CN114380957A - High-performance ultra-slow release slump retaining agent and preparation method thereof - Google Patents
High-performance ultra-slow release slump retaining agent and preparation method thereof Download PDFInfo
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- CN114380957A CN114380957A CN202210073402.9A CN202210073402A CN114380957A CN 114380957 A CN114380957 A CN 114380957A CN 202210073402 A CN202210073402 A CN 202210073402A CN 114380957 A CN114380957 A CN 114380957A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 107
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 86
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 84
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 33
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 18
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 12
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 11
- 239000007800 oxidant agent Substances 0.000 claims abstract description 11
- 230000001590 oxidative effect Effects 0.000 claims abstract description 8
- 239000003999 initiator Substances 0.000 claims abstract description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 20
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical group OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 16
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 14
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 14
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 13
- -1 hydroxyl ester Chemical class 0.000 claims description 13
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000178 monomer Substances 0.000 claims description 12
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 10
- 229930003268 Vitamin C Natural products 0.000 claims description 10
- 235000019154 vitamin C Nutrition 0.000 claims description 10
- 239000011718 vitamin C Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 4
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 2
- 238000007865 diluting Methods 0.000 claims description 2
- 239000004567 concrete Substances 0.000 abstract description 37
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 7
- 239000004568 cement Substances 0.000 description 28
- 239000002245 particle Substances 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 8
- 238000003786 synthesis reaction Methods 0.000 description 8
- 239000011790 ferrous sulphate Substances 0.000 description 5
- 235000003891 ferrous sulphate Nutrition 0.000 description 5
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 5
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000006185 dispersion Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 235000010755 mineral Nutrition 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000004185 ester group Chemical group 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000000701 coagulant Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011372 high-strength concrete Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- 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
- C04B24/2605—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
-
- 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
- C08F4/00—Polymerisation catalysts
- C08F4/40—Redox systems
-
- 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
- C04B2103/308—Slump-loss preventing agents
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention discloses a high-performance ultra-slow release slump retaining agent and a preparation method thereof, belonging to the technical field of concrete admixtures, and the technical scheme is that the slump retaining agent comprises, by weight, 34-36 parts of methyl allyl polyoxyethylene ether, 20-24 parts of water, 15-20 parts of a material A, 15-15.5 parts of a material B, 0.5-0.9 part of a material C and 0.48-0.52 part of a material D, wherein: the material A comprises acrylic acid and water, and the weight ratio of the acrylic acid to the water is (1-3) to 10; the material B comprises a chain transfer agent, a reducing agent and water, and the weight ratio of the chain transfer agent to the reducing agent to the water is (0.05-0.1): (0.12-0.17): 15; the component C comprises an oxidant and water, and the weight ratio of the oxidant to the water is (0.2-0.3) to 0.5; the D material comprises an initiator and water, and the weight ratio of the initiator to the water is (0.003-0.006):0.5, so that the effect of improving the production efficiency of the slump retaining agent is achieved.
Description
Technical Field
The invention relates to the field of slump retaining agents, in particular to a high-performance super slow-release slump retaining agent and a preparation method thereof
Background
The slump retaining agent is widely applied to concrete due to the characteristics of low mixing amount, high water reducing rate, good dispersing performance, small slump, environmental friendliness and the like, and along with the mature use of the slump retaining agent, the slump retaining agent is more and more required in engineering.
The slump retaining agent is characterized in that concrete mixtures are doped with superfine mineral admixtures besides cement, and the superfine mineral admixtures have a large amount of adsorption effect on the slump retaining agent, so that the concentration of the slump retaining agent in a solution is reduced, the slump loss of concrete is large when the slump retaining agent is transported at a high temperature for a long distance, and in order to reduce the slump loss, the mode commonly adopted at present is as follows: adding water for remodeling, adding slump retaining agent for many times, compounding retarder components and the like, but the method not only increases the production cost, but also has certain side effect on the strength of the concrete. Therefore, the slump retaining agent is produced at the same time, called slump retaining agent for short, the existing slump retaining agent synthesis technology is relatively mature, but in the synthesis process, the reaction temperature is as high as 80 ℃, so that the slump retaining agent is low in production efficiency and low in energy consumption in industrial production.
