CN109748532B - Alkali-free accelerator and preparation method and application thereof - Google Patents
Alkali-free accelerator and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title description 11
- 239000004375 Dextrin Substances 0.000 claims abstract description 58
- 229920001353 Dextrin Polymers 0.000 claims abstract description 58
- 235000019425 dextrin Nutrition 0.000 claims abstract description 58
- 238000011049 filling Methods 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 15
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 6
- 239000004005 microsphere Substances 0.000 claims description 28
- 239000004568 cement Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 13
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 12
- -1 alcohol amine Chemical class 0.000 claims description 12
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical group [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 229920000620 organic polymer Polymers 0.000 claims description 9
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 229920002401 polyacrylamide Polymers 0.000 claims description 7
- 239000003381 stabilizer Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims description 6
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 6
- 229920002472 Starch Polymers 0.000 claims description 5
- 235000019698 starch Nutrition 0.000 claims description 5
- 239000008107 starch Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 235000006408 oxalic acid Nutrition 0.000 claims description 4
- 229960004063 propylene glycol Drugs 0.000 claims description 4
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 3
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 3
- HVUMOYIDDBPOLL-XGKPLOKHSA-N [2-[(2r,3r,4s)-3,4-dihydroxyoxolan-2-yl]-2-hydroxyethyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XGKPLOKHSA-N 0.000 claims description 3
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 3
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 3
- 230000015271 coagulation Effects 0.000 claims description 3
- 238000005345 coagulation Methods 0.000 claims description 3
- 238000004132 cross linking Methods 0.000 claims description 3
- 230000000977 initiatory effect Effects 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 239000001630 malic acid Substances 0.000 claims description 3
- 235000011090 malic acid Nutrition 0.000 claims description 3
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 3
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 3
- 239000001384 succinic acid Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 2
- 235000011044 succinic acid Nutrition 0.000 claims description 2
- 238000006703 hydration reaction Methods 0.000 description 13
- 230000036571 hydration Effects 0.000 description 10
- 239000004567 concrete Substances 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000011575 calcium Substances 0.000 description 4
- 230000002035 prolonged effect Effects 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000378 calcium silicate Substances 0.000 description 3
- 229910052918 calcium silicate Inorganic materials 0.000 description 3
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 3
- 230000006835 compression Effects 0.000 description 3
- 238000007906 compression Methods 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000011378 shotcrete Substances 0.000 description 3
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 2
- 229940035437 1,3-propanediol Drugs 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 description 1
- 229910001635 magnesium fluoride Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000000176 sodium gluconate Substances 0.000 description 1
- 229940005574 sodium gluconate Drugs 0.000 description 1
- 235000012207 sodium gluconate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Abstract
The invention discloses a dextrin modified alkali-free setting accelerator which comprises a setting accelerator component, a setting regulator component, micromolecular alcohol and an auxiliary agent. The dextrin modified alkali-free setting accelerator is used for mine filling, the initial setting time of the dextrin modified alkali-free setting accelerator is 25-40 minutes, and the compressive strength of a filling material can reach about 0.2MPa after 8-10 hours.
Description
Technical Field
The invention belongs to the technical field of concrete admixtures, and particularly relates to an alkali-free accelerator as well as a preparation method and application thereof.
Background
The accelerator is a concrete admixture which rapidly sets and hardens cement or concrete. The method has the main effects of increasing the primary spraying thickness of the sprayed concrete, shortening the interval between secondary spraying, and simultaneously improving the early strength of the concrete so as to provide support resistance in time, and is widely applied to the engineering of modern underground engineering, mine engineering, leakage stoppage, emergency rescue and the like at present. The alkali-free accelerator has low corrosivity to human body, high early strength and the like
The prior publications and patents are mainly focused on improving the performance of the alkali-free setting accelerator and the adaptability of cement. The advantages of the accelerator are the fashion trend and the future development direction of the accelerator.
