CN110540620A - polycarboxylate superplasticizer and preparation method thereof - Google Patents
polycarboxylate superplasticizer and preparation method thereof Download PDFInfo
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- CN110540620A CN110540620A CN201910018135.3A CN201910018135A CN110540620A CN 110540620 A CN110540620 A CN 110540620A CN 201910018135 A CN201910018135 A CN 201910018135A CN 110540620 A CN110540620 A CN 110540620A
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- acrylic acid
- ammonium persulfate
- deionized water
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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
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2641—Polyacrylates; Polymethacrylates
- C04B24/2647—Polyacrylates; Polymethacrylates containing polyether side chains
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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
- 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 invention discloses a polycarboxylate superplasticizer and a preparation method thereof, wherein the polycarboxylate superplasticizer comprises methallyl alcohol polyoxyethylene ether, a material C, ammonium persulfate, acrylic acid, sodium hydroxide and deionized water, wherein the weight percentage of each component is as follows: 30-40% of methallyl alcohol polyoxyethylene ether, 0.1-1% of C material, 0.1-0.6% of ammonium persulfate, 2-10% of acrylic acid, 1-10% of sodium hydroxide and 50-65% of deionized water. The polycarboxylic acid water reducing agent is prepared by taking the methallyl alcohol polyoxyethylene ether, the material C, the ammonium persulfate, the acrylic acid and the sodium hydroxide as raw materials, and has the advantages of few raw material types, simple production process, low investment, company cost saving and better economic benefit.
Description
Technical Field
The invention belongs to the technical field, and particularly relates to a polycarboxylic acid water reducing agent and a preparation method thereof.
Background
In recent decades, the concrete engineering technology in China has made great progress, the performance of concrete mixtures is from dry hardness to plasticity and large fluidity, the strength of concrete is from medium and low strength to medium and high strength, and the comprehensive performance of concrete is developed from common performance to high performance. The application and development of the concrete admixture technology play a decisive role in the great technical progress of concrete engineering, and the development of the modern concrete technology is impossible without the application and development of the concrete admixture technology.
The concrete admixture is characterized in that: the mixing amount is small, the effect is large, and the effect on concrete is four points: firstly, the working performance of the fresh concrete is improved; secondly, the mechanical property of the hardened concrete is improved; thirdly, the durability of the concrete is improved; fourthly, cement is saved, and good economic benefit can be obtained. The new technology of modern concrete construction, such as rapid development and wide application of pumping concrete, fluid concrete, self-compacting concrete, high-strength and high-performance concrete, underwater undispersed concrete, sprayed concrete and the like, does not show the important function of an additive, and the additive becomes one of indispensable components in modern concrete.
The synthetic high-efficiency water reducing agent is the most important product in concrete admixtures, can be used independently or compounded with other products, the yield of the high-efficiency water reducing agent in China is the first of the world, wherein the high-efficiency water reducing agent of the naphthalene sulfonate formaldehyde condensate accounts for about 80 percent of the yield of the total synthetic high-efficiency water reducing agent, the production process of the naphthalene high-efficiency water reducing agent in China is mature and stable, the product is close to the foreign level, but more than half of enterprises are too small, the using amount of the high-concentration high-efficiency water reducing agent with better performance (the content of Na2SO4 is less than 5 percent), the production process of the naphthalene high-efficiency water reducing agent is complex, the investment is high, and the economic benefit is.
At present, the types and models of domestic cements are different, such as slag portland cement, pozzolana cement, fly ash portland cement and the like, and the cement performance difference is large due to different mixed materials doped into the cement, sometimes even the mixed materials which do not meet the requirements are doped, so that the cement adaptability is difficult to control. Therefore, how to synthesize the water reducing agent with better comprehensive performance is urgent to adapt to complicated domestic cement varieties and models, and the water reducing agent used in the current market has the defects of large mixing amount, poor water reducing performance and poor plasticizing effect and cannot meet the requirements of the market.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a polycarboxylate water reducer and a preparation method thereof, and solves the problems of complex production process, high investment, poor economic benefit and the like of a naphthalene water reducer in the prior art.
in order to solve the technical problem, the technical scheme of the invention is as follows: a polycarboxylate water reducing agent comprises methallyl alcohol polyoxyethylene ether, a material C, ammonium persulfate, acrylic acid, sodium hydroxide and deionized water, wherein the weight percentage of each component is as follows: 30-40% of methallyl alcohol polyoxyethylene ether, 0.1-1% of C material, 0.1-0.6% of ammonium persulfate, 2-10% of acrylic acid, 1-10% of sodium hydroxide and 50-65% of deionized water.
