CN110982020A - Ether polycarboxylic acid slump retaining agent and preparation method thereof - Google Patents
Ether polycarboxylic acid slump retaining agent and preparation method thereof Download PDFInfo
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- CN110982020A CN110982020A CN201911381030.0A CN201911381030A CN110982020A CN 110982020 A CN110982020 A CN 110982020A CN 201911381030 A CN201911381030 A CN 201911381030A CN 110982020 A CN110982020 A CN 110982020A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/20—Sulfonated aromatic compounds
- C04B24/22—Condensation or polymerisation products thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/20—Retarders
- C04B2103/22—Set retarders
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/308—Slump-loss preventing agents
Abstract
The invention discloses an ether polycarboxylic acid slump retaining agent and a preparation method thereof, belonging to the technical field of slump retaining agent preparation, the ether polycarboxylic acid slump retaining agent and the preparation method thereof can keep the fluidity not lost or even increased within 2h, ensure that the concrete slump loss is very low, realize the regulation and control between the dispersion performance and the retention performance over time of a polycarboxylic acid water reducing agent, overcome the defect of high-temperature synthesis in the traditional additive preparation process, have short reaction period, greatly improve the production efficiency, reduce the production cost, simultaneously, through a color-changing premixing hemisphere arranged in a temperature-sensing reaction kettle, a worker can judge the temperature of an internal reactant according to the color change, reduce the temperature detection steps of the worker, reduce the workload, effectively avoid the introduction of impurities due to temperature detection, and effectively reduce the heat loss due to the reactor per se compared with the prior art, effectively reduces the temperature display error and leads the slump retaining agent finished product to have better quality.
Description
Technical Field
The invention relates to the technical field of slump retaining agents, in particular to an ether polycarboxylic acid slump retaining agent and a preparation method thereof.
Background
The slump retaining agent is an additive capable of keeping the slump of concrete from losing quickly, is a retarder in essence, delays the hydration and the condensation of cement and achieves the effect of keeping the slump. The retarder is a chemical admixture for adjusting thickening time. It can slow down the hydration speed of cement, prolong the time of cement paste from plastic state to solid state, and has no adverse effect on the later strength of cement stone.
In recent years, due to large-scale construction, the demand of raw materials of sand and stone required by concrete is more and more increased, natural resources are in shortage or lack in many places, high-quality sand and stone materials are few, the quality of the sand and stone materials used in most of mixing stations is poor at present, the mud content of some materials is high, the loss of concrete in the use process is very fast due to the fact that machine-made sand is used, the construction environment temperature is sometimes higher, and the like, and the requirements of actual construction cannot be met.
However, with the construction of a large number of national major projects, passenger dedicated lines, water conservancy and hydropower projects and the like, the supply of main raw materials of concrete is short, which causes the quality of coarse aggregates, mineral admixtures, fine aggregates, cement and the like to show a decline trend, and in the preparation process of the slump retaining agent, the requirements of some steps on temperature are high, so that workers need to continuously measure the temperature in the reaction kettle, the measurement modes are generally two, one is to measure the temperature in the reaction kettle through a temperature sensor, but the mode is easy to cause the introduction of impurities, which causes the influence on the quality of the finished slump retaining agent, and the other is to measure the temperature by smearing a color-changing coating on the outer wall of the reactor, but the mode is influenced by the outer shell of the reaction kettle, the heat of reactants in the reaction kettle needs to be conducted to the color-changing coating on the outer wall of the reaction kettle through the outer shell of the reaction kettle, heat loss may be large, resulting in inaccurate reaction temperatures for color change of the color-changing coating.
Disclosure of Invention
1. Technical problem to be solved
Aiming at the problems in the prior art, the invention aims to provide an ether polycarboxylic acid slump retaining agent and a preparation method thereof, which can keep the fluidity within 2h and not lose or even increase, so that the concrete slump loss is very low, the dispersion performance and the time retention performance of the polycarboxylic acid water reducing agent are regulated, the defect of high-temperature synthesis in the traditional additive preparation process is overcome, the reaction period is short, the production efficiency is greatly improved, the production cost is reduced, meanwhile, through a color-changing premixing hemisphere arranged in a temperature sensing reaction kettle, a worker can judge the temperature of reactants in the temperature sensing reaction kettle according to the color change observed by naked eyes, the steps of temperature detection by the worker are reduced, the workload is reduced, the introduction of impurities due to the temperature detection is avoided, and simultaneously, compared with the prior art, the heat loss caused by the heat absorption of the inner wall of the reactor is effectively reduced, the temperature display is more accurate, the temperature error is effectively reduced, and the quality of the finished slump retaining agent is better.
