CN112194407A - Environment-friendly concrete water reducing agent and preparation method thereof - Google Patents
Environment-friendly concrete water reducing agent and preparation method thereof Download PDFInfo
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- CN112194407A CN112194407A CN202011192401.3A CN202011192401A CN112194407A CN 112194407 A CN112194407 A CN 112194407A CN 202011192401 A CN202011192401 A CN 202011192401A CN 112194407 A CN112194407 A CN 112194407A
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
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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 invention discloses an environment-friendly concrete water reducing agent which comprises the following components in parts by weight: 8-12 parts of 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil, 3-6 parts of sulfonated hyperbranched polyethyleneimine, 1-3 parts of glycerol, 2-4 parts of emulsifier and 30-45 parts of water. The invention also provides a preparation method of the environment-friendly concrete water reducing agent. The environment-friendly concrete water reducing agent provided by the invention has the advantages of obvious water reducing effect, excellent environment-friendly performance, no negative influence on the comprehensive performance of concrete, small mixing amount and good adaptability.
Description
Technical Field
The invention relates to the technical field of building materials, in particular to an environment-friendly concrete water reducing agent and a preparation method thereof.
Background
The concrete material is widely used in building construction, the development and application of the concrete material promote the development of building material technology, a power source is provided for the promotion of the construction pace of modern cities, and the safety and the quality of major building engineering projects are effectively guaranteed. The concrete material becomes the indispensable key material in the present building engineering, and the development thereof can not leave the chemical admixture, and the admixture can improve the quality of the concrete by changing the mixture. Therefore, it is very important to develop an admixture with excellent comprehensive performance and obvious effect of improving the performance of concrete.
The concrete admixture has various varieties and functions, wherein the most important and most common concrete admixture is a water reducing agent, the main component of the water reducing agent is a surfactant, and the water reducing agent is an additional chemical additive which can improve the workability of concrete in mixing, transportation, pouring, tamping and other construction operation performances by improving the properties of a solid-liquid interface and keeping the workability of the concrete admixture when the water consumption of fresh concrete is obviously reduced, so that the workability of the concrete in the concrete can be improved, the strength and durability of the concrete can be improved, the consumption of water and cement can be reduced, and the factors of initial defects of the concrete caused by creep, shrinkage, cement hydration heat and the like can be reduced.
The common concrete water reducing agents at present mainly comprise naphthalene water reducing agents, melamine water reducing agents, sulfamic acid water reducing agents and novel polycarboxylic acid water reducing agents. Although the naphthalene water reducer is low in cost, the naphthalene water reducer is poor in compatibility with cement, large in slump loss and capable of causing certain environmental pollution, and the cost advantage of the naphthalene water reducer is lost along with the increase of the price of industrial naphthalene. The melamine water reducing agent is superior to the naphthalene water reducing agent in various performances, but the poor fluidity and high price limit the application range of the melamine water reducing agent. The sulfamic acid high-efficiency water reducing agent has simple synthesis process and brings superior performance to concrete over the former two, but the use range of the sulfamic acid high-efficiency water reducing agent is limited to be smaller due to the sensitivity to the mixing amount. The polycarboxylic acid water reducing agent has the advantages of low mixing amount, good slump retention, large molecular structure freedom degree, environmental protection and the like, but in the practical concrete engineering use, the polycarboxylic acid water reducing agent on the market generally has the problem of compatibility with cement, the use effect of the polycarboxylic acid water reducing agent is greatly influenced by cement composition components, particularly when the polycarboxylic acid water reducing agent contains clay and other components, the interlayer adsorption effect of the clay seriously influences the water reducing dispersibility of the polycarboxylic acid water reducing agent, so that the working performance of concrete is reduced, and the wide application and development of the polycarboxylic acid water reducing agent are restricted.
