CN105085821A - Heat-energy-free novel integrated efficient polycarboxylic acid water reducer and preparation method therefor - Google Patents
Heat-energy-free novel integrated efficient polycarboxylic acid water reducer and preparation method therefor Download PDFInfo
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Abstract
The invention relates to a heat-energy-free novel integrated efficient polycarboxylic acid water reducer and a preparation method therefor. The water reducer is obtained by polymerizing a polymerizable organic acid small monomer with a carboxylic acid group and a polymerizable polyether TPEG large monomer with a long chain at normal temperature. The water reducer is simple in reaction, free of heat energy consumption, short in reaction time and safe and pollution-free in production process. The water reducing rate can reach 45-50%. By adopting he water reducer, the doping amount of mineral admixtures in concrete can be properly improved, the cost of building materials is lowered, and the performance of concrete is improved. The water reducer is small in doping amount, strong in anti-clay ability and high in comprehensive cost performance, and is widely applied to preparing concrete with super-durability.
Description
Technical field
The present invention relates to a kind of concrete admixture, the High-efficiency polycarboxylic acid water reducer of particularly a kind of normal temperature synthesis, belongs to water reducer technical field.
Background technology
Poly carboxylic acid comb polymer molecule admixture is the Japan-US polycarboxylate water-reducer of new generation (PCE) waiting country's exploitation since being the eighties in 20th century, its constructional feature is combed grafting long-chain macromolecule structure, molecular backbone chain is with intensive hydroxy-acid group, molecule side chain is nonionic polyethylene chain, molecule utilizes hydrophilic long side chain to provide " anchoring " effect between the intensive hydroxy-acid group on space steric effect and main chain and cement granules to produce high diminishing, low-dosage, high-thin arch dam performance, thus gradually receive the extensive approval of coagulation pedosphere, for preparation strong concrete and self-leveling concrete, save cement consumption and improve the volume of solid waste, comb polymer molecule has very large advantage under the state of low water-cement ratio.
Within 1981, Japanese NipponShobubai and MasterBuildersTechnology starts to develop polycarboxylate water-reducer and first product was squeezed into the market in 1986.High-efficiency water-reducing agent of poly-carboxylic acid entered China about about 2000 greatly, entered the high-speed developing period before and after 2005.Investigate from long side chain polymeric monomer, the high-efficiency water-reducing agent of poly-carboxylic acid applied in the market is probably divided three classes, the polyether-type high efficiency water reducing agent being long side chain with APEG (allyl polyglycol); With the polyester type high efficiency water reducing agent that MPEG (methoxy poly (ethylene glycol)) is long side chain; The third is applied the polymerization of APEG and MPEG two class polyether macromonomer or derivatives thereof simultaneously and obtains carboxylic acid high efficiency water reducing agent.
Chinese patent document CN102268121A (application number: 201110132868.3) disclose a kind of high water reducing rate high slump-retaining poly carboxylic acid series water reducer, synthetic method and using method.This water reducer is made up of 2-methyl allyl alcohol polyoxyethylene ether (TPEG), 2-acrylamide-2-methylpro panesulfonic acid (AMPS), methacrylic acid (MAA), ammonium persulphate (APS), sodium hydroxide and water.Concrete steps are: the mixing solutions TPEG and AMPS, MAA being mixed with respectively 20% ~ 50% concentration, APS are added appropriate water dissolution simultaneously; In reactor, add TPEG and the AMPS monomer mixture solution prepared, pass into nitrogen, plug prolong, stir and be warming up to 60 ~ 100 DEG C, drip MAA monomer solution and APS solution respectively; The time for adding of monomer solution is 1 ~ 5 hour, and the time for adding of APS solution is 1.5 ~ 5.5 hours; After dropwising, isothermal reaction 1 ~ 2 hour; Cooling, neutralizes by NaOH solution and obtains required product.
