CN111892678B - Ketene concrete glue reducing agent and preparation method thereof - Google Patents
Ketene concrete glue reducing agent and preparation method thereof Download PDFInfo
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- CN111892678B CN111892678B CN202010750642.9A CN202010750642A CN111892678B CN 111892678 B CN111892678 B CN 111892678B CN 202010750642 A CN202010750642 A CN 202010750642A CN 111892678 B CN111892678 B CN 111892678B
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- 239000004567 concrete Substances 0.000 title claims abstract description 100
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 83
- CCGKOQOJPYTBIH-UHFFFAOYSA-N ethenone Chemical compound C=C=O CCGKOQOJPYTBIH-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000003292 glue Substances 0.000 title abstract description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- YYPNJNDODFVZLE-UHFFFAOYSA-N 3-methylbut-2-enoic acid Chemical compound CC(C)=CC(O)=O YYPNJNDODFVZLE-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003999 initiator Substances 0.000 claims abstract description 15
- 239000000178 monomer Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 30
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 13
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 8
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- UCUUFSAXZMGPGH-UHFFFAOYSA-N penta-1,4-dien-3-one Chemical compound C=CC(=O)C=C UCUUFSAXZMGPGH-UHFFFAOYSA-N 0.000 claims description 8
- -1 disaccharide compound Chemical class 0.000 claims description 7
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 claims description 6
- UYLUJGRCKKSWHS-UHFFFAOYSA-N prop-1-en-1-one Chemical compound CC=C=O UYLUJGRCKKSWHS-UHFFFAOYSA-N 0.000 claims description 4
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 3
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 3
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 3
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 2
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 2
- 239000008101 lactose Substances 0.000 claims description 2
- 125000003071 maltose group Chemical group 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000004568 cement Substances 0.000 abstract description 35
- 230000000694 effects Effects 0.000 abstract description 6
- 238000010276 construction Methods 0.000 abstract description 4
- 230000002035 prolonged effect Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 11
- 238000006116 polymerization reaction Methods 0.000 description 9
- 230000036571 hydration Effects 0.000 description 7
- 238000006703 hydration reaction Methods 0.000 description 7
- 229920000642 polymer Polymers 0.000 description 7
- 239000002253 acid Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 239000004575 stone Substances 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- NWXORMWIWGSYJJ-UHFFFAOYSA-N 2-ethylbut-1-en-1-one Chemical compound CCC(CC)=C=O NWXORMWIWGSYJJ-UHFFFAOYSA-N 0.000 description 2
- 229920001732 Lignosulfonate Polymers 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- HOOWDPSAHIOHCC-UHFFFAOYSA-N dialuminum tricalcium oxygen(2-) Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[Al+3].[Al+3].[Ca++].[Ca++].[Ca++] HOOWDPSAHIOHCC-UHFFFAOYSA-N 0.000 description 2
- 239000002986 polymer concrete Substances 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000001361 allenes Chemical class 0.000 description 1
- AGWMJKGGLUJAPB-UHFFFAOYSA-N aluminum;dicalcium;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Al+3].[Ca+2].[Ca+2].[Fe+3] AGWMJKGGLUJAPB-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 229910001653 ettringite Inorganic materials 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000013100 final test Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 125000000468 ketone group Chemical group 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- IIACRCGMVDHOTQ-UHFFFAOYSA-M sulfamate Chemical compound NS([O-])(=O)=O IIACRCGMVDHOTQ-UHFFFAOYSA-M 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate group Chemical group S(=O)(=O)([O-])[O-] QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000011882 ultra-fine particle Substances 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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
-
- 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
-
- 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
- C08F224/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a heterocyclic ring containing oxygen
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses an ketene concrete gel reducing agent and a preparation method thereof, wherein the concrete gel reducing agent consists of the following substances in percentage by weight: 8-25 parts of dimethyl acrylic acid, 8-20 parts of ketene monomer, 3-10 parts of ethylene glycol, 2-8 parts of retarder, 0.5-3 parts of initiator and the balance of water. The invention can improve the working performance of the concrete, in particular, the cement can be more fully dispersed in the concrete, the utilization rate of the cement is higher, and thus the early strength and the later strength of the concrete are obviously improved; in addition, the later toughness and crack resistance of the concrete are improved. Because the glue reducing agent has the effects of improving the strength and the crack resistance of the concrete, the cement consumption of the concrete in unit volume can be reduced on the premise of keeping the strength of the concrete unchanged in engineering operation, the service life of a concrete building is prolonged, and the construction cost is reduced.
