CN112661912A - Polycarboxylic acid series-containing composite activated cement reinforced grinding aid and preparation method thereof - Google Patents
Polycarboxylic acid series-containing composite activated cement reinforced grinding aid and preparation method thereof Download PDFInfo
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- CN112661912A CN112661912A CN202011454413.9A CN202011454413A CN112661912A CN 112661912 A CN112661912 A CN 112661912A CN 202011454413 A CN202011454413 A CN 202011454413A CN 112661912 A CN112661912 A CN 112661912A
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Abstract
The invention discloses a polycarboxylic acid series-containing composite activated cement reinforced grinding aid, which is prepared from the following raw materials in parts by weight: 50-250 parts of polyethylene glycol maleate, 25-125 parts of esterifying agent, 70-200 parts of macromonomer allyl polyethylene glycol, 4-20 parts of initiator, 20-60 parts of solution and the balance of ionized water; the composite activated cement reinforced grinding aid containing the polycarboxylic acid series can prevent particles from agglomerating, can prevent cracks generated on the surfaces of the particles from healing again in the grinding process, is beneficial to the grinding process, and further has a good grinding aid effect.
Description
Technical Field
The invention relates to the technical field of cement production and processing, in particular to a polycarboxylic acid series-containing composite activated cement reinforced grinding aid and a preparation method thereof.
Background
The cement is an indispensable building material in national economic development, has great demand on resources or energy sources such as limestone, coal, electric power and the like, can form industrial dust in the cement production process, discharges a large amount of harmful gases such as C02 and S02 and the like, and has serious influence on the living environment of human beings; at present, in order to improve the grinding efficiency, two methods are mainly adopted by cement enterprises, namely, the structure of a grinding machine, the grinding process flow and the grinding mode are improved to enable more machines to act on the grinding of materials through grinding media, and the most effective method is to add a powder selecting device, so that the grinding efficiency can be improved by about 15%, but equipment, investment and additional power consumption are required to be increased. Secondly, a small amount of chemical agent is added into the grinding system to influence the mechanical and chemical process of grinding operation, improve the fluidity of materials in the mill, accelerate the grinding and the grinding simultaneously, and achieve the purpose of improving the grinding efficiency, the chemical additive is a grinding aid, the two methods use the cement grinding aid as the second method, which is the most convenient and practical, has low investment and quick effect, can greatly improve the grinding efficiency, can reach about 20 percent, and can improve the physical and chemical properties of the cement; at present, most of grinding aids in the market are surfactants, organic alcamines, fatty acids and salts thereof, the quality and the using effect of the grinding aids are low, and a large amount of harmful substances are contained in the grinding aids, so that the grinding aids are easy to corrode reinforcing steel bars and pollute the environment; chinese patent CN101182149A discloses a polycarboxylic acid-containing composite activated cement reinforced grinding aid, which is prepared by synthesizing an esterification catalyst, a polymerization inhibitor, an initiator, a grinding aid, an activating agent, a reinforcing agent, a blender and a chain transfer agent.
At present, the reinforced grinding aid is mainly prepared by mixing raw materials such as triethanolamine, chloride, sodium sulfate and the like, chloride ions in the chloride easily cause corrosion of reinforcing steel bars, so that the reinforced concrete structure is easily damaged, and toxic substances are contained in the raw materials, so that the environment pollution is easily caused.
Disclosure of Invention
In order to overcome the technical problems, the invention provides a polycarboxylic acid series-containing composite activated cement reinforced grinding aid and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
the composite activated cement reinforced grinding aid containing the polycarboxylic acid series is characterized by being prepared from the following raw materials in parts by weight: 50-250 parts of polyethylene glycol maleate, 25-125 parts of esterifying agent, 70-200 parts of macromonomer allyl polyethylene glycol, 4-20 parts of initiator, 20-60 parts of solution and the balance of ionized water.
Further, the esterifying agent is one or two of polyethylene glycol monomethyl ether and triethanolamine; the addition mass of the esterifying agent accounts for 50% of the addition amount of the polyethylene glycol maleic acid ester.
