CN1817916A - Composite materials with high water absorbing and retaining performances containing diatomite and production thereof - Google Patents
Composite materials with high water absorbing and retaining performances containing diatomite and production thereof Download PDFInfo
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- CN1817916A CN1817916A CN 200610018617 CN200610018617A CN1817916A CN 1817916 A CN1817916 A CN 1817916A CN 200610018617 CN200610018617 CN 200610018617 CN 200610018617 A CN200610018617 A CN 200610018617A CN 1817916 A CN1817916 A CN 1817916A
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Abstract
A high-water-absorption and retaining composite material containing diatomite and its production are disclosed. It consists of diatomite, soluble ethylene unsaturated monomer, soluble radical polymerization initiator and cross-linking agent. Soluble radical polymerization initiator: soluble ethylene unsaturated monomer=(0.001~1:100)wt%, cross-linking agent: soluble ethylene unsaturated monomer=(0~5:100)wt%, diatomite: soluble ethylene unsaturated monomer=(2~300:100)wt%. The main mineral ingredient of diatomite is opal, diatomite content is >50%, and average diameter is <=45um. It is cheap, higher absorptivity of solution containing calcium ion and magnesium-aluminum ion and better anti-salt performance.
Description
Technical field
The present invention relates to a kind of composite materials with high water absorbing and retaining performances and preparation method thereof, particularly be applied to composite materials with high water absorbing and retaining performances of agroforestry and preparation method thereof.
Technical background
In recent years, the high water absorbing and retaining agent is widely used in various fields such as agricultural gardening, physiological hygiene articles for use, medicine, oil, chemical industry, environmental protection, building materials and food because of its good suction and water retention property.In known high water absorbing and retaining agent, the kind of existing following several series: vinyl water-soluble monomer homopolymer, multipolymer, starch-grafted vinyl water-soluble mono series, cellulose graft water-soluble vinyl monomer series, cross-linked carboxymethyl cellulose etc.Compound, super absorbent resin and organic compound that super absorbent resin and inorganics gel are arranged in compound series.More than in each series of products, the material cost that has is higher, the salt tolerance that has is bad, the complex process that has, equipment requirements height.And be used for the water-absorbing-retaining material of agroforestry purpose, especially because material cost is higher, gel-strength is low and salt resistance is poor, and its application is restricted.
The present both at home and abroad document about the composite materials with high water absorbing and retaining performances that contains non-metallic mineral powder of report is mostly by hydrophilic layer silicate mineral and polymkeric substance is compound obtains.CN1041601 and CN1621422 are main raw material with wilkinite and acrylamide all, adopt redox initiation system or superoxide initiator system, have synthesized the lower and controlled high-absorbent material of suction multiple of manufacturing cost in the aqueous solution.CN1631970 has done some on this basis and has improved, and it adopts starch and acrylamide and attapulgite in the presence of initiator, makes the water-retaining agent that has strong water-retaining capacity and the favorable biological degradability energy is arranged through graft copolymerization.But product aftertreatment trouble, and exist certain toxicity.CN1542046, CN1542045, CN1542049, CN1542047 and CN1542048 adopt water solution polymerization process, in containing the water-soluble vinyl unsaturated monomer solution of initiator and linking agent, add rectorite leng, illite, sericite, calcined kaolin respectively and contain the attaclay mineral, prepare that to have a raw materials cost low, the water absorbent rate height, salt resistance is better, is applicable to the composite materials with high water absorbing and retaining performances that contains non-metallic mineral powder of agroforestry.The non-metallic minerals that is added in the above matrix material is mainly laminar silicic acid salt mineral, and yet there are no open report about the document and the patent of composite materials with high water absorbing and retaining performances of containing amorphous diatomite ore powder and preparation method thereof.
Summary of the invention
The object of the present invention is to provide that a kind of cost is low, liquid absorbency rate is high, salt resistance contains diatomaceous composite materials with high water absorbing and retaining performances and preparation method thereof preferably.
To achieve these goals, technical scheme of the present invention is: contain diatomaceous composite materials with high water absorbing and retaining performances, it is characterized in that: it comprises diatomite, water-soluble vinyl unsaturated monomer, water-soluble radical polymerization initiator and linking agent, diatomaceous interpolation weight is 2%～300% of the unsaturated water-soluble monomer of vinyl, the interpolation weight of water-soluble radical polymerization initiator is 0.001%～1% of water-soluble vinyl unsaturated monomer, and the interpolation weight of linking agent is 0～5% of water-soluble vinyl unsaturated monomer; Described diatomaceous essential mineral composition is opal (SiO
2NH
2O), diatomite content is greater than 50%, the median size≤45um of diatomite powder.
