CN109133710B - Preparation method of naphthalene water reducer matching glue reducer - Google Patents
Preparation method of naphthalene water reducer matching glue reducer Download PDFInfo
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- CN109133710B CN109133710B CN201811061682.1A CN201811061682A CN109133710B CN 109133710 B CN109133710 B CN 109133710B CN 201811061682 A CN201811061682 A CN 201811061682A CN 109133710 B CN109133710 B CN 109133710B
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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
- 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
- C04B24/2652—Nitrogen containing polymers, e.g. polyacrylamides, polyacrylonitriles
Abstract
The invention provides a preparation method of a naphthalene water reducer matching gel reducer. The naphthalene water reducer matching glue reducer is prepared from the following components in parts by weight: 30-50 parts of polymeric alcohol amine ester compound, 0.01-0.05 part of penetrating agent, 0.08-0.4 part of lubricant, 0.04-0.08 part of emulsifying dispersant, 0.02-0.1 part of sulfate radical precipitator and the balance of water, wherein the total mass is 100 parts; the components are fully stirred in a reaction kettle for 0.5 hour, and the colloid reducer matched with the naphthalene water reducer is obtained. The invention adopts the method of polymerizing the small alcohol amine monomer and the unsaturated acid anhydride to obtain the alcohol amine ester polymer with higher molecular weight to prepare the gel reducing agent, the gel reducing agent has stronger steric hindrance capability and certain slump loss resistance capability, has better matching property with the naphthalene water reducing agent, can obviously improve the workability of concrete, and can ensure that the surface of the solidified concrete is smooth and bright.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to a preparation method of a naphthalene series water reducer matching glue reducer.
Background
The concrete gel reducer is a new generation of concrete admixture, is used together with other admixtures such as a water reducer and the like, can better improve the workability of concrete, and reduces the using amount of cementing materials in the concrete. In practical application, however, the matching property between the common gel reducing agent and other additives, particularly concrete water reducing agents, has limitations, and restricts the large-scale popularization and application of the gel reducing agent. Particularly, the problem of poor matching between the common glue reducing agent and the naphthalene water reducing agent is prominent, and the glue reducing and dispersing effect is difficult to obtain.
The naphthalene water reducer is prepared by condensation reaction of naphthalene sulfonate, formaldehyde and other substances, and cement particles are dispersed mainly through electrostatic repulsion, namely, negative ion sulfonic groups in water reducer molecules are adsorbed on the cement particles with positive charges on the surfaces in the early hydration stage to form an adsorption double electric layer, so that the cement particles are mutually repelled, and the coagulation is prevented. However, the adsorption mode is short-rod adsorption, and the naphthalene water reducer has small molecular weight and weak spatial three-dimensional rejection capability, so that water reducer molecules are easy to separate from the surface of cement particles, and the water reducer molecules adsorbed on the surface of the cement particles are easy to coat along with the hydration reaction, and macroscopically, the concrete loss is large over time.
The common glue reducing agent mainly adopts alcohol amine cation small monomers, disperses a flocculation structure with electronegativity through electrostatic repulsion force, has weaker dispersing capacity, and is difficult to be matched with two substances with small molecular weight when being matched with a naphthalene water reducing agent for use. Aiming at the problem of insufficient dispersing performance of small molecules, the idea of polymerizing alcohol amine can be adopted, so that the cement reducing agent obtains a certain steric hindrance effect, and the capability of dispersing cement particles is greatly enhanced. At the present stage, the research on the preparation of the gel reducing agent by polymerizing the alcohol amine ester compound is not common, but the gel reducing agent has the characteristic of stronger dispersion effect, so that the later development is determined to be more and more emphasized, and the application is more and more extensive.
Patent CN105174774A discloses a concrete gel reducing agent, which comprises the following components in parts by weight: 100 portions of melamine, 400 portions of formaldehyde, 400 portions of water and 80 portions to 100 portions of salicylic acid. The glue reducing agent reduces the cost of concrete and improves the performance of concrete on the premise of keeping the strength unchanged.
Patent CN106116224A discloses a multifunctional concrete synergist, which is specifically prepared from the following raw materials in parts by weight: 26-42 parts of diisopropylethanolamine, 2-8 parts of pentaerythritol, 15-26 parts of sodium lignosulphonate, 8-16 parts of hexadecyl trimethyl ammonium hydroxide, 1-6 parts of xanthan gum, 5-13 parts of alkyl glycoside and 40-80 parts of water. The multifunctional concrete synergist can reduce the cement consumption, enhance the strength of concrete, improve the durability and the thawing resistance of the concrete, and improve the impermeability.
