CN111439947A - Low-air-entraining slow-setting type polycarboxylate superplasticizer and preparation method thereof - Google Patents
Low-air-entraining slow-setting type polycarboxylate superplasticizer and preparation method thereof Download PDFInfo
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- CN111439947A CN111439947A CN202010223736.0A CN202010223736A CN111439947A CN 111439947 A CN111439947 A CN 111439947A CN 202010223736 A CN202010223736 A CN 202010223736A CN 111439947 A CN111439947 A CN 111439947A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
Abstract
The invention discloses a low-air-entraining retarding polycarboxylic acid water reducing agent which comprises the following components in parts by mass: 0.5-1.2 parts of macromonomer, 0.1-0.3 part of acrylic acid, 0.05-0.2 part of sodium methallyl sulfonate, 0.01-0.035 part of 2-hydroxyethyl methacrylate phosphate, 0.002-0.005 part of silane modified graphene, 0.00015-0.0002 part of ammonium persulfate, 0.0001-0.0002 part of neutralizer and 3-6 parts of water. Due to the addition of the silane modified graphene, the combination effect of the components is better in the reaction process, and the gaps among the molecules after the reaction are smaller, so that the gas content is lower.
Description
Technical Field
The invention relates to the technical field of concrete admixtures, in particular to a low-air-entraining retarding polycarboxylic acid water reducer and a preparation method thereof.
Background
In engineering application, a polycarboxylate water reducer can generate excessive air entraining amount, so that the phenomena of excessive air content in concrete and reduction of concrete hardening strength are caused, the conventional method is to compound the polycarboxylate water reducer with a defoaming agent to reduce the air content in the concrete and improve the influence of the polycarboxylate water reducer on the concrete hardening strength, but the effect is not ideal, meanwhile, the polycarboxylate water reducer has weak retarding effect, a retarder and the polycarboxylate water reducer are usually compounded in engineering, although the retarding effect can be achieved, the setting time is often too short or too long due to the influence of certain reasons, and the concrete is greatly influenced.
Chinese invention patent CN108192040A discloses a preparation method of a low-air-entraining type solid polycarboxylic acid water reducing agent, which adopts an amidation method to introduce a benzene ring and an amide group with a rigid structure and a polyether amine structure of ethylene oxide/propylene oxide with a defoaming structure, so that the finally synthesized water reducing agent has good water reducing, slump retaining and low-air-entraining effects, and the durability of concrete is effectively enhanced; the microwave heating method is adopted, the heating speed is high, the operation is simple, the automatic control precision is high, and the cleaning and pollution-free effects are realized. Chinese patent CN 105111387A discloses a preparation method of a low-air-entraining type solid polycarboxylic acid water reducing agent. The method can adjust the surface tension of the water reducing agent by adjusting the composition of polyether monomers in the polycarboxylic water reducing agent and introducing other hydrophobic groups, so that the water reducing agent molecules have a foam eliminating and controlling effect, and the problem of high gas content in concrete is solved. However, the preparation methods of the two water reducing agents have long preparation time and very complicated process.
