CN106693901A - Stable attapulgite adsorbent and preparation method thereof - Google Patents
Stable attapulgite adsorbent and preparation method thereof Download PDFInfo
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- CN106693901A CN106693901A CN201611152177.9A CN201611152177A CN106693901A CN 106693901 A CN106693901 A CN 106693901A CN 201611152177 A CN201611152177 A CN 201611152177A CN 106693901 A CN106693901 A CN 106693901A
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- attapulgite
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- azodiisobutyronitrile
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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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
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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
- B01J20/16—Alumino-silicates
- B01J20/165—Natural alumino-silicates, e.g. zeolites
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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
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
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- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a stable attapulgite adsorbent. The invention is characterized in that the stable attapulgite adsorbent is prepared from the following raw materials in parts by weight: 100 parts of attapulgite raw soil, 600-800 parts of sodium chloride solution, 12-15 parts of nano calcium carbonate, 600-800 parts of anhydrous ethanol, 6-8 parts of vinyltriethoxysilane, 70-80 parts of methyl methacrylate, 30-40 parts of 5-hydroxylevulinic acid, 3-4 parts of azodiisobutyronitrile, 8-10 parts of sodium methallyl sulfonate, 500-600 parts of acetone, 600-800 parts of methanol, a right amount of phosphoric acid and a right amount of deionized water. The method is simple in technique and does not generate secondary pollution; and the prepared attapulgite adsorbent has the characteristics of large particle size, easy settling and recovery, and favorable adsorbability, and is suitable for industrial wastewater treatment.
Description
Technical field
The invention belongs to technical field of absorbent, and in particular to a kind of attapulgite clay adsorbent of stabilization and its preparation side
Method.
Background technology
Industrial wastewater causes human body and the great potential safety hazard of animals and plants to the pollution that water body, soil are brought, and how to have
The harm that effect ground eliminates heavy metal is the outstanding problem that current efforts at environmental protection face.In recent years, sorbing material with high because adsorbing
The advantages of efficiency, easily regeneration, adsorption process are exothermic reaction, is widely used in heavy metal ion pollution control.
Attapulgite has the advantages that cheap raw material, aboundresources and specific surface area are big as a kind of natural material, concavo-convex
Rod soil has special fibre structure and crystal structure, is allowed to, with many special materializations and processing performance, there is " thousand soil
King " and the good reputation of " soil of general-purpose ".Because attapulgite has larger specific surface area, stronger suction-operated is made it have,
High-viscosity suspension can be formed under at a fairly low concentration, its rheological property determines that it can be used as dytory, suspends
Agent, thixotropic agent and binding agent, but attapulgite powder there is a problem of being difficult to precipitate in water, easily causes secondary pollution.
Improvement attapulgite property is paid close attention to by those skilled in the art.
Author Yin Jingzhou et al. exists《The absorption of Heavy Metal Ions on Attapulgite Modified by Chitosan》In one text, with concave convex rod
Soil is carrier, by chitosan loaded in attapulgite's surface, then is chelated with heavy metal ion.The adsorbent can both save shitosan
Addition, makes lock out operation simple and easy to apply again, has the advantages that the rate of adsorption is fast, adsorption capacity is big, pollution-free.
The content of the invention
Present invention aim at a kind of attapulgite clay adsorbent of stabilization of offer and preparation method thereof.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of attapulgite clay adsorbent of stabilization, it is characterised in that it is prepared from by the raw material of following weight portion：Concave convex rod is former
Native 100 parts, sodium chloride solution 600-800 parts, nano-calcium carbonate 12-15 parts, absolute ethyl alcohol 600-800 parts, the ethoxy of vinyl three
Base silane 6-8 parts, methyl methacrylate 70-80 parts, 30-40 parts of 5- hydroxylevulinic acids, azodiisobutyronitrile 3-4 parts, first
8-10 parts of base sodium allylsulfonate, acetone 500-600 parts, methyl alcohol 600-800 parts, appropriate phosphoric acid, appropriate deionized water.