Patent CN105906230A discloses a multifunctional glue reducing agent for high-performance concrete and a preparation method thereof, wherein the multifunctional glue reducing agent consists of modified polyether, mixed alcohol amine, mixed alcohol, unsaturated acid, modified siloxane, an initiator and water. The multifunctional glue reducing agent for high-performance concrete can reduce the using amount of cementing materials used in the concrete, simultaneously can keep the strength grade of the concrete unchanged, and can improve the frost resistance, carbonization resistance and other durability of the concrete.
Different from the patents, the invention introduces polymeric alcohol amine ester into the components of the gel reducing agent, namely a method for polymerizing alcohol amine small monomers into high molecular polymers, so that the components of the gel reducing agent have certain steric hindrance effect, and the dispersion effect of the gel reducing agent on cement particles is obviously improved; the matching performance of the gel reducing agent and the naphthalene water reducing agent is good, the workability of concrete can be improved, and the purpose of reducing the using amount of a cementing material is achieved.
Disclosure of Invention
The invention provides a preparation method of a naphthalene water reducer matching reducer.
The invention aims at improving the dispersing ability of the gel reducing agent, particularly the steric hindrance ability, and polymerizes small-molecule alcohol amine monomers to form alcohol amine ester high-molecular polymers, thereby adding a certain steric hindrance effect to the components of the gel reducing agent and further improving the gel reducing dispersing ability of the gel reducing agent.
The invention adopts a method that alcohol amine small monomers are polymerized under certain process conditions to form alcohol amine ester polymers with higher molecular weight, and in the process of polymerizing cationic compounds, unsaturated anhydride compounds are introduced as important components of the main chain structure of the polymers, and by using the hydrolysis hysteresis of the unsaturated anhydride compounds, the competitive adsorption of the initial glue reducer and the water reducer is avoided as much as possible, and the defect of poor slump retaining capability of the naphthalene water reducer can be made up.
The alcohol amine ester polymer prepared by the invention has stronger steric hindrance capability, and makes up the defect that naphthalene water reducing agent molecules lack steric hindrance effect. In the synthesis process, a small cationic monomer is introduced to improve the adsorption and dispersion capacity of the polymer.
The penetrant is introduced, so that the mixing effect among the components is improved, and the stirring and mixing effect of the gel reducer and each component of concrete, particularly the naphthalene water reducer, can be improved when the gel reducer is used; the introduced lubricant can not only obviously improve the workability of the concrete, but also can enable the surface of the solidified concrete to be smooth and bright; the air entraining agent with low air entraining amount is matched with the defoaming agent for use, so that the generation of large bubbles is reduced, the influence on the strength performance of the concrete is reduced, and no obvious bubbles exist on the surface of the concrete. A sulfate radical precipitator is introduced into the components to inhibit the problem of excessive sulfate radical caused by the use of a naphthalene water reducer; excessive sulfate radicals can cause the generation of pseudo coagulation due to the precipitation of gypsum crystals in the cement slurry, and excessive sulfate radicals can cause the formation of a large amount of ettringite, so that the slurry hardened at the initial stage of cement generates expansion stress and weakens the strength; in addition, the barium salt and the lead salt can react with sulfate radical to form precipitate, which can fill the gap formed in the hydration reaction process and is helpful for strength increase.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a glue reducer for matching a naphthalene water reducer is characterized by comprising the following steps: the naphthalene water reducer matching glue reducer is prepared from the following components in parts by weight:
30-50 parts of polymeric alcohol amine ester compound, 0.01-0.05 part of penetrating agent,
0.08 to 0.4 portion of lubricant, 0.04 to 0.08 portion of emulsifying dispersant,
0.02-0.1 part of sulfate radical precipitator, and 100 parts of water as the balance;
fully stirring the components in a reaction kettle for 0.5 hour to obtain the viscosity reducer for matching the naphthalene water reducer;
wherein: the polymeric alcohol amine ester compound comprises the following components in parts by weight:
50-70 parts of alcohol amine compound, 20-40 parts of unsaturated anhydride,
1 to 6 portions of cation small monomer, 0.1 to 2 portions of catalyst,
1-5 parts of a neutralizing agent, and 100 parts of the total mass;
the preparation method comprises the following steps:
1) 50-70 parts of alcohol amine compound, 20-40 parts of unsaturated anhydride and 1-6 parts of small cationic monomer are put into a reaction kettle and stirred uniformly;
2) controlling the temperature at 30-70 ℃, adding 0.1-2 parts of catalyst, and continuously stirring for 1-4 hours;
3) and after the reaction time is finished, when the temperature is controlled to be 20-30 ℃, adding 1-5 parts of neutralizing agent, and filtering and separating the catalyst carrier to obtain the polymeric alcohol amine ester compound.
