CN103601832A - Carbon-based water absorbent and preparation method thereof - Google Patents
Carbon-based water absorbent and preparation method thereof Download PDFInfo
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- CN103601832A CN103601832A CN201310544362.2A CN201310544362A CN103601832A CN 103601832 A CN103601832 A CN 103601832A CN 201310544362 A CN201310544362 A CN 201310544362A CN 103601832 A CN103601832 A CN 103601832A
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- retaining agent
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- 229910052799 carbon Inorganic materials 0.000 title abstract description 10
- 239000003610 charcoal Substances 0.000 claims abstract description 132
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 29
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 29
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000006386 neutralization reaction Methods 0.000 claims abstract description 19
- 239000003999 initiator Substances 0.000 claims abstract description 13
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002028 Biomass Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 134
- 239000002585 base Substances 0.000 claims description 51
- 239000000243 solution Substances 0.000 claims description 37
- 238000000034 method Methods 0.000 claims description 30
- 230000008569 process Effects 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 25
- 239000011259 mixed solution Substances 0.000 claims description 19
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000000725 suspension Substances 0.000 claims description 12
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- 239000002245 particle Substances 0.000 claims description 9
- 239000003755 preservative agent Substances 0.000 claims description 6
- 230000002335 preservative effect Effects 0.000 claims description 6
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 5
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical group C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 5
- 239000003637 basic solution Substances 0.000 claims description 4
- 239000004160 Ammonium persulphate Substances 0.000 claims description 3
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 3
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 2
- 239000004159 Potassium persulphate Substances 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 235000019394 potassium persulphate Nutrition 0.000 claims description 2
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 2
- 239000002689 soil Substances 0.000 abstract description 21
- 230000000694 effects Effects 0.000 abstract description 6
- 230000035558 fertility Effects 0.000 abstract description 5
- 239000000440 bentonite Substances 0.000 abstract description 4
- 229910000278 bentonite Inorganic materials 0.000 abstract description 4
- 239000003431 cross linking reagent Substances 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 235000013619 trace mineral Nutrition 0.000 abstract description 3
- 239000011573 trace mineral Substances 0.000 abstract description 3
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- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 2
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- 235000010755 mineral Nutrition 0.000 abstract description 2
- 239000000945 filler Substances 0.000 abstract 2
- 230000000052 comparative effect Effects 0.000 description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 238000010521 absorption reaction Methods 0.000 description 7
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- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 235000009973 maize Nutrition 0.000 description 3
- 239000004584 polyacrylic acid Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
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- 241000487918 Acacia argyrodendron Species 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
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- 125000003368 amide group Chemical group 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
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- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Soil Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to the fields of waste utilization and water absorbents and in particular relates to a carbon-based water absorbent and a preparation method thereof. The carbon-based water absorbent is prepared from the following raw materials in parts by weight: 5.245-5.255 parts of partially neutralized acrylic acid, 1.5-2.0 parts of acrylamide, 1.72-2.58 parts of filler, 0.1-0.22 part of initiator and 0.001-0.0015 part of cross-linking agent, wherein the neutralization of the partially neutralized acrylic acid is 70-80 percent; the filler comprises charcoal and bentonite; a weight ratio of the charcoal to the bentonite is 1: (1-2). According to the carbon-based water absorbent and the preparation method thereof provided by the invention, the water absorbent has high water absorbent rate and is prevented from being mildewed and decomposed; after the water absorbent is buried in the ground, the soil fertility can be improved through the mineral trace elements contained in the water absorbent, and the soil structure is improved. Therefore, the water absorbent has the effects of relieving pressure of biomass raw material treatment and environmental pollution.
Description
Technical field
The present invention relates to waste utilization and water-retaining agent field, in particular to a kind of charcoal base water-retaining agent and preparation method thereof.Charcoal base water-retaining agent of the present invention is mainly used in soil, is intended to improve retention capacity of soil, and plays the effect of solid carbon getting fat, also can be applicable to other water-retaining agent industries.