The Chinese invention patent with the application number of 201110395862.5 discloses an aliphatic high-efficiency water reducing agent and a preparation method thereof, wherein the preparation method comprises the following steps: formaldehyde and acetone are used as condensation monomers, anhydrous sodium sulfite is used as a sulfonating agent, an intermediate is synthesized in an aqueous solution by a pyrogen-free method, and an air entraining component, a retarding component, a thickening component and a water retention component are further modified to obtain the aliphatic high-efficiency water reducing agent. The aliphatic high-efficiency water reducing agent prepared by the invention has no crystallization in winter, good adaptability to cementing materials, high water reducing rate, no segregation and bleeding of the mixed concrete, low loss, high strength, no need of heating in the production process, energy conservation, environmental protection, no discharge of three wastes, low requirement on reaction equipment and simple operation. However, the environmental protection performance is poor due to the use of formaldehyde in the raw materials for its preparation.
Therefore, the development of the environment-friendly concrete water reducing agent which has obvious water reducing effect and excellent environment-friendly performance and has no negative influence on the comprehensive performance of concrete is very important, and the environment-friendly concrete water reducing agent has very important significance for promoting the development of concrete material technology.
Disclosure of Invention
The invention aims to provide the environment-friendly concrete water reducing agent and the preparation method thereof, the preparation method has simple process, no special equipment, low requirement on preparation conditions, high preparation efficiency and energy conservation and environmental protection in the whole preparation process, and is suitable for industrial production; the environment-friendly concrete water reducer prepared by the preparation method has the advantages of obvious water reducing effect, excellent environment-friendly performance, no negative influence on the comprehensive performance of concrete, small mixing amount and good adaptability.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows: an environment-friendly concrete water reducing agent comprises the following components in parts by weight: 8-12 parts of 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil, 3-6 parts of sulfonated hyperbranched polyethyleneimine, 1-3 parts of glycerol, 2-4 parts of emulsifier and 30-45 parts of water.
Preferably, the emulsifier is one or more of sodium dodecyl benzene sulfonate, polyoxypropylene polyoxyethylene glycerol ether and nonylphenol polyoxyethylene ether.
Preferably, the preparation method of the sulfonated hyperbranched polyethyleneimine comprises the following steps: adding hyperbranched polyethyleneimine and 1, 4-butyl sultone into a high-boiling-point solvent, stirring and reacting for 6-8 hours at 60-80 ℃ in the atmosphere of nitrogen or inert gas, and then removing the solvent and unreacted 1, 4-butyl sultone by rotary evaporation to obtain the sulfonated hyperbranched polyethyleneimine.
Preferably, the mass ratio of the hyperbranched polyethyleneimine to the 1, 4-butanesultone to the high-boiling-point solvent is 1 (0.3-0.5) to (4-8).
Preferably, the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone; the inert gas is any one of helium, neon and argon.
Preferably, the hyperbranched polyethyleneimine has a weight average molecular weight of 1800 and a degree of branching of 0.52, and is custom made by alfa aesar (china) chemical limited.
Preferably, the preparation method of the 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil comprises the following steps: adding the epoxidized illegal cooking oil into an organic solvent, stirring for 15-25 minutes, adding 9H-carbazole-1-yl boric acid and 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid, refluxing and stirring at 70-80 ℃ for reaction for 5-7 hours, and then performing rotary evaporation to remove the solvent to obtain the 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil.
Preferably, the mass ratio of the epoxidized illegal cooking oil to the organic solvent to the 9H-carbazole-1-yl boric acid to the 2- [ [ tris (hydroxymethyl) methyl ] amino ] ethanesulfonic acid is 1 (3-5) to 0.1: 0.3.
Preferably, the organic solvent is any one of chloroform, ethyl acetate and gasoline.
Preferably, the preparation method of the epoxidized illegal cooking oil is the prior art, which is referred to as Chinese patent application No. 201810555964.0, example 1.
The invention also aims to provide a preparation method of the environment-friendly concrete water reducing agent, which is characterized by comprising the following steps: uniformly mixing the components in parts by weight, adding sodium hydroxide, and adjusting the pH value to 6.5-7.5 to obtain the finished product of the environment-friendly concrete water reducer.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
(1) the preparation method of the environment-friendly concrete water reducing agent disclosed by the invention is simple in process, free of special equipment, low in requirement on preparation conditions, high in preparation efficiency, suitable for industrial production, and energy-saving and environment-friendly in the whole preparation process.
