CN104226263A - Method I for preparing amino-modified attapulgite adsorbent and method II for removing hexavalent chromium from water - Google Patents
Method I for preparing amino-modified attapulgite adsorbent and method II for removing hexavalent chromium from water Download PDFInfo
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Abstract
The invention relates to a method I for preparing an amino-modified attapulgite adsorbent. The method I comprises the following steps: performing the reaction on an amino reagent and a silane coupling agent to obtain solution A; performing the grafting reaction on the surface of preprocessed attapulgite by utilizing the solution A so as to obtain the amino-modified attapulgite adsorbent. The invention further discloses a method II for removing hexavalent chromium from water by utilizing the amino-modified attapulgite adsorbent. The method II comprises the following steps: adding the amino-modified attapulgite adsorbent of which mass is 0.0005 time of a water body to be purified into the water body to be purified; adsorbing hexavalent chromium in the water under the conditions of a temperature of 25 DEG C and pH of 3.0 to 9.9; after adsorbing for 10min to 24h, collecting the amino-modified attapulgite adsorbent and purifying hexavalent chromium in the water body. According to the invention, the amino reagent is adopted to modify the attapulgite so as to synthesize the attapulgite adsorbent with high amino content; the modified attapulgite has stable chemical performance and is not influenced by the outside environmental factors. The method disclosed by the invention is simple to operate, low in cost and high in adsorption property.
Description
Technical field
The invention belongs to technical field of water pollution control, be specifically related to a kind of preparation method of amino modified attapulgite clay adsorbent, the invention still further relates to and utilize the amino modified attapulgite clay adsorbent of above-mentioned preparation to remove chromic method in water.
Background technology
A large amount of discharges of chromate waste water, cause chromic content overproof in water body, seriously compromise the safety of the mankind and natural ecosystems.Chromium mainly exists with trivalent chromium and chromic form in water body, compared with trivalent chromium, chromic toxicity is stronger, enrichment can be gathered for a long time in biology and human body, it is a kind of heavily contaminated surrounding material, Cr VI has very high transfer ability, in water body, chromic existence not only has a significant impact the growth of plant, also exist the health of human body and threaten, chromic long-term absorption can cause the disease such as squamous cell carcinoma, gland cancer, and Long Term Contact Cr VI also may bring harmful effect to the intelligence development of its offspring.
At present, have a variety of for chromic method in removal water, such as reduction precipitation method, ion-exchange, membrane processing method, counter-infiltration, absorption method etc., this several method all has good removal effect to Cr VI in water.Wherein absorption method removal effect is good, easy and simple to handle, be widely used in the Cr VI removed in water, other processing methods have some limitations respectively, such as cost is high, troublesome poeration, removal effect are undesirable, adsorption capacity is low, therefore, exploitation clearance is high, and the adsorbent of low cost becomes a chromic direction in process water.
Absorption method is a kind of simple to operate, method for treating water efficiently and effectively, the loose structure adsorbing metal ions of adsorbent utilization itself, or by contained various active group itself as hydroxyl, carboxyl, amino etc., form coordination or complex compound with metal ion, reach the object removing metal ion.Domestic conventional active carbon is as adsorbent, and remove Cr VI in water, its regeneration is comparatively complicated, and somewhat expensive, processing cost is high.
Attapulgite be a kind of have chain layer structure containing Shuifu County's zeopan clay mineral, become tiny bar-shaped, have larger specific area and more duct, water imbibition is strong, and plasticity is strong.In China, attapulgite rich reserves, compared with active carbon, price is comparatively cheap.Due to attapulgite have that specific area is large, the feature such as absorption property is strong, source is wide and cost is low, therefore can be used for sewage disposal.
Amido class adsorbent is as a kind of new adsorbent, and amido has stronger compatibility to the heavy metal in water, the amido functional group generation protonation utilizing it to contain, and has an effect with containing Cr VI anion thus removes hexavalent chromium.At present, common amido class material mainly contains: polyaniline, amino resin, polymine, polyamide etc.