Further, the solution is specifically one or two of calcium hydroxide and sodium hydroxide; the adding mass of the solution accounts for 2-5% of the total mass of the polycarboxylic acid series-containing composite activated cement reinforced grinding aid.
Further, the initiator is specifically ammonium persulfate; the addition mass of the initiator accounts for 1-4% of the total mass of the polycarboxylic acid series-containing composite activated cement reinforced grinding aid.
The preparation method of the polycarboxylic acid series-containing composite activated cement reinforced grinding aid comprises the following steps:
step one, esterification reaction: adding a certain weight part of polyethylene glycol maleic acid ester and an esterifying agent into a reaction kettle A for reaction, and controlling the temperature to be 45-65 ℃ and the time to be 15-30 min; then adding the mixture into a water bath kettle for heating at the temperature of 70-90 ℃, and stirring by using a stirrer in the heating process for 2-3 hours to obtain a yellow clear mixture;
step two, polymerization reaction: adding macromonomer allyl polyethylene glycol into a reaction kettle B for primary reaction, controlling the temperature to be 60-80 ℃ and the time to be 1.5-3h, after the primary reaction, sequentially adding ionized water, polyethylene glycol maleate, a yellow clear mixture and an initiator into the reaction kettle B for secondary reaction, controlling the temperature to be 50-80 ℃ and the time to be 1.5-3h, and stirring by using a stirrer for 1-1.5 h;
step three, neutralization adjustment: after the dimerization reaction in the steps, the temperature is kept for 30-60min, then cooling is carried out, the temperature is controlled to be below 35 ℃, then the solution is added into a reaction kettle B, the pH value is reduced to 6-8, and standing is carried out for 10-15min, so that the polycarboxylic acid series-containing composite activated cement reinforced grinding aid is obtained.
Further, the stirring speed of the stirrer in the step one is 500r/min, forward rotation and reverse rotation are alternately carried out during stirring, the times of forward rotation and reverse rotation are 3-5 times, and the interval between alternate rotation and reverse rotation is 2-5 minutes; and step two, the stirring speed of the stirrer is 300r/min, forward rotation and reverse rotation are alternately carried out during stirring, the times of forward rotation and reverse rotation are 2-3 times, and the interval of alternate rotation is 1-2 minutes.
Further, the stirrer is a precise timing magnetic stirrer, and the water bath pot is a two-hole intelligent water bath pot.
The invention has the beneficial effects that:
(1) according to the invention, one or more of polyethylene glycol monomethyl ether and triethanolamine are used as an esterifying agent, the esterifying agent can react with polyethylene glycol maleic acid ester, and the esterifying agent and the polyethylene glycol maleic acid ester respectively have polar carboxyl and hydroxyl, so that polar groups can be adsorbed on the particle surface in the cement grinding process, residual valence bonds and charges on the particle surface are balanced, the particles can be prevented from agglomerating with each other, cracks generated on the particle surface in the grinding process can be prevented from healing again, the grinding process is facilitated, and the grinding aid has a good grinding aid effect.
(2) The composite activated cement reinforced grinding aid containing the polycarboxylic acid series is a high-molecular grinding aid, polyethylene glycol maleate and an esterifying agent are used as raw materials of the reinforced grinding aid, and compared with the traditional method for preparing the grinding aid by using triethanolamine, chloride salt, sodium sulfate and other raw materials, the raw materials used by the composite activated cement reinforced grinding aid containing the polycarboxylic acid series are low in price, non-toxic and harmless, beneficial to reducing environmental pollution and easy to popularize.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The composite activated cement reinforced grinding aid containing the polycarboxylic acid series is characterized by being prepared from the following raw materials in parts by weight: 50 parts of polyethylene glycol maleate, 25 parts of esterifying agent, 70 parts of macromonomer allyl polyethylene glycol, 4 parts of initiator, 20 parts of solution and the balance of ionized water.