Chinese patent CN106883355A discloses a low-air-entraining viscosity-reducing type polycarboxylate superplasticizer, which is prepared by polymerizing an alkyl phosphotriester mixture, prenol polyoxyethylene ether and unsaturated carboxylic acid through free radicals under the action of an initiator and a chain transfer agent. According to the method, alkyl phosphate triester monomers containing two double bonds are introduced to the main chain, so that the obtained polycarboxylate water reducer molecules are in a heterocyclic multi-branched structure, the thickness of an adsorption layer of the polycarboxylate water reducer is increased, the plastic viscosity of concrete can be remarkably reduced, and meanwhile, the defoaming performance of the obtained polycarboxylate water reducer can be effectively improved and the air entrainment performance of the polycarboxylate water reducer can be reduced by introducing the phosphate triester structure into the molecular structure of the polycarboxylate water reducer. However, the gas content of the polycarboxylic acid water reducing agent prepared by the method still reaches about 1% when the polycarboxylic acid water reducing agent is applied, so that the process is required to be improved, and the water reducing agent with lower gas content is prepared.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides the low-air-entraining slow-setting polycarboxylate superplasticizer which has the advantages of better dispersibility, good plasticity retention, high water reducing rate, effective reduction of gas introduction, better slow setting effect and capability of effectively solving the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
the low-air-entraining retarding polycarboxylate superplasticizer comprises the following components in parts by weight: 0.5-1.2 parts of macromonomer, 0.1-0.3 part of acrylic acid, 0.05-0.2 part of sodium methallyl sulfonate, 0.01-0.035 part of 2-hydroxyethyl methacrylate phosphate, 0.002-0.005 part of silane modified graphene, 0.00015-0.0002 part of ammonium persulfate, 0.0001-0.0002 part of neutralizer and 3-6 parts of water.
Preferably, the raw materials in the formula comprise the following components in parts by mass: 1 part of macromonomer, 0.235 part of acrylic acid, 0.1 part of sodium methallyl sulfonate, 0.027 part of 2-hydroxyethyl methacrylate phosphate, 0.0035 part of silane modified graphene, 0.0002 part of ammonium persulfate, 0.00015 part of neutralizer and 5 parts of water.
Preferably, the macromonomer consists of isopentenyl, polyoxyethylene and polyoxypropylene ethers.
The preparation method of the low-air-entraining retarding polycarboxylate superplasticizer comprises the following steps:
step 1: extracting the raw materials according to the proportion, dissolving a macromonomer in water to obtain an aqueous solution A, dissolving acrylic acid, sodium methallyl sulfonate, 2-hydroxyethyl methacrylate phosphate and silane modified graphene in water to obtain an aqueous solution B, and dissolving ammonium persulfate in water to obtain an aqueous solution C;
step 2: sequentially adding the aqueous solution A, the aqueous solution B and the aqueous solution C into a container, heating to 75-85 ℃, and then continuously stirring for 6-7 hours;
and step 3: and after stirring, cooling to 30-40 ℃, adding a neutralizing agent to adjust the pH of the solution to 5, and thus obtaining the low-air-entraining slow-setting polycarboxylic acid water reducer.
Preferably, the temperature rise in the step 2 is 80 ℃, and the stirring time is 6 h.
Preferably, the neutralizing agent is a sodium hydroxide solution with a mass concentration of 25%.
Preferably, the preparation method of the silane-modified graphene comprises the following steps: pre-dispersing 40-70 parts of redox graphene powder and 5-8 parts of sodium dodecyl benzene sulfonate in 500 parts of ethanol; then adding 1-3 parts of silane coupling agent, 2-3 parts of active calcium phosphate and 0.1-0.3 part of polyethylene glycol 1000 to modify and disperse graphene, and shearing and stirring at a high speed of 6000-7500 r/min for 1.5-2.5 h; and filtering and drying after modification to obtain the silane modified graphene.
Preferably, the mass ratio of the redox graphene powder to the silane coupling agent is (20-40): 1.
compared with the prior art, the invention has the beneficial effects that: the low-air-entraining retarding polycarboxylate water reducer adopts a macromonomer consisting of isopentenyl, polyoxyethylene and polyoxypropylene ether, can effectively change the hydrophilicity of polycarboxylic acid, change the surface tension of the polycarboxylic acid and reduce the bubble formation rate, simultaneously selects acrylic acid and sodium methallyl sulfonate as unsaturated carboxylic acid, takes ammonium persulfate as an initiator, polymerizes the acrylic acid and the sodium methallyl sulfonate under the action of the ammonium persulfate, and adds 2-hydroxyethyl methacrylate phosphate to ensure that a polymer has a characteristic active group side chain, thereby having excellent retarding effect; in order to further reduce the gas content, the silane modified graphene is added, and compared with the traditional polycarboxylic acid water reducing agent, the silane modified graphene is added, so that the combination effect of all the components is better in the reaction process, and the gaps among all the molecules after the reaction are smaller, so that the gas content is lower.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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 raw materials of the following mass components are selected: 1.2 parts of macromonomer, 0.1 part of acrylic acid, 0.2 part of sodium methallyl sulfonate, 0.01 part of 2-hydroxyethyl methacrylate phosphate, 0.005 part of silane modified graphene, 0.00015 part of ammonium persulfate, 0.0002 part of neutralizer, 3 parts of water, and isopentenyl in the macromonomer: polyoxyethylene: the ratio of polyoxypropylene ether is 1:1.5: 3.