Description
Technical Field
The invention relates to the technical field of concrete admixtures, in particular to an ketene concrete glue reducing agent and a preparation method thereof.
Background
In recent years, the construction industry in China is unprecedentedly developed, and the scale of the building is unprecedented along with the updating and the perfection of infrastructure. Concrete in building materials is widely used in civil engineering construction due to factors such as abundant raw materials, low price, simple production process, wide compression strength grade range and the like. Cement is the main component of concrete, and is a part of the material with the highest cost of concrete. According to a large amount of researches, 10% -15% of cement in the existing concrete is not completely dispersed and hydrated, so that the due effect cannot be fully exerted, and if the hydration rate of the cement can be improved, a large amount of engineering cost can be saved. In addition, the concrete is often broken in the later maintenance, which seriously shortens the service life of the engineering building.
The concrete gel reducing agent is a novel additive different from other concrete additives, and has the main functions of reducing the using amount of cement and simultaneously ensuring that other performances of concrete are not reduced under the same concrete strength requirement.
Patent application publication CN110845672A reports a polycarboxylic acid type concrete gel reducer, which is formed by polymerizing a polyether macromonomer, an unsaturated carboxylic acid, a modified alcohol amine and the like, and side reactions often occur in the actual preparation process, so that the effect of the gel reducer is unstable, and the gel reducer is only compatible with a polycarboxylic acid water reducer, and the application range of the gel reducer is limited.
Patent application publication CN110903435A reports a gel reducer and a preparation method thereof, wherein a polymer with a high molecular structure is formed under the action of unsaturated carboxylic acid and a saccharide compound by taking a common water reducer in the market as a matrix, and the gel reducer certainly improves the early strength of concrete but does not obviously improve the later strength of the concrete.
Disclosure of Invention
The invention aims to provide an ketene concrete glue reducing agent and a preparation method thereof aiming at the defects of the prior art. It can make the cement more fully dispersed in the concrete, thus improving the early strength and the later strength of the concrete. In addition, the glue reducing agent can improve the toughness and the crack resistance of concrete. The vinyl ketone concrete gel reducing agent is selected, so that the durability of concrete is increased while the cement consumption is saved, and the engineering cost is reduced.
The purpose of the invention is realized by the following technical scheme: an ketene concrete glue reducing agent comprises the following raw materials in percentage by weight:
further, the molar ratio of the dimethyl acrylic acid to the ketene monomer to the ethylene glycol to the initiator is 2-6: 1-4: 0.5-3: 0.1-0.3.
Furthermore, the mol ratio of the dimethyl acrylic acid, the ketene monomer, the ethylene glycol and the initiator is preferably 3-6: 1.5-3: 0.5-2: 0.1-0.2.
Furthermore, the ketene monomer is prepared by mixing one or more of diethylketene, methyl ketene, 3,5 dienone, 4,5 allene and the like according to any proportion.
Further, the retarder is a disaccharide compound, and the disaccharide compound comprises lactose and maltose.
Further, the retarder is preferably maltose.
Furthermore, the initiator is formed by mixing one or more of ammonium persulfate, potassium persulfate, sodium persulfate and the like according to any proportion.
Further, the initiator is preferably ammonium persulfate.
The invention also provides a preparation method of the ketene concrete gel reducing agent, which comprises the following steps:
(1) and (3) taking materials, and preparing an initiator solution with the mass percentage concentration of 3-8%.
(2) Adding ketene monomers, dimethyl acrylic acid and ethylene glycol into a reflux reaction tank, starting stirring, gradually heating, finally heating to 90-120 ℃, and controlling the heating time to be 30-40 min;
(3) after the temperature is raised to 90-120 ℃, the initiator solution prepared in the step 1 is dripped into the solution system, the dripping speed is controlled, the dripping time is 2-3 hours, the temperature of the solution system is always constant in the dripping process, and the constant temperature reaction is continued for 3-5 hours after the dripping is finished;
(4) stopping heating, stirring and naturally cooling, adding a retarder and the balance of water when the temperature is reduced to below 60 ℃, adjusting the pH value of the solution to 9-10, stirring at a constant temperature of 35-50 ℃ for 0.5-1 hour, and finally cooling the solution to room temperature to obtain the concrete gel reducer.