The esterifying agent is one or two of polyethylene glycol monomethyl ether and triethanolamine; the addition mass of the esterifying agent accounts for 50% of the addition amount of the polyethylene glycol maleic acid ester.
The solution is one or two of calcium hydroxide and sodium hydroxide; the adding mass of the solution accounts for 2 percent of the total mass of the composite activated cement reinforced grinding aid containing polycarboxylic acid series.
The initiator is specifically ammonium persulfate; the addition mass of the initiator accounts for 1 percent of the total mass of the composite activated cement reinforced grinding aid containing the polycarboxylic acid series.
The preparation method of the polycarboxylic acid series-containing composite activated cement reinforced grinding aid comprises the following steps:
step one, esterification reaction: adding a certain weight part of polyethylene glycol maleic acid ester and an esterifying agent into a reaction kettle A for reaction, and controlling the temperature to be 45 ℃ and the time to be 15 min; then adding the mixture into a water bath kettle for heating, wherein the heating temperature is 70 ℃, and stirring by using a stirrer in the heating process for 2 hours to obtain a yellow clear mixture;
step two, polymerization reaction: adding macromonomer allyl polyethylene glycol into a reaction kettle B to perform a primary reaction, controlling the temperature at 60 ℃ for 1.5h, sequentially adding ionized water, polyethylene glycol maleate, a yellow clear mixture and an initiator into the reaction kettle B to perform a secondary reaction after the primary reaction, controlling the temperature at 50 ℃ for 1.5h, and stirring by using a stirrer for 1 h;
step three, neutralization adjustment: after the dimerization reaction in the steps, the temperature is kept for 30min, then cooling is carried out, the temperature is controlled to be below 35 ℃, then the solution is added into a reaction kettle B, the pH value is reduced to 6, and standing is carried out for 10min, so that the polycarboxylic acid series-containing composite activated cement reinforced grinding aid is obtained.
Step one, the stirring speed of a stirrer is 500r/min, forward rotation and reverse rotation are alternately carried out during stirring, the times of forward rotation and reverse rotation are 3 times, and the interval of alternate rotation is 2 minutes; and step two, the stirring speed of the stirrer is 300r/min, forward rotation and reverse rotation are alternately carried out during stirring, the times of forward rotation and reverse rotation are 2 times, and the interval of alternate rotation is 1 minute.
The stirrer is a precise timing magnetic stirrer, and the water bath pot is a two-hole intelligent water bath pot.
Example 2
The composite activated cement reinforced grinding aid containing the polycarboxylic acid series is characterized by being prepared from the following raw materials in parts by weight: 100 parts of polyethylene glycol maleate, 50 parts of esterifying agent, 100 parts of macromonomer allyl polyethylene glycol, 10 parts of initiator, 30 parts of solution and the balance of ionized water.
The esterifying agent is one or two of polyethylene glycol monomethyl ether and triethanolamine; the addition mass of the esterifying agent accounts for 50% of the addition amount of the polyethylene glycol maleic acid ester.
The solution is one or two of calcium hydroxide and sodium hydroxide; the adding mass of the solution accounts for 3 percent of the total mass of the composite activated cement reinforced grinding aid containing polycarboxylic acid series.
The initiator is specifically ammonium persulfate; the addition mass of the initiator accounts for 2 percent of the total mass of the composite activated cement reinforced grinding aid containing the polycarboxylic acid series.