The preparation process comprises the following steps:
step 1: dissolving the weighed macromonomer in 1 part of water to obtain an aqueous solution A, dissolving acrylic acid, sodium methallyl sulfonate, 2-hydroxyethyl methacrylate phosphate and silane modified graphene in 2 parts of water to obtain an aqueous solution B, and dissolving ammonium persulfate in 1 part of water to obtain an aqueous solution C;
step 2: sequentially adding the aqueous solution A, the aqueous solution B and the aqueous solution C into a container with heating and stirring functions, heating to 75 ℃, and then continuously stirring for 6.5 hours;
and step 3: and after stirring, cooling to 30 ℃, adding a sodium hydroxide solution with the mass concentration of 25% to adjust the pH of the solution to 5, and obtaining the polycarboxylic acid water reducing agent.
The preparation method of the silane modified graphene comprises the following steps: pre-dispersing 70 parts of redox graphene powder and 5 parts of sodium dodecyl benzene sulfonate in 500 parts of ethanol; then adding 3 parts of silane coupling agent KH560, 2 parts of active calcium phosphate and 0.3 part of polyethylene glycol 1000 to modify and disperse the graphene, and shearing and stirring at a high speed of 6000r/min for 2.5 h; and filtering and drying after modification to obtain the silane modified graphene.
The mass ratio of the redox graphene powder to the silane coupling agent is 20: 1.
example 2
The raw materials of the following mass components are selected: 1 part of macromonomer, 0.235 part of acrylic acid, 0.1 part of sodium methallyl sulfonate, 0.027 part of 2-hydroxyethyl methacrylate phosphate, 0.0035 parts of silane modified graphene, 0.0002 part of ammonium persulfate, 0.00015 part of neutralizer, 5 parts of water, and isopentenyl in the macromonomer: polyoxyethylene: the ratio of polyoxypropylene ether is 1:1.5: 3.
The preparation process comprises the following steps:
step 1: dissolving the weighed macromonomer in 1.5 parts of water to obtain an aqueous solution A, dissolving acrylic acid, sodium methallyl sulfonate, 2-hydroxyethyl methacrylate phosphate and silane modified graphene in 1 part of water to obtain an aqueous solution B, and dissolving ammonium persulfate in 2.5 parts of water to obtain an aqueous solution C;
step 2: sequentially adding the aqueous solution A, the aqueous solution B and the aqueous solution C into a container with heating and stirring functions, heating to 80 ℃, and then continuously stirring for 6 hours;
and step 3: and after stirring, cooling to 35 ℃, adding a sodium hydroxide solution with the mass concentration of 25% to adjust the pH to 5, and thus obtaining the polycarboxylic acid water reducing agent.
The preparation method of the silane modified graphene comprises the following steps: pre-dispersing 55 parts of redox graphene powder and 7 parts of sodium dodecyl benzene sulfonate in 500 parts of ethanol; then adding 1.5 parts of silane coupling agent KH560, 2.5 parts of active calcium phosphate and 0.25 part of polyethylene glycol 1000 to modify and disperse graphene, and shearing and stirring at a high speed of 6500r/min for 2 hours; and filtering and drying after modification to obtain the silane modified graphene.
