CN114380957B - 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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- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 109
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 80
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 74
- 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 31
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 31
- 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 11
- 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 compound 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 13
- 229910001379 sodium hypophosphite Inorganic materials 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
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 11
- -1 hydroxy ester Chemical class 0.000 claims description 11
- 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
- 239000000178 monomer Substances 0.000 claims description 10
- 235000019154 vitamin C Nutrition 0.000 claims description 10
- 239000011718 vitamin C Substances 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 5
- 239000000654 additive Substances 0.000 abstract 1
- 239000004568 cement Substances 0.000 description 25
- 238000006243 chemical reaction Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 11
- 239000002245 particle Substances 0.000 description 11
- 230000015572 biosynthetic process Effects 0.000 description 8
- 230000014759 maintenance of location Effects 0.000 description 8
- 238000003786 synthesis reaction Methods 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 6
- 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
- 238000012360 testing method Methods 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 125000004185 ester group Chemical group 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 239000007864 aqueous solution 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
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution 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
- 238000002474 experimental method Methods 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 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
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 125000005394 methallyl group Chemical group 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 235000019260 propionic acid Nutrition 0.000 description 1
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 239000004575 stone 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 application discloses a high-performance ultra-slow release slump retaining agent and a preparation method thereof, which belong to the technical field of concrete additives, and the technical scheme is characterized in that the slump retaining agent comprises 34-36 parts by weight of methyl allyl polyoxyethylene ether, 20-24 parts by weight of water, 15-20 parts by weight of A material, 15-15.5 parts by weight of B material, 0.5-0.9 part by weight of C material and 0.48-0.52 part by weight of D material, wherein: the material A comprises acrylic acid and water, wherein the weight ratio of the acrylic acid to the water is (1-3) 10; the material B comprises chain transfer agent, reducing agent and water, wherein 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 material C comprises an oxidant and water, wherein the weight ratio of the oxidant to the water is (0.2-0.3) 0.5; the material D comprises an initiator and water, wherein 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 application relates to the field of slump retaining agents, in particular to a high-performance ultra-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 dispersion performance, small slump, environmental friendliness and the like, and the requirements on the slump retaining agent in engineering are increasing along with the mature use of the slump retaining agent.
The slump loss of concrete is large when the slump loss is transported at high temperature and long distance, and in order to reduce the slump loss, the mode adopted at present is as follows: adding water for remodeling, adding slump retaining agent for multiple times, compounding retarder components and the like, but the method not only increases the production cost, but also produces certain side effect on the strength of the concrete. Therefore, the slump retaining agent is developed, the slump retaining agent is abbreviated, the synthesis technology of the existing slump retaining agent is relatively mature, but in the synthesis process, the reaction temperature is as high as 80 ℃, so that the production efficiency of the slump retaining agent is lower, and the energy consumption of industrial production is low.
Disclosure of Invention
In order to improve the production efficiency of the slump retaining agent, the application provides a high-performance ultra-slow release slump retaining agent and a preparation method thereof.
In a first aspect, the application provides a high-performance ultra-slow release slump retaining agent, which adopts the following technical scheme:
the high-performance ultra-slow release slump retaining agent comprises 34-36 parts by weight of methyl allyl polyoxyethylene ether, 20-24 parts by weight of water, 15-20 parts by weight of material A, 15-15.5 parts by weight of material B, 0.5-0.9 part by weight of material C and 0.48-0.52 part by weight of material D, wherein:
the material A comprises acrylic acid and water, wherein the weight ratio of the acrylic acid to the water is (1-3) 10;
the material B comprises chain transfer agent, reducing agent and water, wherein 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 material C comprises an oxidant and water, wherein the weight ratio of the oxidant to the water is (0.2-0.3) 0.5;
the material D comprises an initiator and water, wherein the weight ratio of the initiator to the water is (0.003-0.006) 0.5.
