CN101081359A - Xanthation bentonite absorbingsubstance and method for preparing the same - Google Patents
Xanthation bentonite absorbingsubstance and method for preparing the same Download PDFInfo
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Abstract
The present invention is xanthated bentonite as one kind of metal ion adsorbent with high adsorption capacity and its preparation process. The metal ion adsorbent with high adsorption capacity is prepared with bentonite sodium as material, and through dispersing, alkalization, reacting with SO2, and treating with magnesium salt to form stable magnesium salt of xanthated bentonite. The xanthated bentonite has powerful adsorption on heavy metal ion, and may be used in treating waste water containing heavy metal ion. Treating waste water containing heavy metal ion with the xanthated bentonite has the features of simple operation, high speed, high metal ion eliminating rate, easy solid-liquid separation, etc.
Description
Technical field
The invention belongs to water-treatment technology field, relate to the adsorbent for heavy metal in a kind of heavy metal containing wastewater treatment, relate in particular to the high adsorbent for heavy metal of a kind of adsorption capacity---xanthogenation bentonite, also relate to the xanthogenation preparation method for bentonite simultaneously.
Background technology
Along with the progress of science and technology and the fast development of industrial or agricultural, people's living standard improves constantly, and still, the pollution of environment is also serious day by day, and environmental protection and environmental improvement problem more and more are subjected to the attention of government and various circles of society.The important pollution sources of contaminated environment water quality are the heavy metal ion in the industrial wastewater, heavy metal wastewater thereby is mainly derived from the smelting and the part chemical enterprise of machining, mining industry, iron and steel and non-ferrous metal, as: industrial wastewaters such as electrolysis, agricultural chemicals, medicine, paint, pigment.Though some heavy metal is the health trace elements necessary, extensively be present in the muscle and bone of human body, if these heavy metal excess will produce great harm to human body.Heavy metal can not be decomposed in water and soil earth, and easily by the food chain transmission, causes accumulation and poisoning.The method of handling heavy metal wastewater thereby has chemical precipitation method, electrolysis, ion floatation method, ion-exchange, electro-osmosis method and hyperfiltration, solvent extraction, membrane separation process, ferrite process, absorption method etc.Traditional wastewater processing technology show mostly the inorganic agent use amount big, cost an arm and a leg, react wayward, shortcoming such as reaction is slow and effect is undesirable, effluent quality is poor, residue is not easily separated.And absorption method is easy to get because of its material, and is cheap, and removal effect is stable and be subjected to environmentalist's favor, has good application prospects in water treatment field.
Bentonite claims swelling rock or bentonite again, is to be the particulate clay mineral of main component with the montmorillonite, is 2: 1 type phyllosilicates that are made of two-layer tetrahedral si-o film therebetween layer of aluminum (magnesium) oxygen octahedra sheet.Bentonite has very big surface area, good adsorption performance and cation exchange capacity (CEC), and this lays a good foundation in Application of Sewage for it.China's bentonite mineral products resource is very abundant, widely distributed, and gross reserves is at the forefront in the world, but mostly is calcium-base bentonite, and its physicochemical property and process technology performance are relatively poor, so be an important research content of its deep processing to alta-mud modification.The application in heavy metal wastewater thereby of bentonite and modified alta-mud is more extensive.As: use the organic modified bentonite of yin, yang ionic surface active agent (lauryl sodium sulfate and softex kw), to Cu to making after the sodium-ionized bentonite modification
2+Maximum adsorption capacity is 23.10mg/g.At room temperature, be Pb in the solution of 1036ppm during pH=4 to initial concentration
2+Clearance reaches 100%, and maximum adsorption capacity is 51.8mg/g.At pH=6.5, the bentonite of microwave activation is to Cu
2+(initial concentration is 200mg/L) adsorption capacity is 28.31mg/g.When 4-methyl benzo-15-hat-5 modified alta-mud Treatment of Copper, lead waste water, to Cu
2+And Pb
2+Maximum adsorption capacity be respectively 25.59mg/g and 101.11mg/g.And sodium-ionized bentonite Treatment of Copper, lead waste water, its adsorption capacity is respectively 3.04 and 9.58mg/g.
