CN115093154B - Concrete water-retaining agent and preparation method thereof - Google Patents
Concrete water-retaining agent and preparation method thereof Download PDFInfo
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- CN115093154B CN115093154B CN202210600974.8A CN202210600974A CN115093154B CN 115093154 B CN115093154 B CN 115093154B CN 202210600974 A CN202210600974 A CN 202210600974A CN 115093154 B CN115093154 B CN 115093154B
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/46—Water-loss or fluid-loss reducers, hygroscopic or hydrophilic agents, water retention agents
- C04B2103/465—Water-sorbing agents, hygroscopic or hydrophilic agents
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Abstract
The invention utilizes the corncob-based charcoal powder to modify the existing concrete water-retaining agent, and can solve the problem of environmental pollution caused by smoke dust generated by corncob incineration. Simultaneously, the alkenyl polyoxyethylene glycol ether, the ethylene glycol diacrylate, the acrylic acid monomer and the ammonium vinyl alkyl polyoxyethylene ether sulfate are adopted to be matched with the corncob-based charcoal powder to polymerize to produce the concrete water-retaining agent, so that a net structure with strong water absorption is formed, the loss of free water in concrete is effectively inhibited, meanwhile, the aggregate particles are suspended, the settlement is prevented, the concrete wrapping state can be obviously improved, and the strength development of a concrete test piece is quicker.
Description
Technical Field
The invention relates to the technical field of concrete admixtures, in particular to a concrete water-retaining agent and a preparation method thereof.
Background
The concrete water-retaining agent is a concrete admixture, a large number of amide, carboxyl and other hydrophilic groups are arranged in a molecular structure, the hydrophilic groups form a large number of micro-crosslinked structures, and a molecular network can adsorb a large number of water molecules. In the water-deficient environment, water molecules can be released, and the water can be maintained in the cement paste.
The concrete is used as the largest material in infrastructure construction, the demand is large, nearly 30% of components in the concrete are used as fine aggregates, and river sand is one of the most commonly used fine aggregates. In recent years, in order to protect the river sand resources and ecological environment of the main river artery in China, various levels of governments have issued some relevant regulations for prohibiting river sand mining, and the problem of river sand replacement is still slow. The machine-made sand is used as a substitute of river sand, but has inherent defects, and except the influence of particle shape on flowability, the machine-made sand has the problems of unsatisfactory gradation, high stone powder content and the like, so that concrete is particularly seriously separated and secreted with water. At present, several kinds of thickeners such as polyacrylamides, celluloses, polyacrylics and biogums are mostly adopted to improve the wrapping states such as segregation and bleeding. However, the molecular weight is too high, the mixing amount is sensitive, and the delayed slump retaining performance of the concrete is easily reduced. The existing concrete viscosity regulators such as cellulose ether and the like have low dissolving speed, reduce the bleeding, reduce the slump, increase the construction difficulty and have low market acceptance rate.
The corncob is prepared by threshing the corncob and then strictly screening, contains rich cellulose, hemicellulose, lignin and the like, has the advantages of uniform tissue, proper hardness, good toughness, strong water absorption, good wear resistance and the like, and has wide application scenes in high and new technology industries. The compatibility of the corncob-based biochar and a high molecular material is good, the mechanical property of the high molecular material is not influenced basically, and expensive graphene can be replaced to a certain extent, but the application of the corncob-based biochar in the concrete admixture industry is not reported.
Disclosure of Invention
The invention aims to provide a concrete water-retaining agent and a preparation method thereof, wherein the corn core-based charcoal powder is used for modifying the existing concrete water-retaining agent, so that the concrete water-retaining agent which has the advantages of simple synthesis process, low cost and strong water-retaining property and can obviously improve the wrapping state of concrete is provided.
