CN115960322A - Polycarboxylic acid viscosity reducer and preparation method thereof - Google Patents
Polycarboxylic acid viscosity reducer and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a polycarboxylic acid viscosity reducer and a preparation method thereof, wherein the viscosity reducer comprises the following components in parts by weight: 30-35 parts of prenyl alcohol polyoxyethylene ether, 1-5 parts of unsaturated carboxylic acid, 0.5-2 parts of unsaturated carboxylic ester, 0.1-2 parts of cationic monomer, 0.1-2 parts of double bond-containing silane coupling agent, 0.1-0.5 part of oxidant, 0.01-0.1 part of reducing agent, 0.05-0.3 part of chain transfer agent and 0.1-2 parts of neutralizer; wherein the mol ratio of the prenyl alcohol polyoxyethylene ether to the unsaturated carboxylic acid is 1:1.0 to 3.0. The viscosity reducer increases the thickness of a water film layer on the surface of cement particles from a self molecular structure, improves the content of free water, reduces the content of a residual water reducer in cement pore liquid, strengthens the surface activity capability of the cement pore liquid, and achieves the purpose of viscosity reduction. The viscosity reducer can obviously reduce the viscosity of concrete, improve the dispersibility, plasticity retention property and workability.
Description
Technical Field
The invention belongs to the field of building materials, and particularly relates to a polycarboxylic acid viscosity reducer and a preparation method thereof.
Background
Along with the rapid development of modern economy in China, the requirements of countries in the world on the building level and the quality of concrete are higher and higher, and the concrete serving as one of main materials of building engineering is also developed from the common direction to high strength and ultrahigh performance. The high-strength and ultra-high performance concrete is characterized by low water-cement ratio in composition; however, with the decrease of the water-cement ratio, the viscosity of the concrete mixture gradually increases, which causes a series of construction problems such as concrete stirring, transportation, pumping and the like, and greatly limits the popularization and application of high-strength and ultra-high performance concrete. In addition, because of the shortage of river sand resources, a large amount of machine-made sand is applied to the preparation of concrete, the machine-made sand has more edges and poorer gradation, so that the viscosity problem is more prominent, and the pumping and the construction of high-performance and ultrahigh-performance concrete are not facilitated. Therefore, the problem of high viscosity of high-strength and ultrahigh-performance concrete is difficult in concrete construction technology. Therefore, it is of great significance to research how to reduce the viscosity of concrete.
At present, a viscosity reduction method can be mainly developed from two aspects of organic additives and admixtures. The doped organic viscosity reducer mainly takes air-entraining performance as the main part, so that a large amount of micro closed bubbles are formed in the concrete mixture, and the bubbles can weaken the friction resistance among aggregate particles, thereby reducing the viscosity of the concrete; but the air-entraining and viscosity-reducing effects are limited and the strength of the concrete is adversely affected by adding too much air-entraining and viscosity-reducing agents. In the aspect of admixture, the working performance of concrete is improved mainly by adding silica fume, fly ash, micro-beads and the like, although the viscosity of concrete can be reduced by adding the admixture, the viscosity reduction effect of high-strength and ultra-high performance concrete is very limited and the cost is high, the cost of the concrete is increased, and the application of the concrete in the concrete is limited. Therefore, the development of novel polycarboxylic acid viscosity reducers is urgent. CN108299604B discloses a polycarboxylic acid viscosity reducer, the raw materials of which comprise basic raw materials, modified raw materials, an oxidant, a reducing agent and a chain transfer agent; the basic raw materials comprise terminal alkenyl polyether monomers and unsaturated carboxylic acid, and the modified raw materials comprise unsaturated carboxylic ester and alkyl carboxylic ester. Although the viscosity reducer has a good viscosity reducing effect, the viscosity reducer has a large limitation on the application range and has an unobvious adaptation effect on materials, particularly for the concrete mainly comprising machine-made sand at present; and the machine-made sand contains expansive soil components and has great influence on the performances of concrete dispersibility, plasticity retention and the like.
