CN112552465B - Preparation method of early-strength polycarboxylate superplasticizer - Google Patents
Preparation method of early-strength polycarboxylate superplasticizer Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- 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
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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Abstract
The application relates to the technical field of concrete additives, and in particular discloses a preparation method of an early-strength polycarboxylate superplasticizer, which comprises the following steps of: s1, preparing kettle bottom liquid; s2, preparing a dropping liquid A; s3, preparing a dropping liquid B; s4, adding 0.5-2 parts of oxidant into the kettle bottom liquid in the step S1, simultaneously dripping a dripping solution A and a dripping solution B into the kettle bottom liquid in the step S1 at constant speed by using a dripping device at normal temperature after 4-6 minutes, and stirring, wherein the dripping time of the dripping solution A and the dripping solution B is respectively 50-70 minutes and 60-80 minutes, and after the dripping is finished, preserving heat for 1-1.5 hours to finish the reaction to obtain a polycarboxylic acid water reducer solution; and S5, adding NaOH solution into the polycarboxylate water reducer solution obtained in the step S6 to adjust the pH value to be neutral, and obtaining liquid, namely the early-strength polycarboxylate water reducer. The purpose of this patent is to solve the high problem that leads to the energy consumption high of the synthetic high temperature of current early strength formula polycarboxylate water reducing agent.
Description
Technical Field
The application relates to the technical field of concrete additives, in particular to a preparation method of an early-strength polycarboxylate superplasticizer.
Background
In recent years, the construction scale of the infrastructure in China is continuously enlarged, the demand of concrete is continuously increased, and in order to accelerate the construction progress and improve the turnover rate of templates, the prefabricated member production, subway segments and repair protection engineering need higher early strength of concrete. At present, the early strength type admixture which is more commonly used mainly comprises: inorganic salt early strength agents such as sulfate, chloride, silicate, nitrite and the like; organic early strength agents such as calcium formate, triethanolamine, triisopropanolamine, urea and the like; an early strength water reducer, an early strength antifreezing agent, an early strength pumping aid and other composite early strength additives. The inorganic salt early strength agent is high in mixing amount, chloride ions which are easy to cause steel bar corrosion and alkali metals which are easy to cause alkali aggregate reaction are easy to introduce, the organic early strength agent is high in price, the mixing amount is sensitive and is not easy to control, conversely, the early strength polycarboxylate water reducer is low in mixing amount, the workability of mixing concrete is high, and the early strength of the concrete can be effectively improved.
The Chinese patent with application number 201310346345.8 discloses a preparation method of an early-strength polycarboxylate water reducer, which has good early-strength effect, but the synthesis temperature of the polycarboxylate water reducer is 70+/-5 ℃, and the energy consumption is high.
The Chinese patent with the application number of 201811354821.X discloses a preparation method of an early-strength polycarboxylate superplasticizer, wherein the synthesis temperature of the early-strength polycarboxylate superplasticizer is lower and is 40 ℃, but the synthesis time is 3-3.5 hours, and the energy consumption is still higher.
In summary, at present, no early-strength polycarboxylate water reducer with simple process, low energy consumption and cost and excellent performance exists.
Disclosure of Invention
Aiming at the defects of the prior art, the application provides a preparation method of an early-strength polycarboxylate superplasticizer, which solves the problem of high energy consumption caused by high synthesis temperature of the existing early-strength polycarboxylate superplasticizer.
