CN114105517A - Polycarboxylic acid high-performance water reducing agent - Google Patents
Polycarboxylic acid high-performance water reducing agent Download PDFInfo
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- CN114105517A CN114105517A CN202111502493.5A CN202111502493A CN114105517A CN 114105517 A CN114105517 A CN 114105517A CN 202111502493 A CN202111502493 A CN 202111502493A CN 114105517 A CN114105517 A CN 114105517A
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- polycarboxylic acid
- water reducing
- reducing agent
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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
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
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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
Abstract
The application belongs to the technical field of water reducing agents, and particularly relates to a polycarboxylic acid high-performance water reducing agent which comprises the following components in parts by weight: 8-15% of polycarboxylic acid water reducing agent, 0.5-3% of retarder, 0.01-0.1% of thixotropic agent, 0.01-0.05% of foam stabilizer, 0.01-0.05% of air entraining agent and the balance of water. The polycarboxylic acid high-performance water reducing agent is compounded with a polycarboxylic acid water reducing agent, a retarder, a thixotropic agent, a foam stabilizer, an air entraining agent and the like, and the polycarboxylic acid water reducing agent and other additives are uniformly mixed in advance, so that the stability is good, the mixing amount range is wider, and the metering of the polycarboxylic acid water reducing agent is facilitated.
Description
Technical Field
The application belongs to the technical field of water reducing agents, and particularly relates to a polycarboxylic acid high-performance water reducing agent.
Background
The polycarboxylate superplasticizer is an additive widely applied to concrete for dispersing cement, and gradually replaces some traditional superplasticizers due to the advantages of less addition amount, higher water reducing rate, good slump retaining performance, lower concrete shrinkage, adjustable molecular structure, no formaldehyde in the production process and the like after being successfully researched and developed by Japan from the eighties of the twentieth century.
Chinese patent document CN 105504175 a discloses a polycarboxylic acid water reducing agent with polyacrylic acid as a side chain, which is introduced into the side face of a comb-shaped structure to increase the affinity of the water reducing agent molecules to cement particles and improve the dispersibility of the cement particles. However, the addition of the polycarboxylate water reducer is difficult to be effectively controlled because the addition amount of the polycarboxylate water reducer in concrete is generally low and the compatibility with other concrete admixtures is relatively poor.
In view of this, it is necessary to improve the overall stability of the polycarboxylic acid water reducing agent and widen the addition amount of the polycarboxylic acid water reducing agent by compounding other additives with the polycarboxylic acid water reducing agent.
Disclosure of Invention
In order to solve the problems, the application discloses a polycarboxylic acid high-performance water reducing agent, which is prepared by compounding a polycarboxylic acid water reducing agent with a retarder, a thixotropic agent, a foam stabilizer, an air entraining agent and the like, and uniformly mixing the polycarboxylic acid water reducing agent with other additives in advance, so that the polycarboxylic acid high-performance water reducing agent is good in stability, wider in mixing amount range and beneficial to metering of the polycarboxylic acid water reducing agent.
The application provides a polycarboxylic acid high-performance water reducing agent, which adopts the following technical scheme:
a polycarboxylic acid high-performance water reducing agent comprises the following components in percentage by mass:
8 to 15 percent of polycarboxylic acid water reducing agent
0.5 to 3 percent of retarder
0.01 to 0.1 percent of thixotropic agent
Foam stabilizer 0.01-0.05%
0.01 to 0.05 percent of air entraining agent
The balance of water.
The polycarboxylate superplasticizer is compounded with the retarder, the thixotropic agent, the foam stabilizer, the air entraining agent and the like, and the polycarboxylate superplasticizer is uniformly mixed with other additives in advance, so that the stability is good, the mixing amount range is wider, and the metering of the polycarboxylate superplasticizer is facilitated.
Specifically, the structural formula of the polycarboxylic acid water reducing agent is as follows:
wherein a, b and c are integers from 1 to 30, and n is an integer from 10 to 30.