By adopting the technical scheme, the chain transfer agent, the reducing agent and the oxidant are matched with the methallyl polyoxyethylene ether and the acrylic acid, so that the reaction temperature can be effectively reduced, the temperature is 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 methyl allyl polyoxyethylene ether, acrylic acid, chain transfer agent, reducing agent and oxidant, can wrap cement particles to form steric hindrance, improves the dispersion performance of the slump-retaining agent, and carboxyl in acrylic acid, so that slump-retaining agent molecules are preferentially adsorbed on cement particles, and have relatively good dispersion performance, but the content of acrylic acid is beneficial to improving the dispersibility of cement paste when the use amount of acrylic acid is large, but has adverse effect on the maintenance of the dispersibility, so that the content of acrylic acid, methyl allyl polyoxyethylene ether, chain transfer agent, reducing agent and oxidant is limited in the range of the application, the formed slump-retaining agent has better degree of freedom in free water, can promote the slump-retaining agent to be adsorbed and dispersed more rapidly in cement paste, and meanwhile, the thickness of a water film layer formed by polycarboxylic acid molecules in the cement paste is lower, so that more free water can be released, the viscosity of 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 hydroxy ester monomer, wherein the weight ratio of acrylic acid to hydroxy ester monomer to water is (1-3): 4-6): 10.
Preferably, the weight ratio of the acrylic acid to the hydroxy ester monomer to the water in the material A is (1.5-2): 4.5-6): 10.
By adopting the technical scheme, the characteristic that the carboxyl is released by slowly hydrolyzing the ester group in an alkaline environment is utilized by adding the ester group on the main chain of the slump retaining agent, so that the slump retaining agent is provided with long-time slump retaining performance.
In addition, experiments show that the fluidity of the cement paste doped with the slump retaining agent is increased and then reduced along with the increase of the dosage of the hydroxy ester monomer, and the reason is that the increase of the dosage of the hydroxy ester monomer relatively reduces the side chain density of the slump retaining agent, so that the slump retaining agent has a reduced adsorption effect on the cement surface, and the dispersibility and dispersion retention property are both in a reduced trend, so that the slump retaining performance of the cement paste can be effectively improved when the acrylic acid and the hydroxy ester monomer are limited in the range of the cement paste.
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 the 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 hydrophobic propionic 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 further improved. In addition, vitamin C contains a large number of carboxyl and hydroxyl groups with strong polar functional groups, and the groups provide dispersion and flow properties for cement particles through the surface activity actions of adsorption, dispersion, wetting and the like, and reduce the free energy of the interface between the cement particles and water to increase the workability of cement paste. 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 and the cement particles are dispersed, the coagulation tendency of cement paste is inhibited, the contact area of the cement particles and water is increased, cement is fully hydrated, free water surrounded by aggregates is discharged in the process of diffusing the cement particles, and workability is improved and water mixing quantity is reduced.
Preferably, 27.5wt% 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: adding methyl allyl polyoxyethylene ether into water to dissolve and raise the temperature to 25-35 ℃, adding C material and D material, stirring for 10-20min, then starting to drop A material and B material, wherein the drop A material is 1-1.5h, the drop B material is 1.5-2.0h, the temperature is kept between 35-45 ℃ after the drop is finished, and after the temperature is kept for 1-1.5h, adding water to dilute 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, and 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 7-9h synthesis time and 80 ℃ synthesis temperature, the production process of the slump retaining agent reduces the synthesis cost by about 20 percent, and effectively improves the production efficiency.
In summary, the application has the following beneficial effects: according to the application, the acrylic acid, the hydroxy ester monomer, the sodium hypophosphite and the vitamin C are matched with each other, 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 can 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 application will be described in further detail with reference to examples.
The raw materials adopted in the application are all from the market.
