CN104987469A - Preparing method for high dispersion type polycarboxylate water reducing agent - Google Patents
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Abstract
The invention relates to a preparing method for a high dispersion type polycarboxylate water reducing agent. The method comprises the steps that in the normal temperature condition, unsaturated polyoxyethylene ether is mixed with water, stirring is carried out until dissolution is completed, an oxidizing agent and a part of unsaturated carboxylic acid are added, full stirring is carried out until mixing is even, a pre-dissolved mixed solution of a unsaturated carboxylic acid solution, a reducing agent and a chain transferring agent is further added dropwise, after adding is completed, the full stirring and curing are carried out on a reacting solution, aqueous alkali is further added into the reacting solution, neutralizing is carried out until the pH value ranges from 6 to 7, and the high dispersion type polycarboxylate water reducing agent is prepared. Compared with the prior art, a free radical polymerization method is adopted, the water serves as solvent, heating and temperature controlling are not needed in the whole preparing process, the production cycle is short and only in two hours, the production energy consumption is low, resources are saved, the production cost is effectively lowered, and the high dispersion type polycarboxylate water reducing agent can be widely applied to the industrial production.
Description
Technical field
The invention belongs to chemical building material technical field, relate to a kind of preparation method of high dispersive type polycarboxylate water-reducer.
Background technology
Along with the development in an all-round way of China's capital construction, not only facilitate the growth of high performance concrete demand, and promote the fast development of technology of high performance concrete, meanwhile, the performance of concrete high performance to high efficiency water reducing agent is had higher requirement.
Water reducer is a kind of raising slag-based gelling material and the requisite a kind of chemical admixture of concrete product, and it when compared with low water-cement ratio, can significantly improve the over-all propertieies such as the workability of goods, degree of compactness, intensity and weather resistance.Polycarboxylate water-reducer is third generation water reducer product, and it not only can increase substantially slag-based gelling material and concrete over-all properties, and also have the features such as low-dosage, environmental protection, molecular structure degree of freedom be large, application prospect is very extensive.When reality uses, polycarboxylate water-reducer is because of the molecular characterization of its uniqueness, sterically hindered repulsion effect can be produced in cement slurry, stronger to the dispersiveness of fresh concrete, volume is lower, concrete slump gradual loss is less, and the concrete strength increasing degree prepared is large and volume stability of concrete is good.
Compared with traditional water reducer, polycarboxylate water-reducer is prepared from by chain reaction polymerization, and compared to being progressively polymerized, chain polymerization does not have small molecules to produce, and does not substantially produce the three wastes, and simultaneous reactions is very fast, easily meets supply requirement.But in chain reaction polymerization process, the radical polymerization of alkene needs to cause, usual adopted initiator, kick off temperature is often higher than room temperature, and therefore, needing could initiated polymerization to certain temperature by heating raw materials.But Raolical polymerizable is thermopositive reaction, so wayward temperature in reaction process.
Authorization Notice No. is the making method that the Chinese invention patent of CN 103183792 B discloses a kind of polycarboxylate water-reducer, this water reducer is under the effect of redox initiator, by the Soxylat A 25-7 polymeric monomer a containing unsaturated double-bond and unsaturated carboxylic acid and derivatives monomer b thereof, unsaturated sulfonic acid salt monomer c copolymerization in aqueous, finally with in basic solution and obtained.The technical scheme of this patent disclosure is mainly by adopting redox system, temperature of reaction is controlled within the scope of 50-70 DEG C, whole reaction one step completes, although processing condition are relatively simple, and no waste mine discharge, but still need heating raw materials during reaction to certain temperature ability initiated polymerization, and temperature is wayward in reaction process, can not realizes carrying out polyreaction under normal temperature condition, be further improved.
Summary of the invention
Object of the present invention is exactly provide a kind of operation steps simple to overcome defect that above-mentioned prior art exists, and do not need heating and temperature control, production energy consumption is few, the preparation method of high dispersive type polycarboxylate water-reducer with short production cycle.
