CN111960714B - High-water-reduction high-slump-retaining water reducer and synthesis method thereof - Google Patents
High-water-reduction high-slump-retaining water reducer and synthesis method thereof Download PDFInfo
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C—CHEMISTRY; METALLURGY
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- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
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Abstract
The invention disclosesA method for synthesizing a high water-reducing high slump-retaining water reducer comprises the following steps: (1) adding water and prenyl polyoxyethylene ether into a reaction kettle, stirring for dissolving, and keeping the temperature to 25-30 ℃; preparing aqueous solution of a reducing agent as solution A, preparing mixed solution of acrylic acid, hydroxyethyl methacrylate, a chain transfer agent, polyethylene glycol diacrylate and water as solution B, preparing extract of oak leaves and dried orange peel as solution C, and preparing SbCl 3 、ZnCl 2 As solution D; (2) adding an oxidant into the reaction kettle, stirring, and then dropwise adding the solution A, the solution B, the solution C and the solution D; keeping the temperature after the dropwise adding is finished; and (3) neutralizing the mixture by using a sodium hydroxide solution after heat preservation is finished until the pH value is 6-7, adding dimethylacetamide, and stirring to obtain the high water-reducing and high slump-retaining water reducing agent. The preparation method is simple in preparation process and convenient to operate, and the water reducer prepared by the method has good water reducing and slump retaining effects, so that the cost is saved, and the market demand is greatly met.
Description
Technical Field
The invention belongs to the technical field of concrete admixtures, and particularly relates to a high water-reducing high slump-retaining water reducing agent and a synthesis method thereof.
Background
The water reducing agent is used as a concrete chemical additive, can effectively improve the fluidity of concrete, improve the workability of the concrete and reduce the consumption of cement. Due to the high design freedom, products with different properties, such as a reduction type water reducing agent, an early strength type water reducing agent, a slump loss resistant type water reducing agent and the like can be prepared by changing the types of synthetic monomers.
The polycarboxylic acid water reducing agent is widely applied to concrete due to the advantages of high water reducing rate, low mixing amount, small concrete shrinkage, environmental protection and the like. However, for the premixed concrete industry, the problem that the normal construction is always troubled by the overlarge concrete slump decrease along with time is that the later slump loss of the concrete is serious after long-time and long-distance transportation, and the requirement of the normal construction cannot be met. In order to control the loss of the concrete slump, methods such as a post-mixing method, a multiple-mixing method, a composite retarder and the like are adopted, wherein the 2 methods of the post-mixing method and the multiple-mixing method have little practicability in actual production construction due to the complexity of operation and the limitation of stirring equipment; the method for compounding the retarder has the problem that the retarder is compatible with cement, and if the compatibility of the retarder and the cement is poor, the phenomena of too fast slump loss and abnormal coagulation can occur.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for synthesizing a high water-reducing and high slump-retaining water reducing agent, which comprises the following steps:
(1) adding water and prenyl polyoxyethylene ether into a reaction kettle, stirring for dissolving, and keeping the temperature to 25-30 ℃; preparing aqueous solution of a reducing agent as solution A, preparing mixed solution of acrylic acid, hydroxyethyl methacrylate, a chain transfer agent, polyethylene glycol diacrylate and water as solution B, preparing oak leaf-dried orange peel extract as solution C, and preparing SbCl 3 、ZnCl 2 As solution D;
(2) adding an oxidant into the reaction kettle at a constant temperature of 25-30 ℃, stirring for 5-10 min, and then dropwise adding the liquid A, the liquid B, the liquid C and the liquid D, wherein the dropwise adding time of the liquid A is 2-2.5 h, the dropwise adding time of the liquid B is 1.5-2 h, the dropwise adding time of the liquid C is 1.5-2 h, and the dropwise adding time of the liquid D is 2-2.5 h; after the dropwise adding is finished, continuously preserving the heat for 2-2.5 h; and (3) neutralizing with a sodium hydroxide solution after heat preservation is finished until the pH value is 6-7, adding dimethylacetamide, and stirring for 10-15 min to obtain the high water-reducing high slump-retaining water reducer.
Further, the reducing agent is vitamin C, and the mass fraction of the reducing agent in the solution A is 2-3%.
Further, the liquid B comprises the following components in parts by weight: 10-15 parts of acrylic acid, 1-2 parts of hydroxyethyl methacrylate, 0.6-1.4 parts of a chain transfer agent, 2-4 parts of polyethylene glycol diacrylate and 20-30 parts of water; the molecular weight of the polyethylene glycol diacrylate is 400-600 daltons.
Further, the chain transfer agent is mercaptopropionic acid.
