CN105080513B - A kind of chelate fibre, its synthetic method and the method that Cr VI is enriched with from serpentine - Google Patents
A kind of chelate fibre, its synthetic method and the method that Cr VI is enriched with from serpentine Download PDFInfo
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Abstract
The invention discloses a kind of chelate fibre, its synthetic method and the method for being enriched with from serpentine Cr VI, the synthetic method of the chelate fibre includes：1）, using grafted propylene acid polytetrafluoroethylene fibre as parent, grafted propylene acid polytetrafluoroethylene fibre is placed in toluene 12 ~ 14h of immersion；2）, in step 1）Gains in add part, in 30 ~ 50 DEG C of stirring reactions 11 ~ 14 hours；The part is the thiadiazoles of 2 amino 1,2,4, and the mol ratio of parent and part is 1：2~6；3）, by step 2）Products therefrom is filtered, and gained filter cake is dried to constant weight after flushing, is obtained to Cr（）Chelate fibre MATF with selective absorption.The chelate fibre MATF that the present invention synthesizes has high efficiency selected absorption property to hexavalent chromium.
Description
Technical field
The present invention relates to a kind of method of synthesizing new chelate fibre, and in particular to grafted propylene acid fibrillated polytetrafluoroethylene
It is parent to tie up (PTFE-g-AA), and with 2- amino -1,2,4- thiadiazoles (MAT) is part, is had so as to synthesize to Cr (VI) ion
The chelate fibre MATF of high efficiency selected absorption property, for being enriched with Cr VI from serpentine.
Background technology
Serpentine is a kind of general name of aqueous rich magnesium silicate mineral, such as antigorite, lizardite, choysotile
Deng.In compact massive, there are greasy luster, somewhat sliding sense, because they are often dark green alternate as snakeskin, so gaining the name.
It is mainly used as firing calcium magnesium phosphate, steel-making flux, refractory material, structural lumber, artistic carving, extraction magnesia and porous oxygen
SiClx, in terms of being additionally operable to medical treatment, purify high-fluorine water, the manufacture peaceful piece of fluorine etc..Their color is often typically green hue, but also have shallow
Ash, white or yellow etc..Green and emerald green serpentine is often widely distributed containing chromium and nickel.Bar is aoxidized strongly in epigenetic zone
(alkaline medium), Cr under part3+It is oxidized to Cr6+The chromate ion of form, make inactive chromium ion become readily soluble chromium the moon from
Son migrates.At present, serpentine ore is used for extracting metals magnesium, a kind of important meals resource chromium in production process, is but made
It can not be utilized for waste material, and cause serious problem of environmental pollution.
Chromium harm to the human body is larger.The toxic dose of crome metal is 200mg, and lethal dose 6g, chromium poisoning can be by dust
Enter from respiratory tract, or contaminated food is entered by alimentary canal.Chromium ion valence state is different, and the extent of injury is also different.Cr VI and
Its esters is maximum in chromic salts Poisoning.The toxicity of Cr VI is than 100 times of trivalent chromium.Cr VI has stimulation to make to alimentary canal and skin
With Cr VI has carcinogenesis.Chromate waste water and skin contact, the dermatitis to mostly occur based on erythematous papules, it can be changed into wet
Rash.When serpentine produces magnesium oxide product, in multistage links leaching device, 0~1mm serpentine particles 105 DEG C, 20%
Hydrochloric acid in leached.Serpentine particles residence time in hydrochloric acid is 2.5 hours, and leachate is as waste material without exploitation value
Value；If chrome yellow is made using a kind of cheap adsorption and enrichment material recovery Cr VI, turn waste into wealth, the efficient profit of resource can be achieved
With.