(2) The environment-friendly concrete water reducing agent disclosed by the invention overcomes the defects that the traditional concrete water reducing agent is large in mixing amount, the water reducing effect needs to be further improved, the compatibility with cement is poor, the slump loss is large, certain environmental pollution exists, the fluidity is poor, and the working performance of concrete is reduced after the environment-friendly concrete water reducing agent is added, and the environment-friendly concrete water reducing agent prepared by the environment-friendly concrete water reducing agent has the advantages of remarkable water reducing effect, excellent environment-friendly performance, no negative influence on the comprehensive performance of concrete, small mixing amount and good adaptability due to the synergistic effect of the components.
(3) According to the environment-friendly concrete water reducing agent disclosed by the invention, 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil is added, firstly, the substance contains the illegal cooking oil which is a waste, belongs to waste recycling, realizes changing waste into valuable, saves resources and can solve the environmental problem; the drainage oil is used for preparing the water reducing agent for the first time in the prior art, and negative charge groups such as carboxyl and the like contained in the drainage oil can effectively improve the water reducing performance; through co-modification of 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid, boric acid groups and sulfonic acid groups are introduced into a molecular chain, and the negatively charged groups have synergistic effect, so that the water reducing effect can be effectively improved, and particularly, through introducing the carbazole group and having synergistic effect with the carbazole group, the slump retaining capacity of concrete can be effectively improved under multiple effects of a steric hindrance effect, an electronic effect and a conjugation effect, the fluidity of a concrete mixture is increased, and further the comprehensive performance of the concrete is improved; the hydrophilicity of the 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid can be effectively improved and the storage and transportation stability can be improved by modifying the 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid and introducing a hydrophilic structure of the 2- [ [ tri (hydroxymethyl) methyl ] amino ].
(4) The environment-friendly concrete water reducing agent disclosed by the invention is added with a sulfonated hyperbranched polyethyleneimine structure, can be used for synergistic action with 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil, further improving the water reducing rate, and also playing a role in early strength and retardation, thereby effectively improving the comprehensive performance of concrete. Due to the introduction of the hyperbranched molecular structure, the hyperbranched molecular structure can be better contacted with other components of concrete, so that the water reducing effect is better exerted.
(5) The environment-friendly concrete water reducing agent disclosed by the invention is a composition formed by multi-component synergistic effect, and the components are combined for the first time to prepare the concrete water reducing agent, so that a better water reducing effect is obtained on the whole, the negative influence on concrete is avoided, no toxic or harmful substance is used in the whole preparation process of the water reducing agent, and the environment-friendly concrete water reducing agent is safer and more environment-friendly.
Detailed Description
The invention is further described below with reference to examples; the weight average molecular weight of the hyperbranched polyethyleneimine is 1800, the branching degree is 0.52, and the hyperbranched polyethyleneimine is customized to Afahesar (China) chemical company, Inc.; the preparation method of the epoxidized illegal cooking oil is the prior art, and is shown in the Chinese patent application No. 201810555964.0, namely the example 1; other raw materials were all purchased commercially.
Example 1
An environment-friendly concrete water reducing agent comprises the following components in parts by weight: 8 parts of 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil, 3 parts of sulfonated hyperbranched polyethyleneimine, 1 part of glycerol, 2 parts of emulsifier and 30 parts of water; the emulsifier is sodium dodecyl benzene sulfonate.
The preparation method of the sulfonated hyperbranched polyethyleneimine comprises the following steps: adding hyperbranched polyethyleneimine and 1, 4-butyl sultone into a high-boiling-point solvent, stirring and reacting for 6 hours at 60 ℃ in a nitrogen atmosphere, and then removing the solvent and unreacted 1, 4-butyl sultone by rotary evaporation to obtain sulfonated hyperbranched polyethyleneimine; the mass ratio of the hyperbranched polyethyleneimine to the 1, 4-butanesultone to the high-boiling-point solvent is 1:0.3: 4; the high boiling point solvent is dimethyl sulfoxide.
The preparation method of the 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil comprises the following steps: adding the epoxidized illegal cooking oil into an organic solvent, stirring for 15 minutes, adding 9H-carbazole-1-yl boric acid and 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid, refluxing and stirring at 70 ℃ for 5 hours for reaction, and then performing rotary evaporation to remove the solvent to obtain 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil; the weight ratio of the epoxidized illegal cooking oil to the organic solvent to the 9H-carbazole-1-yl boric acid to the 2- [ [ tris (hydroxymethyl) methyl ] amino ] ethanesulfonic acid is 1:3:0.1: 0.3; the organic solvent is chloroform.
