CN109626860A - A kind of preparation method of block viscosity reduction type concrete admixture - Google Patents
A kind of preparation method of block viscosity reduction type concrete admixture Download PDFInfo
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- CN109626860A CN109626860A CN201811581340.2A CN201811581340A CN109626860A CN 109626860 A CN109626860 A CN 109626860A CN 201811581340 A CN201811581340 A CN 201811581340A CN 109626860 A CN109626860 A CN 109626860A
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- 239000004567 concrete Substances 0.000 title claims abstract description 61
- 230000009467 reduction Effects 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000011259 mixed solution Substances 0.000 claims abstract description 29
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000000178 monomer Substances 0.000 claims abstract description 20
- 229920000570 polyether Polymers 0.000 claims abstract description 19
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 18
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 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 13
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 9
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 7
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000007800 oxidant agent Substances 0.000 claims abstract description 5
- 150000002222 fluorine compounds Chemical class 0.000 claims abstract description 4
- 230000001590 oxidative effect Effects 0.000 claims abstract description 3
- 239000003643 water by type Substances 0.000 claims description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 6
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical compound [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 230000017260 vegetative to reproductive phase transition of meristem Effects 0.000 claims description 6
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 5
- DUCAVBJYSSNCJG-UHFFFAOYSA-N 2-fluoroethyl prop-2-enoate Chemical compound FCCOC(=O)C=C DUCAVBJYSSNCJG-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethyl mercaptane Natural products CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
- KOUKXHPPRFNWPP-UHFFFAOYSA-N pyrazine-2,5-dicarboxylic acid;hydrate Chemical compound O.OC(=O)C1=CN=C(C(O)=O)C=N1 KOUKXHPPRFNWPP-UHFFFAOYSA-N 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- DGVVWUTYPXICAM-UHFFFAOYSA-N β‐Mercaptoethanol Chemical compound OCCS DGVVWUTYPXICAM-UHFFFAOYSA-N 0.000 claims description 4
- GOJUJUVQIVIZAV-UHFFFAOYSA-N 2-amino-4,6-dichloropyrimidine-5-carbaldehyde Chemical group NC1=NC(Cl)=C(C=O)C(Cl)=N1 GOJUJUVQIVIZAV-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- ZTZJVAOTIOAZGZ-UHFFFAOYSA-N methyl 2-fluoroacrylate Chemical compound COC(=O)C(F)=C ZTZJVAOTIOAZGZ-UHFFFAOYSA-N 0.000 claims description 3
- NJASLZAPMXEJML-UHFFFAOYSA-N 7-benzyl-1-bromo-6,8-dihydro-5h-imidazo[1,5-a]pyrazine Chemical compound C1C2=C(Br)N=CN2CCN1CC1=CC=CC=C1 NJASLZAPMXEJML-UHFFFAOYSA-N 0.000 claims description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 2
- RQVLGLPAZTUBKX-UHFFFAOYSA-N D-vinylglycine Natural products C=CC(N)C(O)=O RQVLGLPAZTUBKX-UHFFFAOYSA-N 0.000 claims description 2
- PUAHIVMZATZOHW-UHFFFAOYSA-L OC(C(=O)[O-])S(=O)O.[Na+].[Na+].OC(C(=O)[O-])S(=O)O Chemical compound OC(C(=O)[O-])S(=O)O.[Na+].[Na+].OC(C(=O)[O-])S(=O)O PUAHIVMZATZOHW-UHFFFAOYSA-L 0.000 claims description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- FGRVOLIFQGXPCT-UHFFFAOYSA-L dipotassium;dioxido-oxo-sulfanylidene-$l^{6}-sulfane Chemical compound [K+].[K+].[O-]S([O-])(=O)=S FGRVOLIFQGXPCT-UHFFFAOYSA-L 0.000 claims description 2
- IMLUMMDFXRZWGY-UHFFFAOYSA-L disodium 2-hydroxy-2-sulfoacetate Chemical compound [Na+].[Na+].[O-]C(=O)C(O)S(O)(=O)=O.[O-]C(=O)C(O)S(O)(=O)=O IMLUMMDFXRZWGY-UHFFFAOYSA-L 0.000 claims description 2
- 125000005641 methacryl group Chemical group 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 235000019394 potassium persulphate Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 claims description 2
- PENRVBJTRIYHOA-UHFFFAOYSA-L zinc dithionite Chemical compound [Zn+2].[O-]S(=O)S([O-])=O PENRVBJTRIYHOA-UHFFFAOYSA-L 0.000 claims description 2
- 238000003682 fluorination reaction Methods 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 15
- 239000008367 deionised water Substances 0.000 abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 abstract description 9