Object of the present invention can be achieved through the following technical solutions:
A kind of preparation method of high dispersive type polycarboxylate water-reducer, the method is under normal temperature condition, after unsaturated Soxylat A 25-7 is mixed with water, be stirred to and dissolve completely, add oxygenant and part unsaturated carboxylic acid, be stirred well to and mix, drip the mixing solutions of solvent in advance unsaturated carboxylic acid solution, reductive agent and chain-transfer agent more successively, after being added dropwise to complete, after reaction soln is fully stirred slaking, in reaction soln, add alkaline solution again, being neutralized to pH is 6-7, i.e. obtained high dispersive type polycarboxylate water-reducer.
A preparation method for high dispersive type polycarboxylate water-reducer, the method specifically comprises the following steps:
(1) under normal temperature condition, be 100:(100-130 by the mass ratio of unsaturated Soxylat A 25-7 and water), unsaturated Soxylat A 25-7 and water are dropped in reaction vessel, is stirred well to unsaturated Soxylat A 25-7 and dissolves completely;
(2) in the reaction vessel of step (1), disposablely add oxygenant and part unsaturated carboxylic acid, fully stir;
(3) remaining unsaturated carboxylic acid is added to the water, be mixed with the pre-molten unsaturated carboxylic acid solution that mass concentration is 50-55%, after step (2) is stirred to and mixes, drip pre-molten unsaturated carboxylic acid solution, control time for adding is 1-2h, preferred 1-1.5h;
(4) reductive agent and chain-transfer agent are added to the water, be mixed with the mixing solutions of reductive agent and chain-transfer agent, after step (3) residue unsaturated carboxylic acid solution is added dropwise to complete, drip the mixing solutions of reductive agent and chain-transfer agent again, control time for adding < 0.5h;
(5) after the mixing solutions of step (4) reductive agent and chain-transfer agent is added dropwise to complete, fully stirred by reaction soln, slaking 10-30min, then add alkaline solution, being neutralized to pH is 6-7, i.e. obtained high dispersive type polycarboxylate water-reducer.
Described unsaturated Soxylat A 25-7 and the mass ratio of unsaturated carboxylic acid total amount are 100:(12.0-12.3).
Described oxygenant quality is the 1.5-2% of unsaturated Soxylat A 25-7 quality.
Described reductive agent quality is the 0.1-0.5% of unsaturated Soxylat A 25-7 quality.
Described chain-transfer agent quality is the 0.3-0.6% of unsaturated Soxylat A 25-7 quality.
Part unsaturated carboxylic acid described in step (2) accounts for the 10-15% of unsaturated carboxylic acid total mass.
In reductive agent described in step (4) and the mixing solutions of chain-transfer agent, the mass ratio of chain-transfer agent, reductive agent and water is 1:(0.2-1): (45-55).
The isopentenol polyoxyethylene ether of described unsaturated Soxylat A 25-7 to be average molecular mass be 2100-2600, this isopentenol polyoxyethylene ether outward appearance is white flaky solid, degree of unsaturation >=0.37, hydroxyl value (mgKOH/g) is 23.50 ± 2.5, pH value (1% aqueous solution) is 5.0 ~ 7.0, water-soluble and multiple organic solvent.
Described isopentenol polyoxyethylene ether adopts international advanced Press outer circulation spraying second (third) oxygen base addition device and selects highly active catalytic production technology to be prepared from, double bond retention rate is high, when synthesizing water reducer, greatly improve reactive behavior, product appearance is good, adhesive aggregation slump retaining is good.
Described unsaturated carboxylic acid is the one in vinylformic acid, methacrylic acid or maleic anhydride, described oxygenant is one or both in ammonium persulphate, Potassium Persulphate, Sodium Persulfate or hydrogen peroxide, described reductive agent is L-AA, described chain-transfer agent is the one in thiohydracrylic acid or Thiovanic acid, the concentration of described alkaline solution is 20-25%, and described alkaline solution is NaOH solution, KOH solution or Ca (OH)
2in one, described water is tap water.