The mass ratio of the redox graphene powder to the silane coupling agent is 35: 1.
example 3
The low-air-entraining retarding polycarboxylate superplasticizer comprises the following components in parts by weight: 0.5 part of macromonomer, 0.3 part of acrylic acid, 0.05 part of sodium methallyl sulfonate, 0.035 part of 2-hydroxyethyl methacrylate phosphate, 0.002 part of silane modified graphene, 0.0002 part of ammonium persulfate, 0.0002 part of neutralizer and 6 parts of water.
Isopentenyl in the macromonomer: polyoxyethylene: the ratio of polyoxypropylene ether is 1:1.8: 2.5.
The preparation method of the low-air-entraining retarding polycarboxylate superplasticizer comprises the following steps:
step 1: extracting the raw materials according to the proportion, dissolving a macromonomer in water to obtain an aqueous solution A, dissolving acrylic acid, sodium methallyl sulfonate, 2-hydroxyethyl methacrylate phosphate and silane modified graphene in water to obtain an aqueous solution B, and dissolving ammonium persulfate in water to obtain an aqueous solution C;
step 2: sequentially adding the aqueous solution A, the aqueous solution B and the aqueous solution C into a container, heating to 85 ℃, and then continuously stirring for 7 hours;
and step 3: and after stirring, cooling to 40 ℃, adding a neutralizer to adjust the pH of the solution to 5, and thus obtaining the low-air-entraining slow-setting polycarboxylic acid water reducer.
The preparation method of the silane modified graphene comprises the following steps: pre-dispersing 40 parts of redox graphene powder and 8 parts of sodium dodecyl benzene sulfonate in 500 parts of ethanol; then adding 1 part of silane coupling agent KH560, 3 parts of active calcium phosphate and 0.1 part of polyethylene glycol 1000 to modify and disperse graphene, and shearing and stirring at a high speed of 7500r/min for 1.5 h; and filtering and drying after modification to obtain the silane modified graphene.
The mass ratio of the redox graphene powder to the silane coupling agent is 40: 1.
comparative example 1
The silane modified graphene in example 2 was removed, and the rest of the formulation and preparation method were unchanged.
Comparative example 2
The silane-modified graphene in example 2 was replaced with conventional graphene, and the rest of the formulation and preparation method were unchanged.
Application example
The polycarboxylate superplasticizers prepared in examples 1-3 and comparative examples 1-2 of the invention are applied to the preparation of concrete, the polycarboxylate superplasticizer prepared in example 1 of the Chinese invention patent CN106883355A is adopted in comparative example 3, and the prepared concrete is respectively subjected to mechanical property and working property tests, wherein the test method refers to GB/T50080-2002 Standard for testing the performance of common concrete mixture and GB/T50081-2002 Standard for testing the mechanical property of common concrete. The concrete collapse method is adopted to measure the concrete viscosity: inverting the slump bucket, filling the slump bucket with concrete and leveling, quickly lifting the slump bucket about 40cm, measuring the concrete flowing time by using a stopwatch, calculating the mixing amount according to the polycarboxylic acid water reducing agent with the solid content of 40%, and obtaining the test result shown in table 1.
The concrete is composed of a cementing material, Yueyang river sand, a coarse aggregate and water, wherein the content of the cementing material is 590kg/m3 (comprising cement and fly ash, the cement consumption is 480kg/m3, the fly ash is 110kg/m3, the cement is Huang Shi Huaxin P. O42.5R, the fly ash is I-grade ash), the content of the river sand is 700kg/m3 (the fineness modulus is 2.8), the content of the coarse aggregate is 990kg/m3 (5-20 continuous graded basalt), and the water-to-glue ratio is 0.24.