In order to solve the problems, the application adopts the following technical scheme:
a preparation method of an early-strength polycarboxylate superplasticizer is characterized by comprising the following steps of: the method comprises the following steps:
s1, adding 100-150 parts of polyether macromonomer and 100-150 parts of tap water into a reaction kettle according to a proportion, stirring and dissolving to form uniform and transparent solution, and obtaining kettle bottom solution;
s2, mixing 8-15 parts of unsaturated acid monomer, 4-10 parts of prepared early-strength functional monomer, 0.5-1 part of chain transfer agent and 10-30 parts of tap water to form a uniform solution, so as to obtain a dropping liquid A, wherein the early-strength functional monomer is an ester synthesized by amino acid and N-methylolacrylamide;
s3, mixing 0.1-0.6 part of reducing agent and 20-60 parts of tap water to form a uniform solution to obtain a dropping liquid B;
s4, adding 0.5-2 parts of oxidant into the kettle bottom liquid in the step S1, simultaneously dripping a dripping solution A and a dripping solution B into the kettle bottom liquid in the step S1 at constant speed by using a dripping device at normal temperature after 4-6 minutes, and stirring, wherein the dripping time of the dripping solution A and the dripping solution B is respectively 50-70 minutes and 60-80 minutes, and after the dripping is finished, preserving heat for 1-1.5 hours to finish the reaction to obtain a polycarboxylic acid water reducer solution;
and S5, adding NaOH solution into the polycarboxylate water reducer solution obtained in the step S4 to adjust the pH value to be neutral, and obtaining liquid, namely the early-strength polycarboxylate water reducer.
Further, the amino acid is one or more of L-glutamic acid, DL-phenylalanine and sarcosine.
Further, the early-strength functional monomer in the step S2 is prepared by the following method: dissolving a certain amount of N-methylol acrylamide and a catalyst zirconium oxychloride in N, N-dimethylformamide, slowly heating to 110-130 ℃ after the dissolution is completed, slowly adding L-glutamic acid which is in the same mole with the N-methylol acrylamide, stirring and reacting for 4-4.5 hours, and removing the solvent N, N-dimethylformamide by rotary evaporation after the reaction is completed, thus obtaining the early-strength functional monomer.
Further, the unsaturated acid monomer is one or more of maleic anhydride, acrylic acid, methacrylic acid, itaconic acid or fumaric acid.
Further, the chain transfer agent is one or more of thioglycollic acid, mercaptopropionic acid, mercaptoethanol or sodium hypophosphite.
Further, the reducing agent is one or more of vitamin C, sodium sulfite, sodium bisulphite, potassium sulfite or sodium metabisulfite.
Further, the oxidant is one or more of ammonium persulfate, sodium persulfate, hydrogen peroxide, benzoyl peroxide and potassium persulfate.
Further, the concentration of the dropping liquid A is 35-40%.
Further, the concentration of the bottom of the kettle is 50-55%.
Further, the concentration of the dropping liquid B is 1-2%.
Wherein, in step S4, the dropping liquid A or the dropping liquid B adopts the following dropping equipment: the stirring device comprises a frame and a stirring barrel, wherein the stirring barrel is fixed on the frame, a motor is fixed on a part of the frame above the stirring barrel, a rotating rod is fixed on an output shaft of the motor, the lower end of the rotating rod extends to the inner bottom of the stirring barrel, and a blade is fixed on the rotating rod; the part of the rotating rod above the stirring barrel is fixedly sleeved with a cam, the right top of the stirring barrel is fixedly provided with a cylinder body, the cylinder body is provided with a one-way air inlet valve and a one-way air outlet valve, the lower end of the cylinder body is provided with an air vent, the inside of the cylinder body is provided with a piston, the outer side wall of the piston is provided with first external threads, the inner side wall of the cylinder body is provided with first internal threads matched with the first external threads, the inside of the cylinder body is provided with a first spring, one end of the first spring is fixed at the bottom of the cylinder body, and the other end of the first spring is propped against the piston; the upper end of the piston is fixedly connected with a piston rod, the piston rod vertically upwards penetrates through the top of the cylinder body and is in sliding sealing connection with the cylinder body, the upper end of the piston rod is fixedly provided with a shifting block of a rectangular plate arranged along the vertical direction, and in the rotating process of the cam, one end, farthest from the rotating rod, of the cam can shift the shifting block; a dripping barrel is fixed on a part of the frame above the stirring barrel, a threaded column is coaxially fixed in the dripping barrel, a sliding plate is sleeved on the periphery of the threaded column, the edge of the sliding plate is attached to and sealed with the inner side wall of the dripping barrel, and a second internal thread matched with a second external thread on the threaded column is arranged on the sliding plate; the upper part of the dripping bucket is connected with a straw, the straw is fixed on the dripping bucket, a dripping pipe which is arranged along the vertical direction is fixed on the stirring bucket, the straw is communicated with the dripping pipe through a hose, and the lower end of the dripping pipe is provided with a one-way liquid outlet valve; the one-way air inlet valve is communicated with the lower part of the dripping pipe through a connecting pipe, and an automatic valve is arranged at one end of the connecting pipe, which is close to the dripping pipe; the hose penetrates through the upper end and the lower end of the fixed box and is fixedly connected with one side wall of the fixed box, an opening is formed in the top of the fixed box, a gear is rotationally connected with the opening, a rack is meshed with the gear, one end of the rack abuts against the hose, the other end of the rack penetrates through the side wall of the fixed box and is rotationally connected with the fixed box, a limiting block arranged in the vertical direction is fixed at the inner bottom of the fixed box, limiting teeth arranged vertically upwards are arranged on the limiting block, and grooves matched with the limiting teeth are formed in the lower end of the rack.