The addition of described polycarboxylate water-reducer is the 0.3-0.5% of cement quality.
The present invention is by preferred radical polymerization initiator, and formulation manipulation application is optimized to initiator, thus in synthesis technique of the present invention, omnidistance without the need to heating and temperature control, the mother liquor solid content preparing the polycarboxylate water-reducer of gained is 39-41%, for white emulsion shape thick liquid, with short production cycle, be only about 2h, production energy consumption is low, both save energy, greatly reduces production cost again, and can widely apply in the industrial production.
Polycarboxylate water-reducer of the present invention is on the basis meeting GB8076-2008 " concrete admixture " national standard, on in raising concrete water-reducing ratio and long-time mobility retentivity, there is unique advantage, being specially adapted to strength grade is in C30 and following concrete, price is lower, cost performance is high, hot weather function of slump protection is better, and cement adaptability is extensive, and late strength of concrete is higher.
Polycarboxylate water-reducer of the present invention is applied in the works productions such as Steel Concrete, light aggregate concrete, artificial aggregate concrete, bridge, building, water conservancy project and road surface, there is higher water-reducing rate, can effectively improve concrete workability, pumpability, hot weather concrete slump retaining better performances, the stabilise bubbles of a small amount of fine uniform can be introduced, ensure concrete mechanics strength stability, and then improve concrete long durability, obvious hydrophobic effect can be produced, reduce the water sorption of the impurity such as clay, there is excellent starting material adaptability.
Compared with prior art, the present invention has following characteristics:
1) high water reducing rate: polycarboxylate water-reducer of the present invention has higher water-reducing rate, effectively improves concrete workability, pumpability, hot weather concrete slump retaining better performances;
2) low bleed air volume: polycarboxylate water-reducer of the present invention has lower amount of air entrainment, in the concrete performance basis of guarantee, only introduces a small amount of gas, ensures concrete mechanics strength stability, can effectively improve concrete long durability;
3) high-adaptability: polycarboxylate water-reducer of the present invention can produce hydrophobic effect, reduces the water sorption of the impurity such as clay, is conducive to the development of ready-mixed concrete.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1:
In the reactor that whipping appts is housed, add isopentenol polyoxyethylene ether (referred to as TPEG) polymeric monomer 180g, water 180g under normal temperature, open whipping appts, be stirred to TPEG polymeric monomer and dissolve completely.Add ammonium persulphate 2.5g, hydrogen peroxide (purity is 35%) 1g, vinylformic acid 3.3g to reaction system, continue stirring and reaction system is fully mixed.By 19g vinylformic acid, be mixed with homogeneous solution A expect with 18g water, 1g thiohydracrylic acid, 1gL-xitix and 50g water are mixed with solution B material.By valve control device, A material and B material are progressively at the uniform velocity dropped to reaction system, wherein, A expects that time for adding is 1 hour, and B expects that time for adding is 1.5 hours.After A, B material is added dropwise to complete completely, continue stirring reaction system about 10 minutes, finally utilizing the sodium hydroxide solution of 25% concentration reaction soln to be neutralized into pH is 6.5.
Embodiment 2:
In the reactor that whipping appts is housed, add isopentenol polyoxyethylene ether (referred to as TPEG) polymeric monomer 180g, water 230g under normal temperature, open whipping appts, be stirred to TPEG polymeric monomer and dissolve completely.Add hydrogen peroxide (purity is 35%) 4g, methacrylic acid 2.3g to reaction system, continue fully to stir reaction system.22g methacrylic acid and 18g water are mixed with homogeneous solution A expect, 1g thiohydracrylic acid, 0.5gL-xitix and 50g water are mixed with solution B material.By peristaltic-type pump arrangement, A material and B material are progressively at the uniform velocity dropped to reaction system, wherein, A expects that time for adding is 1.5 hours, and B expects that time for adding is 2 hours.After A, B material is added dropwise to complete completely, continue stirring reaction system about 20 minutes, finally utilizing the sodium hydroxide solution of 25% concentration reaction soln to be neutralized into pH is 7.