Disclosure of Invention
In order to solve the technical problems, the invention provides a polycarboxylic acid viscosity reducer. The viscosity reducer increases the thickness of a water film layer on the surface of cement particles from a self molecular structure, improves the content of free water, reduces the content of a residual water reducer in cement pore liquid, strengthens the surface activity capability of the cement pore liquid, and achieves the purpose of viscosity reduction.
The invention is realized by the following technical scheme:
a polycarboxylic acid viscosity reducer is characterized in that: the viscosity reducer comprises the following components in parts by weight: 30-35 parts of isoamylene alcohol polyoxyethylene ether, 1-5 parts of unsaturated carboxylic acid, 0.5-2 parts of unsaturated carboxylic ester, 0.1-2 parts of cationic monomer, 0.1-2 parts of double bond-containing silane coupling agent, 0.1-0.5 part of oxidant, 0.01-0.1 part of reducing agent, 0.05-0.3 part of chain transfer agent and 0.5-2 parts of neutralizer; wherein the mol ratio of the prenyl alcohol polyoxyethylene ether to the unsaturated carboxylic acid is 1:1.0 to 3.0.
The weight average molecular weight of the viscosity reducer is 1-3 ten thousand.
The weight average molecular weight of the prenol polyoxyethylene ether is 300-1200.
The unsaturated carboxylic acid comprises one or more of acrylic acid, methacrylic acid, maleic anhydride and fumaric acid.
The unsaturated carboxylic ester comprises one or more of methyl methacrylate, ethyl methacrylate, methyl acrylate, ethyl acrylate, monomethyl maleate and monomethyl fumarate.
The cationic monomer comprises one or more of tetramethylammonium chloride, methacryloyloxyethyl trimethylammonium chloride and dimethyl diallyl ammonium chloride.
The oxidant comprises one or more of hydrogen peroxide, potassium persulfate, ammonium persulfate and benzoyl peroxide, the reducing agent comprises one or more of sodium bisulfite, ferrous sulfate, sodium hydrosulfite and L-ascorbic acid, and the chain transfer agent comprises one or more of thioglycolic acid, 3-mercaptopropionic acid, 2-mercaptoethanol, sodium hypophosphite and dodecyl mercaptan.
The double-bond silane coupling agent is one or more of vinyl trimethylsilane, 3- (2, 3 epoxypropoxy) propyl methyldiethoxysilane, vinyl triethoxysilane and gamma-methacryloxypropyl trimethoxysilane.
The neutralizer comprises one or more of sodium hydroxide, potassium hydroxide, ethanolamine, triethylamine and AMP-95.
The invention further provides a preparation method of the polycarboxylic viscosity reducer, which comprises the following steps:
(1) Adding prenyl alcohol polyoxyethylene ether and water weighed according to the formula into a reaction kettle, continuously stirring until the prenyl alcohol polyoxyethylene ether and the water are completely dissolved, introducing nitrogen into the reaction kettle, removing air in the reaction kettle, then adding a silane coupling agent containing double bonds, and continuously stirring uniformly;
(2) Adding an oxidant into the reaction kettle, and continuously stirring for 5-10 minutes;
(3) Firstly, dropwise adding a mixed solution A of unsaturated carboxylic acid, unsaturated carboxylic ester, cationic monomer and deionized water into a reaction kettle at a constant speed, dropwise adding a mixed solution B of a reducing agent, a chain transfer agent and deionized water into the reaction kettle at a constant speed after 10min, and controlling the dropwise adding time of the solution A and the dropwise adding time of the solution B to be 2-3.5 h respectively;
(4) Continuously stirring, curing for 1-3h, cooling the temperature of the reaction kettle to 35 ℃ after the curing is finished, adding a neutralizing agent, adjusting the pH of the reactant to 5-7, and finally adjusting the concentration of the reactant to 40% -50% to obtain the polycarboxylic acid viscosity reducer.