For example, patent CN200610098296.0 discloses a liquid alkali-free accelerator for shotcrete, which can improve the applicability of the accelerator to cement, provide excellent performance even for medium-heat cement, and meet the construction requirements of shotcrete.
Patent CN201510912656.5 discloses an alkali-free liquid quick-setting agent and a preparation method thereof, wherein magnesium fluoride is used for remarkably improving the quick-setting effect of the product and the compressive strength of concrete.
The cemented filling mainly uses cement as a gel curing material, forms low-grade concrete by stirring with filling aggregate, and conveys the concrete to an underground stope to construct a working floor or a rock stratum supporting artificial ore pillar and the like. The water consumption is generally very high, the performance requirements of the filling material are that the initial setting is achieved within 30 minutes, the compressive strength reaches 0.2MPa within 8-10 hours, and the compressive strength reaches 10-15MPa within 28 days.
However, the conventional alkali-free setting accelerator has relatively short setting time (initial setting time is less than or equal to 5 minutes, and final setting time is less than or equal to 12 minutes), and cannot be directly applied to special fields such as mine filling, and the like, so that the conventional product needs to be modified and optimized.
Disclosure of Invention
The invention provides a dextrin modified alkali-free accelerator and a preparation method and application thereof, aiming at solving the problem that the existing alkali-free accelerator cannot be applied to the fields of mine filling and the like.
The dextrin modified alkali-free setting accelerator is used for mine filling, the initial setting time of the dextrin modified alkali-free setting accelerator is 25-40 minutes, and the compression strength of a filling material can reach about 0.2MPa after 8-10 hours.
The water-cement ratio of the filling material used for filling the mine is very large and reaches 2.67.
The quick-setting component is aluminum sulfate and alcohol amine;
the alcohol amine is one of diethanolamine, triethanolamine or N, N-dimethylethanolamine.
The coagulation regulating component is dextrin microspheres and is prepared by the following method:
the coagulation regulating component is dextrin microspheres and is prepared by the following method: adding soluble starch into water, heating and stirring until the starch is transparent, and preparing into a 20wt% solution; sequentially adding N, N' -methylene bisacrylamide, ammonium persulfate and sodium bisulfite under the stirring state, wherein the adding interval is not more than 10 minutes; adding Span60 and cyclohexane into a four-neck flask, and heating to 50 ℃; dropwise adding the water phase into the oil phase, finishing dropping for 15min, and initiating polymerization crosslinking for 4 h; washing the reacted dextrin solution with ethyl acetate, ethanol and acetone sequentially for three times, drying in an oven at 60 ℃ for 24 hours, and screening to obtain the 150-200-mesh dextrin microspheres.
The small molecular alcohol is one of 1,2 propylene glycol, 1,3 propylene glycol or glycerol.
The invention introduces dextrin micro-particlesThe ball modifies the alkali-free setting accelerator, a large amount of hydroxyl is adsorbed on the surface of cement to form hydrogen bonds, further hydration of the cement is prevented, the initial setting time of slurry is prolonged to about 30 minutes, and simultaneously, the early dextrin microspheres for hydration can embed partial Ca2+Ions, dextrin microspheres dissolve automatically as the cement hydration progresses, and Ca embedded in the dextrin microspheres2+Ions are also gradually released to promote the generation of hydration products such as post-hydration calcium silicate C-S-H gel and the like, so that the compression strength of the filling material reaches 0.2MPa in 8-10 hours and 10-15MPa in 28 days.
The proper amount of small molecular alcohol can wet the aluminum sulfate solid particles, reduce the interface energy, ensure that the particles are easy to disperse and improve the dispersion stability. In addition, the small molecular alcohol can reduce the freezing point of the alkali-free accelerator aqueous solution, so that the frost resistance of the product is improved.
The auxiliary agent is a dispersing agent or a surfactant and has the function of enabling the dextrin microspheres and the quick-setting component to be stored stably without layering.