Background technology
In China, Water Resources Relationship is to all trades and professions, and water resources shortage has a strong impact on the development of China's national economy.Arid, semiarid zone have accounted for 51% of area, and severe water and soil erosion, retention capacity of soil continuous decrease, and Precipitation Distribution in Time and Space is uneven in addition, and Soil Reservoir cannot be tackled low water season, causes a large amount of crop failures.And the application of soil water-retaining agent can slow down the threat of Crops Drought, be to keep soil moisture, improve a kind of important means of efficiency of water application.
In correlation technique, water-retaining agent is that product water absorbing properties is also better by the polymer formation of vinylformic acid or acrylate, but produce and application in, have problems more, as: intensity is low, repeats energy-absorbing power low, and salt tolerance is poor, and manufacturing cost is high.
Summary of the invention
The object of the invention is to set about from water-retaining agent weighting material, use that organic waste pyrocarbon compound---charcoal is water-retaining agent weighting material, using ultrasound ripple is full cross-linked with the monomer such as vinylformic acid by it, synthesizes a kind of novel super absorbent charcoal base water-retaining agent.The water-retaining capacity of this water-retaining agent is large, and gel-strength is high, repeats good water absorption, and contains the required trace element of plant, is especially rich in carbon.Being applied to after soil, can not only increasing soil moisture content and utilization ratio, but also can play the effect of solid carbon getting fat, is a kind of soil charcoal base water-retaining agent of the novel solid carbon getting fat that absorbs water.
Embodiments of the invention provide a kind of charcoal base water-retaining agent on the one hand, raw material by following weight parts makes: the vinylformic acid of part neutralization: 5.245-5.255, acrylamide: 1.5-2.0, weighting material: 1.72-2.58, initiator: 0.1-0.22, linking agent: 0.001-0.0015;
Acrylic acid degree of neutralization of described part neutralization is: 70-80%;
Described weighting material comprises charcoal and wilkinite, and described charcoal and wilkinite are 1:1-2 according to part by weight.
Embodiments of the invention provide a kind of preparation method of charcoal base water-retaining agent on the other hand, comprising:
A. by charcoal and wilkinite, add in distilled water and mix, supersound process is well dispersed in distilled water charcoal and wilkinite, obtains charcoal and bentonitic mixing suspension liquid, as the described weighting material of preparing charcoal base water-retaining agent;
B. in acrylic acid solution, add basic solution, and stir, obtain the acrylic acid solution that degree of neutralization is 70-80%;
C. in the acrylic acid solution after the neutralization obtaining to step b, add acrylamide and linking agent, and step a charcoal and the bentonitic mixing suspension liquid that obtain, mix; Then in above-mentioned mixed solution, add initiator solution, airtight after stirring;
D. above-mentioned mixed solution under air tight condition is heated to 30-60 ℃, then under the condition of 250w, supersound process 3～5h is gel to mixed solution, is charcoal base water-retaining agent.
Charcoal base water-retaining agent that the embodiment of the present invention provides and preparation method thereof, compare with the water-retaining agent of filled with starch class material of the prior art, by adding charcoal and the wilkinite after supersound process, its surface has a large amount of active groups to be activated, the water-retaining agent being synthesized, not only there is high water absorbent rate, and can not go mouldy and decompose; Simultaneously, because raw material is the extremely abundant charcoal of a kind of carbon content being formed by organic waste charing, bury underground rear upper a century and can not disappear, wherein contained mineral trace element also can supplement organic content for soil, improve the fertility of soil, improve Soil structure; In addition, in preparing the process of charcoal, wide material sources have been utilized, low price, the easily biomass material of processing.Therefore, the water-retaining agent that utilizes charcoal to prepare, also has and alleviates the pressure of biomass material processing and the effect of problem of environmental pollution.
