CN113480221A - Liquid alkali-free accelerator and preparation method and application thereof - Google Patents
Liquid alkali-free accelerator and preparation method and application thereof Download PDFInfo
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- CN113480221A CN113480221A CN202110882968.1A CN202110882968A CN113480221A CN 113480221 A CN113480221 A CN 113480221A CN 202110882968 A CN202110882968 A CN 202110882968A CN 113480221 A CN113480221 A CN 113480221A
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- 239000007788 liquid Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000004568 cement Substances 0.000 claims abstract description 43
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [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 abstract description 34
- 229920001732 Lignosulfonate Polymers 0.000 claims abstract description 23
- GNHOJBNSNUXZQA-UHFFFAOYSA-J potassium aluminium sulfate dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GNHOJBNSNUXZQA-UHFFFAOYSA-J 0.000 claims abstract description 21
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 17
- 239000011734 sodium Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000003857 carboxamides Chemical class 0.000 claims abstract description 10
- YYPNJNDODFVZLE-UHFFFAOYSA-N 3-methylbut-2-enoic acid Chemical compound CC(C)=CC(O)=O YYPNJNDODFVZLE-UHFFFAOYSA-N 0.000 claims abstract description 8
- CERQOIWHTDAKMF-UHFFFAOYSA-N alpha-methacrylic acid Natural products CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 63
- 239000011259 mixed solution Substances 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 12
- UIERETOOQGIECD-ONEGZZNKSA-N tiglic acid Chemical compound C\C=C(/C)C(O)=O UIERETOOQGIECD-ONEGZZNKSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 7
- 229920005906 polyester polyol Polymers 0.000 claims description 7
- 229920005862 polyol Polymers 0.000 claims description 7
- 150000003077 polyols Chemical class 0.000 claims description 7
- 238000005303 weighing Methods 0.000 claims description 7
- HSFQBFMEWSTNOW-UHFFFAOYSA-N sodium;carbanide Chemical group [CH3-].[Na+] HSFQBFMEWSTNOW-UHFFFAOYSA-N 0.000 claims description 6
- AOCWQPKHSMJWPL-UHFFFAOYSA-N 3-methylpyrrolidin-2-one Chemical compound CC1CCNC1=O AOCWQPKHSMJWPL-UHFFFAOYSA-N 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- DKFCNIGGENJIJN-UHFFFAOYSA-L aluminum;iron(2+);sulfate Chemical compound [Al+3].[Fe+2].[O-]S([O-])(=O)=O DKFCNIGGENJIJN-UHFFFAOYSA-L 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 229920000570 polyether Polymers 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000004570 mortar (masonry) Substances 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 7
- 238000002156 mixing Methods 0.000 abstract description 6
- 239000004566 building material Substances 0.000 abstract description 2
- 230000014759 maintenance of location Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 10
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 8
- -1 aluminum ions Chemical class 0.000 description 8
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical compound ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 7
- 239000004567 concrete Substances 0.000 description 7
- 238000006703 hydration reaction Methods 0.000 description 7
- FGSUUFDRDVJCLT-UHFFFAOYSA-N 3-methylazepan-2-one Chemical compound CC1CCCCNC1=O FGSUUFDRDVJCLT-UHFFFAOYSA-N 0.000 description 6
- 239000002202 Polyethylene glycol Substances 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 230000036571 hydration Effects 0.000 description 6
- 229920001223 polyethylene glycol Polymers 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- NAEDWKNFXVUORY-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)propane-1,3-diol;hexanedioic acid Chemical compound OCC(CO)(CO)CO.OC(=O)CCCCC(O)=O NAEDWKNFXVUORY-UHFFFAOYSA-N 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-L adipate(2-) Chemical compound [O-]C(=O)CCCCC([O-])=O WNLRTRBMVRJNCN-UHFFFAOYSA-L 0.000 description 3
- QKZIVVMOMKTVIK-UHFFFAOYSA-M anilinomethanesulfonate Chemical compound [O-]S(=O)(=O)CNC1=CC=CC=C1 QKZIVVMOMKTVIK-UHFFFAOYSA-M 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011378 shotcrete Substances 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- OLQFXOWPTQTLDP-UHFFFAOYSA-N 2-(2-hydroxyethoxy)ethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOCCO OLQFXOWPTQTLDP-UHFFFAOYSA-N 0.000 description 2
- KYRZZPALUVQDRB-UHFFFAOYSA-N 2-methyl-1,4-dioxocane-5,8-dione Chemical compound CC1COC(=O)CCC(=O)O1 KYRZZPALUVQDRB-UHFFFAOYSA-N 0.000 description 2