The final product of the invention is an ketene polymer which is doped into concrete, on one hand, the ketene polymer can generate complex ions which are easy to dissolve in water with calcium ions and iron ions in cement slurry, soluble region points are formed on the surfaces of hydrated cement particles, so that the formation of an impermeable layer is interfered at the initial stage of hydration of the surfaces of the cement particles, the dissolution speed of tricalcium aluminate and tetracalcium aluminoferrite in the cement slurry is accelerated, further tricalcium aluminate and the like and sulfate form needle-column-shaped ettringite crystals, the crystals grow continuously, are mutually crossed and overlapped to form a framework, and are filled and reinforced by C-S-H gel and other hydrates, and the strength of the concrete is improved. On the other hand, due to the strong adsorption capacity, the free energy of the whole system can be greatly reduced, ultrafine particle aggregates in the cementing material can be effectively dispersed, and the secondary agglomeration of cement is reduced, so that cement particles are fully contacted with water, and the hydration of most of cement originally only serving as a filler in concrete is stimulated; in addition, the ketene group-containing polymer can refine and stabilize micro bubbles in slurry due to the special functional group property of the ketene group-containing polymer, the micro bubbles are similar to ball bearings, the cement dispersibility is good, a large number of micro bubbles can improve the pore structure of concrete, the flexural compression ratio of the concrete is higher than that of common concrete, the toughness and the crack resistance of the concrete are improved, and the generation of cracks is reduced. The retarder selects carbohydrate, and a large amount of alcoholic hydroxyl exists in the structure of the retarder, so that the carbohydrate can be adsorbed on the surfaces of cement particles to form hydrophilic films with the same charges, the cement particles are mutually exclusive, early hydration of cement can be prevented while the dispersibility of the cement is improved, and a certain retarding effect is achieved.
Compared with the prior art, the invention has the beneficial effects that:
(1) the ketene concrete gel reducing agent prepared by the invention contains a large amount of ketone groups, and the strong electron-withdrawing property of oxygen enables double bonds to be easily subjected to polymerization reaction so as to generate a stable polymer; moreover, the ketene functional group is easy to form an enol hydrophilic group, has good compatibility with most conventional water reducing agents such as lignosulfonate water reducing agents, polyol series water reducing agents, polycarboxylic acid series water reducing agents and the like, can further disperse cement particles under the action of the water reducing agents, promotes the hydration of the cement particles, and fully exerts the effects of reducing glue and water;
(2) the adhesive reducing agent for the ketene polymer concrete, which is obtained by the invention, can stabilize the service performance of the concrete under the condition of reducing the consumption of cement by about 15 percent;
(3) the ketene polymer concrete gel reducing agent prepared by the invention can improve the early strength and the later strength of concrete, and in addition, the gel reducing agent can increase the toughness of the concrete, improve the breaking ratio and reduce the generation of later cracks of concrete buildings.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the present invention is not limited thereto.
Example 1
An ketene concrete glue reducing agent and a preparation method thereof, comprising the following raw materials by weight percent:
the preparation method of the ketene concrete gel reducing agent is realized by the following steps: 1) adding the diethylenone, the dimethylacrylic acid and the ethylene glycol into a reflux reaction tank, starting stirring, gradually heating, finally heating to 110 ℃, and controlling the heating time to be 40 min;
2) after the temperature is raised to 110 ℃, 1 part of ammonium persulfate solution with the mass percentage concentration of 6% is dripped into the solution system, the dripping speed is controlled, the dripping time is ensured to be 2 hours, the temperature of the solution system is always kept constant in the dripping process, and the constant temperature reaction is continued for 5 hours after the dripping is finished;
3) and 2) stopping heating after the polymerization reaction is finished, stirring and naturally cooling, adding maltose and the balance water when the temperature is reduced to be below 60 ℃, adjusting the pH value of the solution to be 9-10, stirring at constant temperature of 35 ℃ for 0.6 hour, and finally cooling the solution to room temperature (20 ℃) to obtain the concrete gel reducing agent.