The beneficial effect that this scheme produced is:
1. the application uses 2+2 type macromonomer EPEG, the double bond activity of the monomer is higher than that of the common C four or C five monomer, therefore, the addition reaction can be carried out at normal temperature without heating, the reaction time can be greatly shortened, the energy consumption can be effectively reduced, and the cost is saved.
2. The application synthesizes the mother liquor of the early-strength polycarboxylate superplasticizer by using polyether monomer with larger molecular weight and adopting a structure of short main chain and long side chain, and the structure is favorable for promoting cement hydration and can promote the improvement of early strength of concrete.
3. The application uses N, N-methylene bisacrylamide, ester synthesized by amino acid and N-methylol acrylamide, ester synthesized by cinnamic acid and alcohol amine as functional monomers of the early-strength water reducing agent, wherein the monomers contain a plurality of N atoms, the N atoms contain a pair of unshared electrons and can be combined with Ca 2+ And Fe (Fe) 3+ Forming a complex to increase the solubility of the cement particle surfaceIs favorable to C 3 A and C 4 The dissolution of AF accelerates its reaction with gypsum to form calcium sulfoaluminate. At the same time can reduce Ca in liquid phase 2+ And Al 3+ Further promote C 3 S, thereby promoting early strength increase of the concrete.
4. The early-strength polycarboxylate water reducer disclosed by the application does not contain chloride ions, does not rust steel bars, is safe and environment-friendly in raw materials, and is green and pollution-free.
Drawings
Fig. 1 is an overall configuration diagram of the dropping device.
Fig. 2 is an enlarged view of a portion a in fig. 1.
Detailed Description
The following is a further detailed description of the embodiments:
reference numerals in the drawings of the specification include: the stirring barrel 10, a first fixed block 11, a motor 12, a cam 13, a rotating rod 14, a blade 15, a cylinder body 20, a one-way air inlet valve 21, a one-way air outlet valve 22, a piston 23, a first spring 24, a piston rod 25, a shifting block 26, a connecting pipe 27, an automatic valve 28, a dropping barrel 30, a sliding plate 31, a scraping plate 311, a second spring 32, a bolt 33, a suction pipe 34, a second fixed block 35, a hose 36, a dropping pipe 37, a one-way liquid outlet valve 38, a threaded column 39, a fixed box 40, a gear 41, a rack 42, a handle 43, a limiting block 44 and a limiting tooth 45.