- WPECQIDVVNFTFV-UHFFFAOYSA-N OS(=O)(=O)C[Na] Chemical compound OS(=O)(=O)C[Na] WPECQIDVVNFTFV-UHFFFAOYSA-N 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 229920005552 sodium lignosulfonate Polymers 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- PLTOXCBCXNLMME-UHFFFAOYSA-N OCC(C)(CO)C.C(CCCC(=O)O)(=O)O Chemical compound OCC(C)(CO)C.C(CCCC(=O)O)(=O)O PLTOXCBCXNLMME-UHFFFAOYSA-N 0.000 description 1
- 229910001294 Reinforcing steel Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000003487 anti-permeability effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000011083 cement mortar Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000004574 high-performance concrete Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000006072 paste Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920000909 polytetrahydrofuran Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- C04B2103/10—Accelerators; Activators
- C04B2103/12—Set accelerators
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to the field of building materials, in particular to a liquid alkali-free accelerator, a preparation method and an application thereof, wherein the liquid alkali-free accelerator comprises the following components in percentage by weight: 20-50% of aluminum sulfate, 10-30% of aluminum potassium sulfate dodecahydrate, 5-10% of polyhydric alcohol, 1-5% of organic amide, 1-5% of sodium alkyl lignosulfonate and 3-5% of methyl crotonic acid, and the solvent is water, wherein the alkali-free liquid setting accelerator prepared by the invention has the advantages that the initial setting time of cement paste is 2-4 min and the final setting time is 6-8 min under the mixing amount of 2-8 wt%, the compressive strength of 1d of the mortar reaches 12-16 MPa, the compressive strength ratio of 28d is more than 105%, and the retention rate of 90d compressive strength is more than 120%, which are all superior to the national standard. The whole preparation process is safe and reliable, simple and convenient to operate, safe to environment and wide in application prospect in the cement related field.
Description
Technical Field
The invention relates to the field of building materials, in particular to a liquid alkali-free accelerator and a preparation method and application thereof.
Background
As an important component material of the sprayed concrete wet spraying process, the liquid accelerator has the characteristics of remarkably reducing the sliding of a sprayed layer in the spraying construction process, improving the thickness of a primary sprayed layer, accelerating the setting and hardening rate of the sprayed concrete and the like.
The liquid setting accelerators on the market of China currently have two types: one is an alkali accelerating agent and the other is an alkali-free accelerating agent. The alkali accelerating agent has the advantages of good long-term storage stability, low mixing amount, good adaptability and the like, but is gradually replaced by a novel liquid alkali-free accelerating agent due to high alkali content (up to more than 20 wt%), strong corrosivity on operators, large concrete shrinkage and large later strength loss (about 30% strength loss at 28 days). The liquid alkali-free accelerator does not contain chloride ions, does not corrode reinforcing steel bars, does not pollute the environment and does not harm the bodies of operators. The high-performance liquid alkali-free accelerator is doped into the sprayed cement paste, cement mortar and concrete, so that the setting and hardening speed of the cement can be accelerated, the early strength is improved, the influence on the later strength is small, even is not reduced, the cohesiveness and the bonding strength of the concrete and the mortar are greatly improved, the reduction of the rebound rate reaches over 80 percent, the material loss caused by the rebound is effectively reduced, and the economic benefit is improved. As the rebound rate is greatly reduced, the alkaline cement dust polluting the air and injuring the human body is greatly reduced, the environment is protected and the construction progress is accelerated. The liquid alkali-free accelerator also has the effects of micro-expansion, shrinkage reduction and crack resistance, greatly improves the anti-permeability and waterproof performance, has the corrosion-resistant and corrosion-resistant functions, and improves the corrosion resistance coefficient by more than 50 percent compared with the common accelerator. In environmental engineering, high-performance liquid alkali-free setting accelerators are the preferred materials for spraying high-performance concrete, alkali aggregate reactive concrete and durable concrete, so that the liquid alkali-free setting accelerators tend to replace the alkali setting accelerators.
