CN103724567A - Reduced water reducing agent and synthesis method thereof - Google Patents
Reduced water reducing agent and synthesis method thereof Download PDFInfo
- Publication number
- CN103724567A CN103724567A CN201310749205.5A CN201310749205A CN103724567A CN 103724567 A CN103724567 A CN 103724567A CN 201310749205 A CN201310749205 A CN 201310749205A CN 103724567 A CN103724567 A CN 103724567A
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- CN
- China
- Prior art keywords
- reduced
- reducing agent
- type water
- water reducing
- water reducer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 20
- 238000001308 synthesis method Methods 0.000 title 1
- 239000000203 mixture Substances 0.000 claims abstract description 9
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 claims abstract description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 6
- CNCOEDDPFOAUMB-UHFFFAOYSA-N N-Methylolacrylamide Chemical compound OCNC(=O)C=C CNCOEDDPFOAUMB-UHFFFAOYSA-N 0.000 claims abstract description 6
- 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 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 22
- 239000002994 raw material Substances 0.000 claims description 11
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 10
- 238000010189 synthetic method Methods 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 229920001427 mPEG Polymers 0.000 claims description 5
- 239000004160 Ammonium persulphate Substances 0.000 claims description 4
- 239000004159 Potassium persulphate Substances 0.000 claims description 4
- 235000019395 ammonium persulphate Nutrition 0.000 claims description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 4
- 235000019394 potassium persulphate Nutrition 0.000 claims description 4
- 230000032050 esterification Effects 0.000 claims description 3
- 238000005886 esterification reaction Methods 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 125000005395 methacrylic acid group Chemical group 0.000 claims description 2
- 239000004567 concrete Substances 0.000 abstract description 11
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 abstract description 4
- 239000011083 cement mortar Substances 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract description 2
- CNJRPYFBORAQAU-UHFFFAOYSA-N 1-ethoxy-2-(2-methoxyethoxy)ethane Chemical compound CCOCCOCCOC CNJRPYFBORAQAU-UHFFFAOYSA-N 0.000 abstract 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 abstract 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 abstract 1
- 239000002202 Polyethylene glycol Substances 0.000 abstract 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 abstract 1
- 238000001704 evaporation Methods 0.000 abstract 1
- 230000008020 evaporation Effects 0.000 abstract 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 abstract 1
- 229920001223 polyethylene glycol Polymers 0.000 abstract 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 abstract 1
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229920005646 polycarboxylate Polymers 0.000 description 3
- 230000008602 contraction Effects 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000004574 high-performance concrete Substances 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000009429 distress Effects 0.000 description 1
- 239000011440 grout Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
Landscapes
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses a reduced water reducing agent. The reduced water reducing agent is prepared by methoxy polyethylene glycol a, diethylene glycol monomethyl ether, diethylene glycol mono-methyl ethyl ether or a mixture of diethylene glycol monomethyl ether and diethylene glycol mono-methyl ethyl ether b, hydroxymethyl acrylamide c, acrylic acid, methacrylic acid or a mixture of acrylic acid and methacrylic acid d, ammonium persulfate or potassium persulfate e, hydroquinol f and concentrated sulfuric acid g. The reduced water reducing agent has the beneficial effects that the interface tensile force of solution inside cement mortar pores can be reduced, so that the pressure of capillary pores can be reduced; the moisture evaporation rate is influenced, so that the drying shrinkage of the cement mortar can be greatly reduced; the reduced water reducing agent is more suitable for the concrete engineering with high requirement on the reduced fracture resistance.
Description
Technical field
The present invention relates to relate to building trade water reducer, specifically a kind of shrinkage type water reducer and synthetic method thereof.
Background technology
High performance concrete (HPC) has high strength, high workability and excellent weather resistance.In the appearance of optimizing the simultaneous new problem of HPC performance, wherein one of the severeest problem is exactly the aggravation of Plastic Shrinkage of Concrete cracking.So it is own through becoming the emphasis of current engineering circles research which kind of approach to reduce concrete contraction by.
Normal employing added the drying shrinkage that cement expansive material carrys out compensating concrete both at home and abroad.The volume of swelling agent generally accounts for the 6%-15% of binder total amount, and volume is large and must carry out enough moisture-keeping maintainings to concrete.Economization agent for concrete is by reducing the surface tension of water in concrete pore, the convergent force of minimizing moisture evaporative process reduces concrete contraction, to reach the object of minimizing distress in concrete.But there is concrete strength and the expensive problem of affecting in economization agent.