Disclosure of Invention
In order to improve the production efficiency of the slump retaining agent, the invention provides a high-performance super slow-release slump retaining agent and a preparation method thereof.
In a first aspect, the invention provides a high-performance ultra-slow release slump retaining agent, which adopts the following technical scheme:
a high-performance ultra-slow release slump retaining agent comprises, by weight, 34-36 parts of methyl allyl polyoxyethylene ether, 20-24 parts of water, 15-20 parts of a material A, 15-15.5 parts of a material B, 0.5-0.9 part of a material C and 0.48-0.52 part of a material D, wherein:
the material A comprises acrylic acid and water, and the weight ratio of the acrylic acid to the water is (1-3) to 10;
the material B comprises a chain transfer agent, a reducing agent and water, and the weight ratio of the chain transfer agent to the reducing agent to the water is (0.14-0.2): (0.04-0.08): 15;
the component C comprises an oxidant and water, and the weight ratio of the oxidant to the water is (0.2-0.3) to 0.5;
the D material comprises initiator and water, and the weight ratio of the initiator to the water is (0.003-0.006): 0.5.
By adopting the technical scheme, in the application, the chain transfer agent, the reducing agent and the oxidizing agent are matched with the methyl allyl polyoxyethylene ether and the acrylic acid, so that the reaction temperature is effectively reduced and kept at about 40 ℃, the synthesis cost of the slump retaining agent is effectively reduced, and the production efficiency of the slump retaining agent is effectively improved.
In addition, the application adopts the matching use of the methyl allyl polyoxyethylene ether, the acrylic acid, the chain transfer agent, the reducing agent and the oxidizing agent, cement particles can be wrapped to form a steric hindrance effect, the dispersing performance of the slump retaining agent is improved, and carboxyl in the acrylic acid enables slump retaining agent molecules to be preferentially adsorbed on the cement particles, so that the slump retaining agent molecules have relatively good dispersing performance, but the slump retaining agent molecules are beneficial to improving the dispersibility of cement paste when the using amount of the acrylic acid is large, but have adverse effects on the maintenance of the dispersibility, so that when the content of the acrylic acid, the methyl allyl polyoxyethylene ether, the chain transfer agent, the reducing agent and the oxidizing agent is limited within the range of the application, the formed slump retaining agent has better freedom degree in free water, can promote the quick adsorption and dispersion of the slump retaining agent in the cement paste, and meanwhile, the thickness of a water film layer formed by polycarboxylic acid molecules in the cement paste is lower, therefore, more free water can be released, the viscosity of the concrete is reduced, and the slump retaining performance of the slump retaining agent is effectively ensured.
Therefore, the slump retaining agent obtained by the application not only improves the production efficiency, but also can reduce the slump loss rate of concrete and improve the use value of the slump retaining agent.
Preferably, the material A also comprises a hydroxyl ester monomer, wherein the weight ratio of acrylic acid to the hydroxyl ester monomer to water is (1-3) to (4-6) to 10.
Preferably, the weight ratio of acrylic acid, the hydroxyl ester monomer and water in the material A is (1.5-2): (4.5-6): 10.
By adopting the technical scheme, the slump retaining agent is provided with long-time slump retaining performance by adding the ester group to the main chain of the slump retaining agent and utilizing the characteristic that the ester group is slowly hydrolyzed under an alkaline environment to release carboxyl, and in addition, as the hydroxyl ester monomer contains the methyl group with the hydrophobic function and utilizes the hydrophobicity of the methyl group, the surface tension of slump retaining agent molecules is improved, and further more free water is released in cement slurry, so that the aim of reducing viscosity is fulfilled.