Accompanying drawing explanation
Fig. 1 shows the water-retaining capacity graphic representation of the water-retaining agent that embodiment 1 and comparative example provide;
Fig. 2 shows the water retention capacity graphic representation of the water-retaining agent that embodiment 1 and comparative example provide;
Fig. 3 shows the infrared spectrogram of the water-retaining agent that embodiment 1 and comparative example provide;
Fig. 4 shows the transmission electron microscope scintigram of the water-retaining agent that embodiment 1 provides;
Fig. 5 shows the transmission electron microscope scintigram of the water-retaining agent that comparative example provides.
Embodiment
Below by specific embodiment, and by reference to the accompanying drawings the present invention is described in further detail.
A kind of charcoal base water-retaining agent that the embodiment of the present invention provides, raw material by following weight parts makes: the vinylformic acid of part neutralization: 5.245-5.255 part, acrylamide: 1.5-2.0 part, weighting material: 1.72-2.58 part, initiator: 0.1-0.22 part, linking agent: 0.001-0.0015 part;
Acrylic acid degree of neutralization of described part neutralization is: 70-80%;
Described weighting material comprises charcoal and wilkinite, and described charcoal and wilkinite are 1:1-2 according to part by weight.
Wherein, initiator is selected from a kind of in Potassium Persulphate, Sodium Persulfate and ammonium persulphate.The initiator initiator system of ammonium persulfate of the embodiment of the present invention, initiator amount directly affects the length of the speed of polyreaction and the molecular mass of polymerisate and polymer molecular chain, thereby affects the network structure of polymkeric substance.In the embodiment of the present invention, the concentration of ammonium persulfate solution is preferably 100g/L, and the volume of ammonium persulfate solution is preferably 2.0-3.0ml.
The preferred N,N methylene bis acrylamide of linking agent of the embodiment of the present invention.Charcoal base water-retaining agent is the crosslinked high molecular polymer of a kind of low density, along with the increase of dosage of crosslinking agent, the cross-linking set in charcoal base water-retaining agent network increases, and causes cross-linking density to increase the micropore in cross-linked network structure is dwindled, water-intake rate cannot hold water molecules, therefore also can decline.In the embodiment of the present invention, the concentration of N,N methylene bis acrylamide solution is preferably 1g/L, and volume is preferably 0.5-1.5ml.
Wherein, charcoal and bentonitic particle diameter are 200 orders.
In the embodiment of the present invention, charcoal is prepared as follows: after biomass material is pulverized, put into crucible, crucible is put into retort furnace after adding a cover, and under 300-400 ℃ of condition, 0.5-3h is processed in charing, obtains charcoal.
Charcoal is the black wood charcoal that a kind of carbon content is extremely abundant, buries underground rear hundreds of to more than one thousand years and can not disappear, and can be that soil supplements organic content, improves the fertility of soil, and charcoal has a lot of pore textures, has very strong adsorptive power.The embodiment of the present invention be take charcoal and is prepared charcoal base water-retaining agent as one of weighting material, during water-retaining agent is placed into the soil after, not only there is absorbent function, and can also improve the fertility of soil, improve Soil structure.
The charcoal that water-retaining agent that the embodiment of the present invention provides is used, the preferred charcoal of 200 order particle diameters, under the condition of 250w, supersound process 40-50min, is well dispersed in distilled water charcoal.Charcoal is after supersound process, can produce a large amount of active groups, wherein part can with polyacrylic acid in hydroxyl form chemical bond, make charcoal become the part in water-retaining agent, the existence of charcoal has not only increased the gel degree of water-retaining agent, make water-retaining agent be not easy to decompose, increased stability, and the hydrophilic radical in charcoal and micropore have also increased the water absorbent rate of water-retaining agent.
