CN109021182A - Polycarboxylate water-reducer and its preparation method and application from environment-friendly tasteless raw material - Google Patents
Polycarboxylate water-reducer and its preparation method and application from environment-friendly tasteless raw material Download PDFInfo
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- CN109021182A CN109021182A CN201811002003.3A CN201811002003A CN109021182A CN 109021182 A CN109021182 A CN 109021182A CN 201811002003 A CN201811002003 A CN 201811002003A CN 109021182 A CN109021182 A CN 109021182A
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- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 69
- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 52
- 230000009967 tasteless effect Effects 0.000 title claims abstract description 38
- 239000002994 raw material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 60
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 42
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 27
- 229920000570 polyether Polymers 0.000 claims abstract description 19
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 17
- 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 15
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 15
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims abstract description 15
- JPAOMENBKRZQDR-UHFFFAOYSA-N CC=CC.[Na] Chemical compound CC=CC.[Na] JPAOMENBKRZQDR-UHFFFAOYSA-N 0.000 claims abstract description 14
- VYGBQXDNOUHIBZ-UHFFFAOYSA-L sodium formaldehyde sulphoxylate Chemical compound [Na+].[Na+].O=C.[O-]S[O-] VYGBQXDNOUHIBZ-UHFFFAOYSA-L 0.000 claims abstract description 14
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 13
- 229920000056 polyoxyethylene ether Polymers 0.000 claims abstract description 12
- 229940051841 polyoxyethylene ether Drugs 0.000 claims abstract description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 9
- 239000011734 sodium Substances 0.000 claims abstract description 9
- -1 sodium hypophosphites Chemical class 0.000 claims abstract description 9
- QYKIQEUNHZKYBP-UHFFFAOYSA-N Vinyl ether Chemical compound C=COC=C QYKIQEUNHZKYBP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000007613 environmental effect Effects 0.000 claims abstract description 5
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229960000834 vinyl ether Drugs 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 29
- 238000006116 polymerization reaction Methods 0.000 claims description 26
- 239000004568 cement Substances 0.000 claims description 24
- 239000004567 concrete Substances 0.000 claims description 16
- 239000007787 solid Substances 0.000 claims description 13
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 12
- 239000000654 additive Substances 0.000 claims description 12
- 230000000996 additive effect Effects 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- 230000000694 effects Effects 0.000 claims description 9
- 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 8
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 8
- 150000007513 acids Chemical class 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000013019 agitation Methods 0.000 claims description 6
- 230000003467 diminishing effect Effects 0.000 claims description 5
- 230000003020 moisturizing effect Effects 0.000 claims description 5
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000005553 drilling Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 239000004289 sodium hydrogen sulphite Substances 0.000 claims description 4
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 4
- 230000015271 coagulation Effects 0.000 claims 1
- 238000005345 coagulation Methods 0.000 claims 1
- 239000002002 slurry Substances 0.000 claims 1
- 239000002689 soil Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 7
- 238000010276 construction Methods 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 description 12
- 238000003786 synthesis reaction Methods 0.000 description 12
- 239000000843 powder Substances 0.000 description 11
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000003756 stirring Methods 0.000 description 6
- 239000007788 liquid Substances 0.000 description 3
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 125000005395 methacrylic acid group Chemical group 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Natural products OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 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 description 1
- 230000035484 reaction time Effects 0.000 description 1
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- KEAYESYHFKHZAL-IGMARMGPSA-N sodium-23 atom Chemical compound [23Na] KEAYESYHFKHZAL-IGMARMGPSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C 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
- 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
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/163—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/165—Macromolecular compounds comprising sulfonate or sulfate groups obtained by reactions only involving carbon-to-carbon unsaturated bonds containing polyether side chains
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
Abstract
This application involves a kind of polycarboxylate water-reducers from environment-friendly tasteless raw material, it is counted on the basis of parts by weight, it is made of following raw materials: 100 parts of unsaturated polyethers, 8~24 parts of acrylic acid, 1~6 part of methylpropene sodium sulfonate, 0.6~3.0 part of ammonium persulfate, 1.0~2.0 parts of hydrogen peroxide, 0.6~1.0 part of L-AA, 0.2~0.7 part of E51, 0.3~0.9 part of sodium formaldehyde sulphoxylate, 1.5~7.5 parts of sodium hypophosphites and 123~294 parts of water, the number-average molecular weight of the unsaturated polyether is 2000~3000, it and is one or more of following: methyl allyl polyoxyethylene ether, methyl alkene butyl polyoxyethylene ether or glycol divinyl ether polyoxyethylene ether.The application further relates to the preparation method and application method and application in construction projects of the polycarboxylate water-reducer.The polycarboxylate water-reducer preparation process of the application is simple, easy to operate, has good initial flow degree and good slump retaining, has significant economic benefit, social benefit and environmental benefit.
