CN103755897A - Method for preparing palygorskite clay based salt-tolerance super water absorbency composite material - Google Patents

Method for preparing palygorskite clay based salt-tolerance super water absorbency composite material Download PDF

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CN103755897A
CN103755897A CN201410003027.6A CN201410003027A CN103755897A CN 103755897 A CN103755897 A CN 103755897A CN 201410003027 A CN201410003027 A CN 201410003027A CN 103755897 A CN103755897 A CN 103755897A
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water
composite material
based salt
clay
salt tolerance
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CN103755897B (en
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陆泉芳
安宁
孙勇
俞洁
庞二牛
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Northwest Normal University
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Abstract

The invention provides a method for preparing a palygorskite clay based salt-tolerance super water absorbency composite material, which belongs to the field of composite material preparation. The method comprises the following steps: in a water solution system, stirring palygorskite, 2-acrylamide-2-methyl propanesulfonic acid and acrylic acid as raw materials and N,N'-methylene bisacrylamide as a cross-linking agent at 60-80 DEG C for 2-6 hours to form a gel cross-linking product, cooling down, washing in water, dehydrating, drying and crushing to obtain the palygorskite clay based salt-tolerance super water absorbency composite material. The composite water absorbency material prepared by using the method is good in water absorbency, thermal resistance and salt tolerance, rapid in water absorbency velocity, is applicable to rapid absorbency of rain in a short time in dry and semidry areas, and is a drought-resisting water-retaining composite material with excellent properties. Compared with the prior art, the method is cheap and easy to obtain raw materials, simple in preparation process and green and environment-friendly, and has wide application prospects in such fields as agriculture, forestry, gardening, conservation of water and soil, drought resistance, water conservation and medicine release.

Description

The preparation method of palygorskite base salt tolerance composite material with high water absorption
Technical field
The invention belongs to functional high polymer material field, relate to a kind of preparation of palygorskite composite material with high water absorption, relate in particular to a kind of preparation method of palygorskite base salt tolerance composite material with high water absorption.
Background technology
Drought and water shortage and soil Desertification are the important factors of restriction China agricultural sustainable development.According to statistics, China's arid, the semiarid zone total area are 4,550,000 hm 2, account for 47% of territory total area, wherein China In China West Arid Land accounts for 26.6% of territory total area, and desertification of land area is every year with 2 460 km 2speed expanded.So soil conservation and resisting drought saving water are paid attention to by Chinese scholars always.The object of wherein utilizing soil high-absorbent material to reach water-saving and yield-increasing is new way and the novel method of current experimental study.
High-absorbent material claims again polymer water-absorbent, water-loss reducer of soil, is a kind of crosslinking hydrophilic sexual function high molecular polymer with three-dimensional net structure.It can absorb the hundreds of and even water of thousands of times of own wt, even and if be also not easy under external force dehydration after water suction or seldom dewater, but when drought and water shortage, can slowly release again absorbed moisture for soil, plant utilization, while running into extraneous water, it can absorb water again repeatedly, thereby reaches the effect of retaining and conserveing soil moisture.Using of high-absorbent material is a kind of chemical water-saving technology, it can significantly improve the water-holding power of soil, the invalid loss of inhibition soil moisture, improve water resources utilization and slow release fertilizer, the title that has soil " miniature reservoir ", in the field such as agricultural, forestry, gardening, water conservancy performance keeping crop seedling from drought, increasing both production and income, improvement soil, soil conservation, check winds and fix drifting sand, the several functions such as desert afforestation.Thereby high-absorbent material is generally believed it is the 4th agrochemicals product that is hopeful to be accepted by peasant most after chemical fertilizer, agricultural chemicals, mulch film in the world.Yet, investigation discovery, high-absorbent material is few applying of NORTHWEST CHINA area, particularly Desertification, is mainly because the salt tolerance of at present commercially available high-absorbent material in Desertification is poor, suction rainwater speed is slow, water absorbent rate is low.Thereby exploitation has the superabsorbent of adaptation this area characteristic to promoting the agricultural development of NORTHWEST CHINA Desertification, improves the ecological environment, the Implement of sustainable development strategy is significant.