Embodiment 3:
In the reactor that whipping appts is housed, add isopentenol polyoxyethylene ether (referred to as TPEG) polymeric monomer 180g, water 200g under normal temperature, open whipping appts, be stirred to TPEG polymeric monomer and dissolve completely.Add Potassium Persulphate 2g, hydrogen peroxide (purity is 35%) 1g, maleic anhydride 2.5g to reaction system, continue fully to stir reaction system.21g maleic anhydride and 18g water are mixed with homogeneous solution A expect, 1g thiohydracrylic acid, 0.2gL-xitix and 50g water are mixed with solution B material.By peristaltic-type pump arrangement, A material and B material are progressively at the uniform velocity dropped to reaction system, wherein, A expects that time for adding is 1 hour, and B expects that time for adding is 1.5 hours.After A, B material is added dropwise to complete completely, about continuing stirring reaction system half an hour, finally utilizing the sodium hydroxide solution of 25% concentration reaction soln to be neutralized into pH is 6.
To C30 pump concrete (each component proportioning of concrete is in table 1), the concrete properties of the polycarboxylate water-reducer that admixture 1-3 embodiment obtains is in table 2.
Table 1 concrete mix
| Cement | Flyash | Water | Sand | Great Shi | Gravelstone | Glue material total amount | W/C | Sand coarse aggregate ratio |
| 307 | 45 | 172 | 789 | 413 | 619 | 352 | 0.49 | 43％ |
Concrete performance data implemented by table 2
Embodiment 4:
The preparation method of the present embodiment high dispersive type polycarboxylate water-reducer specifically comprises the following steps:
(1) under normal temperature condition, be 100:130 by the mass ratio of unsaturated Soxylat A 25-7 and water, unsaturated Soxylat A 25-7 and water are dropped in reaction vessel, be stirred well to unsaturated Soxylat A 25-7 and dissolve completely;
(2) in the reaction vessel of step (1), disposablely add oxygenant and part unsaturated carboxylic acid, fully stir;
(3) be added to the water by remaining unsaturated carboxylic acid, be mixed with the pre-molten unsaturated carboxylic acid solution that mass concentration is 55%, after step (2) is stirred to and mixes, drip pre-molten unsaturated carboxylic acid solution, control time for adding is 2h;
(4) reductive agent and chain-transfer agent are added to the water, be mixed with the mixing solutions of reductive agent and chain-transfer agent, after step (3) residue unsaturated carboxylic acid solution is added dropwise to complete, drip the mixing solutions of reductive agent and chain-transfer agent again, control time for adding < 0.5h;
(5) after the mixing solutions of step (4) reductive agent and chain-transfer agent is added dropwise to complete, fully stirred by reaction soln, slaking 30min, then add alkaline solution, being neutralized to pH is 6, i.e. obtained high dispersive type polycarboxylate water-reducer.
In step (2), part unsaturated carboxylic acid accounts for 15% of unsaturated carboxylic acid total mass, and in step (4), in the mixing solutions of reductive agent and chain-transfer agent, the mass ratio of chain-transfer agent, reductive agent and water is 1:1:55.
Wherein, unsaturated Soxylat A 25-7 to be average molecular mass be 2600 isopentenol polyoxyethylene ether, degree of unsaturation >=0.37 of this isopentenol polyoxyethylene ether, hydroxyl value is 23.5mgKOH/g, and unsaturated carboxylic acid is vinylformic acid, and oxygenant is ammonium persulphate, reductive agent is L-AA, chain-transfer agent is thiohydracrylic acid, described alkaline solution to be concentration be 20% KOH solution, water is tap water.
In concrete consumption, the mass ratio of isopentenol polyoxyethylene ether and vinylformic acid total amount is 100:12.3, ammonium persulphate quality is 2% of isopentenol polyoxyethylene ether quality, L-AA quality is 0.5% of isopentenol polyoxyethylene ether quality, and thiohydracrylic acid quality is 0.6% of isopentenol polyoxyethylene ether quality.