- 238000010276 construction Methods 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 7
- 239000002002 slurry Substances 0.000 abstract description 3
- 239000007787 solid Substances 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract description 2
- 230000000996 additive effect Effects 0.000 abstract description 2
- 230000002209 hydrophobic effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000010881 fly ash Substances 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 239000004568 cement Substances 0.000 description 3
- 238000007334 copolymerization reaction Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 150000003254 radicals Chemical class 0.000 description 3
- 239000004575 stone Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- NPSWHDAHNWWMEG-UHFFFAOYSA-N 2-aminohex-5-enoic acid Chemical compound OC(=O)C(N)CCC=C NPSWHDAHNWWMEG-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- YXYZMHGSOKYZAF-UHFFFAOYSA-M [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C Chemical class [Cl-].C(C(=C)C)(=O)OCC[N+](C(C)(C)C)(C)C YXYZMHGSOKYZAF-UHFFFAOYSA-M 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000011376 self-consolidating concrete Substances 0.000 description 2
- WNNNWFKQCKFSDK-SCSAIBSYSA-N (2r)-2-azaniumylpent-4-enoate Chemical compound [O-]C(=O)[C@H]([NH3+])CC=C WNNNWFKQCKFSDK-SCSAIBSYSA-N 0.000 description 1
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 description 1
- PMNLUUOXGOOLSP-UHFFFAOYSA-N 2-mercaptopropanoic acid Chemical class CC(S)C(O)=O PMNLUUOXGOOLSP-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- -1 sulfonic group Chemical group 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- SZYJELPVAFJOGJ-UHFFFAOYSA-N trimethylamine hydrochloride Chemical compound Cl.CN(C)C SZYJELPVAFJOGJ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers 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
- 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
- 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
- C08F285/00—Macromolecular compounds obtained by polymerising monomers on to preformed graft polymers
-
- 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
- C04B2103/34—Flow improvers
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention belongs to build additive technical field, more particularly to a kind of preparation method of block viscosity reduction type concrete admixture, include the following steps: that unsaturated polyether monomer A is added in a kettle, unsaturated polyether monomer B, methyl methacrylate, acrylic acid, unsaturated fluorine compounds, complex reducing agent, chain-transferring agent and deionized water, and it is stirred, after material is completely dissolved, hydrogen peroxide is added, continue to stir, after 2-6h, it is again stirring for, and unsaturated polyether monomer B is added, unsaturated polyether monomer C, hydroxymethyl acrylamide, hydrogen peroxide and deionized water, heat temperature raising, start to drip mixed solution I, with mixed solution II, oxidant is added into reaction kettle again after being added dropwise to complete, then it cools after keeping the temperature 1h, viscosity reduction type concrete admixture can be obtained.The present invention reduces solid particle spacing, reduces particle friction, reduce fresh concrete slurry viscosity, improve concrete construction by introducing hydrophobic grouping in molecular backbone.
Description
Technical field
The invention belongs to build additive technical field, and in particular to a kind of preparation of block viscosity reduction type concrete admixture
Method.
Background technique
Concrete is the important materials of modern construction engineering, for monolithic architecture safe mass, construction period, cost etc.
With great influence, and the use of concrete admixture, the fluidity of concrete mix can be made to greatly improve, or protecting
The use amount of deionized water of concrete mix is greatly reduced in the case where holding identical mobility, while concrete can be made to have
High-durability, thus high-flowing concrete can be made, pump concrete, high grade concrete and high compact coagulation
Soil etc., and be able to satisfy many special circumstances under application demand, be realize Concrete Industry " environmental protection, low-carbon, ecology " send out
The indispensable important component of the core and modern concrete of exhibition has very big development potentiality and development space.
