CN102500334A - Ammonium thiocyanate modified seaweed biotype absorbent and preparation method and application thereof - Google Patents
Ammonium thiocyanate modified seaweed biotype absorbent and preparation method and application thereof Download PDFInfo
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- CN102500334A CN102500334A CN201110349087XA CN201110349087A CN102500334A CN 102500334 A CN102500334 A CN 102500334A CN 201110349087X A CN201110349087X A CN 201110349087XA CN 201110349087 A CN201110349087 A CN 201110349087A CN 102500334 A CN102500334 A CN 102500334A
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Abstract
The invention discloses a preparation method of an ammonium thiocyanate modified seaweed biotype absorbent, which comprises the following steps of: drying seaweed, grinding, sieving and immersing in hydrochloric acid to obtain mixed liquid; filtering, washing and drying the mixed liquid to obtain preprocessed seaweed; drying the processed seaweed, and adding ammonium thiocyanate and chloroacetic acid; carrying out modification reaction after adjusting a pH value; and filtering, washing and drying after the reaction to obtain the ammonium thiocyanate modified seaweed biotype absorbent. The ammonium thiocyanate modified seaweed biotype absorbent is used for absorbing Cr6+, the absorbed Cr6+ can be eluted by acid, so that heavy metal is recycled, and a recycled material is reused. In the invention, ammonium thiocyanate is utilized to modify the seaweed, so that the absorption activation point of the seaweed is increased, and the capability of seaweed to absorb the heavy metal is improved. The absorbent disclosed by the invention has high absorption efficiency and volume, and is economic and suitable.
Description
Technical field
The invention belongs to the biological adsorption agent field, particularly a kind of ammonium thiocyanate modification seaweed-type adsorbent.
Background technology
Chromium and compound thereof are widely used in industry, and metallurgy, chemical industry, mineral engineering, plating, process hides, dyestuff, pharmacy, light industry spin a series of industries such as production of dyeing and weaving, chromic salts and chromium compounds, all can produce a large amount of chromate waste waters.The compound of chromium is the most common with the compound of trivalent and sexavalence, and its toxicity is then with the height of sexavalence; Cr VI is easy to be absorbed by the body, and it can invade human body through digestion, respiratory tract, skin and mucous membrane.Hoarse, schneiderian membrane atrophy in various degree arranged when containing the chromic anhybride of variable concentrations in the breathe air, also can make perforation of nasal septum and bronchiectasis etc. when serious.When alimentary canal is invaded, can cause vomiting, abdomen is painful., skin can produce dermatitis and eczema when invading.Harm is maximum is long-term or short term contact or carcinogenic danger is arranged when sucking.Along with industrial expansion, pollution of chromium is more and more serious, therefore, the chromium content in the waste water is reduced to below the discharge standard, and eliminating the harm of chromium and effectively reclaiming chromium in the waste water is face in the current environmental protection work one very distinct issues.
The method of traditional processing waste water containing chrome is a lot; Like ion-exchange, membrane separation process, electrolytic reduction, activated detergent desorption method etc.; These methods or be that chromium in the waste water can't be recycled; Be that waste water after administering also is difficult for reaching discharge standard, expense is too high even also can produce a large amount of mud, causes secondary pollution problems and can not generally be promoted.Therefore, seek efficiently, the technology that economic with practical adsorbent is removed chromium in the waste water seems particularly important.
Summary of the invention
In order to solve the weak point that exists in the above-mentioned prior art, primary and foremost purpose of the present invention is to provide a kind of ammonium thiocyanate modification seaweed-type preparation of adsorbent method.This method utilizes ammonium thiocyanate to modify marine alga, increases the adsorption activity point of marine alga, improves the ability of marine alga absorption heavy metal.
Another object of the present invention is to the ammonium thiocyanate modification seaweed-type adsorbent that provides a kind of method for preparing to obtain; This adsorbents adsorb efficient and capacity are high, economic and practical.
A purpose more of the present invention is to provide the application of above-mentioned ammonium thiocyanate modification seaweed-type adsorbent in Adsorption of Heavy Metal Ions.
