CN117143268A - Functional auxiliary agent of flocculant in environment-friendly machine-made sand for concrete and preparation method thereof - Google Patents
Functional auxiliary agent of flocculant in environment-friendly machine-made sand for concrete and preparation method thereof Download PDFInfo
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- 239000004567 concrete Substances 0.000 title claims abstract description 55
- 239000004576 sand Substances 0.000 title claims abstract description 53
- 239000012752 auxiliary agent Substances 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title abstract description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 35
- 229920000858 Cyclodextrin Polymers 0.000 claims description 30
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 30
- 239000001116 FEMA 4028 Substances 0.000 claims description 27
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 27
- 229960004853 betadex Drugs 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- 230000032050 esterification Effects 0.000 claims description 19
- 238000005886 esterification reaction Methods 0.000 claims description 19
- 150000007524 organic acids Chemical group 0.000 claims description 18
- 230000001376 precipitating effect Effects 0.000 claims description 16
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 claims description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- 238000006467 substitution reaction Methods 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 claims description 5
- 239000000174 gluconic acid Substances 0.000 claims description 5
- 235000012208 gluconic acid Nutrition 0.000 claims description 5
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 5
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 4
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 4
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 4
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 4
- LNOPIUAQISRISI-UHFFFAOYSA-N n'-hydroxy-2-propan-2-ylsulfonylethanimidamide Chemical compound CC(C)S(=O)(=O)CC(N)=NO LNOPIUAQISRISI-UHFFFAOYSA-N 0.000 claims description 4
- 239000001119 stannous chloride Substances 0.000 claims description 4
- 235000011150 stannous chloride Nutrition 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 239000003607 modifier Substances 0.000 claims 2
- 239000013538 functional additive Substances 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 2
- 229920002401 polyacrylamide Polymers 0.000 description 20
- 239000000047 product Substances 0.000 description 14
- 239000008394 flocculating agent Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 239000003638 chemical reducing agent Substances 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 239000004568 cement Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 125000000129 anionic group Chemical group 0.000 description 4
- 125000002091 cationic group Chemical group 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 229920005646 polycarboxylate Polymers 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000178 monomer Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 description 3
- 239000002689 soil Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005189 flocculation Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 239000010881 fly ash Substances 0.000 description 2
- 150000003949 imides Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000008030 superplasticizer Substances 0.000 description 2
- DPZHKLJPVMYFCU-UHFFFAOYSA-N 2-(5-bromopyridin-2-yl)acetonitrile Chemical compound BrC1=CC=C(CC#N)N=C1 DPZHKLJPVMYFCU-UHFFFAOYSA-N 0.000 description 1
- PXRKCOCTEMYUEG-UHFFFAOYSA-N 5-aminoisoindole-1,3-dione Chemical compound NC1=CC=C2C(=O)NC(=O)C2=C1 PXRKCOCTEMYUEG-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 150000001923 cyclic compounds Chemical class 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0009—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Glucans, e.g. polydextrose, alternan, glycogen; (alpha-1,4)(alpha-1,6)-D-Glucans; (alpha-1,3)(alpha-1,4)-D-Glucans, e.g. isolichenan or nigeran; (alpha-1,4)-D-Glucans; (alpha-1,3)-D-Glucans, e.g. pseudonigeran; Derivatives thereof
- C08B37/0012—Cyclodextrin [CD], e.g. cycle with 6 units (alpha), with 7 units (beta) and with 8 units (gamma), large-ring cyclodextrin or cycloamylose with 9 units or more; Derivatives thereof
-
- 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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/38—Polysaccharides or derivatives thereof
Abstract
The invention provides a flocculant functional auxiliary agent in environment-friendly machine-made sand for concrete and a preparation method thereof. The flocculant functional auxiliary agent in the environment-friendly machine-made sand for concrete can effectively reduce the viscosity of the concrete, shorten the reverse extraction time and improve the working performance of the concrete.
Description
Technical Field
The invention relates to the field of concrete building materials, in particular to a flocculant functional auxiliary agent in environment-friendly machine-made sand for concrete, and simultaneously relates to a preparation method of the flocculant functional auxiliary agent in environment-friendly machine-made sand for concrete.