Polytetrafluoroethylene (PTFE) (PTFE) fiber has fabulous chemical stability and higher specific surface area, thus and adsorbate
Contact area is bigger, fluid resistance is smaller, diffusion admittance is shorter, is easier with the reaction of function base, and adsorption capacity is big, selectively
Also more preferable, absorption and elution rate are also higher, while have that plasticity is strong, can be made it is various required for shape the advantages that.Cause
This, makes it connect various chelating function groups, the PTFE chelatings being prepared into are fine if surface graft modification can be carried out to PTFE fiber
Dimension would is that a kind of new material available for separation and concentration heavy metal ion.
The content of the invention
In order to solve the above-mentioned technical problem, the present invention provides a kind of chelate fibre MATF, its synthetic method and from serpentine
The method of middle enrichment Cr VI, the Cr VI in absorption serpentine can effectively be realized using the method for the present invention.
The present invention provides a kind of synthetic method of chelate fibre, comprises the following steps：
1), using grafted propylene acid polytetrafluoroethylene fibre as parent, grafted propylene acid polytetrafluoroethylene fibre is placed in first
12~14h is soaked in benzene；
2) part, is added in the gains of step 1), in 30~50 DEG C of stirring reactions 11~14 hours；The part is
The mol ratio of 2- amino -1,2,4- thiadiazoles, parent and part is 1：2~6；
3), step 2) products therefrom is filtered, gained filter cake is dried to constant weight after flushing, obtains having Cr (VI)
The chelate fibre MATF of selective absorption.
It is preferred that the flushing in step 3) is：Gained filter cake rinses successively through toluene, ether, ethanol, deionized water.
It is preferred that the amount ratio of grafted propylene acid polytetrafluoroethylene fibre and toluene is 20.0mg in step 1)：40~
60ml。
It is preferred that the drying in step 3) is：In 40~60 DEG C of freeze-day with constant temperature.
It is preferred that the rotating speed of stirring is 250~350rpm/min in step 2).
It is preferred that in step 2), the mol ratio of parent and part is 1：4.
The present invention also provides a kind of chelate fibre MATF, is prepared by above-mentioned synthetic method.
The present invention also provides the method that above-mentioned chelate fibre MATF is enriched with Cr VI from serpentine, including：By ball milling 1h
Serpentine power, with 3mol/L HCl with 1:4 solid-to-liquid ratio, flow back 1h at 100 DEG C, is separated by filtration, and filtrate is using fresh
Miberal powder leaches deacidification treatment；Using the hexavalent chromium in above-mentioned chelate fibre MATF separation and concentration pickle liquors, wherein, pickle liquor
The ratio of volume and fiber quality is 1L：1g.
The chelate fibre MATF synthesized using the method for the present invention, is had the following advantages that：
1st, the chelate fibre MATF of gained has that raw material sources are extensive, cheap characteristic；
2nd, heavy metal ion has the rate of adsorption fast, and time of equilibrium adsorption is short, wherein, have efficiently to Cr (VI) ion
Adsorptive selectivity, the shortcomings that overcoming former parent adsorption selectivity difference；
3rd, possesses excellent regenerability, reusability is good, cost-effective, environmental protection.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the reaction principle figure of the present invention；
Fig. 2 is the influence for reacting mol ratio to parent function base conversion ratio；
Fig. 3 is influence of the reaction time to parent function base conversion ratio；
Fig. 4 is influence of the reaction temperature to parent function base conversion ratio；
Fig. 5 be under different pH value MATF to the shadow of the adsorption capacity of the different ions such as metal ion Cr (VI), Cr (III)
Ring；
Fig. 6 is the different time influences of MATF to metal ion Cr (VI) adsorbance with a temperature of.
Embodiment
The present invention is further depicted as with reference to specific embodiment and comparative example, but present disclosure is not limited to
This.
