CN113248381B - Modified fatty acid, polycarboxylate superplasticizer and preparation method of polycarboxylate superplasticizer - Google Patents
Modified fatty acid, polycarboxylate superplasticizer and preparation method of polycarboxylate superplasticizer Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
- C07C69/52—Esters of acyclic unsaturated carboxylic acids having the esterified carboxyl group bound to an acyclic carbon atom
- C07C69/533—Monocarboxylic acid esters having only one carbon-to-carbon double bond
- C07C69/54—Acrylic acid esters; Methacrylic acid esters
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- 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
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
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- C07C67/26—Preparation of carboxylic acid esters by reacting carboxylic acids or derivatives thereof with a carbon-to-oxygen ether bond, e.g. acetal, tetrahydrofuran with an oxirane ring
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- C07D—HETEROCYCLIC COMPOUNDS
- C07D301/00—Preparation of oxiranes
- C07D301/02—Synthesis of the oxirane ring
- C07D301/03—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds
- C07D301/12—Synthesis of the oxirane ring by oxidation of unsaturated compounds, or of mixtures of unsaturated and saturated compounds with hydrogen peroxide or inorganic peroxides or peracids
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- C07D303/02—Compounds containing oxirane rings
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
- C04B2103/302—Water reducers
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Abstract
The invention discloses a modified fatty acid, a polycarboxylate superplasticizer and a preparation method of the polycarboxylate superplasticizer, wherein the modified fatty acid is prepared by the following method: (1) Taking a certain amount of formic acid and hydrogen peroxide (with the concentration of 30%), adding a certain amount of concentrated sulfuric acid, and uniformly mixing at 35 ℃ for later use; (2) Weighing a certain amount of unsaturated fatty acid, adding the unsaturated fatty acid into a reaction container, heating in a water bath, raising the temperature to 60 ℃, stirring at a constant speed, dropwise adding the reagent prepared in the step (1), finishing dropwise adding within 2 hours, and reacting for 1 hour under a constant temperature condition; after the reaction is finished, obtaining an intermediate product; (3) Adding a certain amount of FeCl into a container provided with a reflux cooler, an electric stirrer and a dropping funnel 3 And (3) reacting with methacrylic acid, and then dropwise adding the intermediate product obtained in the step (2) into the container to react for 9 hours to obtain the modified fatty acid. The air entraining performance of the polycarboxylate superplasticizer can be changed by adjusting the using amount of the modified fatty acid in the polycarboxylate superplasticizer.
Description
Technical Field
The invention belongs to the technical field of concrete admixtures, and particularly relates to a modified fatty acid, a polycarboxylic acid water reducing agent and a preparation method of the polycarboxylic acid water reducing agent.
Background
Compared with the traditional naphthalene water reducer and calcium lignosulfonate water reducer, the polycarboxylic acid high-performance water reducer has the advantages of high water reducing rate, high slump loss resistance, good durability, low shrinkage and the like, and is a concrete admixture which is most widely applied at the present stage.
Due to the polyether structure in the polycarboxylate superplasticizer, more air bubbles are easily introduced in the mixing process, and the air content of concrete is easily increased, so that the problem of poor apparent quality of concrete is caused. The bare concrete of some key projects has higher requirements on the concrete appearance quality, and a low-air-entraining polycarboxylate water reducing agent is needed to improve the pitted surface of the concrete.
The method for compounding the defoaming agent and the water reducing agent is simple and easy to implement, but the poor compatibility of part of the defoaming agent and the water reducing agent causes poor dispersibility of the defoaming agent, the homogeneity of the water reducing agent is influenced, and the defoaming agent is easy to separate from water along with the increase of the storage time and floats on the surface of the water reducing agent solution, so that the use effect of the defoaming agent is influenced.
Disclosure of Invention
In view of the above problems of the prior art, an object of an aspect of the present invention is to provide a modified fatty acid having an antifoaming function. And another aspect of the present invention is to provide a polycarboxylic acid water reducing agent comprising the modified fatty acid.
