CN106693902A - Quaternary ammonium salt modified attapulgite adsorbent and preparation method thereof - Google Patents

Quaternary ammonium salt modified attapulgite adsorbent and preparation method thereof Download PDF

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CN106693902A
CN106693902A CN201611152183.4A CN201611152183A CN106693902A CN 106693902 A CN106693902 A CN 106693902A CN 201611152183 A CN201611152183 A CN 201611152183A CN 106693902 A CN106693902 A CN 106693902A
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parts
ammonium salt
attapulgite
quaternary ammonium
solution
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严帝
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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
    • 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
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • 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
    • 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
    • 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
    • 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 & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Water Treatment By Sorption (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention discloses a quaternary ammonium salt modified attapulgite adsorbent which is characterized by being prepared from the following raw materials in parts by weight: 100 parts of raw attapulgite, 600-800 parts of sodium chloride solution, 12-15 parts of basalt fiber, 600-800 parts of absolute ethyl alcohol, 100-120 parts of ammonium acetate solution, 6-8 parts of octadecyl trimethyl ammonium chloride, 70-80 parts of methyl methacrylate, 30-40 parts of diacetone acrylamide, 3-4 parts of tert-butyl peroxybenzoate, 8-10 parts of mercaptoethanol, 500-600 parts of acetone, 600-800 parts of methanol and appropriate deionized water. In the invention, the technology is simple and avoids secondary pollution; and the prepared attapulgite adsorbent has the characteristics of large particle size, easiness in settling and recycling and good adsorption property and is suitable for industrial wastewater treatment.