The object of the invention is realized through following technical proposals: a kind of ammonium thiocyanate modification seaweed-type preparation of adsorbent method comprises following operating procedure:
(1) with the marine alga oven dry, grind, the salt soak is used in the back of sieving, and obtains mixed liquor; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, add ammonium thiocyanate and chloroacetic acid, carry out the modification reaction after the adjusting pH value; Reaction finishes the back filters, flushing, and oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
Said the sieving of step (1) was 50～20 purpose sieves; The concentration of said hydrochloric acid is 0.1mol/L～1mol/L; The time of said immersion is 2～8h.
The mass ratio of said ammonium thiocyanate of step (2) and chloroacetic acid is 0.2: 1～1: 0.2.
The mass ratio of said pretreated marine alga of step (2) and ammonium thiocyanate is 0.2: 1～1: 0.2.
The said adjusting of step (2) pH value is to regulate pH value to 0～7.
The temperature of the said modification reaction of step (2) is 30～60 ℃, and the time is 1～6h.
A kind of ammonium thiocyanate modification seaweed-type adsorbent that obtains according to method for preparing.
The application of above-mentioned ammonium thiocyanate modification seaweed-type adsorbent in Adsorption of Heavy Metal Ions, said heavy metal ion is Cr
6+In application process, the dosage of ammonium thiocyanate modification seaweed-type adsorbent is the Cr of every 100mL
6+Add 1.0～3.0g ammonium thiocyanate modification seaweed-type adsorbent in the solution.Said Cr
6+The concentration of solution is 10～30mg/L.
The present invention has following advantage and beneficial effect with respect to prior art:
(1) marine alga has absorption Cr than other organism
6+Characteristics such as ability is strong, method of modifying is simple and the holding time is long;
(2) it is extensive that technology of the present invention has raw material sources, and modifying process is simple, and the well-formed who forms after the modification can under lower pH, use, and adsorption capacity is big, removes the efficient advantages of higher, is to handle to contain Cr
6+The excellent process of waste water;
(3) modification seaweed-type adsorbent of the present invention can be handled certain metal ion species pointedly, and treatment effect is high, the recovery meaning is big;
(4) modification seaweed-type adsorbent of the present invention can be degraded, and secondary pollution can not take place;
(5) utilize modification seaweed-type adsorbents adsorb Cr of the present invention
6+, the Cr after the absorption
6+Can carry out wash-out with acid, in adsorption process, have the dynamic equilibrium of absorption-desorption, so the way of wash-out capable of using realizes that heavy metal is used for reclaiming, the regrown material frond is reused;
(6) distribute extensively, collect easily, can screen the raw materials for production of suitable algae, under the condition that is fit to, carry out ARTIFICIAL CULTURE as absorption.
Description of drawings
Fig. 1 is the ammonium thiocyanate modification seaweed-type adsorbent of the present invention's preparation and the relativity figure of former algae and physical modification algae difference adsorbing hexavalent chromium, and wherein abscissa is an adsorption time, and ordinate is an adsorption rate.
The specific embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in further detail, but embodiment of the present invention is not limited thereto.
Embodiment 1:
(1) with the marine alga oven dry, grinds, use the salt soak 4h of concentration behind 20 mesh sieves excessively, obtain mixed liquor as 0.3mol/L; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, adding mass ratio is 0.2: 1 ammonium thiocyanate and chloroacetic acid, and the mass ratio of said pretreated marine alga and ammonium thiocyanate is 0.2: 1, regulates pH value to 3, under 30 ℃ of temperature, carries out modification and reacts; Filter behind the reaction 6h, flushing, oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
With the Cr of gained ammonium thiocyanate modification seaweed-type adsorbent according to every 100mL
6+Add the amount of 1.0g in the solution, join the Cr that concentration is 14mg/L
6+In the solution, behind the stirring and adsorbing 2h, adsorption rate reaches 40%.