In addition, the application discovers that the slump retaining performance of the cement paste can be effectively improved when acrylic acid and the hydroxyl ester monomer are limited in the range of the application because the slump retaining performance of the cement paste can be effectively improved as the fluidity of the cement paste doped with the slump retaining agent is increased and then reduced due to the fact that the density of a side chain of the slump retaining agent is relatively reduced as the dosage of the hydroxyl ester monomer is increased, the absorption effect of the slump retaining agent on the surface of cement is reduced, and the dispersibility and the dispersion retentivity of the slump retaining agent are reduced.
Preferably, the hydroxy ester monomer is hydroxyethyl acrylate or hydroxypropyl acrylate.
Preferably, the reducing agent in the material B adopts vitamin C.
Preferably, the chain transfer agent in the material B comprises mercaptopropionic acid and sodium hypophosphite, and the weight ratio of the mercaptopropionic acid to the sodium hypophosphite is (0.9-1.2): 1.
By adopting the technical scheme, when the mercaptopropionic acid, the sodium hypophosphite and the vitamin C are matched for use, the initial reaction temperature of the slump retaining agent can be effectively ensured, the synthesis time of the slump retaining agent is shortened, and the production efficiency of the slump retaining agent is improved. In addition, vitamin C contains a large number of strong polar functional groups of carboxyl and hydroxyl, the groups provide dispersing and flowing properties for cement particles through surface active effects of adsorption, dispersion, wetting and the like, and the workability of cement slurry is improved by reducing the frictional resistance among the cement particles and reducing the free energy of the interface between the cement particles and water. Meanwhile, polycarboxylic acid molecules are adsorbed on the surfaces of cement particles, and carboxylate ions enable the cement particles to carry negative charges, so that electrostatic repulsion is generated among the cement particles, the cement particles are dispersed, the coagulation tendency of cement paste is inhibited, the contact area of the cement particles and water is increased, the cement is fully hydrated, free water surrounded by coagulants is discharged in the process of diffusing the cement particles, the workability is improved, and the water mixing amount is reduced.
Preferably, 27.5 wt% of hydrogen peroxide is used as the oxidant.
In a second aspect, the application provides a preparation method of a high-performance ultra-slow release slump retaining agent, which comprises the following steps: dissolving methyl allyl polyoxyethylene ether in water, heating to 25-35 ℃, adding the material C and the material D, stirring for 10-20min, starting to dropwise add the material A and the material B, keeping the temperature between 35-45 ℃ after dropwise adding, preserving heat for 1-1.5h, and adding water for diluting to obtain the slump retaining agent with the solid content of 40%.
By adopting the technical scheme, the methyl allyl polyoxyethylene ether is dissolved in the aqueous solution, so that the subsequent reaction is more sufficient, in addition, the process is simple and convenient to operate, the reaction temperature is about 40 ℃, the safety is good, the reaction time is within 4 hours, and compared with the existing synthesis time of 7-9h and the synthesis temperature of 80 ℃, the production process reduces the synthesis cost of the slump retaining agent by about 20 percent, and effectively improves the production efficiency.
In conclusion, the invention has the following beneficial effects: according to the invention, the acrylic acid, the hydroxyl ester monomer, the sodium hypophosphite and the vitamin C are mutually matched, so that the synthesis time of the slump retaining agent is shortened, the reaction temperature is controlled within 40 ℃, the production efficiency of the slump retaining agent is effectively improved, the production cost is reduced, and meanwhile, the slump retaining agent obtained by the application can also effectively reduce the free energy of a cement particle and water interface to improve the workability of cement paste and reduce the slump loss rate of concrete.
Detailed Description
The present invention will be described in further detail with reference to examples.
The raw materials used in the application are all commercially available.