The preparation method of the polycarboxylic acid series-containing composite activated cement reinforced grinding aid comprises the following steps:
step one, esterification reaction: adding a certain weight part of polyethylene glycol maleic acid ester and an esterifying agent into a reaction kettle A for reaction, and controlling the temperature to be 50 ℃ and the time to be 20 min; then adding the mixture into a water bath kettle for heating, wherein the heating temperature is 80 ℃, and stirring by using a stirrer in the heating process for 2.5 hours to obtain a yellow clear mixture;
step two, polymerization reaction: adding macromonomer allyl polyethylene glycol into a reaction kettle B to perform a primary reaction, controlling the temperature to be 65 ℃ and the time to be 2 hours, after the primary reaction, sequentially adding ionized water, polyethylene glycol maleate, a yellow clear mixture and an initiator into the reaction kettle B to perform a secondary reaction, controlling the temperature to be 60 ℃ and the time to be 2 hours, and stirring by using a stirrer for 1 hour;
step three, neutralization adjustment: after the dimerization reaction, the temperature is kept for 40min, then cooling is carried out, the temperature is controlled to be below 35 ℃, then the solution is added into a reaction kettle B, the pH value is reduced to 6, and standing is carried out for 10min, so that the polycarboxylic acid series-containing composite activated cement reinforced grinding aid is obtained.
Step one, the stirring speed of a stirrer is 500r/min, forward rotation and reverse rotation are alternately carried out during stirring, the times of forward rotation and reverse rotation are 4 times, and the interval of alternate rotation is 3 minutes; and step two, the stirring speed of the stirrer is 300r/min, forward rotation and reverse rotation are alternately carried out during stirring, the times of forward rotation and reverse rotation are 2 times, and the interval of alternate rotation is 1 minute.
The stirrer is a precise timing magnetic stirrer, and the water bath pot is a two-hole intelligent water bath pot.
Example 3
The composite activated cement reinforced grinding aid containing the polycarboxylic acid series is characterized by being prepared from the following raw materials in parts by weight: 150 parts of polyethylene glycol maleate, 75 parts of esterifying agent, 100 parts of macromonomer allyl polyethylene glycol, 15 parts of initiator, 40 parts of solution and the balance of ionized water.
The esterifying agent is one or two of polyethylene glycol monomethyl ether and triethanolamine; the addition mass of the esterifying agent accounts for 50% of the addition amount of the polyethylene glycol maleic acid ester.
The solution is one or two of calcium hydroxide and sodium hydroxide; the adding mass of the solution accounts for 4 percent of the total mass of the composite activated cement reinforced grinding aid containing polycarboxylic acid series.
The initiator is specifically ammonium persulfate; the addition mass of the initiator accounts for 3 percent of the total mass of the polycarboxylic acid series-containing composite activated cement reinforced grinding aid.
The preparation method of the polycarboxylic acid series-containing composite activated cement reinforced grinding aid comprises the following steps:
step one, esterification reaction: adding a certain weight part of polyethylene glycol maleic acid ester and an esterifying agent into a reaction kettle A for reaction, and controlling the temperature to be 55 ℃ and the time to be 25 min; then adding the mixture into a water bath kettle for heating, wherein the heating temperature is 85 ℃, and stirring by using a stirrer in the heating process for 3 hours to obtain a yellow clear mixture;
step two, polymerization reaction: adding macromonomer allyl polyethylene glycol into a reaction kettle B to perform primary reaction, controlling the temperature to be 75 ℃ and the time to be 2.5h, after the primary reaction, sequentially adding ionized water, polyethylene glycol maleate, a yellow clear mixture and an initiator into the reaction kettle B to perform secondary reaction, controlling the temperature to be 75 ℃ and the time to be 2.5h, and stirring by using a stirrer for 1.5 h;
step three, neutralization adjustment: and (3) after the dimerization reaction, keeping the temperature for 55min, cooling, controlling the temperature to be below 35 ℃, adding the solution into the reaction kettle B, reducing the pH value to 8, and standing for 15min to obtain the polycarboxylic acid series-containing composite activated cement reinforced grinding aid.
Step one, the stirring speed of a stirrer is 500r/min, forward rotation and reverse rotation are alternately carried out during stirring, the times of forward rotation and reverse rotation are 4 times, and the interval of alternate rotation is 4 minutes; and step two, the stirring speed of the stirrer is 300r/min, forward rotation and reverse rotation are alternately carried out during stirring, the times of forward rotation and reverse rotation are 3 times, and the interval of alternate rotation is 2 minutes.