In order to achieve the above first aspect of the present invention, there is provided a modified fatty acid prepared by the following process:
(1) Taking a certain amount of formic acid and hydrogen peroxide (with the concentration of 30%), adding a certain amount of concentrated sulfuric acid, and uniformly mixing at 35 ℃ for later use;
(2) Weighing a certain amount of unsaturated fatty acid, adding the unsaturated fatty acid into a reaction container, heating in a water bath, raising the temperature to 60 ℃, stirring at a constant speed, dropwise adding the reagent prepared in the step (1), finishing dropwise adding within 2 hours, and reacting for 1 hour under a constant temperature condition; after the reaction is finished, cooling to normal temperature, standing for layering, removing a lower water layer by using a separating funnel, washing an oil layer by using hot alkali solution, washing the oil layer to be neutral by using softened water, removing the water layer to obtain an oil layer, then adding a small amount of ethanol, and carrying out reduced pressure distillation to remove an alcohol-oil mixture and impurities with low boiling point to obtain an intermediate product;
(3) Adding a certain amount of FeCl into a container provided with a reflux cooler, an electric stirrer and a dropping funnel 3 And (3) adding methacrylic acid, then dropwise adding the intermediate product obtained in the step (2) into the container within 40min, stirring at room temperature for 15min, heating to 65 ℃ for reaction for 9h, cooling to room temperature, filtering the catalyst, washing with diethyl ether, and distilling the diethyl ether and unreacted substances at normal pressure to obtain the modified fatty acid.
Preferably, during the preparation process, the unsaturated fatty acid is one or more of oleic acid, petroselinic acid and erucic acid.
Preferably, the use amounts of the unsaturated fatty acid, hydrogen peroxide, formic acid and concentrated sulfuric acid are, by weight, 30-35; the intermediate product FeCl 3 And the molar ratio of methacrylic acid is 1.1-1.3.
The polycarboxylic acid water reducing agent provided by the second aspect of the invention comprises the modified fatty acid, the polyether monomer with high molecular weight, unsaturated carboxylic acid, a chain transfer agent, an initiator and a reducing agent; wherein the polyether macromonomer comprises any one or a mixture of two of methyl allyl polyoxyethylene ether and isoamylene polyoxyethylene ether with the molecular weight of 2400-3000; the unsaturated carboxylic acid is one or a mixture of two of acrylic acid and methacrylic acid; the initiator is one or a mixture of more of ammonium persulfate, potassium persulfate and sodium persulfate; the reducing agent is: mixing one or more of vitamin C, sodium formaldehyde sulfoxylate, sodium bisulfite, sodium sulfite, and glucose; the chain transfer agent is one or a mixture of more of thioglycollic acid, mercaptopropionic acid and mercaptoethanol; the neutralizer is one or two of a 30% concentration aqueous solution of sodium hydroxide or a 30% concentration aqueous solution of potassium hydroxide.
Preferably, the content of each component comprises the following components in parts by weight:
350-375 parts of polyether macromonomer, 25-30 parts of unsaturated carboxylic acid, 2-4 parts of modified fatty acid, 5-9 parts of initiator, 0.4-1.6 parts of reducing agent, 0.7-1.5 parts of chain transfer agent, 15-20 parts of neutralizing agent and 381-424 parts of water.
In another aspect of the present invention, a method for preparing the above-mentioned polycarboxylic acid water reducing agent is also provided, which comprises:
uniformly stirring a polyether macromonomer, modified fatty acid, an initiator and a certain amount of water to obtain a solution A; uniformly stirring unsaturated carboxylic acid and a certain amount of water to form a solution B; uniformly stirring a reducing agent, a chain transfer agent and a certain amount of water to form a solution C, and dropwise adding the solution B, C into the solution A to perform free radical polymerization reaction to obtain the polycarboxylic acid water reducing agent.
Preferably, the method further comprises the steps of:
(1) Heating the solution A while stirring, wherein the heating temperature is 30-45 ℃;
(2) After the temperature of the solution A reaches a set temperature, dropwise adding the solution B and the solution C into the solution A at the same time, wherein the dropwise adding time of the solution B is 2-3h, and the dropwise adding time of the solution C is 0.5h longer than that of the solution B;
(3) After the solution B and the solution C are completely dripped, continuously preserving the heat for 2-3h;
(4) And adding a neutralizing agent into the polycarboxylic acid water reducing agent solution after heat preservation is finished, and adjusting the pH value of the solution to be 6-7.
Preferably, in the solution a, the weight ratio of the modified fatty acid to the polyether macromonomer to the initiator to the water is: 2-4:350-375:5-9:311-330.
Preferably, in the solution B, the weight ratio of the unsaturated carboxylic acid to the water is: 25-30:36-38.
Preferably, in the solution C, the weight ratio of the reducing agent to the chain transfer agent to the water is 0.4-1.6.