The attapulgite clay adsorbent of described stabilization, it is characterised in that it is prepared from by following steps：
（1）Concave convex rod original soil is sieved by 200 mesh sieve, is washed with deionized 3-5 times, remove the impurity of remaining, then used
Sodium chloride solution is washed 2-3 times, and moisture removal is removed in drying；The attapulgite and nano-calcium carbonate that will have been washed are mixed
Compound, after being raised to 250 DEG C from room temperature, by inert gas N2Make vapor and mixture haptoreaction as carrier gas, further
High-temperature is risen to 320-350 DEG C, after keeping 2-3h, starts cooling, and stop adding vapor, after temperature is down to room temperature, taken
Go out, the attapulgite for being pre-processed；
（2）The attapulgite of pretreatment is added to 1/3 absolute ethyl alcohol and the deionized water equivalent to absolute ethyl alcohol weight portion
In the solution of configuration, ultrasonic disperse 2-3h is subsequently adding VTES, adds phosphoric acid, adjusts pH=3-4, heating
Backflow 3-4h, is washed with deionized to neutrality, then with remaining absolute ethanol washing 2-3 times, is dried under vacuum at 40 DEG C
Constant weight is standby；
（3）By step（2）Product, methyl methacrylate, 5- hydroxylevulinic acids, 1/3 azodiisobutyronitrile add dress
Have in the reactor of reflux condensate device, be sufficiently stirred for being well mixed reactant；Oil bath heating heats up, and controlling reaction temperature is
80-90 DEG C, after stirring reaction 3-5h under the rotating speed of 300-500r/min, add remaining azodiisobutyronitrile and metering system
Sodium sulfonate, rises high-temperature to 140-150 DEG C, continues agitating heating 8-10h；Room temperature is cooled to, acetone is added, continues to stir 1-
2h, adds methyl alcohol, standing sedimentation 8-10h, filtering, 60-80 DEG C of vacuum drying 10-12h, the attapulgite absorption stablized
Agent.
The attapulgite clay adsorbent of described stabilization, it is characterised in that described concentration of sodium chloride solution is 2-3mol/L,
The concentration of described phosphoric acid is 1-2mol/L.
The beneficial effects of the invention are as follows：The present invention carries out removal of impurities pretreatment to concave convex rod original soil and uses water vapour pair first
Attapulgite carries out activation process, the cavitation for recycling ultrasonic wave to cause, the shock wave and microjet for being formed in the solution
The strong mutual collision between attapulgite aggregation can be caused, the aggregation of the rod crystalline substance beam of attapulgite or brilliant beam is beaten
It is broken, nano-attapulgite suspension is prepared so as to reach, increase the cation exchange capacity of attapulgite, suppress attapulgite certainly
The phenomenon that body is reunited；Recycle VTES to modify its surface grafting, prepared using the method for in-situ polymerization
Go out the modified attapulgite clay adsorbent of polymethyl methacrylate, by the rigidity of attapulgite, dimensional stability and heat endurance
Toughness, machinability and dielectricity with polymethyl methacrylate ideally combine, not only in absorption trade effluent
Heavy metal cation, moreover it is possible to adsorb Organic Pollution；The present invention also added nano-calcium carbonate, also add the bright and clean of adsorbent
Degree and heat-resistant stability.Present invention process is simple and does not produce secondary pollution, and prepared attapulgite clay adsorbent has particle diameter
Greatly, the characteristics of free settling, easy recovery and good absorption property, it is adaptable to Industrial Wastewater Treatment.
Specific embodiment
The attapulgite clay adsorbent of the stabilization of the present embodiment, it is prepared from by the raw material of following weight portion：Concave convex rod is former
100 parts of soil, 800 parts of sodium chloride solution, 15 parts of nano-calcium carbonate, 800 parts of absolute ethyl alcohol, 8 parts of VTES, first
80 parts of base methyl acrylate, 40 parts of 5- hydroxylevulinic acids, 4 parts of azodiisobutyronitrile, 10 parts of methylpropene sodium sulfonate, acetone
600 parts, 800 parts of methyl alcohol, appropriate phosphoric acid, appropriate deionized water.