Concrete admixture has excellent dispersion performance, concrete can be made at low dosage to reach preferable flowing
Property, during the preparation process, free radical copolymerization can be passed in principle according to MOLECULE DESIGN and synthesize polymerizable structural unit
The concrete admixture of predetermined structure and performance, usually by containing some tools such as carboxylic acid group, sulfonic group, ester group and polyethylene oxide bases
There is the monomer of unsaturated group to synthesize by free radicals copolymerization reaction.It is different in the polymerization preparation process of concrete admixture
Monomer makes molecule with having certain Molecular Geometries, special structure is determined to condense together at random or regularly
Its superior function is determined.Currently, the molecular structure of most concrete admixtures is linear comb structure, generally in concrete
Heterogeneous system in steric hindrance effect it is weaker, therefore dispersibility in deionized water slurry body, slump retaining, protect deionized water
Effect and its universality are to be improved.
Emphasis concrete construction engineering in general requires concrete to have higher intensity, better durability, more preferably steady
It is qualitative, and this requires concrete that must reach certain strength grade, concrete strength improves mainly by reducing deionized water
Glue ratio realizes, it is larger that this also results in concrete viscosity, causes a series of construction such as concrete stirring, transport, pumping and asks
Topic, largely limits the popularization and application of high-strength shale ceramsite.
The pumping construction of skyscraper concrete also has very high requirement to the workability of concrete, higher in order to reach
Strength grade, can generally pass through reduces deionized water gray scale, increases gel material content, improves mineral admixture ratio etc.
Method is realized.Deionization water-cement ratio is low, and the deionized water in unit volume is reduced, and solid particle spacing is caused to reduce, and particle rubs
The effects of wiping, is reinforced, and cement amount is high, and paste thickness of having more than needed is big, and can be all added in general match ratio large specific surface area,
The problems such as irregular mineral admixture of particle shape looks, such as silicon ash result in the increase of fresh concrete viscosity, and mobility declines.
Summary of the invention
It is an object of the invention to overcome prior art defect, a kind of preparation of block viscosity reduction type concrete admixture is provided
Method.
Technical scheme is as follows:
By weight:
150-180 parts of unsaturations are added in the reaction kettle with thermostat, agitating device, Dropping feeder and nitrogen tube
A, 2-8 parts of unsaturated polyether monomer B, 2-6 part methyl methacrylates of polyether monomer, 5-15 parts of acrylic acid, 0.5-1.5 parts are not
It is saturated fluorine compounds, 0.8-1.8 parts of complex reducing agents, 0.5-1.5 parts of chain-transferring agents and 100-130 parts of deionized waters；
Starting agitating device is stirred, and thermostat is controlled at 30-40 DEG C, and after material is completely dissolved, 1-5 is added
Part hydrogen peroxide continues to stir 30min, then stops stirring；
It after 2-6h, is again started up agitating device and is stirred, and 1-5 parts of unsaturated polyether monomers are added into reaction kettle
B, 5-10 parts of unsaturated polyether monomer C, 1-2 part hydroxymethyl acrylamide, 1-2 parts of hydrogen peroxide and 30 parts of deionized waters；
Then it is heated to 50-60 DEG C, starts to be added dropwise with Dropping feeder by 2-5 parts of acrylic acid, 1-4 parts of methacryls
The mixed solution I that oxy-ethyl-trimethyl salmiac, 1-5 part unsaturated amino compounds and 30 parts of deionized waters are configured to, and
The mixed solution II being configured to by 0.2-0.5 parts of complex reducing agents, 0.1-0.5 parts of chain-transferring agents and 30 parts of deionized waters, mixing
Solution I and mixed solution II should be added dropwise in 0.5-1.5h, solution I and mixed solution II to be mixed be added dropwise to complete after again
0.5-1 parts of oxidants are added into reaction kettle, cools after then keeping the temperature 1h, viscosity reduction type concrete admixture can be obtained.
Further, unsaturated polyether monomer A includes such as flowering structure (a):
H(OCH2CH2)p(OCH2CH2CH2)qOCH2CH2CR1=CH2 (a)
Wherein, p is integer, and 40≤p≤50；Q is integer, and 1≤q≤2；R1For H or CH3。
Further, unsaturated polyether monomer B includes such as flowering structure (b):
H(OCH2CH2)m(OCH2CH2CH2)nO(CH2)xO(C6H4)(CH2)yCR2=CH2 (b)
Wherein, m is integer, and 25≤m≤30；N is integer, and 2≤n≤4；X and y is integer greater than 0, and 2≤x+
y≤4；R2For H or CH3。
Further, unsaturated fluorine compounds are 2- perfluoroalkyl acrylate, in 2- fluoroacrylic methyl ester, 2- fluoroethyl acrylate
One kind.