The prenyl polyoxyethylene ether, the unsaturated carboxylic acid, the unsaturated carboxylic ester, the cationic monomer and the double-bond-containing silane coupling agent are used as polymerization raw materials and are subjected to free radical polymerization in an inert gas environment under the action of a chain transfer agent and a redox system.
Compared with the prior art, the invention has the following advantages:
1. the viscosity reducer has low energy consumption, small mixing amount and wide adaptability, and can obviously reduce the viscosity of concrete, improve the dispersibility, plasticity retention property and workability. The hydrophobic groups are gathered towards the surface of the water film layer and are directionally arranged on a liquid-gas interface of the bubbles, so that the surface tension is reduced, a plurality of micro bubbles are easily formed in the concrete mixture, the bubbles can generate the ball and the floatage effect, the relative sliding between cement particles and aggregate particles in fresh concrete is facilitated, and the workability of the concrete mixture is improved.
2. According to the invention, double-bond siloxane structure functional group molecules are introduced into the main chain of a polycarboxylic acid molecule and are subjected to copolymerization reaction with unsaturated carboxylic acid, polyoxyethylene ether and the like, the double-bond-containing silane coupling agent is a good chemical bond bonding monomer at present, and hydrolyzed silicic acid oligomers can be chemically bonded with silicate in cement, so that the surface bonding capability stronger than the adsorption effect is achieved, the dispersibility of low-activity cement is improved, and the anchoring capability is obviously improved;
3. according to the invention, by introducing a cationic group, and grafting a cationic functional monomer with a quaternary ammonium group and an unsaturated ethylene group to the methacryloyloxyethyl trimethyl ammonium chloride, the prepared polymer has the characteristics of low doping amount, good dispersibility, excellent plastic retention effect, early strength and the like;
4. the hydrophobic group monomer introduced by the invention has synergistic effect with hydrophilic groups, keeps the state of the water film stable, prevents the water film layer from permeating into cement particles, delays the hydration process to a certain extent, and ensures that the concrete has better state retention capability.
5. The preparation method of the viscosity reducer is convenient to operate, simple and feasible, strong in operability, high in production efficiency, safe and pollution-free in production process and easy for industrial production.
Detailed Description
The present invention will be described in detail below, and technical solutions in embodiments of the present invention will be clearly and completely described below. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1.
A polycarboxylic acid viscosity reducer comprises the following components in parts by mass: prenyl alcohol polyoxyethylene ether TPEG-400 g, acrylic acid 43.1g, methyl methacrylate 8g, methacryloyloxyethyl trimethyl ammonium chloride 15g, vinyl trimethyl silane 3.33g, hydrogen peroxide 1.8g, L-ascorbic acid 0.47g, mercaptoethanol 1.5g, sodium hydroxide 10g, deionized water 270g.
Example 2.
A polycarboxylic acid viscosity reducer comprises the following components in parts by mass: isopentenol polyoxyethylene ether TPEG-600:300g of vinyl trimethyl silane, 2.22g of vinyl trimethyl silane, 1.77g of hydrogen peroxide (the concentration is 27.5 percent), 42.7g of acrylic acid, 8g of methyl methacrylate, 15g of methacryloyloxyethyl trimethyl ammonium chloride, 0.45g of L-ascorbic acid, 1.6g of mercaptoethanol, 10g of sodium hydroxide and 270g of deionized water.
Example 3.
A preparation method of a polycarboxylic viscosity reducer comprises the following steps:
(1.) adding 300g of prenyl alcohol polyoxyethylene ether TPEG-800 and 200g of deionized water into a reaction kettle, introducing nitrogen, removing air in the reaction kettle, controlling the temperature of the reaction kettle to be 40 ℃, stirring until the prenyl alcohol polyoxyethylene ether TPEG-800 and the deionized water are completely dissolved, then adding 1.66g of vinyl trimethylsilane, and continuously stirring;
(2) Adding 1.8g of hydrogen peroxide (with the concentration of 27.5%) into a reaction kettle, and stirring for 5min;
(3) A mixed solution A of 42.7g of acrylic acid, 8g of methyl methacrylate, 15g of methacryloyloxyethyl trimethyl ammonium chloride and 20g of deionized water is dropwise added into a reaction kettle at a constant speed, after 10min, a mixed solution B of 0.45g of L-ascorbic acid, 1.65g of mercaptoethanol and 50g of deionized water is dropwise added at a constant speed, and the dropwise adding time of the solution A and the dropwise adding time of the solution B are respectively 2.5h and 3h.