The attapulgite clay adsorbent of the stabilization of the present embodiment, it is prepared from by following steps：
（1）Concave convex rod original soil is sieved by 200 mesh sieve, is washed with deionized 5 times, remove the impurity of remaining, then use chlorine
Change sodium solution to wash 3 times, moisture removal is removed in drying；The attapulgite and nano-calcium carbonate that will have been washed are mixed
Thing, after being raised to 250 DEG C from room temperature, by inert gas N2Make vapor and mixture haptoreaction as carrier gas, further rise
High-temperature after keeping 3h, starts cooling to 350 DEG C, and stops adding vapor, after temperature is down to room temperature, takes out, and obtains pre-
The attapulgite for the treatment of；
（2）The attapulgite of pretreatment is added to 1/3 absolute ethyl alcohol and the deionized water equivalent to absolute ethyl alcohol weight portion
In the solution of configuration, ultrasonic disperse 3h is subsequently adding VTES, adds phosphoric acid, adjusts pH=3-4, heats back
Stream 4h, is washed with deionized to neutrality, then with remaining absolute ethanol washing 3 times, and it is standby to be dried under vacuum to constant weight at 40 DEG C
With；
（3）By step（2）Product, methyl methacrylate, 5- hydroxylevulinic acids, 1/3 azodiisobutyronitrile add dress
Have in the reactor of reflux condensate device, be sufficiently stirred for being well mixed reactant；Oil bath heating heats up, and controlling reaction temperature is
90 DEG C, after stirring reaction 5h under the rotating speed of 500r/min, remaining azodiisobutyronitrile and methylpropene sodium sulfonate are added, risen
High-temperature continues agitating heating 10h to 150 DEG C；Room temperature is cooled to, acetone is added, continues to stir 2h, add methyl alcohol, stood
Sedimentation 10h, filtering, 80 DEG C of vacuum drying 12h, the attapulgite clay adsorbent stablized.
It is that 20mg/L contains Cu respectively to concentration with the attapulgite clay adsorbent obtained by the present embodiment2+、Cd2+、Pb2+It is useless
Water carries out adsorption treatment, the speed of agitator for 1g/L, 250r/min and absorption in the granular concave rod earth adsorbing dosage
Time be 2h under conditions of, Cu in waste water2+、Cd2+、Pb2+Clearance be all higher than 90%.
Claims (3)
1. a kind of attapulgite clay adsorbent of stabilization, it is characterised in that it is prepared from by the raw material of following weight portion：Concave convex rod
100 parts of original soil, sodium chloride solution 600-800 parts, nano-calcium carbonate 12-15 parts, absolute ethyl alcohol 600-800 parts, the second of vinyl three
TMOS 6-8 parts, methyl methacrylate 70-80 parts, 30-40 parts of 5- hydroxylevulinic acids, azodiisobutyronitrile 3-4 parts,
Methylpropene sodium sulfonate 8-10 parts, acetone 500-600 parts, methyl alcohol 600-800 parts, appropriate phosphoric acid, appropriate deionized water.
2. the attapulgite clay adsorbent of the stabilization according to claims 1, it is characterised in that its prepared by following steps and
Into：
（1）Concave convex rod original soil is sieved by 200 mesh sieve, is washed with deionized 3-5 times, remove the impurity of remaining, then used
Sodium chloride solution is washed 2-3 times, and moisture removal is removed in drying；The attapulgite and nano-calcium carbonate that will have been washed are mixed
Compound, after being raised to 250 DEG C from room temperature, by inert gas N2Make vapor and mixture haptoreaction as carrier gas, further
High-temperature is risen to 320-350 DEG C, after keeping 2-3h, starts cooling, and stop adding vapor, after temperature is down to room temperature, taken
Go out, the attapulgite for being pre-processed；
（2）The attapulgite of pretreatment is added to 1/3 absolute ethyl alcohol and the deionized water equivalent to absolute ethyl alcohol weight portion
In the solution of configuration, ultrasonic disperse 2-3h is subsequently adding VTES, adds phosphoric acid, adjusts pH=3-4, heating
Backflow 3-4h, is washed with deionized to neutrality, then with remaining absolute ethanol washing 2-3 times, is dried under vacuum at 40 DEG C
Constant weight is standby；
（3）By step（2）Product, methyl methacrylate, 5- hydroxylevulinic acids, 1/3 azodiisobutyronitrile add dress
Have in the reactor of reflux condensate device, be sufficiently stirred for being well mixed reactant；Oil bath heating heats up, and controlling reaction temperature is
80-90 DEG C, after stirring reaction 3-5h under the rotating speed of 300-500r/min, add remaining azodiisobutyronitrile and metering system
Sodium sulfonate, rises high-temperature to 140-150 DEG C, continues agitating heating 8-10h；Room temperature is cooled to, acetone is added, continues to stir 1-
2h, adds methyl alcohol, standing sedimentation 8-10h, filtering, 60-80 DEG C of vacuum drying 10-12h, the attapulgite absorption stablized
Agent.