Example 2
An ketene concrete glue reducing agent and a preparation method thereof, comprising the following raw materials by weight percent:
the preparation method of the ketene concrete gel reducing agent is realized by the following steps: 1) adding the diethylenone, the dimethylacrylic acid and the ethylene glycol into a reflux reaction tank, starting stirring, gradually heating, finally heating to 120 ℃, and controlling the heating time to be 40 min;
2) after the temperature is raised to 120 ℃, 1.5 parts of ammonium persulfate solution with the mass percentage concentration of 6% is dripped into the solution system, the dripping speed is controlled, the dripping time is ensured to be 2.5 hours, the temperature of the solution system is always kept constant in the dripping process, and the constant-temperature reaction is continued for 4 hours after the dripping is finished;
3) and 2) stopping heating after the polymerization reaction is finished, stirring and naturally cooling, adding maltose and the balance water when the temperature is reduced to be below 60 ℃, adjusting the pH value of the solution to be 9-10, stirring at the constant temperature of 38 ℃ for 0.5 hour, and finally cooling the solution to room temperature (20 ℃) to obtain the concrete gel reducing agent.
Example 3
An ketene concrete glue reducing agent and a preparation method thereof, comprising the following raw materials by weight percent:
the preparation method of the ketene concrete gel reducing agent is realized by the following steps: 1) adding methyl ketene, dimethyl acrylic acid and ethylene glycol into a reflux reaction tank, starting stirring and gradually heating, finally heating to 115 ℃, and controlling the heating time to 35 min;
2) after the temperature is raised to 115 ℃, beginning to dropwise add 1.2 parts of ammonium persulfate solution with the mass percentage concentration of 5% into the solution system, controlling the dropwise adding speed, ensuring that the dropwise adding time is 2 hours, keeping the temperature of the solution system constant all the time in the dropwise adding process, and continuing to perform constant-temperature reaction for 4.5 hours after the dropwise adding is finished;
3) and 2) after the polymerization reaction is finished, stopping heating, stirring and naturally cooling, adding a retarder and the balance of water when the temperature is reduced to below 60 ℃, adjusting the pH value of the solution to 9-10, stirring at a constant temperature of 40 ℃ for 0.4 hour, and finally cooling the solution to room temperature (20 ℃) to obtain the concrete gel reducing agent.
Example 4
An ketene concrete glue reducing agent and a preparation method thereof, comprising the following raw materials by weight percent:
the preparation method of the ketene concrete gel reducing agent is realized by the following steps: 1) adding the diethylenone, the dimethylacrylic acid and the ethylene glycol into a reflux reaction tank, starting stirring, gradually heating, finally heating to 105 ℃, and controlling the heating time to be 36 min;
2) after the temperature is raised to 105 ℃, 1 part of ammonium persulfate solution with the mass percentage concentration of 4% is dripped into the solution system, the dripping speed is controlled, the dripping time is ensured to be 2.2 hours, the temperature of the solution system is always kept constant in the dripping process, and the constant temperature reaction is continued for 4.5 hours after the dripping is finished;
3) and 2) stopping heating after the polymerization reaction is finished, stirring and naturally cooling, adding maltose and the balance water when the temperature is reduced to be below 60 ℃, adjusting the pH value of the solution to be 9-10, stirring at the constant temperature of 42 ℃ for 0.8 hour, and finally cooling the solution to room temperature (20 ℃) to obtain the concrete gel reducing agent.
Example 5
The vinyl concrete gel reducing agent comprises the following raw materials in percentage by weight:
the preparation method of the ketene concrete gel reducing agent is realized by the following steps: 1) adding the diethylketene, the dimethylacrylic acid and the ethylene glycol into a reflux reaction tank, starting stirring, gradually heating, finally heating to 112 ℃, and controlling the heating time to be 34 min;
2) after the temperature is raised to 112 ℃, 1 part of ammonium persulfate solution with the mass percentage concentration of 7% is dripped into the solution system, the dripping speed is controlled, the dripping time is ensured to be 2.5 hours, the temperature of the solution system is always kept constant in the dripping process, and the constant temperature reaction is continued for 4.2 hours after the dripping is finished;
3) and 2) stopping heating after the polymerization reaction is finished, stirring and naturally cooling, adding maltose and the balance water when the temperature is reduced to be below 60 ℃, adjusting the pH value of the solution to be 9-10, stirring at the constant temperature of 40 ℃ for 0.6 hour, and finally cooling the solution to room temperature (20 ℃) to obtain the concrete gel reducing agent.