The alcohol amine compound is one or more of butyl ethanolamine, methyl diethanolamine, L-phosphatidyl ethanolamine, N- (3-aminopropyl) diethanolamine, N-diisopropyl ethanolamine, dodecyl benzene sulfonic acid triethanolamine, N- (2-amino-4-nitrophenyl) ethanolamine, 1, 2-dilauroyl phosphatidyl ethanolamine, valiolamine, phenylacetic acid ethanolamine, oleic acid monoethanolamine, oleic acid triethanolamine, N-phenyl ethanolamine, hydriodic acid triethanolamine, isoborneol triethanolamine, diacetyl ethanolamine and tert-butyl ethanolamine; preferably, the alcohol amine compound has large molecular weight and certain steric hindrance capability; the preferable mass ratio is 1: 1 of valiolamine and ecamphotelamine.
The unsaturated acid anhydride is one or more of acrylic anhydride, butene anhydride, 2-butene-1-yl succinic anhydride, isobutylene succinic anhydride, angelica anhydride, maleic anhydride, decenyl succinic anhydride, pentadecenyl succinic anhydride, dodecenyl succinic anhydride, (2-methyl-2-propene-1-yl) succinic anhydride, itaconic anhydride and 4-methacryloyloxyethyl trimellitic anhydride; unsaturated anhydride with large molecular weight and certain steric hindrance capability is preferred; the preferable mass ratio is 1: 1 (2-methyl-2-propen-1-yl) succinic anhydride with 4-methacryloyloxyethyl trimellitic anhydride.
The cationic small monomer is one or more of methacryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl dimethyl benzyl ammonium chloride, methacryloxypropyl trimethyl ammonium chloride, methacryloyloxyamido trimethyl silane, 2-acryloyloxyethoxy trimethyl silane, acryloyloxyethyl dimethyl benzyl ammonium chloride, N-hexyl-N-methacryloyloxy-N, N-dimethylamino ammonium bromide, glycidyl trimethyl ammonium chloride, benzyl vinyl trimethyl ammonium chloride, choline chloride, octaalkyltrimethyl ammonium chloride, tetradecyltrimethyl ammonium chloride, decaalkyltrimethyl ammonium chloride, dodecyl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride; the preferable mass ratio is 1: 1 of methacryloyloxyethyl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride.
The catalyst is solid superacid, and is specifically prepared by loading one or two of sulfate and persulfate on one carrier of zirconia, iron oxide or titanium oxide and carrying out high temperature treatment; the sulfate is composed of one or more of sodium sulfate, sodium thiosulfate, sodium bisulfate, copper sulfate, ammonium sulfate, potassium sulfate, magnesium sulfate and zinc sulfate; the preferable mass ratio is 1: 1 sodium sulfate in combination with sodium thiosulfate; the persulfate is composed of one or more of ammonium persulfate, sodium persulfate, potassium monopersulfate and potassium monopersulfate; the preferable mass ratio is 1: 1 potassium monopersulfate and potassium monopersulfate.
The neutralizing agent is one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, sodium methoxide, sodium ethoxide, ethanolamine, diethanolamine, triethanolamine and triisopropanolamine; alkanolamines, preferably cationic monomers; the preferable mass ratio is 1: 1 of triethanolamine and triisopropanolamine.
The penetrant is one or more of sulfated castor oil, sodium alkyl benzene sulfonate, sodium alkyl sulfate, secondary alkyl sodium sulfonate, secondary alkyl sodium sulfate, alkyl naphthalene sodium sulfonate and sodium sulfamate; sodium alkylbenzenesulfonate with good water solubility and benzene ring structure is preferred.