The main product of high-absorbent material is acrylic polymers at present, water-absorbing-retaining ability strong (being generally 300～1000 g/g), thereby in agroforestry, obtained application widely.But have report, soil microorganisms hard degradation acrylic acid or the like high absorbency material, if large scale application also needs conscientiously to assess on the long-range impact of ecotope; Moreover acrylic acid or the like high-absorbent material raw materials cost is high, working condition is harsh, gel-strength is low, salt tolerance is poor, and its range of application is very limited.
In recent years, for improving the anti-salt property of high absorbency material and reducing production costs, many methods have been taked, wherein organic and inorganic composite high-water uptake material, because having higher water absorbing properties and low production cost, is subject to extensive concern in conjunction with the advantage of organic and inorganic materials performance simultaneously effectively.Polygorskite (PGS) is the moisture zeopan clay mineral of a kind of layer of chain structure, and unique ordered arrangement microvoid structure makes it have the advantages such as porosity is high, pore volume is large, quality is light, tap density is little, specific surface area is large, salt tolerance is strong, activity is good.Because polygorskite is widely distributed, cheap, simultaneously there is many wetting ability hydroxyls and active site in its surface, can with vinyl monomer generation graft copolymerization, make it join the performances such as the water suction that improves material in high-absorbent material, salt tolerant, and can effectively reduce product cost, improvement soil.2-acrylamide-2-methylpro panesulfonic acid (AMPS) is a kind of multi-functional soluble anionic monomers, and the sulfonic group in molecule makes it have strong anionic property, water-soluble, good salt tolerance; Amide group makes it have good stability to hydrolysis, anti acid alkali performance and thermostability; Active carbon-carbon double bond be conducive to its homopolymerization or with other vinyl monomer copolymerization, industrial goods are with low cost.
The preparation method of high-absorbent material is adopted radiation initiation, UV-light initiation, plasma body initiation or chemical initiated polymerization and is cross-linked and obtains by one or more monomers.In general, in forming high-absorbent material process, need N 2protection, and add a small amount of linking agent.Its synthesis condition is relatively harsh, synthesis technique is complicated, and cost is higher, and the widespread use of high-absorbent material and popularization are restricted.
Summary of the invention
The object of the invention is for problems of the prior art, a kind of preparation method of synthetic palygorskite base salt tolerance composite material with high water absorption is provided.
One, the preparation of clay-based salt tolerance composite material with high water absorption
The preparation method of clay-based salt tolerance composite material with high water absorption of the present invention, be in water solution system, take polygorskite (PGS), 2-acrylamide-2-methylpro panesulfonic acid (AMPS) and vinylformic acid (AA) is raw material, N, N'-methylene-bisacrylamide (MBA) is linking agent, at 60～80 ℃, stir 2～6h and form gel cross-linking products, cooling, washing, dehydration, dry, pulverize, both obtained clay-based salt tolerance composite material with high water absorption.Concrete preparation technology is as follows:
First palygorskite (PGS) is scattered in water, at 60～80 ℃, stir 40～90 min, then add polygorskite 2-acrylamide-2-methylpro panesulfonic acid (AMPS) and linking agent N, N'-methylene-bisacrylamide (MBA), continues to stir 50～90 min; Then add vinylformic acid, after stirring 30～180min, generate gel cross-linking products; Place 60～180 min, be cooled to room temperature, obtain the jelly shape cross-linking products with polygorskite color similarity; Wash unreacted monomer with water, dehydrated alcohol is sloughed water, vacuum-drying at 50～70 ℃, pulverize, both obtained clay-based salt tolerance composite material with high water absorption---polygorskite/poly-(2-acrylamide-2-methylpro panesulfonic acid-co-vinylformic acid) PGS/P (AMPS-co-AA) composite material with high water absorption.Wherein, the add-on of 2-acrylamide-2-methylpro panesulfonic acid (AMPS) is 2～4 times of palygorskite quality; Acrylic acid add-on is 10～15 times of palygorskite quality; The add-on of linking agent is 2-acrylamide-2-methylpro panesulfonic acid (AMPS) and 0.1%～1% of vinylformic acid (AA) total mass; The consumption of water is 30～60 times of palygorskite quality.The speed of above-mentioned stirring is 90～120 r/min.
Two, the performance test of clay-based salt tolerance composite material with high water absorption
Below by infrared spectra, X-ray diffraction, thermogravimetric analysis, scanning electron microscope, characterize the structure of matrix material, by weighting method, its performance is carried out to analytic explanation.