Embodiment 2:
(1) with the marine alga oven dry, grinds, use the salt soak 6h of concentration behind 50 mesh sieves excessively, obtain mixed liquor as 0.2mol/L; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, adding mass ratio is 0.6: 1 ammonium thiocyanate and chloroacetic acid, and the mass ratio of said pretreated marine alga and ammonium thiocyanate is 0.5: 1, regulates pH value to 4, under 30 ℃ of temperature, carries out modification and reacts; Filter behind the reaction 4h, flushing, oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
With the Cr of gained ammonium thiocyanate modification seaweed-type adsorbent according to every 100mL
6+Add the amount of 3.0g in the solution, join the Cr that concentration is 30mg/L
6+In the solution, behind the stirring and adsorbing 2h, adsorption rate reaches 65%.
Embodiment 3:
(1) with the marine alga oven dry, grinds, use the salt soak 8h of concentration behind 30 mesh sieves excessively, obtain mixed liquor as 0.1mol/L; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, adding mass ratio is 0.8: 1 ammonium thiocyanate and chloroacetic acid, and the mass ratio of said pretreated marine alga and ammonium thiocyanate is 0.8: 1, regulates pH value to 4, under 30 ℃ of temperature, carries out modification and reacts; Filter behind the reaction 5h, flushing, oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
With the Cr of gained ammonium thiocyanate modification seaweed-type adsorbent according to every 100mL
6+Add the amount of 2.0g in the solution, join the Cr that concentration is 14mg/L
6+In the solution, behind the stirring and adsorbing 2h, adsorption rate reaches 69%.
Embodiment 4:
(1) with the marine alga oven dry, grinds, use the salt soak 2h of concentration behind 40 mesh sieves excessively, obtain mixed liquor as 1mol/L; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, adding mass ratio is 0.4: 1 ammonium thiocyanate and chloroacetic acid, and the mass ratio of said pretreated marine alga and ammonium thiocyanate is 0.9: 1, regulates pH value to 3, under 35 ℃ of temperature, carries out modification and reacts; Filter behind the reaction 4h, flushing, oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
With the Cr of gained ammonium thiocyanate modification seaweed-type adsorbent according to every 100mL
6+Add the amount of 2.0g in the solution, join the Cr that concentration is 10mg/L
6+In the solution, behind the stirring and adsorbing 2h, adsorption rate reaches 42%.
Embodiment 5:
(1) with the marine alga oven dry, grinds, use the salt soak 3h of concentration behind 20 mesh sieves excessively, obtain mixed liquor as 0.8mol/L; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, adding mass ratio is 1: 1 ammonium thiocyanate and chloroacetic acid, and the mass ratio of said pretreated marine alga and ammonium thiocyanate is 1: 1, regulates pH value to 1, under 40 ℃ of temperature, carries out modification and reacts; Filter behind the reaction 3h, flushing, oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
With the Cr of gained ammonium thiocyanate modification seaweed-type adsorbent according to every 100mL
6+Add the amount of 2.0g in the solution, join the Cr that concentration is 20mg/L
6+In the solution, behind the stirring and adsorbing 2h, adsorption rate reaches 44%.
Embodiment 6:
(1) with the marine alga oven dry, grinds, use the salt soak 5h of concentration behind 30 mesh sieves excessively, obtain mixed liquor as 0.5mol/L; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, adding mass ratio is 1: 0.6 ammonium thiocyanate and chloroacetic acid, and the mass ratio of said pretreated marine alga and ammonium thiocyanate is 0.3: 1, regulates pH value to 2, under 30 ℃ of temperature, carries out modification and reacts; Filter behind the reaction 5h, flushing, oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
With the Cr of gained ammonium thiocyanate modification seaweed-type adsorbent according to every 100mL
6+Add the amount of 2.5g in the solution, join the Cr that concentration is 14mg/L
6+In the solution, behind the stirring and adsorbing 2h, adsorption rate reaches 55%.
