CN106732455A - Modified attapulgite clay adsorbent of a kind of ceramic fibre and preparation method thereof - Google Patents

Modified attapulgite clay adsorbent of a kind of ceramic fibre and preparation method thereof Download PDF

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Publication number
CN106732455A
CN106732455A CN201611151937.4A CN201611151937A CN106732455A CN 106732455 A CN106732455 A CN 106732455A CN 201611151937 A CN201611151937 A CN 201611151937A CN 106732455 A CN106732455 A CN 106732455A
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parts
ceramic fibre
attapulgite clay
clay adsorbent
attapulgite
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CN201611151937.4A
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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
    • B01J20/02—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
    • 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
    • B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
    • B01J20/0251—Compounds of Si, Ge, Sn, Pb
    • 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
    • B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
    • B01J20/26—Synthetic macromolecular compounds
    • B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
    • 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
    • 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

Abstract

The modified attapulgite clay adsorbent of a kind of ceramic fibre, 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, 600 800 parts of sodium chloride solution, 12 15 parts of nano silicon, 15 20 parts of ceramic fibre, 8 10 parts of polyvinylpyrrolidone, 56 parts of lauric acid diethyl amide, 68 parts of glycerol stearate monoesters, 70 80 parts of methyl methacrylate, 30 40 parts of N N-isopropylacrylamides, 34 parts of peroxide acetic acid butyl ester, 8 10 parts of lauryl mercaptan, 500 600 parts of acetone, 600 800 parts of methyl alcohol, appropriate deionized water.Present invention process is simple and does not produce secondary pollution, and prepared attapulgite clay adsorbent has big particle diameter, free settling, easily reclaim and the characteristics of absorption property is good, it is adaptable to Industrial Wastewater Treatment.