Summary of the invention
The object of this invention is to provide a kind of preparation method of amino modified attapulgite clay adsorbent, the amino modified attapulgite clay adsorbent prepared is with low cost, and absorption property is good.
Another object of the present invention is to provide one and utilizes amino modified attapulgite clay adsorbent to remove chromic method in water.
The technical solution adopted in the present invention is, the preparation method of amino modified attapulgite clay adsorbent, specifically implements according to following steps:
Step 1, the pretreatment of attapulgite;
Step 2, reacts amino agents and silane coupler, obtains solution A;
Step 3, the solution A utilizing step 2 the to obtain attapulgite's surface pretreated to step 1 carries out graft reaction, obtains amino modified attapulgite clay adsorbent.
Feature of the present invention is also,
In step 1, the pretreated specific implementation process of attapulgite is: joined by attapulgite in distilled water and mix ultrasonic disperse 10 ~ 30min, filter remove bottom large particulate matter, centrifugal, dry, grinding, roasting; Baked attapulgite is placed in the hydrochloric acid solution ultrasonic disperse that concentration is 1 ~ 5mol/L, filters after reacting 8 ~ 9h under 80 DEG C ~ 90 DEG C conditions, washing, to neutral, is dried, for subsequent use.
The mass volume ratio of attapulgite and distilled water is 1:10 ~ 20g/mL, and the mass volume ratio of baked attapulgite and hydrochloric acid solution is 1:10 ~ 20g/mL.
The specific implementation process of step 2 is: join in methyl alcohol by silane coupler and amido reagent, filters under nitrogen protection after 80 ~ 90 DEG C of reaction 8 ~ 24h, by the solution A volume concentration that obtains to 40mL, for subsequent use.
The volume ratio of silane coupler, amido reagent, methyl alcohol is 10:3 ~ 9:200.
Silane coupler is γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane; Amido reagent is the one in ethylenediamine EDA, triethylene tetramine TETA or TEPA TEPA.
The specific implementation process of step 3 is: pretreated for step 1 attapulgite is joined ultrasonic disperse 10min in toluene, then the solution A that step 2 obtains is added, wash with methyl alcohol extracting after reaction 12 ~ 36h under the conditions of 110 ~ 120 DEG C stir, and vacuum drying under 60 DEG C of conditions, grinding, obtains.
The mass volume ratio of pretreated attapulgite, toluene, solution A is 1:20:8g/mL.
Another technical scheme of the present invention is, amino modified attapulgite clay adsorbent is utilized to remove chromic method in water, it is the amino modified attapulgite clay adsorbent adding its quality 0.0005 times in the water body of 80 ~ 200mg/L for purification at hexavalent chromium concentration, 25 DEG C, pH be the condition of 3.0 ~ 9.9 under Cr VI in adsorbed water, amino modified attapulgite clay adsorbent is collected, the Cr VI in purifying water body after absorption 10min ~ 24h.
The invention has the beneficial effects as follows, the preparation method of amino modified attapulgite clay adsorbent of the present invention, carries out modification with amido reagent to attapulgite, and synthesis has the attapulgite clay adsorbent of high amino content; Modified attapulgite stable chemical nature, not affect by outside environmental elements, and the inventive method is simple to operate, with low cost, absorption property is good.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
The preparation method of amino modified attapulgite clay adsorbent of the present invention, specifically implements according to following steps:
Step 1, the pretreatment of attapulgite
Attapulgite is joined in distilled water and mix ultrasonic disperse 10 ~ 30min, filter and remove bottom large particulate matter, centrifugal (3500r/min), oven dry (80 DEG C), grinding, roasting (500 DEG C); Baked attapulgite is placed in the hydrochloric acid solution ultrasonic disperse that concentration is 1 ~ 5mol/L, filters after reacting 8 ~ 9h under 80 DEG C ~ 90 DEG C conditions, washing, to neutral, is dried, for subsequent use;
Wherein, the mass volume ratio of attapulgite and distilled water is 1:10 ~ 20g/mL, and the mass volume ratio of baked attapulgite and hydrochloric acid solution is 1:10 ~ 20g/mL;
Step 2, joins in methyl alcohol by silane coupler and amido reagent, filters under nitrogen protection after 80 ~ 90 DEG C of reaction 8 ~ 24h, by the solution A volume concentration that obtains to 40mL, for subsequent use;
Wherein, the volume ratio of silane coupler, amido reagent, methyl alcohol is 10:3 ~ 9:200;
Silane coupler is γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane; Amido reagent is the one in ethylenediamine EDA, triethylene tetramine TETA or TEPA TEPA;
Step 3, pretreated for step 1 attapulgite is joined ultrasonic disperse 10min in toluene, then the solution A (mass volume ratio of pretreated attapulgite, toluene, solution A is 1:20:8g/mL) that step 2 obtains is added, reaction 12 ~ 24h under the conditions of 110 ~ 120 DEG C stir, afterwards with methyl alcohol extracting washing, and vacuum drying under 60 DEG C of conditions, grinding, obtains amino modified attapulgite clay adsorbent.