1, infrared test
With DIGILAB FTS 3000 FT-IR type infrared spectrometers (KBr compressing tablet) at 400～4000 cm – 1characterize the structural changes of matrix material.Fig. 1 is PGS (a), AA (b), AMPS (c) and PGS/P (AMPS-co-AA) infrared spectra (d).From Fig. 1 a, can find out 3615,3545,3411 cm -1si-OH (OH), planar water (OH that the absorption peak that place occurs is PGS 2), zeolite water (H 2o) stretching vibration peak of hydroxyl in; 1643 cm -1the hydroxyl flexural vibration peak that the absorption peak at place is crystal water; 1028 cm -1the absorption peak at place is the stretching vibration absorption peak of polygorskite Si-O-Si key; 470 cm -1place is the flexural vibration absorption peak of Si-O-Si key.In Fig. 1 b, 1706 cm -1place is the C=O stretching vibration peak of AA, the stretching vibration peak that 1632 places are C=C; 1442 and 1367 cm -1asymmetric and the symmetrical stretching vibration absorption peak that place is-COOH.In Fig. 1 c, 3398 cm -1place is N-H stretching vibration peak; 1666 cm 1place is C=O stretching vibration peak; 1613 cm 1place is C=C stretching vibration peak; 1450 cm -1c-N flexural vibration peaks; 1220 cm -1stretching vibration absorption peak for C-N; 1191 and 1048 cm -1place is the asymmetric and symmetrical stretching vibration of S=O; 630 cm -1place is the stretching vibration of S-O in sulfonic acid group.From Fig. 1 d, can find out 3427 cm -1place's peak intensity increases, for-OH and-the stack peak of NH stretching vibration; 2927 cm -1place is the C-H stretching vibration of polymkeric substance; 1717 places are the stack peak of C=O stretching vibration; 1551 and 1453 cm -1asymmetric and the symmetrical stretching vibration absorption peak that place is-COOH; 1219 cm -1place is C-N stretching vibration absorption peak; 1165 places are the stretching vibration of S=O; 1038 cm -1place is the stretching vibration absorption peak of polygorskite Si-O-Si key; 622 cm -1place is the stretching vibration of S-O in sulfonic acid group.In addition, from Fig. 1 d, it can also be seen that 3557 cm of PGS after graft copolymerization -1the almost completely dissolve of the absorption peak of Mg-OH, and PGS feature Si-O-Si absorption peak is shifted to high wave number after forming polymkeric substance; Meanwhile, 1632 cm 1with 1613 cm 1the C=C stretching vibration peak of place AMPS and AA disappears, and shows that polyreaction is abundant, in polymkeric substance, without residual monomer, prove that the hydroxyl on PGS surface and C=C pair of keys in AA and AMPS react to react to have formed organic-inorganic multipolymer.
2, XRD test
With Rigaku D/max-2400 type X-ray powder diffraction instrument (source of radiation is CuK α, 40 kV, 150 mA, λ=0.15406 nm), sample structure is tested.Fig. 2 is PGS (a) and PGS/P (AMPS-co-AA) XRD spectrum (b).By Fig. 2 a, can be found out, it is the main strong diffraction peak of PGS that 2 θ are 20.74 °, 26.54 °, 27.80 °, 30.38 °, 36.46 ° and 50.06 °; Form after matrix material 2b, whole diffraction peak intensity reduces, and peak shape broadens, and presents mild Qiu Zhuanfeng, this is owing to introducing polyacrylic acid (PAA) and gathering (2-acrylamide-2-methylpro panesulfonic acid) (PAMPS) after molecular chain, forming amorphous matrix material.In addition, matrix material is about 20.94 °, 22.42 °, 26.64 °, 27.86 °, 31.66 °, 36.58 °, 45.64 °, 50.12 ° at 2 θ and has stronger absorption peak, this is because PGS proportion in material is little, in graft copolymerization process, after PGS disperses, granularity further diminishes, or the polymkeric substance that is grafted on PGS surface has affected X-ray diffraction.This shows under the synthesis condition of PGS/P (AMPS-co-AA), the coated structure that does not change PGS of AMPS and AA, PAMPS and PAA are present in the surface of PGS with non-crystalline state form, the crystal habit of original component occurs to have changed compared with strong mutual compound action by graft copolymerization for PGS, AMPS and AA tri-components.