The biomass material of preparing charcoal in the embodiment of the present invention is preferably stalk, agricultural wastes (as the waste residue in the stalk of farm crop, careless class, shell class and agricultural byproducts processing process) and fells industrial wood waste (as wood shavings, wood chip, wood fragments).Because above-mentioned biomass material source is abundant, low price, easily processing, therefore, utilizes charcoal to prepare charcoal base water-retaining agent as raw material, can reduce production costs greatly; Meanwhile, due to biomass material contaminate environment, need to carry out artificial special processing, therefore, the embodiment of the present invention is prepared charcoal with biomass material, and recycling charcoal is prepared charcoal base water-retaining agent, has and alleviates the pressure of biomass material processing and the effect of problem of environmental pollution.
The charcoal base water-retaining agent that the embodiment of the present invention provides, the preferred wilkinite of 200 order particle diameters, under the condition of 250w, supersound process 40-50min, is well dispersed in distilled water wilkinite.Wilkinite is after supersound process, and surface can form a large amount of hydrophilic radicals, is not only conducive to improve the network structure of water-retaining agent, and can improves water absorbent rate.
After charcoal supersound process, its surface produces a large amount of active groups, greatly strengthens its adsorptivity, joins gel effect and the water absorbing properties that can improve water-retaining agent in water-retaining agent as weighting agent.Wilkinite forms a large amount of hydrophilic radicals through supersound process rear surface, and this improves water-intake rate and be very helpful, and then affect the water absorbing properties of product improving the network structure of water-retaining agent.In the embodiment of the present invention, charcoal is preferably 1:1-2 with the ratio of bentonitic consumption.
The preparation method of the charcoal base water-retaining agent that the embodiment of the present invention provides, specifically operates in accordance with the following steps:
A. charcoal and wilkinite are all crossed to 200 mesh sieves, then add distilled water to mix, under the condition of 250w, supersound process 40-50min, charcoal and wilkinite are well dispersed in distilled water, obtain charcoal and bentonitic mixing suspension liquid, as the described weighting material of preparing charcoal base water-retaining agent.
B. in acrylic acid solution, add basic solution, and stir, obtain the acrylic acid solution that degree of neutralization is 70-80%.Because vinylformic acid is easy to polymerization reaction take place, in the embodiment of the present invention, in order to prevent acroleic acid polymerization, in vinylformic acid and time in ice-water bath, carry out; Wherein, the concentration of acrylic acid solution is 1.049-1.051g/ml, and basic solution is selected from a kind of in sodium hydroxide solution, potassium hydroxide solution and solution of ammonium hydroxide, preferred sodium hydroxide solution, and the mass concentration of sodium hydroxide solution is 25%.
C. in the acrylic acid solution after the neutralization obtaining to step b, add acrylamide soln and cross-linking agent solution, and step a charcoal and the bentonitic mixing suspension liquid that obtain, mix; Then in above-mentioned mixed solution, add initiator solution, after stirring, vessel port is airtight.Make polymerization and be cross-linked to carry out in confined conditions, prevent that the active group on charcoal and wilkinite surface is oxidized.The embodiment of the present invention preferably adopts preservative film that vessel port is airtight, because preservative film can be avoided bonding between the gelatinous water-retaining agent that forms and glassware, convenient absorbent agent is taken out from glassware.Wherein, the mass concentration of acrylamide soln is 30%, and the mass concentration of cross-linking agent solution is 1g/L.
D. above-mentioned mixed solution under air tight condition is heated to 30-60 ℃, then under the condition of 250w, supersound process 3-5h is gel to mixed solution, is charcoal base water-retaining agent.The gel charcoal base water-retaining agent obtaining is toasted to 20-30h under 75 ℃ of-80 ℃ of conditions in baking oven, then pulverize, obtain 50-60 object water-retaining agent finished product.Supersound process, makes, between the material in mixed solution, polymerization and crosslinking reaction occur, and forms the water-retaining agent with cross-linked structure.The present invention adopts above-mentioned supersound process condition, is conducive to the cancellated formation of water-retaining agent, obtains the water-retaining agent that gel degree is high.