Preparation method of the present invention is in methanol solution, amido reagent and silane coupler generation ring-opening reaction, obtain silane compound, afterwards in toluene solution, the hydroxyl that the hydrolysis of silicon oxygen bond in silane compound and attapulgite contain is utilized to react, thus the attapulgite of obtained amino modified.
Amino modified attapulgite clay adsorbent is utilized to remove chromic method in water, it is the amino modified attapulgite clay adsorbent adding its quality 0.0005 times in the water body of 80 ~ 200mg/L for purification at hexavalent chromium concentration, 25 DEG C, pH be the condition of 3.0 ~ 9.9 under Cr VI in adsorbed water, amino modified attapulgite clay adsorbent is collected, the Cr VI in purifying water body after absorption 10min ~ 24h.
On attapulgite there is protonated positively charged in the amido of grafting in acid condition, and in water, Cr VI exists with anionic form, by electrostatic attraction effect, makes Cr VI in water be adsorbed onto attapulgite's surface, thus reach chromic effect in removal water.
The preparation method of amino modified attapulgite clay adsorbent of the present invention, carries out modification with amido reagent to attapulgite, and synthesis has the attapulgite clay adsorbent of high amino content; Modified attapulgite stable chemical nature, not affect by outside environmental elements, and the inventive method is simple to operate, with low cost, absorption property is good.
Embodiment 1
Step 1, the pretreatment of attapulgite
10g attapulgite ATP is joined in 200mL distilled water and mixes ultrasonic disperse 30min, filter and remove bottom large particulate matter, centrifugal (3500r/min), oven dry (80 DEG C), grinding, roasting (500 DEG C); By the hydrochloric acid solution ultrasonic disperse that baked attapulgite 5g is placed in 100mL, concentration is 1mol/L, filter after reacting 8h under 80 DEG C of conditions, washing, to neutral, is dried, for subsequent use;
Step 2, joins in 100mL methyl alcohol by 5mL γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane and 1.5mL ethylenediamine EDA, filters under nitrogen protection after 80 DEG C of reaction 24h, by the solution A volume concentration that obtains to 40mL, for subsequent use;
Step 3, pretreated for step 1 attapulgite is joined ultrasonic disperse 10min in toluene, then the solution A (mass volume ratio of pretreated attapulgite, toluene, solution A is 1:20:8g/mL) that step 2 obtains is added, 24h is reacted under the conditions of 110 DEG C stir, afterwards with methyl alcohol extracting washing, and vacuum drying under 60 DEG C of conditions, grinding, obtains EDA-ATP adsorbent.