The preparation method of the environment-friendly concrete water reducing agent is characterized by comprising the following steps: and uniformly mixing the components in parts by weight, adding sodium hydroxide, and adjusting the pH value to 6.5 to obtain a finished product of the environment-friendly concrete water reducer.
Example 2
An environment-friendly concrete water reducing agent comprises the following components in parts by weight: 9 parts of 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil, 4 parts of sulfonated hyperbranched polyethyleneimine, 1.5 parts of glycerol, 2.5 parts of emulsifier and 35 parts of water; the emulsifier is polyoxypropylene polyoxyethylene glyceryl ether.
The preparation method of the sulfonated hyperbranched polyethyleneimine comprises the following steps: adding hyperbranched polyethyleneimine and 1, 4-butyl sultone into a high-boiling-point solvent, stirring and reacting for 6.5 hours at 65 ℃ in an inert gas atmosphere, and then performing rotary evaporation to remove the solvent and unreacted 1, 4-butyl sultone to obtain sulfonated hyperbranched polyethyleneimine; the mass ratio of the hyperbranched polyethyleneimine to the 1, 4-butanesultone to the high-boiling-point solvent is 1:0.35: 5; the high boiling point solvent is N, N-dimethylformamide; the inert gas is helium.
The preparation method of the 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil comprises the following steps: adding the epoxidized illegal cooking oil into an organic solvent, stirring for 17 minutes, adding 9H-carbazole-1-yl boric acid and 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid, refluxing and stirring at 73 ℃ for reaction for 5.5 hours, and then performing rotary evaporation to remove the solvent to obtain 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil; the weight ratio of the epoxidized illegal cooking oil to the organic solvent to the 9H-carbazole-1-yl boric acid to the 2- [ [ tris (hydroxymethyl) methyl ] amino ] ethanesulfonic acid is 1:3.5:0.1: 0.3; the organic solvent is ethyl acetate.
The preparation method of the environment-friendly concrete water reducing agent is characterized by comprising the following steps: and uniformly mixing the components in parts by weight, adding sodium hydroxide, and adjusting the pH value to 6.8 to obtain a finished product of the environment-friendly concrete water reducer.
Example 3
An environment-friendly concrete water reducing agent comprises the following components in parts by weight: 10 parts of 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil, 4.5 parts of sulfonated hyperbranched polyethyleneimine, 2 parts of glycerol, 3 parts of emulsifier and 36 parts of water; the emulsifier is nonylphenol polyoxyethylene ether.
The preparation method of the sulfonated hyperbranched polyethyleneimine comprises the following steps: adding hyperbranched polyethyleneimine and 1, 4-butyl sultone into a high-boiling-point solvent, stirring and reacting for 7 hours at 70 ℃ in an inert gas atmosphere, and then removing the solvent and unreacted 1, 4-butyl sultone by rotary evaporation to obtain sulfonated hyperbranched polyethyleneimine; the mass ratio of the hyperbranched polyethyleneimine to the 1, 4-butanesultone to the high-boiling-point solvent is 1:0.4: 6; the high boiling point solvent is N, N-dimethylacetamide; the inert gas is neon.
The preparation method of the 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil comprises the following steps: adding the epoxidized illegal cooking oil into an organic solvent, stirring for 20 minutes, adding 9H-carbazole-1-yl boric acid and 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid, refluxing and stirring for reaction for 6 hours at 75 ℃, and then performing rotary evaporation to remove the solvent to obtain 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil; the weight ratio of the epoxidized illegal cooking oil to the organic solvent to the 9H-carbazole-1-yl boric acid to the 2- [ [ tris (hydroxymethyl) methyl ] amino ] ethanesulfonic acid is 1:4:0.1: 0.3; the organic solvent is gasoline.
The preparation method of the environment-friendly concrete water reducing agent is characterized by comprising the following steps: and uniformly mixing the components in parts by weight, adding sodium hydroxide, and adjusting the pH value to 7 to obtain a finished product of the environment-friendly concrete water reducer.