Example 1
A preparation method of a high-performance ultra-slow release slump retaining agent comprises the following steps:
(1) 34kg of methyl allyl polyoxyethylene ether and 20kg of water are added into a reaction kettle, stirred and dissolved, and heated to 25 ℃;
(2) Adding 0.75kg of C material and 0.51kg of D material into the reaction kettle, and stirring for 10min;
(3) Then 17kg of material A and 15.2kg of material B are added dropwise, the time for adding the material A is 1h, and the time for adding the material B is 1.5h;
(4) After the dripping is finished, keeping the temperature at 35 ℃, preserving the heat for 1h, and adding water for dilution 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 material B comprises chain transfer agent, vitamin C and water, wherein 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 the mercaptopropionic acid and sodium hypophosphite, and 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 the table 1.
Example 2
The preparation method of the 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 the material A was 2:10, and the rest was the same as in example 1, with specific reference to Table 1.
Example 3
The preparation method of the 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 the material A was 3:10, and the rest was the same as in example 1, with specific reference to Table 1.
Example 4
The preparation method of the 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 the material B was 0.17:0.06:15, the remainder being the same as in example 2, with specific reference to Table 1.
Example 5
The preparation method of the 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, sodium hypophosphite and water in the material B is 0.2:0.0.08:15, and the rest is the same as in the example 2, and the specific reference is shown in the table 1.
Example 6
The preparation method of the 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 the material C is 0.25:0.5, and the rest is the same as in the example 4, specifically referring to Table 1.
Example 7
The preparation method of the 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 the material C is 0.3:0.5, and the rest is the same as in the example 4, specifically referring to Table 1.
Example 8
The preparation method of the high-performance ultra-slow release slump retaining agent is different from that of 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 examples 1-8A, B, C and D were prepared from the following components in units: kg (kg)
Example 9
The preparation method of the high-performance ultra-slow release slump retaining agent is different from that of the embodiment 8 in that: the total amount of the A material was 15kg, the total amount of the B material was 15kg, the total amount of the C material was 5kg, the total amount of the D material was 4.8kg, and the other components were the same as those in example 8 in terms of the preparation method and the proportions of the component in the A material, the component in the B material, the component in the C material and the component in the D material were the same as those in example 8, and the specific contents of the components are shown in Table 2.
Example 10
The preparation method of the high-performance ultra-slow release slump retaining agent is different from that of the embodiment 8 in that: the total amount of the A material was 20kg, the total amount of the B material was 15.5kg, the total amount of the C material was 9kg, the total amount of the D material was 5.2kg, and the preparation method and the proportions of the component in the A material, the component in the B material, the component in the C material and the component in the D material were the same as those in the respective examples 8, except that the specific contents of the components are shown in Table 2.
Table 2 examples 9-10A, B, C and D, components and contents, unit: kg (kg)
Example 11
The preparation method of the high-performance ultra-slow release slump retaining agent is different from the embodiment 8 in that the material A comprises acrylic acid, hydroxyethyl acrylate and water, wherein the 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 content is shown in Table 3.
Example 12
The preparation method of the high-performance ultra-slow release slump retaining agent is different from the embodiment 8 in that the material A comprises acrylic acid, hydroxyethyl acrylate and water, wherein the acrylic acid: hydroxyethyl acrylate: the weight ratio of water was 1.5:4.5:10, the remainder being the same as in example 8, the specific contents being as in Table 3.
Example 13
The preparation method of the high-performance ultra-slow release slump retaining agent is different from the embodiment 8 in that the material A comprises acrylic acid, hydroxyethyl acrylate and water, wherein the acrylic acid: hydroxyethyl acrylate: the weight ratio of water was 2:5:10, the remainder being the same as in example 8, the specific contents being as shown in Table 3.
Example 14
The preparation method of the high-performance ultra-slow release slump retaining agent is different from the embodiment 8 in that the material A comprises acrylic acid, hydroxyethyl acrylate and water, wherein the acrylic acid: hydroxyethyl acrylate: the weight ratio of water was 3:6:10, the remainder being the same as in example 8, the specific contents being as shown in Table 3.