2. Technical scheme
In order to solve the above problems, the present invention adopts the following technical solutions.
The preparation method of the ether polycarboxylic acid slump retaining agent comprises the following steps: the method comprises the following steps:
s1, weighing the components according to the proportion of 50-75 parts of methyl allyl polyoxyethylene ether, 10-12 parts of citric acid, 5-8 parts of carbonic acid, 3-8 parts of sodium p-styrene sulfonate, 0.5-3 parts of hydrogen peroxide, 5-20 parts of acrylic ester, 5-20 parts of acrylic acid, 0-1 part of reducing agent, 0-0.5 part of chain transfer agent, 0.1-0.6 part of fluid loss agent, 1-2 parts of hexametaphosphate and 10-15 parts of water;
s2, putting methyl allyl polyoxyethylene ether, sodium p-styrene sulfonate and hydrogen peroxide into a temperature-sensitive reaction kettle, adding water, mixing and stirring to obtain a uniform mixed solution;
s3, judging the temperature of the mixed solution according to the color of the surface of the temperature-sensitive reaction kettle, and after the mixed solution reaches a proper temperature, simultaneously dropwise adding the mixed solution of acrylic ester and acrylic acid dissolved in 3-5 parts of water and the mixed solution of reducing agent and chain transfer agent dissolved in 3-5 parts of water, wherein the dropwise adding time is controlled to be 2-3h and 2.5-3.5h respectively, and stirring is carried out while dropwise adding;
s4, when the temperature of the final product in the S3 is reduced to room temperature, adding citric acid, carbonic acid, fluid loss agent and hexametaphosphoric acid into the product, and stirring the mixture evenly;
and S5, after stirring, adjusting the pH value by 20-30 parts of 30-50% sodium hydroxide solution, adding deionized water to adjust the final concentration to 40%, and discharging to obtain the ether polycarboxylic acid slump retaining agent.
Further, the pH value of the slump retaining agent is adjusted to be 7 in the S4, so that the slump retaining agent is finally neutral and does not have acidic or alkaline influence on the cement, and the influence on the service life of the cement is basically negligible.
Further, the S2 is operated in the environment of 40-60 ℃, and the suitable temperature for the mixed solution in S3 is 30-60 ℃.
Further, the liquid level of the mixed solution in the S2 is located above the central line of the temperature-sensitive reaction kettle, the mixed solution is too little, waste of the inner space of the temperature-sensitive reaction kettle can be caused, and the slump retaining agent preparation efficiency can be too low, and the mixed solution is too much, so that the reaction is incomplete, and the quality of the slump retaining agent finished product is not high.
Furthermore, the reaction kettle comprises a reaction bottom, a temperature sensing middle part and a reaction upper part with a cover, the reaction bottom, the temperature sensing middle part and the reaction upper part are fixedly connected in sequence from bottom to top, an opening color changing cavity is formed in the inner wall of the temperature sensing middle part, a plurality of uniformly distributed color changing premixing hemispheres are arranged in the opening color changing cavity, a heat conducting inner panel is arranged at the cavity opening of the opening color changing cavity, the heat conducting inner panel and the middle part shell are of an integral structure, the color changing premixing hemispheres in the temperature sensing middle part can change colors according to the change of the temperature, a worker can judge the temperature of reactants in the temperature sensing reaction kettle according to the color change observed by naked eyes, the worker does not need to perform a temperature detection step, and; meanwhile, the condition that impurities are introduced due to temperature detection is effectively avoided, and meanwhile, compared with the prior art that the temperature sensing material is coated on the surface of the reactor, the heat loss caused by heat absorption of the inner wall of the reactor is effectively reduced, so that the temperature display is more accurate, the temperature error is effectively reduced, and the effect on the preparation result is better.
Further, the hemisphere is mixed in advance including location bump, high temperature discoloration layer, transition discoloration layer and low temperature discoloration layer to discolour, location bump, high temperature discoloration layer, transition discoloration layer and low temperature discoloration layer are folded in proper order and are fixed connection with the heat conduction embedded plate, through per two spaces that change color between the hemisphere in advance, can observe the volume of its inside mixed solution to confirm that the last liquid level of mixed solution is higher than temperature sensing reation kettle's central line, lie in the central line top at temperature sensing middle part promptly, observe the specific colour that the temperature sensing middle part appears, can judge the change of its inside temperature.