The addition amount of the existing alkali-free setting accelerator is reduced or the retarder is added, so that the initial setting time of the clean slurry can be prolonged to 30 minutes, but the final setting of the slurry can not be achieved after 8-10 hours.
The quick-setting admixture can adjust the initial setting time of the filling material to be 25-40 minutes, the final setting time to be 40-50 minutes, and the compressive strength of the filling material can reach 0.2MPa after 8-10 hours and 10-15MPa after 28 days.
The auxiliary agent comprises a stabilizer and an organic polymer
The stabilizer is one of lactic acid, oxalic acid, malic acid or succinic acid.
The organic polymer is nonionic polyacrylamide, and the molecular weight of the organic polymer is 300-500 ten thousand.
The dextrin modified alkali-free accelerator comprises the following components in parts by weight:
the preparation method of the dextrin modified alkali-free accelerator comprises the following steps:
(1) mixing aluminum sulfate, alcohol amine and water, heating to 60-80 ℃, and reacting for 0.5-2 hours;
(2) cooling to 40 ℃, adding a stabilizer and micromolecular alcohol, and continuing to react for 10-30 minutes;
(3) and cooling to room temperature, adding dextrin microspheres and an organic polymer, and treating for 5-15 minutes by using an ultrasonic cell disruption instrument to obtain the dextrin modified alkali-free accelerator.
The frequency of the ultrasonic cell disruptor is 20KHz, and the output power is 200-300W.
The invention also provides an application method of the dextrin modified alkali-free accelerator, and the dextrin modified alkali-free accelerator is used in the field of mine filling, and the mixing amount of the dextrin modified alkali-free accelerator is 6-10 wt% of the cement dosage in a mine filling material.
Has the advantages that: the dextrin modified alkali-free accelerator provided by the invention can be applied to special fields such as mine filling and the like. The alkali-free setting accelerator is modified by introducing dextrin microspheres, a large number of hydroxyl groups are adsorbed on the surface of cement to form hydrogen bonds, so that the further hydration of the cement is prevented, the initial setting time of slurry is prolonged to about 30 minutes, and meanwhile, part of Ca can be embedded in the early dextrin microspheres after hydration2+Ions, dextrin microspheres dissolve automatically as the cement hydration progresses, and Ca embedded in the dextrin microspheres2+Ions are also gradually released to promote the generation of hydration products such as post-hydration calcium silicate C-S-H gel and the like, so that the compression strength of the filling material reaches 0.2MPa in 8-10 hours and 10-15MPa in 28 days.
Detailed Description
In order to better understand the invention, the following examples are given for further illustration of the invention, but the invention is not limited to the scope of the examples.
Firstly, preparing dextrin microspheres, adding 100g of soluble starch into water, heating and stirring until the mixture is transparent, and preparing into a 20wt% solution; sequentially adding 0.1g of N, N' -methylene bisacrylamide, 1.5g of ammonium persulfate and 0.3g of sodium bisulfite under the stirring state, wherein the adding interval is not more than 10 minutes; adding 1g of Span60 and 400g of cyclohexane into a four-neck flask, and heating to 50 ℃; dropwise adding the water phase into the oil phase, finishing dropping for 15min, and initiating polymerization crosslinking for 4 h; washing the reacted dextrin solution with ethyl acetate, ethanol and acetone sequentially for three times, drying in an oven at 60 ℃ for 24 hours, and screening to obtain 150-200-mesh dextrin microspheres.
Example 1
The preparation method of the dextrin modified alkali-free accelerator comprises the following steps:
(1) mixing 30g of aluminum sulfate, 2g of alcohol amine and 50g of water, heating to 60 ℃, and reacting for 2 hours;
(2) after the temperature is reduced to 40 ℃, 0.5g of lactic acid and 1g of 1, 2-propylene glycol are added, and the reaction is continued for 10 minutes;
(3) and cooling to room temperature, adding 5g of dextrin microspheres and 0.1g of polyacrylamide, and treating for 5 minutes by using an ultrasonic cell disruptor under the conditions that the frequency is 20KHz and the output power is 200W to obtain the dextrin modified alkali-free accelerator.