3, thermogravimetric test
Thermostability with PE TG/DTA 6300 type thermogravimetric-difference formula scanning amount thermal analyzer working samples, 20～800 ℃ of temperature ranges, nitrogen flow rate 50 mL/min, 10 ℃/min of heat-up rate Fig. 3 is PGS (a) and PGS/P (AMPS-co-AA) thermogravimetric curve (b).Can find out, PGS has 2.7% weightlessness 215 ℃ of left and right, this be by the free water absorbing, irreducible water and a small amount of water of constitution, slowly lost due to.PGS also has 2.9% weightlessness between 215～786 ℃, corresponding to PGS in conjunction with water and self weightlessness, total weightless 5.6%.The weightlessness of PGS/P (AMPS-co-AA) can be divided into four-stage: have 5.1% weightlessness before 224 ℃, due to slowly losing corresponding to planar water and partial crystallization water; 224-279 ℃ has 18.7% weightlessness, corresponding to polyacrylic acid, sloughs CO 2; 279～324 ℃ have 9.5% weightlessness, and this is due to due to AMPS and lose-NH of linking agent; 324～786 ℃ have 49.2% weightlessness, and this is because main chain decomposes due to fracture, adjacent polymer chains dehydration, decarboxylation and sulfonic decomposition; 786 ℃ of weightlessness are complete, and total rate of weight loss is 82.5%.This result shows, effective chemical action has occurred between PGS, AMPS, AA, has slowed down the decomposition of thermal destruction product, has improved the thermostability of matrix material.According to above analysis, can also draw, total percentage of grafting of PGS surface A MPS and AA is 76.9%.
4, sem test
Pattern with sample after JSM-5600LV scanning electron microscopic observation metal spraying.Fig. 4 is the scanning electron microscope (SEM) of PGS/P (AMPS-co-AA) matrix material.As can be seen from Figure 4, in matrix material, PGS, AA and AMPS form three-dimensional crosslinked network structure; PGS distributes more even, and granule boundary is fuzzy, and inorganic organic two-phase consistency is better, shows that PGS particle is aggregated thing network and contains preferably and fix, and does not produce and is separated; Material totally presents cellular threedimension hole.Because polynuclear plane has larger specific surface area than smooth, spherical particle, when high absorbency material is met water, greatly increased the contact area of particle and water, this just means that extraneous water molecules can fully contact with matrix material particle, enter rapidly inside particles and make its network expansion, effectively improve its water-retaining capacity and absorption speed.5, water suction kinetic test
By weighting method, measure the water-intake rate of high-absorbent material.Testing method is: accurately take the dry water-absorbing material of certain mass in beaker, add distilled water, make, after its water suction certain hour (5,10,15,20,20,40,50,60 min), to cross 100 eye mesh screens and filter unnecessary water, be calculated as follows water-intake rate:
Figure 2014100030276100002DEST_PATH_IMAGE002
In formula, m 0quality (g) for dry substance before absorbing water; m tfor the quality (g) after water suction certain hour.
Test result is found, after PGS/P (AMPS-co-AA) high water absorption composite material water absorption and swelling, can keep corresponding skeleton construction, can not dissolve.The Swelling Dynamics curve of PGS/P (AMPS-co-AA) high water absorption composite material in distilled water and rainwater is shown in Fig. 5.There is Fig. 5 to find out, prolongation in time of the swelling ratio of matrix material and increasing, linearly rises front 300 min are approximate, and after 40 min, swelling ratio increases slowly, 50 min left and right swellings reach balance substantially, and its maximum swelling rate in distilled water and rainwater is about 700 g/g and 200 g/g.Illustrate that PGS/P (AMPS-co-AA) matrix material prepared by the present invention has rate of water absorption and higher water-intake rate faster.