Embodiment 2
Step 1, the pretreatment of attapulgite
10g attapulgite ATP is joined in 200mL distilled water and mixes ultrasonic disperse 30min, filter and remove bottom large particulate matter, centrifugal (3500r/min), oven dry (80 DEG C), grinding, roasting (500 DEG C); By the hydrochloric acid solution ultrasonic disperse that baked attapulgite 5g is placed in 100mL, concentration is 1mol/L, filter after reacting 8h under 80 DEG C of conditions, washing, to neutral, is dried, for subsequent use;
Step 2, joins in 100mL methyl alcohol by 5mL γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane and 3.4mL triethylene tetramine TETA, filters under nitrogen protection after 80 DEG C of reaction 24h, by the solution A volume concentration that obtains to 40mL, for subsequent use;
Step 3, pretreated for step 1 attapulgite is joined ultrasonic disperse 10min in toluene, then the solution A (mass volume ratio of pretreated attapulgite, toluene, solution A is 1:20:8g/mL) that step 2 obtains is added, 24h is reacted under the conditions of 110 DEG C stir, afterwards with methyl alcohol extracting washing, and vacuum drying under 60 DEG C of conditions, grinding, obtains TETA-ATP adsorbent.
Embodiment 3
Step 1, the pretreatment of attapulgite
10g attapulgite ATP is joined in 200mL distilled water and mixes ultrasonic disperse 30min, filter and remove bottom large particulate matter, centrifugal (3500r/min), oven dry (80 DEG C), grinding, roasting (500 DEG C); By the hydrochloric acid solution ultrasonic disperse that baked attapulgite 5g is placed in 100mL, concentration is 1mol/L, filter after reacting 8h under 80 DEG C of conditions, washing, to neutral, is dried, for subsequent use;
Step 2, joins in 100mL methyl alcohol by 5mL γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane and 4.4ml TEPA TEPA, filters under nitrogen protection after 80 DEG C of reaction 8h, by the solution A volume concentration that obtains to 40mL, for subsequent use;
Step 3, pretreated for step 1 attapulgite is joined ultrasonic disperse 10min in toluene, then the solution A (mass volume ratio of pretreated attapulgite, toluene, solution A is 1:20:8g/mL) that step 2 obtains is added, 24h is reacted under the conditions of 110 DEG C stir, afterwards with methyl alcohol extracting washing, and vacuum drying under 60 DEG C of conditions, grinding, obtains TEPA-ATP adsorbent.
Embodiment 4
Step 1, the pretreatment of attapulgite
10g attapulgite ATP is joined in 100mL distilled water and mixes ultrasonic disperse 10min, filter and remove bottom large particulate matter, centrifugal (3500r/min), oven dry (80 DEG C), grinding, roasting (500 DEG C); By the hydrochloric acid solution ultrasonic disperse that baked attapulgite 5g is placed in 50mL, concentration is 3mol/L, filter after reacting 9h under 85 DEG C of conditions, washing, to neutral, is dried, for subsequent use;
Step 2, joins in 100mL methyl alcohol by 5mL γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane and 4.5mL ethylenediamine EDA, filters under nitrogen protection after 85 DEG C of reaction 18h, by the solution A volume concentration that obtains to 40mL, for subsequent use;
Step 3, pretreated for step 1 attapulgite is joined ultrasonic disperse 10min in toluene, then the solution A (mass volume ratio of pretreated attapulgite, toluene, solution A is 1:20:8g/mL) that step 2 obtains is added, 18h is reacted under the conditions of 115 DEG C stir, afterwards with methyl alcohol extracting washing, and vacuum drying under 60 DEG C of conditions, grinding, obtains EDA-ATP adsorbent.
Embodiment 5
Step 1, the pretreatment of attapulgite
10g attapulgite ATP is joined in 150mL distilled water and mixes ultrasonic disperse 20min, filter and remove bottom large particulate matter, centrifugal (3500r/min), oven dry (80 DEG C), grinding, roasting (500 DEG C); By the hydrochloric acid solution ultrasonic disperse that baked attapulgite 5g is placed in 75mL, concentration is 5mol/L, filter after reacting 8.5h under 90 DEG C of conditions, washing, to neutral, is dried, for subsequent use;
Step 2, joins in 100mL methyl alcohol by 5mL γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane and 2.0mL ethylenediamine EDA, filters under nitrogen protection after 90 DEG C of reaction 15h, by the solution A volume concentration that obtains to 40mL, for subsequent use;
Step 3, pretreated for step 1 attapulgite is joined ultrasonic disperse 10min in toluene, then the solution A (mass volume ratio of pretreated attapulgite, toluene, solution A is 1:20:8g/mL) that step 2 obtains is added, 12h is reacted under the conditions of 120 DEG C stir, afterwards with methyl alcohol extracting washing, and vacuum drying under 60 DEG C of conditions, grinding, obtains EDA-ATP adsorbent.