Preferably, the weight percentage of each component is as follows: 30-35% of methallyl alcohol polyoxyethylene ether, 0.1-0.6% of C material, 0.1-0.4% of ammonium persulfate, 3-6% of acrylic acid, 2-5% of sodium hydroxide and 55-60% of deionized water.
Preferably, the weight percentage of each component is as follows: 33% of methyl allyl alcohol polyoxyethylene ether, 0.4% of C material, 0.2% of ammonium persulfate, 4% of acrylic acid, 3% of sodium hydroxide and 59.4% of deionized water.
preferably, the preparation method of the polycarboxylate superplasticizer comprises the following steps:
Step 1), adding deionized water into a reaction kettle, heating to 40-50 ℃, and adding methallyl alcohol polyoxyethylene ether;
step 2) preparing ammonium persulfate and an acrylic acid solution, dissolving the ammonium persulfate in deionized water, wherein the content of the ammonium persulfate in the ammonium persulfate solution is 2-6%, and dissolving acrylic acid in the deionized water, wherein the content of the acrylic acid in the acrylic acid solution is 30-50%;
step 3), raising the temperature in the reaction kettle to 55-60 ℃, adding the material C, and stirring for 10 min;
step 4) dropping ammonium persulfate and an acrylic acid solution, wherein the dropping time of the ammonium persulfate solution is 2-3 h, the dropping time of the acrylic acid solution is 1.5-2.5 h, the temperature is maintained between 55-60 ℃ after the dropping is finished, and the temperature is kept for 1 h;
and 5) dissolving sodium hydroxide in deionized water, dripping the deionized water into the reaction kettle for 10min, and cooling the reaction kettle to prepare the polycarboxylic acid water reducer.
preferably, the temperature is increased to 45 ℃ in the step 1) and the temperature is increased to 57 ℃ in the step 3).
Preferably, in the step 4), the dropping time of the ammonium persulfate solution is 2.5 hours, the dropping time of the acrylic acid solution is 2 hours, and the temperature of the reaction kettle is 59 +/-2 ℃ when the ammonium persulfate solution and the acrylic acid solution are dropped.
Compared with the prior art, the invention has the advantages that:
(1) The invention takes methallyl alcohol polyoxyethylene ether, C material, ammonium persulfate, acrylic acid and sodium hydroxide as raw materials to prepare the polycarboxylic acid water reducing agent, wherein the C material is taken as an initiator and an oxidant to replace hydrogen peroxide (2% -3%), vitamin C/ascorbic acid (0.5% -0.7%) and mercaptopropionic acid (1.5% -2.5%) of the original water reducing agent, wherein the hydrogen peroxide and the mercaptopropionic acid belong to dangerous chemicals, so the invention reduces the types of the raw materials, ensures that the production process is safer and more reliable, has simple production process, less investment and lower company cost, and has better economic benefit;
(2) the invention has strong applicability, and can be mixed with different types or models of cement for use; the water reducing rate is high, the slump loss is small, the cohesiveness and the workability of concrete can be effectively improved, and the pumping requirement of concrete is met; meanwhile, the reinforcing effect is obvious, and the strength can be improved by more than 50 percent;
(3) The water reducing agent and the concrete material are compounded for use, so that the chemical corrosion resistance, the durability, the fluidity and the breaking strength of the concrete can be greatly improved, the water reducing agent can be widely applied to the construction of high-rise buildings, large-span bridges and other buildings, the working performance is excellent, the setting time of the concrete can be remarkably delayed, and the mixing amount is low.
Detailed Description
the following describes embodiments of the present invention with reference to examples:
It should be noted that the structures, proportions, sizes, and other elements shown in the specification are included for the purpose of understanding and reading only, and are not intended to limit the scope of the invention, which is defined by the claims, and any modifications of the structures, changes in the proportions and adjustments of the sizes, without affecting the efficacy and attainment of the same.
in addition, the terms "upper", "lower", "left", "right", "middle" and "one" used in the present specification are for clarity of description, and are not intended to limit the scope of the present invention, and the relative relationship between the terms and the terms is not to be construed as a scope of the present invention.
example 1
The invention discloses a polycarboxylate superplasticizer which comprises methallyl alcohol polyoxyethylene ether, a material C, ammonium persulfate, acrylic acid, sodium hydroxide and deionized water, wherein the weight percentage of each component is as follows: 30-40% of methallyl alcohol polyoxyethylene ether, 0.1-1% of C material, 0.1-0.6% of ammonium persulfate, 2-10% of acrylic acid, 1-10% of sodium hydroxide and 50-65% of deionized water.