Furthermore, the heat-conducting inner panel and the positioning salient points are made of heat-conducting materials, the thickness of the heat-conducting inner panel is 1/3-1/2 of the thickness of the middle shell (1) on the side opposite to the heat-conducting inner panel (3), the heat conduction is faster and more sensitive due to the materials with good heat-conducting performance, the heat loss in the heat conduction can be effectively reduced, the displayed color of the color-changing premixing hemisphere can accurately represent the temperature of the mixed solution in the color-changing premixing hemisphere, the excessive thickness of the heat-conducting inner panel can cause the heat loss caused by the heat-conducting inner panel per se to be increased, certain errors exist in the displayed color of the color-changing premixing hemisphere, the control and the accuracy of the reaction temperature are reduced, and the quality of a slump retaining agent finished product is influenced.
Further, high temperature discoloration layer, transition discoloration layer and low temperature discoloration layer are made by the heat conduction material that dopes reversible temperature sensing discoloration powder, and reversible temperature sensing discoloration powder dopes the proportion of heat conduction material and is 1: 0.8-1.2, the color-changing temperature nodes of the three are sequentially reduced, the color-changing temperature nodes are respectively 30 ℃, 40 ℃ and 60 ℃, when the temperature is below the color-changing node, the temperature-sensitive color-changing powder displays the natural color, and when the temperature is above the color-changing node, the color-changing premixed hemisphere is colorless, so that at different temperatures, the color-changing premixed hemisphere can display different colors, and a worker can judge the temperature according to the change of the colors.
Further, the area of the contact section of panel increases in proper order in high temperature discoloration layer, transition discoloration layer and low temperature discoloration layer and the heat conduction, high temperature discoloration layer, transition discoloration layer and low temperature discoloration layer three colour each other are the colour that contrasts strongly, and the summit of high temperature discoloration layer, transition discoloration layer and low temperature discoloration layer hemisphere is more and more distant from middle part casing inside, therefore sets up bigger and bigger area of contact, can make its temperature variation faster for the colour that observes from outside staff can be more accurate show the temperature of inside mixed solution.
Furthermore, the outer surface in the middle part of the temperature sensing is made of transparent materials, so that a worker can observe the color change of the color-changing premixing hemisphere inside the temperature sensing device, and the temperature can be judged conveniently.
3. Advantageous effects
Compared with the prior art, the invention has the advantages that:
(1) the scheme can realize that the fluidity is kept not to be lost or even increased within 2h, so that the concrete slump loss is very low, the dispersion performance and the long-term retention performance of the polycarboxylate water reducing agent are regulated, the defect that high-temperature synthesis is needed in the traditional additive preparation process is overcome, the reaction period is short, the production efficiency is improved to a great extent, the production cost is reduced, meanwhile, through the color-changing premixing hemisphere arranged in the temperature-sensing reaction kettle, a worker can judge the temperature of reactants in the temperature-sensing reaction kettle according to the color change observed by naked eyes, the temperature detection steps of the worker are reduced, the workload is reduced, and the introduction of impurities caused by temperature detection is avoided, meanwhile, compared with the prior art, the heat loss caused by heat absorption of the inner wall of the reactor is effectively reduced, the temperature display is more accurate, and the temperature error is effectively reduced, so that the finished product of the slump retaining agent has better quality.
(2) The pH is adjusted to 7 in S4 so that the slump retaining agent is finally neutral and does not have acidic or alkaline influence on the cement, and the influence on the service life of the cement is basically negligible.
(3) S2 was operated at 40-60 deg.C, and the appropriate temperature to which the mixed solution in S3 was brought was 30-60 deg.C.
(4) The liquid level of the mixed solution in the S2 is located above the central line of the temperature-sensing reaction kettle, the mixed solution is too little, waste of the inner space of the temperature-sensing reaction kettle can be caused, the slump retaining agent preparation efficiency is too low, the mixed solution is too much, the reaction is incomplete, and the quality of the slump retaining agent finished product is not high.
(5) The reaction kettle comprises a reaction bottom, a temperature sensing middle part and a reaction upper part with a cover, wherein the reaction bottom, the temperature sensing middle part and the reaction upper part are fixedly connected in sequence from bottom to top, an opening color changing cavity is formed in the inner wall of the temperature sensing middle part, a plurality of uniformly distributed color changing premixing hemispheres are arranged in the opening color changing cavity, a heat conducting inner panel is arranged at the cavity opening of the opening color changing cavity, the heat conducting inner panel and the middle shell are of an integral structure, the color changing premixing hemispheres in the temperature sensing middle part can change colors according to the change of the temperature, a worker can judge the temperature of reactants in the temperature sensing reaction kettle according to the color change observed by naked eyes, the worker does not need to carry out; meanwhile, the condition that impurities are introduced due to temperature detection is effectively avoided, and meanwhile, compared with the prior art that the temperature sensing material is coated on the surface of the reactor, the heat loss caused by heat absorption of the inner wall of the reactor is effectively reduced, so that the temperature display is more accurate, the temperature error is effectively reduced, and the effect on the preparation result is better.