The invention has the following beneficial effects:
fatty acids are common defoaming agents, and the defoaming agents have good defoaming function, so that fatty acids with unsaturated bonds are polymerized to the molecular main chain of the polycarboxylate water reducer, but the double bonds of the unsaturated fatty acids are not easy to generate free radical polymerization reaction, so that the double bonds of the unsaturated fatty acids need to be modified to prepare modified fatty acids, the activity of the modified fatty acids is greatly enhanced, the polycarboxylate water reducer with various molecular weights can be synthesized by free radicals, and the air entraining property of the polycarboxylate water reducer can be changed by adjusting the amount of the modified fatty acids.
Through free radical polymerization, the modified fatty acid is polymerized into a polycarboxylic acid molecular structure, so that the problem of poor water solubility of the fatty acid defoaming agent is solved to a great extent, and the problems of poor compatibility and poor placement stability caused by compounding the defoaming agent are avoided.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.
This document provides an overview of various implementations or examples of the technology described in this disclosure, and is not a comprehensive disclosure of the full scope or all features of the disclosed technology.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present disclosure more apparent, the technical solutions of the embodiments of the present disclosure will be clearly and completely described below.
It is to be understood that the described embodiments are only a few embodiments of the present disclosure, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the disclosure without any inventive step, are within the scope of protection of the disclosure.
Example 1
The preparation method of the low-air-entraining polycarboxylate superplasticizer comprises the following steps of:
(1) Synthesis of modified fatty acid:
70g of formic acid and 285g of hydrogen peroxide (with the concentration of 30%) are taken, 2.5g of concentrated sulfuric acid is added, and the mixture is uniformly mixed at the temperature of 35 ℃ for later use. And then weighing 310g of oleic acid, adding the oleic acid into a reaction vessel, heating in a water bath, raising the temperature to 60 ℃, uniformly stirring, dropwise adding a mixture of hydrogen peroxide and formic acid into the mixture within 2 hours, and reacting for 1 hour under a constant temperature condition. After the reaction is finished, cooling to normal temperature, standing for layering, removing a lower water layer by using a separating funnel, washing an oil layer by using hot alkali solution, washing to be neutral by using softened water, removing the water layer to obtain an oil layer, adding 80ml of ethanol, and distilling under reduced pressure to remove an alcohol-oil mixture and impurities with low boiling point to obtain an intermediate product.
1.58g of FeCl was added to a vessel equipped with a reflux condenser, an electric stirrer and a dropping funnel 3 And 86g of methacrylic acid, then 298.1g of intermediate product is dripped into the container within 40min, stirred at room temperature for 15min, heated to 65 ℃ for reaction for 9h, cooled to room temperature, the catalyst is filtered and washed by diethyl ether, and diethyl ether and unreacted substances are distilled out at normal pressure to obtain the modified fatty acid ZF-1.
355g of isoamylene polyoxyethylene ether with the molecular weight of 2400, 2.3g of modified fatty acid ZF-1 and 304g of water are added into a four-neck flask, stirred until the polyether is completely dissolved, then heated to 35 ℃, and after the temperature is constant, 5.5g of sodium persulfate is added, stirred uniformly, and prepared into liquid A. 27g of acrylic acid and 37g of water were mixed to prepare a solution B, and 1.5g of thioglycolic acid, 0.7g of vitamin C and 48g of water were mixed to prepare a solution C.
Simultaneously, dropwise adding the solution B and the solution C into the solution A, dropwise adding the solution B for 2h, dropwise adding the solution C for 2.5h, and preserving heat for 2h after dropwise adding. And (3) when the temperature is reduced to 30 ℃, slowly adding 16g of sodium hydroxide solution with the mass fraction of 30%, and fully stirring for 20min to obtain the low air entraining type water reducing agent XP-1 with the mass fraction of about 50%.
Example 2
The preparation method of the low-air-entraining polycarboxylate superplasticizer comprises the following steps of:
(1) Synthesis of modified fatty acid:
73g of formic acid and 295g of hydrogen peroxide (30 percent concentration) are taken, 3.5g of concentrated sulfuric acid is added, and the mixture is uniformly mixed at the temperature of 35 ℃ for later use. And then 324g of petroselinic acid is weighed and added into a reaction vessel, after the reaction vessel is heated in a water bath and heated to 60 ℃, the mixture of hydrogen peroxide and formic acid is dropwise added into the reaction vessel at a constant speed and stirred at a constant speed, the dropwise addition is finished within 2 hours, and then the reaction vessel is reacted for 1 hour under a constant temperature condition. After the reaction is finished, cooling to normal temperature, standing for layering, removing a lower water layer by using a separating funnel, washing an oil layer by using hot alkali solution, washing the oil layer to be neutral by using softened water, removing the water layer to obtain an oil layer, adding 95ml of ethanol, and distilling under reduced pressure to remove an alcohol-oil mixture and impurities with low boiling point to obtain an intermediate product.