Xanthan acid group anionic functional group has stronger trapping ability to metal cation.The existing report of the xanthogenation of organic polymer (as cellulose, lignin, starch, shitosan etc.) and application thereof, as: during insoluble starch xanthate Treatment of Copper waste water, adsorption capacity is 31.27mg/g.When cellulose xanthate is handled heavy metal wastewater thereby, Cu
2+Adsorption capacity is 1.49mg/g.Above method has all obtained effect preferably to the removal of heavy metal ion, but its processing and manufacturing cost height need expend the wide variety of materials and the energy, and the adsorption capacity to heavy metal ion is also lower generally.Mesoporous material with-SH modification can be used for the absorption of heavy metal ion, and the result shows that adsorbent is to Cu
2+Adsorption capacity be 62.00mg/g and 82mg/g.But its cost of material is relatively more expensive, and preparation technology and equipment require high, the process more complicated, and application process takes time and effort, so exist certain defective.
The application of the activation of bentonitic acid activation, salt, various method of modifying such as organically-modified and products thereof all has report, but to bentonitic xanthogenation and use and do not appear in the newspapers.
Summary of the invention
The objective of the invention is deficiency, the adsorbent for heavy metal that a kind of cost is low, adsorption capacity is high be provided at prior art and technology---xanthogenation bentonite (XB).
Another object of the present invention provides a kind of preparation method of this high-adsorption-capacity adsorbent for heavy metal.
Xanthogenation bentone adsorbent of the present invention is to be linked with xanthates on the bentonite surface.Its chemical constitution is shown below:
The preparation method of this xanthogenation bentone adsorbent comprises following processing step:
1. the solid-to-liquid ratio of sodium-ionized bentonite (NaB) with 1: 3～1: 12 is scattered in the distilled water, stirs and form the sodium-ionized bentonite suspension;
2. the solid sodium hydroxide that adds 0.1～2.5 times of sodium-ionized bentonite quality in suspension stirs 0.3～5h down in 15～45 ℃ constant temperature, forms muddy system;
3. carbon disulfide (the CS that in muddy system, adds sodium-ionized bentonite quality 0.5～1.0
2), react 1～9h down in 15～45 ℃ constant temperature, generate the bentonitic sodium salt of xanthogen; For fear of CS
2Add too fast the decomposition, carbon disulfide should progressively be added drop-wise in the system.
4. the solubility magnesium salts that adds 0.2～0.5 times of sodium-ionized bentonite quality reacts 0.5～5.0h down, the bentonitic magnesium salts of generation xanthogen in 15～45 ℃; Here the optional magnesium sulfate of using of solubility magnesium salts.
5. the rare magnesium salt solution washing that adds, suction filtration, to filtrate be colourless after, wash with acetone again; It is 5～10% Adlerika that rare magnesium salt solution can adopt concentration.
6. suction filtration, drying get the xanthogenation bentonite.
Structure, pattern and the surface functional group of the xanthogenation bentonite product of the present invention preparation by characterization methods such as FT-IR, TG-DTA, XRD, SEM and chemical analyses, show that xanthogen receives on the bentonite.
Infrared spectrum (FT-IR) figure of xanthogenation bentonite of the present invention (XB) and raw material sodium-ionized bentonite (NaB) thereof as shown in Figure 1.3500cm among the figure
-1Near absorption, and 1650cm for Al-OH stretching vibration on the imvite lattice
-1Near be-flexural vibrations of OH, belong to the flexural vibrations of intermediary water molecule, show and contain constitution water, the crystallization water, adsorbed water in the bentonite.1030cm
-1Neighbouring is that the Si-O-Si flexural vibrations absorb 910cm
-1Neighbouring is the Al-OH flexural vibrations, 840cm
-1Neighbouring is the Mg-OH flexural vibrations, 600cm
-1～400cm
-1Be Al-O and Si-O flexural vibrations, 520cm
-1Neighbouring is the Si-O-Al flexural vibrations, 470cm
-1Neighbouring is the Si-O-Si flexural vibrations.NaB is at 1460cm
-1Near tangible CO has appearred
3 2-Absworption peak because it is through purifying and using anhydrous Na by the bentonite original soil
2CO
3Sodium obtains transition, and the raw material of synthetic XB is NaB, so its spectrogram also has more weak CO herein
3 2-Absworption peak.Different with NaB, XB is at 1250-1020cm
-1The characteristic absorption that has occurred tangible carbon-sulfur bond in the scope, 600cm simultaneously
-1～400cm
-1The Al-O stretching vibration and the Si-O symmetrical stretching vibration absworption peak at place, and 2800cm
-1The stretching vibration absworption peak of above O-H, it is wide and blunt obviously to become, and illustrates that having carbon-sulfur bond has received the bentonite surface, and the result shows bentonitic xanthogenation modification success.