Amino modified attapulgite clay adsorbent removes chromic embodiment in water
Embodiment 6
Using EDA-ATP as adsorbent, Cr VI in Adsorption water.The EDA-ATP of its quality 0.0005 times is added to the water body for purification, chromic initial concentration is 80mg/L, it is 25 DEG C in temperature, pH is constant temperature oscillation absorption under the condition of 3.00, adsorption time is after 24h, 24h, crosses leaching filtrate, recording chromic adsorbance is 137.91mg/g, and clearance is 73.09%.
Embodiment 7
With embodiment 6, using TETA-ATP as adsorbent, other conditions are constant, and recording chromic adsorbance is 182.00mg/g, and clearance is 91.00%.
Embodiment 8
With embodiment 6, using TEPA-ATP as adsorbent, other conditions are constant, and recording chromic adsorbance is 186.96mg/g, and clearance is 98.62%.
Embodiment 9
With embodiment 7, using TETA-ATP as adsorbent, chromic initial solubility is 100mg/L, and other conditions are constant, and recording chromic adsorption capacity is 207.32mg/g, and clearance is 81.27%.
Embodiment 10
With embodiment 9, using TETA-ATP as adsorbent, chromic initial solubility is 200mg/L, and other conditions are constant, and recording chromic adsorption capacity is 251.34mg/g, and clearance is 51.53%.
As can be seen from embodiment 7,9,10, adsorbent increases along with the increase of initial concentration chromic adsorbance, has higher clearance when low concentration.
Embodiment 11
With embodiment 7, using TETA-ATP as adsorbent, adsorption time is 10min, and chromic initial solubility is 100mg/L, and other conditions are constant, and recording chromic adsorbance is 87.92mg/g, and clearance is 35.17%.
Embodiment 12
With embodiment 11, using TETA-ATP as adsorbent, adsorption time is 240min, and other conditions are constant, and recording chromic adsorbance is 182.63mg/g, and clearance is 73.05%.
Embodiment 13
With embodiment 11, using TETA-ATP as adsorbent, adsorption time is 720min, and other conditions are constant, and recording chromic adsorbance is 201.06mg/g, and clearance is 80.42%.
From embodiment 11 ~ 13, before reaching adsorption equilibrium, chromic adsorbance increases gradually along with the increase of time, and adsorption time is longer, and clearance is higher.
Embodiment 14
With embodiment 7, using TETA-ATP as adsorbent, as PO in solution
4 3-when ion concentration is 2mmol/L, chromic initial solubility is 100mg/L, and other conditions are constant, and recording chromic adsorbance is 174.15mg/g, and clearance is 69.66%;
Embodiment 15
With embodiment 14, using TETA-ATP as adsorbent, as PO in solution
4 3-when ion concentration is 10mmol/L, other conditions are constant, and recording chromic adsorbance is 122.07mg/g, and chromic clearance is 51.27%;
Embodiment 16
With embodiment 14, using TETA-ATP as adsorbent, as PO in solution
4 3-when ion concentration is 20mmol/L, other conditions are constant, and recording chromic adsorbance is 113.06mg/g, and chromic clearance is 48.39%;
From embodiment 14 ~ 16, PO in water
4 3-it is attapulgite modified to chromic adsorbance that the existence of ion can reduce triethylene tetramine merit.
Embodiment 17
With embodiment 7, using TETA-ATP as adsorbent, in adsorption conditions, pH is adjusted to 3.89, other conditions are constant, and recording chromic adsorbance is 108.78mg/g, and clearance is 45.25%.
Embodiment 18
With embodiment 17, using TETA-ATP as adsorbent, pH is adjusted to 6.81, other conditions are constant, and recording chromic adsorbance is 50.85mg/g, and clearance is 21.36%.