Embodiment 1
To after corn straw smashing, put into crucible, crucible is put into retort furnace after adding a cover, and under 300 ℃ of conditions, 0.5h is processed in charing, obtains charcoal.
0.86g charcoal and the 0.86g wilkinite of crossing respectively 200 mesh sieves are mixed, add in 30ml distilled water, stir, under the condition of 250w, supersound process 40min, is well dispersed in distilled water charcoal and wilkinite, obtains charcoal and bentonitic mixing suspension liquid.
Get 5ml concentration and be the acrylic acid solution of 1.049g/ml in beaker, beaker is placed under ice-water bath condition, adding 5ml mass concentration is 25% sodium hydroxide solution.
Under normal temperature condition, to adding 5ml mass concentration in the acrylic acid solution after above-mentioned neutralization, be the N,N methylene bis acrylamide solution that 30% acrylamide soln and 1ml concentration are 1g/L, mix; Add again charcoal obtained above and bentonitic mixing suspension liquid, mix; Then to adding 2.2ml concentration in above-mentioned mixed solution, be the ammonium persulfate solution of 100g/L, after stirring, beaker mouth sealed with preservative film.
Above-mentioned mixed solution under air tight condition is heated to 30 ℃, and then under the condition of 250w, supersound process 3h is gel to mixed solution, is charcoal base water-retaining agent.The gel charcoal base water-retaining agent obtaining is toasted to 20h under 75 ℃ of conditions in baking oven, then pulverize, obtain 50 object water-retaining agent finished products.
After sawdust is pulverized, put into crucible, crucible is put into retort furnace after adding a cover, and under 400 ℃ of conditions, 2h is processed in charing, obtains charcoal.
0.86g charcoal and the 1.72g wilkinite of crossing respectively 200 mesh sieves are mixed, add in 50ml distilled water, stir, under the condition of 250w, supersound process 50min, is well dispersed in distilled water charcoal and wilkinite, obtains charcoal and bentonitic mixing suspension liquid.
Get 5ml concentration and be the acrylic acid solution of 1.051g/ml in beaker, beaker is placed under ice-water bath condition, adding 5ml mass concentration is 25% sodium hydroxide solution.
Under normal temperature condition, to adding 6ml mass concentration in the acrylic acid solution after above-mentioned neutralization, be the N,N methylene bis acrylamide solution that 30% acrylamide soln and 1.5ml concentration are 1g/L, mix; Add again charcoal obtained above and bentonitic mixing suspension liquid, mix; Then to adding 2ml concentration in above-mentioned mixed solution, be the ammonium persulfate solution of 100g/L, after stirring, beaker mouth sealed with preservative film.
Above-mentioned mixed solution under air tight condition is heated to 60 ℃, and then under the condition of 250w, supersound process 5h is gel to mixed solution, is charcoal base water-retaining agent.The gel charcoal base water-retaining agent obtaining is toasted to 30h under 80 ℃ of conditions in baking oven, then pulverize, obtain 60 object water-retaining agent finished products.
Embodiment 3
After ight soil is pulverized, put into crucible, crucible is put into retort furnace after adding a cover, and under 350 ℃ of conditions, 3h is processed in charing, obtains charcoal.
0.86g charcoal and the 1.35g wilkinite of crossing respectively 200 mesh sieves are mixed, add in 40ml distilled water, stir, under the condition of 250w, supersound process 45min, is well dispersed in distilled water charcoal and wilkinite, obtains charcoal and bentonitic mixing suspension liquid.
Get 5ml concentration and be the acrylic acid solution of 1.05g/ml in beaker, beaker is placed under ice-water bath condition, adding 5ml mass concentration is 25% sodium hydroxide solution.
Under normal temperature condition, to adding 5ml mass concentration in the acrylic acid solution after above-mentioned neutralization, be the N that 30% acrylamide soln and 0.5ml concentration are 1g/L, N-methylene-bisacrylamide solution, and charcoal obtained above and bentonitic mixing suspension liquid, mix; Then to adding 3ml concentration in above-mentioned mixed solution, be the ammonium persulfate solution of 100g/L, after stirring, beaker mouth sealed with preservative film.