At present, the liquid alkali-free accelerator is most applied to aluminum sulfate series. The main component of the aluminum sulfate accelerating agent is aluminum sulfate. The aluminum ions can react with the cement hydration products to cause the cement paste to be coagulated, thereby achieving the quick setting effect. Aluminum sulfate has good effect as a coagulation accelerating component, the coagulation accelerating effect of the liquid accelerator is improved, when saturated solution of aluminum sulfate is used as the liquid accelerator, the requirement can be met when the doping amount reaches 12%, but the excessively high doping amount can lead the accelerator to be non-uniform in dispersion and has certain harm to the environment, thereby reducing the applicability of the accelerator.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a liquid alkali-free accelerator, which is expected to solve the technical problems that the accelerator is not uniformly dispersed, has great environmental hazard, expensive raw materials, difficult popularization in field production and the like due to high mixing amount of similar accelerators in the prior art.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a liquid alkali-free accelerator comprises the following components in percentage by weight: 20 to 50 percent of aluminum sulfate, 10 to 30 percent of aluminum potassium sulfate dodecahydrate, 5 to 10 percent of polyalcohol, 1 to 5 percent of organic amide, 1 to 5 percent of sodium alkyl lignosulfonate and 3 to 5 percent of methyl crotonic acid, and the solvent is water.
Compared with the prior art, the liquid alkali-free accelerator provided by the invention has the following advantages:
the main quick-setting function of the invention is aluminum salt, and aluminum ions generated by aluminum sulfate can react with hydration products in cement to achieve the quick-setting effect; the potassium aluminum sulfate dodecahydrate is used as a system to introduce additional active aluminum ions, so that the obvious change of pH after the cement is hydrated is buffered, the pH value of the system is stabilized, the strength of a hydrated product is increased, the coagulation and hydration speed of the cement is improved, the quick setting effect can be obviously improved, and the compressive strength of the early cement is enhanced; by introducing organic amide and polyhydric alcohol, the solubility of aluminum sulfate and aluminum potassium sulfate dodecahydrate is effectively enhanced, a high-activity aluminum ion crosslinking system is further obtained, and the hydration rate and the early strength of cement are greatly improved; the methyl butenoic acid is used for controlling the pH value of the system, improving the stability of the accelerator and accelerating the hydration rate of the cement; the sodium alkyl lignosulfonate can greatly improve the fluidity and plasticity of cement, reduce harmful pores and enhance the compressive strength.
Preferably, the polyol is at least one of a polyester polyol or a polyether polyol.
The polyester polyol is one or two of polyethylene glycol adipate diol, polypropylene glycol succinate diol, neopentyl glycol glutarate triol, diethylene glycol methacrylate triol or pentaerythritol adipate triol.
The polyether polyol is one or two of polyethylene glycol, polypropylene glycol or polytetrahydrofuran.
Through the polarization of hydroxyl in the polyhydric alcohol, the agglomeration of cement can be reduced, and the dispersibility and the solubility of aluminum ions in the cement are improved, so that the aluminum sulfate and the aluminum potassium sulfate dodecahydrate are mixed and distributed more uniformly, the hydration of the cement is accelerated, the early strength of the cement is improved, and particularly the 1d strength of the cement can be improved.
Preferably, the organic amide is selected from at least one of methylbutyrolactam or methylhexalactam.