(6) The hemisphere that mixes discolours is including fixing a position the bump, high temperature discoloration layer, transition discoloration layer and low temperature discoloration layer, fix a position the bump, high temperature discoloration layer, transition discoloration layer and low temperature discoloration layer from inside to outside in proper order with heat conduction embedded plate fixed connection, through per two spaces that mix between the hemisphere that discolours, can observe the volume of its inside mixed solution, thereby confirm that the last liquid level of mixed solution is higher than temperature sensing reation kettle's central line, be located the top of central line in the middle part of the temperature sensing promptly, observe the specific colour that the temperature sensing middle part appears, can judge the change of its inside temperature.
(7) The heat-conducting inner embedded plate and the positioning salient points are made of heat-conducting materials, the thickness of the heat-conducting embedded plate is 1/3-1/2 of the thickness of the middle shell on one side opposite to the heat-conducting embedded plate, the heat conduction is faster and more sensitive due to the materials with good heat-conducting performance, the heat loss in the heat conduction can be effectively reduced, the temperature of the internal mixed solution can be represented more accurately by the displayed color of the color-changing premixing hemisphere, the heat loss caused by the heat-conducting inner embedded plate is increased due to the fact that the heat-conducting inner embedded plate is too thick in the heat-conducting inner embedded plate, certain errors exist in the displayed color of the color-changing premixing hemisphere, the control and accuracy of the reaction temperature are reduced, and the quality of a.
(8) The high-temperature discoloring layer, the transition discoloring layer and the low-temperature discoloring layer are all made of heat conducting materials doped with reversible temperature-sensitive discoloring powder, and the proportion of the reversible temperature-sensitive discoloring powder doped with the heat conducting materials is 1: 0.8-1.2, the color-changing temperature nodes of the three are sequentially reduced, the color-changing temperature nodes are respectively 30 ℃, 40 ℃ and 60 ℃, when the temperature is below the color-changing node, the temperature sensing color-changing powder displays the natural color, and when the temperature is above the color-changing node, the color-changing premixing semisphere is colorless, so that at different temperatures, the color-changing premixing semisphere can display different colors, and a worker can judge the temperature according to the change of the colors.
(9) The area of the contact cross section of panel increases in proper order in high temperature discoloration layer, transition discoloration layer and low temperature discoloration layer and the heat conduction, high temperature discoloration layer, transition discoloration layer and low temperature discoloration layer three colour each other are the colour that contrast is strong, high temperature discoloration layer, the summit of transition discoloration layer and low temperature discoloration layer hemisphere is more and more far away from middle part casing inside, therefore set up bigger and bigger area of contact, can make its temperature variation faster, make from the outside, the colour that the staff observed can be more accurate shows the temperature of inside mixed solution.
(10) The outer surface in temperature sensing middle part is transparent material to the staff of being convenient for observes the colour change of its inside colour change premix hemisphere, and then is convenient for judge the temperature.
Drawings
FIG. 1 is a principal process flow diagram of the present invention;
FIG. 2 is a schematic view of the main structure of the temperature-sensitive reaction vessel of the present invention;
FIG. 3 is a front view of the temperature sensing middle part of the present invention;
FIG. 4 is a schematic view of the structure at A in FIG. 3;
fig. 5 is a schematic structural view of the color-changing pre-mixing hemisphere of the present invention.
The reference numbers in the figures illustrate:
the color-changing light-emitting diode comprises a middle shell 1, a color-changing cavity 2 with an opening, a heat-conducting inner panel 3, positioning salient points 41, a high-temperature color-changing layer 42, a transition color-changing layer 43 and a low-temperature color-changing layer 44.
Detailed Description
The drawings in the embodiments of the invention will be combined; the technical scheme in the embodiment of the invention is clearly and completely described; obviously; the described embodiments are only some of the embodiments of the invention; but not all embodiments, are based on the embodiments of the invention; all other embodiments obtained by a person skilled in the art without making any inventive step; all fall within the scope of protection of the present invention.