Further, complex reducing agent by weight, has following composition:
2- hydroxyl -2- sulfinatoacetic acid disodium salt: 10-30%；
2- hydroxyl -2- sulfonatoacetic acid disodium salt: 5-15%；
L-AA: 35-45%；
It is a kind of in sodium dithionite, potassium hyposulfite or zinc dithionite: 20-30%；
It is a kind of in sodium carbonate, sodium bicarbonate, potassium carbonate or saleratus: 5-15%.
Further, chain-transferring agent is one of thioacetic acid, mercaptopropionic acid, mercaptoethanol.
Further, unsaturated polyether monomer C includes such as flowering structure (c):
CH3O(CH2CH2O)h(CH2CH2CH2O)kCH2CH2OOCH2CR3=CH2 (c)
Wherein, h is integer, and 35≤h≤50；K is integer, and 1≤k≤3；R3For H or CH3。
Further, unsaturated amino compounds are D- allylglycine, 2- amino -4- methyl -4- penetenoic acid, 2- ammonia
One of base -3-butenoic acid, 2- amino -5- hexenoic acid.
Further, oxidant is one of hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate.
The beneficial effects of the present invention are: using aqueous free radical copolymerization, using unsaturated monomer, initiator,
Chain-transferring agent etc., which is synthesized by two-step process, prepares block polymer, has strong operability, reaction process is easy to control, to reaction
The features such as condition responsive is low, easy to industrialized production.By the polyethers side for introducing different type and length in molecular side chain
Chain can regulate and control concrete admixture and steric configuration and unfold degree in concrete heterogeneous system, can change concrete admixture
The amount of Free water in the water film thickness and system of formation；By introducing hydrophobic grouping in molecular backbone, reduce solid particle
Spacing reduces particle friction, reduces fresh concrete slurry viscosity, improves concrete construction.
Specific embodiment
In order to which the technical problems, technical solutions and beneficial effects solved by the present invention is more clearly understood, below in conjunction with
Embodiment, the present invention will be described in further detail.It should be appreciated that specific embodiment described herein is only used to explain
The present invention is not intended to limit the present invention.
Wherein, in embodiment 1-4, the ingredient and ratio of used complex reducing agent are as listed in table 1.
1 complex reducing agent ingredient of table and ratio
Embodiment 1
By weight, 180 parts of H are added in the reaction kettle with thermostat, agitating device, Dropping feeder and nitrogen tube
(OCH2CH2)40OCH2CH2CH2OCH2CH2CCH3=CH2, 8 parts of H (OCH2CH2)25(OCH2CH2CH2)2OCH2OC6H4CH2CH=
CH2, 6 parts of methyl methacrylates, 5 parts of acrylic acid, 0.5 part of 2- perfluoroalkyl acrylate, 1.8 parts of complex reducing agents, 1.4 parts of thioacetic acid
With 130 parts of deionized waters, starting agitating device and be stirred, thermostat is controlled at 30 DEG C, after material is completely dissolved,
5 parts of hydrogen peroxide are added, continues to stir 30min, then stops stirring, after 5h, be again started up agitating device and be stirred, and
5 parts are added into reaction kettle
H(OCH2CH2)25(OCH2CH2CH2)2OCH2OC6H4CH2CH=CH2, 8 parts of CH3O(CH2CH2O)35CH2CH2CH2OCH2CH2OOCH2CH=CH2, 1 part of hydroxymethyl acrylamide, 1.5 parts of hydrogen peroxide and 30 parts of deionized waters, so
After be heated to 50 DEG C, start with Dropping feeder be added dropwise by 5 parts of acrylic acid, 1 part of methylacryoyloxyethyl trimethyl ammonia chloride
The mixed solution I that ammonium, 2 parts of D- allylglycines and 30 parts of deionized waters are configured to, and by 0.4 part of complex reducing agent, 0.4
The mixed solution II that part thioacetic acid and 30 parts of deionized waters are configured to, mixed solution I and mixed solution II should drip in 0.5h
Add it is complete, solution I and mixed solution II to be mixed be added dropwise to complete after again into reaction kettle be added 0.5 part of ammonium persulfate, then protect
It cools after warm 1h, viscosity reduction type concrete admixture can be obtained.