Embodiment 7:
(1) with the marine alga oven dry, grinds, use the salt soak 6h of concentration behind 50 mesh sieves excessively, obtain mixed liquor as 0.2mol/L; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, adding mass ratio is 1: 0.6 ammonium thiocyanate and chloroacetic acid, and the mass ratio of said pretreated marine alga and ammonium thiocyanate is 0.4: 1, regulates pH value to 2, under 50 ℃ of temperature, carries out modification and reacts; Filter behind the reaction 2h, flushing, oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
With the Cr of gained ammonium thiocyanate modification seaweed-type adsorbent according to every 100mL
6+Add the amount of 1.5g in the solution, join the Cr that concentration is 30mg/L
6+In the solution, behind the stirring and adsorbing 2h, adsorption rate reaches 46%.
Embodiment 8:
(1) with the marine alga oven dry, grinds, use the salt soak 4h of concentration behind 20 mesh sieves excessively, obtain mixed liquor as 0.3mol/L; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, adding mass ratio is 1: 0.8 ammonium thiocyanate and chloroacetic acid, and the mass ratio of said pretreated marine alga and ammonium thiocyanate is 1: 0.2, regulates pH value to 1, under 60 ℃ of temperature, carries out modification and reacts; Filter behind the reaction 4h, flushing, oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
With the Cr of gained ammonium thiocyanate modification seaweed-type adsorbent according to every 100mL
6+Add the amount of 2g in the solution, join the Cr that concentration is 25mg/L
6+In the solution, behind the stirring and adsorbing 2h, adsorption rate reaches 44%.
Embodiment 9:
(1) with the marine alga oven dry, grinds, use the salt soak 4h of concentration behind 40 mesh sieves excessively, obtain mixed liquor as 0.3mol/L; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, adding mass ratio is 1: 0.4 ammonium thiocyanate and chloroacetic acid, and the mass ratio of said pretreated marine alga and ammonium thiocyanate is 0.7: 1, regulates pH value to 1, under 60 ℃ of temperature, carries out modification and reacts; Filter behind the reaction 1h, flushing, oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
With the Cr of gained ammonium thiocyanate modification seaweed-type adsorbent according to every 100mL
6+Add the amount of 2.5g in the solution, join the Cr that concentration is 30mg/L
6+In the solution, behind the stirring and adsorbing 2h, adsorption rate reaches 61%.
Embodiment 10:
(1) with the marine alga oven dry, grinds, use the salt soak 6h of concentration behind 20 mesh sieves excessively, obtain mixed liquor as 0.2mol/L; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, adding mass ratio is 1: 0.2 ammonium thiocyanate and chloroacetic acid, and the mass ratio of said pretreated marine alga and ammonium thiocyanate is 0.9: 1, regulates pH value to 2, under 40 ℃ of temperature, carries out modification and reacts; Filter behind the reaction 6h, flushing, oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
With the Cr of gained ammonium thiocyanate modification seaweed-type adsorbent according to every 100mL
6+Add the amount of 3g in the solution, join the Cr that concentration is 14mg/L
6+In the solution, behind the stirring and adsorbing 2h, adsorption rate reaches 63%.
Embodiment 11:
(1) with the marine alga oven dry, grinds, use the salt soak 4h of concentration behind 50 mesh sieves excessively, obtain mixed liquor as 0.3mol/L; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, adding mass ratio is 1: 0.6 ammonium thiocyanate and chloroacetic acid, and the mass ratio of said pretreated marine alga and ammonium thiocyanate is 1: 0.1, regulates pH value to 2, under 35 ℃ of temperature, carries out modification and reacts; Filter behind the reaction 6h, flushing, oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
With the Cr of gained ammonium thiocyanate modification seaweed-type adsorbent according to every 100mL
6+Add the amount of 2.8g in the solution, join the Cr that concentration is 14mg/L
6+In the solution, behind the stirring and adsorbing 4h, adsorption rate reaches 55%.