Further, the preparation method of the solution C comprises the following steps: mixing and chopping fresh oak leaves and dry orange peel, pouring the chopped materials into ethyl acetate to form a mixture, carrying out water bath on the mixture, keeping the temperature to be 50-60 ℃, and carrying out heat preservation for 2-3 hours; and after the heat preservation is finished, air cooling to normal temperature, filtering to remove solid phase, decompressing and concentrating liquid phase to obtain the oak leaf-dried orange peel extracting solution.
Further, the mixing mass ratio of the fresh oak leaves to the dry orange peel is =10: 2-3; the feed liquid mass ratio of the chopped materials to the ethyl acetate is that the chopped materials/ethyl acetate = 1-3: 10; the liquid phase was concentrated under reduced pressure to 1/3 in its unconcentrated volume.
Further, the mass ratio of each component in the solution D is configured to be SbCl 3 ：ZnCl 2 : water = 1-5: 8-13: 100.
Further, in the step (1), the molecular weight of the isoamylene alcohol polyoxyethylene ether is 3000 daltons, and the mass parts of the water, the isoamylene alcohol polyoxyethylene ether and the water are 70-76 parts by mass and 100 parts by mass.
Further, the oxidant is hydrogen peroxide with the mass percent of hydrogen peroxide of 30%, and the mass parts of the oxidant, the solution A, the solution B, the solution C, the solution D and the dimethylacetamide to the prenyl alcohol polyoxyethylene ether are as follows: 100 parts of prenyl polyoxyethylene ether, 0.4-0.8 part of oxidant, 8-10 parts of liquid A, 1.0-1.3 parts of liquid B, 5-9 parts of liquid C, 3-10 parts of liquid D and 1-7 parts of dimethylacetamide; the percentage content of solute in the sodium hydroxide solution is 30%.
The invention also discloses a high water-reducing high slump-retaining water reducing agent prepared by adopting the method.
Therefore, the beneficial effects of the invention are as follows: the preparation method is simple in preparation process and convenient to operate, and the water reducer prepared by the method has good water reducing and slump retaining effects, so that the cost is saved, and the market demand is greatly met.
Detailed Description
The following is a detailed description with reference to examples:
example 1
A synthetic method of a high water-reducing and high slump-retaining water reducing agent comprises the following steps:
(1) adding water and prenyl polyoxyethylene ether into a reaction kettle according to the proportion that the mass portions are 70 parts of water and 100 parts of prenyl polyoxyethylene ether (the relative molecular mass is 3000), stirring and dissolving, and keeping the temperature to 25-30 ℃; preparing aqueous solution of a reducing agent as solution A, preparing mixed solution of acrylic acid, hydroxyethyl methacrylate, mercaptopropionic acid, polyethylene glycol diacrylate and water as solution B, preparing extract of oak leaves and dried orange peel as solution C, and preparing SbCl 3 、ZnCl 2 Water of (2)The solution is used as solution D; wherein the reducing agent is vitamin C, and the mass fraction of the reducing agent in the solution A is 2%; the liquid B comprises the following components in parts by weight: 10 parts of acrylic acid, 1 part of hydroxyethyl methacrylate, 0.6 part of mercaptopropionic acid, 2 parts of polyethylene glycol diacrylate and 20 parts of water, wherein the relative molecular weight of the polyethylene glycol diacrylate is 500 daltons; the preparation method of the solution C comprises the following steps: mixing and chopping fresh oak leaves and dry orange peel according to the mass ratio of the oak leaves to the dry orange peel =10:2, pouring the chopped materials into ethyl acetate to form a mixture, keeping the feed liquid mass ratio of the chopped materials to the ethyl acetate =1:10, keeping the mixture at the constant temperature of 55 +/-5 ℃ in a water bath, and keeping the temperature for 2 hours; after the heat preservation is finished, air cooling to normal temperature, filtering to remove solid phase, decompressing and concentrating liquid phase to 1/3 of the volume before concentration to obtain the oak leaf-dried orange peel extracting solution; the mass ratio of each component in the solution D is SbCl 3 ：ZnCl 2 : water =1:8: 100;
(2) adding hydrogen peroxide with the mass percent of 30% into the reaction kettle at the constant temperature of 25-30 ℃, stirring for 5min, and then dropwise adding the solution A, the solution B, the solution C and the solution D, wherein the dropwise adding time of the solution A is 2h, the dropwise adding time of the solution B is 1.5h, the dropwise adding time of the solution C is 1.5h, and the dropwise adding time of the solution D is 2 h; after the dropwise addition is finished, continuously preserving the heat for 2 hours; and (3) neutralizing the mixture by using a sodium hydroxide aqueous solution with the solute percentage content of 30% until the pH value is 7 after heat preservation is finished, adding dimethylacetamide, stirring for 10min, and adding water to adjust the solid content to 40% to obtain the high water-reducing high slump-retaining water reducer. Wherein the addition amount of the hydrogen peroxide, the solution A, the solution B, the solution C, the solution D and the dimethylacetamide is as follows according to the mass part ratio of the prenyl polyoxyethylene ether in the raw materials: 100 parts of prenyl polyoxyethylene ether, 0.4 part of hydrogen peroxide, 8 parts of liquid A, 1.0 part of liquid B, 5 parts of liquid C, 3 parts of liquid D and 1 part of dimethylacetamide.