Summary of the invention
The object of this invention is to provide a kind of shrinkage type water reducer and synthetic method thereof, plastic shrinkage is little, and resistance to cleavage is good.
Technical scheme of the present invention is achieved in that by following raw material and makes:
A methoxy poly (ethylene glycol)
B diethylene glycol monomethyl ether or diglycol monotertiary B ether or both mixtures
C n-methylolacrylamide
The acid of d acrylic or methacrylic or both mixtures
E ammonium persulphate or Potassium Persulphate
F Resorcinol
The g vitriol oil
The mol ratio of its raw material is: a:b:c: d=1:0.1 ~ 0.2: 0.05 ~ 0.1: 3 ~ 4, f consumption is total weight of material 0.04 ~ 0.06%, and e consumption is total weight of material 0.05 ~ 0.1%, and g consumption is total weight of material 0.5 ~ 0.8%.
The preferred molar ratio a:b:c of raw material: d=1:0.1:0.05:3.
The synthetic method of shrinkage type water reducer, its step is as follows: 1) by a, b, c, d adds reactor successively, stirs and heats up, and after mixing of materials is even, by f, g adds successively, and continues to be warming up to 120 degree reaction 8 hours, obtains esterification products; 2) temperature of charge is down to 60 degree, and thin up reactant, keep 60 degree; 3) e is dissolved in water, make and drips material A, evenly to reactor, drip, minute within 4 hours, add, add rear continuation and stir 1 hour, with appropriate liquid caustic soda neutralization reactant to PH be 6-7.
In described step 1), in reaction process, constantly by vacuumizing, remove moisture in reactor.
The concentration of described dropping liquid A is 5 ~ 10% massfractions.
Beneficial effect of the present invention is: shrinkage type water reducer of the present invention significantly reduces the ability of the interfacial tension of grout hole internal solution, thereby reduction capillary pressure, affect moisture vaporator rate, and then more significantly reduce the dry shrinkage can significantly reduce cement mortar, the concrete works that is applied to reducing and anti-cracking to have higher requirements preferably.
Embodiment
Below in conjunction with specific embodiment, the present invention is further explained to explanation.
Embodiment 1
The composition of raw material and proportioning thereof:
A methoxy poly (ethylene glycol)
B diethylene glycol monomethyl ether
C n-methylolacrylamide
D vinylformic acid
E ammonium persulphate
F Resorcinol
The g vitriol oil
The mol ratio of its raw material is: a:b:c: d==1:0.1:0.05:3, and f consumption is total weight of material 0.05%, and e consumption is total weight of material 0.05%, and g consumption is total weight of material 0.5%.
The synthetic method of shrinkage type water reducer, its step is as follows: 1) by a, b, c, d adds reactor successively, stir and heat up, after mixing of materials is even, by f, g adds successively, and continues to be warming up to 120 degree reaction 8 hours, obtain esterification products, in reaction process, constantly by vacuumizing, remove moisture in reactor; 2) temperature of charge is down to 60 degree, and thin up reactant, keep 60 degree; 3) e is dissolved in water, make and drips material A, evenly to reactor, drip, minute within 4 hours, add, add rear continuation and stir 1 hour, with appropriate liquid caustic soda neutralization reactant to PH be 6-7.
Embodiment 2
The composition of raw material and proportioning thereof are:
A methoxy poly (ethylene glycol)
B diglycol monotertiary B ether
C n-methylolacrylamide
D methacrylic acid
E Potassium Persulphate
F Resorcinol
The g vitriol oil
The mol ratio of its raw material is: a:b:c: d=1:0.2: 0.1: 4, f consumption was total weight of material 0.04%, and e consumption is total weight of material 0.1%, and g consumption is total weight of material 0.8%.
Its synthetic method is with embodiment 1.
Embodiment 3
A methoxy poly (ethylene glycol)
B diethylene glycol monomethyl ether and diglycol monotertiary B ether
C n-methylolacrylamide
D vinylformic acid and methacrylic acid
E ammonium persulphate and Potassium Persulphate
F Resorcinol
The g vitriol oil
The mol ratio of its raw material is: a:b:c: d=1:0.15:0.08:3.5, and f consumption is total weight of material 0.06%, and e consumption is total weight of material 0.06%, and g consumption is total weight of material 0.6%.
Its synthetic method is with embodiment 1.
Synthetic 40% polycarboxylate water-reducer, the results are shown in following table to this sintetics and market polycarboxylate water-reducer with proportioning comparison and detection as stated above.