Embodiment 2
By weight, 170 parts of H are added in the reaction kettle with thermostat, agitating device, Dropping feeder and nitrogen tube
(OCH2CH2)42(OCH2CH2CH2)2OCH2CH2CH=CH2, 6 parts of H (OCH2CH2)26(OCH2CH2CH2)4OCH2OC6H4CH2CH2CCH3=CH2, 2 parts of methyl methacrylates, 8 parts of acrylic acid, 1 part of 2- fluoroethyl acrylate, 1.5 parts
Complex reducing agent, 1.5 parts of mercaptopropionic acids and 120 parts of deionized waters, starting agitating device be stirred, thermostat controlled at
35 DEG C, after material is completely dissolved, 1 part of hydrogen peroxide is added, continues to stir 30min, then stops stirring, after 2h, again
Starting agitating device is stirred, and 2 parts of H (OCH are added into reaction kettle2CH2)26(OCH2CH2CH2)4OCH2OC6H4CH2CH2CCH3=CH2, 8 parts of CH3O(CH2CH2O)40(CH2CH2CH2O)2CH2CH2OOCH2CCH3=CH2, 1.2 parts
Hydroxymethyl acrylamide, 2 parts of hydrogen peroxide and 30 parts of deionized waters, are then heated to 60 DEG C, start to be dripped with Dropping feeder
Add by 3 parts of acrylic acid, 3 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, 3 parts of 2- amino -4- methyl -4- penetenoic acids and 30
The mixed solution I that part deionized water is configured to, and by 0.3 part of complex reducing agent, 0.2 part of mercaptopropionic acid and 30 parts of deionized waters
The mixed solution II being configured to, mixed solution I and mixed solution II should be added dropwise in 1.5h, solution I to be mixed and mixing
1 part of ammonium persulfate is added after being added dropwise to complete in solution II into reaction kettle again, cools after then keeping the temperature 1h, viscosity reduction can be obtained
Type concrete admixture.
Embodiment 3
By weight, 160 parts of H are added in the reaction kettle with thermostat, agitating device, Dropping feeder and nitrogen tube
(OCH2CH2)46(OCH2CH2CH2)2OCH2CH2CH=CH2, 4 parts of H (OCH2CH2)27(OCH2CH2CH2)3OCH2CH2OC6H4CH2CH
=CH2, 3 parts of methyl methacrylates, 15 parts of acrylic acid, 1.5 parts of 2- fluoroethyl acrylates, 0.8 part of complex reducing agent, 1 part
Mercaptopropionic acid and 110 parts of deionized waters, starting agitating device are stirred, and temperature controller is controlled at 40 DEG C, when material is complete
After dissolution, 2 parts of hydrogen peroxide are added, continue stir 30min, then stop stirring, after 3h, be again started up agitating device into
Row stirring, and 3 parts of H (OCH are added into reaction kettle2CH2)27(OCH2CH2CH2)3OCH2CH2OC6H4CH2CH=CH2, 5 parts
CH3O(CH2CH2O)45(CH2CH2CH2O)3CH2CH2OOCH2CCH3=CH2, 1.6 parts of hydroxymethyl acrylamide, 1 part of hydrogen peroxide and
30 parts of deionized waters, are then heated to 55 DEG C, start to be added dropwise with the Dropping feeder by 2 parts of acrylic acid, 4 parts of metering systems
The mixed solution I that acyloxyethyl trimethyl ammonium chloride, 1 part of 2- amino -3-butenoic acid and 30 parts of deionized waters are configured to, and
The mixed solution II being configured to by 0.3 part of complex reducing agent, 0.1 part of mercaptopropionic acid and 30 parts of deionized waters, mixed solution I and mixed
Closing solution II should be added dropwise in 1h, and solution I and mixed solution II to be mixed are added 1 part after being added dropwise to complete into reaction kettle again
Ammonium persulfate cools after then keeping the temperature 1h, viscosity reduction type concrete admixture can be obtained.