The lubricant is composed of an organic siloxane lubricant and a hydrocarbon lubricant, and specifically is composed of one or more of polydimethylsiloxane, polymethylphenylsiloxane, polydiethylsiloxane, polyethylene wax, oxidized polyethylene wax and chlorinated paraffin; preferably a composite lubricant; the preferable mass ratio is 1: 1 with an oxidized polyethylene wax.
The emulsifying dispersant is one or more of alpha-sodium alkenyl sulfonate, polyvinyl alcohol ether, polyethylene glycol monooleate, stearyl alcohol polyoxyethylene ether, polyoxyethylene lauryl ether, polyoxyethylene sorbitan tristearate, nonylphenol polyoxyethylene ether and castor oil polyoxyethylene ether; the alpha-alkenyl sodium sulfonate with better matching property with the naphthalene water reducing agent is preferred.
The sulfate precipitator is one or more of barium nitrate, barium chloride, barium hydroxide, barium acetate, barium sulfide, barium thiocyanate trihydrate, barium iodide, barium acetate, barium butyrate, barium propionate, lead chloride, lead nitrate, lead oxalate, lead formate, lead acetate, lead bromate and lead hypoacetate; preferably, organic and inorganic barium salts are compounded for use; the preferable mass ratio is 3: 1 of barium nitrate and lead acetate.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts the method that the small alcohol amine monomer and the unsaturated acid anhydride are polymerized to obtain the alcohol amine ester polymer with higher molecular weight to prepare the glue reducing agent component, and the structure of the alcohol amine ester polymer has better designability and stronger steric hindrance capability; the selected unsaturated anhydride compound is used as an important component of a polymer main chain structure, and the delayed hydrolysis of the unsaturated anhydride compound is utilized to avoid competitive adsorption of the initial glue reducer and the water reducer as much as possible, so that the unsaturated anhydride compound has certain slump retaining capacity and better matching property with a naphthalene water reducer; introducing a cationic small monomer to enhance the dispersion effect of polymeric alcohol amine ester macromolecules on the negative charge cement aggregate;
2. the penetrant is introduced, so that the mixing effect among the components is improved, and the stirring and mixing effect of the gel reducer and each component of concrete, particularly the naphthalene water reducer, can be improved when the gel reducer is used;
3. the introduced lubricant can not only obviously improve the workability of concrete, but also can make the surface of the solidified concrete smooth and bright;
4. the emulsifying dispersant and the defoaming agent are matched for use, so that the compactness of concrete is enhanced, the strength of the concrete is improved, and the apparent appearance of the concrete is ensured to have no obvious bubbles;
5. according to the invention, the sulfate radical precipitator is introduced into the components, so that the condition that the excessive sulfate radicals can cause pseudo coagulation in the cement slurry due to precipitation of gypsum crystals is inhibited, and the problem that the excessive sulfate radicals can cause a large amount of ettringite to form expansion stress to weaken the strength is reduced; in addition, the precipitate formed by the action of the precipitating agent and the sulfate radical can fill the gap formed in the hydration reaction process and is helpful for strength increase.
Detailed Description
The technical solution of the present invention is further clearly and completely described below with reference to the following examples.
Example 1 (the amounts of the components are in parts by weight)
1. Preparation of polymeric alcohol amine ester compound: the preparation method comprises the following steps:
1) and mixing the components in a mass ratio of 1: 50 parts of a composition of valiolamine and ecamsulolamine of 1, 40 parts of acrylic anhydride and 5 parts of methacryloyloxyethyl dimethylbenzyl ammonium chloride are put into a reaction kettle and stirred uniformly;
2) controlling the temperature at 60 ℃, and adding iron oxide for solidification according to the mass ratio of 1: 1.8 parts of baking material of the composition of sodium sulfate and sodium thiosulfate, and continuously stirring for 3.5 hours;
3) and after the reaction time is over, when the temperature is controlled to be 20 ℃, adding 3.2 parts of diethanol amine, and filtering and separating the catalyst carrier to obtain the polymeric alcohol amine ester compound.
2. Preparing the gel reducing agent: the gel reducing agent is prepared from the following components in parts by weight: 30 parts of polymeric alcohol amine ester compound, 0.05 part of sodium alkyl benzene sulfonate, and the mass ratio of 1: 0.4 part of polymethylphenylsiloxane and oxidized polyethylene wax composition of 1, 0.08 part of alpha-sodium alkenyl sulfonate, 0.1 part of barium nitrate and the balance of water, wherein the total mass is 100 parts. The components are fully stirred in a reaction kettle for 0.5 hour, and the colloid reducer matched with the naphthalene water reducer is obtained.