Embodiment 12:
(1) with the marine alga oven dry, grinds, use the salt soak 4h of concentration behind 30 mesh sieves excessively, obtain mixed liquor as 0.3mol/L; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, adding mass ratio is 1: 0.6 ammonium thiocyanate and chloroacetic acid, and the mass ratio of said pretreated marine alga and ammonium thiocyanate is 0.7: 1, regulates pH value to 2, under 45 ℃ of temperature, carries out modification and reacts; Filter behind the reaction 6h, flushing, oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
With the Cr of gained ammonium thiocyanate modification seaweed-type adsorbent according to every 100mL
6+Add the amount of 1.6g in the solution, join the Cr that concentration is 14mg/L
6+In the solution, behind the stirring and adsorbing 8h, adsorption rate reaches 76%.
Embodiment 13:
(the physical modification algae is that former algae is soaked with the 0.1mol/L hydrochloric acid solution with former algae, physical modification algae; And with six agitators stirring 6h; Filter; Be flushed to neutrality with deionized water then, place baking oven, 60 ℃ down oven dry obtain) and embodiment 11 gained ammonium thiocyanate modification seaweed-type adsorbents (being the ammonium thiocyanate modification algae that Fig. 1 indicates) respectively according to the Cr of every 100mL
6+Add the amount of 1.0g in the solution, join the Cr that concentration is 14mg/L
6+In the solution, stirring and adsorbing, separately adsorption rate behind the test absorption different time, the result is as shown in Figure 1.
Visible from Fig. 1, the ability of the alga biology absorbent absorption after the ammonium thiocyanate modification is much higher than former algae and physical modification algae, and is visible through the adsorbents adsorb superior performance after the modification of the present invention.
The foregoing description is a preferred implementation of the present invention; But embodiment of the present invention is not restricted to the described embodiments; Other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; All should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (10)
1. ammonium thiocyanate modification seaweed-type preparation of adsorbent method is characterized in that comprising following operating procedure:
(1) with the marine alga oven dry, grind, the salt soak is used in the back of sieving, and obtains mixed liquor; Mixed liquor is filtered, flushing, oven dry obtains pretreated marine alga;
(2) in pretreated marine alga, add ammonium thiocyanate and chloroacetic acid, carry out the modification reaction after the adjusting pH value; Reaction finishes the back filters, flushing, and oven dry obtains ammonium thiocyanate modification seaweed-type adsorbent.
2. a kind of ammonium thiocyanate modification seaweed-type preparation of adsorbent method according to claim 1 is characterized in that: said the sieving of step (1) was 20～50 purpose sieves; The concentration of said hydrochloric acid is 0.1mol/L～1mol/L; The time of said immersion is 2～8h.
3. a kind of ammonium thiocyanate modification seaweed-type preparation of adsorbent method according to claim 1, it is characterized in that: the mass ratio of said ammonium thiocyanate of step (2) and chloroacetic acid is 0.2: 1～1: 0.2.
4. a kind of ammonium thiocyanate modification seaweed-type preparation of adsorbent method according to claim 1, it is characterized in that: the mass ratio of said pretreated marine alga of step (2) and ammonium thiocyanate is 0.2: 1～1: 0.2.
5. a kind of ammonium thiocyanate modification seaweed-type preparation of adsorbent method according to claim 1 is characterized in that: the said adjusting of step (2) pH value is to regulate pH value to 0～7.
6. a kind of ammonium thiocyanate modification seaweed-type preparation of adsorbent method according to claim 1 is characterized in that: the temperature of the said modification reaction of step (2) is 30～60 ℃, and the time is 1～6h.
7. ammonium thiocyanate modification seaweed-type adsorbent for preparing according to the said method of claim 1.
8. the application of ammonium thiocyanate modification seaweed-type adsorbent according to claim 1 in Adsorption of Heavy Metal Ions is characterized in that: said heavy metal ion is Cr
6+
9. application according to claim 8 is characterized in that: the dosage of said ammonium thiocyanate modification seaweed-type adsorbent is the Cr of every 100mL
6+Add 1.0～3.0g ammonium thiocyanate modification seaweed-type adsorbent in the solution.
10. application according to claim 9 is characterized in that: said Cr
6+The concentration of solution is 10～30mg/L.
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Application publication date: 20120620 |