Example 2
the invention discloses a polycarboxylate superplasticizer which comprises methallyl alcohol polyoxyethylene ether, a material C, ammonium persulfate, acrylic acid, sodium hydroxide and deionized water, wherein the weight percentage of each component is as follows: 30-40% of methallyl alcohol polyoxyethylene ether, 0.1-1% of C material, 0.1-0.6% of ammonium persulfate, 2-10% of acrylic acid, 1-10% of sodium hydroxide and 50-65% of deionized water.
Preferably, the weight percentage of each component is as follows: 30-35% of methallyl alcohol polyoxyethylene ether, 0.1-0.6% of C material, 0.1-0.4% of ammonium persulfate, 3-6% of acrylic acid, 2-5% of sodium hydroxide and 55-60% of deionized water.
example 3
The invention discloses a polycarboxylate superplasticizer which comprises methallyl alcohol polyoxyethylene ether, a material C, ammonium persulfate, acrylic acid, sodium hydroxide and deionized water, wherein the weight percentage of each component is as follows: 30-40% of methallyl alcohol polyoxyethylene ether, 0.1-1% of C material, 0.1-0.6% of ammonium persulfate, 2-10% of acrylic acid, 1-10% of sodium hydroxide and 50-65% of deionized water.
Preferably, the weight percentage of each component is as follows: 30-35% of methallyl alcohol polyoxyethylene ether, 0.1-0.6% of C material, 0.1-0.4% of ammonium persulfate, 3-6% of acrylic acid, 2-5% of sodium hydroxide and 55-60% of deionized water.
Preferably, the weight percentage of each component is as follows: 33% of methyl allyl alcohol polyoxyethylene ether, 0.4% of C material, 0.2% of ammonium persulfate, 4% of acrylic acid, 3% of sodium hydroxide and 59.4% of deionized water.
Example 4
The invention discloses a polycarboxylate superplasticizer which comprises methallyl alcohol polyoxyethylene ether, a material C, ammonium persulfate, acrylic acid, sodium hydroxide and deionized water, wherein the weight percentage of each component is as follows: 30-40% of methallyl alcohol polyoxyethylene ether, 0.1-1% of C material, 0.1-0.6% of ammonium persulfate, 2-10% of acrylic acid, 1-10% of sodium hydroxide and 50-65% of deionized water.
Preferably, the weight percentage of each component is as follows: 30-35% of methallyl alcohol polyoxyethylene ether, 0.1-0.6% of C material, 0.1-0.4% of ammonium persulfate, 3-6% of acrylic acid, 2-5% of sodium hydroxide and 55-60% of deionized water.
preferably, the weight percentage of each component is as follows: 33% of methyl allyl alcohol polyoxyethylene ether, 0.4% of C material, 0.2% of ammonium persulfate, 4% of acrylic acid, 3% of sodium hydroxide and 59.4% of deionized water.
Preferably, the preparation method of the polycarboxylate superplasticizer comprises the following steps:
Step 1), adding deionized water into a reaction kettle, heating to 40-50 ℃, and adding methallyl alcohol polyoxyethylene ether;
Step 2) preparing ammonium persulfate and an acrylic acid solution, dissolving the ammonium persulfate in deionized water, wherein the content of the ammonium persulfate in the ammonium persulfate solution is 2-6%, and dissolving acrylic acid in the deionized water, wherein the content of the acrylic acid in the acrylic acid solution is 30-50%;
Step 3), raising the temperature in the reaction kettle to 55-60 ℃, adding the material C, and stirring for 10 min;
step 4) dropping ammonium persulfate and an acrylic acid solution, wherein the dropping time of the ammonium persulfate solution is 2-3 h, the dropping time of the acrylic acid solution is 1.5-2.5 h, the temperature is maintained between 55-60 ℃ after the dropping is finished, and the temperature is kept for 1 h;
and 5) dissolving sodium hydroxide in deionized water, dripping the deionized water into the reaction kettle for 10min, and cooling the reaction kettle to prepare the polycarboxylic acid water reducer.