Example 2 (the amounts of the components are in parts by weight)
1. Preparation of polymeric alcohol amine ester compound: the preparation method comprises the following steps:
1) 57 parts of methyldiethanolamine in a mass ratio of 1: 30 parts of a composition of (2-methyl-2-propylene-1-yl) succinic anhydride and 4-methacryloyloxyethyl trimellitic anhydride of 1 and 6 parts of acryloyloxyethyl dimethyl benzyl ammonium chloride are put into a reaction kettle and stirred uniformly;
2) controlling the temperature at 70 ℃, adding 2 parts of titanium oxide solidified potassium sulfate baking material, and continuously stirring for 4 hours;
3) and after the reaction time is finished, controlling the temperature to be 25 ℃, adding 5 parts of potassium carbonate, and filtering and separating the catalyst carrier to obtain the polymeric alcohol amine ester compound.
2. Preparing the gel reducing agent: the gel reducing agent is prepared from the following components in parts by weight: 35 parts of polymeric alcohol amine ester compound, 0.04 part of sulfated castor oil, 0.35 part of polydimethylsiloxane, 0.07 part of aromatic alcohol polyvinyl ether, and the mass ratio of (3): 1, 0.09 part of the composition of barium nitrate and lead acetate, and the balance of water, wherein the total mass is 100 parts. The components are fully stirred in a reaction kettle for 0.5 hour, and the colloid reducer matched with the naphthalene water reducer is obtained.
Example 3 (amounts of the ingredients are in parts by weight)
1. Preparation of polymeric alcohol amine ester compound: the preparation method comprises the following steps:
1) 60 parts of L-phosphatidylethanolamine, 32.5 parts of 2-butene-1-yl succinic anhydride and a mass ratio of 1: 3 parts of the composition of the methacryloyloxyethyl trimethyl ammonium chloride and the octadecyl trimethyl ammonium chloride of the 1 is put into a reaction kettle and stirred uniformly;
2) controlling the temperature at 55 ℃, adding 1.5 parts of baked zirconium oxide cured sodium hydrogen persulfate, and continuing stirring for 3.5 hours;
3) and after the reaction time is over, when the temperature is controlled to be 27 ℃, adding 3 parts of sodium hydroxide, and filtering and separating the catalyst carrier to obtain the polymeric alcohol amine ester compound.
2. Preparing the gel reducing agent: the gel reducing agent is prepared from the following components in parts by weight: 40 parts of polymeric alcohol amine ester compound, 0.03 part of sodium alkyl sulfate, 0.3 part of polydiethyl siloxane, 0.06 part of stearyl alcohol polyoxyethylene ether, 0.08 part of barium chloride and the balance of water, wherein the total mass is 100 parts. The components are fully stirred in a reaction kettle for 0.5 hour, and the colloid reducer matched with the naphthalene water reducer is obtained.
Example 4 (amounts of the ingredients are in parts by weight)
1. Preparation of polymeric alcohol amine ester compound: the preparation method comprises the following steps:
1) adding 69 parts of N, N-diisopropylethanolamine, 20 parts of angelica anhydride and 5.5 parts of N-hexyl-N-methacryloyloxy-N, N-dimethylamino ammonium bromide into a reaction kettle, and uniformly stirring;
2) controlling the temperature at 45 ℃, adding 1.6 parts of titanium oxide solidified sodium sulfate baking material, and continuing stirring for 2 hours;
3) and after the reaction time is finished, when the temperature is controlled to be 28 ℃, adding 3.9 parts of ethanolamine, and filtering and separating the catalyst carrier to obtain the polymeric alcohol amine ester compound.
2. Preparing the gel reducing agent: the gel reducing agent is prepared from the following components in parts by weight: 45 parts of polymeric alcohol amine ester compound, 0.02 part of sodium secondary alkyl sulfate, 0.25 part of polyethylene wax, 0.06 part of stearyl alcohol polyoxyethylene ether, 0.07 part of lead oxalate and the balance of water, wherein the total mass is 100 parts. The components are fully stirred in a reaction kettle for 0.5 hour, and the colloid reducer matched with the naphthalene water reducer is obtained.