Example 1
A preparation method of a high-performance ultra-slow release slump retaining agent comprises the following steps:
(1) adding 34kg of methyl allyl polyoxyethylene ether and 20kg of water into a reaction kettle, stirring for dissolving, and heating to 25 ℃;
(2) adding 0.75kg of material C and 0.51kg of material D into the reaction kettle, and stirring for 10 min;
(3) 17kg of the material A and 15.2kg of the material B are added dropwise, wherein the adding time of the material A is 1 hour, and the adding time of the material B is 1.5 hours;
(4) after the dropwise adding, keeping the temperature at 35 ℃, preserving the heat for 1h, and adding water to dilute to obtain the slump retaining agent with the solid content of 40%;
wherein the material A comprises acrylic acid and water, and the weight ratio of the acrylic acid to the water is 1: 10;
the B material comprises a chain transfer agent, vitamin C and water, and the weight ratio of the chain transfer agent to the vitamin C to the water is 0.14:0.04: 15; the chain transfer agent comprises mercaptopropionic acid and sodium hypophosphite, wherein the weight ratio of the mercaptopropionic acid to the sodium hypophosphite is 1: 1;
the material C comprises hydrogen peroxide and water, and the weight ratio of the hydrogen peroxide to the water is 0.2: 0.5;
the material D comprises ferrous sulfate and water, the weight ratio of the ferrous sulfate to the water is 0.003:0.5, and the content of each component in the material A, the material B, the material C and the material D is shown in Table 1.
Example 2
A preparation method of a high-performance ultra-slow release slump retaining agent is different from that of the embodiment 1 in that:
the weight ratio of acrylic acid to water in feed A was 2:10, the remainder being the same as in example 1, with specific reference to Table 1.
Example 3
A preparation method of a high-performance ultra-slow release slump retaining agent is different from that of the embodiment 1 in that:
the weight ratio of acrylic acid to water in feed A was 3:10, the remainder being the same as in example 1, with specific reference to Table 1.
Example 4
A preparation method of a high-performance ultra-slow release slump retaining agent is different from that of the embodiment 2 in that:
the weight ratio of chain transfer agent, vitamin C and water in feed B was 0.17:0.06:15, and the rest was the same as in example 2, with specific reference to Table 1.
Example 5
A preparation method of a high-performance ultra-slow release slump retaining agent is different from that of the embodiment 2 in that:
the weight ratio of the mercaptopropionic acid, the sodium hypophosphite and the water in the material B is 0.2:0.0.08:15, and the rest is the same as that in the example 2, and the specific reference is shown in the table 1.
Example 6
A preparation method of a high-performance ultra-slow release slump retaining agent is different from that of the embodiment 4 in that:
the weight ratio of hydrogen peroxide to water in charge C was 0.25:0.5, the remainder being the same as in example 4, with specific reference to Table 1.
Example 7
A preparation method of a high-performance ultra-slow release slump retaining agent is different from that of the embodiment 4 in that:
the weight ratio of hydrogen peroxide to water in charge C was 0.3:0.5, the remainder being the same as in example 4, with specific reference to Table 1.
Example 8
A preparation method of a high-performance ultra-slow release slump retaining agent is different from that of the slump retaining agent in the embodiment 6 in that:
the weight ratio of ferrous sulfate to water in feed D was 0.006:0.5, the remainder being the same as in example 6, with specific reference to Table 1.
Table 1 compositions and amounts of materials a, B, C and D of examples 1-8, units: kg of
Example 9
A preparation method of a high-performance ultra-slow release slump retaining agent is different from that of the slump retaining agent in the embodiment 8 in that: the total amount of the material A was 15kg, the total amount of the material B was 15kg, the total amount of the material C was 5kg, the total amount of the material D was 4.8kg, the rest was the same as in example 8, the preparation method and the proportions of the components in the material A, the component in the material B, the component in the material C, and the component in the material D were the same as in all example 8, and the specific contents of the components are shown in Table 2.