Chinese patent document CN103059231A (application number: the preparation method 201310016801.2) disclosing a kind of combed macromolecular sand-fixation water-holding agent, comprise the steps: first alkyl vinyl polyglycol ether and tetraalkoxysilane and catalyzer tosic acid to be joined in reaction vessel, at temperature 50-150 DEG C, reaction 2-10 hour, solvent evaporation in vacuo, obtains polymeric monomer; Again vinyl acetate, butyl acrylate and acrylamide are mixed to get copolymerization minor comonomer; Finally by polymeric monomer obtained above, join in reaction vessel, add copolymerization minor comonomer, water and emulsifying agent, be warmed up to 60-80 DEG C, drip 40-100 part 5% ammonium persulfate aqueous solution, within 180 minutes, dropwise, insulation reaction 180-240 minute, cooling, obtains combed macromolecular sand-fixation water-holding agent.
But the disadvantage of above-mentioned high-efficiency water-reducing agent of poly-carboxylic acid is the bad adaptability to cement, maximum water-reducing rate is no more than 40%, and production temperature is many more than 50 DEG C, and production energy consumption is large.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of strong to cement adaptability, there is superelevation water-reducing property, super-efficient carboxylic acid water reducer that preparation process thermal energy consumption is low.
Term illustrates:
TPEG: allyl polyglycol is a kind of modified polyether, has the structure shown in formula (II),
In formula (II), x is the integer of 0 ~ 100, and y is the integer of 0 ~ 35, is 0 when x with y is different; R
4, R
5separately be selected from H or-CH
3.Commercial products, also can prepare by prior art.The TPEG that can select different molecular weight is required according to difference.
Technical scheme of the present invention is as follows:
A kind of without heat energy novel all-in-one High-efficiency polycarboxylic acid water reducer, there is structure shown in formula (I):
In formula (I), x is the integer of 0 ~ 100, and y is the integer of 0 ~ 35, is 0 when x with y is different; M be greater than 1 positive integer, n be greater than 1 positive integer; R
1, R
3, R
4, R
5separately be selected from H or-CH
3, R
2be selected from H, COOH.
According to the present invention, preferably, in formula (I), x is the integer of 30 ~ 50, and y is the integer of 21 ~ 25.
According to the present invention, preferably, in formula (I), m is the integer of 20 ~ 70, and n is the integer of 5 ~ 20.
According to the present invention, the above-mentioned preparation method without heat energy novel all-in-one High-efficiency polycarboxylic acid water reducer, comprises step as follows:
(1) preparation that added water by TPEG obtains substrate solution;
(2) preparation that added water by organic acid obtains solution B, and described organic acid has the structure shown in formula (III),
In formula (III), R
1, R
2, R
3cotype (I);
(3) preparation that adds water after initiator and molecular weight regulator mixing is obtained solution A, described initiator be hydrogen peroxide, ammonium persulfate or/and Potassium Persulphate, described molecular weight regulator is that vinyl acetate, thiohydracrylic acid, Thiovanic acid are or/and methylpropene sodium sulfonate;
(4) solution A and solution B are added drop-wise in substrate solution simultaneously, the mass ratio of organic acid, TPEG, initiator and molecular weight regulator is made to be 1: (3.3 ~ 10): (0.004 ~ 0.009): (0.004 ~ 0.03), after being added dropwise to complete, in 20 ~ 40 DEG C of stirring reaction 0.5 ~ 2h, to obtain final product.
According to the present invention, preferably, the molecular weight of the TPEG described in step (1) is 1200 ~ 3000, further preferably 2000 ~ 3000;
Preferably, the concentration of described substrate solution is 50 ~ 65wt%.
According to the present invention, preferably, the organic acid described in step (2) is acrylic or methacrylic acid, and the concentration of described solution B is 70-85wt%.
According to the present invention, preferably, in step (3), in solution A, the total concn of initiator and molecular weight regulator is 2 ~ 5wt%.