Background
In recent years, with the continuous expansion of the market demand of concrete, the sand usage amount is rapidly increased, natural sand resources are gradually reduced, the yield is reduced, the yield of natural sand is seriously insufficient to meet the building demand, and machine-made sand is a main raw material for commercial concrete production. The machine-made sand can generate a large amount of soil and stone powder in the ore exploitation and crushing process, wherein the soil has great negative influence on the concrete performance, measures are needed to control the content of the soil powder in the machine-made sand, and a water washing mode is often adopted for treatment, but a large amount of sand washing sewage is generated. In order to reduce the production water and meet the environmental protection requirement, a water washing machine-made sand production enterprise usually adopts a flocculating agent to quickly settle, purify and clarify sand washing water for quickening recycling, but the upper clean water is recycled to wash sand again, so that a certain amount of flocculating agent remains on the surfaces of machine-made sand particles and in the water contained in the machine-made sand, the recycling of the sand water can cause the residual accumulation of the flocculating agent in the machine-made sand, and the residual quantity of polyacrylamide which can be dissolved out in the recycling water washing machine-made sand is 0.0002% -0.0020% (based on the mass of the machine-made sand). The content of polyacrylamide is usually 10-100 times higher than the actual content, which seriously affects the performance of concrete, and the quality accident of concrete is caused in recent years.
At present, most flocculating agents adopted by sandstone enterprises are anionic polyacrylamide PAM (molecular weight is 1200 ten thousand, 1800 ten thousand and the like), nonionic polyacrylamide and cationic polyacrylamide flocculating agents. In the concrete production process, the flocculant remained in the machine-made sand can cause interference on competitive adsorption and dispersion performance of the polycarboxylic acid water reducer in cement particles due to the excessively high molecular weight of the flocculant, so that the doping amount of the additive is greatly increased, the problems of increased cohesiveness, accelerated slump loss and the like of the concrete mixture are solved, and the adjustment difficulty and cost of the concrete additive are increased, so that the flocculant is one of the common problems in the current industry.
CN113773441a proposes a deflocculant, which is mainly formed by copolymerizing several cationic monomers and styrene, and is used together with a water reducing agent, so that the influence of the deflocculant on fluidity can be reduced, but the deflocculant is based on that the cationic monomers have positive charge branched chains and absorb different charges of the flocculating agent with negative charges, so that the flocculating agent is firmly adsorbed together to form a large group, thus precipitating from cement slurry solution, only effectively precipitating anionic polyacrylamide, but not overcoming nonionic and cationic polyacrylamide. The patent CN112661913A synthesizes a functional polycarboxylate water reducer for resisting flocculating agent in machine-made sand by using imide, unsaturated carboxylic acid and macromonomer, has better effect of resisting flocculating agent compared with the commonly used polycarboxylate water reducer, but the preparation process is complex, and the monomer such as imide which is more expensive is used, so that the use cost is too high, and the preparation method has no practical application value.
Therefore, research and development of the flocculant functional auxiliary agent in the machine-made sand for preventing the flocculant from affecting the concrete quality has important significance for popularization and application of the machine-made sand 。
Disclosure of Invention
In view of the above, the invention provides an environment-friendly flocculant functional auxiliary agent in machine-made sand for concrete, so as to effectively reduce the viscosity of concrete prepared from machine-made sand containing flocculant and improve the working performance of the concrete.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
the flocculant functional auxiliary agent in the environment-friendly machine-made sand for the concrete comprises an esterification modified substance of grafting an organic acid group on the hydroxyl group of beta-cyclodextrin.
Further, the organic acid includes maleic anhydride, sulfamic acid, gluconic acid or citric acid.
Further, the esterification degree of substitution of the esterification modified product is 0.5 to 0.7.
The invention also provides a preparation method of the flocculant functional auxiliary agent in the environment-friendly machine-made sand for concrete, which comprises the following steps:
adding beta-cyclodextrin into a solvent for dissolution, adding an organic acid and a catalyst, heating, precipitating a solid by using acetone, filtering the solid, drying, adding absolute methanol into the solid for dissolution and filtration, precipitating a product by using acetone, crystallizing by using distilled water acetone, and drying in vacuum to obtain the flocculant functional auxiliary agent in the environment-friendly machine-made resistant sand for concrete.