Product | Volume % | Shrinkage ratio % | 28d intensity Mpa | Impervious grade |
Common polycarboxylate water-reducer | 0.4 | 108 | 32.6 | P8 |
Embodiment 1 | 0.4 | 95 | 34.8 | P10 |
Embodiment 2 | 0.4 | 97 | 34.4 | P10 |
Embodiment 3 | 0.4 | 98 | 35.1 | P10 |
The above; it is only preferably embodiment of the present invention; but protection scope of the present invention is not limited to this; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; according to technical scheme of the present invention and inventive concept thereof, be equal to replacement or changed, within all should being encompassed in protection scope of the present invention.
Claims (5)
1. a shrinkage type water reducer, is characterized in that, by following raw material, is made:
A methoxy poly (ethylene glycol)
B diethylene glycol monomethyl ether or diglycol monotertiary B ether or both mixtures
C n-methylolacrylamide
The acid of d acrylic or methacrylic or both mixtures
E ammonium persulphate or Potassium Persulphate or both mixtures
F Resorcinol
The g vitriol oil
The mol ratio of its raw material is: a:b:c: d=1:0.1 ~ 0.2: 0.05 ~ 0.1: 3 ~ 4, f consumption is total weight of material 0.04 ~ 0.06%, and e consumption is total weight of material 0.05 ~ 0.1%, and g consumption is total weight of material 0.5 ~ 0.8%.
2. shrinkage type water reducer according to claim 1, is characterized in that, the mol ratio a:b:c of raw material: d=1:0.1:0.05:3.
3. the synthetic method of shrinkage type water reducer as claimed in claim 1 or 2, is characterized in that, 1) and by a, b, c, d adds reactor successively, stir to heat up, when mixing of materials evenly after by f, g adds successively, and continues to be warming up to 120 degree reaction 8 hours, obtains esterification products; 2) temperature of charge is down to 60 degree, and thin up reactant, keep 60 degree; 3) e is dissolved in water, make and drips material A, evenly to reactor, drip, minute within 4 hours, add, add rear continuation and stir 1 hour, with appropriate liquid caustic soda neutralization reactant to PH be 6-7.
4. the synthetic method of shrinkage type water reducer according to claim 3, is characterized in that, in described step 1) reaction process, constantly by vacuumizing, removes moisture in reactor.
5. the synthetic method of shrinkage type water reducer according to claim 3, is characterized in that, the concentration of described dropping liquid A is 5 ~ 10% massfractions.
Priority Applications (1)
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CN201310749205.5A CN103724567B (en) | 2013-12-31 | 2013-12-31 | A kind of shrinkage type water reducer and synthetic method thereof |
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CN201310749205.5A CN103724567B (en) | 2013-12-31 | 2013-12-31 | A kind of shrinkage type water reducer and synthetic method thereof |
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Publication Number | Publication Date |
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CN103724567A true CN103724567A (en) | 2014-04-16 |
CN103724567B CN103724567B (en) | 2015-11-18 |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110395934A (en) * | 2019-07-16 | 2019-11-01 | 江苏博思通新材料有限公司 | A kind of concrete shrinkage type water-reducing agent |
CN114957559A (en) * | 2022-05-24 | 2022-08-30 | 佳化化学科技发展(上海)有限公司 | Amide water reducing agent and preparation method thereof |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102875047A (en) * | 2012-10-17 | 2013-01-16 | 兰州大学 | Polycarboxylic high-efficiency water reducing agent and preparation method thereof |
CN103450412A (en) * | 2013-09-16 | 2013-12-18 | 贵州科之杰新材料有限公司 | Preparation method of ester early-strength polycarboxylic acid water reducing agent |
-
2013
- 2013-12-31 CN CN201310749205.5A patent/CN103724567B/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102875047A (en) * | 2012-10-17 | 2013-01-16 | 兰州大学 | Polycarboxylic high-efficiency water reducing agent and preparation method thereof |
CN103450412A (en) * | 2013-09-16 | 2013-12-18 | 贵州科之杰新材料有限公司 | Preparation method of ester early-strength polycarboxylic acid water reducing agent |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110395934A (en) * | 2019-07-16 | 2019-11-01 | 江苏博思通新材料有限公司 | A kind of concrete shrinkage type water-reducing agent |
CN114957559A (en) * | 2022-05-24 | 2022-08-30 | 佳化化学科技发展(上海)有限公司 | Amide water reducing agent and preparation method thereof |
CN114957559B (en) * | 2022-05-24 | 2023-09-15 | 佳化化学科技发展(上海)有限公司 | Amide water reducer and preparation method thereof |
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Granted publication date: 20151118 |