The thermogravimetric analysis result of xanthogenation bentonite of the present invention (XB) and raw material sodium-ionized bentonite (NaB) thereof as shown in Figure 2.R.T.～100 weightlessness is mainly adsorbed water and organic solvent in ℃ temperature range, mainly loses intermediary water in 130～200 ℃ of scopes, in 370～550 ℃ of scopes, is organic matter decomposition weightlessness, mainly loses constitution water in 550～690 ℃ of scopes.NaB compares with XB, and in ℃ temperature range of R.T.～100, the former is mainly adsorbed water at weightlessness, and is weightless less, and XB is weightless more in this scope, has also lost the used solvent of a certain amount of washing because of it has not only lost adsorbed water.In 370～550 ℃ of scopes the NaB weightlessness seldom, but XB weightlessness is more, shows that there has been great number of organic matters in XB inside, and it is weightless less in 550～690 ℃ of scopes, illustrate that xanthogenation has reduced bentonitic hydrophilicity, make constitution water obviously reduce, the result shows xanthogenation modification success.
Fig. 3 is the XRD figure of sodium-ionized bentonite (NaB) and xanthogenation bentonite (XB).As can be seen: 2 θ angles of the characteristic diffraction peak correspondence of sodium-ionized bentonite are 6.80 °～7.10 °, d
001Value 12.3016nm.NaB gets XB through xanthogenation, so 2 θ angles are similar to its raw material NaB greater than 35 ° of later diffraction peak shape situations, it is at the bentonitic characteristic diffraction peak of little angular region (5 °～7 °), change in location very little (2 θ angles are 6.060 °), but peak shape becomes wide and blunt, d
001Value becomes 14.5724nm, and ° has located to occur the new peak of a d=4.9568 in 2 θ=17.88, and this is that xanthogen has replaced due to the part of hydroxyl in the bentonite.
The above results shows that xanthogen receives on the bentonite, thereby strengthens its counterweight Adsorption Properties for Metal Ions and trapping ability.
Because the xanthogenation bentonite has very strong absorption property and trapping ability to heavy metal ion, so can be used as adsorbent for heavy metal, is applied in the processing of heavy metal wastewater thereby.
The mechanism of xanthogenation bentonite in treatment heavy metal wastewater thereby of the present invention is: the bentonite base xanthan acid radical anion that xanthogenation bentonite sodium salt and magnesium salts disassociation back generate can combine with heavy metal ion, form multiple insoluble chelate or bentonite base xanthates, sedimentary solubility product (Ksp) is much smaller than other sediment solubility products that heavy metal ion forms, and heavy metal ion is separated from waste water with the form of precipitation and reached the purpose that removes.
The present invention compares in prior art and has the following advantages:
1, xanthogenation bentone adsorbent employing sodium-ionized bentonite of the present invention (NaB) is a raw material, react with carbon disulfide, again with the reaction that makes the transition of the magnesium salts of solubility, make xanthogen receive on the bentonite and get, heavy metal ion had very strong ion exchangeable and absorption property, trapping ability, be applied in the processing of heavy metal wastewater thereby, dosage is few, high adsorption capacity, adsorption capacity are big.Handle back adsorbent good stability, can satisfy the requirement of handling heavy metal wastewater thereby fully, the waste water after the processing is limpid, transparent, free from extraneous odour, and the pH value reaches the discharge standard of country between 5～10, do not cause secondary pollution, helps environmental protection.
2, raw material bentonite of the present invention is abundant in china natural resources, and cheap and easy to get, cost is low; Preparation technology is simple, is convenient to operation; Separation of Solid and Liquid is easy, quick after handling heavy metal wastewater thereby.
3, because xanthates residue good stability also can be realized the recovery of heavy metal by the regeneration of acid pickle washing by soaking after the processing, reach the purpose of comprehensive utilization of resources.