When practical application, the addition of the polycarboxylate water-reducer that the present embodiment obtains is 0.5% of cement quality.
Embodiment 5:
The preparation method of the present embodiment high dispersive type polycarboxylate water-reducer specifically comprises the following steps:
(1) under normal temperature condition, be 100:120 by the mass ratio of unsaturated Soxylat A 25-7 and water, unsaturated Soxylat A 25-7 and water are dropped in reaction vessel, be stirred well to unsaturated Soxylat A 25-7 and dissolve completely;
(2) in the reaction vessel of step (1), disposablely add oxygenant and part unsaturated carboxylic acid, fully stir;
(3) be added to the water by remaining unsaturated carboxylic acid, be mixed with the pre-molten unsaturated carboxylic acid solution that mass concentration is 52%, after step (2) is stirred to and mixes, drip pre-molten unsaturated carboxylic acid solution, control time for adding is 1.5h;
(4) reductive agent and chain-transfer agent are added to the water, be mixed with the mixing solutions of reductive agent and chain-transfer agent, after step (3) residue unsaturated carboxylic acid solution is added dropwise to complete, drip the mixing solutions of reductive agent and chain-transfer agent again, control time for adding < 0.5h;
(5) after the mixing solutions of step (4) reductive agent and chain-transfer agent is added dropwise to complete, fully stirred by reaction soln, slaking 25min, then add alkaline solution, being neutralized to pH is 7, i.e. obtained high dispersive type polycarboxylate water-reducer.
In step (2), part unsaturated carboxylic acid accounts for 13% of unsaturated carboxylic acid total mass, and in step (4), in the mixing solutions of reductive agent and chain-transfer agent, the mass ratio of chain-transfer agent, reductive agent and water is 1:0.2:45.
Wherein, unsaturated Soxylat A 25-7 to be average molecular mass be 2100 isopentenol polyoxyethylene ether, degree of unsaturation >=0.37 of this isopentenol polyoxyethylene ether, hydroxyl value is 21mgKOH/g, and unsaturated carboxylic acid is methacrylic acid, and oxygenant is Potassium Persulphate, reductive agent is L-AA, chain-transfer agent is Thiovanic acid, alkaline solution to be concentration be 25% KOH solution, water is tap water.
In concrete consumption, the mass ratio of isopentenol polyoxyethylene ether and methacrylic acid total amount is 100:12, Potassium Persulphate quality is 1.5% of isopentenol polyoxyethylene ether quality, L-AA quality is 0.1% of isopentenol polyoxyethylene ether quality, and Thiovanic acid quality is 0.3% of isopentenol polyoxyethylene ether quality.
When practical application, the addition of the polycarboxylate water-reducer that the present embodiment obtains is 0.3% of cement quality.
Embodiment 6:
The preparation method of the present embodiment high dispersive type polycarboxylate water-reducer specifically comprises the following steps:
(1) under normal temperature condition, be 100:110 by the mass ratio of unsaturated Soxylat A 25-7 and water, unsaturated Soxylat A 25-7 and water are dropped in reaction vessel, be stirred well to unsaturated Soxylat A 25-7 and dissolve completely;
(2) in the reaction vessel of step (1), disposablely add oxygenant and part unsaturated carboxylic acid, fully stir;
(3) be added to the water by remaining unsaturated carboxylic acid, be mixed with the pre-molten unsaturated carboxylic acid solution that mass concentration is 50%, after step (2) is stirred to and mixes, drip pre-molten unsaturated carboxylic acid solution, control time for adding is 1h;
(4) reductive agent and chain-transfer agent are added to the water, be mixed with the mixing solutions of reductive agent and chain-transfer agent, after step (3) residue unsaturated carboxylic acid solution is added dropwise to complete, drip the mixing solutions of reductive agent and chain-transfer agent again, control time for adding < 0.5h;
(5) after the mixing solutions of step (4) reductive agent and chain-transfer agent is added dropwise to complete, fully stirred by reaction soln, slaking 10min, then add alkaline solution, being neutralized to pH is 6, i.e. obtained high dispersive type polycarboxylate water-reducer.