In order to achieve the purpose, the invention provides the following technical scheme:
step 1, sequentially crushing, cleaning and drying corncobs to obtain dried corncob granules; carrying out oxygen-isolated carbonization on the dried corn cob granules under the condition that the oxygen content is less than 5 percent of the volume percentage content, and cooling to room temperature to obtain carbonized corn cob granules;
step 2, acidizing the carbonized corn cob granules by using acid liquor to obtain acidized mixed liquor A1, introducing ammonia into the acidized mixed liquor A1, adjusting the pH value to 7.5-8.0, standing for 1-2h, filtering, and drying a solid product to obtain carbonized corn cobs; grinding the carbonized corn cob into powder, and sieving the powder by a 200-mesh sieve to obtain corn cob-based charcoal powder;
step 3, adding 40-50 parts of alkenyl polyoxyethylene glycol ether, 4-5 parts of ethylene glycol diacrylate and 2000-2500 parts of deionized water into a reaction kettle, stirring until the materials are completely dissolved, heating to 70-80 ℃, adding 20-40 parts of the corncob-based charcoal powder obtained in the step 2, 20-60 parts of acrylic acid monomer and 4-5 parts of vinyl alkyl polyoxyethylene ether ammonium sulfate, and stirring for 90-120min at the temperature of 70-80 ℃;
and 4, step 4: dissolving 0.7-1.0 part of initiator in 15 parts of water to obtain an initiator aqueous solution for later use;
and 5: and (3) adding the initiator aqueous solution obtained in the step (4) into the reaction kettle in the step (3), keeping the system reaction temperature in the reaction kettle at 75-80 ℃, controlling the dropping speed, dropping for 2-3 hours, heating to 85-90 ℃, and keeping the temperature for 0.5-1 hour to obtain the corn cob-based charcoal powder modified water-retaining agent.
Further, the carbonization temperature in the step 1 is 450-550 ℃, and the carbonization time is 75-150min.
Further, the infrared spectrogram of the corncob-based charcoal powder obtained in the step 2 is 3100cm -1 、1700cm -1 、1530cm -1 、1300cm -1 There is a distinct absorption peak.
Further, the corn cob-based charcoal powder obtained in the step 2 can fade the acid potassium permanganate solution.
Further, the concentration of the potassium permanganate solution in the potassium permanganate acidic solution is 0.1mol/L, and H is used 2 SO 4 And (4) acidifying.
Further, in the step 3, the alkenyl polyoxyethylene glycol ether is one of allyl polyethylene glycol ether, 2-methallyl polyethylene glycol ether and 3-methyl-3-butene-1-polyethylene glycol ether.
Further, the average molecular weight of the alkenyl polyoxyethylene glycol ether in the step 3 is 1800-2200.
Further, in the step 4, the initiator is any one of ammonium persulfate, potassium persulfate and sodium persulfate.
Compared with the prior art, the invention has the beneficial effects that: 1. the preparation method of the corncob-based charcoal powder provided by the invention is simple in process, can be obtained without complex treatment, is easy to obtain preparation raw materials, low in price, suitable for mass production, and capable of avoiding air pollution caused by direct corncob burning. 2. The heterogeneous substance of the corncob-based biochar surrounded by the alkenyl polyoxyethylene glycol ether, the ethylene glycol diacrylate, the acrylic acid monomer and the like is polymerized to form a net structure with strong water absorption, thereby effectively inhibiting the loss of free water in concrete, and simultaneously playing a role in suspending aggregate particles and preventing sedimentation. 3. The pH value of the prepared corncob-based charcoal powder is alkaline and can be combined with-COOH groups in an acrylic monomer; in addition, the charcoal powder has a natural skeleton structure, and the charcoal powder has functional groups such as carbon-carbon double bonds, amide bonds and the like through characterization, so that a more effective cross-linking structure can be formed, and the final water-retaining agent product has high stability and stronger adsorption capacity.
Detailed Description
The present invention will be described in further detail with reference to examples, which are illustrative of the present invention and are not to be construed as being limited thereto.
Preparing the corncob-based biological carbon powder:
sequentially crushing, cleaning and drying corncobs to obtain dried corncob granules; and (3) carrying out oxygen-isolated carbonization on the dried corn cob particles under the condition that the oxygen content is less than 5% by volume percentage, and cooling to room temperature to obtain carbonized corn cob particles. Acidifying the carbonized corncob granules by adopting acid liquor to obtain acidified mixed liquor A1, introducing ammonia gas into the acidified mixed liquor A1, adjusting the pH value to 7.5-8.0, standing for 1-2h, filtering, and drying a solid product to obtain carbonized corncobs; grinding the carbonized corncobs into powder, and sieving the powder by a 200-mesh sieve to obtain the corncob-based biochar powder.