Example 5 (amounts of the ingredients are in parts by weight)
1. Preparation of polymeric alcohol amine ester compound: the preparation method comprises the following steps:
1) 68 parts of phenylacetic acid alcohol amine, 27 parts of decenyl succinic anhydride and 2 parts of benzyl vinyl trimethyl ammonium chloride are put into a reaction kettle and stirred uniformly;
2) controlling the temperature at 40 ℃, adding 0.5 part of zirconia solidified sodium thiosulfate baking material, and continuing stirring for 1.5 hours;
3) and after the reaction time is over, controlling the temperature to be 29 ℃, adding a mixture of the components in a mass ratio of 1: 2.5 parts of the composition of triethanolamine and triisopropanolamine of 1, and filtering and separating the catalyst carrier to obtain the polymeric alcohol amine ester compound.
2. Preparing the gel reducing agent: the gel reducing agent is prepared from the following components in parts by weight: 47 parts of polymeric alcohol amine ester compound, 0.03 part of alkyl sodium naphthalene sulfonate, 0.15 part of chlorinated paraffin, 0.05 part of polyoxyethylene sorbitan tristearate, 0.04 part of lead bromate and the balance of water, wherein the total mass is 100 parts. The components are fully stirred in a reaction kettle for 0.5 hour, and the colloid reducer matched with the naphthalene water reducer is obtained.
Example 6 (amounts of the ingredients are in parts by weight)
1. Preparation of polymeric alcohol amine ester compound: the preparation method comprises the following steps:
1) 70 parts of tert-butyl ethanolamine, 27.9 parts of 4-methacryloyloxyethyl trimellitic anhydride and 1 part of choline chloride are put into a reaction kettle and stirred uniformly;
2) controlling the temperature at 30 ℃, and adding titanium oxide for solidification according to the mass ratio of 1: 1, 0.1 part of baked product of the composition of potassium monopersulfate and potassium monopersulfate, and continuously stirring for 1 hour;
3) and after the reaction time is finished, controlling the temperature to be 30 ℃, adding 1 part of sodium methoxide, and filtering and separating the catalyst carrier to obtain the polymeric alcohol amine ester compound.
2. Preparing the gel reducing agent: the gel reducing agent is prepared from the following components in parts by weight: 50 parts of polymeric alcohol amine ester compound, 0.01 part of sodium sulfamate, and the mass ratio of 1: 0.08 part of a composition of polydimethylsiloxane and polyethylene wax of 1, 0.04 part of castor oil polyoxyethylene ether, 0.02 part of lead formate and the balance of water, wherein the total mass is 100 parts. The components are fully stirred in a reaction kettle for 0.5 hour, and the colloid reducer matched with the naphthalene water reducer is obtained.
Results of example testing
The test takes C30 concrete as an object (Table 1), the cement adopts Huaxing 42.5 ordinary portland cement, the sand is river sand with fineness modulus of 2.4, the pebbles are continuous graded broken stones with the thickness of 5-25mm, and the water reducing agents are 3 different naphthalene water reducing agents which are marked as naphthalene water reducing agent A, naphthalene water reducing agent B and naphthalene water reducing agent C. The concrete glue reducing agents prepared in examples 1 to 6 were applied to concrete, and compared with a blank case without adding or reducing glue agents and different naphthalene water reducing agents. The performance of the concrete mixture is tested according to GB/T50080 Standard test method for the Performance of common concrete mixtures; the concrete strength is tested according to GB/T50081 Standard test method for mechanical Properties of ordinary concrete.
TABLE 1C 30 concrete mixing ratio
| Cement | Fly ash | Sand | Stone | Water (W) | Water reducing agent |
| 300 | 80 | 850 | 1020 | 160 | 7.7 |
The concrete admixture performance test results of the concrete test performed by using the concrete gel reducing agent prepared in examples 1, 3 and 5 are shown in table 2.
TABLE 2 concrete Performance test results
As can be seen from the test results in Table 2, after the gel reducer of the invention is added into concrete, the initial slump/expansion and 1h slump/expansion of the concrete are improved, and the compressive strength of 7d, 8d and 64d are enhanced, and the gel reducer of the invention has better matching performance with naphthalene water reducers and has good adaptability with various different naphthalene water reducers.
The mixing proportion of the concrete is adjusted, the using amount of the cement is reduced, concrete tests are carried out by using the concrete cement reducing agents prepared in the examples 2, 4 and 6, the mixing proportion of the concrete is adjusted and shown in a table 3, and the performance and mechanical property test results of concrete mixtures are shown in a table 4 (the original mixing proportion is adopted in blank examples, and the adjusted mixing proportion is adopted in other examples).