Example 5
The invention discloses a polycarboxylate superplasticizer which comprises methallyl alcohol polyoxyethylene ether, a material C, ammonium persulfate, acrylic acid, sodium hydroxide and deionized water, wherein the weight percentage of each component is as follows: 30-40% of methallyl alcohol polyoxyethylene ether, 0.1-1% of C material, 0.1-0.6% of ammonium persulfate, 2-10% of acrylic acid, 1-10% of sodium hydroxide and 50-65% of deionized water.
preferably, the weight percentage of each component is as follows: 30-35% of methallyl alcohol polyoxyethylene ether, 0.1-0.6% of C material, 0.1-0.4% of ammonium persulfate, 3-6% of acrylic acid, 2-5% of sodium hydroxide and 55-60% of deionized water.
Preferably, the weight percentage of each component is as follows: 33% of methyl allyl alcohol polyoxyethylene ether, 0.4% of C material, 0.2% of ammonium persulfate, 4% of acrylic acid, 3% of sodium hydroxide and 59.4% of deionized water.
Preferably, the preparation method of the polycarboxylate superplasticizer comprises the following steps:
step 1), adding deionized water into a reaction kettle, heating to 40-50 ℃, and adding methallyl alcohol polyoxyethylene ether;
step 2) preparing ammonium persulfate and an acrylic acid solution, dissolving the ammonium persulfate in deionized water, wherein the content of the ammonium persulfate in the ammonium persulfate solution is 2-6%, and dissolving acrylic acid in the deionized water, wherein the content of the acrylic acid in the acrylic acid solution is 30-50%;
step 3), raising the temperature in the reaction kettle to 55-60 ℃, adding the material C, and stirring for 10 min;
Step 4) dropping ammonium persulfate and an acrylic acid solution, wherein the dropping time of the ammonium persulfate solution is 2-3 h, the dropping time of the acrylic acid solution is 1.5-2.5 h, the temperature is maintained between 55-60 ℃ after the dropping is finished, and the temperature is kept for 1 h;
And 5) dissolving sodium hydroxide in deionized water, dripping the deionized water into the reaction kettle for 10min, and cooling the reaction kettle to prepare the polycarboxylic acid water reducer.
Preferably, the temperature in step 1) is increased to 45 ℃.
Example 6
The invention discloses a polycarboxylate superplasticizer which comprises methallyl alcohol polyoxyethylene ether, a material C, ammonium persulfate, acrylic acid, sodium hydroxide and deionized water, wherein the weight percentage of each component is as follows: 30-40% of methallyl alcohol polyoxyethylene ether, 0.1-1% of C material, 0.1-0.6% of ammonium persulfate, 2-10% of acrylic acid, 1-10% of sodium hydroxide and 50-65% of deionized water.
Preferably, the weight percentage of each component is as follows: 30-35% of methallyl alcohol polyoxyethylene ether, 0.1-0.6% of C material, 0.1-0.4% of ammonium persulfate, 3-6% of acrylic acid, 2-5% of sodium hydroxide and 55-60% of deionized water.
preferably, the weight percentage of each component is as follows: 33% of methyl allyl alcohol polyoxyethylene ether, 0.4% of C material, 0.2% of ammonium persulfate, 4% of acrylic acid, 3% of sodium hydroxide and 59.4% of deionized water.
Preferably, the preparation method of the polycarboxylate superplasticizer comprises the following steps:
Step 1), adding deionized water into a reaction kettle, heating to 40-50 ℃, and adding methallyl alcohol polyoxyethylene ether;
Step 2) preparing ammonium persulfate and an acrylic acid solution, dissolving the ammonium persulfate in deionized water, wherein the content of the ammonium persulfate in the ammonium persulfate solution is 2-6%, and dissolving acrylic acid in the deionized water, wherein the content of the acrylic acid in the acrylic acid solution is 30-50%;
step 3), raising the temperature in the reaction kettle to 55-60 ℃, adding the material C, and stirring for 10 min;
Step 4) dropping ammonium persulfate and an acrylic acid solution, wherein the dropping time of the ammonium persulfate solution is 2-3 h, the dropping time of the acrylic acid solution is 1.5-2.5 h, the temperature is maintained between 55-60 ℃ after the dropping is finished, and the temperature is kept for 1 h;
And 5) dissolving sodium hydroxide in deionized water, dripping the deionized water into the reaction kettle for 10min, and cooling the reaction kettle to prepare the polycarboxylic acid water reducer.