Above-mentioned mixed solution under air tight condition is heated to 45 ℃, and then under the condition of 250w, supersound process 4h is gel to mixed solution, is charcoal base water-retaining agent.The gel charcoal base water-retaining agent obtaining is toasted to 25h under 78 ℃ of conditions in baking oven, then pulverize, obtain 50 object water-retaining agent finished products.
Comparative example is not for adding the acrylate copolymer type water-retaining agent of any material, and preparation method is with embodiment 1.
Water absorbing properties and the water retention property of the water-retaining agent providing of embodiment 1 and comparative example are provided.
Wherein, rate of water absorption is measured as follows:
0.1g water-retaining agent is placed in to the bottom of 100ml graduated cylinder, a thieving paper is cut into the circular paper that diameter is slightly smaller than graduated cylinder diameter, and be overlying on the water-retaining agent of graduated cylinder bottom, record the initial scale of the graduated cylinder that the little scraps of paper are corresponding, then to the deionized water that adds 100ml in graduated cylinder, and every the scale of graduated cylinder corresponding to the little scraps of paper of 1 hour record, utilize the scale of the graduated cylinder that the little scraps of paper of a certain moment are corresponding to deduct the initial scale of the graduated cylinder that the little scraps of paper are corresponding, calculate water-retaining agent in this water regain constantly.The time dependent curve of water regain in measuring 10 hours, as shown in Figure 1, wherein, line 1 represents the water absorbing properties curve of the charcoal base water-retaining agent that embodiment 1 provides, line 2 represents the water absorbing properties curve of the water-retaining agent that does not add charcoal that comparative example provides.
Water retention is measured as follows:
Water-retaining agent after above-mentioned abundant water suction is placed on watch-glass, in 80 degree drying bakers, measure not the weight of water-retaining agent in the same time, utilize the quality of arbitrary moment water-retaining agent to deduct the water yield containing in the Mass Calculation water-retaining agent of water-retaining agent itself, be the water-retaining capacity of this moment water-retaining agent, the water-retaining capacity of measuring water-retaining agent in 10 hours is curve over time, as shown in Figure 2.Wherein, line 1 represents the water retention property curve of the charcoal base water-retaining agent that embodiment 1 provides, and line 2 represents the water retention property curve of the water-retaining agent that does not add charcoal that comparative example provides.
As can be seen from Figure 1, more than the water regain of the charcoal base water-retaining agent that the embodiment of the present invention 1 provides has increased 1000ml in 10 hours, and the water regain of the water-retaining agent that does not add charcoal that comparative example provides has increased less than 400ml in 10 hours, visible, the charcoal base water-retaining agent that the embodiment of the present invention 1 provides has good water absorbing properties, and the water absorbing properties of the water-retaining agent that does not add charcoal that comparative example provides is poor.
As can be seen from Figure 2, the charcoal base water-retaining agent that the embodiment of the present invention 1 provides water-retaining capacity after 9 hours in the baking oven of 80 ℃ is still more than 20ml, the water-retaining agent that does not add charcoal that comparative example provides water-retaining capacity after 9 hours in the baking oven of 80 ℃ is 0, visible, the charcoal base water-retaining agent that the embodiment of the present invention 1 provides has good water retention property, and the water-retaining agent water retention property that does not add charcoal that comparative example provides is poor.
Embodiment 1 is carried out to infrared measurement with the water-retaining agent that comparative example provides.
Measuring method is: take 1-2mg water-retaining agent sample, compressing tablet is prepared into infrared scan sample together with KBr respectively, uses Nicolet5700 model Fourier transformation infrared spectrometer (Nicolet) at wave number 4000-400cm
-1scope interscan is also recorded infrared spectrogram.