Naphthalene ring and benzene ring structures containing large steric hindrance are introduced into the structure of the polycarboxylate water reducer, so that the dispersing effect can be remarkably improved, meanwhile, the benzene ring and the naphthalene ring at the tail end of the side chain are beneficial to improving the stability of the side chain, and the phenomenon that the dispersing effect is reduced again due to the curling or winding of the side chain after initial dispersing is avoided. In addition, the side chain introduces an N-phenyl-alpha-naphthylamine structure similar to the anti-aging agent A, which is beneficial to improving the aging resistance of concrete and prolonging the service life of the concrete.
Specifically, the preparation method of the polycarboxylic acid water reducing agent comprises the following steps:
s1, mixing methyl 3- [4- (naphthalene-1-amino) phenyl ] propionate and 15-hexadecenol
Performing ester exchange reaction to obtain an anti-aging monomer; the reaction equation is:
s2, adding an acrylic monomer, an unsaturated polyether macromonomer and the anti-aging monomer prepared in the step (1) into a polymerization kettle for polymerization reaction to obtain the polycarboxylic acid water reducing agent, wherein the reaction equation is as follows:
specifically, the unsaturated polyether macromonomer is prenyl polyoxyethylene ether.
Specifically, the specific method of step S1 includes: starting nitrogen protection, putting 3- [4- (naphthalene-1-amino) phenyl ] methyl propionate and 15-hexadecenol into an ester exchange kettle according to the molar ratio of 1:1-1.2 for ester exchange reaction, adding a small amount of tetrabutyl titanate catalyst, stirring and reacting at 140 ℃ and 150 ℃ until the amount of collected methanol reaches 80-85% of a theoretical calculated value, and obtaining the anti-aging monomer.
Specifically, the specific method of step S2 includes: adding unsaturated polyether macromonomer and water into a reaction kettle, heating to 50-60 ℃, adding acrylic monomer, anti-aging monomer, chain transfer agent and initiator into the reaction kettle under stirring, reacting for 1-2h, naturally cooling the reactant, and adding sodium hydroxide solution to adjust the pH value to 6.0-6.5.
Specifically, the retarder is one or more of polyalcohol and derivatives thereof, inorganic phosphate and hydroxyl carboxylate.
Specifically, the thixotropic agent is one or more of magnesium aluminum silicate, fumed silica and bentonite.
Specifically, the foam stabilizer is one or more of xanthan gum, polyvinyl alcohol and polyacrylamide.
Specifically, the air entraining agent is one or more of triterpenoid saponin, sodium alkyl benzene sulfonate and sodium alkyl sulfonate.
The application has the following beneficial effects:
(1) the polycarboxylic acid high-performance water reducing agent is compounded with a polycarboxylic acid water reducing agent, a retarder, a thixotropic agent, a foam stabilizer, an air entraining agent and the like, and the polycarboxylic acid water reducing agent and other additives are uniformly mixed in advance, so that the stability is good, the mixing amount range is wider, and the metering of the polycarboxylic acid water reducing agent is facilitated.
(2) This application introduces naphthalene ring and benzene ring structure that contains big steric hindrance in polycarboxylate water reducing agent's structure, can show and promote dispersion effect, can avoid influencing the mobility of concrete slurry because of the reunion of gel particle, and simultaneously, the terminal benzene ring of side chain and naphthalene ring help improving the stability of side chain, lead to dispersion effect to descend once more because of the curling or winding etc. of side chain at the concrete in-process of stewing after avoiding initial dispersion, can play effectual slump loss retaining effect.
(3) The side chain of the polycarboxylate water reducer introduces an N-phenyl-alpha-naphthylamine structure similar to the anti-aging agent A, so that the anti-aging performance of concrete is improved, the service life of the concrete is prolonged, and the anti-aging agent structure is bonded and connected to the side chain of the polycarboxylate water reducer.
Detailed Description
The present application will now be described in further detail with reference to examples.
Preparing a polycarboxylic acid water reducing agent used in the polycarboxylic acid high-performance water reducing agent:
s1: under the protection of nitrogen, 3- [4- (naphthalene-1-amino) phenyl ] methyl propionate and 15-hexadecenol are put into an ester exchange kettle according to the molar ratio of 1:1.1 for ester exchange reaction, 20ppm of tetrabutyl titanate is added as a catalyst, the temperature is raised to 145 ℃, and the reaction is stirred until the amount of collected methanol reaches 80% of a theoretical calculated value, so that the anti-aging monomer is obtained.