Preferably, the temperature in step 1) is increased to 45 ℃.
Preferably, the temperature in said step 3) is raised to 57 ℃.
Preferably, in the step 4), the dropping time of the ammonium persulfate solution is 2.5 hours, the dropping time of the acrylic acid solution is 2 hours, and the temperature of the reaction kettle is 59 +/-2 ℃ when the ammonium persulfate solution and the acrylic acid solution are dropped.
Example 7
Step 1), 488kg of deionized water is added into a reaction kettle, the temperature is raised to 40 ℃, and 300kg of methallyl alcohol polyoxyethylene ether is added;
Step 2) preparing ammonium persulfate and acrylic acid solution, dissolving 1kg of ammonium persulfate in 40kg of deionized water, and dissolving 20kg of acrylic acid in 40kg of deionized water;
Step 3), heating the temperature in the reaction kettle to 55 ℃, adding the 1kgC material, and stirring for 10 min;
Step 4) dropping ammonium persulfate and an acrylic acid solution, wherein the dropping time of the ammonium persulfate solution is 2 hours, the dropping time of the acrylic acid solution is 1.5 hours, the temperature of the reaction kettle is 59 +/-2 ℃ when the ammonium persulfate and the acrylic acid solution are dropped, the temperature is maintained between 55 and 60 ℃ after the dropping is finished, and the temperature is kept for 1 hour;
And 5) dissolving 10kg of sodium hydroxide in 100kg of deionized water, dripping into the reaction kettle for 10min, and cooling the reaction kettle to prepare the polycarboxylic acid water reducing agent.
Example 8
Step 1) adding 300kg of deionized water into a reaction kettle, heating to 50 ℃, and adding 400kg of methallyl alcohol polyoxyethylene ether;
Step 2) preparing ammonium persulfate and acrylic acid solution, dissolving 4kg of ammonium persulfate in 50kg of deionized water, and dissolving 40kg of acrylic acid in 80kg of deionized water;
step 3), raising the temperature in the reaction kettle to 60 ℃, adding the 6kgC material, and stirring for 10 min;
Step 4) dropping ammonium persulfate and acrylic acid solution, wherein the dropping time of the ammonium persulfate solution is 3 hours, the dropping time of the acrylic acid solution is 2.5 hours, the temperature of the reaction kettle is 59 +/-2 ℃ when the ammonium persulfate and the acrylic acid solution are dropped, the temperature is maintained at 57 ℃ after the dropping is finished, and the temperature is kept for 1 hour;
and 5) dissolving 20kg of sodium hydroxide in 100kg of deionized water, dripping into the reaction kettle for 10min, and cooling the reaction kettle to prepare the polycarboxylic acid water reducing agent.
example 9
step 1), adding 240kg of deionized water into a reaction kettle, heating to 50 ℃, and adding 330kg of methallyl alcohol polyoxyethylene ether;
step 2) preparing ammonium persulfate and acrylic acid solution, dissolving 3kg of ammonium persulfate in 55kg of deionized water, and dissolving 60kg of acrylic acid in 110kg of deionized water;
Step 3), raising the temperature in the reaction kettle to 60 ℃, adding the 2kgC material, and stirring for 10 min;
step 4) dropping ammonium persulfate and acrylic acid solution, wherein the dropping time of the ammonium persulfate solution is 2.5h, the dropping time of the acrylic acid solution is 2h, the temperature of the reaction kettle is maintained at 55 ℃ after the dropping of the ammonium persulfate and the acrylic acid solution is completed at 59 +/-2 ℃, and the temperature is kept for 1 h;
And 5) dissolving 50kg of sodium hydroxide in 150kg of deionized water, dripping into the reaction kettle for 10min, and cooling the reaction kettle to prepare the polycarboxylic acid water reducing agent.