In step (2), part unsaturated carboxylic acid accounts for 10% of unsaturated carboxylic acid total mass, and in step (4), in the mixing solutions of reductive agent and chain-transfer agent, the mass ratio of chain-transfer agent, reductive agent and water is 1:0.8:52.
Wherein, unsaturated Soxylat A 25-7 to be average molecular mass be 2400 isopentenol polyoxyethylene ether, degree of unsaturation >=0.37 of this isopentenol polyoxyethylene ether, hydroxyl value is 26mgKOH/g, and unsaturated carboxylic acid is maleic anhydride, and oxygenant is Sodium Persulfate and ammonium persulphate is the blending oxidizing agent of 1:1 in mass ratio, reductive agent is L-AA, chain-transfer agent is Thiovanic acid, alkaline solution to be concentration be 24% NaOH solution, water is tap water.
In concrete consumption, the mass ratio of isopentenol polyoxyethylene ether and maleic anhydride total amount is 100:12.1, the total mass of Sodium Persulfate and ammonium persulphate is 1.7% of isopentenol polyoxyethylene ether quality, L-AA quality is 0.2% of isopentenol polyoxyethylene ether quality, and Thiovanic acid quality is 0.4% of isopentenol polyoxyethylene ether quality.
When practical application, the addition of the polycarboxylate water-reducer that the present embodiment obtains is 0.5% of cement quality.
Embodiment 7:
The preparation method of the present embodiment high dispersive type polycarboxylate water-reducer specifically comprises the following steps:
(1) under normal temperature condition, be 100:100 by the mass ratio of unsaturated Soxylat A 25-7 and water, unsaturated Soxylat A 25-7 and water are dropped in reaction vessel, be stirred well to unsaturated Soxylat A 25-7 and dissolve completely;
(2) in the reaction vessel of step (1), disposablely add oxygenant and part unsaturated carboxylic acid, fully stir;
(3) be added to the water by remaining unsaturated carboxylic acid, be mixed with the pre-molten unsaturated carboxylic acid solution that mass concentration is 54%, after step (2) is stirred to and mixes, drip pre-molten unsaturated carboxylic acid solution, control time for adding is 1.2h;
(4) reductive agent and chain-transfer agent are added to the water, be mixed with the mixing solutions of reductive agent and chain-transfer agent, after step (3) residue unsaturated carboxylic acid solution is added dropwise to complete, drip the mixing solutions of reductive agent and chain-transfer agent again, control time for adding < 0.5h;
(5) after the mixing solutions of step (4) reductive agent and chain-transfer agent is added dropwise to complete, fully stirred by reaction soln, slaking 15min, then add alkaline solution, being neutralized to pH is 7, i.e. obtained high dispersive type polycarboxylate water-reducer.
In step (2), part unsaturated carboxylic acid accounts for 11% of unsaturated carboxylic acid total mass, and in step (4), in the mixing solutions of reductive agent and chain-transfer agent, the mass ratio of chain-transfer agent, reductive agent and water is 1:0.6:48.
Wherein, unsaturated Soxylat A 25-7 to be average molecular mass be 2500 isopentenol polyoxyethylene ether, degree of unsaturation>=0.37 of this isopentenol polyoxyethylene ether, hydroxyl value is 23.5mgKOH/g, unsaturated carboxylic acid is maleic anhydride, and oxygenant is hydrogen peroxide, and reductive agent is L-AA, chain-transfer agent is Thiovanic acid, alkaline solution to be concentration be 23% Ca (OH)
2, water is tap water.
In concrete consumption, the mass ratio of isopentenol polyoxyethylene ether and maleic anhydride total amount is 100:12.2, hydrogen peroxide (purity is 35%) is 1.8% of isopentenol polyoxyethylene ether quality, L-AA quality is 0.3% of isopentenol polyoxyethylene ether quality, and Thiovanic acid quality is 0.5% of isopentenol polyoxyethylene ether quality.