6, the impact of salt ionic concentration on water-intake rate
Accurately take salts solution (NaCl, MgCl that the dry water-absorbing material of 0.5 g is placed in different concns 2and AlCl 3) in, 50 min measure water-intake rate after reaching balance, assess its salt tolerance.Fig. 6 is the water-intake rate of water-absorbing material in various salts.Can find out, the water-intake rate of matrix material is along with extraneous salts solution (NaCl, MgCl 2and AlCl 3) ionic strength increase and decline, this is because water-absorbing material during swelling, has been introduced the positively charged ion in salts solution in salts solution in the network of matrix material, in matrix material-COO -,-SO 3 -produce electron screening effect, caused the permeable pressure head of gel network and external solution to decline.By Fig. 6, it can also be seen that, the water-intake rate of composite water conservation material in univalent cation salts solution is than higher in polyvalent cation solution, and water-intake rate is sequentially: NaCl> MgCl 2>AlCl 3; Higher for ionic valence condition, water-intake rate is less, main because polyvalent cation (Mg 2+, Al 3+) than univalent cation (Na +) except the ionomer effect that forms strengthens, reduce the inside and outside osmotic pressure of gel in material, meanwhile, polyvalent cation also can the carboxylic acid ion in material be combined and be formed stable complex compound, causes material water absorption and swelling hardly.Experimental result shows, at NaCl, the MgCl of 0.1 mol/L 2, AlCl 3in solution, the water regain of water-absorbing material reaches respectively 35.8,19.8,0.306 g/g, has certain salt resistant character.
7, the impact of pH value of solution value on water-intake rate
With NaOH and the HCl of 0.1 mol/L, configure respectively the different pH value of pH>6 and pH<6, and use pH meter Accurate Measurement.Accurately take several parts of certain mass dry substance ( m 0), immerse respectively in different pH solution, it is absorbed water after 90 min, cross 100 eye mesh screens and filter unnecessary water, weigh ( m t), calculate water-intake rate.Fig. 7 is the impact of pH on material water-intake rate.As can be seen from Figure 7, material water-intake rate when pH value of solution < 4 or pH>12 is lower, and between pH 4～10, water-intake rate is higher, and variation is less, is platform-like, and reaches maximum at pH=11 left and right water-intake rate.This is due in lower pH value solution, Ionized-COO -,-SO 3 -change into-COOH ,-SO 3h, makes-COO -,-SO 3 -between repulsive force reduce, osmotic pressure reduces; In addition, due to-COO -,-SO 3 -protonated, the removable amount of ions of gel inside reduces, and makes the inside and outside elastic pressure decline producing because ionic concn is poor of gel; Moreover, protonated-COOH ,-SO 3intramolecular hydrogen bond reactive force between H shrinks gel network, and swelling ability reduces.In the solution of pH 4～10, keep water-retaining capacity substantially constant, be because-the acid dissociation constant p of COOH k abe about 4.5, thus when pH>4.5, dissociate completely, in material-COO -with-COOH ,-SO 3 -with-SO 3h can form buffer system, and certain shock absorption is played in the variation of pH to external world.In high pH value solution, too much Na in alkaline solution +can form " electron screening effect " and " ionomer " effect to polymer chain, cause swelling ability to decline.
8, swelling and the deswelling in different pH solution
High-absorbent material is placed in to solution swelling for some time (180 min) of pH=6.3, then be placed in the acidic solution of pH=2, there is rapidly deswelling behavior in the water-absorbing material of swelling, and contraction rate is fast more a lot of than swelling rate, in tens minutes, just can reach contraction equilibrium state.Fig. 8 is swelling and the deswelling curve of PGS/P (AMPS-co-AA) in different pH solution.The water-keeping material of deswelling is placed in to neutral environment lower time again, still there is good swelling behavior.Repeatedly, after circulation, this water-absorbing material has good pH reversibility.Its swelling ratio is periodical change substantially, shows good swelling-deswelling behavior and recycling behavior.Prove that this matrix material has good water absorbing properties and recycling performance.
In sum, the relative prior art of the present invention has following effect:
1, to take polygorskite, 2-acrylamide-2-methylpro panesulfonic acid and vinylformic acid be raw material in the present invention, N, N'-methylene-bisacrylamide is linking agent, in water solution system, a step makes polygorskite/poly-(2-acrylamide-2-methylpro panesulfonic acid-co-vinylformic acid) multipolymer water-absorbing material---PGS/P (AMPS-co-AA), raw material is easy to get, preparation technology is simple, and synthetic cost is low;
2, preparation condition of the present invention is gentle, does not need to add chemical initiator, does not also need other initiation method, secondary pollution and the synthetic material non-uniform phenomenon of initiation of having avoided initiator to bring;
3, the whole preparation process of the present invention is to carry out in water solution system, has simplified the enrichment purifying technique of water-absorbent composite material, has reduced the pollution of emulsifying agent to water-absorbing material, has improved the purity of matrix material, has strengthened its biological safety;
4, the matrix material that prepared by the present invention has higher water regain, good salt tolerance, rate of water absorption faster, and the quick absorption of applicable Desertification rainfall in short-term, is a kind of desert drought resisting water-absorbent composite material of excellent performance;
5, the matrix material that prepared by the present invention has pH susceptibility, brine sensitivity, has absorbent function repeatedly simultaneously, therefore can reuse;
6, the matrix material thermostability that prepared by the present invention is higher, be difficult to decompose, thereby the scope of application is wider before 200 ℃.