Description

Modified attapulgite clay adsorbent of a kind of ceramic fibre and preparation method thereof
Technical field
The invention belongs to technical field of absorbent, and in particular to a kind of modified attapulgite clay adsorbent of ceramic fibre and its 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 modified attapulgite clay adsorbent of a kind of ceramic fibre of offer and preparation method thereof.
To achieve these goals, the technical solution adopted by the present invention is as follows：
The modified attapulgite clay adsorbent of a kind of ceramic fibre, 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, nano silicon 12-15 parts, ceramic fibre 15-20 parts, poly- second Alkene pyrrolidone 8-10 parts, lauric acid diethyl amide 5-6 parts, 6-8 parts of glycerol stearate monoesters, methyl methacrylate 70- 80 parts, NIPA 30-40 parts, peroxide acetic acid butyl ester 3-4 parts, lauryl mercaptan 8-10 parts, acetone 500-600 parts, methyl alcohol 600-800 parts, appropriate deionized water.
The modified attapulgite clay adsorbent of described ceramic fibre, 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；The attapulgite that will have been washed is added to going equivalent to 50-60 times of concave convex rod original soil weight portion In ionized water, nano silicon is added, mechanical agitation is prepared into suspension, and natural subsidence 3-4d, drying is removed moisture removal, obtained To the attapulgite of pretreatment；
（2）The attapulgite of pretreatment, ceramic fibre and polyvinylpyrrolidone are mixed and heated to 300-350 DEG C, insulation 1.5-2h, adds it to lauric acid diethyl amide, glycerol stearate monoesters and equivalent to concave convex rod original soil after natural cooling In the solution of the deionized water configuration of 8-10 times of weight portion, ultrasonic disperse 2-3h, it is standby at 40 DEG C to be dried under vacuum to constant weight；
（3）By step（2）Product, methyl methacrylate, NIPA, 1/3 peroxide acetic acid butyl ester 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 remaining peroxide acetic acid butyl ester And lauryl mercaptan, high-temperature is risen to 140-150 DEG C, continue agitating heating 8-10h；Room temperature is cooled to, acetone is added, continued Stirring 1-2h, adds methyl alcohol, and standing sedimentation 8-10h, filtering, 60-80 DEG C of vacuum drying 10-12h obtains ceramic fibre and be modified Attapulgite clay adsorbent.
The modified attapulgite clay adsorbent of described ceramic fibre, it is characterised in that described concentration of sodium chloride solution is 2-3mol/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 first, recycles ultrasonic wave The cavitation for causing, the shock wave for being formed in the solution and microjet can cause strong between attapulgite aggregation Mutually collision, the aggregation of the rod crystalline substance beam of attapulgite or brilliant beam is smashed, and nano-attapulgite suspension is prepared so as to reach, Increase the cation exchange capacity of attapulgite, suppress the phenomenon that attapulgite itself is reunited；Recycle laurate diethanol acyl Amine and glycerol stearate monoesters are modified to its surface, and polymethyl methacrylate cladding is prepared using the method for in-situ polymerization Attapulgite clay adsorbent, by the toughness of the rigidity of attapulgite, dimensional stability and heat endurance and polymethyl methacrylate, Machinability and dielectricity ideally combine, and not only adsorb the heavy metal cation in trade effluent, moreover it is possible to adsorb organic Thing pollutes；Lauric acid diethyl amide and glycerol stearate monoesters are added and increased polymethyl methacrylate and attapulgite Compatibility；The present invention also added ceramic fibre and nano silicon, also add resistance to elevated temperatures and the absorption of adsorbent Capacity.Present invention process is simple and does not produce secondary pollution, prepared attapulgite clay adsorbent have big particle diameter, free settling, The characteristics of easily reclaiming good with absorption property, it is adaptable to Industrial Wastewater Treatment.
Specific embodiment
The modified attapulgite clay adsorbent of the ceramic fibre of the present embodiment, it is prepared from by the raw material of following weight portion： 100 parts of concave convex rod original soil, 800 parts of sodium chloride solution, 15 parts of nano silicon, 20 parts of ceramic fibre, polyvinylpyrrolidone 10 parts, 6 parts of lauric acid diethyl amide, 8 parts of glycerol stearate monoesters, 80 parts of methyl methacrylate, N- isopropyl acrylamides 40 parts of amine, 4 parts of peroxide acetic acid butyl ester, 10 parts of lauryl mercaptan, 600 parts of acetone, 800 parts of methyl alcohol, appropriate deionized water.
The modified attapulgite clay adsorbent of the ceramic fibre 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；The attapulgite that will have been washed is added to the deionized water equivalent to 60 times of concave convex rod original soil weight portion In, nano silicon is added, mechanical agitation is prepared into suspension, and natural subsidence 4d, drying is removed moisture removal, pre-processed Attapulgite；
（2）The attapulgite of pretreatment, ceramic fibre and polyvinylpyrrolidone are mixed and heated to 350 DEG C, 2h is incubated, it is natural Lauric acid diethyl amide, glycerol stearate monoesters are added it to after cooling and equivalent to 10 times of concave convex rod original soil weight portion In the solution of deionized water configuration, ultrasonic disperse 3h, it is standby at 40 DEG C to be dried under vacuum to constant weight；
（3）By step（2）Product, methyl methacrylate, NIPA, 1/3 peroxide acetic acid butyl ester 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 peroxide acetic acid butyl ester and dodecane Base mercaptan, rises high-temperature to 150 DEG C, continues agitating heating 10h；Room temperature is cooled to, acetone is added, continues to stir 2h, added Methyl alcohol, standing sedimentation 10h, filtering, 80 DEG C of vacuum drying 12h obtain the modified attapulgite clay adsorbent of ceramic fibre.
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. the attapulgite clay adsorbent that a kind of ceramic fibre is modified, it is characterised in that it is by the raw material preparation of following weight portion Into：100 parts of concave convex rod original soil, sodium chloride solution 600-800 parts, nano silicon 12-15 parts, ceramic fibre 15-20 parts, it is poly- Vinylpyrrolidone 8-10 parts, lauric acid diethyl amide 5-6 parts, 6-8 parts of glycerol stearate monoesters, methyl methacrylate 70-80 parts, NIPA 30-40 parts, peroxide acetic acid butyl ester 3-4 parts, lauryl mercaptan 8-10 parts, acetone 500-600 parts, methyl alcohol 600-800 parts, appropriate deionized water.
2. the modified attapulgite clay adsorbent of ceramic fibre according to claims 1, it is characterised in that it by walking as follows Suddenly 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；The attapulgite that will have been washed is added to going equivalent to 50-60 times of concave convex rod original soil weight portion In ionized water, nano silicon is added, mechanical agitation is prepared into suspension, and natural subsidence 3-4d, drying is removed moisture removal, obtained To the attapulgite of pretreatment；
（2）The attapulgite of pretreatment, ceramic fibre and polyvinylpyrrolidone are mixed and heated to 300-350 DEG C, insulation 1.5-2h, adds it to lauric acid diethyl amide, glycerol stearate monoesters and equivalent to concave convex rod original soil after natural cooling In the solution of the deionized water configuration of 8-10 times of weight portion, ultrasonic disperse 2-3h, it is standby at 40 DEG C to be dried under vacuum to constant weight；
（3）By step（2）Product, methyl methacrylate, NIPA, 1/3 peroxide acetic acid butyl ester 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 remaining peroxide acetic acid butyl ester And lauryl mercaptan, high-temperature is risen to 140-150 DEG C, continue agitating heating 8-10h；Room temperature is cooled to, acetone is added, continued Stirring 1-2h, adds methyl alcohol, and standing sedimentation 8-10h, filtering, 60-80 DEG C of vacuum drying 10-12h obtains ceramic fibre and be modified Attapulgite clay adsorbent.
3. the modified attapulgite clay adsorbent of ceramic fibre according to claims 1,2, it is characterised in that described chlorine It is 2-3mol/L to change sodium solution concentration.
CN201611151937.4A 2016-12-14 2016-12-14 Modified attapulgite clay adsorbent of a kind of ceramic fibre and preparation method thereof Withdrawn CN106732455A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107500464A (en) * 2017-09-27 2017-12-22 唐山三友集团兴达化纤有限公司 A kind of method for handling viscose rayon factory acid waste water
CN110395462A (en) * 2019-07-23 2019-11-01 董明宇 A kind of liquid crystal display plastic sucking disc and its processing technology

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
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
CN104587954A (en) * 2014-12-25 2015-05-06 东莞市粤威环保科技有限公司 Preparation method of activated adsorbent and application of prepared activated adsorbent
CN105642257A (en) * 2016-03-13 2016-06-08 宿州学院 Adsorptive magnetic nano material 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

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
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
CN104587954A (en) * 2014-12-25 2015-05-06 东莞市粤威环保科技有限公司 Preparation method of activated adsorbent and application of prepared activated adsorbent
CN105642257A (en) * 2016-03-13 2016-06-08 宿州学院 Adsorptive magnetic nano material 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

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107500464A (en) * 2017-09-27 2017-12-22 唐山三友集团兴达化纤有限公司 A kind of method for handling viscose rayon factory acid waste water
CN110395462A (en) * 2019-07-23 2019-11-01 董明宇 A kind of liquid crystal display plastic sucking disc and its processing technology

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Application publication date: 20170531