Example 10
A preparation method of a high-performance ultra-slow release slump retaining agent is different from that of the slump retaining agent in the embodiment 8 in that: the total amount of the material A was 20kg, the total amount of the material B was 15.5kg, the total amount of the material C was 9kg, and the total amount of the material D was 5.2kg, the rest was the same as in example 8, the preparation methods and the proportions of the components in the material A, the component in the material B, the component in the material C, and the component in the material D were the same as in all example 8, and the specific contents of the components are shown in Table 2.
Table 2 compositions and amounts of materials a, B, C and D of examples 9-10, units: kg of
Example 11
The difference between the preparation method and the example 8 is that the material A comprises acrylic acid, hydroxyethyl acrylate and water, wherein the ratio of acrylic acid: hydroxyethyl acrylate: the weight ratio of water was 1:4:10, the rest was the same as in example 8, and the specific contents are shown in Table 3.
Example 12
The difference between the preparation method and the example 8 is that the material A comprises acrylic acid, hydroxyethyl acrylate and water, wherein the ratio of acrylic acid: hydroxyethyl acrylate: the weight ratio of water was 1.5:4.5:10, the rest being the same as in example 8, and the specific contents are shown in Table 3.
Example 13
The difference between the preparation method and the example 8 is that the material A comprises acrylic acid, hydroxyethyl acrylate and water, wherein the ratio of acrylic acid: hydroxyethyl acrylate: the weight ratio of water was 2:5:10, the rest was the same as in example 8, and the specific contents are shown in Table 3.
Example 14
The difference between the preparation method and the example 8 is that the material A comprises acrylic acid, hydroxyethyl acrylate and water, wherein the ratio of acrylic acid: hydroxyethyl acrylate: the weight ratio of water was 3:6:10, the rest was the same as in example 8, and the specific contents are shown in Table 3.
Table 3 contents of the components in the examples 8, 11-14A, in units: kg of
Example 15
A preparation method of a high-performance ultra-slow release slump retaining agent is different from that of the slump retaining agent in the embodiment 8 in that the weight ratio of the mercaptopropionic acid to the sodium hypophosphite in the material B is 0.9:1, namely 0.08kg of the mercaptopropionic acid and 0.09kg of the sodium hypophosphite, and the rest is the same as that in the embodiment 8.
Example 16
A preparation method of a high-performance ultra-slow release slump retaining agent is different from that of the slump retaining agent in the embodiment 8 in that the weight ratio of the mercaptopropionic acid to the sodium hypophosphite in the material B is 1.2:1, namely 0.09kg of the mercaptopropionic acid and 0.08kg of the sodium hypophosphite, and the rest is the same as that in the embodiment 8.
Example 17
A preparation method of a high-performance ultra-slow release slump retaining agent is different from that of the embodiment 8 in the following specific points of methyl allyl polyoxyethylene ether, reaction temperature and reaction time:
(1) adding 36kg of methyl allyl polyoxyethylene ether and 24kg of water into a reaction kettle, stirring for dissolving, and heating to 35 ℃;
(2) adding 0.75kg of material C and 0.51kg of material D into the reaction kettle, and stirring for 20 min;
(3) 17kg of the material A and 15.2kg of the material B are added dropwise, wherein the adding time of the material A is 1.5 hours, and the adding time of the material B is 2.0 hours;
(4) after the dropwise addition, the temperature is kept at 45 ℃, and after heat preservation is carried out for 1.5 hours, water is added for dilution to obtain the slump retaining agent with the solid content of 40%.
Comparative example 1
The difference from example 8 was that 14kg of the material A, 14kg of the material B, 0.4kg of the material C and 0.4kg of the material D were used, and the amounts of the specific components of the materials A, B, C and D were as shown in Table 4, except that the amounts of the materials A, B, C and D were the same as in example 8.
Comparative example 2
The difference from example 8 was that 25kg of the material A, 17kg of the material B, 1.0kg of the material C and 0.6kg of the material D were used, and the amounts of the specific components of the materials A, B, C and D were as shown in Table 4, except that the contents were the same as those in example 8.
