CN106390936A - Illite adsorbent as well as preparation method and application thereof - Google Patents
Illite adsorbent as well as preparation method and application thereof Download PDFInfo
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- CN106390936A CN106390936A CN201611116378.3A CN201611116378A CN106390936A CN 106390936 A CN106390936 A CN 106390936A CN 201611116378 A CN201611116378 A CN 201611116378A CN 106390936 A CN106390936 A CN 106390936A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Dispersion Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Hydrology & Water Resources (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses an illite adsorbent as well as a preparation method and application thereof. The adsorbent comprises the following raw materials in parts by weight: 33 to 41 parts of illite, 1 to 5 parts of triethanolamine oleate, 7 to 15 parts of mercaptoacetic acid, and 3 to 7 parts of trimethyl citrate. The method comprises the following steps: mixing and grinding illite and trimethyl citrate, adding a mercaptoacetic acid solution, performing sealing, heating and stirring treatment and ultrasonic treatment, dropwise adding triethanolamine oleate, heating, stirring, and performing high temperature calcinations, so as to obtain the adsorbent. According to the method, the optimal technological parameters are screened out through a large quantity of tests, the adsorbent with good heavy metal ion adsorption property can be effectively prepared, and the adsorbent has a wider pH value application range, and has extremely high heavy metal adsorption capacity even in an acidic condition. The preparation method is simple, economical and environmental-friendly, reduces the cost, is wide in raw material source, guarantees the precondition for the preparation of a large amount of adsorbents, does not cause secondary pollution, and is easy for heavy metal recovery and suitable for industrial production.
Description
Technical field
The present invention relates to environment-friendly materials technical field, specifically a kind of illite adsorbent and its preparation method and application.
Background technology
At present China due in the exploitation of heavy metal, smelting, process, cause many heavy metals for example lead, mercury, cadmium,
Cobalt etc. enters big gas and water, soil causes serious environmental pollution.As the heavy metal discharged with waste water, even if concentration is little, also can be
Accumulate in algae and bed mud, adsorbed by fish and shellfish body surface, produce food chain and concentrate, thus causing public hazards.At present, heavy metal gives up
Method for treating water mainly has three classes:Chemical reaction removal method, Adsorption Concentration separation removal method and microorganism or plant removal method.
The conventional processes generally existing high cost of metallic wastewater, reaction is slow, easily cause secondary pollution, regeneration effect is poor, low concentration
The shortcomings of wastewater treatment is difficult.Absorption method be using adsorbent unique texture toward removing heavy metals ion a kind of effective ways.Inhale
Attached method processes heavy metal wastewater thereby and has efficient, easy and good selective, particularly strong to low concentration, contaminative, other
The heavy metal wastewater thereby that method is difficult to effective process has unique using value.Although the adsorbent of pure chemical material preparation goes
Except efficiency high, but the amount of each preparation is relatively fewer, and preparation cost is higher, can produce secondary pollution, needs to meet during use
Certain acid-base value, is difficult to realize large-scale industrialization application.Process the conventional suction of electroplated heavy metals waste water using absorption method
Attached dose of active charcoal, humic acid, sepiolite etc..Illite makes it seldom be used due to the structural limitation of its own.
Content of the invention
It is an object of the invention to provide a kind of illite adsorbent and its preparation method and application, to solve above-mentioned background
The problem proposing in technology.
For achieving the above object, the present invention provides following technical scheme:
A kind of illite adsorbent, is made up of the following raw material according to weight portion:Illite 33-41 part, oleic acid triethanolamine
Amine 1-5 part, TGA 7-15 part, trimethyl citrate 3-7 part.
As the further scheme of the present invention:Described illite adsorbent, is made up of the following raw material according to weight portion:She
Sharp stone 35-39 part, triethanolamine oleate 2-4 part, TGA 9-13 part, trimethyl citrate 4-6 part.
As the further scheme of the present invention:Described illite adsorbent, is made up of the following raw material according to weight portion:She
37 parts of sharp stone, 3 parts of triethanolamine oleate, 11 parts of TGA, 5 parts of trimethyl citrate.
The present invention another object is that provides a kind of preparation method of illite adsorbent, comprises the steps of:
1) deionized water of 10.8 times of TGA and its quality is mixed, prepared mercaptoacetic acid solution;
2) by illite and trimethyl citrate mixed grinding, cross 120 mesh sieves, add mercaptoacetic acid solution, Ran Housheng
Temperature to 143 DEG C and at such a temperature seals stir process 42min, then is down to 65 DEG C and ultrasonically treated 37min at such a temperature, super
Acoustical power is 800W, then drips triethanolamine oleate, stirs 93min, Ran Hou after dripping again at a temperature of 79 DEG C
Stir at a temperature of 100-103 DEG C to dry, then calcining 3.3h obtains final product adsorbent at a temperature of 400 DEG C.
The present invention another object is that offer application in heavy metal-polluted water process for the described adsorbent.