Description of drawings
Fig. 1 is the bentonitic FT-IR figure of xanthogenation of the present invention
Fig. 2 is the bentonitic TG figure of xanthogenation of the present invention
Fig. 3 is the bentonitic XRD figure of xanthogenation of the present invention
The specific embodiment
Be described further below by the preparation and the application in handling heavy metal wastewater thereby thereof of specific embodiment xanthogenation bentonite of the present invention (XB).
Embodiment 1: the 20g sodium-ionized bentonite is added in the 120mL distilled water, after stirring makes and is uniformly dispersed, add 8g NaOH, stir 1h at 35 ℃ of constant temperature, drip CS
22.41mL, behind the reaction 1h, add 5.0g magnesium sulfate and 50mL H
2O continues constant temperature and stirs 30min for 35 ℃, and suction filtration is that 5～10% Adlerika washing 3-5 time is colourless to filtrate with concentration, with acetone washing 3 times, gets the pale blue green solid then, at 45 ℃ of following vacuum drying 10h, gets the XB1 product, and output is 31.3g.
Embodiment 2: preparation process and raw material etc. are identical with embodiment 1, and wherein, the addition of NaOH is 8g, CS
2Dripping quantity be 7.23mL, the reaction time is 1h, the XB2 product, output is 28.4g.
Embodiment 3: preparation process and raw material etc. are identical with embodiment 1, and wherein, the addition of NaOH is 8g, CS
2Dripping quantity be 7.23mL, the reaction time is 6h, the XB3 product, output is 26.4g.
Embodiment 4: preparation process and raw material etc. are identical with embodiment 1, and wherein, the addition of NaOH is 40g, CS
2Dripping quantity be 2.41mL, the reaction time is 9h, the XB4 product, output is 26.5g.
Embodiment 5: preparation process and raw material etc. are identical with embodiment 1, and wherein, the addition of NaOH is 16g, CS
2Dripping quantity be 4.82mL, the reaction time is 6h, the XB5 product, output is 30.2g.
Embodiment 6: preparation process and raw material etc. are identical with embodiment 1, and wherein, the addition of NaOH is 8g, CS
2Dripping quantity be 12.05mL, the reaction time is 1h, the XB6 product, output is 28.6g.
Embodiment 7: preparation process and raw material etc. are identical with embodiment 1, and wherein, the addition of NaOH is 32g, CS
2Dripping quantity be 2.41mL, the reaction time is 6h, the XB7 product, output is 26.4g.
Embodiment 8: preparation process and raw material etc. are identical with embodiment 1, and wherein, the addition of NaOH is 32g, CS
2Dripping quantity be 4.82mL, the reaction time is 1h, the XB8 product, output is 32.0g.
Embodiment 9: preparation process and raw material etc. are identical with embodiment 1, and wherein, the addition of NaOH is 16g, CS
2Dripping quantity be 12.05mL, the reaction time is 1h, the XB9 product, output is 30.2g.
Embodiment 10: preparation process and raw material etc. are identical with embodiment 1, and wherein, the addition of NaOH is 16g, CS
2Dripping quantity be 2.41mL, the reaction time is 3h, the XB10 product, output is 28.6g.
Embodiment 11: preparation process and raw material etc. are identical with embodiment 1, and the addition of NaOH is 48g, CS
2Dripping quantity be 7.23mL, the reaction time is 9h, the XB11 product, output is 38.5g.
Embodiment 12: preparation process and raw material etc. are identical with embodiment 1, and wherein, the addition of NaOH is 16g, CS
2Dripping quantity be 7.23mL, the reaction time is 1h, the XB12 product, output is 30.7g.
Embodiment 13: preparation process and raw material etc. are identical with embodiment 1, and wherein, the addition of NaOH is 4g, CS
2Dripping quantity be 2.41mL, the reaction time is 6h, the XB13 product, output is 23.6g.
Embodiment 14: preparation process and raw material etc. are identical with embodiment 1, and wherein, the addition of NaOH is 32g, CS
2Dripping quantity be 7.23mL, the reaction time is 3h, the XB14 product, output is 24.5g.
Embodiment 15: preparation process and raw material etc. are identical with embodiment 1, and wherein, the addition of NaOH is 8g, CS
2Dripping quantity be 4.82mL, the reaction time is 3h, the XB15 product, output is 24.1g.