Embodiment 19
With embodiment 17, using TETA-ATP as adsorbent, pH is adjusted to 9.9, other conditions are constant, and recording chromic adsorbance is 18.16mg/g, and clearance is 9.22%.
From embodiment 17 ~ 19, triethylene tetramine is attapulgite modified to be reduced along with the rising of pH adsorbance chromic in water, and low pH is conducive to chromic removal in water.
Comparative example 20
With concave convex rod original soil for adsorbent, adsorption conditions is with embodiment 1, and recording attapulgite to chromic adsorbance is 1.26mg/g, and clearance is 1.02%, is starkly lower than Egyptian modified attapulgite earth adsorbing.
Claims (9)
1. the preparation method of amino modified attapulgite clay adsorbent, is characterized in that, specifically implements according to following steps:
Step 1, the pretreatment of attapulgite;
Step 2, reacts amino agents and silane coupler, obtains solution A;
Step 3, the solution A utilizing step 2 the to obtain attapulgite's surface pretreated to step 1 carries out graft reaction, obtains amino modified attapulgite clay adsorbent.
2. the preparation method of amino modified attapulgite clay adsorbent according to claim 1, it is characterized in that, in step 1, the pretreated specific implementation process of attapulgite is: joined by attapulgite in distilled water and mix ultrasonic disperse 10 ~ 30min, filter remove bottom large particulate matter, centrifugal, dry, grinding, roasting; Baked attapulgite is placed in the hydrochloric acid solution ultrasonic disperse that concentration is 1 ~ 5mol/L, filters after reacting 8 ~ 9h under 80 DEG C ~ 90 DEG C conditions, washing, to neutral, is dried, for subsequent use.
3. the preparation method of amino modified attapulgite clay adsorbent according to claim 2, it is characterized in that, the mass volume ratio of attapulgite and distilled water is 1:10 ~ 20g/mL, and the mass volume ratio of baked attapulgite and hydrochloric acid solution is 1:10 ~ 20g/mL.
4. the preparation method of amino modified attapulgite clay adsorbent according to claim 1; it is characterized in that; the specific implementation process of step 2 is: join in methyl alcohol by silane coupler and amido reagent; filter after 80 ~ 90 DEG C of reaction 8 ~ 24h under nitrogen protection; by the solution A volume concentration that obtains to 40mL, for subsequent use.
5. the preparation method of amino modified attapulgite clay adsorbent according to claim 4, is characterized in that, the volume ratio of silane coupler, amido reagent, methyl alcohol is 10:3 ~ 9:200.
6. the preparation method of the amino modified attapulgite clay adsorbent according to claim 4 or 5, is characterized in that, silane coupler is γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane; Amido reagent is the one in ethylenediamine EDA, triethylene tetramine TETA or TEPA TEPA.
7. the preparation method of amino modified attapulgite clay adsorbent according to claim 1, it is characterized in that, the specific implementation process of step 3 is: pretreated for step 1 attapulgite is joined ultrasonic disperse 10min in toluene, then the solution A that step 2 obtains is added, wash with methyl alcohol extracting after reaction 12 ~ 36h under the conditions of 110 ~ 120 DEG C stir, and vacuum drying under 60 DEG C of conditions, grinding, obtains.
8. the preparation method of amino modified attapulgite clay adsorbent according to claim 7, is characterized in that, the mass volume ratio of pretreated attapulgite, toluene, solution A is 1:20:8g/mL.
9. utilize the amino modified attapulgite clay adsorbent described in claim 1 to remove chromic method in water, it is characterized in that, it is the amino modified attapulgite clay adsorbent adding its quality 0.0005 times in the water body of 80 ~ 200mg/L for purification at hexavalent chromium concentration, 25 DEG C, pH be the condition of 3.0 ~ 9.9 under Cr VI in adsorbed water, amino modified attapulgite clay adsorbent is collected, the Cr VI in purifying water body after absorption 10min ~ 24h.
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| CN104722265A (en) * | 2015-03-27 | 2015-06-24 | 陕西科技大学 | Preparation method and application of modified attapulgite adsorbent |
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