(4) After the dripping is finished, keeping the temperature at 60 ℃ for continuous curing for 1h, after the curing is finished, starting circulating water, cooling to 35 ℃, adding 10g of sodium hydroxide (with the concentration of 32%) to neutralize the solution to 6 +/-1, and supplementing water to adjust the concentration to 50% to obtain the polycarboxylic acid viscosity reducer.
Example 4.
A preparation method of a polycarboxylic viscosity reducer comprises the following steps:
(1.) adding 300g of prenyl alcohol polyoxyethylene ether TPEG-1000 and 200g of deionized water into a reaction kettle, introducing nitrogen, stirring until the prenyl alcohol polyoxyethylene ether TPEG-1000 and the deionized water are completely dissolved, removing air in the reaction kettle, controlling the temperature of the reaction kettle to be 40 ℃, then adding 2.23g of gamma-methacryloxypropyl trimethoxysilane, and continuously stirring;
(2) Adding 1.8g of hydrogen peroxide (with the concentration of 27.5%) into a reaction kettle, and stirring for 5min;
(3) Dropwise adding a mixed solution of 34g of acrylic acid, 6g of methyl methacrylate, 13g of methacryloyloxyethyl trimethyl ammonium chloride and 20g of deionized water into the reaction kettle at a constant speed, controlling the time to be 2.5, dropwise adding a mixed solution of 0.55g of L-ascorbic acid, 1.72g of mercaptoethanol and 50g of deionized water into the reaction kettle at a constant speed after 10min, and completing dropwise adding for 3 h; .
(4) After the dripping is finished, keeping the temperature of 60 ℃ for continuous curing for 1h, starting circulating water, cooling to 40 ℃, then adding 10g of sodium hydroxide (with the concentration of 32%) solution for neutralization to 6 +/-1, and supplementing water to adjust the concentration to 50% to obtain the polycarboxylic acid viscosity reducer.
Example 5.
A preparation method of a polycarboxylic viscosity reducer comprises the following steps:
(1.) adding 300g of prenyl alcohol polyoxyethylene ether TPEG-1200 and 200g of deionized water into a reaction kettle, introducing nitrogen, stirring until the prenyl alcohol polyoxyethylene ether TPEG-1200 and the deionized water are completely dissolved, removing air in the reaction kettle, controlling the temperature of the reaction kettle to be 40 ℃, then adding 2.23g of gamma-methacryloxypropyl trimethoxysilane, and continuously stirring;
(2) Adding 1.84g of hydrogen peroxide (with the concentration of 27.5%) into a reaction kettle, and stirring for 5min;
(3) Dropwise adding a mixed solution of 34g of acrylic acid, 6g of methyl methacrylate, 13g of methacryloyloxyethyl trimethyl ammonium chloride and 20g of deionized water into the reaction kettle at a constant speed, controlling the time to be 2.5, dropwise adding a mixed solution of 0.5g of L-ascorbic acid, 1.2g of mercaptoethanol and 50g of deionized water into the reaction kettle at a constant speed after 10min, and completing dropwise adding for 3 h;
(4) After the dripping is finished, keeping the temperature of 60 ℃ for continuous curing for 1h, starting circulating water, cooling to 40 ℃, then adding 10g of sodium hydroxide (with the concentration of 32%) solution for neutralization to 6 +/-1, and supplementing water to adjust the concentration to 50% to obtain the polycarboxylic acid viscosity reducer.
Example 6.