Embodiment 16: xanthogenation bentonite of the present invention is to the adsorption test of leaded heavy metal simulated wastewater: choose 10 kinds of stating among the embodiment gained XB and be adsorbent, by following waste water treatment process, experimental result is as shown in table 1.
1, gets the simulated wastewater 100mL that the initial concentration that contains lead ion is 500mg/L;
2, regulate pH value to 3.0～7.0;
3, add xanthogenation bentonite (XB) in simulated wastewater, the adsorbent consumption is the 0.2g/100mL water sample;
4, the mixed liquor 60min of constant temperature vibration waste water and xanthogenation bentonite (XB);
5, leave standstill, suction filtration, filtrate is measured remaining plumbum ion concentration with atomic absorption spectrophotometer, calculates clearance and adsorption capacity.
Table 1 xanthogenation bentonite is to the adsorption capacity of lead ion
| The adsorbent title | XB1 | ?XB3 | ?XB5 | ?XB7 | ?XB8 | ?XB9 | ?XB10 | ?XB12 | ?XB14 | ?XB15 |
| Clearance (%) adsorption capacity (mg/g) | 99.46 248.91 | ?98.93 ?247.85 | ?99.79 ?249.59 | ?99.46 ?248.91 | ?99.61 ?249.21 | ?99.91 ?249.77 | ?99.39 ?248.77 | ?99.54 ?249.07 | ?99.76 ?249.51 | ?98.84 ?247.67 |
By table 1 result displayed, illustrate xanthogenation bentonite of the present invention to the clearance of heavy lead ion in the waste water basically more than 99%, adsorption capacity is more than 247mg/g.
Embodiment 17: xanthogenation bentonite of the present invention is to the adsorption test of the leaded heavy metal simulated wastewater of different initial concentrations: the waste water treatment process of pressing embodiment 16, the initial concentration that delivery is intended lead ion in the waste water is respectively 500mg/L, 800mg/L, 1000mg/L, 2000mg/L, with XB1 is that adsorbent carries out wastewater treatment test, the clearance of experiment gained lead ion is respectively 99.24%, 98.18%, 94.61%, 81.36%, and adsorption capacity is respectively 248.49mg/g, 393.73mg/g, 473.02mg/g, 981.08mg/g.
Embodiment 18: xanthogenation bentonite of the present invention is to the adsorption test of cupric heavy metal simulated wastewater: choose 10 kinds of stating among the embodiment gained XB and be adsorbent, press the waste water treatment process of embodiment 16, the initial concentration 80mg/L of copper ion, experimental result is as shown in table 2.
Table 2 XB adsorbent is to the adsorption test of cupric simulated wastewater
| The adsorbent title | XB 1 | ?XB 3 | ?XB 5 | ?XB 7 | ?XB 8 | ?XB 9 | ?XB 10 | ?XB 11 | ?XB 12 | ?XB 14 |
| Clearance (%) adsorption capacity (mg/g) | 99.47 39.79 | ?89.38 ?35.75 | ?99.86 ?39.94 | ?99.66 ?39.87 | ?99.47 ?39.79 | ?99.57 ?39.83 | ?99.57 ?39.83 | ?99.90 ?39.96 | ?99.71 ?39.88 | ?99.81 ?39.92 |
By table 2 result displayed, illustrate xanthogenation bentonite of the present invention to the clearance of heavy copper ion in the waste water more than 90%, adsorption capacity is more than 39mg/g.
Embodiment 19: xanthogenation bentonite of the present invention is to the adsorption test of the cupric heavy metal simulated wastewater of different initial concentrations: the waste water treatment process of pressing embodiment 16, the initial concentration that delivery is intended copper ion in the waste water is respectively 200mg/L, 500mg/L, 800mg/L, 1000mg/L, with XB3 is that adsorbent carries out wastewater treatment test, the clearance of experiment gained copper ion is respectively 88.15,76.08%, 89.66%, 64.33%, and adsorption capacity is respectively 88.15mg/g, 190.19mg/g, 358.65mg/g, 321.64mg/g.