Further, the solvent includes N, N-dimethylformamide.
Further, the catalyst comprises at least one of concentrated sulfuric acid, zinc oxide, stannous chloride and dibutyl tin dilaurate.
Further, the heating temperature is controlled to be 60-70 ℃.
The flocculant functional auxiliary agent in the environment-friendly type anti-machine-made sand for concrete is used for carrying out chemical esterification modification on beta-cyclodextrin (beta-CD), grafting organic acid groups, and by means of the unique structure of the modified beta-cyclodextrin, the flocculant functional auxiliary agent can be preferentially adsorbed on a polyacrylamide molecular chain in preference to polycarboxylic acid molecules, and meanwhile, the distance between the polycarboxylic acid molecules and the polyacrylamide molecules is increased, so that the probability that the polycarboxylic acid molecules are adsorbed and embedded by the polyacrylamide is reduced, the flocculation effect of a polyacrylamide flocculant is weakened, the viscosity of the concrete is reduced, and the working performance of the concrete containing the machine-made sand is improved. The invention prepares the flocculant functional auxiliary agent in the anti-machine-made sand by taking the natural beta-cyclodextrin as the raw material, has the advantages of environmental protection and low cost, and is beneficial to industrial use.
Detailed Description
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The experimental methods in the following examples are conventional methods unless otherwise specified. The test materials used in the examples described below, unless otherwise specified, were purchased from conventional biochemical reagent stores. In addition, unless specifically described otherwise, each term and process referred to in this embodiment is understood by those skilled in the art in light of the commonly recognized and conventional approaches in the art.
The flocculant functional auxiliary agent in the environment-friendly machine-made sand for concrete comprises an esterification modified substance of grafting organic acid groups on hydroxyl groups of beta-cyclodextrin.
The flocculant functional auxiliary agent in the environment-friendly machine-made sand for concrete disclosed by the invention is used for modifying the organic acid of the beta-cyclodextrin grafted organic acid group. Beta-cyclodextrin is a cyclic compound prepared by extracting starch by microbial enzyme action and formed by combining 7 glucose residues by beta-1, 4-glycosidic bond ， The anionic groups introduced by grafting the organic acid break the intermolecular hydrogen bonds of the cyclodextrin, so that the solubility of the cyclodextrin is improved; meanwhile, the polyacrylamide side chains are nested into cyclodextrin cavities, so that the intermolecular action of the polycarboxylate superplasticizer and the polyacrylamide is weakened, and the failure of the polycarboxylate superplasticizer is prevented. By means of the unique structure of the modified beta-cyclodextrin, the modified beta-cyclodextrin can be preferentially adsorbed on a polyacrylamide molecular chain, and meanwhile, the distance between the polycarboxylic acid molecules and the polyacrylamide molecules is increased, so that the probability that the polycarboxylic acid molecules are adsorbed and embedded by the polyacrylamide is reduced, flocculation of a polyacrylamide flocculant is weakened, the viscosity of concrete is reduced, and the working performance of concrete containing machine-made sand is improved.
Among them, the organic acid preferably includes maleic anhydride, sulfamic acid, gluconic acid or citric acid. More preferably, the esterification degree of substitution of the esterification modified product is 0.5 to 0.7 。 The substitution degree esterification modification can not only firmly adsorb the negatively charged carboxylic acid adsorption groups, but also ensure that the beta-cyclodextrin has better solubility, and can also prevent the cement strength from being reduced due to excessive carboxyl.