(1.) adding 300g of prenyl alcohol polyoxyethylene ether TPEG-800 and 200g of deionized water into a reaction kettle, introducing nitrogen, stirring until the prenyl alcohol polyoxyethylene ether TPEG-800 and the deionized water are completely dissolved, removing air in the reaction kettle, controlling the temperature of the reaction kettle to be 40 ℃, then adding 2.79g of gamma-methacryloxypropyl trimethoxysilane, and continuously stirring;
(2) Adding 2.6g of ammonium persulfate into the reaction kettle, and stirring for 5min;
(3) Dropwise adding a mixed solution of 42.7g of acrylic acid, 8g of methyl methacrylate, 15g of methacryloyloxyethyl trimethyl ammonium chloride and 20g of deionized water into a reaction kettle at a constant speed, controlling the time to be 2.5h, dropwise adding a mixed solution of 0.48g of L-ascorbic acid, 1.8g of mercaptopropionic acid and 50g of deionized water into the reaction kettle at a constant speed after 10min, and completing dropwise adding for 3 h;
(4) After the dripping is finished, keeping the temperature at 60 ℃ for continuous curing for 1h, starting circulating water to cool to 40 ℃, then adding 10g of sodium hydroxide (with the concentration of 32%) solution for neutralization to 6 +/-1, and supplementing water to adjust the concentration to 50% to obtain the polycarboxylic acid viscosity reducer.
Comparative example 1
This comparative example is based on example 3, and no cationic monomer was added to prepare a polycarboxylic acid viscosity reducer.
A preparation method of a polycarboxylic viscosity reducer comprises the following steps:
(1.) adding 300g of prenyl alcohol polyoxyethylene ether TPEG-800 and 200g of deionized water into a reaction kettle, introducing nitrogen, removing air in the reaction kettle, controlling the temperature of the reaction kettle to be 40 ℃, stirring until the prenyl alcohol polyoxyethylene ether TPEG-800 and the deionized water are completely dissolved, then adding 1.72g of vinyl trimethylsilane, and continuously stirring;
(2) Adding 1.85g hydrogen peroxide (with a concentration of 27.5%) into the reaction kettle, and stirring for 5min;
(3) And dropwise adding a mixed solution A of 40.3g of acrylic acid, 16g of methyl methacrylate and 20g of deionized water into the reaction kettle at a constant speed, and after 10min, dropwise adding a mixed solution B of 0.48g of L-ascorbic acid, 1.62g of mercaptoethanol and 50g of deionized water at a constant speed, wherein the dropwise adding time of the solution A and the dropwise adding time of the solution B are 2.5h and 3h respectively.
(4) After the dropwise addition, keeping the temperature of 60 ℃ for continuous curing for 1h, after the curing is finished, starting circulating water, cooling to 35 ℃, adding 10g of sodium hydroxide (with the concentration of 32%) to neutralize the solution to 6 +/-1, and supplementing water to adjust the concentration to 50% to obtain the polycarboxylic acid viscosity reducer.
Comparative example 2
This comparative example was prepared without adding a double bond-containing silane coupling agent to the polycarboxylic acid viscosity reducer of example 3.
A preparation method of a polycarboxylic viscosity reducer comprises the following steps:
(1.) 300g of isopentenol polyoxyethylene ether TPEG-800 and 200g of deionized water are added into a reaction kettle, nitrogen is introduced, air in the reaction kettle is removed, the temperature of the reaction kettle is controlled at 40 ℃, stirring is carried out until the isopentenol polyoxyethylene ether TPEG-800 and the deionized water are completely dissolved, and stirring is continuously carried out;
(2) Adding 1.83g hydrogen peroxide (with a concentration of 27.5%) into the reaction kettle, and stirring for 5min;
(3) A mixed solution A of 41.5g of acrylic acid, 7.2g of methyl methacrylate, 15.3g of methacryloyloxyethyl trimethyl ammonium chloride and 20g of deionized water is dropwise added into a reaction kettle at a constant speed, after 10min, a mixed solution B of 0.5g of L-ascorbic acid, 1.61g of mercaptoethanol and 50g of deionized water is dropwise added at a constant speed, and the dropwise adding time of the solution A and the dropwise adding time of the solution B are respectively 2.5h and 3h.