1.86g FeCl was added to a vessel equipped with a reflux condenser, an electric stirrer, and a dropping funnel 3 And 86g of methacrylic acid, dripping 299g of an intermediate product into the container within 40min, stirring at room temperature for 15min, heating to 65 ℃, reacting for 9h, cooling to room temperature, filtering out the catalyst, washing with diethyl ether, and distilling the diethyl ether and unreacted substances at normal pressure to obtain the modified fatty acid ZF-2.
Adding 360g of methyl allyl polyoxyethylene ether with the molecular weight of 2800, 3g of modified fatty acid ZF-2 and 315g of water into a four-neck flask, stirring until the polyether is completely dissolved, then heating to 35 ℃, adding 6.2g of ammonium persulfate after the temperature is constant, and stirring uniformly to prepare solution A. Liquid B was prepared by mixing 26g of acrylic acid with 37g of water, and liquid C was prepared by mixing 1.3g of mercaptopropionic acid, 0.7g of sodium formaldehyde sulfoxylate C, and 45g of water.
Simultaneously dripping the solution B and the solution C into the solution A, dripping the solution B for 2.5 hours, dripping the solution C for 3 hours, and preserving heat for 2 hours after dripping is finished. And (3) when the temperature is reduced to 30 ℃, slowly adding 17g of 30 mass percent sodium hydroxide solution, and fully stirring for 20min to obtain the low air entraining type water reducing agent XP-2 with the mass percent of about 50%.
Actual test results
The two types of low bleed air type water reducing agents described above were compared with a commercially available water reducing agent in a comparative test using a C30 concrete as an evaluation target, and the air content, the extension, the 7d and 28d compressive strengths, the apparent quality of the concrete, and the like of the concrete were compared. The performance of the concrete mixture is tested according to GB/T50080-2016 Standard test method for the Performance of common concrete mixtures; the concrete strength is tested according to GB/T50081-2019 Standard of mechanical Properties test method of ordinary concrete.
Table 1: concrete mixing proportion
| Material | Cement | Mineral powder | River sand | Stone | Water (W) | Additive agent |
| Dosage (kg) | 312 | 78 | 817 | 998 | 175 | 6.5kg |
Note: the additive is 10% solid, the fineness modulus of river sand is 2.6, and the broken stone is 5-20mm continuous graded broken stone.
Table 2: concrete Performance test results
As shown in table 2, the spread was the smallest in example 1, the largest in example 2 and market 1, and the spread was the largest in market 2. The gas contents of the concrete in the examples 1 and 2 are respectively 1.9% and 2.1%, the gas contents are obviously reduced compared with the two water reducing agents sold in the market, and the concrete surface is smooth and has no large bubbles compared with the two water reducing agents sold in the market, so that the defoaming type polycarboxylate water reducing agent has low air entraining property and has a great effect of improving the apparent quality of the concrete. The strength of the concrete doped with the water reducing agent of the example 1 and the water reducing agent of the example 2 is higher in both 7d and 28d than those of the two water reducing agents sold in the market, so that the defoaming type polycarboxylate water reducing agent can enhance the compactness of a concrete structure and improve the strength of the concrete in different ages.
The above examples are only used to illustrate the technical solution of the present invention, and not to limit the same; numerous embodiments can be derived, and it will be understood by those skilled in the art that modifications can be made to the embodiments described in the foregoing examples, or equivalent replacements can be made to some or all of the technical features, without departing from the scope of the embodiments of the present invention.
The above embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and the scope of the present invention is defined by the claims. Various modifications and equivalents may be made by those skilled in the art within the spirit and scope of the present invention, and such modifications and equivalents should also be considered as falling within the scope of the present invention.
Claims (10)
1. A modified fatty acid prepared by the process of:
(1) Taking a certain amount of formic acid and hydrogen peroxide with the concentration of 30%, adding a certain amount of concentrated sulfuric acid, and uniformly mixing at 35 ℃ for later use;
(2) Weighing a certain amount of unsaturated fatty acid, adding the unsaturated fatty acid into a reaction container, heating in a water bath, raising the temperature to 60 ℃, stirring at a constant speed, dropwise adding the reagent prepared in the step (1), finishing dropwise adding within 2 hours, and reacting for 1 hour under a constant temperature condition; after the reaction is finished, cooling to normal temperature, standing for layering, removing a lower water layer by using a separating funnel, washing an oil layer by using hot alkali solution, washing the oil layer to be neutral by using softened water, removing the water layer to obtain an oil layer, adding a small amount of ethanol, and distilling under reduced pressure to remove an alcohol-oil mixture and impurities with low boiling point to obtain an intermediate product;
(3) Adding a certain amount of FeCl into a container provided with a reflux cooler, an electric stirrer and a dropping funnel 3 And (3) adding methacrylic acid, then dropwise adding the intermediate product obtained in the step (2) into the container within 40min, stirring at room temperature for 15min, heating to 65 ℃ for reaction for 9h, cooling to room temperature, filtering the catalyst, washing with diethyl ether, and distilling the diethyl ether and unreacted substances at normal pressure to obtain the modified fatty acid.