The interpolation weight of described linking agent is 0.05～1% of water-soluble vinyl unsaturated monomer.
The preparation method who contains diatomaceous composite materials with high water absorbing and retaining performances is characterized in that its bag following steps: 1). diatomaceous deep processing: diatomaceous essential mineral composition is opal (SiO
2NH
2O), diatomite content is crushed to median size≤45um greater than 50% with diatomite original soil; 2). diatomite is joined in the water soluble ethylene monomer solution of 5～50% concentration that are dissolved with water-soluble radical polymerization initiator or water-soluble radical polymerization initiator and linking agent blending dispersion; Diatomaceous interpolation weight is 2%～300% of the unsaturated water-soluble monomer of vinyl, the interpolation weight of water-soluble radical polymerization initiator is 0.001%～1% of water-soluble vinyl unsaturated monomer, and the interpolation weight of linking agent is 0～5% of water-soluble vinyl unsaturated monomer; 3). after 20～90 ℃ (preferred 40～70 ℃) heated 1～10 hour (preferred 3～7 hours), 10～30 ℃ of reactions of elevated temperature were 1～3 hour again, get polymerisate in reactor for polyreaction, the mixture after the dispersion; 4). polymerisate is in vacuum or be not dried to water content less than 10% in 40～150 ℃ under vacuum condition, makes it be crushed to 0.1～5.0mm with the method for machinery, finally obtains granulated product.
Described blending dispersion is: the employing homogenizer carries out dispersed with stirring or disperses with colloidal mill, or adopt ultrasonic wave to carry out ultra-sonic dispersion, if adopt ultrasonic dispersion, the power of ultrasonic generator is 20～4000W, and frequency of ultrasonic is 10 kilo hertzs～300 megahertzes.
Introduce the present invention below in detail.
1. diatomite
Diatomite is a kind of rock with biological structure, mainly by 80～90%, by the diatom test that reaches more than 90% form, its essential mineral composition forms opal (SiO for the aqueous silicon dioxide gel after taking off portion water
2NH
2And contain clay (the female class of kaolinite class, moisture and a small amount of montmorillonite class), carbonaceous (organic matter), irony (limonite, rhombohedral iron ore, pyrite), carbonate minerals (calcite, rhombspar, a small amount of spathic iron ore), quartz, white mica, glaukonine, feldspar O).Have numerous small holes on the diatom shell, its porosity reaches 90～92%, and light weight, porous, specific surface area is big, bulk density is high, nontoxic, neutral, good chemical stability, and with acid-base reaction, adsorptivity is not strong.The diatomite surface is covered by a large amount of silicon hydroxyls, and there is hydrogen bond to exist, hydroxyl also distributes at diatomite pore internal surface, thereby make the diatomite surface have activity, can form reticulated structure with the organic resin reaction, by the level difference analysis of orthogonal experiment, determined that the mineral content in the matrix material has considerable influence to the liquid absorbency rate that contains ionized water; This is because the ultramicropore structure of diatomaceous uniqueness has extremely strong adsorption function, can adsorb a certain amount of calcium ions and magnesium ions in the water.So, contain diatomaceous high water absorbing and retaining agent and have certain anti-ionomer and certain salt resistance.
Diatomite content is greater than 50%, and the median size≤45um of mineral powder, diatomaceous addition are 2～300% of water-soluble vinyl unsaturated monomer weight, preferred 10～150% (weight).Any diatomite that meets above mineralogical characteristic all can be used for the present invention.
2. water-soluble vinyl unsaturated monomer
Typical water-soluble ionic-type vinyl unsaturated monomer is: ionic comonomer: acrylic or methacrylic acid and alkali metal salts or ammonium salt thereof.Typical nonionic monomers is: acrylamide and derivative thereof.Wherein preferably vinylformic acid and sodium salt thereof or ammonium salt and acrylamide.These water-soluble vinyl unsaturated monomers can use separately, also can mix use, 1), be any proportioning between each concrete monomer of ionic comonomer during any mixing more than two kinds:, 2), be any proportioning between each concrete monomer of nonionic monomers; 3), when ionic comonomer and nonionic monomers are mixed, ionic comonomer: nonionic monomers=99: 1 or 1: 99 (mol ratio).