In the description of the present invention, it should be noted that the terms "upper", "lower", "inner", "outer", "top/bottom", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus should not be construed as limiting the present invention. Furthermore, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "disposed," "sleeved/connected," "connected," and the like are to be construed broadly, e.g., "connected," which may be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
Example 1:
referring to fig. 1, a slump retaining agent of ether polycarboxylic acid is prepared by the following steps: the method comprises the following steps:
s1, weighing the components according to the proportion of 50 parts of methyl allyl polyoxyethylene ether, 10 parts of citric acid, 5 parts of carbonic acid, 3 parts of sodium p-styrene sulfonate, 0.5 part of hydrogen peroxide, 5 parts of acrylic ester, 5 parts of acrylic acid, 0.2 part of reducing agent, 0.1 part of chain transfer agent, 0.1 part of fluid loss agent, 1 part of hexametaphosphoric acid and 10 parts of water;
s2, putting methyl allyl polyoxyethylene ether, sodium p-styrene sulfonate and hydrogen peroxide into a temperature-sensitive reaction kettle, adding water, mixing and stirring to obtain a uniform mixed solution;
s3, judging the temperature of the mixed solution according to the color of the surface of the temperature-sensitive reaction kettle, and after the mixed solution reaches a proper temperature, simultaneously dropwise adding the mixed solution of acrylic ester and acrylic acid dissolved in 5 parts of water and the mixed solution of reducing agent and chain transfer agent dissolved in 5 parts of water, wherein the dropwise adding time is controlled to be 2-3h and 2.5-3.5h respectively, and stirring is carried out while dropwise adding;
s4, when the temperature of the final product in the S3 is reduced to room temperature, adding citric acid, carbonic acid, fluid loss agent and hexametaphosphoric acid into the product, and stirring the mixture evenly;
and S5, after stirring, adjusting the pH value by 20 parts of sodium hydroxide solution with the concentration of 30, adding deionized water to adjust the final concentration to 40%, and discharging to obtain the ether polycarboxylic acid slump retaining agent.
Example 2:
referring to fig. 1, a slump retaining agent of ether polycarboxylic acid is prepared by the following steps: the method comprises the following steps:
s1, weighing the components according to the proportion of 60 parts of methyl allyl polyoxyethylene ether, 11 parts of citric acid, 7 parts of carbonic acid, 5 parts of sodium p-styrene sulfonate, 2 parts of hydrogen peroxide, 13 parts of acrylic ester, 15 parts of acrylic acid, 0.7 part of reducing agent, 0.3 part of chain transfer agent, 0.4 part of fluid loss agent, 1.5 parts of hexametaphosphoric acid and 12 parts of water;
s2, putting methyl allyl polyoxyethylene ether, sodium p-styrene sulfonate and hydrogen peroxide into a temperature-sensitive reaction kettle, adding water, mixing and stirring to obtain a uniform mixed solution;
s3, judging the temperature of the mixed solution according to the color of the surface of the temperature-sensitive reaction kettle, and after the mixed solution reaches a proper temperature, simultaneously dropwise adding the mixed solution of acrylic ester and acrylic acid dissolved in 3 parts of water and the mixed solution of reducing agent and chain transfer agent dissolved in 3 parts of water, wherein the dropwise adding time is controlled to be 2-3h and 2.5-3.5h respectively, and stirring is carried out while dropwise adding;
s4, when the temperature of the final product in the S3 is reduced to room temperature, adding citric acid, carbonic acid, fluid loss agent and hexametaphosphoric acid into the product, and stirring the mixture evenly;
and S5, after stirring, adjusting the pH value by 25 parts of 40% sodium hydroxide solution, adding deionized water to adjust the final concentration to 40%, and discharging to obtain the ether polycarboxylic acid slump retaining agent.
Example 3:
referring to fig. 1, a slump retaining agent of ether polycarboxylic acid is prepared by the following steps: the method comprises the following steps:
s1, weighing the components according to the mixture ratio of 75 parts of methyl allyl polyoxyethylene ether, 12 parts of citric acid, 8 parts of carbonic acid, 8 parts of sodium p-styrene sulfonate, 3 parts of hydrogen peroxide, 20 parts of acrylic ester, 20 parts of acrylic acid, 1 part of reducing agent, 0.5 part of chain transfer agent, 0.6 part of fluid loss agent, 2 parts of hexametaphosphoric acid and 15 parts of water;
s2, putting methyl allyl polyoxyethylene ether, sodium p-styrene sulfonate and hydrogen peroxide into a temperature-sensitive reaction kettle, adding water, mixing and stirring to obtain a uniform mixed solution;
s3, judging the temperature of the mixed solution according to the color of the surface of the temperature-sensitive reaction kettle, and after the mixed solution reaches a proper temperature, simultaneously dropwise adding the mixed solution of acrylic ester and acrylic acid dissolved in 4 parts of water and the mixed solution of reducing agent and chain transfer agent dissolved in 4 parts of water, wherein the dropwise adding time is controlled to be 2-3h and 2.5-3.5h respectively, and stirring is carried out while dropwise adding;
s4, when the temperature of the final product in the S3 is reduced to room temperature, adding citric acid, carbonic acid, fluid loss agent and hexametaphosphoric acid into the product, and stirring the mixture evenly;
and S5, after stirring, adjusting the pH value by 30 parts of 50% sodium hydroxide solution, adding deionized water to adjust the final concentration to 40%, and discharging to obtain the ether polycarboxylic acid slump retaining agent.