Embodiment 1
A kind of chelate fibre MATF synthetic method, is followed the steps below successively：
1), will about 20.0mg parents --- grafted propylene acid polytetrafluoroethylene fibre (PTFE-g-AA) be placed in the three of 100mL
In neck bottle, add toluene 50mL and soak 12 hours；
Remarks explanation：Also name polytetrafluoroethylene (PTFE) grafted propylene is sour for grafted propylene acid polytetrafluoroethylene fibre (PTFE-g-AA)
Copolymer, acrylic acid modified polytetrafluoroethylene fibre etc..In grafted propylene acid polytetrafluoroethylene fibre (PTFE-g-AA)
PTFE-g-AA functions base (that is ,-COOH) content is 3.07mmol/g；
2) 0.246mmol part --- 2- amino -1,2, is added into three-necked bottle again, 4- thiadiazoles (MAT) is (i.e.,
The reaction mol ratio of PTFE-g-AA and part is 1：4), 35 DEG C of stirring reactions 12 hours, agitator speed 300rpm/min；
3), products therefrom in step 2) is filtered, gained filter cake rushes successively through toluene, ether, ethanol, deionized water
Wash 3 times, it is every in：Toluene, ether, ethanol, the dosage of deionized water are 100ml；
By the filter cake after above-mentioned flushing be put into vacuum drying chamber under 40~60 DEG C of drying temperature dry to constant weight (when
Between about 3~5 days), obtain chelate fibre MATF；According to the content of N in products therefrom, calculate chelate fibre MATF function base
Conversion ratio is 51.1%.
Wherein, the chelate fibre MATF of synthesis function base conversion ratio can be calculated by following formula：
In above formula, F0(3.07mmol/g) is grafted propylene acid polytetrafluoroethylene fibre (PTFE-g-AA) functional group content,
X be chelate fibre function base conversion ratio, N0For grafted propylene acid polytetrafluoroethylene fibre (PTFE-g-AA) nitrogen content (%),
Nc be synthesis after chelate fibre (MATF) nitrogen content (%), nNFor the quantity of nitrogen-atoms in grafting part, MLFor grafting part
Molal weight (mol/g).
Wherein, above-mentioned reaction principle figure is as shown in Figure 1.
Comparative example 1-1
By the mol ratio 1 of parent in embodiment 1 and part：4 are changed to 1:2、1:3、1:5、1:6, other conditions and embodiment 1
It is identical, it is as shown in Figure 2 to obtain influence of the reaction mol ratio to parent function base conversion ratio.
It can be seen from Fig. 2, in MATF building-up process, the optimum mole ratio of parent and part is 1:4.
Comparative example 1-2
The 12 hours reaction time of step 2) in embodiment 1 is changed to 6 hours, 8 hours, 10 hours, 14 hours, other
Part is same as Example 1, and it is as shown in Figure 3 to obtain influence of the reaction time to parent function base conversion ratio.
It can be seen from Fig. 3, in MATF building-up process, optimum reacting time is 12 hours.
Comparative example 1-3
35 DEG C of the reaction temperature of step 2) in embodiment 1 is changed to 15 DEG C, 25 DEG C, 45 DEG C, 55 DEG C, other conditions are with implementing
Example 1 is identical, and it is as shown in Figure 4 to obtain influence of the reaction temperature to parent function base conversion ratio.
It can be seen from Fig. 4, in MATF building-up process, optimal reaction temperature is 35 DEG C.
Cr (VI) ion in the MATF adsorption aqueous solutions that experiment 1, embodiment 1 are prepared
The MATF 15.0mg for weighing the gained of embodiment 1 are placed in 100mL iodine flask, move into 25mL pH=5 vinegar
Acid-sodium acetate buffer soaks 24 hours, then adds 5mL standards Cr (VI) (concentration 2mg/mL) solion,
Under 308K, constant temperature oscillation adsorbs after 12 hours reaches balance, and wherein frequency of oscillation is 100rpm.It is dense that quality is made into distilled water water
The hydrazine of diphenyl phosphinylidyne two spent for 0.2% is developer, and iodine flask supernatant is detected at ultraviolet-visible spectrophotometer 542nm
Middle Cr (VI) ion concentration, it is 86.5mg/g to the adsorbance of Cr (VI) ion to extrapolate MATF.