The weight concentration of water-soluble vinyl unsaturated monomer in aqueous solution is 5% to saturation concentration, preferred 20～50% (weight).Vinylformic acid can be partly or wholly to use with basic metal or ammonium compound neutral form.Degree of neutralization is 20～100% (molar percentages).
If when water-soluble vinyl unsaturated monomer methacrylic acid or acrylamide and derivative thereof, its degree of neutralization is 20～100%.
3. water-soluble radical polymerization initiator
Being fit to this type of polymeric water-soluble radical polymerization initiator is persulphate, as: Potassium Persulphate, Sodium Persulfate, ammonium persulphate, these water soluble starters can mix use, mix when using, and are any proportioning.Persulphate also can fit in redox system with reducing substances such as ferrous ion, sodium bisulfite, S-WAT etc. and use.Each proportioning components is determined by the quantitative relation of chemical equation when being used.
The consumption of water-soluble radical polymerization initiator is 0.001～1.0% of a water-soluble vinyl unsaturated monomer weight, preferred 0.1～0.3% (weight).
4. linking agent
In the present invention, if this stands so-called self-crosslinking monomer under the situation of no any linking agent, linking agent can save, certainly, this depends on monomer condition (for example monomer type, monomer concentration and the monomer in the aqueous solution gets degree of neutralization), yet, need to use linking agent to satisfy the requirement on the performance in some cases.
The linking agent per molecule that uses among the present invention contains two polymerisable unsaturated groups at least.Typical linking agent has: two of many alcohol-or three-(methyl) acrylate, said many alcohol are ethylene glycol, propylene glycol, glycerol polyoxyethylene glycol, polyoxy propylene glycol, polyglycerol for example; Typical linking agent also has: how pure unsaturated acid or acid anhydrides (for example toxilic acid, fumaric acid, maleic anhydride), the unsaturated polyester that fumaric acid or maleic anhydride and many alcohol reactions obtain; Bisacrylamide (as N, N '-methylene-bisacrylamide), two-or three-(methyl) acrylate that obtain by polyoxy compounds and methacrylic acid-respons; (methyl) acrylic-amino formyl fat that obtains by polymeric polyisocyanate (for example two isocyanic acid benzene methylene esters and two isocyanic acids inferior own ester) and hydroxyethyl (methyl) acrylate reactions; Polynary allylic cpd (for example allylation starch, allylation Mierocrystalline cellulose, O-phthalic allyl propionate etc.).In these linking agents, N preferably, N '-methylene-bisacrylamide, EGMa.
The consumption of linking agent is 0～5% of a water-soluble vinyl unsaturated monomer weight, preferred 0.05～1% (weight)
In the present invention, adopt following method to measure and calculate the liquid absorbency rate of inhaling distilled water, tap water and physiological saline:
The granulated product that takes by weighing after 0.5～1.0g drying and the pulverization process places the 500-1000ml beaker, granulated product after adding 450～900ml distilled water or tap water or taking by weighing 0.5～1.0g drying and pulverization process places the 150ml beaker to add 100ml 0.9%NaCl solution, after leaving standstill 24 hours, with 30 order mesh screens with unnecessary water elimination, weigh up gel quality affects, be calculated as follows water absorbent rate:
Liquid absorbency rate=(gel quality affects-xerogel quality)/xerogel quality.
The present invention is by adopting cheap diatomite and water-soluble vinyl unsaturated monomer elder generation blending dispersion repolymerization compound operational path, obtain thus that material cost is low, preparation technology is simple, inhale contain calcium ions and magnesium ions aqueous solution multiplying power height, gel-strength is higher (can improve polymer network structure after adding mineral, thereby improve gel-strength), salt resistant character is better, is applicable to containing of agroforestry of diatomaceous composite materials with high water absorbing and retaining performances.
The present invention makes contains diatomaceous composite materials with high water absorbing and retaining performances, and material cost descends 20～50% than sodium polyacrylate.The scope that experiment records the liquid absorbency rate of this serial high water absorbing and retaining agent is: the multiplying power of inhaling distilled water is 480～1600g/g, and the multiplying power of inhaling tap water is 110～390g/g, and the multiplying power of inhaling physiological saline is 50～85g/g.