TABLE 3C 30 concrete mix ratio adjustment
| Cement | Fly ash | Sand | Stone | Water (W) | Water reducing agent | Glue reducing agent |
| 300 | 80 | 850 | 1020 | 160 | 8 | 0 |
| 270 | 80 | 860 | 1030 | 157 | 8 | 1.7 |
TABLE 4 results of the adjusted concrete Properties
As can be seen from the experimental data in Table 4, the workability of the concrete added with the concrete reducer of the invention is still better than that of the blank sample using the original mix ratio under the condition of 10% reduction of the cement dosage, and the 28d strength and the 60d strength are enhanced. The matching performance of the glue reducer of the invention and naphthalene water reducers is good, and the glue reducer has good adaptability with various naphthalene water reducers.
In conclusion, the glue reducing agent prepared by naphthalene can obviously improve the workability of concrete mixtures and the compressive strength of concrete; the invention can also reduce 10% of the cement consumption under the condition of ensuring the concrete strength, greatly reduce the production cost, realize the full utilization of raw materials and bring great economic benefits to the society; the glue reducer of the invention has good matching performance with polycarboxylic acid water reducing agents, and has good adaptability with various polycarboxylic acid water reducing agents.
All of the features disclosed in this specification, or all of the formulations and amounts disclosed, may be combined in any combination, except features and/or formulations, amounts, etc. that are mutually exclusive. Any feature disclosed in this specification (including any accompanying claims and abstract) may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
The above description is only a non-limiting embodiment of the invention, and many embodiments can be derived, and those skilled in the art can make several modifications and improvements without departing from the inventive concept and without making creative efforts, which all belong to the protection scope of the present invention.
Claims (6)
1. A preparation method of a glue reducer for matching a naphthalene water reducer is characterized by comprising the following steps: the naphthalene water reducer matching glue reducer is prepared from the following components in parts by weight:
30-50 parts of polymeric alcohol amine ester compound, 0.01-0.05 part of penetrating agent,
0.08 to 0.4 portion of lubricant, 0.04 to 0.08 portion of emulsifying dispersant,
0.02-0.1 part of sulfate radical precipitator, and 100 parts of water as the balance;
the penetrant is one or more of sulfated castor oil, sodium alkyl benzene sulfonate, sodium alkyl sulfate, secondary alkyl sodium sulfonate, secondary alkyl sodium sulfate, alkyl naphthalene sodium sulfonate and sodium sulfamate;
fully stirring the components in a reaction kettle for 0.5 hour to obtain the viscosity reducer for matching the naphthalene water reducer;
wherein: the polymeric alcohol amine ester compound comprises the following components in parts by weight:
50-70 parts of alcohol amine compound, 20-40 parts of unsaturated anhydride,
1 to 6 portions of cation small monomer, 0.1 to 2 portions of catalyst,
1-5 parts of a neutralizing agent, and 100 parts of the total mass;
the alcohol amine compound is one or more of butyl ethanolamine, methyl diethanolamine, L-phosphatidyl ethanolamine, N- (3-aminopropyl) diethanolamine, N-diisopropyl ethanolamine, dodecyl benzene sulfonic acid triethanolamine, N- (2-amino-4-nitrophenyl) ethanolamine, 1, 2-dilauroyl phosphatidyl ethanolamine, valiolamine, phenylacetic acid ethanolamine, oleic acid monoethanolamine, oleic acid triethanolamine, N-phenyl ethanolamine, hydriodic acid triethanolamine, isoborneol triethanolamine, diacetyl ethanolamine and tert-butyl ethanolamine;
the cationic small monomer is one or more of methacryloyloxyethyl trimethyl ammonium chloride, methacryloyloxyethyl dimethyl benzyl ammonium chloride, methacryloxypropyl trimethyl ammonium chloride, methacryloyloxyamido trimethyl silane, 2-acryloyloxyethoxy trimethyl silane, acryloyloxyethyl dimethyl benzyl ammonium chloride, N-hexyl-N-methacryloyloxy-N, N-dimethylamino ammonium bromide, glycidyl trimethyl ammonium chloride, benzyl vinyl trimethyl ammonium chloride, choline chloride, octaalkyltrimethyl ammonium chloride, tetradecyltrimethyl ammonium chloride, decaalkyltrimethyl ammonium chloride, dodecyl trimethyl ammonium chloride and octadecyl trimethyl ammonium chloride;
the catalyst is prepared by loading one or two of sulfate and persulfate onto one carrier of zirconia, iron oxide or titanium oxide through high temperature; the sulfate is one or more of sodium sulfate, sodium thiosulfate, sodium bisulfate, copper sulfate, ammonium sulfate, potassium sulfate, magnesium sulfate and zinc sulfate; the persulfate is one or more of ammonium persulfate, sodium persulfate, potassium monopersulfate and potassium monopersulfate;
the preparation method comprises the following steps:
1) 50-70 parts of alcohol amine compound, 20-40 parts of unsaturated anhydride and 1-6 parts of small cationic monomer are put into a reaction kettle and stirred uniformly;
2) controlling the temperature at 30-70 ℃, adding 0.1-2 parts of catalyst, and continuously stirring for 1-4 hours;
3) and after the reaction time is finished, when the temperature is controlled to be 20-30 ℃, adding 1-5 parts of neutralizing agent, and filtering and separating the catalyst carrier to obtain the polymeric alcohol amine ester compound.