Preferably, the sodium alkyl lignosulfonate is at least one of sodium methyl lignosulfonate and sodium sulfomethyl lignosulfonate.
Preferably, the source of aluminum sulfate is one of industrial aluminum sulfate or non-iron aluminum sulfate, and the aluminum content in the industrial aluminum sulfate or the non-iron aluminum sulfate is Al2O3Measured on Al2O3The content is more than or equal to 15wt percent, and the Fe content is less than or equal to 0.5wt percent.
When Al is present2O3When the content is less than 15 wt% of the total weight of the aluminum sulfate, the effective components are insufficient, and the quick setting effect is deteriorated, and when the content of Fe is more than 0.5 wt% of the total weight of the aluminum sulfate, unnecessary impurity components are introduced, and the chelating effect with other components in the quick setting agent is generated, so that the quick setting effect is influenced.
The invention also provides a preparation process of the liquid alkali-free accelerator, which specifically comprises the following steps:
step A, weighing all components according to the weight percentage of the components of the liquid alkali-free accelerator for later use;
b, adding the aluminum potassium sulfate dodecahydrate into the water, heating to 60-80 ℃, stirring for dissolving, then adding the aluminum sulfate, heating to 60-80 ℃, and continuously stirring for dissolving to obtain a first mixed solution;
step C, adding the organic amide into the first mixed solution, uniformly stirring, adding the polyol, and uniformly stirring at 50-70 ℃ to obtain a second mixed solution;
and D, adding the sodium alkyl lignin sulfonate into the second mixed solution, uniformly stirring, adding the methyl butenoic acid, regulating the pH to 5-6 under stirring at 50-60 ℃, and cooling to obtain the liquid alkali-free accelerator.
The liquid alkali-free accelerator prepared in the whole preparation process is safe and reliable, simple and convenient to operate and safe to the environment, has good applicability to different types of cement, shortens the initial setting time and the final setting time of cement paste, improves the strength of mortar, and has wide application prospects in the fields related to cement.
Preferably, in the step B, the stirring speed of adding the aluminum potassium sulfate dodecahydrate is 250-350 r/min, and the stirring time is 30-60 min.
Preferably, in the step B, the stirring speed of the aluminum sulfate is 450-550 r/min, and the stirring time is 30-60 min.
Preferably, in the step C, the stirring speed for adding the organic amide is 260-300r/min, and the stirring time is 20-40 min.
Preferably, in the step C, the stirring speed of adding the polyhydric alcohol is 350-450 r/min, and the stirring time is 60-120 min.
Preferably, in the step D, the adding of the sodium alkyl lignosulfonate is carried out at a stirring speed of 350-450 r/min for 20-30 min.
Preferably, in the step D, the stirring speed of the methyl butenoic acid is 150-250 r/min, and the stirring time is 30-60 min.
The invention also provides application of the liquid alkali-free accelerator, wherein the liquid alkali-free accelerator is added into cement, and the adding amount is 2-8 wt% of the using amount of the cement.
According to the experimental conditions of GB/T35159 and 2017, the accelerator provided by the invention has the advantages that the initial setting time of cement paste is 2-4 min and the final setting time is 6-8 min under a small mixing amount (2-8 wt%).
According to the experimental conditions of GB/T35159 and 2017, the compressive strength of the mortar at 1d can reach 12-16 MPa, the compressive strength ratio at 28d is more than 105%, and the retention rate at 90d is more than 120%, which are all superior to the national standard.
The liquid accelerator can be used as a concrete additive to be added into cement, can also be used for preparing cement products, such as cement pantile, tile, cement binder, cement floor brick, cement pipeline, cement decorative board, inner wall cement guard board, cement sandwich board, cement shaving board and other cement products, can accelerate the hydration reaction of cement, shorten the early-stage setting time, improve the strength and performance of concrete or cement products, and has the advantage of no substitution in the application field.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1:
a liquid alkali-free accelerator comprises the following components in percentage by weight: 40% of aluminum sulfate, 20% of aluminum potassium sulfate dodecahydrate, 8% of polyethylene glycol adipate, 3% of methyl butyl lactam, 5% of sodium sulfomethyl lignin sulfonate, 3% of methyl crotonic acid and 21% of water.