Example 10
Step 1), 216kg of deionized water is added into a reaction kettle, the temperature is raised to 50 ℃, and 350kg of methallyl alcohol polyoxyethylene ether is added;
step 2) preparing ammonium persulfate and acrylic acid solution, dissolving 4kg of ammonium persulfate in 70kg of deionized water, and dissolving 30kg of acrylic acid in 70kg of deionized water;
step 3), heating the temperature in the reaction kettle to 57 ℃, adding 10kgC materials, and stirring for 10 min;
Step 4) dropping ammonium persulfate and acrylic acid solution, wherein the dropping time of the ammonium persulfate solution is 3 hours, the dropping time of the acrylic acid solution is 2.5 hours, the temperature of the reaction kettle is 59 +/-2 ℃ when the ammonium persulfate and the acrylic acid solution are dropped, the temperature is maintained at 60 ℃ after the dropping is finished, and the temperature is kept for 1 hour;
And 5) dissolving 100kg of sodium hydroxide in 150kg of deionized water, dripping into the reaction kettle for 10min, and cooling the reaction kettle to prepare the polycarboxylic acid water reducing agent.
example 11
Step 1), adding 354kg of deionized water into a reaction kettle, heating to 45 ℃, and adding 330kg of methallyl alcohol polyoxyethylene ether;
step 2) preparing ammonium persulfate and acrylic acid solution, dissolving 2kg of ammonium persulfate in 60kg of deionized water, and dissolving 40kg of acrylic acid in 60kg of deionized water;
Step 3), heating the temperature in the reaction kettle to 57 ℃, adding 4kgC materials, and stirring for 10 min;
Step 4) dropping ammonium persulfate and acrylic acid solution, wherein the dropping time of the ammonium persulfate solution is 3 hours, the dropping time of the acrylic acid solution is 2.5 hours, the temperature of the reaction kettle is 59 +/-2 ℃ when the ammonium persulfate and the acrylic acid solution are dropped, the temperature is maintained at 58 ℃ after the dropping is finished, and the temperature is kept for 1 hour;
And 5) dissolving 30kg of sodium hydroxide in 120kg of deionized water, dripping into the reaction kettle for 10min, and cooling the reaction kettle to prepare the polycarboxylic acid water reducing agent.
The invention discloses a polycarboxylic acid water reducer homogeneity detection method, and sets two groups of comparison tests, wherein the comparison tests are used for detecting the existing water reducers of different types, and the detection results are shown in table 1:
TABLE 1 examples 7 to 11 examination of homogeneity of polycarboxylic acid water reducing agent
| examples | Density (g/ml) | pH value | content of solid% | The water reduction rate% | the bleeding rate is% |
| Example 7 | 1.064 | 3.2 | 40.1 | 30 | 25 |
| example 8 | 1.060 | 3.3 | 40.3 | 32 | 24 |
| Example 9 | 1.071 | 3.2 | 40.2 | 34 | 25 |
| Example 10 | 1.070 | 3.1 | 40.4 | 33 | 24 |
| Example 11 | 1.075 | 3.0 | 40.5 | 35 | 22 |
| Comparative experiment 1 | 1.002 | 4.8 | 36.8 | 25 | 35 |
| comparative experiment 2 | 1.005 | 4.3 | 37.5 | 22 | 37 |
as can be seen from Table 1, the density of the polycarboxylate superplasticizer of the invention is greater than 1.060g/ml, the pH value is less than 3.3, the solid content is greater than 40.1%, the water reducing rate is greater than 30%, the bleeding rate is less than 25%, the density of comparative experiments 1 and 2 is less than that of the polycarboxylate superplasticizer of the invention, the pH value is greater than that of the polycarboxylate superplasticizer of the invention, the solid content is less than that of the polycarboxylate superplasticizer of the invention, the water reducing rate is less than that of the polycarboxylate superplasticizer of the invention, and the bleeding rate is greater than that of the polycarboxylate superplasticizer of the invention, therefore, the polycarboxylate superplasticizer of the invention has obviously better properties than that of the existing.
The polycarboxylic acid water reducing agent is applied to the materials required by the determination experiment of the fluidity of cement paste when the polycarboxylic acid water reducing agent is applied to cement: 300 g of cement and 87 g of water, and measuring the net slurry fluidity data of which the mixing amount is 0.3 percent of the mass by adopting a circular cutting and sawing die (upper 36mm and lower 64 mm); the cement is Jidong P042.5, conch P042.5, and shenwei P042.5; the water is tap water (5 kg of the same batch); 10g of each of examples 10 and 11 was taken, and a comparative test was set up to detect the presence of different types of water reducing agents, the results of which are shown in Table 2:
TABLE 2 examples 10 to 11 examination of the homogeneity of the polycarboxylic acid water reducing agent
as can be seen from Table 2, the initial values of the fluidity of the polycarboxylate water reducer of the invention are all higher than that of the existing water reducer, and can reach 265mm at most, and are still higher than that of the existing water reducer after 30min and 1h, and the fluidity value after 1h is all larger than 235mm, and for different cements, the polycarboxylate water reducer of the invention can achieve higher fluidity.