Comparative example 1
An ketene concrete glue reducing agent and a preparation method thereof, comprising the following raw materials by weight percent:
the preparation method of the ketene concrete gel reducing agent is realized by the following steps: 1) adding 4, 5-allene ketone, dimethyl acrylic acid and ethylene glycol into a reflux reaction tank, starting stirring, gradually heating to 110 ℃, and controlling the heating time to be 40 min;
2) after the temperature is raised to 110 ℃, beginning to dropwise add 2 parts of ammonium persulfate solution with the mass percentage concentration of 4% into the solution system, controlling the dropwise adding speed, ensuring that the dropwise adding time is 3 hours, keeping the temperature of the solution system constant all the time in the dropwise adding process, and continuing to perform constant-temperature reaction for 5 hours after the dropwise adding is finished;
3) and 2) after the polymerization reaction is finished, stopping heating, stirring and naturally cooling, adding a retarder and the balance of water when the temperature is reduced to below 60 ℃, adjusting the pH value of the solution to 9-10, stirring at constant temperature of 35 ℃ for 0.6 hour, and finally cooling the solution to room temperature (20 ℃) to obtain the concrete gel reducing agent.
Comparative example 2
An ketene concrete glue reducing agent and a preparation method thereof, comprising the following raw materials by weight percent:
the preparation method of the ketene concrete gel reducing agent is realized by the following steps: 1) adding the diethylenone, the dimethylacrylic acid and the ethylene glycol into a reflux reaction tank, starting stirring, gradually heating, finally heating to 120 ℃, and controlling the heating time to be 35 min;
2) after the temperature is raised to 120 ℃, 1.5 parts of potassium persulfate solution with the mass percent concentration of 4% is dripped into the solution system, the dripping speed is controlled, the dripping time is ensured to be 3 hours, the temperature of the solution system is always kept constant in the dripping process, and the constant temperature reaction is continued for 4 hours after the dripping is finished;
3) and 2) after the polymerization reaction is finished, stopping heating, stirring and naturally cooling, adding a retarder and the balance of water when the temperature is reduced to below 60 ℃, adjusting the pH value of the solution to 9-10, stirring at a constant temperature of 45 ℃ for 0.5 hour, and finally cooling the solution to room temperature (20 ℃) to obtain the concrete gel reducing agent.
Comparative example 3
An ketene concrete glue reducing agent and a preparation method thereof, comprising the following raw materials by weight percent:
the preparation method of the ketene concrete gel reducing agent is realized by the following steps: 1) adding methyl ketene, dimethyl acrylic acid and ethylene glycol into a reflux reaction tank, starting stirring and gradually heating, finally heating to 125 ℃, and controlling the heating time to be 30 min;
2) after the temperature is raised to 125 ℃, 1.2 parts of sodium persulfate solution with the mass percent concentration of 5% is dripped into the solution system, the dripping speed is controlled, the dripping time is ensured to be 2 hours, the temperature of the solution system is always kept constant in the dripping process, and the constant temperature reaction is continued for 3 hours after the dripping is finished;
3) and 2) stopping heating after the polymerization reaction is finished, stirring and naturally cooling, adding a retarder and the balance of water when the temperature is reduced to below 60 ℃, adjusting the pH value of the solution to 9-10, stirring at a constant temperature of 42 ℃ for 0.4 hour, and finally cooling the solution to room temperature (20 ℃) to obtain the concrete gel reducing agent.
Performance testing
The performance of examples 1-3 and comparative examples 1-3 is tested according to the specification of JC/T2469-2018 concrete gel reducer, and the compressive strength is tested according to GB/T5008-2016 Standard test method for mechanical properties of common concrete. The cement in the raw materials is P.O 32.5 grade sold in the market, the fineness modulus of river sand is 2.5, the broken stone is continuous graded broken stone with the thickness of 5-20 mm, the water reducing agent is a polycarboxylic acid water reducing agent sold in the market, the mixing amount of the water reducing agent is 1.8 percent of the total mass of the cementing material, and the mixing amount of the glue reducing agent is 0.6 percent of the total mass of the cementing material. The blank control group is concrete without adding or reducing the glue agent, other mixing amounts of the blank control group are the same as those of the embodiment group, and the final test results are shown in the following table 1.
Table 1: concrete Performance test results
From the performance test data of the concrete, the overall results show that the strength of the C30 concrete is obviously increased after the vinyl ketone gel reducing agent is added into the concrete, the vinyl ketone polymer can better disperse cement particles in a system, the cement particles are fully excited to perform hydration, the utilization rate of the cement is improved, and the cement dosage can be reduced by about 15% by adding the gel reducing agent under the same 28d strength.