S2: adding 9kg of prenyl alcohol polyoxyethylene ether TPEG-2400 and 9kg of water into a reaction kettle, heating to 55 ℃, adding 0.3kg of acrylic monomer, 1.8kg of anti-aging monomer, 0.12kg of chain transfer agent and 0.18kg of initiator into the reaction kettle under stirring, reacting for 1.5h, naturally cooling reactants, and adding a sodium hydroxide solution to adjust the pH value to 6.5.
Polycarboxylic acid high-performance water reducing agent (the total amount of each component in the polycarboxylic acid high-performance water reducing agent of each example and comparative example is 100 kg):
example 1
8kg of polycarboxylic acid water reducing agent, 3kg of retarder (2 kg of glycerol and 1kg of sodium tripolyphosphate), 0.01kg of thixotropic agent (0.01 kg of fumed silica), 0.05kg of foam stabilizer (0.02 kg of xanthan gum and 0.03kg of polyvinyl alcohol), 0.01kg of air entraining agent (0.01 kg of triterpenoid saponin) and the balance of water.
Example 2
15kg of polycarboxylic acid water reducing agent, 0.5kg of retarder (0.3 kg of sodium tripolyphosphate and 0.2kg of sodium citrate), 0.1kg of thixotropic agent (0.05 kg of magnesium aluminum silicate and 0.05kg of bentonite), 0.01kg of foam stabilizer (0.01 kg of polyacrylamide), 0.05kg of air entraining agent (0.02 kg of sodium dodecyl benzene sulfonate and 0.03kg of sodium dodecyl sulfate) and the balance of water.
Example 3
11kg of polycarboxylic acid water reducing agent, 1.5kg of retarder (0.5 kg of glycerol and 1kg of sodium tripolyphosphate), 0.05kg of thixotropic agent (0.02 kg of magnesium aluminum silicate and 0.03kg of fumed silica), 0.03kg of foam stabilizer (0.01 kg of polyvinyl alcohol and 0.02kg of polyacrylamide), 0.03kg of air entraining agent (0.01 kg of triterpenoid saponin and 0.02kg of sodium dodecyl benzene sulfonate) and the balance of water.
Comparative example 1 is substantially the same as example 3 except that the polycarboxylic acid water reducing agent used in comparative example 1 is prepared by the method comprising: adding 10.8kg of prenyl alcohol polyoxyethylene ether TPEG-2400 and 9kg of water into a reaction kettle, heating to 55 ℃, adding 0.3kg of acrylic monomer, 0.12kg of chain transfer agent and 0.18kg of initiator into the reaction kettle under stirring, reacting for 1.5h, naturally cooling reactants, and adding a sodium hydroxide solution to adjust the pH value to 6.5.
Comparative example 2 is substantially the same as example 3 except that the polycarboxylic acid water reducing agent used in comparative example 2 is prepared by: adding 9kg of prenyl alcohol polyoxyethylene ether TPEG-2400 and 9kg of water into a reaction kettle, heating to 55 ℃, adding 0.3kg of acrylic monomer, 1.8kg of 15-hexadecenol, 0.12kg of chain transfer agent and 0.18kg of initiator into the reaction kettle while stirring, reacting for 1.5h, naturally cooling reactants, and adding a sodium hydroxide solution to adjust the pH value to 6.5.
Comparative example 3 is substantially the same as comparative example 1 except that the amount of the polycarboxylic acid water reducing agent used in comparative example 3 was 10kg, and 1kg of the antioxidant A was additionally added. That is, the formulation of comparative example 3 was: 10kg of polycarboxylic acid water reducing agent (prepared in comparative example 1), 1.5kg of retarder (0.5 kg of glycerol and 1kg of sodium tripolyphosphate), 0.05kg of thixotropic agent (0.02 kg of magnesium aluminum silicate and 0.03kg of fumed silica), 0.03kg of foam stabilizer (0.01 kg of polyvinyl alcohol and 0.02kg of polyacrylamide), 0.03kg of air entraining agent (0.01 kg of triterpenoid saponin and 0.02kg of sodium dodecyl benzene sulfonate), anti-aging agent A1kg and the balance of water.