Example 1
The preparation method of the early-strength polycarboxylate superplasticizer comprises the following steps of:
s1, adding 120g of EPEG with the molecular weight of 4000 and 100g of tap water into a reaction kettle according to a proportion, stirring and dissolving to obtain uniform and transparent kettle bottom solution;
s2, uniformly mixing 10g of acrylic acid, 4g of N, N-methylene bisacrylamide, 0.5g of mercaptopropionic acid and 30g of tap water to obtain a dropping liquid A;
s3, uniformly mixing 0.15g of vitamin C and 20g of tap water to obtain a dripping solution B;
s4, adding 0.5g of 27.5% hydrogen peroxide into the kettle bottom liquid obtained in the step S1 at normal temperature, and after 5 minutes, simultaneously dripping a dripping solution A and a dripping solution B into the kettle bottom liquid obtained in the step S1 at constant speed by using a dripping device at normal temperature, stirring, wherein the dripping time of the dripping solution A and the dripping solution B is respectively 60 minutes and 70 minutes, and after dripping is finished, preserving heat for 1 hour to finish the reaction to obtain a polycarboxylate water reducer solution;
and S5, adding NaOH solution into the polycarboxylate water reducer solution obtained in the step S4 to adjust the pH value to be neutral, and obtaining liquid, namely the early-strength polycarboxylate water reducer.
Wherein, in step S4, the dropping liquid A or the dropping liquid B adopts the following dropping equipment: the stirring device comprises a frame and a stirring barrel 10, as shown in fig. 1, wherein the stirring barrel 10 is fixed on the frame, the stirring barrel 10 is cylindrical in shape, the axis of the stirring barrel 10 is arranged along the vertical direction, a motor 12 is fixed on the part, right above the stirring barrel 10, of the frame, the motor 12 is electrically connected with a motor switch, the motor switch is fixed on the frame, the motor switch is pressed down, the motor 12 rotates, the motor switch is pressed down again, and the motor 12 stops rotating; the output shaft of the motor 12 is arranged vertically downwards, a rotating rod 14 of the rotating rod 14 is fixed on the output shaft of the motor 12 and is arranged coaxially with the stirring barrel 10, the lower end of the rotating rod 14 extends to the inner bottom of the stirring barrel 10, and paddles 15 are fixed at the lower end and the lower part of the rotating rod 14.
The stirring barrel 10 is internally used for storing kettle bottom liquid, the motor 12 is started, the motor 12 drives the rotating rod 14 to rotate, and the rotating rod 14 drives the paddles 15 to stir the kettle bottom liquid.
As shown in fig. 1, a cam 13 is fixedly sleeved on a part of a rotating rod 14 above a stirring barrel 10, a cylinder body 20 is fixed on the right top of the stirring barrel 10, a one-way air inlet valve 21 and a one-way air outlet valve 22 are arranged at the upper end of the cylinder body 20, an air vent is arranged at the lower end of the cylinder body 20, the air vent is used for communicating the interior of the cylinder body 20 with the outside, a piston 23 is arranged in the cylinder body 20, a first external thread is arranged on the outer side wall of the piston 23, a first internal thread matched with the first external thread on the piston 23 is arranged on the inner side wall of the cylinder body 20, the first external thread on the piston 23 is not self-locked with the first internal thread on the inner side wall of the cylinder body 20, a first spring 24 is arranged in the cylinder body 20, one end of the first spring 24 is fixed at the bottom of the cylinder body 20, and the other end of the first spring 24 is propped against the piston 23; when the piston 23 rotates forward under the action of external force, the first internal thread is matched with the first external thread to enable the piston 23 to move downwards, after the external force acting on the piston 23 disappears, the piston 23 moves upwards under the action of the first spring 24, and meanwhile, the first internal thread is matched with the first external thread to enable the piston 23 to rotate reversely; the upper end fixedly connected with piston rod 25 of piston 23, piston rod 25 runs through the top of cylinder body 20 vertically upwards and with cylinder body 20 sliding seal connection, the upper end of piston rod 25 is fixed with the shifting block 26 of arranging along the horizontal direction, shifting block 26 is the rectangular shaped plate of arranging along vertical direction, the quantity of shifting block 26 is provided with four and with the axis circumference evenly distributed of piston rod 25, the in-process of cam 13 rotation, one of them shifting block 26 can be stirred to the furthest one end of cam 13 from dwang 14, shifting block 26 rotation drives piston rod 25 and piston 23 rotation.