Comparative example 3
The difference from example 8 is that the weight ratio of acrylic acid to water in feed a is 4: 10; the weight ratio of the chain transfer agent to the vitamin C to the water in the material B is 0.13:0.02: 15; the weight ratio of hydrogen peroxide to water in the material C is 0.4: 0.5; the weight ratio of ferrous sulfate to water in feed D was 0.007:0.5, all other things being equal to example 8.
Comparative example 4
The difference from example 8 is that the weight ratio of acrylic acid to water in feed a is 0.8: 10; the weight ratio of the chain transfer agent to the vitamin C to the water in the material B is 0.22:0.1: 15; the weight ratio of hydrogen peroxide to water in the material C is 0.1: 0.5; the weight ratio of ferrous sulfate to water in feed D was 0.001:0.5, the rest being the same as in example 8.
Comparative example 5
The slump retaining agent is sold in the market, the pH value is 6.0-8.0, the solid content is 40.0 +/-1.0, and the water reducing rate is 33%.
TABLE 4 ingredients and contents of materials A, B, C and D in example 8 and comparative examples 1-4, in kg
Performance detection
The slump retaining agents obtained in the examples 1-17 and the comparative examples 1-4 are added into concrete for performance detection, the detection results are shown in Table 5, and the concrete proportion is as follows: 280kg of cement, 65kg of fly ash, 90kg of mineral powder, 800kg of sand, 1000kg of stones, 170kg of water and 12kg of slump retaining agent.
Testing the fluidity of the cement paste according to GB8067-2008 'concrete admixture'; the concrete viscosity performance is evaluated by testing the air flow time of the concrete mixture by adopting an inverted slump bucket according to the regulation of JGJ281-2012 'technical specification for high-strength concrete application'.
TABLE 5 concrete test results table
As can be seen from table 5 of the present application:
as can be seen from examples 1 to 17 and comparative example 5, after the slump retaining agent obtained in each example of the application is applied to concrete, the slump loss rate of 2h is smaller than that of comparative example 5, and besides, the influence of the slump retaining agent obtained in the application on the setting performance of the concrete is smaller than that of the slump retaining agent in comparative example 5, so that the formula of the application can not only improve the slump retaining and flowing performance of the concrete, but also has little influence on the setting performance of the concrete.
In examples 1 to 3, the slump retention ability of the concrete tended to increase and decrease with increasing acrylic acid content, and the viscosity property also tended to decrease, and both slump retention ability and viscosity property were better in example 2.
In examples 4 to 8, the fluidity of the concrete is in a rising trend, and the slump loss of the concrete 2h in example 8 is 210mm, the slump loss at 2h is 525mm, and the fluidity is good, which indicates that the slump retaining agent in example 8 can effectively improve the slump retaining performance of the concrete. In addition, the setting time difference of the concrete is in the range of GB8067-2008, and the setting time difference of the concrete in the embodiments 4-8 is within +/-25 min, so that the influence on the initial setting and the final setting of the concrete is very little.
Examples 9-10 compared with example 8, when the ratio of each component in materials A, B, C and D was constant and the total amount of materials A, B, C and D was changed, the slump retaining ability of the concrete in examples 9 and 10 was reduced compared with that of the concrete in example 8, and the difference in setting time was increased compared with that in example 8, indicating that the lower the total amount of materials A, B, C and D, the poorer the flow property of the concrete and the reduced slump retaining ability.
Compared with the example 8, when the hydroxyethyl acrylate is added into the material A, the flow performance of the concrete in the examples 11 to 14 is increased firstly and then reduced, and in the example 13, the flow performance of the concrete is optimal, which shows that the combination of the acrylic acid and the hydroxyethyl acrylate can effectively improve the flow performance of the concrete, and simultaneously, the slump loss of the concrete for 2h is less than 3%, and the slump retaining performance of the concrete is effectively improved.
Examples 15-16 compare with example 8, when the ratio of mercaptopropionic acid to sodium hypophosphite in the B material is in the range, the fluidity and slump retention of concrete are also better, which shows that the chain transfer agent in the range of the application can reduce the free energy of the cement particle and water interface, thereby improving the workability of concrete.