Example 2
A synthetic method of a high water-reducing and high slump-retaining water reducing agent comprises the following steps:
(1) adding water and prenyl polyoxyethylene ether into a reaction kettle according to the proportion that the water accounts for 73 parts by mass and the prenyl polyoxyethylene ether accounts for 100 parts by mass (relative molecular mass is 3000), stirring and dissolving, and keeping the temperature to 25-30 ℃; preparing water solution of reducing agentPreparing solution A, preparing mixed solution of acrylic acid, hydroxyethyl methacrylate, mercaptopropionic acid, polyethylene glycol diacrylate and water as solution B, preparing extractive solution of oak leaves and dried orange peel as solution C, and preparing SbCl 3 、ZnCl 2 As solution D; wherein the reducing agent is vitamin C, and the mass fraction of the reducing agent in the solution A is 2%; the liquid B comprises the following components in parts by weight: 12 parts of acrylic acid, 1 part of hydroxyethyl methacrylate, 0.9 part of mercaptopropionic acid, 3 parts of polyethylene glycol diacrylate and 20 parts of water, wherein the relative molecular weight of the polyethylene glycol diacrylate is 500 daltons; the preparation method of the solution C comprises the following steps: mixing and chopping fresh oak leaves and dry orange peels according to the mass ratio of the oak leaves to the dry orange peels =10:2, pouring the chopped materials into ethyl acetate to form a mixture, keeping the mass ratio of the feed liquid in the mixture to the chopped materials to the ethyl acetate =2:10, carrying out water bath on the mixture, keeping the temperature to 55 +/-5 ℃, and keeping the temperature for 2 hours; cooling in air to normal temperature after heat preservation, filtering to remove solid phase, decompressing and concentrating liquid phase to 1/3 of volume before concentration to obtain the oak leaf-dried orange peel extracting solution; the mass ratio of each component in the solution D is SbCl 3 ：ZnCl 2 : water =2:10: 100;
(2) adding hydrogen peroxide with the mass percent of 30% into the reaction kettle at the constant temperature of 25-30 ℃, stirring for 8min, and then dropwise adding the solution A, the solution B, the solution C and the solution D, wherein the dropwise adding time of the solution A is 2h, the dropwise adding time of the solution B is 1.5h, the dropwise adding time of the solution C is 1.5h, and the dropwise adding time of the solution D is 2 h; after the dropwise addition is finished, continuously preserving the heat for 2 hours; and (3) neutralizing the mixture by using a sodium hydroxide aqueous solution with the solute percentage content of 30% until the pH value is 7 after heat preservation is finished, adding dimethylacetamide, stirring for 10min, and adding water to adjust the solid content to 40% to obtain the high water-reducing high slump-retaining water reducer. Wherein the addition amount of the hydrogen peroxide, the solution A, the solution B, the solution C, the solution D and the dimethylacetamide is as follows according to the mass part ratio of the prenyl polyoxyethylene ether in the raw materials: 100 parts of prenyl polyoxyethylene ether, 0.6 part of hydrogen peroxide, 9 parts of liquid A, 1.2 parts of liquid B, 6 parts of liquid C, 5 parts of liquid D and 3 parts of dimethylacetamide.