The preparation process specifically comprises the following steps:
a, weighing the components according to the weight percentage of the components of the liquid alkali-free accelerator for later use;
b, adding aluminum potassium sulfate dodecahydrate into the water, heating to 80 ℃, stirring at the rotating speed of 300r/min for 60min, adding aluminum sulfate, and continuously stirring at the rotating speed of 500r/min at 80 ℃ for 60min to obtain a first mixed solution;
step C, adding methylbutyrolactam into the first mixed solution, stirring at the rotating speed of 300r/min for 30min, adding polydiethylene glycol adipate, and stirring at the rotating speed of 400r/min at 70 ℃ for 120min to obtain a second mixed solution;
and D, adding sodium sulfomethyl lignin sulfonate into the second mixed solution, stirring at the rotating speed of 400r/min for 30min, adding methyl butenoic acid, stirring at the rotating speed of 200r/min for 60min at the temperature of 50 ℃, adjusting the pH to be 5, and cooling to 30 ℃ to obtain the liquid alkali-free accelerator.
Example 2:
a liquid alkali-free accelerator comprises the following components in percentage by weight: 30% of aluminum sulfate, 15% of aluminum potassium sulfate dodecahydrate, 5% of poly (propylene succinate) glycol, 3% of methyl caprolactam, 3% of sulfomethyl sodium lignosulfonate, 4% of methyl crotonic acid and 40% of water.
The preparation process specifically comprises the following steps:
a, weighing the components according to the weight percentage of the components of the liquid alkali-free accelerator for later use;
step B, firstly adding aluminum potassium sulfate dodecahydrate into the water, heating to 75 ℃, stirring at the rotating speed of 300r/min for 55min, then adding aluminum sulfate, and continuously stirring at the rotating speed of 500r/min at 75 ℃ for 40min to obtain a first mixed solution;
step C, adding methyl caprolactam into the first mixed solution, stirring at the rotating speed of 280r/min for 30min, adding poly (propylene succinate) glycol, and stirring at the rotating speed of 400r/min at 60 ℃ for 80min to obtain a second mixed solution;
and D, adding sodium sulfomethyl lignin sulfonate into the second mixed solution, stirring at the rotating speed of 400r/min for 30min, adding methyl butenoic acid, stirring at the rotating speed of 200r/min for 40min at the temperature of 55 ℃, adjusting the pH value to be 6, and cooling to 30 ℃ to obtain the liquid alkali-free accelerator.
Example 3:
a liquid alkali-free accelerator comprises the following components in percentage by weight: 50% of aluminum sulfate, 10% of aluminum potassium sulfate dodecahydrate, 5% of polyester polyol, 2% of methyl caprolactam, 4% of sodium methyl lignin sulfonate, 3% of methyl crotonic acid and 26% of water, wherein the polyester polyol is diethylene glycol methacrylate triol and poly pentaerythritol adipate triol, and the mass ratio of the polyester polyol is 1: 1.
The preparation process specifically comprises the following steps:
a, weighing the components according to the weight percentage of the components of the liquid alkali-free accelerator for later use;
step B, firstly adding aluminum potassium sulfate dodecahydrate into the water, heating to 65 ℃, stirring at the rotating speed of 300r/min for 35min, then adding aluminum sulfate, heating to 75 ℃, and stirring at the rotating speed of 500r/min for 35min to obtain a first mixed solution;
step C, adding methyl caprolactam into the first mixed solution, stirring for 30min at the rotating speed of 290r/min, adding polyester polyol, and stirring for 80min at the rotating speed of 400r/min at 65 ℃ to obtain a second mixed solution;
and D, adding sodium methyl lignin sulfonate into the second mixed solution, stirring at the rotating speed of 400r/min for 20min, adding methyl butenoic acid, stirring at the rotating speed of 200r/min for 40min at the temperature of 55 ℃, adjusting the pH value to be 6, and cooling to 40 ℃ to obtain the liquid alkali-free accelerator.