Comparative example 4 is substantially the same as comparative example 2 except that the amount of the polycarboxylic acid water reducing agent used in comparative example 4 was 10kg, and 1kg of the antioxidant A was additionally added. That is, the formulation of comparative example 4 was: 10kg of polycarboxylic acid water reducing agent (prepared in comparative example 2), 1.5kg of retarder (0.5 kg of glycerol and 1kg of sodium tripolyphosphate), 0.05kg of thixotropic agent (0.02 kg of magnesium aluminum silicate and 0.03kg of fumed silica), 0.03kg of foam stabilizer (0.01 kg of polyvinyl alcohol and 0.02kg of polyacrylamide), 0.03kg of air entraining agent (0.01 kg of triterpenoid saponin and 0.02kg of sodium dodecyl benzene sulfonate), anti-aging agent A1kg and the balance of water.
The polycarboxylic acid high-performance water reducing agent prepared in the example 1, the example 2, the example 3, the comparative example 1, the comparative example 2, the comparative example 3 and the comparative example 4 is applied to concrete, the concrete is self-made concrete, and the concrete formula is as follows: 500kg of cement, 630kg of sand, 1100kg of broken stone, 180kg of water and 10kg of polycarboxylic acid high-performance water reducing agent.
The concrete prepared by using the polycarboxylic acid high-performance water reducing agent prepared in the examples 1 to 3 and the comparative examples 1 to 4 was subjected to performance test, and the test results are shown in table 1.
TABLE 1
In Table 1, the aging method in the compressive strength loss after aging is to perform an aging test on the concrete with age of 28d in a thermal aging box under the aging conditions of 80 ℃ and 720 h.
From table 1, it can be seen that the concrete slump loss of the polycarboxylic acid high-performance water reducing agent prepared in examples 1 to 3 of the present application is 0 in 1h, the concrete slump loss of the polycarboxylic acid high-performance water reducing agent in example 1 in 3h is changed from 195mm to 190mm, the loss is small, and the concrete slump loss of the polycarboxylic acid high-performance water reducing agent in examples 2 to 3 in 3h is 0, which indicates that the polycarboxylic acid high-performance water reducing agent prepared in the present application can obtain a good slump loss prevention effect. The concrete adopting the polycarboxylic acid high-performance water reducing agent prepared in the examples 1 to 3 has the compressive strength of 57.8 to 58.7MPa after 7d, the compressive strength of 28d of 65.6 to 66.9MPa and higher strength, and the compressive strength loss of the concrete (aged 28d) after 720h of heat aging is only 4.8 to 6.2 percent, which shows that the anti-aging effect is better.
As can be seen from comparative examples 1 and 2, when the anti-aging monomer is not added in the preparation process of the polycarboxylic acid water reducer used in comparative example 1, the anti-aging monomer is replaced by isoamylol polyoxyethylene ether with equal mass; in comparative example 2, the anti-aging monomer was replaced with 15-hexadecenol; after the polycarboxylic acid high-performance water reducing agent prepared by the two is applied to concrete, slump of the concrete is obviously reduced within 1h and 3h, which indicates that the slump retaining effect of the polycarboxylic acid high-performance water reducing agent prepared in comparative example 1 and comparative example 2 is poor, and probably because the polycarboxylic acid water reducing agent used in comparative example 1 and comparative example 2 does not contain naphthalene rings and benzene rings at the tail ends of side chains, cement particles have a good initial dispersing effect, but long side chains are easy to curl and wind in the concrete standing process along with the lapse of time, so that the cement particles are agglomerated again, the integral fluidity of the concrete is reduced, and the slump loss is caused. But also has certain loss of strength due to the loss of rigid benzene ring and naphthalene ring structures.