Description
Technical field
This application involves building material technical fields, and in particular to a kind of polycarboxylic acids diminishing from environment-friendly tasteless raw material
Agent, the preparation method of the polycarboxylate water-reducer from environment-friendly tasteless raw material, the polycarboxylic acids from environment-friendly tasteless raw material
The application method of water-reducing agent and the polycarboxylate water-reducer from environment-friendly tasteless raw material to concrete initial flow degree and
Protect the application in the high architectural engineering of effect requirements of collapsing.
Background technique
Poly carboxylic acid series water reducer has multiple charged groups, and side chain band due to its unique comb-type structure that is, on main chain
There is hydrophilic active group, thus plays the effect of disperse cement particles.Low with volume, water-reducing rate is high, the slump through when
Lose the advantages that small, it has also become current most popular cement water reducing agent.Recently as country to environmentally protective weight
Depending on and each manufacturing enterprise for energy-saving and emission-reduction and shorten the production cycle, the demand improved efficiency, by conventional high-temperature reaction synthesize
Polyacids acid water-reducing agent, also develops room temperature synthetic method successively, but the conventional small powder used such as mercaptopropionic acid, thioacetic acid, sulfydryl
Ethyl alcohol etc. has strong sulphide smell, and especially during the broiling summer, smell more allows people to be difficult to endure.
For this purpose, there is an urgent need in the art to develop a kind of polycarboxylate water-reducer and preparation method thereof from environment-friendly tasteless raw material
And application.
Summary of the invention
The application's is designed to provide a kind of polycarboxylate water-reducer from environment-friendly tasteless raw material, to solve above-mentioned skill
Art problem.Specifically, the polycarboxylate water-reducer of the application does not include the molecular weight regulator based on sulfydryl, but by environment-friendly tasteless
Molecular weight regulator and other components be made.The tasteless environmentally friendly small powder of the application, meets the trend of Green Chemistry, can be in room temperature
Into the wide temperature range of high temperature, short time rapid synthesis polyacids acid water-reducing agent, and product has water-reducing rate high, and it is good to protect effect of collapsing
Good feature.Enterprises production efficiency not only can be improved, reduce production energy consumption and production cost, and due to its synthesis temperature model
Width is enclosed, the production requirement of different enterprises can be met, had a good application prospect.The polycarboxylate water-reducer preparation process of the application
Simply, easy to operate, synthesis cycle is short, and has good initial flow degree and good slump retaining, has significant economical
Benefit, social benefit and environmental benefit.
The application also provides a kind of method for preparing the polycarboxylate water-reducer as described above from environment-friendly tasteless raw material.
The application also provides a kind of application method of polycarboxylate water-reducer from environment-friendly tasteless raw material as described above.
The application also provides one kind and is originated from the polycarboxylate water-reducer of environment-friendly tasteless raw material as described above at the beginning of concrete
Beginning fluidity and guarantor are collapsed the application in the high architectural engineering of effect requirements.
To achieve the goals above, the application provides following technical proposals.
In the first aspect, the application provides a kind of polycarboxylate water-reducer from environment-friendly tasteless raw material, with parts by weight
On the basis of count, be made of following raw materials: 100 parts of unsaturated polyethers, 8~24 parts of acrylic acid, 1~6 part of methylpropene sodium sulfonate,
0.6~3.0 part of ammonium persulfate, 1.0~2.0 parts of hydrogen peroxide, 0.6~1.0 part of L-AA, 0.2~0.7 part of E51 (mainly at
Be divided into: sodium formaldehyde sulphoxylate, sodium carbonate are purchased from Shanghai Ying Luosha Chemical Industry Science Co., Ltd), 0.3~0.9 part of formaldehyde closes
Sodium bisulphite, 1.5~7.5 parts of sodium hypophosphites and 123~294 parts of water, the number-average molecular weight of the unsaturated polyether are
2000~3000, and the unsaturated polyether is one or more of following: methyl allyl polyoxyethylene ether, methyl alkene fourth
Base polyoxyethylene ether or glycol divinyl ether polyoxyethylene ether.