Claims (4)
1, a kind of xanthogenation bentone adsorbent is characterized in that: be to be linked with xanthates on the bentonite surface; Its chemical constitution is shown below:
2, a kind of preparation method of xanthogenation bentone adsorbent comprises following processing step:
1. the solid-to-liquid ratio of sodium-ionized bentonite with 1: 3～1: 12 is scattered in the distilled water, stirs and form the sodium-ionized bentonite suspension;
2. the solid sodium hydroxide that adds 0.1～2.5 times of sodium-ionized bentonite quality in suspension stirs 0.3～5h down in 15～45 ℃ constant temperature, forms muddy system;
3. the carbon disulfide that adds sodium-ionized bentonite quality 0.5～1.0 in muddy system reacts 1～9h down in 15～45 ℃ constant temperature, generates the bentonitic sodium salt of xanthogen;
4. the solubility magnesium salts that adds 0.2～0.5 times of sodium-ionized bentonite quality reacts 0.5～5h down, the bentonitic magnesium salts of generation xanthogen in 15～45 ℃;
5. the rare magnesium salt solution washing that adds, suction filtration, to filtrate be colourless after, wash with acetone again;
6. suction filtration, drying get the xanthogenation bentonite.
3, the preparation method of xanthogenation bentone adsorbent as claimed in claim 2 is characterized in that: the 4. described solubility magnesium salts of step is a magnesium sulfate.
4, the preparation method of xanthogenation bentone adsorbent as claimed in claim 2 is characterized in that: the 5. described rare magnesium salt solution of step is that concentration is 5～10% Adlerika.
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| CN101362073B (en) * | 2008-09-27 | 2010-10-13 | 山东大学 | Preparation method of acidification sludge bentonite granules |
| CN102360659A (en) * | 2011-06-24 | 2012-02-22 | 中国科学院宁波材料技术与工程研究所 | Magnetic submicron composite core-shell particles, and preparation method and application thereof |
| CN102463104A (en) * | 2010-11-19 | 2012-05-23 | 王永斌 | Clay-based xanthogenate, and preparation method and application thereof |
| CN102908998A (en) * | 2012-11-09 | 2013-02-06 | 济南大学 | Preparation method of xanthate macro-pore dextrangel adsorbent |
| CN103071461A (en) * | 2013-02-26 | 2013-05-01 | 西北师范大学 | Preparation of xanthated loess adsorbent and application of xanthated loess adsorbent to waste water treatment |
| CN103785361A (en) * | 2014-03-05 | 2014-05-14 | 北京师范大学 | Method for preparing heavy metal ion absorbent through xanthation of granule sludge |
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| CN101362073B (en) * | 2008-09-27 | 2010-10-13 | 山东大学 | Preparation method of acidification sludge bentonite granules |
| CN102463104A (en) * | 2010-11-19 | 2012-05-23 | 王永斌 | Clay-based xanthogenate, and preparation method and application thereof |
| CN102360659A (en) * | 2011-06-24 | 2012-02-22 | 中国科学院宁波材料技术与工程研究所 | Magnetic submicron composite core-shell particles, and preparation method and application thereof |
| CN102908998A (en) * | 2012-11-09 | 2013-02-06 | 济南大学 | Preparation method of xanthate macro-pore dextrangel adsorbent |
| CN102908998B (en) * | 2012-11-09 | 2014-07-30 | 济南大学 | Preparation method of xanthate macro-pore dextrangel adsorbent |
| CN103071461A (en) * | 2013-02-26 | 2013-05-01 | 西北师范大学 | Preparation of xanthated loess adsorbent and application of xanthated loess adsorbent to waste water treatment |
| CN103071461B (en) * | 2013-02-26 | 2015-08-19 | 西北师范大学 | The preparation of xanthogenation loess adsorbent and application in the treatment of waste water |
| CN103785361A (en) * | 2014-03-05 | 2014-05-14 | 北京师范大学 | Method for preparing heavy metal ion absorbent through xanthation of granule sludge |
| CN107162152A (en) * | 2017-06-19 | 2017-09-15 | 扬州工业职业技术学院 | A kind of silicon dioxide carried sulfuric acid xanthates sewage-treating agent |
| CN107497400A (en) * | 2017-08-02 | 2017-12-22 | 哈尔滨工业大学 | A kind of preparation method using rice husk as the modified adsorbent of matrix applied to sudden water pollution emergency processing |
| CN112755960A (en) * | 2020-12-30 | 2021-05-07 | 四川省冶金地质勘查局六0五大队 | Sulfur-modified biochar, preparation method thereof, recyclable sulfur-modified biochar material and application |
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