Example 4:
a liquid alkali-free accelerator comprises the following components in percentage by weight: 35% of aluminum sulfate, 30% of aluminum potassium sulfate dodecahydrate, 10% of polyethylene glycol, 4% of methyl caprolactam, 5% of sodium methyl lignin sulfonate, 3% of methyl crotonic acid and 13% of water.
The preparation process specifically comprises the following steps:
a, weighing the components according to the weight percentage of the components of the liquid alkali-free accelerator for later use;
b, adding aluminum potassium sulfate dodecahydrate into the water, heating to 60 ℃, stirring at the rotating speed of 300r/min for 30min, adding aluminum sulfate, heating to 75 ℃, and stirring at the rotating speed of 500r/min for 45min to obtain a first mixed solution;
step C, adding methyl caprolactam into the first mixed solution, stirring at the rotating speed of 260r/min for 30min, adding polyethylene glycol, and stirring at the rotating speed of 400r/min at 65 ℃ for 70min to obtain a second mixed solution;
and D, adding sodium methyl lignin sulfonate into the second mixed solution, stirring at the rotating speed of 400r/min for 20min, adding methyl butenoic acid, stirring at the rotating speed of 200r/min for 40min at the temperature of 55 ℃, cooling to 30 ℃, and adjusting the pH to 5 to obtain the liquid alkali-free accelerator.
Example 5:
a liquid alkali-free accelerator comprises the following components in percentage by weight: 45% of aluminum sulfate, 25% of aluminum potassium sulfate dodecahydrate, 8% of pentaerythritol adipate triol, 3% of methylbutyrolactam, 5% of sulfomethyl sodium lignosulfonate, 4% of methyl crotonic acid and 10% of water.
The preparation process specifically comprises the following steps:
a, weighing the components according to the weight percentage of the components of the liquid alkali-free accelerator for later use;
b, adding aluminum potassium sulfate dodecahydrate into the water, heating to 65 ℃, stirring at the rotating speed of 300r/min for 55min, adding aluminum sulfate, heating to 75 ℃, and stirring at the rotating speed of 500r/min for 45min to obtain a first mixed solution;
step C, adding methylbutyrolactam into the first mixed solution, stirring at a rotating speed of 270r/min for 30min, adding poly (pentaerythritol adipate) triol, and stirring at a rotating speed of 400r/min at 70 ℃ for 80min to obtain a second mixed solution;
and D, adding sodium sulfomethyl lignin sulfonate into the second mixed solution, stirring at the rotating speed of 400r/min for 25min, adding methyl butenoic acid, stirring at the rotating speed of 200r/min for 50min at the temperature of 55 ℃, cooling to 40 ℃, and adjusting the pH value to 6 to obtain the liquid alkali-free accelerator.
Comparative example 1:
on the basis of the example 1, aluminum potassium sulfate dodecahydrate is replaced by aluminum sulfate, and other components and preparation methods are unchanged.
Comparative example 2:
the polyethylene glycol adipate glycol is omitted on the basis of the example 1, and other components and the preparation method are unchanged.
Comparative example 3:
sodium sulfomethyl lignosulfonate is omitted on the basis of example 1, and other components and the preparation method are not changed.
Application example 1
The liquid alkali-free setting accelerators obtained in examples 1 to 5 were used as treatment groups, the neat paste and mortar without the setting accelerator added were used as blank groups, and the liquid alkali-free setting accelerators obtained in comparative examples 1 to 3 were used as control groups to carry out comparative tests, and the tests of the setting time of the neat paste and mortar and the compressive strength of the mortar were carried out according to the requirements of GB/T35159 and 2017 accelerating agent for shotcrete. Wherein, the mixing amount of the accelerator is calculated according to the mass percentage of the cement, and the test result is shown in the table 1:
TABLE 1 test results
From the test results in table 1, the setting time of the accelerator provided by the embodiment of the invention is far lower than the requirements of the initial setting time being less than or equal to 5min and the setting time being less than or equal to 12min specified in GB/T35159-.