Embodiment
In order to understand the present invention better, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention not only is confined to the following examples.
Embodiment 1:
In concentration is that 15% degree of neutralization is in 100% acrylic acid solution, 300 grams, stir and add N down, N '-methylene-bisacrylamide 0.0022 gram, Potassium Persulphate 0.0225 gram, dissolving, the diatomite that mechanical disintegration is crossed (content is greater than 50%) 10 grams add wherein ultra-sonic dispersion 10 minutes again.In 50 ℃ of heating after 7 hours, the reaction of 30 ℃ of elevated temperatures is 1 hour again in reactor for mixture, and the gel of generation makes its pulverizing obtain the finished product with mechanical method in following 50 ℃ of dryings of vacuum condition 5 hours then.
Embodiment 2:
In concentration is that 30% degree of neutralization is in 80% acrylic acid solution, 300 grams, stir and add N down, N '-methylene-bisacrylamide 0.022 gram, Potassium Persulphate 0.425 gram, dissolving, the diatomite that mechanical disintegration is crossed (content is greater than 90%) 50 grams add wherein ultra-sonic dispersion 20 minutes again.In 70 ℃ of heating after 3 hours, the reaction of 10 ℃ of elevated temperatures is 2 hours again in reactor for mixture, and the gel of generation makes its pulverizing obtain the finished product with mechanical method in 110 ℃ of dryings 5 hours then.
Embodiment 3:
In concentration is that 45% degree of neutralization is in 20% acrylic acid solution, 200 grams, stir and add N down, N '-methylene-bisacrylamide 0.005 gram, Potassium Persulphate 0.050 gram, dissolving, the diatomite that mechanical disintegration is crossed (content is greater than 60%) 30 grams add wherein again, and colloidal mill disperses.In 60 ℃ of heating after 4 hours, the reaction of 20 ℃ of elevated temperatures is 3 hours again in reactor for mixture, and the gel of generation makes its pulverizing obtain the finished product with mechanical method in 150 ℃ of dryings 1 hour then.
Embodiment 4:
In concentration is that 15% degree of neutralization is in 50% acrylic acid solution, 300 grams, stir and add N down, N '-methylene-bisacrylamide 0.0026 gram, Potassium Persulphate 0.0255 gram, dissolving, the diatomite that mechanical disintegration is crossed (content is greater than 50%) 40 grams add wherein again, and high-speed stirring was disperseed 30 minutes.In 65 ℃ of heating after 3 hours, the reaction of 25 ℃ of elevated temperatures is 1 hour again in reactor for mixture, and the gel of generation makes its pulverizing obtain the finished product with mechanical method in 90 ℃ of dryings 7 hours then.
Embodiment 5:
With concentration is that 30% degree of neutralization is in 100% acrylic acid solution, 280 grams, stir and add acrylamide 20 grams down, N, N '-methylene-bisacrylamide 0.022 gram, ammonium persulphate 0.425 gram, dissolving, the diatomite that mechanical disintegration is crossed (content is greater than 90%) 50 grams add wherein ultra-sonic dispersion 20 minutes again.In 70 ℃ of heating after 3 hours, the reaction of 10 ℃ of elevated temperatures is 2 hours again in reactor for mixture, and the gel of generation makes its pulverizing obtain the finished product with mechanical method in 90 ℃ of dryings 7 hours then.
Embodiment 6:
With concentration is that 30% degree of neutralization is in 40% acrylic acid solution, 280 grams, stir and add acrylamide 40 grams down, N, N '-methylene-bisacrylamide 0.05 gram, ammonium persulphate 0.225 gram, sodium bisulfite 0.200 gram, dissolving, the diatomite that mechanical disintegration is crossed (content is greater than 60%) 50 grams add wherein ultra-sonic dispersion 20 minutes again.In 60 ℃ of heating after 3 hours, the reaction of 20 ℃ of elevated temperatures is 2 hours again in reactor for mixture, and the gel of generation makes its pulverizing obtain the finished product with mechanical method in 140 ℃ of dryings 2 hours then.