Embodiment 4
By weight, 150 parts of H are added in the reaction kettle with thermostat, agitating device, Dropping feeder and nitrogen tube
(OCH2CH2)50OCH2CH2CH2OCH2CH2CH=CH2, 2 parts of H (OCH2CH2)30(OCH2CH2CH2)2OCH2CH2CH2OC6H4CH2CCH3=CH2, 5 parts of methyl methacrylates, 10 parts of acrylic acid, 0.8 part of 2- fluoroacrylic methyl ester, 1
Part complex reducing agent, 0.5 part of mercaptoethanol and 100 parts of deionized waters, starting agitating device is stirred, controlled at 45
DEG C, after material is completely dissolved, 3 parts of hydrogen peroxide are added, continues to stir 30min, then stops stirring, after 6h, open again
Dynamic agitating device is stirred, and 1 part of H (OCH is added into reaction kettle2CH2)30(OCH2CH2CH2)2OCH2CH2CH2OC6H4CH2CCH3=CH2, 10 parts of CH3O(CH2CH2O)50(CH2CH2CH2O)2CH2CH2OOCH2CCH3=CH2, 2
Part hydroxymethyl acrylamide, 1.2 parts of hydrogen peroxide and 30 parts of deionized waters, are then heated to 60 DEG C, start with dropwise addition dress
Dropwise addition is set to be gone by 5 parts of acrylic acid, 2 parts of MethacryloyloxyethylTrimethyl Trimethyl Ammonium Chlorides, 5 parts of 2- amino -5- hexenoic acids and 30 parts
The mixed solution I that ionized water is configured to, and matched by 0.2 part of complex reducing agent, 0.5 part of mercaptoethanol and 30 parts of deionized waters
The mixed solution II being set to, mixed solution I and mixed solution II should be added dropwise in 1.5h, and solution I to be mixed and mixing are molten
0.8 part of ammonium persulfate is added after being added dropwise to complete in liquid II into reaction kettle again, cools after then keeping the temperature 1h, viscosity reduction can be obtained
Type concrete admixture.
By the embodiment 1-4 sample synthesized and comparative sample (commercial standard type high-performance water reducing agent, HPWR-S),
It is " common according to GB/T 50080-2016 " Standard for test methods of properties of ordinary concrete mixture standard " and GB/T 50081-2016
Mechanical performance of concrete test method standard " carry out concrete mixture characteristic test method and properties of hardened concrete test；
The test of V-type funnel flushing time is carried out according to CECS 203-2006 " self-compacting concrete application technology regulation "；Using CCES
The test of 02-2004 " self-compacting concrete direction of design and construction " progress L-type case flowing time.
The main raw material(s) that performance test uses:
Cement (C): 42.5 ordinary portland cement of P.O, Fujian China Resources Cement Co., Ltd；
Flyash (FA): II grade of flyash, Xiamen Sha Ye trade Co., Ltd；
Miberal powder (SL): S95 grades, Fujian Triratna Iron And Steel Co., Ltd；
Sand (S): fineness modulus 2.8, clay content is less than 1%, Xiamen Wan Xiangtong Industrial Co., Ltd.；Stone (G): 5-25mm
Graded broken stone, Xiamen is along building materials Co., Ltd of heap of stone；
Test water (W): tap water meets the regulation of JGJ 63-2006 " concrete water standard ".Performance test uses
Concrete mix be shown in Table 2, performance test data is shown in Table 3.
2 concrete mix of table
| Raw material | C | FA | SL | S | G | W |
| Dosage/(kg/m3) | 360 | 40 | 60 | 780 | 1020 | 160 |
3 concrete test performance of table
From the performance test data of table 3, it can be seen that technical solution of the present invention has the effect of obvious viscosity reduction.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, therefore, as long as with this
Any modifications, equivalent replacements, and improvements made by description of the invention content etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of preparation method of block viscosity reduction type concrete admixture, characterized by the following steps:
By weight:
150-180 parts of unsaturated polyether lists are added in the reaction kettle with thermostat, agitating device, Dropping feeder and nitrogen tube
A, 2-8 parts of unsaturated polyether monomer B, 2-6 part methyl methacrylates of body, 5-15 parts of acrylic acid, 0.5-1.5 parts of unsaturated fluorinations
Close object, 0.8-1.8 parts of complex reducing agents, 0.5-1.5 parts of chain-transferring agents and 100-130 parts of deionized waters；
Start the agitating device to be stirred, the thermostat after material is completely dissolved, adds controlled at 30-40 DEG C
Enter 1-5 parts of hydrogen peroxide, continues to stir 30min, then stop stirring；
It after 2-6h, is again started up the agitating device and is stirred, and 1-5 parts of unsaturated polyethers are added into the reaction kettle
B, 5-10 parts of unsaturated polyether monomer C, 1-2 part hydroxymethyl acrylamide of monomer, 1-2 parts of hydrogen peroxide and 30 parts of deionized waters；
Then it is heated to 50-60 DEG C, starts to be added dropwise with the Dropping feeder by 2-5 parts of acrylic acid, 1-4 parts of methacryls
The mixed solution I that oxy-ethyl-trimethyl salmiac, 1-5 part unsaturated amino compounds and 30 parts of deionized waters are configured to, and
The mixed solution II being configured to by 0.2-0.5 parts of complex reducing agents, 0.1-0.5 parts of chain-transferring agents and 30 parts of deionized waters, it is described
Mixed solution I and the mixed solution II should be added dropwise in 0.5-1.5h, to the mixed solution I and the mixed solution
II be added dropwise to complete after again into the reaction kettle be added 0.5-1 part oxidants, then heat preservation 1h after cool, drop can be obtained
Viscous type concrete admixture.