Table 3 the contents of the components in the materials of examples 8, 11-14A, unit: kg (kg)
Example 15
The preparation method of the high-performance ultra-slow release slump retaining agent is different from that 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
The preparation method of the high-performance ultra-slow release slump retaining agent is different from that in the embodiment 8 in that the weight ratio of the mercaptopropionic acid to sodium hypophosphite in the material B is 1.2:1, namely 0.09kg of the mercaptopropionic acid and 0.08kg of sodium hypophosphite, and the rest is the same as that in the embodiment 8.
Example 17
The preparation method of the high-performance ultra-slow release slump retaining agent is different from that of the embodiment 8 in that the methyl allyl polyoxyethylene ether, the reaction temperature and the reaction time are as follows:
(1) Adding 36kg of methyl allyl polyoxyethylene ether and 24kg of water into a reaction kettle, stirring for dissolution, and heating to 35 ℃;
(2) Adding 0.75kg of C material and 0.51kg of D material into the reaction kettle, and stirring for 20min;
(3) Then 17kg of material A and 15.2kg of material B are added dropwise, the time for adding the material A is 1.5h, and the time for adding the material B is 2.0h;
(4) After the dripping is finished, the temperature is kept at 45 ℃, and after the heat preservation is carried out for 1.5 hours, water is added for dilution, and the slump retaining agent with the solid content of 40% is obtained.
Comparative example 1
The difference from example 8 was that the amount of the specific components of the materials A, B, C and D were 14kg, 14kg of the material B, 0.4kg of the material C and 0.4kg of the material D, which were the same as those in example 8, and the specific components of the materials A, B, C and D were as shown in Table 4.
Comparative example 2
The difference from example 8 was that the amount of the specific components of the materials A, B, C and D were as shown in Table 4, except that the materials A, B, C and D were 25kg, 17kg, 1.0kg and 0.6kg, respectively.
Comparative example 3
The difference from example 8 is that the weight ratio of acrylic acid to water in the material 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, with the same exception as in example 8.
Comparative example 4
The difference from example 8 is that the weight ratio of acrylic acid to water in the material 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, all other things being equal to example 8.
Comparative example 5
Commercial slump retaining agent with pH value of 6.0-8.0 and solid content of 40.0 + -1.0 and water reducing rate of 33%.
TABLE 4 composition and content of A, B, C, D in example 8 and comparative examples 1 to 4, unit kg
Performance detection
The slump retaining agents obtained in examples 1 to 17 and comparative examples 1 to 4 were added to concrete for performance test, the test results are shown in Table 5, and the concrete proportions are: 280kg of cement, 65kg of fly ash, 90kg of mineral powder, 800kg of sand, 1000kg of stone, 170kg of water and 12kg of slump retaining agent.
Testing the fluidity of cement paste according to GB8067-2008 concrete admixture; the viscosity performance of the concrete is evaluated by testing the flow time of the concrete mixture by adopting an inverted slump bucket according to the specification of JGJ 281-2012.
Table 5 concrete test results table
As can be seen from table 5 of the present application:
examples 1 to 17 and comparative example 5 show that the slump loss rate of the slump retention agent obtained in each example of the present application is smaller than that in comparative example 5 after the slump retention agent is applied to concrete, and in addition, the slump retention agent obtained in the present application has less influence on the setting property of concrete than that in comparative example 5, which means that the formulation of the present application can not only improve the slump retention and flow properties of concrete, but also has little influence on the setting property of concrete.
In examples 1 to 3, the slump retaining performance of concrete tended to decrease after increasing the acrylic acid content, the viscosity performance also tended to decrease, and both the slump retaining performance and the viscosity performance were better in example 2.