Embodiment 7:
In concentration is that 15% degree of neutralization is in 100% acrylic acid solution, 300 grams, stir to add Sodium Persulfate 0.0238 gram down, and dissolving, the diatomite that mechanical disintegration is crossed (content is greater than 70%) 10 grams add wherein ultra-sonic dispersion 10 minutes again.In 50 ℃ of heating after 7 hours, the reaction of 30 ℃ of elevated temperatures is 1 hour again in reactor for mixture, and the gel of generation makes its pulverizing obtain the finished product with mechanical method in 100 ℃ of dryings 4 hours then.
Embodiment 8:
In concentration is in 15% acrylamide soln, 300 grams, stir and add N down, N '-methylene-bisacrylamide 0.0050 gram, Sodium Persulfate 0.0115 and ammonium persulphate 0.0110 gram, dissolving, the diatomite that mechanical disintegration is crossed (content is greater than 50%) 10 grams add wherein ultra-sonic dispersion 10 minutes again.In 50 ℃ of heating after 7 hours, the reaction of 30 ℃ of elevated temperatures is 1 hour again in reactor for mixture, and the gel of generation makes its pulverizing obtain the finished product with mechanical method in following 50 ℃ of dryings of vacuum condition 5 hours then.
Embodiment 9:
In concentration is that 25% degree of neutralization is to add acrylamide 20 grams in 90% acrylic acid solution, 200 grams, dissolving, stir and add N down, N '-methylene-bisacrylamide 0.0031 gram, Sodium Persulfate 0.0115 and ammonium persulphate 0.0110 gram, dissolving, the diatomite that mechanical disintegration is crossed (content is greater than 50%) 10 grams add wherein ultra-sonic dispersion 10 minutes again.In 40 ℃ of heating after 7 hours, the reaction of 30 ℃ of elevated temperatures is 1 hour again in reactor for mixture, and the gel of generation makes its pulverizing obtain the finished product with mechanical method in 150 ℃ of dryings 1 hour then.
Embodiment 10:
In concentration is that 5% degree of neutralization is to add acrylamide 40 grams in 90% acrylic acid solution, 200 grams, dissolving, stir and add N down, N '-methylene-bisacrylamide 0.0027, Sodium Persulfate 0.0115 and ammonium persulphate 0.0110 gram, dissolving, the diatomite that mechanical disintegration is crossed (content is greater than 80%) 40 grams add wherein again, and high-speed stirring was disperseed 30 minutes.In 50 ℃ of heating after 5 hours, the reaction of 30 ℃ of elevated temperatures is 1 hour again in reactor for mixture, and the gel of generation makes its pulverizing obtain the finished product with mechanical method in 105 ℃ of dryings 4 hours then.
Embodiment 11:
In concentration is that 40% degree of neutralization is to add acrylamide 40 grams in 90% methacrylic acid solution, 200 grams, dissolving, stir and add N down, N '-methylene-bisacrylamide 0.0024 gram, Sodium Persulfate 0.0115 and ammonium persulphate 0.0110 gram, dissolving, the diatomite that mechanical disintegration is crossed (content is greater than 90%) 10 grams add wherein again, and colloidal mill disperses.In 70 ℃ of heating after 1 hour, the reaction of 10 ℃ of elevated temperatures is 1 hour again in reactor for mixture, and the gel of generation makes its pulverizing obtain the finished product with mechanical method in 140 ℃ of dryings 1 hour then.
Embodiment 12:
In concentration is that 40% degree of neutralization is to add acrylamide 40 grams in 90% methacrylic acid solution, 200 grams, dissolving, stir and add N down, N '-methylene-bisacrylamide 0.0030 gram, Sodium Persulfate 0.0110 and ammonium persulphate 0.0115 gram, dissolving, the diatomite that mechanical disintegration is crossed (content is greater than 50%) 2.4 grams add wherein again, and high-speed stirring was disperseed 10 minutes.In 70 ℃ of heating after 1 hour, the reaction of 10 ℃ of elevated temperatures is 1 hour again in reactor for mixture, and the gel of generation makes its pulverizing obtain the finished product with mechanical method in 140 ℃ of dryings 1 hour then.
Embodiment 13:
In concentration is that 10% degree of neutralization is to add acrylamide 40 grams in 90% acrylic acid solution, 400 grams, dissolving, stir and add N down, N '-methylene-bisacrylamide 0.0028 gram, Sodium Persulfate 0.0120 and ammonium persulphate 0.0114 gram, dissolving, the diatomite that mechanical disintegration is crossed (content is greater than 50%) 240 grams add wherein again, and colloidal mill disperses.In 70 ℃ of heating after 1 hour, the reaction of 10 ℃ of elevated temperatures is 1 hour again in reactor for mixture, and the gel of generation makes its pulverizing obtain the finished product with mechanical method in 140 ℃ of dryings 1 hour then.