Compared with prior art, the invention has the beneficial effects as follows:
Illite and trimethyl citrate mixed grinding in the present invention, recycle TGA heated sealed, ultrasonically treated,
The preparation technologies such as dropping triethanolamine oleate heating, high-temperature calcination, filter out optimal technological parameter by lot of experiments,
The adsorbent with fine Adsorption of Heavy Metal Ions performance can efficiently be prepared, there is wider array of pH value range of application,
Equally there is under acid condition high heavy metal adsorption capacity.Preparation method of the present invention is simple, economy, environmental protection, reduces
The preparation of adsorbent and follow-up application cost, and raw material sources are extensively, ensured the premise bar of a large amount of adsorbents preparations
Part, illite is high with the product yield after other raw material mixed processing, and preparation time is short, non-secondary pollution, and heavy metal recovery holds
Easily, it is suitable to industrialized production, be suitable to high-concentration and low-concentration heavy metal containing wastewater treatment field.The present invention is recyclable heavy using rear acid treatment
Metal, then 450 DEG C of high-temperature calcinations are renewable, repeats using number of times up to more than 10 times, through test, after reusing 10 times
The adsorption capacity of adsorbent is more than 85% adsorbing first.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the present invention is clearly and completely described,
Obviously, described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based in the present invention
Embodiment, the every other embodiment that those of ordinary skill in the art are obtained under the premise of not making creative work, all
Belong to the scope of protection of the invention.
Embodiment 1
In the embodiment of the present invention, a kind of illite adsorbent, it is made up of the following raw material according to weight portion:Illite 33
Part, 1 part of triethanolamine oleate, 7 parts of TGA, 3 parts of trimethyl citrate.
10.8 times of deionized water of TGA and its quality is mixed, prepared mercaptoacetic acid solution.By illite and lemon
Lemon acid trimethyl mixed grinding, cross 120 mesh sieves, add mercaptoacetic acid solution, then heat to 143 DEG C and close at such a temperature
Envelope stir process 42min, then it is down to 65 DEG C and ultrasonically treated 37min at such a temperature, ultrasonic power is 800W, and then dropping is oily
Triethylenetetraminehexaacetic acid hydramine, stirs 93min after dripping again at a temperature of 79 DEG C, then stirs at a temperature of 100 DEG C to dry, then
At a temperature of 400 DEG C, calcining 3.3h obtains final product adsorbent.
Embodiment 2
In the embodiment of the present invention, a kind of illite adsorbent, it is made up of the following raw material according to weight portion:Illite 41
Part, 5 parts of triethanolamine oleate, 15 parts of TGA, 7 parts of trimethyl citrate.
10.8 times of deionized water of TGA and its quality is mixed, prepared mercaptoacetic acid solution.By illite and lemon
Lemon acid trimethyl mixed grinding, cross 120 mesh sieves, add mercaptoacetic acid solution, then heat to 143 DEG C and close at such a temperature
Envelope stir process 42min, then it is down to 65 DEG C and ultrasonically treated 37min at such a temperature, ultrasonic power is 800W, and then dropping is oily
Triethylenetetraminehexaacetic acid hydramine, stirs 93min after dripping again at a temperature of 79 DEG C, then stirs at a temperature of 103 DEG C to dry, then
At a temperature of 400 DEG C, calcining 3.3h obtains final product adsorbent.
Embodiment 3
In the embodiment of the present invention, a kind of illite adsorbent, it is made up of the following raw material according to weight portion:Illite 35
Part, 2 parts of triethanolamine oleate, 9 parts of TGA, 4 parts of trimethyl citrate.
10.8 times of deionized water of TGA and its quality is mixed, prepared mercaptoacetic acid solution.By illite and lemon
Lemon acid trimethyl mixed grinding, cross 120 mesh sieves, add mercaptoacetic acid solution, then heat to 143 DEG C and close at such a temperature
Envelope stir process 42min, then it is down to 65 DEG C and ultrasonically treated 37min at such a temperature, ultrasonic power is 800W, and then dropping is oily
Triethylenetetraminehexaacetic acid hydramine, stirs 93min after dripping again at a temperature of 79 DEG C, then stirs at a temperature of 101 DEG C to dry, then
At a temperature of 400 DEG C, calcining 3.3h obtains final product adsorbent.
Embodiment 4
In the embodiment of the present invention, a kind of illite adsorbent, it is made up of the following raw material according to weight portion:Illite 39
Part, 4 parts of triethanolamine oleate, 13 parts of TGA, 6 parts of trimethyl citrate.
10.8 times of deionized water of TGA and its quality is mixed, prepared mercaptoacetic acid solution.By illite and lemon
Lemon acid trimethyl mixed grinding, cross 120 mesh sieves, add mercaptoacetic acid solution, then heat to 143 DEG C and close at such a temperature
Envelope stir process 42min, then it is down to 65 DEG C and ultrasonically treated 37min at such a temperature, ultrasonic power is 800W, and then dropping is oily
Triethylenetetraminehexaacetic acid hydramine, stirs 93min after dripping again at a temperature of 79 DEG C, then stirs at a temperature of 101 DEG C to dry, then
At a temperature of 400 DEG C, calcining 3.3h obtains final product adsorbent.