In the process that the rotating rod 14 drives the cam 13 to rotate, the cam 13 rotates to stir the shifting block 26 to rotate positively, the shifting block 26 drives the piston rod 25 and the piston 23 to rotate positively, the first internal thread is matched with the first external thread to enable the piston 23 to move downwards, the piston 23 extrudes the first spring 24, negative pressure is generated inside the cylinder 20, the one-way air inlet valve 21 is opened, the one-way air outlet valve 22 is closed, and air is sucked inside the cylinder 20; when the cam 13 is separated from the shifting block 26, the piston 23 moves upwards under the action of the first spring 24, and meanwhile, the first internal thread and the first external thread cooperate to enable the piston 23 to rotate reversely, positive pressure is generated inside the cylinder 20, the one-way air inlet valve 21 is closed, the one-way air outlet valve 22 is opened, and the cylinder 20 is exhausted. During the periodic rotation of the cam 13, the cylinder 20 intermittently sucks and discharges air to form an aspiration pump.
As shown in fig. 1, a part of the frame above the stirring barrel 10 is fixed with a dropping barrel 30 with an upward opening, the shape of the dropping barrel 30 is cylindrical, a threaded column 39 is coaxially fixed inside the dropping barrel 30, a sliding plate 31 is sleeved on the periphery of the threaded column 39, the edge of the sliding plate 31 is attached to and sealed with the inner side wall of the dropping barrel 30, a second internal thread matched with a second external thread on the threaded column 39 is arranged on the sliding plate 31, the second external thread and the second internal thread are not self-locking, and when the sliding plate 31 moves downwards under the action of external force, the second external thread and the second internal thread are matched to enable the sliding plate 31 to rotate positively, and meanwhile, the second spring 32 is compressed; when the external force acting on the slide plate 31 disappears, the second spring 32 moves the slide plate 31 upward, and the second external thread cooperates with the second internal thread to rotate the slide plate 31 reversely; as shown in fig. 1, the scrapers 311 are fixedly provided on the slide plate 31, the scrapers 311 are arranged along the radial direction of the slide plate 31, the scrapers 311 are arranged along the vertical direction, one end of the scrapers 311 far away from the axis of the slide plate 31 is attached to the inner side wall of the drip barrel 30, and 4 scrapers 311 are provided and are uniformly distributed along the circumferential direction of the axis of the slide plate 31. As shown in fig. 1 and 2, the upper part of the dropping barrel 30 is connected with a 7-shaped suction pipe 34, the suction pipe 34 is fixed on the dropping barrel 30 through a second fixed block 35, a dropping pipe 37 arranged along the vertical direction is fixed on the left side wall of the stirring barrel 10 through a first fixed block 11, the suction pipe 34 is communicated with the dropping pipe 37 through a hose 36, the hose 36 is made of fluororubber, and a one-way liquid outlet valve 38 is arranged at the lower end of the dropping pipe 37; the one-way air inlet valve 21 is communicated with the lower part of the drip tube 37 through a connecting tube 27, one end, close to the drip tube 37, of the connecting tube 27 is provided with an automatic valve 28, the automatic valve 28 is electrically connected with a first automatic valve switch and a second automatic valve switch, the first automatic valve switch and the second automatic valve switch are respectively arranged at the inner top and the bottom of the cylinder body 20, when the piston 23 moves to the limit positions above and below, the piston 23 can be pressed to the first automatic valve switch and the second automatic valve switch, when the piston 23 is pressed to the first automatic valve switch, the first automatic valve 28 is opened, and when the piston 23 is pressed to the second automatic valve switch, the automatic valve 28 is closed.