Wherein, for MATF, pH=5 NaAc_HAc buffer solution is optimal, remaining pH acetic acid-vinegar
MATF after sour sodium cushioning liquid immersion is below 86.5mg/g to the adsorbance of Cr (VI) ion.
In addition, adsorption temp and time are as shown in Figure 6 to the Adsorption Effect of Cr (VI) ion.It is optimal to inhale it can be seen from Fig. 6
Enclosure temperature is 35 DEG C, and adsorption time is 2.5 hours.
Comparative example 2
By the part in embodiment 1 by 2- amino -1,2,4- thiadiazoles (MAT) be changed to 2- aminobenzothiazoles, 3- sulfydryls -
1,2,4- triazole, 3- amino -5- methyl isoxazole, 4-aminopyridine formamide, remaining is equal to embodiment 1.
Finally using grafted propylene acid polytetrafluoroethylene fibre as parent, toluene is reaction dissolvent, 2- aminobenzothiazoles, 3-
Sulfydryl -1,2,4- triazoles, 3- amino -5- methyl isoxazole, 4-aminopyridine formamide turn for the chelate fibre function base of part
Rate is respectively 21.4%, 9.5%, 3.2%, 15.2%.
Comparative example 3
By the part in embodiment 1 by 2- amino -1,2,4- thiadiazoles (MAT) be changed to 2- aminobenzothiazoles, 3- sulfydryls -
1,2,4- triazole, 3- amino -5- methyl isoxazole, 4-aminopyridine formamide, reaction dissolvent are changed by DMF
For toluene, Isosorbide-5-Nitrae-dioxane, acetone, remaining is equal to embodiment 1.
Finally using grafted propylene acid polytetrafluoroethylene fibre as parent, toluene, Isosorbide-5-Nitrae-dioxane, acetone are molten for reaction
Agent, 2- aminobenzothiazoles, 3- sulfydryls -1,2,4- triazoles, 3- amino -5- methyl isoxazole, 4-aminopyridine formamide be with
The chelate fibre function base conversion ratio of body see the table below 1,
Table 1, different ligands the gained chelate fibre function base conversion ratio under differential responses solvent
Contrast experiment 1-1
With 2- amino -1,2 in 1 being tested, chelate fibre of the 4- thiadiazoles (MAT) obtained by ligand reaction, it is changed to 2-
Aminobenzothiazole, 3- sulfydryl -1,2,4- triazoles, 3- amino -5- methyl isoxazole, 4-aminopyridine formamide are ligand reaction
The chelate fibre of gained, remaining is equal to experiment 1.
Finally measure using grafted propylene acid polytetrafluoroethylene fibre as parent, 2- aminobenzothiazoles, 3- sulfydryls -1,2,4-
The chelate fibre of triazole, 3- amino -5- methyl isoxazole, 4-aminopyridine formamide obtained by ligand reaction is to Cr (VI) ion
Adsorbance be respectively 87.1mg/g, 37.6mg/ml, 19.1mg/ml, 29.8mg/ml.
Contrast experiment 1-2
With 2- amino -1,2 in 1 being tested, chelate fibre of the 4- thiadiazoles (MAT) obtained by ligand reaction, it is changed to 2-
Aminobenzothiazole, 3- sulfydryl -1,2,4- triazoles, 3- amino -5- methyl isoxazole, 4-aminopyridine formamide are ligand reaction
The chelate fibre of gained, the pH of cushioning liquid Acetic acid-sodium acetate used are changed to 2.5,3.5,5.5,6.5 by 5, and remaining is equal to reality
Test 1.