Accompanying drawing explanation
Fig. 1 is PGS (a), AA (b), AMPS (c) and PGS/P (AMPS-co-AA) infrared spectra (d).
Fig. 2 is PGS (a) and PGS/P (AMPS-co-AA) XRD spectrum (b).
Fig. 3 is PGS (a) and PGS/P (AMPS-co-AA) TG curve (b).
Fig. 4 is the SEM pattern of PGS/P (AMPS-co-AA).
Fig. 5 is the water suction kinetic curve of PGS/P (AMPS-co-AA) water-absorbing material.
Fig. 6 is the swelling behavior test of PGS/P (AMPS-co-AA) in various salts.
Fig. 7 is the impact of pH on PGS/P (AMPS-co-AA) water-intake rate.
Fig. 8 is swelling and the deswelling curve of PGS/P (AMPS-co-AA) in different pH solution.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further, but content of the present invention is not limited to lifted example.
Embodiment 1
In 100 mL there-necked flasks, add 0.6 g PGS and 30 mL distilled water, at 80 ℃, stir 1 h; Then add 2 g AMP and 0.02 g MBA, continue to stir 40 min; Then add 8 mL AA, continuation has gel to produce stir 1 h at 75 ℃ after, places for 3 h(post polymerization times), cool to room temperature.Take out product and be cut into scissors the fragment that length is 2～5 mm.With distilled water wash for several times to remove unreacted monomer, small molecules and oligopolymer, with ethanol, slough the water in material again, after 60 ℃ of vacuum-dryings to constant weight obtains PGS/P (AMPS-co-AA) high-absorbent material, pulverized 100 mesh sieves, carry out water absorption test.Productive rate is about 81%, and percentage of grafting is 76.9%.
Performance index are as follows:
Water absorbing properties: inhale distilled water during 50 min and substantially reach saturatedly, maximum amount of inhaling distilled water is 750 g/g; The amount of inhaling the sodium chloride solution of rainwater, Huanghe water, tap water, 0.1mol/L during 50 min is respectively 190,110,98,82 g/g.
Embodiment 2
In 100 mL there-necked flasks, add 0.9 g PGS and 40 mL distilled water, mixture stirs 1 h at 60 ℃, then add 2 g AMP and 0.05 g MBA, continue to stir 60 min, then add 8 mL AA, continue to stir after 50 min at 60 ℃, have gel to produce, place 2.5h (post polymerization time), then cooled product is to room temperature.Take out product and be cut into scissors the fragment that length is 2～5 mm.Afterwards, product with distilled water wash for several times to remove unreacted monomer, small molecules and oligopolymer, with ethanol, slough the water in material, after 50 ℃ of 0 vacuum-drying to constant weight obtain PGS/P (AMPS-co-AA) high-absorbent material, pulverized 100 mesh sieves, carry out water absorption test.Productive rate is about 73%, and percentage of grafting is 69%.
Performance index are as follows:
Water absorbing properties: inhale distilled water during 50 min and substantially reach saturatedly, maximum amount of inhaling distilled water is 520 g/g; The amount of inhaling the sodium chloride solution of rainwater, Huanghe water, tap water, 0.1mol/L during 50 min is respectively 150,93,95,76 g/g.
Embodiment 3
In 100 mL there-necked flasks, add 0.4 g PGS and 30 mL distilled water, mixture stirs 1 h at 70 ℃, then add 2 g AMP and 0.07 g MBA, continue to stir 40 min, then add 10 mL AA, continue to stir after 1 h at 70 ℃, have gel to produce, at 70 ℃, placed for 2 h(post polymerization times), then cooled product is to room temperature.Take out product and be cut into scissors the fragment that length is 2～5 mm.Product with distilled water wash for several times to remove unreacted monomer, small molecules and oligopolymer, with ethanol, slough the water in material, after 70 ℃ of vacuum-dryings to constant weight obtains PGS/P (AMPS-co-AA) high-absorbent material, pulverized 100 mesh sieves, carry out water absorption test.Productive rate is about 89%, and percentage of grafting is 72%.