In the process of sucking air from the cylinder 20, the cylinder 20 sucks liquid in the drip barrel 30 through the connecting pipe 27, the drip tube 37, the hose 36 and the suction pipe 34 by utilizing the siphon principle, when the piston 23 moves to the lower limit position, the piston 23 presses the second automatic valve switch, the automatic valve 28 is closed, a part of the drip liquid drips into the stirring barrel 10 through the drip tube 37 under the action of gravity, a part of the drip liquid drips back into the drip barrel 30 under the action of gravity, after the drip liquid enters the suction pipe 34, the drip liquid in the drip barrel 30 is reduced, therefore, the sliding plate 31 moves upwards under the action of the second spring 32, the second internal thread is matched with the second external thread to enable the sliding plate 31 to rotate positively, the scraping plate 311 stirs the inside of the drip barrel 30 and scrapes the side wall of the drip barrel 30, the drip liquid is prevented from remaining on the inner side wall of the drip barrel 30, when a part of the drip liquid drips back into the inside of the drip barrel 30 under the action of gravity, the drip liquid in the drip barrel 30 is increased, the drip liquid in the drip barrel 30 moves downwards under the action of gravity, the second external thread is matched with the second external thread to enable the sliding plate 31 to rotate positively, and the inner side wall of the drip barrel 30 is prevented from being scraped off; the cylinder body 20 intermittently sucks air, realizes intermittent dripping of the dripping liquid, realizes up-and-down reciprocating sliding of the sliding plate 31 and simultaneously rotates forward and backward, stirs the dripping liquid in the dripping barrel 30, and avoids influencing the final quality of the water reducer caused by precipitation of the dripping liquid caused in the long-time dripping process.
As shown in fig. 2, the bottom of the drip barrel 30 is screw-connected with a bolt 33, and the pretightening force of the second spring 32 can be adjusted by screwing the bolt 33, so that the second spring 32 can still drive the slide plate 31 to slide upwards after long-time use.
Since the dropping time of the dropping liquid is constant, it is necessary to adjust the amount of each drop of the dropping liquid according to the total amount of the dropping liquid to be dropped and the dropping time of the dropping liquid.
Therefore, as shown in fig. 1, a fixed box 40 is fixed on the frame, the appearance of the fixed box 40 is cuboid, the right part of the fixed box 40 is provided with a through hole penetrating through the upper end and the lower end of the fixed box 40, the hose 36 penetrates through the through hole and is fixedly connected with the through hole, the right end of the hose 36 is attached to the right side wall of the fixed box 40, the top of the fixed box 40 is provided with a rectangular opening, the gear 41 is rotationally connected with the rectangular opening, the gear 41 is meshed with a rack 42, the right end of the rack 42 is propped against the hose 36 through a disc-shaped extrusion plate (not shown in the drawing), the extrusion plate is parallel to the right side wall of the fixed box 40, the left end of the rack 42 penetrates through the left side wall of the fixed box 40 and is rotationally connected with the left side wall of the fixed box 40, the left end of the rack 42 is fixedly provided with a handle 43, the handle 43 is conveniently arranged to rotate the rack 42, the inner bottom of the fixed box 40 is fixedly provided with a limit block 44 arranged along the vertical direction, the limit tooth 45 is arranged on the limit block 44, the shape of the cross section of the limit tooth 45 is in a right triangle, the right triangle is obliquely inclined downwards, the right triangle, the lower end of the right triangle is meshed with the rack 42 is provided with a right-angle bevel edge 45 which is matched with the limit tooth 45, and can slide to the limit tooth 45 under the limit tooth 42, and can slide under the limit tooth 42, and can not slide under the action of the rack 42, so that the limit force can slide under the limit force.
By rotating the gear 41, the gear 41 drives the rack 42 to move rightward, and the squeeze plate on the rack 42 squeezes the hose 36 to reduce the cross-sectional area of the hose 36, thereby controlling the flow rate of the drip liquid flowing through the hose 36, and adjusting the speed of the drip liquid as required, and controlling the drip acceleration, the principle being similar to that of a transfusion tube used by a hospital patient. When the dropping rate needs to be increased, the handle 43 rotates the rack 42 to disengage the rack 42 from the gear 41 and the stopper tooth 45, and after the rack 42 is manually moved to the left limit position, the handle 43 rotates the rack 42 again to reengage the rack 42 with the gear 41 and the stopper tooth 45. And similarly, the adjustment of the dropping speed is realized.
