process.React complete, after being dried by mixture, grinding is opened, and obtained chitosan loaded amount is the chitin modified vermiculite absorbent of 0.05g/g.
4. be 1: 7.5 × 10 by chitin modified vermiculite according to quantity of sorbent and mercury ion amount ratio
-3with 1: 1.5 × 10
-4ratio join in mercury ion waste water, pH value of solution is transferred to 6-7, filters after stirred at ambient temperature 40min, measures mercury ion content in supernatant, finally calculating the former to mercury ion clearance is 96%, and the latter obtains the mercury-containing waste water after adsorbing can reach discharging standards completely.
Claims (5)
1. PERFORMANCE OF MODIFIED VERMICULITE mercury-removing adsorbent and preparation method thereof and application, its feature is: take vermiculite as raw material, filtered out a certain size former vermiculite, below 100 orders are ground to after making it expand with finite concentration hydrogen peroxide and microwave, shitosan is selected to be that modifier carries out immersion modification to it again, obtained chitin modified vermiculite mercury-removing adsorbent after drying, and be applied to the process of mercury-containing waste water.
2., according to PERFORMANCE OF MODIFIED VERMICULITE mercury-removing adsorbent described in claim 1 and preparation method thereof, it is characterized in that the vermiculite size screened is: vermiculite thickness is 0.6-1mm, particle diameter is 7-8mm.
3., according to PERFORMANCE OF MODIFIED VERMICULITE mercury-removing adsorbent described in claim 1 and preparation method thereof, it is characterized in that comprising the following steps:
1) expanded vermiculite preparation: the vermiculite distilled water in right 2 is washed post-drying, then the ratio being 1: 10 according to solid-to-liquid ratio joins in the hydrogen peroxide of 25% soaks, stir and evenly mix, at 80 DEG C, heating and thermal insulation remains to no liquid, with microwave high fire heating 1-2min after taking out, then levigate for subsequent use to being less than 100 orders.
2) chitosan solution preparation: getting a certain amount of shitosan, to be dissolved in volume fraction with the ratio that solid-to-liquid ratio is 1: 1000-1: 200 be in the acetum of 1%, makes it slowly fully dissolve, obtained chitosan solution.
3) chitin modified vermiculite preparation process: by step 1) in vermiculite be join step 2 at 1: 10 by solid-to-liquid ratio) in chitosan solution in, fully infiltrate, at 50 DEG C, heat 2h, constantly stir in process.React complete, after being dried by mixture, grinding is opened, and obtained chitosan loaded amount is the PERFORMANCE OF MODIFIED VERMICULITE adsorbent of 0.01g/g-0.05g/g.
According to the application of the PERFORMANCE OF MODIFIED VERMICULITE adsorbent described in right 1, it is characterized in that the mercury ion for mercury-containing waste water is removed.
4. according to the application of the PERFORMANCE OF MODIFIED VERMICULITE adsorbent described in right 1, it is characterized in that with the PERFORMANCE OF MODIFIED VERMICULITE adsorbent in claim 3 as follows for the absorption concrete steps of mercury ion: the chitin modified vermiculite absorbent prepared is joined in mercury-containing waste water by a certain percentage, filter after stirring and adsorbing certain hour, the rear discharge up to standard of supernatant liquor mercury ion content.
5. according to the application of the PERFORMANCE OF MODIFIED VERMICULITE mercury-removing adsorbent described in right 4, it is characterized in that in mercury-containing waste water, ion concentration of mercury is in extensive range, can be high concentration mercury waste water, also can be low mercury or Trace Hg waste water; In mercury-containing waste water, water body pH scope is at 6-7; In mercury-containing waste water, water temperature is room temperature.
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Application publication date: 20150909 |