The higher the carbonization temperature and the longer the carbonization time, the lower the carbonization yield and the higher the ash content of the carbide, and the ash content of the carbide will affect the water retention property of the final water retaining agent. Therefore, the apparent density of the corncob-based charcoal powder is tested according to the standard requirements of GB/T12496.1-1999 determination of apparent density of test method of wooden activated carbon. And testing the particle size distribution of the corn cob based charcoal powder according to the standard requirement of GB/T12496.2-1999 determination of particle size distribution of wood activated carbon test method. And testing the ash content of the corn cob-based charcoal powder according to the standard requirements of GB/T12496.3-1999 determination of ash content of wood activated charcoal test method. And testing the pH value of the corn cob based charcoal powder according to the standard requirements of GB/T12496.7-1999 determination of pH value of test method for wooden activated carbon. And testing the content of the non-carbonized substance in the corn cob based charcoal powder according to the standard requirements of GB/T12496.13-1999 determination of non-carbonized substance in test method of wood activated carbon.
And determining the apparent density, the particle size distribution, the ash content, the pH value and the content of non-carbonized substances of the corn cob-based charcoal powder prepared under different conditions according to the standards, and determining the optimal carbonization temperature to be 495 ℃ and the carbonization time to be 110min through analysis and test results.
Performing infrared spectrum test on the prepared corncob-based biological carbon powder, wherein the infrared spectrum is 3100cm -1 、1700cm -1 、1530cm -1 、1300cm -1 There is a distinct absorption peak. Potassium permanganate is prepared into a solution with the concentration of 0.1mol/L, and H is used 2 SO 4 Acidifying to prepare an acidic potassium permanganate solution, and adding the corn cob-based biological carbon powder into the prepared acidic potassium permanganate solution to fade the acidic potassium permanganate solution.
Preparing a concrete water-retaining agent:
example 1:
adding 40 parts of allyl polyglycol ether with the average molecular weight of 2200, 5 parts of ethylene glycol diacrylate and 2500 parts of deionized water into a reaction kettle, stirring until the components are completely dissolved, heating to 80 ℃, adding 22 parts of corn cob-based biological carbon powder, 45 parts of acrylic acid monomer and 4 parts of ammonium vinyl alkyl polyoxyethylene ether sulfate, and stirring for 120min at the temperature of 80 ℃; 0.7 part of ammonium persulfate was dissolved in 15 parts of deionized water to obtain an aqueous initiator solution. Adding an initiator aqueous solution into a reaction kettle, keeping the system reaction temperature in the reaction kettle at 75-80 ℃, controlling the dripping acceleration, dripping within 3 hours, heating to 85-90 ℃, and preserving heat for 1 hour to obtain the corn cob based charcoal powder modified water-retaining agent.
Example 2:
adding 50 parts of 3-methyl-3-butylene-1-polyglycol ether with the average molecular weight of 1800, 5 parts of ethylene glycol diacrylate and 2200 parts of deionized water into a reaction kettle, stirring until the components are completely dissolved, heating to 80 ℃, adding 35 parts of corncob-based biochar powder, 60 parts of acrylic monomer and 5 parts of ammonium vinyl alkyl polyoxyethylene ether sulfate, and stirring for 100min at the temperature of 75 ℃; 1 part of potassium persulfate was dissolved in 15 parts of deionized water to obtain an aqueous initiator solution. Adding an initiator aqueous solution into a reaction kettle, keeping the system reaction temperature in the reaction kettle at 75-80 ℃, controlling the dropping speed, dropping within 3 hours, heating to 85-90 ℃, and keeping the temperature for 45 minutes to obtain the corn cob-based charcoal powder modified water-retaining agent.
Example 3:
adding 40 parts of 2-methallyl polyglycol ether with the average molecular weight of 1900, 4 parts of ethylene glycol diacrylate and 2000 parts of deionized water into a reaction kettle, stirring until the components are completely dissolved, heating to 70 ℃, adding 40 parts of corn cob-based biological carbon powder, 60 parts of acrylic monomer and 5 parts of ammonium vinyl alkyl polyoxyethylene ether sulfate, and stirring for 120min at the temperature of 70 ℃; 1 part of potassium persulfate was dissolved in 15 parts of deionized water to obtain an aqueous initiator solution. Adding an initiator aqueous solution into a reaction kettle, keeping the system reaction temperature in the reaction kettle at 75-80 ℃, controlling the dropping speed, dropping after 2 hours, heating to 85-90 ℃, and keeping the temperature for 45 minutes to obtain the corn cob-based charcoal powder modified water-retaining agent.