Measurement result as shown in Figure 3.Wherein, line 1 represents the infrared spectrogram of the charcoal base water-retaining agent that embodiment 1 obtains, and line 2 represents the infrared spectrogram of the water-retaining agent of comparative example.
As can be seen from Figure 3, at 500cm
-1-1000cm
-1in wave-number range and 1700cm
-1-2900cm
-1in wave-number range, embodiment 1 presents significantly different from the absorption peak of the water-retaining agent of comparative example.Hydroxyl (3430cm on online 1
-1), amide group (1652cm
-1) and carbonyl (1557cm
-1and 1458cm
-1) infrared absorption peak be all better than line 2, and at 3628cm
-1, 3176cm
-1hydroxyl and 1565cm
-1and 1458cm
-1amide group, 1712cm
-1and 790cm
-1aromatic base, 1238cm
-1aryl amine, 1171cm
-1sulfahydantoin, 1014cm
-1the infrared absorption peak of the water-absorbent groups such as ether be also all better than the water-retaining agent that does not add charcoal.Therefore, this Infrared spectroscopy spectrogram has illustrated that the inside of the water-retaining agent that contains charcoal contains a large amount of hydrophilic radicals fully, exactly because also added the charcoal of supersound process, form a large amount of water suction groups, just greatly improved the water absorbing properties of water-retaining agent.
After being processed according to ordinary method with the water-retaining agent of comparative example, embodiment 1 carries out transmission electron microscope scanning.As shown in Figure 4 and Figure 5, wherein, the acceleration voltage adopting when the sample of embodiment 1 is carried out to transmission electron microscope scanning is 100kv to result, and the enlargement ratio of the scanned photograph obtaining is 40000; The acceleration voltage adopting when the sample of comparative example is carried out to transmission electron microscope scanning is 100kv, and the enlargement ratio of the scanned photograph obtaining is 70000.In Fig. 4,1 represents charcoal particle, and 2 represent bentonite clay particle.
As can be seen from Figure 4, the interpolation that embodiment 1 provides charcoal and bentonitic water-retaining agent soft thin, colloid is expansion shape, wherein contains large number of biological charcoal and bentonite clay particle (as shown in 1 in Fig. 4,2), and charcoal and wilkinite and polyacrylic acid crosslinked, form reticulated structure.Charcoal particle wherein, at pyrolytic process, form a large amount of pore textures, charcoal surface forms more active group, as: hydroxyl and aromatic group and derivative thereof, can improve the absorption property of charcoal, interweave fully and form three-dimensional netted space structure with polyacrylic acid in water-retaining agent and other monomer, and form certain physics hole.When the water-retaining agent that contains charcoal particle contacts with water, moisture is easy to enter water-retaining agent, thereby the water-retaining capacity of water-retaining agent is improved.
As can be seen from Figure 5, the not interpolation charcoal that comparative example provides and bentonitic water-retaining agent, show as one closely, and surperficial major part is level and smooth, there is no obvious fold, and without through hole.It is too little that such structure not only makes water-retaining agent and water engaging surface amass, and can hinder water molecules to water-retaining agent internal divergence, causes the seepage velocity of water molecules in water-retaining agent low, and then make the rate of water absorption of water-retaining agent low, and water-retaining capacity declines.
Measure as follows the water absorbent rate of the water-retaining agent that charcoal base water-retaining agent that the embodiment of the present invention provides and comparative example provide:
Accurately take 1g water-retaining agent powder and be put in the small beaker of 100ml, add the distilled water of 100ml, place at ambient temperature 10 hours, by the 100 order nylon net filters for resin after water suction.Weigh the water-absorbing resin obtaining after filtering, and calculate water absorbent rate with following formula: the quality (g) of water-retaining agent before water absorbent rate=(quality (g) of water-retaining agent before quality (the g)-water suction of the rear water-retaining agent of water suction)/water suction
As a result, the water absorbent rate of the charcoal base water-retaining agent that the embodiment of the present invention 1, embodiment 2 and embodiment 3 provide, is respectively: 1156,1120 and 1130, and the water absorbent rate of the water-retaining agent that comparative example provides is 310.Illustrate that charcoal base water-retaining agent provided by the invention has high water absorbing properties.