Example 3
A synthetic method of a high water-reducing and high slump-retaining water reducing agent comprises the following steps:
(1) adding water and prenyl polyoxyethylene ether into a reaction kettle according to the proportion that the water accounts for 73 parts by mass and the prenyl polyoxyethylene ether accounts for 100 parts by mass (relative molecular mass is 3000), stirring and dissolving, and keeping the temperature to 25-30 ℃; preparing aqueous solution of reducing agent as solution A, preparing mixed solution of acrylic acid, hydroxyethyl methacrylate, mercaptopropionic acid, polyethylene glycol diacrylate and water as solution B, preparing extract of oak leaves and dried orange peel as solution C, and preparing SbCl 3 、ZnCl 2 As solution D; wherein the reducing agent is vitamin C, and the mass fraction of the reducing agent in the solution A is 3 percent; the liquid B comprises the following components in parts by weight: 14 parts of acrylic acid, 2 parts of hydroxyethyl methacrylate, 1.2 parts of mercaptopropionic acid, 3 parts of polyethylene glycol diacrylate and 30 parts of water, wherein the relative molecular weight of the polyethylene glycol diacrylate is 500 daltons; the preparation method of the solution C comprises the following steps: mixing and chopping fresh oak leaves and dry orange peels according to the mass ratio of the oak leaves to the dry orange peels =10:3, pouring the chopped materials into ethyl acetate to form a mixture, keeping the mass ratio of the materials in the mixture to the ethyl acetate =2:10, carrying out water bath on the mixture at constant temperature of 55 +/-5 ℃, and keeping the temperature for 3 hours; after the heat preservation is finished, air cooling to normal temperature, filtering to remove solid phase, decompressing and concentrating liquid phase to 1/3 of the volume before concentration to obtain the oak leaf-dried orange peel extracting solution; the mass ratio of each component in the solution D is SbCl 3 ：ZnCl 2 : water =4:11: 100;
(2) adding hydrogen peroxide with the mass percent of 30% into the reaction kettle at the constant temperature of 25-30 ℃, stirring for 10min, and then dropwise adding the solution A, the solution B, the solution C and the solution D, wherein the dropwise adding time of the solution A is 2h, the dropwise adding time of the solution B is 1.5h, the dropwise adding time of the solution C is 1.5h, and the dropwise adding time of the solution D is 2 h; after the dropwise addition is finished, continuously preserving the heat for 2 hours; and (3) neutralizing the mixture by using a sodium hydroxide aqueous solution with the solute percentage content of 30% until the pH value is 7 after heat preservation is finished, adding dimethylacetamide, stirring for 15min, and adding water to adjust the solid content to 40% to obtain the high water-reducing high slump-retaining water reducer. Wherein the addition amount of the hydrogen peroxide, the solution A, the solution B, the solution C, the solution D and the dimethylacetamide is as follows according to the mass part ratio of the prenyl polyoxyethylene ether in the raw materials: 100 parts of prenyl alcohol polyoxyethylene ether, 0.6 part of hydrogen peroxide, 9 parts of solution A, 1.1 parts of solution B, 8 parts of solution C, 8 parts of solution D and 5 parts of dimethylacetamide.
Example 4
A synthetic method of a high water-reducing and high slump-retaining water reducing agent comprises the following steps:
(1) adding water and isoamylene alcohol polyoxyethylene ether into a reaction kettle according to the proportion of 76 parts of water and 100 parts of isoamylene alcohol polyoxyethylene ether (relative molecular weight is 3000), stirring for dissolving, and keeping the temperature to be 25-30 ℃; preparing aqueous solution of reducing agent as solution A, preparing mixed solution of acrylic acid, hydroxyethyl methacrylate, mercaptopropionic acid, polyethylene glycol diacrylate and water as solution B, preparing extract of oak leaves and dried orange peel as solution C, and preparing SbCl 3 、ZnCl 2 As solution D; wherein the reducing agent is vitamin C, and the mass fraction of the reducing agent in the solution A is 3%; the liquid B comprises the following components in parts by weight: 15 parts of acrylic acid, 2 parts of hydroxyethyl methacrylate, 1.4 parts of mercaptopropionic acid, 4 parts of polyethylene glycol diacrylate and 30 parts of water, wherein the relative molecular weight of the polyethylene glycol diacrylate is 500 daltons; the preparation method of the solution C comprises the following steps: mixing and chopping fresh oak leaves and dry orange peels according to the mass ratio of the oak leaves to the dry orange peels =10:3, pouring the chopped materials into ethyl acetate to form a mixture, keeping the mass ratio of the feed liquid in the mixture to the chopped materials to the ethyl acetate =3:10, carrying out water bath on the mixture, keeping the temperature to 55 +/-5 ℃, and keeping the temperature for 3 hours; after the heat preservation is finished, air cooling to normal temperature, filtering to remove solid phase, decompressing and concentrating liquid phase to 1/3 of the volume before concentration to obtain the oak leaf-dried orange peel extracting solution; the mass ratio of each component in the solution D is SbCl 3 ：ZnCl 2 : water =5:13: 100;
(2) adding hydrogen peroxide with the mass percent of 30% into the reaction kettle at the constant temperature of 25-30 ℃, stirring for 10min, and then dropwise adding the solution A, the solution B, the solution C and the solution D, wherein the dropwise adding time of the solution A is 2h, the dropwise adding time of the solution B is 1.5h, the dropwise adding time of the solution C is 1.5h, and the dropwise adding time of the solution D is 2 h; after the dropwise addition is finished, continuously preserving the heat for 2 hours; and (3) neutralizing the mixture by using a sodium hydroxide aqueous solution with the solute percentage content of 30% until the pH value is 7 after heat preservation is finished, adding dimethylacetamide, stirring for 15min, and adding water to adjust the solid content to 40% to obtain the high water-reducing high slump-retaining water reducer. Wherein the addition amount of the hydrogen peroxide, the solution A, the solution B, the solution C, the solution D and the dimethylacetamide is as follows according to the mass part ratio of the prenyl polyoxyethylene ether in the raw materials: 100 parts of prenyl alcohol polyoxyethylene ether, 0.8 part of hydrogen peroxide, 10 parts of solution A, 1.3 parts of solution B, 9 parts of solution C, 10 parts of solution D and 7 parts of dimethylacetamide.