Finally measure with 2- aminobenzothiazoles, 3- sulfydryl -1,2,4- triazoles, 3- amino -5- methyl isoxazole, 4- amino
Pyridine carboxamide is the chelate fibre obtained by ligand reaction, 2.5,3.5,5.5,6.5 is changed to by 5 in cushioning liquid pH, to Cr
(VI) adsorbance of ion see the table below 2：
Table 2
Experiment 2
The MATF that embodiment 1 is prepared Cr (VI) and Cr (III), Pb (II), Cd (II), Fe (III), Mg (II),
Selective absorption in Ca (II) mixed ion solutions to Cr (VI) ion carries out confirmatory experiment：
Mixed solution is prepared with compound chromic nitrate, potassium bichromate, Cr (VI) and Cr (III) ion concentration in mixed solution
It is 2mg/ml, specific experiment content is as follows：
Accurately weigh 15.0mg MATF to be placed in 100mL iodine flask, the Acetic acid-sodium acetate for moving into 25mL pH=5 delays
Solution immersion 24h is rushed, then adds 5mL mixed ion solutions, under 308K, constant temperature oscillation adsorbs after 1 day reaches balance, wherein
Frequency of oscillation is 100rpm.
Remarks explanation：The measure of Cr (VI) ion concentration in mixed solution：Phosphoric acid (1:1) (concentrated phosphoric acid deionized water is dilute
Release 1 times), 0.2% diphenylcarbazide developer (water is solvent), at 542nm with ultraviolet-visible scene photometer detect inhale
Luminosity；
Cr (VI) ion concentration after adsorbing is calculated with following formula：
C in formulaeCr (VI) ion concentration (mg/ml) during to balance, C0For Cr before absorption (VI) ion concentration (mg/ml), Ae
To measure Cr (VI) ion absorbance, A during balance0To measure Cr (VI) ion absorbance before absorption.
Other ion concentrations measure also uses ICP (inductively coupled plasma).
Shown in reference picture 5, final acquired results are that MATF is 86.5mg/g to the adsorbance of Cr (VI) ion, to other from
Subbase does not originally adsorb, and illustrates MATF chelate fibres in the case of other ions such as Cr (VI) and Cr (III) are simultaneous to Cr
(VI) ion has efficient specific selection performance.
Experiment 3, Cr (VI) ion regeneration tests
The MATF tested in 1 after adsorption equilibrium is filtered out, is rinsed 3~5 times and (removed with pH=5 NaAc_HAc buffer solutions
Remove to float on Cr (VI) ion on surface), it is placed in iodine flask and (adsorption equilibrium in an experiment 1 is only put in an iodine flask
MATF fibers), the thiourea solution 30mL of various concentrations is separately added into, is placed under the conditions of 308K, constant temperature oscillation 24h, frequency of oscillation
For 100rmp/min.It is respectively 79.6%, 91.1%, 92.6%, 92.6% to measure MATF regeneration rates.From environmental protection and reduction
Cost angle considers that the thiourea solution from concentration 6% is optimal MATF regenerative agents.
MATF adsorbs the desorption efficiency of Cr (VI) ion under 3 different thiourea concentrations of table
Embodiment 2
By ball milling 1h serpentine power, with 3mol/L HCl with 1:4 solid-to-liquid ratio, flow back 1h at 100 DEG C, filtering point
From filtrate is using fresh miberal powder leaching deacidification treatment；Deacidification is leached using fresh miberal powder, on the one hand can make the pH value of pickle liquor
Suitable fibers absorption Cr (VI) scope is adjusted to, is advantageous to separation and concentration；On the other hand the Cr in pickle liquor can be improved
(VI) concentration of ion, the efficiency of separation and concentration process is improved；Afterwards, using Cr in fibers adsorption technology separation and concentration pickle liquor
(VI) ion, wherein, pickle liquor volume (L)：MATF fiber qualities (g)=1：1.Wherein, fibers adsorption technology is using absorption
Material adsorbs to adsorbate.It is the active Carbon fibe of sorbing material that is often used in fibers adsorption technology, alginic acid fibre, each
Kind includes each heavy metal species, harmful chemical agents, toxic gas etc. by modified chemical fibre, the adsorbate of research, wherein
Heavy metal includes iron, zinc, copper, gold, silver, chromium, lead, mercury etc..