Take respectively the charcoal base water-retaining agent that 0.02g embodiment 1, embodiment 2 and embodiment 3 and comparative example provide, and respectively under identical condition, after fully mixing with soil, be filled into respectively in nutrition pot, then the maize seedling of the same terms (such as height, growing state etc.) is transplanted in the nutrition pot that different charcoal base water-retaining agents is housed, the 40ml that all waters, places 10 days, observes its wilting situation.
After 10 days, the maize seedling in the nutrition pot that contains the charcoal base water-retaining agent that embodiment 1, embodiment 2 and embodiment 3 provide is still in erectility, and upgrowth situation is good; There is serious wilting in the maize seedling in the nutrition pot that contains the charcoal base water-retaining agent that comparative example provides.The water-retaining agent that the above results explanation embodiment of the present invention provides not only has good water-absorbing-retaining performance, repeats water absorbing properties, and has higher fertility.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a charcoal base water-retaining agent, is characterized in that, by the raw material of following weight parts, is made: the vinylformic acid of part neutralization: 5.245-5.255 part, acrylamide: 1.5-2.0 part, weighting material: 1.72-2.58 part, initiator: 0.1-0.22 part, linking agent: 0.001-0.0015 part;
Acrylic acid degree of neutralization of described part neutralization is: 70-80%;
Described weighting material comprises charcoal and wilkinite, and described charcoal and wilkinite are 1:1-2 according to part by weight.
2. charcoal base water-retaining agent according to claim 1, is characterized in that, described charcoal and bentonitic particle diameter are 200 orders.
3. charcoal base water-retaining agent according to claim 1, is characterized in that, described initiator is selected from a kind of in Potassium Persulphate, Sodium Persulfate and ammonium persulphate.
4. charcoal base water-retaining agent according to claim 3, is characterized in that, described initiator is ammonium persulphate.
5. charcoal base water-retaining agent according to claim 1, is characterized in that, described linking agent is N,N methylene bis acrylamide.
6. charcoal base water-retaining agent according to claim 1, it is characterized in that, described charcoal is prepared as follows: after biomass material is pulverized, put into crucible, crucible is put into retort furnace after adding a cover, under 300-400 ℃ of condition, 0.5-3h is processed in charing, obtains charcoal.
7. the preparation method of the charcoal base water-retaining agent described in claim 1-6 any one, is characterized in that, comprising:
A. by charcoal and wilkinite, add in distilled water and mix, supersound process is well dispersed in distilled water charcoal and wilkinite, obtains charcoal and bentonitic mixing suspension liquid, as the described weighting material of preparing charcoal base water-retaining agent;
B. in acrylic acid solution, add basic solution, and stir, obtain the acrylic acid solution that degree of neutralization is 70-80%;
C. in the acrylic acid solution after the neutralization obtaining to step b, add acrylamide and linking agent, and step a charcoal and the bentonitic mixing suspension liquid that obtain, mix; Then in above-mentioned mixed solution, add initiator solution, airtight after stirring;
D. above-mentioned mixed solution under air tight condition is heated to 30-60 ℃, then under the condition of 250w, supersound process 3～5h is gel to mixed solution, is charcoal base water-retaining agent.
8. preparation method as claimed in claim 7, is characterized in that, described airtight employing preservative film.
9. preparation method as claimed in claim 7, is characterized in that, in described step a, described supersound process is under the condition of 250w, supersound process 40～50min.
10. preparation method as claimed in claim 7, is characterized in that, described steps d also comprises the step of oven dry, and described oven dry for to toast 20-30h under 75 ℃～80 ℃ conditions.
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