Example 2
The preparation method of the early-strength polycarboxylate superplasticizer comprises the following steps of:
s1, dissolving 30g N-methylol acrylamide and 1g of zirconium oxychloride serving as a catalyst in N, N-dimethylformamide, slowly heating to 120 ℃ after the dissolution is completed, slowly adding L-glutamic acid which is in the same mole with the N-methylol acrylamide, stirring and reacting for 4 hours, and removing the solvent N, N-dimethylformamide by oil pump rotary evaporation after the reaction is finished, thus obtaining the early-strength functional monomer.
S2, adding 100g of EPEG with the molecular weight of 4000 and 100g of tap water into a reaction kettle according to a proportion, stirring and dissolving to obtain uniform and transparent kettle bottom solution;
s3, mixing 12g of acrylic acid, 6g of the early-strength functional monomer obtained in the step S1, 0.6g of thioglycollic acid and 30g of tap water to form uniform dropwise liquid A;
s3, mixing 0.6g of the white suspended block with 50g of tap water to form uniform dripping liquid B;
s5, adding 2g of ammonium persulfate into the kettle bottom solution obtained in the step S1 at normal temperature, simultaneously dripping a dripping solution A and a dripping solution B into the bottom solution obtained in the step I at constant speed by using a dripping device at normal temperature for stirring, wherein the dripping time of the dripping solution A and the dripping solution B is respectively 60 minutes and 70 minutes, and after the dripping is completed, preserving the heat for 1 hour to finish the reaction to obtain a polycarboxylate water reducer solution;
and S6, adding NaOH solution into the polycarboxylate water reducer solution obtained in the step S5 to adjust the pH value to be neutral, and obtaining liquid, namely the early-strength polycarboxylate water reducer.
Example 3
The preparation method of the early-strength polycarboxylate superplasticizer comprises the following steps of:
s1, placing 1g of catalyst p-toluenesulfonic acid and 60g of triethanolamine into a dry three-neck flask, stirring, slowly adding 20g of cinnamic acid after the p-toluenesulfonic acid is dissolved, heating to 110 ℃, stirring and reacting for 3 hours, and obtaining triethanolamine cinnamate (unsaturated amine monomer) after the reaction is finished;
s2, adding 100g of EPEG with the molecular weight of 4000 and 100g of tap water into a reaction kettle according to a proportion, stirring and dissolving to obtain uniform and transparent kettle bottom solution;
s3, mixing 10g of acrylic acid, 5g of triethanolamine cinnamate (unsaturated amine monomer) obtained in the step S1, 0.8g of mercaptoethanol and 12g of tap water to obtain uniform dropwise liquid A;
s4, mixing 0.6g of the white suspended block with 50g of tap water to form uniform dripping liquid B;
s5, adding 3g of ammonium persulfate into the kettle bottom liquid obtained in the step S2 at normal temperature, simultaneously dripping a dripping solution A and a dripping solution B into the kettle bottom liquid obtained in the step S1 at constant speed by using a dripping device at normal temperature for stirring, wherein the dripping time of the dripping solution A and the dripping solution B is respectively 60 minutes and 70 minutes, and after the dripping is finished, preserving the heat for 1 hour to finish the reaction to obtain a polycarboxylate water reducer solution;
and S6, adding NaOH solution into the polycarboxylate water reducer solution obtained in the step S5 to adjust the pH value to be neutral, and obtaining liquid, namely the early-strength polycarboxylate water reducer.
Concrete experiments were performed to compare the examples of the present application with commercially available early strength polycarboxylate water reducers (comparative examples). The mechanical properties of the concrete are carried out according to the method specified in GB/T50080-2002 standard of common method for testing mechanical properties of concrete, and the test results of C50 concrete are shown in the following table:
TABLE 1 comparison of the Performance of several early-strength polycarboxylate water reducers
As can be seen from Table 1, the early-strength polycarboxylate superplasticizer prepared by the embodiment of the application has high water reducing rate and good concrete working performance compared with the commercial early-strength polycarboxylate superplasticizer, and can obviously improve the early strength of concrete.