When practical application, the addition of the polycarboxylate water-reducer that the present embodiment obtains is 0.4% of cement quality.
Claims (10)
1. the preparation method of a high dispersive type polycarboxylate water-reducer, it is characterized in that, the method is under normal temperature condition, after unsaturated Soxylat A 25-7 is mixed with water, be stirred to and dissolve completely, add oxygenant and part unsaturated carboxylic acid, be stirred well to and mix, drip the mixing solutions of solvent in advance unsaturated carboxylic acid solution, reductive agent and chain-transfer agent more successively, after being added dropwise to complete, after reaction soln is fully stirred slaking, then add alkaline solution in reaction soln, being neutralized to pH is 6-7, i.e. obtained high dispersive type polycarboxylate water-reducer.
2. the preparation method of a kind of high dispersive type polycarboxylate water-reducer according to claim 1, it is characterized in that, the method specifically comprises the following steps:
(1) under normal temperature condition, be 100:(100-130 by the mass ratio of unsaturated Soxylat A 25-7 and water), unsaturated Soxylat A 25-7 and water are dropped in reaction vessel, is stirred well to unsaturated Soxylat A 25-7 and dissolves completely;
(2) in the reaction vessel of step (1), disposablely add oxygenant and part unsaturated carboxylic acid, fully stir;
(3) remaining unsaturated carboxylic acid is added to the water, be mixed with the pre-molten unsaturated carboxylic acid solution that mass concentration is 50-55%, after step (2) is stirred to and mixes, drip pre-molten unsaturated carboxylic acid solution, control time for adding is 1-2h;
(4) reductive agent and chain-transfer agent are added to the water, be mixed with the mixing solutions of reductive agent and chain-transfer agent, after step (3) residue unsaturated carboxylic acid solution is added dropwise to complete, drip the mixing solutions of reductive agent and chain-transfer agent again, control time for adding < 0.5h;
(5) after the mixing solutions of step (4) reductive agent and chain-transfer agent is added dropwise to complete, fully stirred by reaction soln, slaking 10-30min, then add alkaline solution, being neutralized to pH is 6-7, i.e. obtained high dispersive type polycarboxylate water-reducer.
3. the preparation method of a kind of high dispersive type polycarboxylate water-reducer according to claim 2, is characterized in that, described unsaturated Soxylat A 25-7 and the mass ratio of unsaturated carboxylic acid total amount are 100:(12.0-12.3).
4. the preparation method of a kind of high dispersive type polycarboxylate water-reducer according to claim 2, is characterized in that, described oxygenant quality is the 1.5-2% of unsaturated Soxylat A 25-7 quality.
5. the preparation method of a kind of high dispersive type polycarboxylate water-reducer according to claim 2, is characterized in that, described reductive agent quality is the 0.1-0.5% of unsaturated Soxylat A 25-7 quality.
6. the preparation method of a kind of high dispersive type polycarboxylate water-reducer according to claim 2, is characterized in that, described chain-transfer agent quality is the 0.3-0.6% of unsaturated Soxylat A 25-7 quality.
7. the preparation method of a kind of high dispersive type polycarboxylate water-reducer according to claim 2, it is characterized in that, the part unsaturated carboxylic acid described in step (2) accounts for the 10-15% of unsaturated carboxylic acid total mass.
8. the preparation method of a kind of high dispersive type polycarboxylate water-reducer according to claim 2, it is characterized in that, in reductive agent described in step (4) and the mixing solutions of chain-transfer agent, the mass ratio of chain-transfer agent, reductive agent and water is 1:(0.2-1): (45-55).