Claims (4)
1. contain diatomaceous composite materials with high water absorbing and retaining performances, it is characterized in that: it comprises diatomite, water-soluble vinyl unsaturated monomer, water-soluble radical polymerization initiator and linking agent, diatomaceous interpolation weight is 2%～300% of the unsaturated water-soluble monomer of vinyl, the interpolation weight of water-soluble radical polymerization initiator is 0.001%～1% of water-soluble vinyl unsaturated monomer, and the interpolation weight of linking agent is 0～5% of water-soluble vinyl unsaturated monomer; Described diatomaceous essential mineral composition is an opal, and diatomite content is greater than 50%, the median size≤45um of diatomite powder.
2. according to claim 1ly contain diatomaceous composite materials with high water absorbing and retaining performances, it is characterized in that: the interpolation weight of described linking agent is 0.05～1% of water-soluble vinyl unsaturated monomer.
3. the preparation method who contains diatomaceous composite materials with high water absorbing and retaining performances as claimed in claim 1, it is characterized in that its bag following steps: 1). diatomaceous deep processing: diatomaceous essential mineral composition is an opal, diatomite content is crushed to median size≤45um greater than 50% with diatomite original soil; 2). diatomite is joined in the water soluble ethylene monomer solution of 5～50% concentration that are dissolved with water-soluble radical polymerization initiator or water-soluble radical polymerization initiator and linking agent blending dispersion; Diatomaceous interpolation weight is 2%～300% of the unsaturated water-soluble monomer of vinyl, the interpolation weight of water-soluble radical polymerization initiator is 0.001%～1% of water-soluble vinyl unsaturated monomer, and the interpolation weight of linking agent is 0～5% of water-soluble vinyl unsaturated monomer; 3). in 20～90 ℃ of heating after 1～10 hour, the reaction of 10～30 ℃ of elevated temperatures is 1～3 hour again in reactor for polyreaction, the mixture after the dispersion, polymerisate; 4). polymerisate is dried to water content less than 10% in 40～150 ℃, makes it be crushed to 0.1～5.0mm with the method for machinery, granulated product.
4. the preparation method who contains diatomaceous composite materials with high water absorbing and retaining performances as claimed in claim 3, it is characterized in that: described blending dispersion is: the employing homogenizer carries out dispersed with stirring or disperses with colloidal mill, or adopt ultrasonic wave to carry out ultra-sonic dispersion, if adopt ultrasonic dispersion, the power of ultrasonic generator is 20～4000W, and frequency of ultrasonic is 10 kilo hertzs～300 megahertzes.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102585420A (en) * | 2012-02-27 | 2012-07-18 | 中国地质大学（武汉） | Magnetic expansion adsorption composite material and preparation method thereof |
| CN102653637A (en) * | 2011-03-02 | 2012-09-05 | 中国矿业大学(北京) | Method for improving expansion character of bentonite in brine |
| CN105348430A (en) * | 2015-12-11 | 2016-02-24 | 河南省有色金属地质矿产局第三地质大队 | Sanitary dolomite clay composite absorption resin and preparation method thereof |
-
2006
- 2006-03-23 CN CN 200610018617 patent/CN1817916A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102653637A (en) * | 2011-03-02 | 2012-09-05 | 中国矿业大学(北京) | Method for improving expansion character of bentonite in brine |
| CN102653637B (en) * | 2011-03-02 | 2013-11-20 | 中国矿业大学(北京) | Method for improving expansion character of bentonite in brine |
| CN102585420A (en) * | 2012-02-27 | 2012-07-18 | 中国地质大学（武汉） | Magnetic expansion adsorption composite material and preparation method thereof |
| CN102585420B (en) * | 2012-02-27 | 2014-06-25 | 中国地质大学（武汉） | Magnetic expansion adsorption composite material and preparation method thereof |
| CN105348430A (en) * | 2015-12-11 | 2016-02-24 | 河南省有色金属地质矿产局第三地质大队 | Sanitary dolomite clay composite absorption resin and preparation method thereof |
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