Example 4:
adding 43 parts of 3-methyl-3-butylene-1-polyglycol ether with the average molecular weight of 1800, 4.5 parts of ethylene glycol diacrylate and 2500 parts of deionized water into a reaction kettle, stirring until the components are completely dissolved, heating to 70 ℃, adding 20 parts of corncob-based biological carbon powder, 20 parts of acrylic monomer and 4.2 parts of ammonium vinyl alkyl polyoxyethylene ether sulfate, and stirring for 90min at the temperature of 80 ℃; 0.8 part of ammonium persulfate was dissolved in 15 parts of deionized water to obtain an aqueous initiator solution. Adding an initiator aqueous solution into a reaction kettle, keeping the system reaction temperature in the reaction kettle at 75-80 ℃, controlling the dropping speed, dropping after 3 hours, heating to 85-90 ℃, and keeping the temperature for 1 hour to obtain the corn cob based charcoal powder modified water-retaining agent.
Comparative example 1:
adding 46 parts of 2-methyl allyl polyglycol ether with the average molecular weight of 1900, 4.8 parts of ethylene glycol diacrylate and 2300 parts of deionized water into a reaction kettle, stirring until the components are completely dissolved, heating to 80 ℃, adding 60 parts of acrylic acid monomer and 4 parts of acrylamide, and stirring for 100min at the temperature of 75 ℃; 0.9 part of potassium persulfate was dissolved in 15 parts of deionized water to obtain an aqueous initiator solution. Adding an initiator aqueous solution into a reaction kettle, keeping the reaction temperature of the system in the reaction kettle at 75-80 ℃, controlling the dropping speed, dropping after 3 hours, and then heating to 85-90 ℃ and preserving heat for 45 minutes to obtain the water-retaining agent.
Comparative example 2:
adding 42 parts of allyl polyglycol ether with the average molecular weight of 2200, 4.3 parts of ethylene glycol diacrylate and 2000 parts of deionized water into a reaction kettle, stirring until the components are completely dissolved, heating to 70 ℃, adding 30 parts of acrylic monomer and 5 parts of vinyl alkyl polyoxyethylene ether ammonium sulfate, and stirring for 120min at the temperature of 70 ℃; 1 part of potassium persulfate was dissolved in 15 parts of deionized water to obtain an aqueous initiator solution. Adding an initiator aqueous solution into a reaction kettle, keeping the system reaction temperature in the reaction kettle at 75-80 ℃, controlling the dropping speed, dropping after 2 hours, and then heating to 85-90 ℃ and preserving the heat for 45 minutes to obtain the water-retaining agent.
Testing the performance of the concrete:
the water retention rate was measured according to the method of Water-retaining Agents for concrete (draft of comments) of the Chinese Association for building materials Standard. The water retention was calculated according to the following formula:
in the formula:
B-Water Retention,%;
Δ Sf0 — differential standard concrete segregation expansion in millimeters (mm);
Δ Sf 1-difference in segregation expansion of the tested concrete in millimeters (mm).
The water consumption should be determined by the segregation spread difference, at 5kg/m 3 Increments were made for baseline until the spread difference reached (80 ± 20) mm.
And manufacturing and curing the concrete test piece according to the method specified in GB 8076.
The samples obtained in the examples and the commercially available conventional water-retaining agent were used as comparative example 3, the solid content of the samples in the cement was 0.2%, and the water retention rate and the compressive strength of the test pieces were measured using P.O 42.5 sea snail cement, and the test results are shown in Table 1.