Example 4
An environment-friendly concrete water reducing agent comprises the following components in parts by weight: 11 parts of 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil, 5.5 parts of sulfonated hyperbranched polyethyleneimine, 2.5 parts of glycerol, 3.5 parts of emulsifier and 43 parts of water; the emulsifier is formed by mixing sodium dodecyl benzene sulfonate, polyoxypropylene polyoxyethylene glycerol ether and nonylphenol polyoxyethylene ether according to the mass ratio of 1:3: 2.
The preparation method of the sulfonated hyperbranched polyethyleneimine comprises the following steps: adding hyperbranched polyethyleneimine and 1, 4-butyl sultone into a high-boiling-point solvent, stirring and reacting for 7.5 hours at 78 ℃ in an inert gas atmosphere, and then performing rotary evaporation to remove the solvent and unreacted 1, 4-butyl sultone to obtain sulfonated hyperbranched polyethyleneimine; the mass ratio of the hyperbranched polyethyleneimine to the 1, 4-butanesultone to the high-boiling-point solvent is 1:0.45: 7.5; the high-boiling-point solvent is formed by mixing dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone according to a mass ratio of 1:3:5: 2; the inert gas is argon.
The preparation method of the 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil comprises the following steps: adding the epoxidized illegal cooking oil into an organic solvent, stirring for 23 minutes, adding 9H-carbazole-1-yl boric acid and 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid, refluxing and stirring for reaction for 6.5 hours at 78 ℃, and then performing rotary evaporation to remove the solvent to obtain 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil; the weight ratio of the epoxidized illegal cooking oil to the organic solvent to the 9H-carbazole-1-yl boric acid to the 2- [ [ tris (hydroxymethyl) methyl ] amino ] ethanesulfonic acid is 1:4.6:0.1: 0.3; the organic solvent is ethyl acetate.
The preparation method of the environment-friendly concrete water reducing agent is characterized by comprising the following steps: and uniformly mixing the components in parts by weight, adding sodium hydroxide, and adjusting the pH value to 7.3 to obtain a finished product of the environment-friendly concrete water reducer.
Example 5
An environment-friendly concrete water reducing agent comprises the following components in parts by weight: 12 parts of 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil, 6 parts of sulfonated hyperbranched polyethyleneimine, 3 parts of glycerol, 4 parts of emulsifier and 45 parts of water; the emulsifier is sodium dodecyl benzene sulfonate.
The preparation method of the sulfonated hyperbranched polyethyleneimine comprises the following steps: adding hyperbranched polyethyleneimine and 1, 4-butyl sultone into a high-boiling-point solvent, stirring and reacting for 8 hours at 80 ℃ in a nitrogen atmosphere, and then removing the solvent and unreacted 1, 4-butyl sultone by rotary evaporation to obtain sulfonated hyperbranched polyethyleneimine; the mass ratio of the hyperbranched polyethyleneimine to the 1, 4-butanesultone to the high-boiling-point solvent is 1:0.5: 8; the high boiling point solvent is N-methyl pyrrolidone.
The preparation method of the 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil comprises the following steps: adding the epoxidized illegal cooking oil into an organic solvent, stirring for 25 minutes, adding 9H-carbazole-1-yl boric acid and 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid, refluxing and stirring for reaction for 7 hours at 80 ℃, and then performing rotary evaporation to remove the solvent to obtain 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil; the weight ratio of the epoxidized illegal cooking oil to the organic solvent to the 9H-carbazole-1-yl boric acid to the 2- [ [ tris (hydroxymethyl) methyl ] amino ] ethanesulfonic acid is 1:5:0.1: 0.3; the organic solvent is gasoline.
The preparation method of the environment-friendly concrete water reducing agent is characterized by comprising the following steps: and uniformly mixing the components in parts by weight, adding sodium hydroxide, and adjusting the pH value to 7.5 to obtain a finished product of the environment-friendly concrete water reducer.
Comparative example 1
An environment-friendly concrete water reducer has a formula and a preparation method which are basically the same as those in example 1, except that 2- [ [ tris (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil is not added with the 2- [ [ tris (hydroxymethyl) methyl ] amino ] ethanesulfonic acid in the preparation process.