2. The preparation method of the naphthalene series water reducer matching gel reducer according to claim 1 is characterized in that: the unsaturated acid anhydride is one or more of acrylic anhydride, butene anhydride, 2-butene-1-yl succinic anhydride, isobutylene succinic anhydride, angelica anhydride, maleic anhydride, decenyl succinic anhydride, pentadecenyl succinic anhydride, dodecenyl succinic anhydride, (2-methyl-2-propene-1-yl) succinic anhydride, itaconic anhydride and 4-methacryloyloxyethyl trimellitic anhydride.
3. The preparation method of the naphthalene series water reducer matching gel reducer according to claim 1 is characterized in that: the neutralizing agent is one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, potassium carbonate, sodium methoxide, sodium ethoxide, ethanolamine, diethanolamine, triethanolamine and triisopropanolamine.
4. The preparation method of the naphthalene series water reducer matching gel reducer according to claim 1 is characterized in that: the lubricant is one or more of polydimethylsiloxane, polymethylphenylsiloxane, polydiethylsiloxane, polyethylene wax, oxidized polyethylene wax and chlorinated paraffin.
5. The preparation method of the naphthalene series water reducer matching gel reducer according to claim 1 is characterized in that: the emulsifying dispersant is composed of one or more of alpha-sodium alkenyl sulfonate, polyvinyl alcohol ether, polyethylene glycol monooleate, stearyl alcohol polyoxyethylene ether, polyoxyethylene lauryl ether, polyoxyethylene sorbitan tristearate, nonylphenol polyoxyethylene ether and castor oil polyoxyethylene ether.
6. The preparation method of the naphthalene series water reducer matching gel reducer according to claim 1 is characterized in that: the sulfate precipitator is one or more of barium nitrate, barium chloride, barium hydroxide, barium acetate, barium sulfide, barium thiocyanate trihydrate, barium iodide, barium acetate, barium butyrate, barium propionate, lead chloride, lead nitrate, lead oxalate, lead formate, lead acetate, lead bromate and lead hypoacetate.
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| CN111825368A (en) * | 2019-04-18 | 2020-10-27 | 安徽海盾建材有限公司 | Concrete with good workability and preparation method thereof |
| CN109942219B (en) * | 2019-04-26 | 2021-08-31 | 山西格瑞特建筑科技股份有限公司 | Concrete glue reducing agent with slump retaining effect |
| CN110386773A (en) * | 2019-06-28 | 2019-10-29 | 浙江老虎山建材有限公司 | A kind of concrete subtracts the preparation method of jelly |
| CN110204240B (en) * | 2019-07-16 | 2022-02-11 | 江苏苏博特新材料股份有限公司 | Organic amphoteric high-molecular activity excitant, preparation method thereof and application thereof in high-admixture cement-based material |
| CN113121771B (en) * | 2019-12-30 | 2022-12-02 | 江苏苏博特新材料股份有限公司 | Air-entraining modified naphthalene water reducer and preparation method thereof |
| CN115819005B (en) * | 2022-11-15 | 2024-02-02 | 安徽海螺材料科技股份有限公司 | Modified alcohol amine efficient cement grinding aid and preparation method thereof |
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