In examples 4 to 8, the fluidity of the concrete tended to increase, and in example 8, the slump of the concrete 2h was 210mm, and the expansion at 2h was 525mm, and the fluidity was good, thus indicating that the slump retention agent in example 8 was able to effectively improve the slump retention performance of the concrete. In addition, the setting time difference of the concrete is within the range of GB8067-2008, and the setting time difference of the concrete in the embodiment 4-8 is within +/-25 min, so that the influence on initial setting and final setting of the concrete is very little.
Examples 9 to 10 showed that when the proportions of the respective components in the materials a, B, C and D were unchanged as compared with example 8, the slump retaining properties of the concrete in examples 9 and 10 were lowered as compared with example 8, and the setting time difference was prolonged as compared with example 8, indicating that the lower the total amounts of the materials a, B, C and D were, the poorer the flowability of the concrete and the slump retaining properties were lowered.
Compared with example 8, when hydroxyethyl acrylate is added into the material A, the flow property of the concrete in examples 11-14 is firstly increased and then decreased, and when the material A is used in example 13, the flow property of the concrete is optimal, which shows that the combination of acrylic acid and hydroxyethyl acrylate can effectively improve the flow property of the concrete, and meanwhile, the slump loss of the concrete for 2 hours is less than 3 percent, so that the slump retention property of the concrete is effectively improved.
Examples 15-16 compared with example 8, when the ratio of the mercaptopropionic acid to the sodium hypophosphite in the material B is within the range, the fluidity and slump retaining performance of the concrete are also better, which shows that the chain transfer agent can reduce the free energy of the cement particle-water interface within the scope of the application, thereby improving the workability of the concrete.
Comparative examples 1 to 4 compared with example 8, when the total amount of the materials A, B, C and D is lower or higher than the limit of the present application and the ratio of the components in the materials A, B, C and D is out of the limit of the present application, the slump retaining performance and the fluidity of the concrete are remarkably reduced, and thus, it is seen that the slump retaining performance and the fluidity of the concrete can be effectively improved by the mutual cooperation of the components in the formulation of the present application.
The embodiments of the present application are all preferred embodiments of the present application, and are not intended to limit the scope of the present application in this way, therefore: all equivalent changes in structure, shape and principle of the application should be covered in the scope of protection of the application.
Claims (3)
1. A high-performance ultra-slow release slump retaining agent is characterized in that: the slump retaining agent comprises 34-36 parts of methyl allyl polyoxyethylene ether, 20-24 parts of water, 15-20 parts of material A, 15-15.5 parts of material B, 0.5-0.9 part of material C and 0.48-0.52 part of material D, wherein the slump retaining agent comprises the following components in parts by weight:
the material A comprises (1.5-2) 10 of hydroxy ester monomer, acrylic acid and water;
the material B comprises chain transfer agent, reducing agent and water, wherein 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 chain transfer agent comprises the weight ratio of the mercaptopropionic acid to the sodium hypophosphite (0.9-1.2) 1; the reducing agent adopts vitamin C;
the material C comprises an oxidant and water, wherein the weight ratio of the oxidant to the water is (0.2-0.3) 0.5;
the material D comprises an initiator and water, wherein the weight ratio of the initiator to the water is (0.003-0.006) 0.5;
the preparation method of the high-performance ultra-slow release slump retaining agent comprises the following steps: adding methyl allyl polyoxyethylene ether into water to dissolve and raise the temperature to 25-35 ℃, adding C material and D material, stirring for 10-20min, then starting to drop A material and B material, wherein the drop A material is 1-1.5h, the drop B material is 1.5-2.0h, maintaining the temperature at 35-45 ℃ after the drop is finished, preserving the heat for 1-1.5h, and adding water to dilute to obtain the slump retaining agent with the solid content of 40%.
2. The high-performance ultra-slow release slump retaining agent according to claim 1, wherein: the hydroxy ester monomer adopts hydroxyethyl acrylate or hydroxypropyl acrylate.
3. The high-performance ultra-slow release slump retaining agent according to claim 1, wherein: the oxidant adopts hydrogen peroxide.
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