It is noted that in this application, the dosage of the sodium formaldehyde sulphoxylate (also known as sodium formaldehyde sulfoxylate) does not include in E51
The dosage of sodium formaldehyde sulphoxylate.
In a kind of embodiment of first aspect, the polycarboxylate water-reducer from environment-friendly tasteless raw material is free of and is based on
The molecular weight regulator of sulfydryl.
In a kind of embodiment of first aspect, the concentration of hydrogen peroxide is 30wt% in the hydrogen peroxide；
And/or the dosage of the acrylic acid is 10~18 parts；
And/or the dosage of the methylpropene sodium sulfonate is 2~5 parts；
And/or the dosage of the ammonium persulfate is 1.0~2.2 parts；
And/or the dosage of the hydrogen peroxide is 1.3~1.7 parts；
And/or the dosage of the L-AA is 0.6~0.9 part；
And/or the dosage of the E51 is 0.4~0.7 part；
And/or the dosage of the sodium formaldehyde sulphoxylate is 0.5~0.7 part；
And/or the dosage of the sodium hypophosphite is 2.0~6.0 parts；
And/or the dosage of the water is 125~234 parts, above-mentioned part is all parts by weight.
In a kind of embodiment of first aspect, the solid content of the polycarboxylate water-reducer is
30wt%~50wt%, preferably 50wt%.
In second aspect, the application provides a kind of poly- carboxylic from environment-friendly tasteless raw material prepared as described in relation to the first aspect
The method of sour water-reducing agent, the method includes under agitation, ammonium persulfate being added into mixture A, solution is then added dropwise
B, solution C, solution D carry out polymerization reaction, and after curing predetermined amount of time, water use regulation to required solid content obtains described be originated from
The polycarboxylate water-reducer of environment-friendly tasteless raw material；
Wherein, the mixture A is mixed to get by unsaturated polyether, sodium hypophosphite and water；
Wherein, the solution B is mixed to get by L-AA, E51, sodium formaldehyde sulphoxylate and water；
Wherein, the solution C is mixed to get by hydrogen peroxide and water；
Wherein, the solution D is mixed to get by acrylic acid, methylpropene sodium sulfonate and water.
In a kind of embodiment of second aspect, the solid content of the polycarboxylate water-reducer is 30wt%~50wt%,
Preferably 50wt%.
In a kind of embodiment of second aspect comprising following step:
(1) mixture A is put into polymerization reaction kettle, is stirred evenly, be heated to 25~70 DEG C, spare, wherein institute
Mixture A is stated to be mixed by 100 parts by weight unsaturated polyethers, 1.5~7.5 parts by weight sodium hypophosphites and 50~80 parts by weight water
It arrives；
(2) under agitation, 0.6~3.0 parts by weight ammonium persulfate is added into mixture A；
(3) it is stirred 10 minutes after ammonium persulfate being added, dropwise addition solution B, solution C and solution D into mixture A, while into
Row polymerization reaction, polymeric reaction temperature are 25 DEG C~70 DEG C；
(4) after solution B, solution C and solution D are added dropwise, 25~70 DEG C of heat preservations is continued at and carry out polymerization reaction 30~150
Minute；
(5) solid content is adjusted with 18~194 parts by weight water to be uniformly mixed to 30wt%~50wt%, obtain described from ring
Protect the polycarboxylate water-reducer of tasteless raw material；
Wherein, in step (3), solution B is dripped off in 40~200 minutes, and solution C is dripped off in 35~190 minutes, molten
Liquid D is dripped off in 30~180 minutes；
Wherein, solution B is by 0.0~1.0 parts by weight L-AA, 0.0~0.7 parts by weight E51,0.0~0.9 parts by weight
Sodium formaldehyde sulphoxylate and 12~23 parts by weight water are mixed to get；
Wherein, solution C is mixed to get by 1.0~2.0 parts by weight hydrogen peroxide and 8~20 parts by weight water；
Wherein, solution D is by 8~24 parts by weight of acrylic acid, 1~6 parts by weight methylpropene sodium sulfonate and 5~13 parts by weight water
It is mixed to get；And
Wherein, total dosage of water described in mixture A, solution B, solution C and solution D is 100~107 parts by weight.