The pH is adjusted in S4 to make the final solution neutral, i.e., pH 7, so that the slump retaining agent is finally neutral and has no acidic or alkaline influence on the cement, so that the influence on the service life of the cement is basically negligible, S2 is operated in an environment of 40-60 ℃, and the proper temperature required to reach the mixed solution in S3 is 30-60 ℃.
And (3) carrying out the preparation processes for multiple times at the same temperature, and controlling the temperature of the mixture obtained in the preparation process S2 to be different every time, so that the preparation efficiency of the slump retaining agent is different under different temperature conditions, and in the actual slump retaining agent preparation process, the slump retaining agent can be prepared under the temperature condition corresponding to the optimal preparation efficiency as required.
Referring to fig. 2, in S2, the liquid level of the mixed solution is located above the centerline of the temperature-sensitive reaction kettle, and too little mixed solution may cause waste of the internal space of the temperature-sensitive reaction kettle, and may cause too low preparation efficiency of the slump retaining agent, and too much mixed solution may cause incomplete reaction, so that the quality of the finished slump retaining agent is not high, and the reaction kettle includes a reaction bottom, a temperature-sensitive middle part, and a reaction upper part with a cover, and the three parts are sequentially and fixedly connected from bottom to top.
Referring to fig. 3-4, an opening color-changing cavity 2 is arranged on the inner wall of the temperature sensing middle part, a plurality of uniformly distributed color-changing premixing hemispheres are arranged in the opening color-changing cavity 2, a heat-conducting inner panel 3 is arranged at the cavity opening of the opening color-changing cavity 2, the heat-conducting inner panel 3 and the middle shell 1 are of an integral structure, the color-changing premixing hemispheres in the temperature sensing middle part can change colors according to the change of the temperature, a worker can judge the temperature of reactants in the temperature sensing reaction kettle according to the color change observed by naked eyes, the worker does not need to perform a temperature detection step, and the workload is reduced; meanwhile, the condition that impurities are introduced due to temperature detection is effectively avoided, and meanwhile, compared with the prior art that the temperature sensing material is coated on the surface of the reactor, the heat loss caused by heat absorption of the inner wall of the reactor is effectively reduced, so that the temperature display is more accurate, the temperature error is effectively reduced, and the effect on the preparation result is better.
Referring to fig. 5, the color-changing premixing hemispheres include positioning bumps 41, a high-temperature color-changing layer 42, a transition color-changing layer 43 and a low-temperature color-changing layer 44, the positioning bumps 41, the high-temperature color-changing layer 42, the transition color-changing layer 43 and the low-temperature color-changing layer 44 are fixedly connected with the heat-conducting inner panel 3 from inside to outside in sequence, and the amount of the mixed solution inside the temperature-changing premixing hemispheres can be observed through a gap between every two color-changing premixing hemispheres, so that the upper liquid level of the mixed solution is higher than the central line of the temperature-sensing reaction kettle, namely, the mixed solution is located above the central line of the temperature-sensing middle.