Performance index are as follows:
Water absorbing properties: inhale distilled water during 50 min and substantially reach saturatedly, maximum amount of inhaling distilled water is 740 g/g; The amount of inhaling the sodium chloride solution of rainwater, Huanghe water, tap water, 0.1mol/L during 50 min is respectively 163,115,105,83 g/g.

Claims (8)

1. the preparation method of a clay-based salt tolerance composite material with high water absorption, be in water solution system, take polygorskite, 2-acrylamide-2-methylpro panesulfonic acid and vinylformic acid is raw material, N, N'-methylene-bisacrylamide is linking agent, at 60～80 ℃, stir 2～6h and form gel cross-linking products, cooling, wash with water, dehydration, dry, pulverize, both obtained clay-based salt tolerance composite material with high water absorption.
2. the preparation method of clay-based salt tolerance composite material with high water absorption as claimed in claim 1, it is characterized in that: first palygorskite is scattered in water, at 60～80 ℃, stir 40～90 min, then add polygorskite 2-acrylamide-2-methylpro panesulfonic acid and linking agent N, N'-methylene-bisacrylamide, continues to stir 50～90 min; Then add vinylformic acid, after stirring 30～180min, generate gel cross-linking products; Place 60～180 min, be cooled to room temperature, obtain the jelly shape cross-linking products with polygorskite color similarity; Wash unreacted monomer with water, dehydrated alcohol is sloughed water, dry, pulverize, and has both obtained clay-based salt tolerance composite material with high water absorption.
3. the preparation method of clay-based salt tolerance composite material with high water absorption as claimed in claim 1, is characterized in that: the add-on of 2-acrylamide-2-methylpro panesulfonic acid is 2～4 times of palygorskite quality.
4. the preparation method of clay-based salt tolerance composite material with high water absorption as claimed in claim 1, is characterized in that: acrylic acid add-on is 10～15 times of palygorskite quality.
5. the preparation method of clay-based salt tolerance composite material with high water absorption as claimed in claim 1, is characterized in that: the add-on of linking agent is 0.1%～1% of 2-acrylamide-2-methylpro panesulfonic acid and vinylformic acid total mass.
6. the preparation method of clay-based salt tolerance composite material with high water absorption as claimed in claim 1, is characterized in that: the consumption of water is 30～60 times of palygorskite quality.
7. the preparation method of clay-based salt tolerance composite material with high water absorption as claimed in claim 1, is characterized in that: described dry be vacuum-drying at 50～70 ℃.
8. the preparation method of clay-based salt tolerance composite material with high water absorption as claimed in claim 1, is characterized in that: the speed of above-mentioned stirring is 90～120 r/min.
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CN109336717A (en) * 2018-11-16 2019-02-15 西北师范大学 A kind of preparation method of multi-functional concave convex rod ground mass wisdom ceramsite material
CN109704868A (en) * 2019-02-28 2019-05-03 南开大学 A kind of novel membrane-biological membrane inhibits the sustainable release method of molecule
CN110591722A (en) * 2019-09-19 2019-12-20 西北师范大学 Preparation method of high-water-absorptivity composite resin with functions of preventing soil epidermis from shrinking and reducing water evaporation
CN112625195A (en) * 2020-11-18 2021-04-09 华中科技大学 Novel sludge-based hydrogel material and preparation method thereof
CN113698659A (en) * 2021-08-27 2021-11-26 西安交通大学 Palygorskite-double-network gel sponge with oil repellency and water absorption functions as well as preparation method and application thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109336717A (en) * 2018-11-16 2019-02-15 西北师范大学 A kind of preparation method of multi-functional concave convex rod ground mass wisdom ceramsite material
CN109704868A (en) * 2019-02-28 2019-05-03 南开大学 A kind of novel membrane-biological membrane inhibits the sustainable release method of molecule
CN110591722A (en) * 2019-09-19 2019-12-20 西北师范大学 Preparation method of high-water-absorptivity composite resin with functions of preventing soil epidermis from shrinking and reducing water evaporation
CN112625195A (en) * 2020-11-18 2021-04-09 华中科技大学 Novel sludge-based hydrogel material and preparation method thereof
CN113698659A (en) * 2021-08-27 2021-11-26 西安交通大学 Palygorskite-double-network gel sponge with oil repellency and water absorption functions as well as preparation method and application thereof

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