The stirrer is a precise timing magnetic stirrer, and the water bath pot is a two-hole intelligent water bath pot.
Example 4
The composite activated cement reinforced grinding aid containing the polycarboxylic acid series is characterized by being prepared from the following raw materials in parts by weight: 250 parts of polyethylene glycol maleate, 125 parts of esterifying agent, 200 parts of macromonomer allyl polyethylene glycol, 20 parts of initiator, 60 parts of solution and the balance of ionized water.
The esterifying agent is one or two of polyethylene glycol monomethyl ether and triethanolamine; the addition mass of the esterifying agent accounts for 50% of the addition amount of the polyethylene glycol maleic acid ester.
The solution is one or two of calcium hydroxide and sodium hydroxide; the adding mass of the solution accounts for 5 percent of the total mass of the composite activated cement reinforced grinding aid containing polycarboxylic acid series.
The initiator is specifically ammonium persulfate; the addition mass of the initiator accounts for 4% of the total mass of the polycarboxylic acid series-containing composite activated cement reinforced grinding aid.
The preparation method of the polycarboxylic acid series-containing composite activated cement reinforced grinding aid comprises the following steps:
step one, esterification reaction: adding a certain weight part of polyethylene glycol maleic acid ester and an esterifying agent into a reaction kettle A for reaction, and controlling the temperature to be 65 ℃ and the time to be 30 min; then adding the mixture into a water bath kettle for heating, wherein the heating temperature is 90 ℃, and stirring by using a stirrer in the heating process for 3 hours to obtain a yellow clear mixture;
step two, polymerization reaction: adding macromonomer allyl polyethylene glycol into a reaction kettle B to perform a primary reaction, controlling the temperature to be 80 ℃ and the time to be 3h, after the primary reaction, sequentially adding ionized water, polyethylene glycol maleate, a yellow clear mixture and an initiator into the reaction kettle B to perform a secondary reaction, controlling the temperature to be 80 ℃ and the time to be 3h, and stirring by using a stirrer for 1.5 h;
step three, neutralization adjustment: after the dimerization reaction, the temperature is kept for 60min, then cooling is carried out, the temperature is controlled to be below 35 ℃, then the solution is added into a reaction kettle B, the pH value is reduced to 8, and standing is carried out for 15min, so that the polycarboxylic acid series-containing composite activated cement reinforced grinding aid is obtained.
Step one, the stirring speed of a stirrer is 500r/min, forward rotation and reverse rotation are alternately carried out during stirring, the times of forward rotation and reverse rotation are 5 times, and the interval of alternate rotation is 5 minutes; and step two, the stirring speed of the stirrer is 300r/min, forward rotation and reverse rotation are alternately carried out during stirring, the times of forward rotation and reverse rotation are 3 times, and the interval of alternate rotation is 2 minutes.
The stirrer is a precise timing magnetic stirrer, and the water bath pot is a two-hole intelligent water bath pot.
Comparative example 1
The comparative example is a cement reinforced grinding aid in the market.
Placing 60% of clinker, 5% of gypsum and 35% of fly ash into a mill, and respectively adding 0.08% of cement reinforced grinding aid in examples 1, 2, 3, 4 and 1, wherein the mixing amount is the same; the test results were measured as shown in the following table;
as can be seen from the above-mentioned examples 1-4 and comparative example 1, compared with the cement reinforced grinding aid in the market, the polycarboxylic acid series-containing composite activated cement reinforced grinding aid of the invention has better grinding aid effect, lower cement fineness and larger specific surface area, and the flexural strength of 3 days and 28 days and the compressive strength of 3 days and 28 days are both stronger than those of the cement reinforced grinding aid sold in the market.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. The composite activated cement reinforced grinding aid containing the polycarboxylic acid series is characterized by being prepared from the following raw materials in parts by weight: 50-250 parts of polyethylene glycol maleate, 25-125 parts of esterifying agent, 70-200 parts of macromonomer allyl polyethylene glycol, 4-20 parts of initiator, 20-60 parts of solution and the balance of ionized water.