TABLE 1 test results of water retention and compressive strength of concrete
Compared with the comparative example and the commercial water-retaining agent product, the bleeding phenomenon is improved to a certain extent, but the bleeding phenomenon still exists in the initial state, the water retention rate is still greatly different from that of the embodiment of the invention, the post bleeding and stone exposure still exist in the concrete after 1 hour, and the fluidity of the concrete is poor. The embodiment of the water retaining agent provided by the embodiment of the invention has a remarkable improvement effect on the initial bleeding phenomenon of concrete, and has the advantages of obvious water retaining effect, no bleeding wrapping, and fast strength development of a test piece from the view of water retaining rate data.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A preparation method of a concrete water-retaining agent is characterized by comprising the following steps: the preparation method comprises the following steps:
step 1, sequentially crushing, cleaning and drying corncobs to obtain dried corncob granules; carrying out oxygen-isolated carbonization on the dried corn cob particles under the condition that the oxygen content is less than 5% of the volume percentage content, and cooling to room temperature to obtain carbonized corn cob particles;
step 2, acidizing the carbonized corn cob granules by using acid liquor to obtain acidized mixed liquor A1, introducing ammonia into the acidized mixed liquor A1, adjusting the pH value to 7.5-8.0, standing for 1-2h, filtering, and drying a solid product to obtain carbonized corn cobs; grinding the carbonized corncobs into powder, and sieving the powder by a 200-mesh sieve to obtain corncob-based charcoal powder;
step 3, adding 40-50 parts of alkenyl polyglycol ether, 4-5 parts of ethylene glycol diacrylate and 2000-2500 parts of deionized water into a reaction kettle, stirring until the materials are completely dissolved, heating to 70-80 ℃, adding 20-40 parts of the corncob-based charcoal powder obtained in the step 2, 20-60 parts of acrylic acid monomer and 4-5 parts of vinyl alkyl polyoxyethylene ether ammonium sulfate, and stirring for 90-120min at the temperature of 70-80 ℃;
and 4, step 4: dissolving 0.7-1.0 part of initiator in 15 parts of water to obtain an initiator aqueous solution for later use;
and 5: and (4) adding the initiator aqueous solution obtained in the step (4) into the reaction kettle in the step (3), keeping the system reaction temperature in the reaction kettle at 75-80 ℃, controlling the dripping speed, dripping within 2-3 hours, heating to 85-90 ℃, and preserving heat for 0.5-1 hour to obtain the concrete water-retaining agent.
2. The preparation method of the concrete water-retaining agent according to claim 1, characterized in that the carbonization temperature in step 1 is 450-550 ℃ and the carbonization time is 75-150min.
3. The method for preparing concrete water-retaining agent according to claim 1, wherein step 2 is to obtainThe infrared spectrogram of the corncob-based charcoal powder is 3100cm -1 、1700cm -1 、1530cm -1 、1300cm -1 There is a distinct absorption peak.
4. The preparation method of the concrete water-retaining agent as claimed in claim 1, wherein the corncob based charcoal powder obtained in step 2 can discolor 0.1mol/L potassium permanganate acid solution.
5. The method for preparing a concrete water retaining agent as claimed in claim 1, wherein in step 3, the alkenyl polyglycol ether is one of allyl polyglycol ether, 2-methyl allyl polyglycol ether and 3-methyl-3-butene-1-polyglycol ether.
6. The method for preparing a concrete water-retaining agent as claimed in claim 1, wherein the average molecular weight of the alkenyl polyglycol ether in step 3 is 1800-2200.
7. The method for preparing the concrete water-retaining agent according to claim 1, wherein the initiator in step 4 is any one of ammonium persulfate, potassium persulfate and sodium persulfate.
8. A concrete water-retaining agent, which is prepared by the preparation method of any one of claims 1 to 7.
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| CN102558618A (en) * | 2011-12-07 | 2012-07-11 | 北京林业大学 | Substrate water retaining agent and preparation method thereof |
| CN105131208A (en) * | 2015-08-13 | 2015-12-09 | 浙江省林业科学研究院 | Rice husk carbon-based water retention agent preparation method and rice husk carbon-based water retention agent |
| CN110606694A (en) * | 2019-09-23 | 2019-12-24 | 江苏博思通新材料有限公司 | Water-retaining agent for improving concrete state and preparation method thereof |
| AU2020101477A4 (en) * | 2020-07-24 | 2020-08-27 | Jiangxi Agricultural University | A Water-retaining Agent of Oil-tea Camellia Dregs Biochar and Its Applications in Soil Improvements |
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| CN102558618A (en) * | 2011-12-07 | 2012-07-11 | 北京林业大学 | Substrate water retaining agent and preparation method thereof |
| CN105131208A (en) * | 2015-08-13 | 2015-12-09 | 浙江省林业科学研究院 | Rice husk carbon-based water retention agent preparation method and rice husk carbon-based water retention agent |
| CN110606694A (en) * | 2019-09-23 | 2019-12-24 | 江苏博思通新材料有限公司 | Water-retaining agent for improving concrete state and preparation method thereof |
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