Description

A kind of quaternary ammonium salt-modified attapulgite clay adsorbent and preparation method thereof
Technical field
The invention belongs to technical field of absorbent, and in particular to a kind of quaternary ammonium salt-modified attapulgite clay adsorbent and its system Preparation 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 quaternary ammonium salt-modified attapulgite clay adsorbent of offer and preparation method thereof.
To achieve these goals, the technical solution adopted by the present invention is as follows：
A kind of quaternary ammonium salt-modified attapulgite clay adsorbent, it is characterised in that it is prepared from by the raw material of following weight portion：It is recessed 100 parts of convex rod original soil, sodium chloride solution 600-800 parts, basalt fibre 12-15 parts, absolute ethyl alcohol 600-800 parts, ammonium acetate Solution 100-120 parts, OTAC 6-8 parts, methyl methacrylate 70-80 parts, DAAM 30-40 parts, peroxidized t-butyl perbenzoate 3-4 parts, mercaptoethanol 8-10 parts, acetone 500-600 parts, methyl alcohol 600-800 parts, go Ion appropriate amount of water.
Described quaternary ammonium salt-modified attapulgite clay adsorbent, 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 basalt fibre 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 OTAC, adds ammonium acetate solution, stirring Continue ultrasound 1.5-2h after 0.5-1h, be washed with deionized to neutrality, then with remaining absolute ethanol washing 2-3 times, 40 8-10h is vacuum dried at DEG C standby；
（3）By step（2）Product, methyl methacrylate, DAAM, 1/3 peroxidized t-butyl perbenzoate Add in the reactor equipped with reflux condensate device, be sufficiently stirred for being well mixed reactant；Oil bath heating heats up, control reaction Temperature is 80-90 DEG C, after stirring reaction 3-5h under the rotating speed of 300-500r/min, adds the remaining tertiary fourth of perbenzoic acid Ester and mercaptoethanol, rise high-temperature to 140-150 DEG C, continue agitating heating 8-10h；Room temperature is cooled to, acetone is added, continues to stir 1-2h is mixed, methyl alcohol is added, standing sedimentation 8-10h, filtering, 60-80 DEG C of vacuum drying 10-12h obtains quaternary ammonium salt-modified recessed Convex rod earth adsorbing.
Described quaternary ammonium salt-modified attapulgite clay adsorbent, it is characterised in that described concentration of sodium chloride solution is 2- 3mol/L, the concentration of described ammonium acetate solution 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；The quaternary ammonium salt OTAC of belt length chain radicals is recycled to modify its surface grafting, The attapulgite clay adsorbent of polymethyl methacrylate cladding is prepared using the method for in-situ polymerization, by the firm of attapulgite The toughness of property, dimensional stability and heat endurance and polymethyl methacrylate, machinability and dielectricity have ideally been combined Come, not only adsorb the heavy metal cation in trade effluent, moreover it is possible to adsorb Organic Pollution；The present invention uses belt length chain radicals Quaternary ammonium salt grafting and modifying attapulgite, intercalation enter attapulgite in, increased interlamellar spacing, not only strengthen attapulgite with The compatibility of polymethyl methacrylate, also enhances the rate of adsorption and adsorption capacity of adsorbent, and the present invention with the addition of the Black Warrior Rock fiber, also add the intensity of adsorbent, corrosion-resistant and heat-resistant stability.Present invention process is simple and does not produce secondary dirt Dye, prepared attapulgite clay adsorbent has particle diameter big, free settling, easily reclaim and the characteristics of absorption property is good, it is adaptable to Industrial Wastewater Treatment.
Specific embodiment
The quaternary ammonium salt-modified attapulgite clay adsorbent of the present embodiment, it is characterised in that its by following weight portion raw material It is prepared from：100 parts of concave convex rod original soil, 800 parts of sodium chloride solution, 15 parts of basalt fibre, 800 parts of absolute ethyl alcohol, ammonium acetate 120 parts of solution, 8 parts of OTAC, 80 parts of methyl methacrylate, 40 parts of DAAM, peroxide Change 4 parts of t-butyl perbenzoate, 10 parts of mercaptoethanol, 600 parts of acetone, 800 parts of methyl alcohol, appropriate deionized water.
The quaternary ammonium salt-modified attapulgite clay adsorbent 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 basalt fibre 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 OTAC, ammonium acetate solution is added, after stirring 1h Continue ultrasound 2h, be washed with deionized to neutrality, then with remaining absolute ethanol washing 3 times, 10h is vacuum dried at 40 DEG C It is standby；
（3）By step（2）Product, methyl methacrylate, DAAM, 1/3 peroxidized t-butyl perbenzoate Add in the reactor equipped with reflux condensate device, be sufficiently stirred for being well mixed reactant；Oil bath heating heats up, control reaction Temperature is 90 DEG C, after stirring reaction 5h under the rotating speed of 500r/min, adds remaining peroxidized t-butyl perbenzoate and sulfydryl Ethanol, rises high-temperature to 150 DEG C, continues agitating heating 10h；Room temperature is cooled to, acetone is added, continues to stir 2h, add first Alcohol, standing sedimentation 10h, filtering, 80 DEG C of vacuum drying 12h obtain quaternary ammonium salt-modified attapulgite clay adsorbent.
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 quaternary ammonium salt-modified attapulgite clay adsorbent, it is characterised in that it is prepared from by the raw material of following weight portion： 100 parts of concave convex rod original soil, sodium chloride solution 600-800 parts, basalt fibre 12-15 parts, absolute ethyl alcohol 600-800 parts, acetic acid Ammonium salt solution 100-120 parts, OTAC 6-8 parts, methyl methacrylate 70-80 parts, diacetone acrylamide acyl Amine 30-40 parts, peroxidized t-butyl perbenzoate 3-4 parts, mercaptoethanol 8-10 parts, acetone 500-600 parts, methyl alcohol 600-800 parts, Appropriate deionized water.
2. the quaternary ammonium salt-modified attapulgite clay adsorbent according to claims 1, it is characterised in that it is by following steps It is prepared from：
（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 basalt fibre 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 OTAC, adds ammonium acetate solution, stirring Continue ultrasound 1.5-2h after 0.5-1h, be washed with deionized to neutrality, then with remaining absolute ethanol washing 2-3 times, 40 8-10h is vacuum dried at DEG C standby；
（3）By step（2）Product, methyl methacrylate, DAAM, 1/3 peroxidized t-butyl perbenzoate Add in the reactor equipped with reflux condensate device, be sufficiently stirred for being well mixed reactant；Oil bath heating heats up, control reaction Temperature is 80-90 DEG C, after stirring reaction 3-5h under the rotating speed of 300-500r/min, adds the remaining tertiary fourth of perbenzoic acid Ester and mercaptoethanol, rise high-temperature to 140-150 DEG C, continue agitating heating 8-10h；Room temperature is cooled to, acetone is added, continues to stir 1-2h is mixed, methyl alcohol is added, standing sedimentation 8-10h, filtering, 60-80 DEG C of vacuum drying 10-12h obtains quaternary ammonium salt-modified recessed Convex rod earth adsorbing.
3. the quaternary ammonium salt-modified attapulgite clay adsorbent according to claims 1,2, it is characterised in that described chlorination Sodium solution concentration is 2-3mol/L, and the concentration of described ammonium acetate solution is 1-2mol/L.
CN201611152183.4A 2016-12-14 2016-12-14 Quaternary ammonium salt modified attapulgite adsorbent and preparation method thereof Withdrawn CN106693902A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113563983A (en) * 2021-06-16 2021-10-29 江阴润玛电子材料股份有限公司 Cleaning liquid for semiconductor integrated circuit and production process thereof
CN114130372A (en) * 2021-11-30 2022-03-04 北京北环之星智能环保科技有限公司 Basalt fiber modified adsorption filler and preparation method thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN104787776A (en) * 2014-11-30 2015-07-22 赵明 Organic modified calcium-based attapulgite by using long-chained alkyl quaternary ammonium salts
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

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN104787776A (en) * 2014-11-30 2015-07-22 赵明 Organic modified calcium-based attapulgite by using long-chained alkyl quaternary ammonium salts
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

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113563983A (en) * 2021-06-16 2021-10-29 江阴润玛电子材料股份有限公司 Cleaning liquid for semiconductor integrated circuit and production process thereof
CN114130372A (en) * 2021-11-30 2022-03-04 北京北环之星智能环保科技有限公司 Basalt fiber modified adsorption filler and preparation method thereof

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Application publication date: 20170524