The invention also provides a preparation method of the flocculant functional auxiliary agent in the environment-friendly machine-made sand for concrete, which specifically comprises the following steps:
adding 10-20 parts of beta-cyclodextrin into a solvent for dissolution, adding 10-15 parts of organic acid and 1-5 parts of catalyst, heating, precipitating solid by using acetone, filtering the solid, drying, adding anhydrous methanol into the solid for dissolution and filtration, precipitating the product by using acetone, crystallizing by using distilled water acetone, and drying in vacuum to obtain the flocculant functional auxiliary agent in the environment-friendly anti-machine-made sand for concrete. The solvent can be N, N-Dimethylformamide (DMF), and the dosage of DMF is 9-11 times of the weight of beta-cyclodextrin. The catalyst adopts at least one of concentrated sulfuric acid, zinc oxide, stannous chloride and dibutyl tin dilaurate. The heating temperature is controlled to be 60-70 ℃ so as to improve the efficiency.
The above reagents are commercially available, and detailed descriptions of specific embodiments of the present invention are provided below.
Example 1
In a 100ml three-necked flask, 15 parts of β -CD was dissolved in a suitable amount of DMF, and then 10 parts of Maleic Anhydride (MA) and 1.5 parts of concentrated sulfuric acid were added thereto, followed by heating to 60℃and stirring at a low speed for 24 hours. Cooling to room temperature, precipitating beta-CD-CAS and unreacted beta-CD with acetone, filtering, drying, adding 60ml of absolute methanol, dissolving, filtering to remove a small amount of beta-CD, precipitating the product with acetone, repeatedly crystallizing with distilled water acetone for several times, and vacuum drying to obtain an organic acid group esterification modified product of beta-cyclodextrin, wherein the esterification substitution degree of the flocculant functional auxiliary agent in the anti-machine-made sand prepared by the embodiment is 0.6 through detection.
Example 2
In a 100ml three-neck flask, 10 parts of β -CD was dissolved in a proper amount of DMF, and then 10 parts of sulfamic Acid (ACS) and 2.5 parts of dibutyltin dilaurate were added, followed by heating to 65℃and stirring at a low speed for 20 hours. Cooling to room temperature, precipitating beta-CD-ACS and unreacted beta-CD with acetone, filtering, drying, adding 70ml of absolute methanol, dissolving, filtering to remove a small amount of beta-CD, precipitating the product with acetone, repeatedly crystallizing with distilled water acetone for several times, and vacuum drying to obtain an organic acid group esterification modified product of beta-cyclodextrin, wherein the esterification substitution degree of the flocculant functional auxiliary agent in the anti-machine-made sand prepared by the embodiment is 0.7 through detection.
Example 3
In a 100ml three-neck flask, 20 parts of beta-CD is added and dissolved in a proper amount of DMF, and then 10 parts of Citric Acid (CA) and 3 parts of stannous chloride are added, and the mixture is heated to 70 ℃ and stirred at a low speed for 30 hours. Cooling to room temperature, precipitating beta-CD-CA and unreacted beta-CD with acetone, filtering, drying, adding 80ml of absolute methanol, dissolving, filtering to remove a small amount of beta-CD, precipitating the product with acetone, repeatedly crystallizing with distilled water acetone for several times, and vacuum drying to obtain an organic acid group esterification modified product of beta-cyclodextrin, wherein the esterification substitution degree of the flocculant functional auxiliary agent in the anti-machine-made sand prepared by the embodiment is 0.4 through detection.
Example 4
In a 100ml three-necked flask, 20 parts of β -CD was dissolved in a suitable amount of DMF, and then 10 parts of gluconic acid (GLCA) and 5 parts of zinc oxide were added thereto, followed by heating to 70℃and stirring at a low speed for 35 hours. Cooling to room temperature, precipitating beta-CD-GLCA and unreacted beta-CD with acetone, filtering, drying, adding 80ml of absolute methanol, dissolving, filtering to remove a small amount of beta-CD, precipitating a product with acetone, repeatedly crystallizing with distilled water acetone for several times, and vacuum drying to obtain an organic acid group esterification modified product of beta-cyclodextrin, wherein the esterification substitution degree of a flocculant functional auxiliary agent in the anti-machine-made sand prepared by the embodiment is 0.5 through detection.
Comparative example 1
The comparative example was a commercially available product, model X007, sichuan road warfare building materials Co., ltd.
Comparative example 2
The comparative example uses beta-cyclodextrin which has not been modified with an organic acid.