Therefore, the liquid alkali-free accelerator provided by the invention can solve the technical problems that the accelerator is not uniformly dispersed, the environmental hazard is large, the raw materials are expensive and the field production is difficult to popularize due to the high mixing amount of similar accelerators in the prior art, shortens the initial setting time and the final setting time of cement paste, improves the mortar strength and has wide application prospects in the fields related to cement.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The liquid alkali-free accelerator is characterized by comprising the following components in percentage by weight: 20 to 50 percent of aluminum sulfate, 10 to 30 percent of aluminum potassium sulfate dodecahydrate, 5 to 10 percent of polyalcohol, 1 to 5 percent of organic amide, 1 to 5 percent of sodium alkyl lignosulfonate and 3 to 5 percent of methyl crotonic acid, and the solvent is water.
2. The liquid alkali-free accelerator according to claim 1, wherein the polyol is at least one of a polyester polyol or a polyether polyol.
3. The liquid alkali-free accelerator according to claim 1, wherein the organic amide is at least one selected from the group consisting of methylbutyrolactam and methylhexacaprolactam.
4. The liquid alkali-free accelerator according to claim 1, wherein the sodium alkyl lignosulfonate is at least one of sodium methyl lignosulfonate and sodium sulfomethyl lignosulfonate.
5. The liquid alkali-free accelerator according to claim 1, wherein the source of aluminum sulfate is one of industrial aluminum sulfate or non-iron aluminum sulfate, and the content of aluminum element in the industrial aluminum sulfate or the non-iron aluminum sulfate is Al2O3Measured on Al2O3The content is more than or equal to 15wt percent, and the Fe content is less than or equal to 0.5wt percent.
6. A preparation process of a liquid alkali-free accelerator is characterized by comprising the following steps:
a, weighing the components according to the weight percentage of the components of the alkali-free liquid accelerator as claimed in any one of claims 1 to 5 for later use;
b, adding the aluminum potassium sulfate dodecahydrate into the water, heating to 60-80 ℃, stirring for dissolving, then adding the aluminum sulfate, heating to 60-80 ℃, and continuously stirring for dissolving to obtain a first mixed solution;
step C, adding the organic amide into the first mixed solution, uniformly stirring, adding the polyol, and uniformly stirring at 50-70 ℃ to obtain a second mixed solution;
and D, adding the sodium alkyl lignin sulfonate into the second mixed solution, uniformly stirring, adding the methyl butenoic acid, regulating the pH to 5-6 under stirring at 50-60 ℃, and cooling to obtain the liquid alkali-free accelerator.
7. The preparation process of the liquid alkali-free accelerator according to claim 6, wherein in the step B, the stirring speed of adding the aluminum potassium sulfate dodecahydrate is 250-350 r/min, and the stirring time is 30-60 min; and/or
The stirring speed of the aluminum sulfate is 450-550 r/min, and the stirring time is 30-60 min.
8. The process for preparing the liquid alkali-free accelerator according to claim 6, wherein in the step C, the organic amide is added at a stirring speed of 260 to 300r/min for 20 to 40 min; and/or
The stirring speed of the added polyhydric alcohol is 350-450 r/min, and the stirring time is 60-120 min.
9. The preparation process of the liquid alkali-free accelerator according to claim 6, wherein in the step D, the sodium alkyl lignosulfonate is added at a stirring speed of 350-450 r/min for 20-30 min; and/or
The stirring speed of the methyl butenoic acid is 150-250 r/min, and the stirring time is 30-60 min.
10. The use of the liquid alkali-free accelerator as claimed in any one of claims 1 to 5, wherein the liquid alkali-free accelerator is incorporated into cement in an amount of 2 to 8 wt% based on the amount of the cement.
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