Comparative example 1
A synthetic method of a water reducing agent comprises the following steps:
(1) adding water and prenyl polyoxyethylene ether into a reaction kettle according to the proportion that the water accounts for 73 parts by mass and the prenyl polyoxyethylene ether accounts for 100 parts by mass (relative molecular mass is 3000), stirring and dissolving, and keeping the temperature to 25-30 ℃; preparing a reducing agent aqueous solution as a solution A, preparing a mixed solution of acrylic acid, hydroxyethyl methacrylate, mercaptopropionic acid, polyethylene glycol diacrylate and water as a solution B, and preparing an oak leaf-dried orange peel extracting solution as a solution C; wherein the reducing agent is vitamin C, and the mass fraction of the reducing agent in the solution A is 3 percent; the liquid B comprises the following components in parts by weight: 14 parts of acrylic acid, 2 parts of hydroxyethyl methacrylate, 1.2 parts of mercaptopropionic acid, 3 parts of polyethylene glycol diacrylate and 30 parts of water, wherein the relative molecular weight of the polyethylene glycol diacrylate is 500 daltons; the preparation method of the solution C comprises the following steps: mixing and chopping fresh oak leaves and dry orange peel according to the mass ratio of the oak leaves to the dry orange peel =10:3, pouring the chopped materials into ethyl acetate to form a mixture, keeping the feed liquid mass ratio of the chopped materials to the ethyl acetate =2:10, keeping the mixture at the constant temperature of 55 +/-5 ℃ in a water bath, and keeping the temperature for 3 hours; cooling in air to normal temperature after heat preservation, filtering to remove solid phase, decompressing and concentrating liquid phase to 1/3 of volume before concentration to obtain the oak leaf-dried orange peel extracting solution;
(2) adding hydrogen peroxide with the mass percent of 30% into the reaction kettle at the constant temperature of 25-30 ℃, stirring for 10min, and then dropwise adding the liquid A, the liquid B and the liquid C, wherein the dropwise adding time of the liquid A is 2h, the dropwise adding time of the liquid B is 1.5h, and the dropwise adding time of the liquid C is 1.5 h; after the dropwise addition is finished, continuously preserving the heat for 2 hours; and (3) after the heat preservation is finished, neutralizing the mixture by using a sodium hydroxide aqueous solution with the solute percentage content of 30% until the pH value is 7, adding dimethylacetamide, stirring for 15min, and adding water to adjust the solid content to 40% to obtain the water reducer of the comparative example. Wherein the addition amount of the hydrogen peroxide, the solution A, the solution B, the solution C and the dimethylacetamide is as follows according to the mass part ratio of the prenyl alcohol polyoxyethylene ether in the raw materials: 100 parts of prenyl polyoxyethylene ether, 0.6 part of hydrogen peroxide, 9 parts of liquid A, 1.1 parts of liquid B, 8 parts of liquid C and 5 parts of dimethylacetamide.
Comparative example 2
A synthetic method of a water reducing agent comprises the following steps:
(1) adding water and isoamylene alcohol polyoxyethylene ether into a reaction kettle according to the proportion of 73 parts of water and 100 parts of isoamylene alcohol polyoxyethylene ether (relative molecular weight is 3000), stirring for dissolving, and keeping the temperature to be 25-30 ℃; preparing aqueous solution of a reducing agent as solution A, preparing mixed solution of acrylic acid, hydroxyethyl methacrylate, mercaptopropionic acid, polyethylene glycol diacrylate and water as solution B, preparing extract of oak leaves and dried orange peel as solution C, and preparing ZnCl 2 As solution D; wherein the reducing agent is vitamin C, and the mass fraction of the reducing agent in the solution A is 3 percent; the liquid B comprises the following components in parts by weight: 14 parts of acrylic acid, 2 parts of hydroxyethyl methacrylate, 1.2 parts of mercaptopropionic acid, 3 parts of polyethylene glycol diacrylate and 30 parts of water, wherein the relative molecular weight of the polyethylene glycol diacrylate is 500 daltons; the preparation method of the solution C comprises the following steps: mixing and chopping fresh oak leaves and dry orange peel according to the mass ratio of the oak leaves to the dry orange peel =10:3, pouring the chopped materials into ethyl acetate to form a mixture, keeping the feed liquid mass ratio of the chopped materials to the ethyl acetate =2:10, keeping the mixture at the constant temperature of 55 +/-5 ℃ in a water bath, and keeping the temperature for 3 hours; after the heat preservation is finished, air cooling to normal temperature, filtering to remove solid phase, decompressing and concentrating liquid phase to 1/3 of the volume before concentration to obtain the oak leaf-dried orange peel extracting solution; the mass ratio of each component in the solution D is ZnCl 2 : water =11: 100;