Example 2
The preparation method of the dextrin modified alkali-free accelerator comprises the following steps:
(1) mixing 40g of aluminum sulfate, 6g of alcohol amine and 40g of water, heating to 80 ℃, and reacting for 0.5 hour;
(2) cooling to 40 ℃, adding 2.5g of oxalic acid and 4g of 1, 3-propanediol, and continuing to react for 30 minutes;
(3) and cooling to room temperature, adding 10g of dextrin microspheres and 0.5g of polyacrylamide, and treating for 15 minutes by using an ultrasonic cell disruptor under the conditions that the frequency is 20KHz and the output power is 300W to obtain the dextrin modified alkali-free accelerator.
Example 3
The preparation method of the dextrin modified alkali-free accelerator comprises the following steps:
(1) mixing 35g of aluminum sulfate, 3g of alcohol amine and 50g of water, heating to 60 ℃, and reacting for 2 hours;
(2) cooling to 40 ℃, adding 1.5g of malic acid and 1g of 1, 2-propanetriol, and continuing to react for 15 minutes;
(3) and cooling to room temperature, adding 8g of dextrin microspheres and 0.1g of polyacrylamide, and treating for 10 minutes by using an ultrasonic cell disruptor under the frequency of 20KHz and the output power of 200W to obtain the dextrin modified alkali-free accelerator.
Example 4
The preparation method of the dextrin modified alkali-free accelerator comprises the following steps:
(1) mixing 30g of aluminum sulfate, 5g of alcohol amine and 45g of water, heating to 70 ℃, and reacting for 1 hour;
(2) cooling to 40 ℃, adding 0.5g of succinic acid and 3g of 1, 2-propylene glycol, and continuing to react for 15 minutes;
(3) and cooling to room temperature, adding 5g of dextrin microspheres and 0.3g of polyacrylamide, and treating for 8 minutes by using an ultrasonic cell disruptor under the conditions that the frequency is 20KHz and the output power is 250W to obtain the dextrin modified alkali-free accelerator.
Example 5
The preparation method of the dextrin modified alkali-free accelerator comprises the following steps:
(1) mixing 40g of aluminum sulfate, 5g of alcohol amine and 50g of water, heating to 70 ℃, and reacting for 2 hours;
(2) cooling to 40 ℃, adding 0.5g of oxalic acid and 1g of 1, 3-propanediol, and continuing to react for 10 minutes;
(3) and cooling to room temperature, adding 7g of dextrin microspheres and 0.2g of polyacrylamide, and treating for 5 minutes by using an ultrasonic cell disruptor under the conditions that the frequency is 20KHz and the output power is 250W to obtain the dextrin modified alkali-free accelerator.
Comparative example 1
An alkali-free accelerator was prepared in example 1 with reference to patent CN 200610098296.0.
Comparative example 2
An alkali-free accelerator was prepared by adding 1 wt% of sodium gluconate based on comparative example 1.
The alkali-free accelerators obtained in examples 1 to 5 and comparative examples 1 to 3 were tested for their performance and the results are shown in Table 1.
The mixing proportion of the filling material for testing is 120kg/m of the reference cement3320kg/m of water31500kg/m of tailing slag3. The test method of the setting time and the compressive strength refers to the Chinese building material industry standard JC 477-2005.
Table 1 results of performance test of examples and comparative examples
As can be seen from table 1: the conventional alkali-free setting accelerator has too short setting time to meet the actual construction requirement; although the combination of reducing the conventional alkali-free setting accelerator and introducing the retarder can delay the initial setting time, the filling material has no compressive strength after 10 hours. The dextrin modified alkali-free accelerator provided by the invention is modified by introducing dextrin microspheres, a large amount of hydroxyl is adsorbed on the surface of cement to form hydrogen bonds, so that the further hydration of the cement is prevented, and the initial setting time of a filling material is prolonged; at the same time, the early dextrin microspheres can embed part of Ca2+Ions, dextrin microspheres dissolve automatically as the cement hydration progresses, and Ca embedded in the dextrin microspheres2+Ions are also gradually released, so that the generation of hydration products such as calcium silicate C-S-H gel and the like in the later stage is promoted, and the later-stage compressive strength of the filling material is ensured.