It can be seen from comparative examples 3 and 4 that when the antioxidant structures in comparative examples 3 and 4 were added in the form of small molecule antioxidant a, the loss of slump with time was still severe as in comparative examples 1 and 2, but the addition of antioxidant a made the anti-aging effect of the concrete using the polycarboxylic acid high performance water reducing agent of comparative examples 3 and 4 better than that of comparative examples 1 and 2. However, compared with example 3, the aging resistance of example 3 and comparative example 4 is longer than that of example 3 because the structure of the antioxidant is linked to the side chain of the polycarboxylate water reducer and does not migrate or precipitate with time, and the antioxidant A added in comparative example 3 and comparative example 4 is a small molecular substance and migrates or precipitates with time to lose the corresponding aging resistance.
The present embodiment is merely illustrative and not restrictive, and various changes and modifications may be made by persons skilled in the art without departing from the scope of the present invention as defined in the appended claims. The technical scope of the present application is not limited to the contents of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. A polycarboxylic acid high-performance water reducing agent is characterized in that: the paint comprises the following components in percentage by mass:
8 to 15 percent of polycarboxylic acid water reducing agent
0.5 to 3 percent of retarder
0.01 to 0.1 percent of thixotropic agent
Foam stabilizer 0.01-0.05%
0.01 to 0.05 percent of air entraining agent
The balance of water.
2. The polycarboxylic acid high-performance water reducing agent according to claim 1, characterized in that: the structural formula of the polycarboxylate superplasticizer is as follows:
wherein a, b and c are integers from 1 to 30, and n is an integer from 10 to 30.
3. The polycarboxylic acid high-performance water reducing agent according to claim 2, characterized in that: the preparation method of the polycarboxylate superplasticizer comprises the following steps:
s1, carrying out ester exchange reaction on 3- [4- (naphthalene-1-amino) phenyl ] methyl propionate and 15-hexadecenol to obtain an anti-aging monomer;
s2, adding an acrylic monomer, an unsaturated polyether macromonomer and the anti-aging monomer prepared in the step (1) into a polymerization kettle for polymerization reaction to obtain the polycarboxylate superplasticizer.
4. The polycarboxylic acid high-performance water reducing agent according to claim 3, characterized in that: the unsaturated polyether macromonomer is isopentenol polyoxyethylene ether.
5. The polycarboxylic acid high-performance water reducing agent according to claim 3, characterized in that: the specific method of step S1 is as follows: starting nitrogen protection, putting 3- [4- (naphthalene-1-amino) phenyl ] methyl propionate and 15-hexadecenol into an ester exchange kettle according to the molar ratio of 1:1-1.2 for ester exchange reaction, adding a small amount of tetrabutyl titanate catalyst, stirring and reacting at 140 ℃ and 150 ℃ until the amount of collected methanol reaches 80-85% of a theoretical calculated value, and obtaining the anti-aging monomer.
6. The polycarboxylic acid high-performance water reducing agent according to claim 3, characterized in that: the specific method of step S2 is as follows: adding unsaturated polyether macromonomer and water into a reaction kettle, heating to 50-60 ℃, adding acrylic monomer, anti-aging monomer, chain transfer agent and initiator into the reaction kettle under stirring, reacting for 1-2h, naturally cooling the reactant, and adding sodium hydroxide solution to adjust the pH value to 6.0-6.5.
7. The polycarboxylic acid high-performance water reducing agent according to claim 1, characterized in that: the retarder is one or more of polyalcohol and derivatives thereof, inorganic phosphate and hydroxyl carboxylate.
8. The polycarboxylic acid high-performance water reducing agent according to claim 1, characterized in that: the thixotropic agent is one or more of magnesium aluminum silicate, fumed silica and bentonite.
9. The polycarboxylic acid high-performance water reducing agent according to claim 1, characterized in that: the foam stabilizer is one or more of xanthan gum, polyvinyl alcohol and polyacrylamide.
10. The polycarboxylic acid high-performance water reducing agent according to claim 1, characterized in that: the air entraining agent is one or more of triterpenoid saponin, sodium alkyl benzene sulfonate and sodium alkyl sulfonate.
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