Comparative example 2
An environment-friendly concrete water reducer has a formula and a preparation method which are basically the same as those of example 1, except that 9H-carbazole-1-yl boric acid is not added in the preparation process of 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil.
Comparative example 3
An environment-friendly concrete water reducing agent has a formula and a preparation method which are basically the same as those of the environment-friendly concrete water reducing agent in example 1, except that sulfonated hyperbranched polyethyleneimine is not added.
The environment-friendly concrete water reducing agents described in examples 1 to 5 and comparative examples 1 to 3 were subjected to performance tests, and the test results are shown in table 1. The performance test method is carried out by referring to JG/T223-2007, and the mixing amount of the water reducing agent is 0.1%.
TABLE 1
As can be seen from Table 1, the environment-friendly concrete water reducing agent disclosed in the embodiment of the invention has better water reducing effect compared with a comparative product, can obviously increase the initial slump of concrete, improve the compressive strength and reduce the bleeding rate and the shrinkage ratio, and is a result of the synergistic effect of all the components.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. An environment-friendly concrete water reducing agent comprises the following components in parts by weight: 8-12 parts of 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil, 3-6 parts of sulfonated hyperbranched polyethyleneimine, 1-3 parts of glycerol, 2-4 parts of emulsifier and 30-45 parts of water.
2. The environment-friendly concrete water reducer according to claim 1, wherein the emulsifier is one or more of sodium dodecyl benzene sulfonate, polyoxypropylene polyoxyethylene glycerol ether and nonylphenol polyoxyethylene ether.
3. The environment-friendly concrete water reducer according to claim 1, characterized in that the preparation method of the sulfonated hyperbranched polyethyleneimine comprises the following steps: adding hyperbranched polyethyleneimine and 1, 4-butyl sultone into a high-boiling-point solvent, stirring and reacting for 6-8 hours at 60-80 ℃ in the atmosphere of nitrogen or inert gas, and then removing the solvent and unreacted 1, 4-butyl sultone by rotary evaporation to obtain the sulfonated hyperbranched polyethyleneimine.
4. The environment-friendly concrete water reducer according to claim 3, wherein the mass ratio of the hyperbranched polyethyleneimine, the 1, 4-butanesultone and the high-boiling-point solvent is 1 (0.3-0.5) to (4-8).
5. The environment-friendly concrete water reducer according to claim 3, wherein the high boiling point solvent is at least one of dimethyl sulfoxide, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
6. The environment-friendly concrete water reducer according to claim 3, wherein the inert gas is any one of helium, neon and argon.
7. The environment-friendly concrete water reducer according to claim 3, wherein the hyperbranched polyethyleneimine has a weight average molecular weight of 1800 and a branching degree of 0.52.
8. The environment-friendly concrete water reducer according to claim 1, characterized in that the preparation method of the 2- [ [ tris (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazol-1-yl boronic acid co-modified epoxidized illegal cooking oil comprises the following steps: adding the epoxidized illegal cooking oil into an organic solvent, stirring for 15-25 minutes, adding 9H-carbazole-1-yl boric acid and 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid, refluxing and stirring at 70-80 ℃ for reaction for 5-7 hours, and then performing rotary evaporation to remove the solvent to obtain the 2- [ [ tri (hydroxymethyl) methyl ] amino ] ethanesulfonic acid/9H-carbazole-1-yl boric acid co-modified epoxidized illegal cooking oil.
9. The environment-friendly concrete water reducer according to claim 8, characterized in that the mass ratio of the epoxidized illegal cooking oil to the organic solvent to the 9H-carbazole-1-yl boric acid to the 2- [ [ tris (hydroxymethyl) methyl ] amino ] ethanesulfonic acid is 1 (3-5) to 0.1: 0.3; the organic solvent is any one of chloroform, ethyl acetate and gasoline.
10. The environment-friendly concrete water reducer according to any one of claims 1 to 9, wherein the preparation method of the environment-friendly concrete water reducer comprises the following steps: uniformly mixing the components in parts by weight, adding sodium hydroxide, and adjusting the pH value to 6.5-7.5 to obtain the finished product of the environment-friendly concrete water reducer.
Priority Applications (1)
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