the polycarboxylic acid water reducing agent is prepared into concrete strength tests, and the concrete strength tests require the following materials: 376g of Jidong P042.5, 766g of sand and 200g of other additives, the use amounts of the polycarboxylic acid water reducing agents in the examples 7 to 11 are all 5%, a comparison test is set, the comparison test detects that the water reducing agents of different types exist, the use amount is also 5%, strength values in 7 days and 28 days are obtained, and the test results are shown in Table 3:
table 3 concrete strength test of examples 7 to 11 using polycarboxylate superplasticizer
as can be seen from Table 3, the strength of the concrete prepared by the polycarboxylate superplasticizer of the invention is higher than that of the existing superplasticizer, the strength value after 7 days can reach 46.9MPa, the strength value after 28 days can reach 50.7MPa, the strength is higher, the performance is excellent, the quality is good, and the concrete meets the construction requirements.
The reaction equation of the polycarboxylic acid water reducing agent is as follows:
CH＝C(CH(CHO(CHCHO)H+HO+NaHPO+{(NH)SO+HO}+ {CHO+HO}+NaOH
→
The invention takes methallyl alcohol polyoxyethylene ether, C material, ammonium persulfate, acrylic acid and sodium hydroxide as raw materials to prepare the polycarboxylic acid water reducing agent, wherein the C material is taken as an initiator and an oxidant to replace hydrogen peroxide (2-3%), vitamin C/ascorbic acid (0.5-0.7%) and mercaptopropionic acid (1.5-2.5%) of the original water reducing agent, and the hydrogen peroxide and the mercaptopropionic acid belong to dangerous chemicals.
the invention has strong applicability, and can be mixed with different types or models of cement for use; the water reducing rate is high and can reach 20-30%, the slump loss is small, the cohesiveness and the workability of concrete can be effectively improved, and the pumping requirement of concrete is met; meanwhile, the reinforcing effect is obvious, and the strength can be improved by more than 50%.
the water reducing agent and the concrete material are compounded for use, so that the chemical corrosion resistance, the durability, the fluidity and the breaking strength of the concrete can be greatly improved, the water reducing agent can be widely applied to the construction of high-rise buildings, large-span bridges and other buildings, the working performance is excellent, the setting time of the concrete can be remarkably delayed, and the mixing amount is low.
While the preferred embodiments of the present invention have been described in detail, the present invention is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present invention within the knowledge of those skilled in the art.
Many other changes and modifications can be made without departing from the spirit and scope of the invention. It is to be understood that the invention is not to be limited to the specific embodiments, but only by the scope of the appended claims.
Claims (6)
1. A polycarboxylate water reducing agent is characterized in that: the paint consists of methallyl alcohol polyoxyethylene ether, a material C, ammonium persulfate, acrylic acid, sodium hydroxide and deionized water, wherein the weight percentage of each component is as follows: 30-40% of methallyl alcohol polyoxyethylene ether, 0.1-1% of C material, 0.1-0.6% of ammonium persulfate, 2-10% of acrylic acid, 1-10% of sodium hydroxide and 50-65% of deionized water.
2. the polycarboxylate water reducer according to claim 1, characterized in that: the weight percentage of each component is as follows: 30-35% of methallyl alcohol polyoxyethylene ether, 0.1-0.6% of C material, 0.1-0.4% of ammonium persulfate, 3-6% of acrylic acid, 2-5% of sodium hydroxide and 55-60% of deionized water.
3. the polycarboxylate water reducer according to claim 2, characterized in that: the weight percentage of each component is as follows: 33% of methyl allyl alcohol polyoxyethylene ether, 0.4% of C material, 0.2% of ammonium persulfate, 4% of acrylic acid, 3% of sodium hydroxide and 59.4% of deionized water.