2. The modified fatty acid of claim 1, wherein the unsaturated fatty acid is one or more of oleic acid, petroselinic acid, and erucic acid.
3. The modified fatty acid as claimed in claim 1, wherein in the preparation process, the unsaturated fatty acid, hydrogen peroxide, formic acid and concentrated sulfuric acid are used in the following ratio of 30-35 (parts by weight); the intermediate product FeCl 3 And the molar ratio of methacrylic acid is 1.1-1.3.
4. A polycarboxylic acid water reducing agent comprising the modified fatty acid of any one of claims 1 to 3, a high molecular weight polyether monomer, an unsaturated carboxylic acid, a chain transfer agent, an initiator, a neutralizing agent and a reducing agent; wherein, the polyether monomer with large molecular weight comprises any one or the mixture of two of methyl allyl polyoxyethylene ether and isoamylene polyoxyethylene ether with the molecular weight of 2400-3000; the unsaturated carboxylic acid is one or a mixture of two of acrylic acid and methacrylic acid; the initiator is one or a mixture of ammonium persulfate, potassium persulfate and sodium persulfate; the reducing agent is: mixing one or more of vitamin C, sodium formaldehyde sulfoxylate, sodium bisulfite, sodium sulfite, and glucose; the chain transfer agent is one or a mixture of more of thioglycolic acid, mercaptopropionic acid and mercaptoethanol; the neutralizer is one or two of a 30% concentration aqueous solution of sodium hydroxide or a 30% concentration aqueous solution of potassium hydroxide.
5. The polycarboxylate water reducer as set forth in claim 4, wherein the contents of said components are, in parts by weight:
350-375 parts of high molecular weight polyether monomer, 25-30 parts of unsaturated carboxylic acid, 2-4 parts of modified fatty acid, 5-9 parts of initiator, 0.4-1.6 parts of reducing agent, 0.7-1.5 parts of chain transfer agent, 15-20 parts of neutralizing agent and 383-421 parts of water.
6. The method for producing a polycarboxylic acid water reducing agent according to claim 4 or 5, comprising:
uniformly stirring a polyether monomer with large molecular weight, modified fatty acid, an initiator and a certain amount of water to obtain a solution A; uniformly stirring unsaturated carboxylic acid and a certain amount of water to form a solution B; uniformly stirring a reducing agent, a chain transfer agent and a certain amount of water to form a solution C, and dropwise adding the solution B, C into the solution A to perform free radical polymerization reaction to obtain the polycarboxylic acid water reducing agent.
7. The method for preparing a polycarboxylic acid water reducing agent as claimed in claim 6, comprising the steps of:
(1) Heating the solution A while stirring, wherein the heating temperature is 30-45 ℃;
(2) After the temperature of the solution A reaches a set temperature, dropwise adding the solution B and the solution C into the solution A at the same time, wherein the dropwise adding time of the solution B is 2-3h, and the dropwise adding time of the solution C is 0.5h longer than that of the solution B;
(3) After the solution B and the solution C are completely dripped, continuously preserving the heat for 2-3h;
(4) And adding a neutralizing agent into the polycarboxylic acid water reducing agent solution after heat preservation is finished, and adjusting the pH value of the solution to be 6-7.
8. The method for preparing a polycarboxylic acid water reducing agent according to claim 7, wherein in the solution A, the weight ratio of the modified fatty acid, the high molecular weight polyether monomer, the initiator and the water is as follows: 2-4:350-375:5-9:311-330.
9. The method for preparing a polycarboxylic acid water reducing agent according to claim 7, wherein in the solution B, the weight ratio of the unsaturated carboxylic acid to the water is: 25-30:36-38.
10. The method for preparing a polycarboxylic acid water reducing agent according to claim 7, wherein in said solution C, the weight ratio of reducing agent, chain transfer agent and water is 0.4-1.6.
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