Table 1: the working performance test result of the concrete obtained in the application example;
according to the test data, the gas content of the carboxylic acid water reducing agent is remarkably reduced due to the addition of the silane modified graphene.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The low-air-entraining retarding polycarboxylate superplasticizer is characterized by comprising the following components in parts by mass: 0.5-1.2 parts of macromonomer, 0.1-0.3 part of acrylic acid, 0.05-0.2 part of sodium methallyl sulfonate, 0.01-0.035 part of 2-hydroxyethyl methacrylate phosphate, 0.002-0.005 part of silane modified graphene, 0.00015-0.0002 part of ammonium persulfate, 0.0001-0.0002 part of neutralizer and 3-6 parts of water.
2. The low-air-entraining retarding polycarboxylate superplasticizer according to claim 1, wherein the raw materials in the formula comprise the following components in parts by mass: 1 part of macromonomer, 0.235 part of acrylic acid, 0.1 part of sodium methallyl sulfonate, 0.027 part of 2-hydroxyethyl methacrylate phosphate, 0.0035 part of silane modified graphene, 0.0002 part of ammonium persulfate, 0.00015 part of neutralizer and 5 parts of water.
3. The low-bleed air retarding polycarboxylate water reducer according to claim 1 or 2, characterized in that said macromonomer consists of isopentenyl, polyoxyethylene and polyoxypropylene ether.
4. The preparation method of the low-air-entraining retarding polycarboxylate superplasticizer according to claim 1, characterized by comprising the following steps:
step 1: extracting the raw materials according to the proportion, dissolving a macromonomer in water to obtain an aqueous solution A, dissolving acrylic acid, sodium methallyl sulfonate, 2-hydroxyethyl methacrylate phosphate and silane modified graphene in water to obtain an aqueous solution B, and dissolving ammonium persulfate in water to obtain an aqueous solution C;
step 2: sequentially adding the aqueous solution A, the aqueous solution B and the aqueous solution C into a container, heating to 75-85 ℃, and then continuously stirring for 6-7 hours;
and step 3: and after stirring, cooling to 30-40 ℃, adding a neutralizer to adjust the pH of the solution to 5, and obtaining the low-air-entraining slow-setting polycarboxylic acid water reducer.
5. The preparation method of the low-air-entraining retarding polycarboxylate superplasticizer according to claim 4, wherein the temperature rise in the step 2 is 80 ℃ and the stirring time is 6 hours.
6. The preparation method of the low-air-entraining retarding polycarboxylate superplasticizer according to claim 4, characterized in that the neutralizing agent is a sodium hydroxide solution with a mass concentration of 25%.
7. The preparation method of the low-air-entraining retarding polycarboxylate superplasticizer according to claim 4, wherein the preparation method of the silane-modified graphene comprises the following steps: pre-dispersing 40-70 parts of redox graphene powder and 5-8 parts of sodium dodecyl benzene sulfonate in 500 parts of ethanol; then adding 1-3 parts of silane coupling agent, 2-3 parts of active calcium phosphate and 0.1-0.3 part of polyethylene glycol 1000 to modify and disperse graphene, and shearing and stirring at a high speed of 6000-7500 r/min for 1.5-2.5 h; and filtering and drying after modification to obtain the silane modified graphene.
8. The preparation method of the low-air-entraining retarding polycarboxylic acid water reducer according to claim 7, characterized in that the mass ratio of the redox graphene powder to the silane coupling agent is (20-40): 1.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112028574A (en) * | 2020-09-14 | 2020-12-04 | 江西龙正科技发展有限公司 | Concrete material suitable for manufacturing bridge prestressed pipe pile |
| CN112707673A (en) * | 2020-09-15 | 2021-04-27 | 科之杰新材料集团有限公司 | Super-shrinkage type polycarboxylate superplasticizer and preparation method thereof |
| CN113184841A (en) * | 2021-05-19 | 2021-07-30 | 深圳港创建材股份有限公司 | Method for enhancing dispersibility of low-oxygen-content graphene |
| CN114315380A (en) * | 2022-01-11 | 2022-04-12 | 贵州万为金科特种建材有限公司 | Green environment-friendly chromium-removing ceramic water reducing agent |
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