According to the present invention, preferably, in step (4), the mass ratio of organic acid, TPEG, initiator and molecular weight regulator is 1: (5.5 ~ 7): (0.005 ~ 0.009): (0.004 ~ 0.03), the drop rate of solution A is 0.45 ~ 0.8ml/min, the drop rate of solution B is 0.8 ~ 1.4ml/min, and temperature of reaction is 25 ~ 30 DEG C.Can add water after having reacted and regulate reaction product concentration to be 35 ~ 45wt%, and regulate pH to be 6.5 ~ 7.0.
According to the present invention, in formula (I), m, n are respectively organic acid and the polymerization degree of TPEG in whole polymeric.
Principle of the present invention:
Water reducer of the present invention provides " anchoring " between cement granules point by means of the carboxyl in molecular structure, the long side chain of grafting on main chain is utilized to provide space steric effect, utilize methyl group on side chain near main chain to regulate absorption property between the wetting ability of side chain and the gelling material particles such as backbone and cement, thus jointly obtain good water-reducing property.
Feature of the present invention and beneficial effect:
1, the water-reducing property of water reducer of the present invention is higher than various polycarboxylate water-reducers commercially available at present, water-reducing rate can reach 45 ~ 50%, can obtain the large fluidity ultra-high performance concrete of degree of mobilization at 18 ~ 22cm easily, the intensity of maturing can reach more than 120MPa.
2, adopt water reducer of the present invention suitably can improve the volume of concrete Minerals adulterant, reduce material of construction cost, improve concrete performance.
3, water reducer of the present invention can synthesize at normal temperatures, organic acid is as minor comonomer, TPEG is as polymeric monomer, and the two direct polymerization reacts, under the acting in conjunction of molecular weight regulator and initiator, synthesize comb shape super-efficient carboxylic acid water reducer of the present invention, preparation process is without the need to additional heat energy, and the production time is short, pollution-free, production process safety, has very high economic benefit and social benefit.
4, water reducer of the present invention can not affect concrete time of coagulation and strong in early days with the composite use of other carboxylic acid water reducing agent existing on market, can with the composite uses such as other air entrapment agent, retardant, hardening accelerator, defoamer, to improve the over-all properties of product.Water reducer of the present invention has good adaptability to the cement type of domestic more than 95%, can meet various construction requirement, applied range.
Accompanying drawing explanation
Fig. 1 is the infared spectrum of the water reducer that the embodiment of the present invention 1 obtains.
Embodiment
Below by specific embodiment, the present invention will be further described, but be not limited thereto.
Embodiment 1
Without a preparation method for heat energy novel all-in-one High-efficiency polycarboxylic acid water reducer, comprise step as follows:
(1) bed material is prepared: be first the substrate solution 220g that TPEG stirring and dissolving together with water of 2000-3000 is configured to 60wt% by molecular weight;
(2) B material is prepared: solution B 27g vinylformic acid and water being made in advance 77wt%;
(3) prepare A material: aqueous solution 30g initiator ammonium persulfate being made in advance 0.15wt% concentration, and then add molecular weight regulator vinyl acetate 0.3g successively, hydrogen peroxide (30wt%) 0.2g stirs, and obtains solution A;
(4) at 30 DEG C ± 1 DEG C, drip solution B and solution A in substrate solution, the time for adding of solution A controls at 1.5 hours, and the time for adding of solution B controls at 1.0 hours simultaneously; Solution A dropwises, and is incubated 1.0 hours; Then add water stir (concentration controls at about 40wt%), and with NaOH solution adjust ph to 6.5 ~ 7.0 of 30wt% concentration, discharging, obtains water reducer.
The water reducer that the present embodiment is obtained, molecular structure is as follows:
The infrared spectrum of water reducer as shown in Figure 1.