Experiment shows that the concentration of Cr VI has reached country and arranged on high concentration chrome wastewater in the pickle liquor through MATF fiber treatments
Standard when putting, follow-up ore is avoided from source and produces hexavalent chromium polluted problem using process.
Table 4 is the reality that MATF fibers are enriched with hexavalent chromium with the chelate fibre prepared with other parts from serpentine
Contrast on effect table.From table 4, effect that MATF fibers are enriched with hexavalent chromium from serpentine is preferable, and other chelas
The effect of condensating fiber is unsatisfactory.
The actual effect of table 4 --- pickle liquor volume (V/L)：Synthetic fibers quality (M/g)=1：1
Finally, it is also necessary to it is noted that listed above is only several specific embodiments of the invention.Obviously, this hair
It is bright to be not limited to above example, there can also be many deformations.One of ordinary skill in the art can be from present disclosure
All deformations for directly exporting or associating, are considered as protection scope of the present invention.
Claims (7)
1. a kind of synthetic method of chelate fibre, it is characterised in that comprise the following steps：
1）, using grafted propylene acid polytetrafluoroethylene fibre as parent, grafted propylene acid polytetrafluoroethylene fibre is placed in toluene
Soak 12 ~ 14h；
2）, in step 1）Gains in add part, in 30 ~ 50 DEG C of stirring reactions 11 ~ 14 hours；The part is 2- ammonia
The mol ratio of base -1,2,4- thiadiazoles, parent and part is 1：2~6；
3）, by step 2）Products therefrom is filtered, and gained filter cake is dried to constant weight after flushing, is obtained to Cr（）With choosing
The chelate fibre MATF of selecting property absorption.
2. according to the method for claim 1, it is characterised in that step 3）In flushing be：Gained filter cake is through toluene, second
Ether, ethanol, deionized water are rinsed successively.
3. according to the method for claim 1, it is characterised in that step 1）Middle grafted propylene acid polytetrafluoroethylene fibre and first
The amount ratio of benzene is 20.0mg：40~60ml.
4. according to the method for claim 1, it is characterised in that step 3）In drying be：In 40 ~ 60 DEG C of freeze-day with constant temperature.
5. according to the method for claim 1, it is characterised in that step 2）The rotating speed of middle stirring is 250 ~ 350rpm/min.
6. according to the method for claim 1, it is characterised in that step 2）In, the mol ratio of parent and part is 1：4.
7. a kind of chelate fibre MATF, it is characterised in that be prepared as the method described in any one of claim 1 to 6.
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| CN102861558A (en) * | 2012-09-24 | 2013-01-09 | 浙江工商大学 | Method for preparing chelate-resin metal adsorbing material from polyacrylonitrile |
| CN104018346A (en) * | 2014-05-26 | 2014-09-03 | 浙江工商大学 | Synthetic method of chelating fiber with selective adsorption on Cr (VI) |
| CN104389159A (en) * | 2014-10-20 | 2015-03-04 | 中国石油化工股份有限公司 | Preparation method of polyphenylene sulfide chelate fiber |
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|---|---|---|---|---|
| CN102861558A (en) * | 2012-09-24 | 2013-01-09 | 浙江工商大学 | Method for preparing chelate-resin metal adsorbing material from polyacrylonitrile |
| CN104018346A (en) * | 2014-05-26 | 2014-09-03 | 浙江工商大学 | Synthetic method of chelating fiber with selective adsorption on Cr (VI) |
| CN104389159A (en) * | 2014-10-20 | 2015-03-04 | 中国石油化工股份有限公司 | Preparation method of polyphenylene sulfide chelate fiber |
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