(2) adding hydrogen peroxide with the mass percent of 30% into the reaction kettle at the constant temperature of 25-30 ℃, stirring for 10min, and then dropwise adding the solution A, the solution B, the solution C and the solution D, wherein the dropwise adding time of the solution A is 2h, the dropwise adding time of the solution B is 1.5h, the dropwise adding time of the solution C is 1.5h, and the dropwise adding time of the solution D is 2 h; after the dropwise addition is finished, continuously preserving the heat for 2 hours; and after the heat preservation is finished, neutralizing the mixture by using a sodium hydroxide aqueous solution with the solute percentage content of 30% until the pH value is 7, adding dimethylacetamide, stirring for 15min, and adding water to adjust the solid content to 40% to obtain the water reducing agent of the comparative example. Wherein the addition amount of the hydrogen peroxide, the solution A, the solution B, the solution C, the solution D and the dimethylacetamide is as follows according to the mass part ratio of the prenyl polyoxyethylene ether in the raw materials: 100 parts of prenyl alcohol polyoxyethylene ether, 0.6 part of hydrogen peroxide, 9 parts of solution A, 1.1 parts of solution B, 8 parts of solution C, 8 parts of solution D and 5 parts of dimethylacetamide.
Comparative example 3
A synthetic method of a high water-reducing and high slump-retaining water reducing agent comprises the following steps:
(1) adding water and prenyl polyoxyethylene ether into a reaction kettle according to the proportion that the water accounts for 73 parts by mass and the prenyl polyoxyethylene ether accounts for 100 parts by mass (relative molecular mass is 3000), stirring and dissolving, and keeping the temperature to 25-30 ℃; preparing aqueous solution of a reducing agent as solution A, preparing mixed solution of acrylic acid, hydroxyethyl methacrylate, mercaptopropionic acid, polyethylene glycol diacrylate and water as solution B, and preparing SbCl 3 、ZnCl 2 As solution D; wherein the reducing agent is vitamin C, and the mass fraction of the reducing agent in the solution A is 3 percent; the liquid B comprises the following components in parts by weight: 14 parts of acrylic acid, 2 parts of hydroxyethyl methacrylate, 1.2 parts of mercaptopropionic acid, 3 parts of polyethylene glycol diacrylate and 30 parts of water, wherein the relative molecular weight of the polyethylene glycol diacrylate is 500 daltons; the mass ratio of each component in the solution D is SbCl 3 ：ZnCl 2 : water =4:11: 100;
(2) adding hydrogen peroxide with the mass percent of 30% into the reaction kettle at the constant temperature of 25-30 ℃, stirring for 10min, and then dropwise adding the liquid A, the liquid B and the liquid D, wherein the dropwise adding time of the liquid A is 2h, the dropwise adding time of the liquid B is 1.5h, and the dropwise adding time of the liquid D is 2 h; after the dropwise addition is finished, continuously preserving the heat for 2 hours; and (3) after the heat preservation is finished, neutralizing the mixture by using a sodium hydroxide aqueous solution with the solute percentage content of 30% until the pH value is 7, adding dimethylacetamide, stirring for 15min, and adding water to adjust the solid content to 40% to obtain the water reducer of the comparative example. Wherein the addition amount of the hydrogen peroxide, the solution A, the solution B, the solution D and the dimethylacetamide is as follows according to the mass part ratio of the prenyl alcohol polyoxyethylene ether in the raw materials: 100 parts of prenyl alcohol polyoxyethylene ether, 0.6 part of hydrogen peroxide, 9 parts of solution A, 1.1 parts of solution B, 8 parts of solution D and 5 parts of dimethylacetamide.