The deflocculant prepared in each example and comparative example above was used in concrete experiments, and to simulate the effect of the polyacrylamide flocculant on the working performance of concrete, 0.15% of anionic polyacrylamide (molecular weight 1200 w) was added to the concrete mix water by the mass of water, and the initial and 1h expansion, slump and fall times of concrete were tested according to GB/T50080-2016 Standard for Performance test of common concrete mix. The cement used for preparing the concrete is P.O42.5 Emei cement, the fly ash is Ming Xiang I-grade fly ash, the water reducer is GK-3000 polycarboxylic acid high-performance water reducer (product of Shi Jia Shi Gao Jiu building materials Co., ltd.), the mixing amount of the water reducer is 1.0% of the mass of the cementing material, and the mixing amount of the deflocculant prepared in each example and comparative example is 0.05% of the mass of the cementing material. The concrete reference mix ratios are shown in Table 1, and the test results are shown in Table 2. The blank is concrete without deflocculant added.
TABLE 1 concrete mix ratio
Table 2 concrete test results
By comparing the test results of each example, comparative example 1 (commercial product), comparative example 2 and blank group, the flocculant functional auxiliary agent in the environment-friendly machine-made sand for concrete can effectively reduce the viscosity of the concrete, shorten the reverse extraction time and improve the working performance of the concrete.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited to the specific details of the above embodiments, and various simple modifications can be made to the technical solution of the present invention within the scope of the technical concept of the present invention, and all the simple modifications belong to the protection scope of the present invention.
In addition, the specific features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various possible combinations are not described further.
Claims (7)
1. The utility model provides a flocculant function auxiliary agent in environment-friendly machine-made sand for concrete which characterized in that: the flocculant functional auxiliary agent in the environment-friendly machine-made sand for concrete contains an esterification modifier grafted with an organic acid group on the hydroxyl of beta-cyclodextrin.
2. The functional auxiliary agent of flocculant in environment-friendly machine-made sand for concrete, which is characterized in that: the organic acid comprises maleic anhydride, sulfamic acid, gluconic acid or citric acid.
3. The functional auxiliary agent of flocculant in environment-friendly machine-made sand for concrete, which is characterized in that: the esterification degree of substitution of the esterification modifier is 0.5-0.7.
4. A method for preparing the flocculant functional additive in environment-friendly machine-made sand for concrete according to any one of claims 1-3, which is characterized by comprising the following steps: the method comprises the following steps:
adding beta-cyclodextrin into a solvent for dissolution, adding an organic acid and a catalyst, heating, precipitating a solid by using acetone, filtering the solid, drying, adding absolute methanol into the solid for dissolution and filtration, precipitating a product by using acetone, crystallizing by using distilled water acetone, and drying in vacuum to obtain the flocculant functional auxiliary agent in the environment-friendly machine-made resistant sand for concrete.
5. The method for preparing the flocculant functional auxiliary agent in the environment-friendly machine-made sand for concrete, which is characterized by comprising the following steps of: the solvent comprises N, N-dimethylformamide.
6. The method for preparing the flocculant functional auxiliary agent in the environment-friendly machine-made sand for concrete, according to claim 4, wherein the catalyst comprises at least one of concentrated sulfuric acid, zinc oxide, stannous chloride and dibutyl tin dilaurate.
7. The method for preparing the flocculant functional auxiliary agent in the environment-friendly machine-made sand for concrete according to any one of claims 4 to 6, which is characterized in that: the heating temperature is controlled between 60 ℃ and 70 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310887248.3A CN117143268A (en) | 2023-07-19 | 2023-07-19 | Functional auxiliary agent of flocculant in environment-friendly machine-made sand for concrete and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117342834A (en) * | 2023-12-06 | 2024-01-05 | 甘肃建投商品混凝土有限公司 | Machine-made sand concrete with high workability and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117342834A (en) * | 2023-12-06 | 2024-01-05 | 甘肃建投商品混凝土有限公司 | Machine-made sand concrete with high workability and preparation method thereof |
| CN117342834B (en) * | 2023-12-06 | 2024-02-09 | 甘肃建投商品混凝土有限公司 | Machine-made sand concrete with high workability and preparation method thereof |
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