Embodiment 2
(1) bed material is prepared: be first the substrate solution 264g that TPEG stirring and dissolving together with water of 2000-3000 is configured to 50wt% by molecular weight;
(2) B material is prepared: solution B 29.7g vinylformic acid and water being made in advance 70wt%;
(3) prepare A material: aqueous solution 30g initiator ammonium persulfate being made in advance 0.2wt% concentration, and then add molecular weight regulator thiohydracrylic acid 0.1g, hydrogen peroxide (30wt%) 0.4g successively, stir, obtain solution A;
(4) at 25 DEG C ± 1 DEG C, drip solution B and solution A in substrate solution, the time for adding of solution A controls at 3.5 hours, and the time for adding of solution B controls at 3.0 hours, and solution A dropwises insulation 0.5 hour simultaneously.Be incubated complete stir (concentration controls at about 40wt%) that add water, then add 30wt%NaOH solution adjust ph get final product discharging within the scope of 6.5-7.0, obtain water reducer.
Embodiment 3
(1) bed material is prepared: be first the substrate solution 240g that TPEG stirring and dissolving together with water of 2000-3000 is configured to 55wt% by molecular weight;
(2) B material is prepared: solution B 26g vinylformic acid and water being made in advance 80wt%;
(3) prepare A material: aqueous solution 30g initiator ammonium persulfate being made in advance 0.18wt% concentration, and then add molecular weight regulator methylpropene sodium sulfonate 0.5g, hydrogen peroxide (30wt%) 0.15g successively, stir, obtain solution A;
(4) at 20 DEG C ± 1 DEG C, simultaneously in bed material, drip solution B and solution A, during the dropping of solution A, time controling was at 3.5 hours, and the time for adding of solution B controls at 3.0 hours, and solution A dropwises insulation 1.5 hours.Be incubated complete stir (concentration controls at about 40wt%) that add water, then add 30wt%NaOH solution adjust ph get final product discharging within the scope of 6.5-7.0, obtain water reducer.
Embodiment 4
(1) bed material is prepared: be first the substrate solution 203g that TPEG stirring and dissolving together with water of 2000-3000 is configured to 65wt% by molecular weight;
(2) B material is prepared: solution B 53.3g vinylformic acid and water being made in advance 75wt%;
(3) prepare A material: aqueous solution 30g initiator potassium persulfate being made in advance 0.18wt% concentration, and then add molecular weight regulator Thiovanic acid 0.2g, hydrogen peroxide (30wt%) 0.15g successively, stir, obtain solution A;
(4) at 35 DEG C ± 1 DEG C, simultaneously in bed material, drip solution B and solution A, during the dropping of solution A, time controling was at 3.5 hours, and the time for adding of solution B controls at 3.0 hours, and solution A dropwises insulation 1.5 hours.Be incubated complete stir (concentration controls at about 40wt%) that add water, then add 30wt%NaOH solution adjust ph get final product discharging within the scope of 6.5-7.0, obtain water reducer.
Embodiment 5
(1) bed material is prepared: be first the substrate solution 240g that TPEG stirring and dissolving together with water of 2000-3000 is configured to 55wt% by molecular weight;
(2) B material is prepared: solution B 30g vinylformic acid and water being made in advance 80wt%;
(3) prepare A material: aqueous solution 30g initiator ammonium persulfate being made in advance 0.1wt% concentration, and then add molecular weight regulator methylpropene sodium sulfonate 0.4g, hydrogen peroxide (30wt%) 0.15g successively, stir, obtain solution A;
(4) at 20 DEG C ± 1 DEG C, simultaneously in bed material, drip solution B and solution A, during the dropping of solution A, time controling was at 3.5 hours, and the time for adding of solution B controls at 3.0 hours, and solution A dropwises insulation 1.5 hours.Be incubated complete stir (concentration controls at about 40wt%) that add water, then add 30wt%NaOH solution adjust ph get final product discharging within the scope of 6.5-7.0, obtain water reducer.