The heat-conducting inner panel 3 and the positioning salient points 41 are both made of heat-conducting materials, the thickness of the heat-conducting inner panel is 1/3-1/2 of the thickness of the middle shell at the side opposite to the heat-conducting inner panel, the heat-conducting material with good heat-conducting property enables the temperature conduction to be faster and more sensitive, the heat loss in the heat conduction can be effectively reduced, so that the displayed color of the color-changing premixing hemisphere can more accurately represent the temperature of the mixed solution therein, the excessive thickness of the heat-conducting inner panel 3 can result in increased heat loss due to the heat-conducting inner panel 3 itself, make the colour that the premixed hemisphere that discolours shows have certain error, cause to the accuse of reaction temperature and the accuracy reduces, influence the off-the-shelf quality of slump retaining agent, high temperature discoloration layer, transition discoloration layer and low temperature discoloration layer 44 are made by the heat conduction material that has the reversible temperature sensing discoloration powder of doping, and the proportion that reversible temperature sensing discoloration powder dopes the heat conduction material is 1: 0.8-1.2, the color-changing temperature nodes of the three are sequentially reduced, the color-changing temperature nodes are respectively 60 ℃, 40 ℃ and 30 ℃, when the temperature is below the color-changing node, the temperature sensing color-changing powder displays the natural color, and when the temperature is above the color-changing node, the color-changing premixing semisphere is colorless, so that at different temperatures, the color-changing premixing semisphere can display different colors, and a worker can judge the temperature according to the change of the colors. When the temperature is below 30 ℃, the low temperature discoloring layer 44 is positioned at the outermost layer, so that the color of the low temperature discoloring layer 44 is seen by the operator, when the temperature is between 30 ℃ and 40 ℃, the low temperature discoloring layer 44 is colorless, the color of the transition discoloring layer is seen by the operator, when the temperature is between 40 ℃ and 60 ℃, the color of the high temperature discoloring layer is seen by the operator, when the temperature exceeds 60 ℃, the color is displayed as a whole, or the color of the positioning bump 41 is seen by the operator.
High temperature discoloration layer 42, transition discoloration layer 43 and low temperature discoloration layer 44 increase in proper order with the area of the contact cross-section of panel 3 in the heat conduction, high temperature discoloration layer 42, transition discoloration layer 43 and the mutual contrast strong colour of low temperature discoloration layer 44 three colour, high temperature discoloration layer 42, the summit of transition discoloration layer 43 and low temperature discoloration layer 44 hemisphere is more and more distant from 1 inside middle part casing, therefore set up bigger and bigger area of contact, can make its temperature variation faster, make from the outside, the colour that the staff observed can be more accurate shows the temperature of inside mixed solution, the temperature sensing middle part is transparent material, thereby be convenient for the staff observes the colour change of its inside mixed solution that discolours, and then be convenient for judge the temperature.
The loss and even increase of the fluidity can be kept within 2h, the slump loss of concrete can be very low when the polycarboxylic acid water reducer is applied to the concrete, the dispersion performance and the retention performance of the polycarboxylic acid water reducer can be regulated and controlled with time, the defect that high-temperature synthesis is needed in the traditional additive preparation process is overcome, the reaction period is short, the production efficiency is improved to a great extent, and the production cost is reduced, so that the application range of the polycarboxylic acid slump retainer is widened, meanwhile, the color change can be realized according to the temperature change through the color-changing premixing hemisphere arranged in the temperature sensing middle part, the temperature of reactants in the temperature sensing reaction kettle can be judged by workers according to the color change observed by naked eyes, the temperature detection step is not needed by the workers, and the workload is reduced; meanwhile, the condition that impurities are introduced due to temperature detection is effectively avoided, and compared with the prior art, the heat loss caused by heat absorption of the inner wall of the reactor is effectively reduced, so that the temperature display is more accurate, the temperature error is effectively reduced, and the effect on the preparation result is better.
The above; but are merely preferred embodiments of the invention; the scope of the invention is not limited thereto; any person skilled in the art is within the technical scope of the present disclosure; the technical scheme and the improved concept of the invention are equally replaced or changed; are intended to be covered by the scope of the present invention.
Claims (10)
1. The ether polycarboxylic acid slump retaining agent is characterized in that: the preparation method comprises the following steps: the method comprises the following steps:
s1, weighing the components according to the proportion of 50-75 parts of methyl allyl polyoxyethylene ether, 10-12 parts of citric acid, 5-8 parts of carbonic acid, 3-8 parts of sodium p-styrene sulfonate, 0.5-3 parts of hydrogen peroxide, 5-20 parts of acrylic ester, 5-20 parts of acrylic acid, 0-1 part of reducing agent, 0-0.5 part of chain transfer agent, 0.1-0.6 part of fluid loss agent, 1-2 parts of hexametaphosphate and 10-15 parts of water;
s2, putting methyl allyl polyoxyethylene ether, sodium p-styrene sulfonate and hydrogen peroxide into a temperature-sensitive reaction kettle, adding water, mixing and stirring to obtain a uniform mixed solution;
s3, judging the temperature of the mixed solution according to the color of the surface of the temperature-sensitive reaction kettle, and after the mixed solution reaches a proper temperature, simultaneously dropwise adding the mixed solution of acrylic ester and acrylic acid dissolved in 3-5 parts of water and the mixed solution of reducing agent and chain transfer agent dissolved in 3-5 parts of water, wherein the dropwise adding time is controlled to be 2-3h and 2.5-3.5h respectively, and stirring is carried out while dropwise adding;
s4, when the temperature of the final product in the S3 is reduced to room temperature, adding citric acid, carbonic acid, fluid loss agent and hexametaphosphoric acid into the product, and stirring the mixture evenly;
and S5, after stirring, adjusting the pH value by 20-30 parts of 30-50% sodium hydroxide solution, adding deionized water to adjust the final concentration to 40%, and discharging to obtain the ether polycarboxylic acid slump retaining agent.