Embodiment 5
In the embodiment of the present invention, a kind of illite adsorbent, it is made up of the following raw material according to weight portion:Illite 37
Part, 3 parts of triethanolamine oleate, 11 parts of TGA, 5 parts of trimethyl citrate.
10.8 times of deionized water of TGA and its quality is mixed, prepared mercaptoacetic acid solution.By illite and lemon
Lemon acid trimethyl mixed grinding, cross 120 mesh sieves, add mercaptoacetic acid solution, then heat to 143 DEG C and close at such a temperature
Envelope stir process 42min, then it is down to 65 DEG C and ultrasonically treated 37min at such a temperature, ultrasonic power is 800W, and then dropping is oily
Triethylenetetraminehexaacetic acid hydramine, stirs 93min after dripping again at a temperature of 79 DEG C, then stirs at a temperature of 101 DEG C to dry, then
At a temperature of 400 DEG C, calcining 3.3h obtains final product adsorbent.
Comparative example 1
In addition to not containing TGA, its material content and preparation process are consistent with embodiment 5.
Comparative example 2
In addition to not containing triethanolamine oleate, its material content and preparation process are consistent with embodiment 5.
Comparative example 3
In addition to not containing TGA and triethanolamine oleate, its material content and preparation process are consistent with embodiment 5.
1g embodiment 1-5 and comparative example 1-3 is taken to be the Pb that adsorbent is added to 1L 1000mg/L respectively respectively2+、Cd2+、
Cu2+、Ni2+In solution (pH=4), finally calculate the adsorption capacity to each metal for each adsorbent, result is as shown in table 1.Can
Know, present invention heavy metal under the interaction of each raw material has high adsorption capacity.
Table 1
It is obvious to a person skilled in the art that the invention is not restricted to the details of above-mentioned one exemplary embodiment, Er Qie
In the case of the spirit or essential attributes of the present invention, the present invention can be realized in other specific forms.Therefore, no matter
From the point of view of which point, embodiment all should be regarded as exemplary, and be nonrestrictive, the scope of the present invention is by appended power
Profit requires rather than described above limits, it is intended that all in the implication and scope of the equivalency of claim by falling
Change is included in the present invention.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment only wraps
Containing an independent technical scheme, only for clarity, those skilled in the art should for this narrating mode of specification
Using specification as an entirety, the technical scheme in each embodiment can also form those skilled in the art through appropriately combined
Understandable other embodiment.
Claims (5)
1. a kind of illite adsorbent is it is characterised in that be made up of the following raw material according to weight portion:Illite 33-41 part, oil
Triethylenetetraminehexaacetic acid hydramine 1-5 part, TGA 7-15 part, trimethyl citrate 3-7 part.
2. illite adsorbent according to claim 1 is it is characterised in that be made up of the following raw material according to weight portion:
Illite 35-39 part, triethanolamine oleate 2-4 part, TGA 9-13 part, trimethyl citrate 4-6 part.
3. illite adsorbent according to claim 1 is it is characterised in that be made up of the following raw material according to weight portion:
37 parts of illite, 3 parts of triethanolamine oleate, 11 parts of TGA, 5 parts of trimethyl citrate.
4. a kind of preparation method of described illite adsorbent as arbitrary in claim 1-3 is it is characterised in that by following steps
Composition:
1) deionized water of 10.8 times of TGA and its quality is mixed, prepared mercaptoacetic acid solution;
2) by illite and trimethyl citrate mixed grinding, cross 120 mesh sieves, add mercaptoacetic acid solution, then heat to
143 DEG C and seal stir process 42min at such a temperature, then it is down to 65 DEG C and ultrasonically treated 37min at such a temperature, ultrasonic work(
Rate is 800W, then drips triethanolamine oleate, stirs 93min again, then in 100-103 after dripping at a temperature of 79 DEG C
Stir at a temperature of DEG C to dry, then calcining 3.3h obtains final product adsorbent at a temperature of 400 DEG C.
5. application in heavy metal-polluted water process for the described adsorbent as arbitrary in claim 1-3.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108176351A (en) * | 2017-12-29 | 2018-06-19 | 薛彦芳 | A kind of sewage disposal vermiculite based material and its preparation method and application |
CN108176352A (en) * | 2018-01-05 | 2018-06-19 | 成伟 | A kind of inorganic agent of treated sewage and its preparation method and application |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108176351A (en) * | 2017-12-29 | 2018-06-19 | 薛彦芳 | A kind of sewage disposal vermiculite based material and its preparation method and application |
CN108176352A (en) * | 2018-01-05 | 2018-06-19 | 成伟 | A kind of inorganic agent of treated sewage and its preparation method and application |
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Application publication date: 20170215 |