In a kind of embodiment of second aspect, mixture A, solution B, solution C, water and step (5) described in solution D
In after moisturizing total dosage be 123~294 parts by weight, preferably 125~234 parts by weight.
In a kind of embodiment of second aspect, in step (3), solution B, solution C and solution D are respectively from different
It is added drop-wise in polymerization reaction kettle in head tank.
In a kind of embodiment of second aspect, in step (3) and (4), the temperature of the polymerization reaction is 35 DEG C
~60 DEG C.
In a kind of embodiment of second aspect, in step (3), the time for adding of the solution B is 40~140 points
Clock；
And/or the time for adding of the solution C is 35~130 minutes；
And/or the time for adding of the solution D is 30~120 minutes.
In a third aspect, the application provides the polycarboxylic acids from environment-friendly tasteless raw material of one kind as described in relation to the first aspect and subtracts
The application method of aqua, the application method include that the polycarboxylate water-reducer is added in cement paste；Alternatively, will be described
Polycarboxylate water-reducer is added in concrete.
In a kind of embodiment of the third aspect, when the polycarboxylate water-reducer is added in cement paste, institute
The additive amount for stating polycarboxylate water-reducer is the 0.30wt% of cement weight.
It is described when the polycarboxylate water-reducer to be added in concrete in a kind of embodiment of the third aspect
The additive amount of polycarboxylate water-reducer is the 0.40wt% of cement weight.
In fourth aspect, the application provides the polycarboxylic acids from environment-friendly tasteless raw material of one kind as described in relation to the first aspect and subtracts
Application of the aqua in the high architectural engineering of effect requirements of collapsing to concrete initial flow degree and guarantor.
In a kind of embodiment of fourth aspect, the architectural engineering includes high-rise, Longspan Bridge, ocean
Drilling platforms, tunnel, dam or airport.
Compared with prior art, the beneficial effects of the present application are as follows:
(1) the present invention provides a kind of poly carboxylic acid series water reducers, have water-reducing rate high, and guarantor, which is collapsed, to work well.It is colourless
To light yellow transparent liquid, solid content is 30wt%~50wtwt%.When adding for the polycarboxylate water-reducer described in cement paste
When dosage is the 0.30% of cement weight, can make the cement paste initial flow degree of the ratio of mud 0.29 is 255mm~275mm, 1
Hour fluidity is maintained at 225mm~255mm.When the additive amount of the water-reducing agent described in concrete is the 0.40% of cement weight
When, fresh concrete initial slump is good, and divergence is big, and water-reducing rate is high, and 1h keeps also preferable, can be improved concrete water conservation
Property, suitable for collapsing demanding architectural engineering to the initial diminishing of concrete and protecting.
(2) the preparation method simple process of poly carboxylic acid series water reducer of the present invention, easy to operate, synthesis cycle is short, energy conservation drop
Consumption is conducive to large-scale industrial production.
(3) sodium hypophosphite small powder involved in the preparation method of poly carboxylic acid series water reducer of the present invention, the tasteless environmental protection of the small powder,
And reaction is helped speed up, shorten the reaction time, improves reaction efficiency.
(4) present invention is for the production of additive factory, have cost of material is low, performance is good, one-step polymerization and obtain etc. excellent
Point, suitable for initial diminishing, protect collapse demanding high-rise, Longspan Bridge, marine drilling platform, tunnel, dam,
In the engineerings such as airport construction.
Specific embodiment
Term "comprising", " comprising ", " having " and their derivative are not excluded for any other component, step or mistake
The presence of journey, and whether disclose in this application with these other components, step or process unrelated.To eliminate any query,
Unless expressly stated, otherwise in the application it is all use term "comprising"s, " comprising ", or " having " composition may include appoint
What additional additive, auxiliary material or compound.On the contrary, in addition to necessary to operating characteristics those, term " substantially by ...
Composition " excludes any other component, step or process except the hereinafter described range of any term.Term " by ...
Composition " does not include any component, step or the process for not specifically describing or listing.Unless expressly stated, otherwise term "or" refers to
Separate member listed or any combination thereof.