Comparing the ketene type gel reducing agent with a certain common gel reducing agent in the market, and carrying out a series of performance tests such as slump, expansion degree, compressive strength and the like aiming at the compatible effect of the mixing of the ketene type gel reducing agent and a plurality of water reducing agents, wherein the cement in the raw materials is selected from the commercially available P.O 32.5 grade, the fineness modulus of river sand is 2.5, the crushed stone is 5-20 mm of continuous graded crushed stone, the mixing amount of the water reducing agent is 1.8 percent of the total mass of the cementing material, and the mixing amount of the gel reducing agent is 0.6 percent of the total mass of the cementing material.
Table 2: test result of concrete performance comparison experiment
From the comparison of various performances of concrete in table 2, the ketene concrete gel reducer prepared by the invention can be well compatible with most conventional water reducers such as lignosulfonate water reducers, sulfamate water reducers, polycarboxylic acid water reducers and the like, and has a synergistic effect, the gel reducer can further disperse cement particles under the action of the water reducers, promote the hydration of the cement particles, and fully exert the effects of reducing gel and water.
In addition, the ketene concrete gel reducing agent prepared by the invention can improve the compressive strength of the concrete in the early and later stages, and can improve the flexural strength of the concrete, so that the application range of the concrete is wider.
In conclusion, the invention can improve the working performance of the concrete. Particularly, the cement can be more fully dispersed in the concrete, the utilization rate of the cement is higher, the early strength of the concrete is obviously improved, the later strength of the concrete is stabilized, the cement using amount of the concrete in unit volume can be reduced on the premise of keeping the concrete strength unchanged in engineering operation, the service life of a concrete building is prolonged, and the construction cost is reduced.
The above description is only exemplary of the present invention and should not be construed as limiting the invention, and it should be understood that any modification and improvement that fall within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. The vinyl concrete gel reducing agent is characterized by comprising the following raw materials in percentage by weight:
8-25% of dimethyl acrylic acid;
8-20% of an ketene monomer;
3-10% of ethylene glycol;
2-8% of retarder;
0.5-3% of an initiator;
the balance of water;
the ketene monomer is formed by mixing one or more of diethylenone, methyl ketene and 4, 5-allene ketone according to any proportion;
the retarder is a disaccharide compound, and the disaccharide compound is lactose or maltose.
2. The vinyl ketone concrete gel reducing agent as claimed in claim 1, wherein the molar ratio of the dimethyl acrylic acid, the vinyl ketone monomer, the ethylene glycol and the initiator is 2-6: 1-4: 0.5-3: 0.1-0.3.
3. The vinyl ketone concrete gel reducing agent as claimed in claim 2, wherein the molar ratio of the dimethyl acrylic acid, the vinyl ketone monomer, the ethylene glycol and the initiator is 3-6: 1.5-3: 0.5-2: 0.1-0.2.
4. The ketene concrete gel reducing agent according to claim 1, wherein the retarder is maltose.
5. The vinyl ketone concrete gel reducer according to claim 1, wherein the initiator is formed by mixing one or more of ammonium persulfate, potassium persulfate and sodium persulfate according to any proportion.
6. The ketene concrete gel reducing agent according to claim 5, wherein the initiator is ammonium persulfate.
7. The preparation method of the ketene concrete gel reducer of claim 1, which is characterized by comprising the following steps:
(1) taking materials, and preparing an initiator into an initiator solution with the mass percentage concentration of 3-8%;
(2) adding ketene monomers, dimethyl acrylic acid and ethylene glycol into a reflux reaction tank, starting stirring, gradually heating, finally heating to 90-120 ℃, and controlling the heating time to be 30-40 min;
(3) after the temperature is raised to 90-120 ℃, dropwise adding the initiator solution prepared in the step (1) into a solution system, controlling the dropwise adding speed to ensure that the dropwise adding time is 2-3 hours, keeping the temperature of the solution system constant all the time in the dropwise adding process, and continuing to perform constant-temperature reaction for 3-5 hours after the dropwise adding is finished;
(4) stopping heating, stirring and naturally cooling, adding a retarder and the balance of water when the temperature is reduced to below 60 ℃, adjusting the pH of the solution to be = 9-10, stirring at a constant temperature of 35-50 ℃ for 0.5-1 hour, and finally cooling the solution to room temperature to obtain the concrete gel reducer.
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