Claims (3)
1. A dextrin modified alkali-free setting accelerator is characterized by comprising a setting accelerator component, a setting regulator component, micromolecular alcohol and an auxiliary agent;
the quick-setting component is aluminum sulfate and alcohol amine;
the alcohol amine is one of diethanolamine, triethanolamine or N, N-dimethylethanolamine;
the coagulation regulating component is dextrin microspheres and is prepared by the following method: adding soluble starch into water, heating and stirring until the starch is transparent, and preparing into a 20wt% solution; sequentially adding N, N' -methylene bisacrylamide, ammonium persulfate and sodium bisulfite under the stirring state, wherein the adding interval is not more than 10 minutes; adding Span60 and cyclohexane into a four-neck flask, and heating to 50 ℃; dropwise adding the water phase into the oil phase, finishing dropping for 15min, and initiating polymerization crosslinking for 4 h; washing the reacted dextrin solution with ethyl acetate, ethanol and acetone sequentially for three times, drying in a 60 ℃ drying oven for 24 hours, and screening to obtain 150-200-mesh dextrin microspheres;
the small molecular alcohol is one of 1,2 propylene glycol, 1,3 propylene glycol or glycerol;
the auxiliary agent enables the dextrin microspheres and the quick-setting component to be stored stably without layering;
the auxiliary agent comprises a stabilizing agent and an organic polymer,
the stabilizer is one of lactic acid, oxalic acid, malic acid or succinic acid;
the organic polymer is nonionic polyacrylamide, and the molecular weight of the organic polymer is 300-500 ten thousand;
the components are calculated by weight fraction as follows:
30 to 40 percent of aluminum sulfate,
2 to 6 percent of alcohol amine,
5 to 10 percent of dextrin microspheres,
1-4% of small molecular alcohol,
0.5 to 2.5 percent of stabilizer,
0.1 to 0.5% of an organic polymer,
the balance of water.
2. The method for preparing the dextrin-modified alkali-free accelerator according to claim 1, characterized by comprising the steps of:
(1) mixing aluminum sulfate, alcohol amine and water, heating to 60-80 ℃, and reacting for 0.5-2 hours;
(2) cooling to 40 ℃, adding a stabilizer and micromolecular alcohol, and continuing to react for 10-30 minutes;
(3) cooling to room temperature, adding dextrin microspheres and an organic polymer, and treating for 5-15 minutes by using an ultrasonic cell disruption instrument to obtain a dextrin modified alkali-free accelerator;
the frequency of the ultrasonic cell disruptor is 20KHz, and the output power is 200-300W.
3. The application method of the dextrin-modified alkali-free accelerator as claimed in claim 1, wherein the dextrin-modified alkali-free accelerator is used in the field of mine filling, and the mixing amount of the dextrin-modified alkali-free accelerator is 6-10 wt% of the cement amount in a mine filling material.
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| CN111499248A (en) * | 2020-05-22 | 2020-08-07 | 山西海裕隆建材有限公司 | High-performance alkali-free liquid accelerator special for moderate-heat low-heat cement and preparation method thereof |
| CN112608061B (en) * | 2020-12-18 | 2022-08-09 | 徐州中矿大贝克福尔科技股份有限公司 | Accelerating agent composition for coal mine paste filling and preparation method and application thereof |
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Denomination of invention: A alkali free rapid setting agent and its preparation method and application Effective date of registration: 20231228 Granted publication date: 20220318 Pledgee: Bank of Communications Ltd. Jiangsu branch Pledgor: SOBUTE NEW MATERIALS Co.,Ltd. Registration number: Y2023980074584 |
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