In comparison with example 8, when the total amount of the materials A, B, C and D is lower or higher than the limit of the application and the proportion range of the components in the materials A, B, C and D is beyond the limit of the application, the slump retaining performance and the flow performance of the concrete are obviously reduced, so that the mutual matching of the components in the formula can effectively improve the slump retaining performance and the flow performance of the concrete.
The embodiments of the present invention are preferred embodiments of the present invention, and the scope of the present invention is not limited by these embodiments, so: all equivalent changes made according to the structure, shape and principle of the invention are covered by the protection scope of the invention.
Claims (8)
1. A high-performance ultra-slow release slump retaining agent is characterized in that: the slump retaining agent comprises, by weight, 34-36 parts of methyl allyl polyoxyethylene ether, 20-24 parts of water, 15-20 parts of a material A, 15-15.5 parts of a material B, 0.5-0.9 part of a material C and 0.48-0.52 part of a material D, wherein:
the material A comprises acrylic acid and water, and the weight ratio of the acrylic acid to the water is (1-3) to 10;
the material B comprises a chain transfer agent, a reducing agent and water, and the weight ratio of the chain transfer agent to the reducing agent to the water is (0.14-0.2): (0.04-0.08): 15;
the component C comprises an oxidant and water, and the weight ratio of the oxidant to the water is (0.2-0.3) to 0.5;
the D material comprises initiator and water, and the weight ratio of the initiator to the water is (0.003-0.006): 0.5.
2. The high-performance ultra-slow release slump retaining agent as claimed in claim 1, wherein: the material A also comprises a hydroxyl ester monomer, wherein the weight ratio of acrylic acid to the hydroxyl ester monomer to water is (1-3) to (4-6) to 10.
3. The high-performance ultra-slow release slump retaining agent as claimed in claim 2, wherein: the weight ratio of acrylic acid, hydroxyl ester monomer and water in the material A is (1.5-2) to (4.5-6) to 10.
4. The high-performance ultra-slow release slump retaining agent as claimed in claim 2, wherein: the hydroxyl ester monomer adopts hydroxyethyl acrylate or hydroxypropyl acrylate.
5. The high-performance ultra-slow release slump retaining agent as claimed in claim 1, wherein: and the reducing agent in the material B adopts vitamin C.
6. The high-performance ultra-slow release slump retaining agent as claimed in claim 1, wherein: the chain transfer agent in the material B comprises mercaptopropionic acid and sodium hypophosphite, wherein the weight ratio of the mercaptopropionic acid to the sodium hypophosphite is (0.9-1.2): 1.
7. The high-performance ultra-slow release slump retaining agent as claimed in claim 1, wherein: the oxidant is hydrogen peroxide.
8. A preparation method of the high-performance ultra-slow release slump retaining agent as claimed in any one of claims 1 to 7, comprising the following steps: dissolving methyl allyl polyoxyethylene ether in water, heating to 25-35 ℃, adding the material C and the material D, stirring for 10-20min, starting to dropwise add the material A and the material B, keeping the temperature at 35-45 ℃ after dropwise adding, keeping the temperature for 1-1.5h, adding water for diluting to obtain the slump retaining agent with the solid content of 40%, wherein the dropwise adding time of the material A is 1-1.5h, and the dropwise adding time of the material B is 1.5-2.0 h.
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Address after: 030023 Building 1, No. 10, Xindian street, Jiancaoping District, Taiyuan City, Shanxi Province Patentee after: Shanxi Tiandingheng Concrete Admixture Technology Development Co.,Ltd. Address before: 030023 Building 1, No. 10, Xindian street, Jiancaoping District, Taiyuan City, Shanxi Province Patentee before: TAIYUAN CITY TIANDINGHENG CONCRETE ADMIXTURES TECHNOLOGY DEVELOPMENT Co.,Ltd. |