4. The preparation method of the polycarboxylate superplasticizer according to claim 1, characterized by comprising the following steps:
step 1), adding deionized water into a reaction kettle, heating to 40-50 ℃, and adding methallyl alcohol polyoxyethylene ether;
step 2) preparing ammonium persulfate and an acrylic acid solution, dissolving the ammonium persulfate in deionized water, wherein the content of the ammonium persulfate in the ammonium persulfate solution is 2-6%, and dissolving acrylic acid in the deionized water, wherein the content of the acrylic acid in the acrylic acid solution is 30-50%;
Step 3), raising the temperature in the reaction kettle to 55-60 ℃, adding the material C, and stirring for 10 min;
Step 4) dropping ammonium persulfate and an acrylic acid solution, wherein the dropping time of the ammonium persulfate solution is 2-3 h, the dropping time of the acrylic acid solution is 1.5-2.5 h, the temperature is maintained between 55-60 ℃ after the dropping is finished, and the temperature is kept for 1 h;
And 5) dissolving sodium hydroxide in deionized water, dripping the deionized water into the reaction kettle for 10min, and cooling the reaction kettle to prepare the polycarboxylic acid water reducer.
5. The preparation method of the polycarboxylate water reducer according to claim 4, characterized by comprising the following steps: the temperature in the step 1) is increased to 45 ℃, and the temperature in the step 3) is increased to 57 ℃.
6. The preparation method of the polycarboxylate water reducer according to claim 4, characterized by comprising the following steps: in the step 4), the dropping time of the ammonium persulfate solution is 2.5h, the dropping time of the acrylic acid solution is 2h, and the temperature of the reaction kettle is 59 +/-2 ℃ when the ammonium persulfate solution and the acrylic acid solution are dropped.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757539A (en) * | 2011-04-26 | 2012-10-31 | 上饶市天佳新型材料有限公司 | Preparation method of polycarboxylic acid high-performance water reducing agent |
| CN104371076A (en) * | 2014-12-04 | 2015-02-25 | 河北铁园科技发展有限公司 | Method of synthesizing polycarboxylate superplasticizer at normal temperature |
| CN105524230A (en) * | 2015-12-24 | 2016-04-27 | 湖南铭煌科技发展有限公司 | Preparation method of polycarboxylate superplasticizer |
| CN106699982A (en) * | 2015-07-20 | 2017-05-24 | 石家庄市海森化工有限公司 | Polycarboxylate superplasticizer for ceramic and preparation method of polycarboxylate superplasticizer |
| CN107987223A (en) * | 2017-11-30 | 2018-05-04 | 湖北工业大学 | A kind of ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic and preparation method |
| CN108751774A (en) * | 2018-04-24 | 2018-11-06 | 安徽海螺建材设计研究院有限责任公司 | A kind of preparation method of concrete prefabricated element polycarboxylate water-reducer |
| CN109021182A (en) * | 2018-08-30 | 2018-12-18 | 上海东大化学有限公司 | Polycarboxylate water-reducer and its preparation method and application from environment-friendly tasteless raw material |
-
2019
- 2019-01-09 CN CN201910018135.3A patent/CN110540620A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102757539A (en) * | 2011-04-26 | 2012-10-31 | 上饶市天佳新型材料有限公司 | Preparation method of polycarboxylic acid high-performance water reducing agent |
| CN104371076A (en) * | 2014-12-04 | 2015-02-25 | 河北铁园科技发展有限公司 | Method of synthesizing polycarboxylate superplasticizer at normal temperature |
| CN106699982A (en) * | 2015-07-20 | 2017-05-24 | 石家庄市海森化工有限公司 | Polycarboxylate superplasticizer for ceramic and preparation method of polycarboxylate superplasticizer |
| CN105524230A (en) * | 2015-12-24 | 2016-04-27 | 湖南铭煌科技发展有限公司 | Preparation method of polycarboxylate superplasticizer |
| CN107987223A (en) * | 2017-11-30 | 2018-05-04 | 湖北工业大学 | A kind of ester modified high-adaptability polycarboxylate water-reducer of alkyl acrylic and preparation method |
| CN108751774A (en) * | 2018-04-24 | 2018-11-06 | 安徽海螺建材设计研究院有限责任公司 | A kind of preparation method of concrete prefabricated element polycarboxylate water-reducer |
| CN109021182A (en) * | 2018-08-30 | 2018-12-18 | 上海东大化学有限公司 | Polycarboxylate water-reducer and its preparation method and application from environment-friendly tasteless raw material |
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