The foregoing is merely exemplary embodiments of the present application, and specific structures and features that are well known in the art are not described in detail herein. It should be noted that modifications and improvements can be made by those skilled in the art without departing from the structure of the present application, and these should also be considered as the scope of the present application, which does not affect the effect of the implementation of the present application and the utility of the patent. The protection scope of the present application is subject to the content of the claims, and the description of the specific embodiments and the like in the specification can be used for explaining the content of the claims.
Claims (7)
1. A preparation method of an early-strength polycarboxylate superplasticizer is characterized by comprising the following steps of: the method comprises the following steps:
s1, adding 100-150 parts of polyether macromonomer and 100-150 parts of tap water into a reaction kettle according to a proportion, stirring and dissolving to form uniform and transparent solution, and obtaining kettle bottom solution;
s2, mixing 8-15 parts of unsaturated acid monomer, 4-10 parts of prepared early-strength functional monomer, 0.5-1 part of chain transfer agent and 10-30 parts of tap water to form a uniform solution, so as to obtain a dropping liquid A, wherein the early-strength functional monomer is an ester synthesized by amino acid and N-methylolacrylamide;
s3, mixing 0.1-0.6 part of reducing agent and 20-60 parts of tap water to form a uniform solution to obtain a dropping liquid B;
s4, adding 0.5-2 parts of oxidant into the kettle bottom liquid in the step S1, simultaneously dripping a dripping solution A and a dripping solution B into the kettle bottom liquid in the step S1 at constant speed by using a dripping device at normal temperature after 4-6 minutes, and stirring, wherein the dripping time of the dripping solution A and the dripping solution B is respectively 50-70 minutes and 60-80 minutes, and after the dripping is finished, preserving heat for 1-1.5 hours to finish the reaction to obtain a polycarboxylic acid water reducer solution;
and S5, adding NaOH solution into the polycarboxylate water reducer solution obtained in the step S4 to adjust the pH value to be neutral, and obtaining liquid, namely the early-strength polycarboxylate water reducer.
2. The method for preparing the early-strength polycarboxylate superplasticizer, as set forth in claim 1, is characterized in that: the amino acid is one or more of L-glutamic acid, DL-phenylalanine and sarcosine.
3. The method for preparing the early-strength polycarboxylate superplasticizer, as set forth in claim 2, characterized in that: the early-strength functional monomer in the step S2 is prepared by the following method: dissolving a certain amount of N-methylol acrylamide and a catalyst zirconium oxychloride in N, N-dimethylformamide, slowly heating to 110-130 ℃ after the dissolution is completed, slowly adding L-glutamic acid which is in the same mole with the N-methylol acrylamide, stirring and reacting for 4-4.5 hours, and removing the solvent N, N-dimethylformamide by rotary evaporation after the reaction is completed, thus obtaining the early-strength functional monomer.
4. The method for preparing the early-strength polycarboxylate superplasticizer, as set forth in claim 1, is characterized in that: the unsaturated acid monomer is one or more of maleic anhydride, acrylic acid, methacrylic acid, itaconic acid or fumaric acid.
5. The method for preparing the early-strength polycarboxylate superplasticizer, as set forth in claim 1, is characterized in that: the chain transfer agent is one or more of thioglycollic acid, mercaptopropionic acid, mercaptoethanol or sodium hypophosphite.
6. The method for preparing the early-strength polycarboxylate superplasticizer, as set forth in claim 1, is characterized in that: the reducing agent is one or more of vitamin C, sodium sulfite, sodium bisulphite, potassium sulfite or sodium metabisulfite.
7. The method for preparing the early-strength polycarboxylate superplasticizer, as set forth in claim 1, is characterized in that: the oxidant is one or more of ammonium persulfate, sodium persulfate, hydrogen peroxide, benzoyl peroxide and potassium persulfate.
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