9. the preparation method of a kind of high dispersive type polycarboxylate water-reducer according to claim 2, it is characterized in that, the isopentenol polyoxyethylene ether of described unsaturated Soxylat A 25-7 to be average molecular mass be 2100-2600, degree of unsaturation>=0.37 of this isopentenol polyoxyethylene ether, hydroxyl value is 23.50 ± 2.5mgKOH/g, described unsaturated carboxylic acid is vinylformic acid, one in methacrylic acid or maleic anhydride, described oxygenant is ammonium persulphate, Potassium Persulphate, one or both in Sodium Persulfate or hydrogen peroxide, described reductive agent is L-AA, described chain-transfer agent is the one in thiohydracrylic acid or Thiovanic acid, the concentration of described alkaline solution is 20-25%, and described alkaline solution is NaOH solution, KOH solution or Ca (OH)
2in one, described water is tap water.
10. the preparation method of a kind of high dispersive type polycarboxylate water-reducer according to claim 1 and 2, is characterized in that, the addition of described polycarboxylate water-reducer is the 0.3-0.5% of cement quality.
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| CN107759746A (en) * | 2017-10-08 | 2018-03-06 | 山西黄河新型化工有限公司 | The synthetic method of collapse protective poly-carboxylic acid high-performance water reducing agent |
| CN108484839A (en) * | 2018-03-23 | 2018-09-04 | 刘翠芬 | A kind of amphipathic carboxylic dispersants and preparation method thereof |
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| CN105330193A (en) * | 2015-11-24 | 2016-02-17 | 同济大学 | Polycarboxylate water reducer for ultra-compact concrete for nuclear power and preparation method of polycarboxylate water reducer |
| CN105330193B (en) * | 2015-11-24 | 2017-12-26 | 同济大学 | Nuclear power ultra dense real concrete polycarboxylate water-reducer and preparation method thereof |
| CN105542092A (en) * | 2016-01-20 | 2016-05-04 | 南京师范大学 | Method for synthesizing slow release type high slump loss resistant polycarboxylate water reducer at normal temperature |
| CN105542092B (en) * | 2016-01-20 | 2018-01-05 | 南京师范大学 | The method that normal temperature synthesizes spacetabs type high-slump-retentionpolycarboxylate polycarboxylate water reducer |
| CN106397686A (en) * | 2016-09-29 | 2017-02-15 | 湖北工业大学 | Modified polycarboxylate superplasticizer master batch and preparation method thereof |
| CN106632881A (en) * | 2016-09-29 | 2017-05-10 | 湖北工业大学 | Low water-reducing and high slump loss resistant type polycarboxylate superplasticizer master batch |
| CN107759746A (en) * | 2017-10-08 | 2018-03-06 | 山西黄河新型化工有限公司 | The synthetic method of collapse protective poly-carboxylic acid high-performance water reducing agent |
| CN108484839A (en) * | 2018-03-23 | 2018-09-04 | 刘翠芬 | A kind of amphipathic carboxylic dispersants and preparation method thereof |
| CN111825365A (en) * | 2019-09-12 | 2020-10-27 | 尧柏特种水泥技术研发有限公司 | Sulphoaluminate cement concrete additive |
| CN111635490A (en) * | 2020-06-24 | 2020-09-08 | 安徽海螺新材料科技有限公司 | Branched chain type polycarboxylate superplasticizer mother liquor and preparation method thereof |
| CN112920347A (en) * | 2021-04-07 | 2021-06-08 | 甘肃建投商品混凝土有限公司 | Preparation method of C70-based high-strength concrete crushed pebble and crushed stone concrete admixture |
| CN114772971A (en) * | 2022-04-12 | 2022-07-22 | 江苏万邦新材料科技有限公司 | Preparation method of powdery polycarboxylate superplasticizer for gypsum-based dry powder mortar |
| CN116333228A (en) * | 2023-03-16 | 2023-06-27 | 英德市竣冠新型材料有限公司 | Synthesis method of polycarboxylic acid high-performance water reducer under low temperature condition |
| CN116333228B (en) * | 2023-03-16 | 2023-09-19 | 英德市竣冠新型材料有限公司 | Synthesis method of polycarboxylic acid high-performance water reducer under low temperature condition |
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