2. The composite activated cement reinforced grinding aid containing the polycarboxylic acid series as claimed in claim 1, wherein the esterifying agent is one or two of polyethylene glycol monomethyl ether and triethanolamine; the addition mass of the esterifying agent accounts for 50% of the addition amount of the polyethylene glycol maleic acid ester.
3. The composite activated cement reinforced grinding aid containing the polycarboxylic acid series according to claim 1, characterized in that the solution is one or two of calcium hydroxide and sodium hydroxide; the adding mass of the solution accounts for 2-5% of the total mass of the polycarboxylic acid series-containing composite activated cement reinforced grinding aid.
4. The polycarboxylic acid series-containing composite activated cement reinforced grinding aid as claimed in claim 1, wherein the initiator is ammonium persulfate; the addition mass of the initiator accounts for 1-4% of the total mass of the polycarboxylic acid series-containing composite activated cement reinforced grinding aid.
5. The preparation method of the composite activated cement reinforced grinding aid containing the polycarboxylic acid series is characterized by comprising the following steps:
step one, esterification reaction: adding a certain weight part of polyethylene glycol maleic acid ester and an esterifying agent into a reaction kettle A for reaction, and controlling the temperature to be 45-65 ℃ and the time to be 15-30 min; then adding the mixture into a water bath kettle for heating at the temperature of 70-90 ℃, and stirring by using a stirrer in the heating process for 2-3 hours to obtain a yellow clear mixture;
step two, polymerization reaction: adding macromonomer allyl polyethylene glycol into a reaction kettle B for primary reaction, controlling the temperature to be 60-80 ℃ and the time to be 1.5-3h, after the primary reaction, sequentially adding ionized water, polyethylene glycol maleate, a yellow clear mixture and an initiator into the reaction kettle B for secondary reaction, controlling the temperature to be 50-80 ℃ and the time to be 1.5-3h, and stirring by using a stirrer for 1-1.5 h;
step three, neutralization adjustment: after the dimerization reaction in the steps, the temperature is kept for 30-60min, then cooling is carried out, the temperature is controlled to be below 35 ℃, then the solution is added into a reaction kettle B, the pH value is reduced to 6-8, and standing is carried out for 10-15min, so that the polycarboxylic acid series-containing composite activated cement reinforced grinding aid is obtained.
6. The preparation method of the composite activated cement reinforced grinding aid containing polycarboxylic acid series according to claim 5, characterized in that the stirring speed of the stirrer in the step one is 500r/min, the forward rotation and the reverse rotation are alternately carried out during stirring, the times of the forward rotation and the reverse rotation are 3-5 times, and the interval between the forward rotation and the reverse rotation is 2-5 minutes; and step two, the stirring speed of the stirrer is 300r/min, forward rotation and reverse rotation are alternately carried out during stirring, the times of forward rotation and reverse rotation are 2-3 times, and the interval of alternate rotation is 1-2 minutes.
7. The method for preparing the composite activated cement reinforced grinding aid containing the polycarboxylic acid series according to claim 5, wherein the stirrer is a precise timing magnetic stirrer, and the water bath kettle is a two-hole intelligent water bath kettle.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1550474A (en) * | 2003-04-10 | 2004-12-01 | 株式会社日本触媒 | Polycarboxylic acid cement dispersant and method for producing concrete secondary product |
| CN101798198A (en) * | 2010-04-03 | 2010-08-11 | 山东宏艺科技股份有限公司 | Polycarboxylic acid cement activation reinforced grinding aid and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1550474A (en) * | 2003-04-10 | 2004-12-01 | 株式会社日本触媒 | Polycarboxylic acid cement dispersant and method for producing concrete secondary product |
| CN101798198A (en) * | 2010-04-03 | 2010-08-11 | 山东宏艺科技股份有限公司 | Polycarboxylic acid cement activation reinforced grinding aid and preparation method thereof |
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Application publication date: 20210416 |