In a specific embodiment, this application provides a kind of polycarboxylic acids diminishings of tasteless environmentally friendly small powder rapid synthesis
Agent is made by raw material, and raw material includes following component in parts by weight: 100 parts of unsaturated polyethers, 8~24 parts of acrylic acid,
1~6 part of methylpropene sodium sulfonate, 0.6~3.0 part of ammonium persulfate, 1.0~2.0 parts of hydrogen peroxide, 0.6~1.0 part of L- Vitamin C
Acid, 0.2~0.7 part of E51,0.3~0.9 part of sodium formaldehyde sulphoxylate, 1.5~7.5 parts of sodium hypophosphites and 123~294 parts
Water, the unsaturated polyether are methacrylic/methyl alkene butyl/glycol divinyl ether polyoxyethylene ether, number-average molecular weight
It is 2000~3000.
In the present invention, the methacrylic/methyl alkene butyl/glycol divinyl ether polyoxyethylene ether is commercially available production
Product are preferably provided by Shanghai Dongda Chemical Co., Ltd..The molecular weight of the unsaturated polyether is preferably 2000~
3000.The unsaturated polyether forms side chain in the course of the polymerization process, generates steric hindrance effect, prevents cement granules from agglomerating,
Keep dispersibility.With acrylic acid, methylpropene sodium sulfonate etc. polymerization reaction can occur for unsaturated polyether, introduce carboxyl and amino.
Ammonium persulfate, hydrogen peroxide and L-AA, E51, sodium formaldehyde sulphoxylate form redox system, as initiator,
Each monomer is set to participate in polymerization reaction.Sodium hypophosphite is as chain-transferring agent, the molecular weight of control synthesis water-reducing agent.
Wherein, the concentration of hydrogen peroxide is this field normal concentration, generally 30wt% in the hydrogen peroxide.
Wherein, the dosage of the acrylic acid is preferably 10~18 parts.The dosage of the methylpropene sodium sulfonate is preferably
It is 2~5 parts.The dosage of the ammonium persulfate is preferably 1.0~2.2 parts.The dosage of the hydrogen peroxide is preferably 1.3~
1.7 part.The dosage of the L-AA is preferably 0.6~0.9 part.The dosage of the E51 is preferably 0.4~0.7 part.
The dosage of the sodium formaldehyde sulphoxylate is preferably 0.5~0.7 part.The dosage of the sodium hypophosphite is preferably 2.0
~6.0 parts.The dosage of the water is preferably 125~234 parts.Above-mentioned part is all parts by weight.
In the present invention, the solid content of the polycarboxylate water-reducer of the tasteless environmentally friendly small powder rapid synthesis of described one kind is preferably
30wt%~50wt% is more preferably 50wt%.
The present invention also provides the preparation method of the polycarboxylate water-reducer of the tasteless environmentally friendly small powder rapid synthesis of described one kind,
Include the following steps: under agitation, ammonium persulfate to be added into mixture A, solution B, solution C, solution D be then added dropwise,
Polymerization reaction is carried out, after curing a period of time, water use regulation to solid content is 30wt%~50wt%, as a kind of tasteless environmental protection
The polycarboxylate water-reducer of small powder rapid synthesis；
The mixture A is mixed to get by unsaturated polyether, sodium hypophosphite and water；
The solution B is mixed to get by L-AA, E51, sodium formaldehyde sulphoxylate and water；
The solution C is mixed to get by hydrogen peroxide and water；
The solution D is mixed to get by acrylic acid, methylpropene sodium sulfonate and water.
Preferably, the preparation method of the polycarboxylate water-reducer of the tasteless environmentally friendly small powder rapid synthesis of described one kind comprising under
State step:
(1) by mixture A:100 parts by weight unsaturated polyether, 1.5~7.5 parts by weight sodium hypophosphites and 50~80 weight
Part water puts into polymerization reaction kettle, stirs evenly, and is heated to 25~70 DEG C, spare；
(2) under agitation, 0.6~3.0 parts by weight ammonium persulfate is added into mixture A；
(3) it is stirred 10 minutes after ammonium persulfate being added, dropwise addition solution B, solution C and solution D into mixture A, while into
Row polymerization reaction, polymeric reaction temperature are 25 DEG C~70 DEG C；Wherein, solution B is dripped off in 40~200 minutes, solution C in 35~
It is dripped off in 190 minutes；Solution D is dripped off in 30~180 minutes；Solution B includes 0.0~1.0 parts by weight L-AA, 0.0
~0.7 parts by weight E51,0.0~0.9 parts by weight of formaldehyde close sodium bisulphite and 12~23 parts by weight water, and solution C includes 1.0~
2.0 parts by weight hydrogen peroxide and 8~20 parts by weight water, solution D include 8~24 parts by weight of acrylic acid, 1~6 parts by weight metering system
Sodium sulfonate and 5~13 parts by weight water；Total dosage of water described in mixture A, solution B, solution C and solution D is 100~107 weights
Measure part；
(4) after being added dropwise, 25~70 DEG C of heat preservations is continued at and are carried out polymerization reaction 30~150 minutes；
(5) it is uniformly mixed with 18~194 parts by weight water adjusting solid content to 30wt%~50wt%；
Wherein, in mixture A, solution B, solution C, water described in solution D and step (5) after total dosage of moisturizing be 123
~294 parts by weight.