3. the attapulgite clay adsorbent of the stabilization according to claims 1,2, it is characterised in that described sodium chloride solution
Concentration is 2-3mol/L, and the concentration of described phosphoric acid is 1-2mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611152177.9A CN106693901A (en) | 2016-12-14 | 2016-12-14 | Stable attapulgite adsorbent and preparation method thereof |
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| CN201611152177.9A CN106693901A (en) | 2016-12-14 | 2016-12-14 | Stable attapulgite adsorbent and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107282024A (en) * | 2017-08-31 | 2017-10-24 | 安庆徽云博冠化妆品科技有限公司 | A kind of preparation method of organic adsorption type material for air purification |
| CN108212112A (en) * | 2018-02-07 | 2018-06-29 | 宁波甬凌新材料科技有限公司 | A kind of system chaff modified material for handling heavy metal containing sewage and its preparation method and application |
| CN110129065A (en) * | 2019-04-02 | 2019-08-16 | 淮阴工学院 | A kind of mercapto-functionalized concave convex rod and preparation method thereof |
| CN113913190A (en) * | 2021-10-14 | 2022-01-11 | 上海市农产品质量安全中心 | Preparation method of soil heavy metal passivator based on electrostatic effect |
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| CN102977256A (en) * | 2012-12-05 | 2013-03-20 | 淮阴师范学院 | Acrylic ester-attapulgite composite oil-absorbing material and preparation method thereof |
| CN103012699A (en) * | 2012-12-05 | 2013-04-03 | 常州大学 | Attapulgite grafted polymethyl methacrylate hybrid particle and preparation method thereof |
| CN103894143A (en) * | 2014-03-18 | 2014-07-02 | 苏州宇希新材料科技有限公司 | Method for activating attapulgite |
| CN104275161A (en) * | 2014-11-07 | 2015-01-14 | 中国科学院兰州化学物理研究所 | Granular cationic dye adsorbent and preparation method thereof |
| CN106000356A (en) * | 2016-06-16 | 2016-10-12 | 江苏麦阁吸附剂有限公司 | Attapulgite/polyacrylic acid compound heavy metal absorbent and preparation method thereof |
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2016
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Patent Citations (5)
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| CN102977256A (en) * | 2012-12-05 | 2013-03-20 | 淮阴师范学院 | Acrylic ester-attapulgite composite oil-absorbing material and preparation method thereof |
| CN103012699A (en) * | 2012-12-05 | 2013-04-03 | 常州大学 | Attapulgite grafted polymethyl methacrylate hybrid particle and preparation method thereof |
| CN103894143A (en) * | 2014-03-18 | 2014-07-02 | 苏州宇希新材料科技有限公司 | Method for activating attapulgite |
| CN104275161A (en) * | 2014-11-07 | 2015-01-14 | 中国科学院兰州化学物理研究所 | Granular cationic dye adsorbent and preparation method thereof |
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Cited By (4)
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| CN107282024A (en) * | 2017-08-31 | 2017-10-24 | 安庆徽云博冠化妆品科技有限公司 | A kind of preparation method of organic adsorption type material for air purification |
| CN108212112A (en) * | 2018-02-07 | 2018-06-29 | 宁波甬凌新材料科技有限公司 | A kind of system chaff modified material for handling heavy metal containing sewage and its preparation method and application |
| CN110129065A (en) * | 2019-04-02 | 2019-08-16 | 淮阴工学院 | A kind of mercapto-functionalized concave convex rod and preparation method thereof |
| CN113913190A (en) * | 2021-10-14 | 2022-01-11 | 上海市农产品质量安全中心 | Preparation method of soil heavy metal passivator based on electrostatic effect |
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Application publication date: 20170524 |