Embodiment 6
(1) bed material is prepared: be first the substrate solution 240g that TPEG stirring and dissolving together with water of 2000-3000 is configured to 55wt% by molecular weight;
(2) B material is prepared: solution B 27g vinylformic acid and water being made in advance 70wt%;
(3) prepare A material: aqueous solution 30g initiator ammonium persulfate being made in advance 0.2wt% concentration, and then add molecular weight regulator Thiovanic acid 0.3g, hydrogen peroxide (30wt%) 0.15g successively, stir, obtain solution A;
(4) at 40 DEG C ± 1 DEG C, simultaneously in bed material, drip solution B and solution A, during the dropping of solution A, time controling was at 3.5 hours, and the time for adding of solution B controls at 3.0 hours, and solution A dropwises insulation 1.5 hours.Be incubated complete stir (concentration controls at about 40wt%) that add water, then add 30wt%NaOH solution adjust ph get final product discharging within the scope of 6.5-7.0, obtain water reducer.
Embodiment 7
(1) bed material is prepared: be first the substrate solution 264g that TPEG stirring and dissolving together with water of 2000-3000 is configured to 50wt% by molecular weight;
(2) B material is prepared: solution B 15.5g vinylformic acid and water being made in advance 85wt%;
(3) prepare A material: aqueous solution 30g initiator ammonium persulfate being made in advance 0.18wt% concentration, and then add molecular weight regulator methylpropene sodium sulfonate 0.5g, hydrogen peroxide (30wt%) 0.15g successively, stir, obtain solution A;
(4) at 20 DEG C ± 1 DEG C, simultaneously in bed material, drip solution B and solution A, during the dropping of solution A, time controling was at 3.5 hours, and the time for adding of solution B controls at 3.0 hours, and solution A dropwises insulation 1.5 hours.Be incubated complete stir (concentration controls at about 40wt%) that add water, then add 30wt%NaOH solution adjust ph get final product discharging within the scope of 6.5-7.0, obtain water reducer.
The performance test of experimental example water reducer
The water reducer obtained by embodiment 1-3 and the application performance of commercial products high-efficiency water-reducing agent of poly-carboxylic acid HW respectively in mortar, cement paste and concrete do simultaneous test.
(1) mortar, only starch experiment
Respectively water reducer obtained for embodiment 1, embodiment 2 and embodiment 3 is all mixed (admixture and cement weight per-cent) by solid volume 0.5% to perform.
Mortar is tested: 1350g standard sand, 170 water, 450g scenery with hills and waters cement (P.O42.5);
Clean slurry experiment: 300g scenery with hills and waters cement (P.O52.5), 87g water.
Determination data is in table 1.
Table 1 adds the degree of mobilization contrast of the mortar after water reducer, cement paste
As known from Table 1, water reducer of the present invention to collapse effect to concrete water-reducing effect and guarantor, all than commercial high-efficiency water-reducing agent of poly-carboxylic acid HW excellent performance.
(2) concrete experiments
Because admixture is most widely used with concrete in actual applications, therefore add in concrete by water reducer obtained for embodiment 3 by solid volume 1.0% (admixture and cement weight per-cent) respectively, the cement in concrete all adopts scenery with hills and waters cement (P.O42.5).Concrete initial slump controls at 18-22cm, and detect slump retention rate and index of correlation performance after 1 hour, determination data is in table 2.
The concrete performance index of product of the present invention and other water reducer mixed by table 2
As known from Table 2, the application performance of product of the present invention in concrete, also higher than high-efficiency water-reducing agent of poly-carboxylic acid HW, no matter be water-reducing rate, air content, slump retaining, time of coagulation, or intensity is all than the excellent performance of high-efficiency water-reducing agent of poly-carboxylic acid HW.