2. The slump retaining agent of ether polycarboxylic acid according to claim 1, wherein: in the step S4, the pH was adjusted to 7.
3. The slump retaining agent of ether polycarboxylic acid according to claim 1, wherein: the S2 is operated in the environment of 40-60 ℃, and the suitable temperature for the mixed solution in the S3 is 30-60 ℃.
4. The slump retaining agent of ether polycarboxylic acid according to claim 1, wherein: the liquid level of the mixed solution in the S2 is positioned above the central line of the temperature sensing reaction kettle.
5. The slump retaining agent of ether polycarboxylic acid according to claim 1, wherein: the reaction kettle comprises a reaction bottom, a temperature sensing middle part and a reaction upper part with a cover, wherein the three parts are sequentially and fixedly connected from bottom to top, an opening color changing cavity (2) is formed in the inner wall of the temperature sensing middle part, a plurality of uniformly distributed color changing premixing hemispheres are arranged in the opening color changing cavity (2), a heat conducting inner panel (3) is arranged at the cavity opening of the opening color changing cavity (2), and the heat conducting inner panel (3) and the middle shell (1) are of an integrated structure.
6. The slump retaining agent of ether polycarboxylic acid according to claim 1, wherein: the color-changing premixing hemisphere comprises a positioning salient point (41), a high-temperature color-changing layer, a transition color-changing layer and a low-temperature color-changing layer (44), wherein the positioning salient point (41), the high-temperature color-changing layer, the transition color-changing layer and the low-temperature color-changing layer (44) are sequentially overlapped and fixedly connected with the heat-conducting inner embedded plate (3).
7. The slump retaining agent of ether polycarboxylic acid according to claim 1, wherein: the heat-conducting inner panel (3) and the positioning salient points (41) are both made of heat-conducting materials, and the thickness of the heat-conducting inner panel (3) is 1/3-1/2 of the thickness of the middle shell (1) on the side opposite to the heat-conducting inner panel (3).
8. The slump retaining agent of ether polycarboxylic acid according to claim 6, wherein: high temperature discoloration layer, transition discoloration layer and low temperature discoloration layer (44) are made by the heat conduction material that has the reversible temperature sensing discoloration powder of doping, and the proportion that reversible temperature sensing discoloration powder dopes the heat conduction material is 1: 0.8-1.2, and the color-changing temperature nodes of the three are sequentially reduced and are respectively at 30 ℃, 40 ℃ and 60 ℃.
9. The slump retaining agent of ether polycarboxylic acid according to claim 6, wherein: the area of the contact section of the panel (3) in the high temperature discoloration layer, the transition discoloration layer and the low temperature discoloration layer (44) and the heat conduction is increased in sequence, and the colors of the high temperature discoloration layer, the transition discoloration layer and the low temperature discoloration layer (44) are strong in contrast.
10. The slump retaining agent of ether polycarboxylic acid according to claim 5, wherein: the temperature sensing middle part is made of transparent materials on the outer surface.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603996A (en) * | 2012-02-28 | 2012-07-25 | 武汉理工大学 | Ether type polycarboxylic acid slump retaining agent and preparation method thereof |
| CN109970385A (en) * | 2019-04-23 | 2019-07-05 | 刘翠芬 | One kind is super to protect the concrete water-reducing agent that collapses |
| CN110407985A (en) * | 2019-07-30 | 2019-11-05 | 广州建盛建材有限公司 | A kind of polycarboxylate water-reducer of Narrow Molecular Weight Distribution and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603996A (en) * | 2012-02-28 | 2012-07-25 | 武汉理工大学 | Ether type polycarboxylic acid slump retaining agent and preparation method thereof |
| CN109970385A (en) * | 2019-04-23 | 2019-07-05 | 刘翠芬 | One kind is super to protect the concrete water-reducing agent that collapses |
| CN110407985A (en) * | 2019-07-30 | 2019-11-05 | 广州建盛建材有限公司 | A kind of polycarboxylate water-reducer of Narrow Molecular Weight Distribution and preparation method thereof |
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