Comparative example 4
A synthetic method of a high water-reducing and high slump-retaining water reducing agent comprises the following steps:
(1) adding water and prenyl polyoxyethylene ether into a reaction kettle according to the proportion that the water accounts for 73 parts by mass and the prenyl polyoxyethylene ether accounts for 100 parts by mass (relative molecular mass is 3000), stirring and dissolving, and keeping the temperature to 25-30 ℃; preparing aqueous solution of reducing agent as solution A, preparing mixed solution of acrylic acid, hydroxyethyl methacrylate, mercaptopropionic acid, polyethylene glycol diacrylate and water as solution B, preparing extract of oak leaves and dried orange peel as solution C, and preparing SbCl 3 、ZnCl 2 As solution D; wherein the reducing agent is vitamin C, and the mass fraction of the reducing agent in the solution A is 3 percent; the liquid B comprises the following components in parts by weight: 14 parts of acrylic acid, 2 parts of hydroxyethyl methacrylate, 1.2 parts of mercaptopropionic acid, 3 parts of polyethylene glycol diacrylate and 30 parts of water, wherein the relative molecular weight of the polyethylene glycol diacrylate is 500 daltons; the preparation method of the solution C comprises the following steps: mixing and chopping fresh oak leaves and dry orange peel according to the mass ratio of the oak leaves to the dry orange peel =10:3, pouring the chopped materials into ethyl acetate to form a mixture, keeping the feed liquid mass ratio of the chopped materials to the ethyl acetate =2:10, keeping the mixture at the constant temperature of 55 +/-5 ℃ in a water bath, and keeping the temperature for 3 hours; cooling in air to normal temperature after heat preservation, filtering to remove solid phase, decompressing and concentrating liquid phase to 1/3 of volume before concentration to obtain the oak leaf-dried orange peel extracting solution; the mass ratio of each component in the solution D is SbCl 3 ：ZnCl 2 : water =4:11: 100;
(2) adding hydrogen peroxide with the mass percent of 30% into the reaction kettle at the constant temperature of 25-30 ℃, stirring for 10min, and then dropwise adding the solution A, the solution B, the solution C and the solution D, wherein the dropwise adding time of the solution A is 2h, the dropwise adding time of the solution B is 1.5h, the dropwise adding time of the solution C is 1.5h, and the dropwise adding time of the solution D is 2 h; after the dropwise addition is finished, continuously preserving the heat for 2 hours; and after the heat preservation is finished, neutralizing the mixture by using a sodium hydroxide aqueous solution with the solute percentage content of 30% until the pH value is 7, and adding water to adjust the solid content to 40% to obtain the water reducing agent of the comparative example. Wherein the addition of the hydrogen peroxide, the solution A, the solution B, the solution C and the solution D and the mass portion ratio of the prenyl alcohol polyoxyethylene ether in the raw materials are as follows: 100 parts of prenyl polyoxyethylene ether, 0.6 part of hydrogen peroxide, 9 parts of liquid A, 1.1 parts of liquid B, 8 parts of liquid C and 8 parts of liquid D.
The water reducing agents prepared in the examples 1-4 and the comparative examples 1-4 are subjected to concrete function detection according to the method described in the national standard GB/8076- 3 ) Comprises the following steps: m (cement): m (fly ash): m (mineral powder): m (stone): m (sand): m (water) = 270: 75: 70: 1085: 785: 160, the mixing amount of the water reducing agent is 0.64 percent by mass, and the obtained results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the water reducer prepared by the method disclosed by the invention is high in initial fluidity when mixed with concrete, small in slump loss and expansion loss after 2 hours, good in water reducing performance, high in compressive strength and excellent in performance. As can be seen from comparison between example 3 and comparative examples 1 to 4, the solutions C and D of the present invention have an effect of improving the performance of the water reducing agent, which is probably caused by the fact that the reaction is more sufficient and the ionic groups on the internal main chain of the water reducing agent are increased.
While the technical solutions provided by the present invention have been described in detail above, for a person skilled in the art, according to the ideas of the embodiments of the present invention, there may be changes in the specific implementation manners and application ranges, and in summary, the contents of the present specification should not be construed as limiting the present invention.
Claims (8)
1. A synthetic method of a high water-reducing high slump-retaining water reducing agent is characterized by comprising the following steps:
(1) adding water and prenyl polyoxyethylene ether into a reaction kettle, stirring for dissolving, and keeping the temperature to 25-30 ℃; preparing aqueous solution of reducing agent as A liquid, preparing acrylic acid and hydroxyethyl methacrylateMixing the solution of ester, chain transfer agent, polyethylene glycol diacrylate and water as solution B, preparing the extractive solution of oak leaves and dried orange peel as solution C, and preparing SbCl 3 、ZnCl 2 As solution D; the preparation method of the solution C comprises the following steps: mixing and chopping fresh oak leaves and dry orange peel, pouring the chopped materials into ethyl acetate to form a mixture, carrying out water bath on the mixture, keeping the temperature to be 50-60 ℃, and carrying out heat preservation for 2-3 hours; after the heat preservation is finished, air cooling to normal temperature, filtering to remove solid phase, decompressing and concentrating liquid phase to obtain the oak leaf-dried orange peel extracting solution;
(2) adding an oxidant into the reaction kettle at a constant temperature of 25-30 ℃, stirring for 5-10 min, and then dropwise adding the solution A, the solution B, the solution C and the solution D, wherein the dropwise adding time of the solution A is 2-2.5 h, the dropwise adding time of the solution B is 1.5-2 h, the dropwise adding time of the solution C is 1.5-2 h, and the dropwise adding time of the solution D is 2-2.5 h; after the dropwise adding is finished, continuously preserving the heat for 2-2.5 h; neutralizing the mixture by using a sodium hydroxide solution until the pH value is 6-7 after heat preservation is finished, adding dimethylacetamide, and stirring for 10-15 min to obtain the high water-reducing high slump-retaining water reducer; wherein the oxidant is hydrogen peroxide with the mass percent of 30%, and the mass parts of the added oxidant, the solution A, the solution B, the solution C, the solution D and the dimethylacetamide to the prenyl alcohol polyoxyethylene ether are as follows: 100 parts of prenyl polyoxyethylene ether, 0.4-0.8 part of oxidant, 8-10 parts of liquid A, 1.0-1.3 parts of liquid B, 5-9 parts of liquid C, 3-10 parts of liquid D and 1-7 parts of dimethylacetamide; the percentage content of solute in the sodium hydroxide solution is 30%.