Claims (10)
1. without a heat energy novel all-in-one High-efficiency polycarboxylic acid water reducer, it is characterized in that, this water reducer has structure shown in formula (I):
In formula (I), x is the integer of 0 ~ 100, and y is the integer of 0 ~ 35, is 0 when x with y is different; M be greater than 1 positive integer, n be greater than 1 positive integer; R
1, R
3, R
4, R
5separately be selected from H or-CH
3, R
2be selected from H, COOH.
2. water reducer according to claim 1, is characterized in that, in formula (I), x is the integer of 30 ~ 50, and y is the integer of 21 ~ 25.
3. water reducer according to claim 1, is characterized in that, in formula (I), m is the integer of 20 ~ 70, and n is the integer of 5 ~ 20.
4. a preparation method for the water reducer described in any one of claim 1-3, comprises step as follows:
(1) preparation that added water by TPEG obtains substrate solution;
(2) preparation that added water by organic acid obtains solution B, and described organic acid has the structure shown in formula (III),
In formula (III), R
1, R
2, R
3cotype (I);
(3) preparation that adds water after initiator and molecular weight regulator mixing is obtained solution A, described initiator be hydrogen peroxide, ammonium persulfate or/and Potassium Persulphate, described molecular weight regulator is that vinyl acetate, thiohydracrylic acid, Thiovanic acid are or/and methylpropene sodium sulfonate;
(4) solution A and solution B are added drop-wise in substrate solution simultaneously, the mass ratio of organic acid, TPEG, initiator and molecular weight regulator is made to be 1: (3.3 ~ 10): (0.004 ~ 0.009): (0.004 ~ 0.03), after being added dropwise to complete, in 20 ~ 40 DEG C of stirring reaction 0.5 ~ 2h, to obtain final product.
5. the preparation method of water reducer according to claim 4, is characterized in that, the molecular weight of the TPEG described in step (1) is 1200 ~ 3000, further preferably 2000 ~ 3000.
6. the preparation method of water reducer according to claim 4, is characterized in that, described in step (1), the concentration of substrate solution is 50 ~ 65wt%.
7. the preparation method of water reducer according to claim 4, is characterized in that, the organic acid described in step (2) is acrylic or methacrylic acid, and the concentration of described solution B is 70-85wt%.
8. the preparation method of water reducer according to claim 4, is characterized in that, in step (3), in solution A, the total concn of initiator and molecular weight regulator is 2 ~ 5wt%.
9. the preparation method of water reducer according to claim 4, it is characterized in that, in step (4), the mass ratio of organic acid, TPEG, initiator and molecular weight regulator is 1: (5.5 ~ 7): (0.005 ~ 0.009): (0.004 ~ 0.03).
10. the preparation method of water reducer according to claim 4, is characterized in that, in step (4), the drop rate of solution A is 0.45 ~ 0.8ml/min, and the drop rate of solution B is 0.8 ~ 1.4ml/min, and temperature of reaction is 25 ~ 30 DEG C.
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| CN108033705A (en) * | 2017-12-28 | 2018-05-15 | 钊美新材料（上海）有限公司 | A kind of compound as auxiliary water-reducing agent |
| CN109503773A (en) * | 2018-10-15 | 2019-03-22 | 湖州绿色新材股份有限公司 | High-slump-retentionpolycarboxylate polycarboxylate water reducer and its synthetic method |
| CN109942757A (en) * | 2017-12-20 | 2019-06-28 | 中冶建筑研究总院有限公司 | A kind of polycarboxylate water-reducer |
| CN110204663A (en) * | 2019-05-30 | 2019-09-06 | 上海宏韵新型建材有限公司 | Viscosity reduction type polycarboxylic acid concrete additive |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109942757A (en) * | 2017-12-20 | 2019-06-28 | 中冶建筑研究总院有限公司 | A kind of polycarboxylate water-reducer |
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| CN110204663A (en) * | 2019-05-30 | 2019-09-06 | 上海宏韵新型建材有限公司 | Viscosity reduction type polycarboxylic acid concrete additive |
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Application publication date: 20151125 |