(4) After the dripping is finished, keeping the temperature at 60 ℃ for continuous curing for 1h, after the curing is finished, starting circulating water, cooling to 35 ℃, adding 10g of sodium hydroxide (with the concentration of 32%) to neutralize the solution to 6 +/-1, and supplementing water to adjust the concentration to 50% to obtain the polycarboxylic acid viscosity reducer.
Comparative example 3
This comparative example was prepared without adding a double bond-containing silane coupling agent and a cationic monomer to the viscosity reducing agent of example 3.
A preparation method of a polycarboxylic viscosity reducer comprises the following steps:
(1.) adding 300g of prenyl alcohol polyoxyethylene ether TPEG-800 and 200g of deionized water into a reaction kettle, introducing nitrogen, removing air in the reaction kettle, controlling the temperature of the reaction kettle to be 40 ℃, stirring until the prenyl alcohol polyoxyethylene ether TPEG-800 and the deionized water are completely dissolved, and continuously stirring;
(2) Adding 1.8g of hydrogen peroxide (with the concentration of 27.5%) into a reaction kettle, and stirring for 5min;
(3) And dropwise adding a mixed solution A of 41.9g of acrylic acid, 13.8g of methyl methacrylate and 20g of deionized water into the reaction kettle at a constant speed, and dropwise adding a mixed solution B of 0.52g of L-ascorbic acid, 1.63g of mercaptoethanol and 50g of deionized water at a constant speed after 10min, wherein the dropwise adding time of the solution A and the dropwise adding time of the solution B are respectively 2.5h and 3h.
(4) After the dropwise addition, keeping the temperature of 60 ℃ for continuous curing for 1h, after the curing is finished, starting circulating water, cooling to 35 ℃, adding 10g of sodium hydroxide (with the concentration of 32%) to neutralize the solution to 6 +/-1, and supplementing water to adjust the concentration to 50% to obtain the polycarboxylic acid viscosity reducer.
1. Neat paste test example 1
The polycarboxylic acid viscosity reducer provided by the embodiments 1-6 and the comparative examples 1-3 of the invention is compared with the viscosity reducer PC-1 and the viscosity reducer PC-2 which are both 50% in concentration in the market, and the net slurry fluidity, the time loss and the Marsh time of the viscosity reducer are measured. The specific test mode is as follows:
the cement used in the experiment is 42.5 ordinary silica cement, and the initial fluidity and the time-dependent fluidity of the cement paste are tested by referring to GB 8077.
Test samples: water cement ratio 0.20
The mixing ratio of the clear paste is as follows: 500g of cement, 100g of water, 1g of polycarboxylic acid water reducing agent and viscosity reducer.
Automatic Marsh time measuring instrument method:
pouring cement paste which is uniformly stirred into a Marsh cylinder, ensuring that the cement paste is full and a cylinder opening is strickled off by a scraper, then opening a working switch to a working position, when the paste flows out of 200mL from a lower material nozzle, automatically stopping timing, and reading and recording the Marsh time which is the time on a display screen. The 60min time loss is from the first water adding time, stirring is carried out again after 60min, charging is carried out, and the net pulp fluidity and the Marsh time are tested again; the shorter the Marsh time, the better the flow properties of the slurry.
And (4) judging a result:
1. the dosage of the water reducing agent is fixed, and the shorter the Marsh time is under the condition of ensuring that the initial fluidity is basically consistent by adjusting the mixing amount of the viscosity reducing agent, the better the viscosity reducing effect of the viscosity reducing agent with small mixing amount is compared with the viscosity reducing agent with large mixing amount is shown.
2. Under the condition of ensuring that the initial fluidity is basically consistent under the same mixing amount, the shorter the Marsh time is, the better the effect of the viscosity reducer is. The results are shown in Table 1.