Wherein, in water described in mixture A, solution B, solution C and solution D and step (5) after moisturizing total dosage it is preferable
Ground is 125~234 parts by weight.
In step (3), solution B is preferably added drop-wise in polymerization reaction kettle from a third head tank.
In step (3), solution C is preferably added drop-wise in polymerization reaction kettle from one second head tank.
In step (3), solution D is preferably added drop-wise in polymerization reaction kettle from one first head tank.
In step (3) and (4), the temperature of the polymerization reaction is preferably 35 DEG C~60 DEG C.
In step (3), the time for adding of the solution B is preferably 40~140 minutes.The time for adding of the solution C
Preferably 35~130 minutes.The time for adding of the solution D is preferably 30~120 minutes.
In step (3), there is no particular/special requirement for the speed of the stirring, as long as solution B, solution C and solution D can be made
It is uniformly mixed with mixture A.
The present invention also provides the application method of the polycarboxylate water-reducer of the tasteless environmentally friendly small powder rapid synthesis of described one kind,
Are as follows: the polycarboxylate water-reducer is added in cement paste, the additive amount of the polycarboxylate water-reducer is cement weight
0.30wt%；Or are as follows: the polycarboxylate water-reducer is added in concrete, the additive amount of the polycarboxylate water-reducer is cement
The 0.40wt% of weight.
Poly carboxylic acid series water reducer of the present invention is suitable for high-rise, Longspan Bridge, marine drilling platform, tunnel
Road, dam or airport etc. are to concrete initial flow degree and protect in the high architectural engineering of effect requirements of collapsing.
On the basis of common knowledge of the art, above-mentioned each optimum condition, can any combination to get each preferable reality of the application
Example.
Reagent and raw material used herein are commercially available.
Embodiment
Below in conjunction with embodiments herein, clear and complete description is carried out to the technical solution of the application, but simultaneously
Therefore the invention is limited to the scope of the described embodiments.Unless otherwise instructed, reagent used and raw material all may be used
It is bought by commercial sources.
Embodiment 1
(1) prepare before polymerization:
The preparation of mixture A: the methyl allyl polyoxyethylene ether and 50 that 100 parts by weight average molecular weights are 2400 is weighed
Parts by weight water, 1.5 parts of sodium hypophosphites put into polymerization reaction kettle, stir evenly, and 25 DEG C of holding is spare；
The preparation of solution B: 1.0 parts by weight L-AAs are weighed, 0.9 parts by weight of formaldehyde closes sodium bisulphite and 23 weight
Part water, stirs evenly, standby to be added dropwise；
The preparation of solution C: weighing 2.0 parts by weight hydrogen peroxide, 20 parts by weight water, stir evenly, standby to be added dropwise；
The preparation of solution D: weighing 24 parts by weight of acrylic acid and 1 parts by weight methylpropene sodium sulfonate, standby to be added dropwise；
(2) polymerize: step (1) has put into the polymerization reaction kettle of mixture A, starts stirring, and temperature is stablized at 25 DEG C, together
When solution B, solution C and solution D is added dropwise, control rate of addition, solution B was dripped off in 70 minutes, and solution C was dripped off in 65 minutes, molten
Liquid D was dripped off in 60 minutes；After being added dropwise, continue heat preservation polymerization reaction 150 minutes；
(3) moisturizing afterwards: poly carboxylic acid series water reducer can be quickly made in 91 parts by weight water of addition adjusting solid content to 40%.