2. The method for synthesizing the high water reducing and slump retaining water reducing agent according to claim 1, wherein the reducing agent is vitamin C, and the mass fraction of the reducing agent in the solution A is 2-3%.
3. The method for synthesizing the high water reducing and high slump retaining water reducing agent according to claim 1, wherein the solution B comprises the following components in parts by weight: 10-15 parts of acrylic acid, 1-2 parts of hydroxyethyl methacrylate, 0.6-1.4 parts of a chain transfer agent, 2-4 parts of polyethylene glycol diacrylate and 20-30 parts of water; the molecular weight of the polyethylene glycol diacrylate is 400-600 daltons.
4. The method for synthesizing the high water reducing and slump retaining water reducing agent according to claim 3, wherein the chain transfer agent is mercaptopropionic acid.
5. The method for synthesizing the high water reducing and slump retaining water reducing agent according to claim 1, wherein the mixing mass ratio of fresh oak leaves to dry orange peel is oak leaves/dry orange peel =10: 2-3; the feed liquid mass ratio of the chopped materials to the ethyl acetate is that the chopped materials/ethyl acetate = 1-3: 10; the liquid phase was concentrated under reduced pressure to 1/3 in its unconcentrated volume.
6. The method for synthesizing the high water reducing and high slump retaining water reducing agent according to claim 1, wherein the mass ratio of the components in the solution D is SbCl 3 ：ZnCl 2 : water = 1-5: 8-13: 100.
7. The method for synthesizing the high water reducing and slump retaining water reducing agent according to claim 1, wherein in the step (1), the molecular weight of the isoamylene alcohol polyoxyethylene ether is 3000 daltons, the mass parts of water and the isoamylene alcohol polyoxyethylene ether are 70-76 parts of water, and the mass parts of the isoamylene alcohol polyoxyethylene ether are 100 parts.
8. A high water-reducing high slump-retaining water reducing agent, which is characterized by being prepared by the method of any one of claims 1 to 7.
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| CN101906167A (en) * | 2010-06-07 | 2010-12-08 | 新疆大学 | Method for preparing concrete water reducing agent by utilizing waste cellulose deposited in pulping black liquor |
| CN102786255A (en) * | 2012-07-17 | 2012-11-21 | 中科院广州化学有限公司 | Water-based mortar modifier, its preparation method and application |
| JP2013018672A (en) * | 2011-07-08 | 2013-01-31 | Hymo Corp | Additive for concrete or mortar, and use thereof |
| CN105367720A (en) * | 2015-11-25 | 2016-03-02 | 科之杰新材料集团有限公司 | Water-reducing slump-retaining type polycarboxylic acid water reducing agent and preparing method thereof |
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| CN101906167A (en) * | 2010-06-07 | 2010-12-08 | 新疆大学 | Method for preparing concrete water reducing agent by utilizing waste cellulose deposited in pulping black liquor |
| JP2013018672A (en) * | 2011-07-08 | 2013-01-31 | Hymo Corp | Additive for concrete or mortar, and use thereof |
| CN102786255A (en) * | 2012-07-17 | 2012-11-21 | 中科院广州化学有限公司 | Water-based mortar modifier, its preparation method and application |
| CN105367720A (en) * | 2015-11-25 | 2016-03-02 | 科之杰新材料集团有限公司 | Water-reducing slump-retaining type polycarboxylic acid water reducing agent and preparing method thereof |
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Denomination of invention: A high water reducing and high slump retaining water reducing agent and its synthesis method Effective date of registration: 20230620 Granted publication date: 20220913 Pledgee: Zhangping Branch of Industrial and Commercial Bank of China Ltd. Pledgor: Fujian Huifeng Construction Technology Co.,Ltd. Registration number: Y2023980044452 |