TABLE 1 neat cement fluidity test results and Marsh time for different viscosity reducers
And (4) conclusion:
1. as can be seen from the results in Table 1, the initial fluidity of the neat paste is designed to be basically consistent by adjusting the mixing amount of the viscosity reducer, the mixing amount of the viscosity reducer in the examples 1 to 6 is lower than that in the comparative examples, and the effect of the viscosity reducer and the plasticity retention of the neat paste are obviously superior to those of the comparative examples 1 to 3 and the viscosity reducers PC-1 and PC-2 on the market; the molecular structure is introduced with the silane coupling agent containing double bonds and the cationic group simultaneously, so that the viscosity of the cement paste can be obviously reduced, and an excellent plastic-retaining effect can be obtained.
2. Concrete test example 1
The polycarboxylic acid viscosity reducer provided by the embodiments 1-6 and the comparative examples 1-3 of the invention is compared with viscosity reducer PC-1 and viscosity reducer PC-2 on the market, and the test adopts the mixing ratio of the ultra-high performance concrete with the water cement ratio of 0.2, and the mixing ratio is shown in Table 2.
The test method comprises the following steps: the cement used in the test is Emei P.O 42.5 ordinary silicon cement, and 20L of concrete is mixed according to the relevant regulations of the national standard GB/T50080-2019 'common concrete mixture Performance test method'; keeping the dosage of the polycarboxylate superplasticizer unchanged, ensuring the initial state of the concrete to be basically consistent by adjusting the dosage of the viscosity reducer, and respectively testing the slump loss time of the mixture, the slump loss and the slump loss after initial slump loss and 60min time loss, the slump loss and the slump loss after 500mm time loss, wherein the results are shown in Table 3
TABLE 2 ultra high Performance concrete mix ratio (Kg/m) 3 )
TABLE 3 concrete mix Performance results
And (4) conclusion: as can be seen from the table 3, the slump and the extensibility of the concrete mixture are designed to be basically consistent by adjusting the mixing amount of the viscosity reducer, and the mixing amount of the viscosity reducer in the examples 1 to 6 is lower than that in the comparative examples; compared with comparative examples 1-3, the cross test proves that the viscosity reducer of the embodiment can obviously reduce the viscosity of concrete, improve the dispersibility and have good plasticity retention property by introducing the double-bond-containing silane coupling agent and the cationic group simultaneously.
Claims (10)
1. A polycarboxylic viscosity reducer is characterized in that: the viscosity reducer comprises the following components in parts by weight: 30-35 parts of prenyl alcohol polyoxyethylene ether, 1-5 parts of unsaturated carboxylic acid, 0.5-2 parts of unsaturated carboxylic ester, 0.1-2 parts of cationic monomer, 0.1-2 parts of double bond-containing silane coupling agent, 0.1-0.5 part of oxidant, 0.01-0.1 part of reducing agent, 0.05-0.3 part of chain transfer agent and 0.1-2 parts of neutralizer; wherein the mole ratio of the prenyl polyoxyethylene ether to the unsaturated carboxylic acid is 1:1.0 to 3.0.
2. The polycarboxylic acid-based viscosity reducer according to claim 1, having a weight average molecular weight of 1 to 3 ten thousand.
3. The polycarboxylic acid-based viscosity reducer according to claim 1 or 2, wherein the prenyl polyoxyethylene ether has a weight average molecular weight of 300 to 1200.
4. The polycarboxylic acid viscosity reducer according to claim 1 or 2, wherein the unsaturated carboxylic acid comprises one or more of acrylic acid, methacrylic acid, maleic anhydride and fumaric acid.
5. The polycarboxylic acid viscosity reducer according to claim 1 or 2, wherein the unsaturated carboxylic acid ester comprises one or more of methyl methacrylate, ethyl methacrylate, methyl acrylate, ethyl acrylate, monomethyl maleate and monomethyl fumarate.