Embodiment 1 is added to cement paste using a kind of poly carboxylic acid series water reducer that tasteless environmentally friendly small powder is quickly prepared
In, additive amount is the 0.30% of cement weight, the cement paste initial flow degree of the ratio of mud 0.29 can be made to reach 260mm, 1 is small
When fluidity be maintained at 225mm.It is added in concrete, additive amount is the 0.40% of cement weight, and initial slump is
180mm, initial extension degree are 470mm, and the slump is maintained at 160mm within 1 hour.
Embodiment 2~5
The preparation method of embodiment 2~5 is same as Example 1, and difference specifically marks in table 1 below.
Effect example 1
According to the method and steps of Examples 1 to 5, by the poly carboxylic acid series water reducer of rapid synthesis according to the formula in table 1, and root
Obtained poly carboxylic acid series water reducer is added in cement paste and concrete by identical volume according to additive amount shown in table 1,
The performance data of gained cement paste and concrete is equally shown in Table 1.Wherein, contrast sample 1 is that commercially available conventional polycarboxylic-acid subtracts
Aqua TJ-188, contrast sample 2 be by being accordingly formulated in table 1, using common molecular weight regulator mercaptopropionic acid and at poly- carboxylic
Sour based water reducer.
The raw material of 1 Examples 1 to 5 of table, experiment condition and and performance data of the contrast sample under 0.40wt% volume
Compare
The above-mentioned description to embodiment is that this Shen can be understood and applied for the ease of those skilled in the art
Please.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiments without paying creative labor.Therefore, the application is not limited to implementation here
Example, those skilled in the art make according to herein disclosed content in the case where not departing from the application scope and spirit
It improves and modifies within all scope of the present application.
Claims (16)
1. a kind of polycarboxylate water-reducer from environment-friendly tasteless raw material, is counted on the basis of parts by weight, it is made of following raw materials:
100 parts of unsaturated polyethers, 8~24 parts of acrylic acid, 1~6 part of methylpropene sodium sulfonate, 0.6~3.0 part of ammonium persulfate, 1.0~
2.0 parts of hydrogen peroxide, 0.6~1.0 part of L-AA, 0.2~0.7 part of E51,0.3~0.9 part of sodium formaldehyde sulphoxylate, 1.5
~7.5 parts of sodium hypophosphites and 123~294 parts of water, the number-average molecular weight of the unsaturated polyether are 2000~3000, and described
Unsaturated polyether is one or more of following: methyl allyl polyoxyethylene ether, methyl alkene butyl polyoxyethylene ether or
Glycol divinyl ether polyoxyethylene ether.
2. being originated from the polycarboxylate water-reducer of environment-friendly tasteless raw material as described in claim 1, which is characterized in that described to be originated from environmental protection
The polycarboxylate water-reducer of tasteless raw material is free of the molecular weight regulator based on sulfydryl.
3. being originated from the polycarboxylate water-reducer of environment-friendly tasteless raw material as described in claim 1, which is characterized in that in the hydrogen peroxide
The concentration of hydrogen peroxide is 30wt%；
And/or the dosage of the acrylic acid is 10~18 parts；
And/or the dosage of the methylpropene sodium sulfonate is 2~5 parts；
And/or the dosage of the ammonium persulfate is 1.0~2.2 parts；
And/or the dosage of the hydrogen peroxide is 1.3~1.7 parts；
And/or the dosage of the L-AA is 0.6~0.9 part；
And/or the dosage of the E51 is 0.4~0.7 part；
And/or the dosage of the sodium formaldehyde sulphoxylate is 0.5~0.7 part；
And/or the dosage of the sodium hypophosphite is 2.0~6.0 parts；
And/or the dosage of the water is 125~234 parts, above-mentioned part is all parts by weight.
4. being originated from the polycarboxylate water-reducer of environment-friendly tasteless raw material as described in claim 1, which is characterized in that the polycarboxylic acids subtracts
The solid content of aqua is 30wt%~50wt%, preferably 50wt%.