2. a kind of preparation method of block viscosity reduction type concrete admixture as described in claim 1, it is characterised in that: described
Unsaturated polyether monomer A includes such as flowering structure (a):
H(OCH2CH2)p(OCH2CH2CH2)qOCH2CH2CR1=CH2 (a)
Wherein, p is integer, and 40≤p≤50；Q is integer, and 1≤q≤2；R1For H or CH3。
3. a kind of preparation method of block viscosity reduction type concrete admixture as described in claim 1, it is characterised in that: described
Unsaturated polyether monomer B includes such as flowering structure (b):
H(OCH2CH2)m(OCH2CH2CH2)nO(CH2)xO(C6H4)(CH2)yCR2=CH2 (b)
Wherein, m is integer, and 25≤m≤30；N is integer, and 2≤n≤4；X and y is integer greater than 0, and 2≤x+y≤4；
R2For H or CH3。
4. a kind of preparation method of block high dispersive type concrete admixture as described in claim 1, it is characterised in that: described
Unsaturated fluorine compounds be one of 2- perfluoroalkyl acrylate, 2- fluoroacrylic methyl ester, 2- fluoroethyl acrylate.
5. a kind of preparation method of block viscosity reduction type concrete admixture as described in claim 1, it is characterised in that: described
Complex reducing agent by weight, has following composition:
2- hydroxyl -2- sulfinatoacetic acid disodium salt: 10-30%；
2- hydroxyl -2- sulfonatoacetic acid disodium salt: 5-15%；
L-AA: 35-45%；
It is a kind of in sodium dithionite, potassium hyposulfite or zinc dithionite: 20-30%；
It is a kind of in sodium carbonate, sodium bicarbonate, potassium carbonate or saleratus: 5-15%.
6. a kind of preparation method of block viscosity reduction type concrete admixture as described in claim 1, it is characterised in that: described
Chain-transferring agent is one of thioacetic acid, mercaptopropionic acid, mercaptoethanol.
7. a kind of preparation method of block viscosity reduction type concrete admixture as described in claim 1, it is characterised in that: described
Unsaturated polyether monomer C includes such as flowering structure (c):
CH3O(CH2CH2O)h(CH2CH2CH2O)kCH2CH2OOCH2CR3=CH2 (c)
Wherein, h is integer, and 35≤h≤50；K is integer, and 1≤k≤3；R3For H or CH3。
8. a kind of preparation method of block viscosity reduction type concrete admixture as described in claim 1, it is characterised in that: described
Unsaturated amino compounds areD- allylglycine、2- amino -4- methyl -4- penetenoic acid、2- amino -3-butenoic acid, 2- ammonia
One of base -5- hexenoic acid.
9. a kind of preparation method of block viscosity reduction type concrete admixture as described in claim 1, it is characterised in that: described
Oxidant is one of hydrogen peroxide, ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate.
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| CN113416282A (en) * | 2021-08-12 | 2021-09-21 | 石家庄市长安育才建材有限公司 | Concrete black paste inhibitor and preparation method thereof |
| CN113754361A (en) * | 2021-08-21 | 2021-12-07 | 徐振江 | Method for manufacturing viscosity-reducing concrete |
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