6. The viscosity reducer according to claim 1 or 2, wherein the cationic monomer comprises one or more of tetramethylammonium chloride, methacryloyloxyethyl trimethylammonium chloride, and dimethyldiallylammonium chloride.
7. The polycarboxylic acid-based viscosity reducer according to claim 1 or 2, characterized in that: the oxidant comprises one or more of hydrogen peroxide, potassium persulfate, ammonium persulfate and benzoyl peroxide, the reducing agent comprises one or more of sodium bisulfite, ferrous sulfate, sodium bisulfite and L-ascorbic acid, and the chain transfer agent comprises one or more of thioglycolic acid, 3-mercaptopropionic acid, 2-mercaptoethanol, sodium hypophosphite and dodecyl mercaptan.
8. The viscosity reducer of claim 1 or 2, wherein the double bond-containing silane coupling agent is one or more of vinyltrimethylsilane, 3- (2, 3 glycidoxy) propylmethyldiethoxysilane, vinyltriethoxysilane, and γ -methacryloxypropyltrimethoxysilane.
9. The polycarboxylic acid viscosity reducer according to claim 1 or 2, wherein the neutralizing agent comprises one or more of sodium hydroxide, potassium hydroxide, ethanolamine, triethylamine, and AMP-95.
10. A process for producing a polycarboxylic acid viscosity reducer according to claim 1, characterized in that: the method comprises the following steps:
(1) Adding prenyl alcohol polyoxyethylene ether and water weighed according to the formula into a reaction kettle, continuously stirring until the prenyl alcohol polyoxyethylene ether and the water are completely dissolved, introducing nitrogen into the reaction kettle, then adding a silane coupling agent containing double bonds, and continuously stirring uniformly;
(2) Adding an oxidant into the reaction kettle, and continuously stirring for 5-10 minutes;
(3) Firstly, dropwise adding a mixed solution A of unsaturated carboxylic acid, unsaturated carboxylic ester, cationic monomer and deionized water into a reaction kettle at a constant speed, dropwise adding a mixed solution B of a reducing agent, a chain transfer agent and deionized water into the reaction kettle at a constant speed after 10min, and controlling the dropwise adding time of the solution A and the dropwise adding time of the solution B to be 2-3.5 h respectively;
(4) And (3) continuously stirring after the dropwise adding is finished, curing for 1-3h, cooling the temperature of the reaction kettle to 35 ℃ after the curing is finished, adding a neutralizing agent, adjusting the pH of the reactant to 5-7, and finally adjusting the concentration of the reactant to 40% -50% to obtain the polycarboxylic acid viscosity reducer.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116574223A (en) * | 2023-05-09 | 2023-08-11 | 贵州天威建材科技有限责任公司 | High-performance viscosity-reducing polycarboxylate superplasticizer and preparation method thereof |
| CN117164274A (en) * | 2023-11-03 | 2023-12-05 | 四川蜀道建筑科技有限公司 | Water reducer for mass concrete, preparation method and concrete |
| CN117819864A (en) * | 2024-03-04 | 2024-04-05 | 四川蜀道建筑科技有限公司 | Polycarboxylic acid high-performance water reducer |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116574223A (en) * | 2023-05-09 | 2023-08-11 | 贵州天威建材科技有限责任公司 | High-performance viscosity-reducing polycarboxylate superplasticizer and preparation method thereof |
| CN117164274A (en) * | 2023-11-03 | 2023-12-05 | 四川蜀道建筑科技有限公司 | Water reducer for mass concrete, preparation method and concrete |
| CN117164274B (en) * | 2023-11-03 | 2024-01-05 | 四川蜀道建筑科技有限公司 | Water reducer for mass concrete, preparation method and concrete |
| CN117819864A (en) * | 2024-03-04 | 2024-04-05 | 四川蜀道建筑科技有限公司 | Polycarboxylic acid high-performance water reducer |
| CN117819864B (en) * | 2024-03-04 | 2024-05-14 | 四川蜀道建筑科技有限公司 | Polycarboxylic acid high-performance water reducer |
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