5. a kind of method for preparing the polycarboxylate water-reducer as described in claim 1 from environment-friendly tasteless raw material, the method
Including under agitation, ammonium persulfate being added into mixture A, solution B, solution C, solution D is then added dropwise, polymerize anti-
It answers, after curing predetermined amount of time, water use regulation to required solid content obtains the polycarboxylic acids diminishing for being originated from environment-friendly tasteless raw material
Agent；
Wherein, the mixture A is mixed to get by unsaturated polyether, sodium hypophosphite and water；
Wherein, the solution B is mixed to get by L-AA, E51, sodium formaldehyde sulphoxylate and water；
Wherein, the solution C is mixed to get by hydrogen peroxide and water；
Wherein, the solution D is mixed to get by acrylic acid, methylpropene sodium sulfonate and water.
6. method as claimed in claim 5, which is characterized in that the solid content of the polycarboxylate water-reducer be 30wt%~
50wt%, preferably 50wt%.
7. method as claimed in claim 5, which is characterized in that it includes the following steps:
(1) mixture A is put into polymerization reaction kettle, is stirred evenly, be heated to 25~70 DEG C, it is spare, wherein described mixed
Object A is closed to be mixed to get by 100 parts by weight unsaturated polyethers, 1.5~7.5 parts by weight sodium hypophosphites and 50~80 parts by weight water；
(2) under agitation, 0.6~3.0 parts by weight ammonium persulfate is added into mixture A；
(3) it is stirred 10 minutes after ammonium persulfate being added, solution B, solution C and solution D is added dropwise into mixture A, while being gathered
Reaction is closed, polymeric reaction temperature is 25 DEG C~70 DEG C；
(4) after solution B, solution C and solution D are added dropwise, 25~70 DEG C of heat preservations is continued at and carry out 30~150 points of polymerization reaction
Clock；
(5) solid content is adjusted with 18~194 parts by weight water to be uniformly mixed to 30wt%~50wt%, obtain described from environmentally friendly nothing
The polycarboxylate water-reducer of taste raw material；
Wherein, in step (3), solution B is dripped off in 40~200 minutes, and solution C is dripped off in 35~190 minutes, solution D
It is dripped off in 30~180 minutes；
Wherein, solution B is by 0.0~1.0 parts by weight L-AA, 0.0~0.7 parts by weight E51,0.0~0.9 parts by weight of formaldehyde
It closes sodium bisulphite and 12~23 parts by weight water is mixed to get；
Wherein, solution C is mixed to get by 1.0~2.0 parts by weight hydrogen peroxide and 8~20 parts by weight water；
Wherein, solution D is mixed by 8~24 parts by weight of acrylic acid, 1~6 parts by weight methylpropene sodium sulfonate and 5~13 parts by weight water
It obtains；And
Wherein, total dosage of water described in mixture A, solution B, solution C and solution D is 100~107 parts by weight.
8. the method for claim 7, which is characterized in that mixture A, solution B, solution C, water and step described in solution D
Suddenly total dosage of rear moisturizing is 123~294 parts by weight, preferably 125~234 parts by weight in (5).
9. the method for claim 7, which is characterized in that in step (3), solution B, solution C and solution D difference are never
It is added drop-wise in polymerization reaction kettle in same head tank.
10. the method for claim 7, which is characterized in that in step (3) and (4), the temperature of the polymerization reaction is
35 DEG C~60 DEG C.
11. the method for claim 7, which is characterized in that in step (3), the time for adding of the solution B is 40~
140 minutes；
And/or the time for adding of the solution C is 35~130 minutes；
And/or the time for adding of the solution D is 30~120 minutes.
12. a kind of application method of the polycarboxylate water-reducer from environment-friendly tasteless raw material as described in claim 1, the use
Method includes that the polycarboxylate water-reducer is added in cement paste；Alternatively, the polycarboxylate water-reducer is added to coagulation
In soil.
13. application method as claimed in claim 12, which is characterized in that net when the polycarboxylate water-reducer is added to cement
When in slurry, the additive amount of the polycarboxylate water-reducer is the 0.30wt% of cement weight.
14. application method as claimed in claim 12, which is characterized in that when the polycarboxylate water-reducer is added to concrete
When middle, the additive amount of the polycarboxylate water-reducer is the 0.40wt% of cement weight.
15. a kind of polycarboxylate water-reducer from environment-friendly tasteless raw material as described in claim 1 is to concrete initial flow
Spend and protect the application in the high architectural engineering of effect requirements of collapsing.
16. application as claimed in claim 15, which is characterized in that the architectural engineering includes high-rise, long-span bridge
Beam, marine drilling platform, tunnel, dam or airport.
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