CN104860567A - Disperse thickening agent for phosphorus gypsum based self-leveling mortar and preparation method - Google Patents
Disperse thickening agent for phosphorus gypsum based self-leveling mortar and preparation method Download PDFInfo
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- CN104860567A CN104860567A CN201510238807.3A CN201510238807A CN104860567A CN 104860567 A CN104860567 A CN 104860567A CN 201510238807 A CN201510238807 A CN 201510238807A CN 104860567 A CN104860567 A CN 104860567A
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- leveling mortar
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Abstract
The invention relates to a disperse thickening agent for phosphorus gypsum based self-leveling mortar and a preparation method. The molecular weight of the disperse thickening agent is 110000-260000, the general molecular formula of the disperse thickening agent is shown in the instruction, a=20-45, b=10-20, c=15-35, and d=10-30. The disperse thickening agent has the advantages that the disperse thickening agent has excellent adaptability and large steric hindrance, initial and 30min fluidity can be kept at 150-180mm, exudation and separation are omitted, the water-reducing rate of the prepared disperse thickening agent can reach 27-30%, the strength of the phosphorus gypsum based self-leveling mortar can be effectively enhanced, 1d flexural and compressive strength can reach 155-206% and 144-159%, and absolute dry flexural and compressive strength can reach 134-155% and 146-156%.
Description
Technical field
The invention belongs to additive for building material field, be specifically related to a kind of dispersion thickening material for phosphogypsum based self-leveling mortar and preparation method.
Background technology
Self-leveling material is that a class can obtain smooth, firmly ornamental earth material quickly and efficiently.The focus mainly phosphogypsum based self-leveling mortar of current research, it is base-material with phosphogypsum, adds adulterant and admixture, for the new terrestrial material of ground self-leveling.
Phosphogypsum is the sulfate dihydrate Ca-deposit containing a small amount of undecomposed phosphorus ore and free acid of discharging in the process of Wet-process phosphoric acid (WPPA), is topmost industry byproduct during phosphorous chemical industry is produced.Due to raw-material source and the difference such as production technique of producing phosphoric acid, the phosphogypsum of different place discharges there are differences, this makes the complicated component of phosphogypsum, impure kind is more, gravity flowing levelling mortar will ensure larger mobility simultaneously, this makes water-cement ratio increase, and the water tolerance and intensity that cause gravity flowing levelling mortar reduce by these, have a strong impact on the performance of phosphogypsum based self-leveling mortar.Phosphogypsum based self-leveling mortar is the effective way solving China's phosphogypsum solid waste bulk deposition, but due to phosphogypsum complicated component, the reasons such as impurity is more cause phosphogypsum based self-leveling mortar to there is certain problem, limit the recycling of phosphogypsum, therefore searce way improves that phosphogypsum based self-leveling mortar exists water tolerance, intensity reduces and keep the problem such as high workability to be extremely urgent.
But the problem solving phosphogypsum based self-leveling mortar mobility at present generally adopts traditional water reducer, but all there is following problem:
(1) bad adaptability.Be adapted to the conventional water reducing agents of certain phosphogypsum, due to the change of phosphogypsum composition, the change of dopant species, traditional water reducer cannot adapt to this kind of phosphogypsum, do not have desirable water-reducing effect, therefore traditional water reducer is for the changeable phosphogypsum bad adaptability of composition.
(2) mobility hold facility is poor.For phosphogypsum based self-leveling mortar, require that 30mi liquidity value added is less, have good mobility, traditional method adopts retardant to delay gypsum aquation, thus improves the flowing retentivity of slurry.But retardant can delay aquation, reduce early strength.
(3) slurry stability is poor.The slurry stability of gravity flowing levelling mortar is an important indicator.For avoiding segregation, the problems such as bleeding, traditional method adds thickening material and improves slurry stability, but easily causes detrimentally affect to mobility and intensity, and volume sensitivity is wayward simultaneously.
Therefore, how to solve phosphogypsum base mortar high workability problem and become the technical bottleneck restricting phosphogypsum and apply in gravity flowing levelling mortar field.Be necessary that research is a kind of and there is stronger adaptability, be applied to the dispersion thickening material of phosphogypsum gravity flowing levelling mortar, solve the water tolerance of phosphogypsum based self-leveling mortar existence, intensity reduction and keep the problems such as high workability.
Summary of the invention
Technical problem to be solved by this invention proposes a kind of dispersion thickening material for phosphogypsum based self-leveling mortar and preparation method for above-mentioned prior art, it can improve the resistance to water problems of phosphogypsum based self-leveling mortar effectively, improve mobility, gain in strength simultaneously.
The problem that the present invention is the above-mentioned proposition of solution by the following technical solutions: a kind of dispersion thickening material for phosphogypsum based self-leveling mortar, is characterized in that, its molecular weight is 110000 ~ 260000, and its general structure is:
Wherein, a=20 ~ 45, b=10 ~ 20, c=15 ~ 35, d=10 ~ 30.
The preparation method of the described dispersion thickening material for phosphogypsum based self-leveling mortar, is characterized in that, include following steps:
1) starting material are chosen: by the chain-transfer agent of the polyether macromonomer of 45 ~ 65wt%, 15 ~ 35wt% vinylformic acid, 7 ~ 25wt% vinylbenzene, 10 ~ 30% methylpropene sodium sulfonates, the oxygenant of 1.0 ~ 1.5wt%, the reductive agent of 1.0 ~ 1.5wt% and 0.5 ~ 1.0wt%, each component total amount is 100% above, chooses starting material;
2) by described polyether macromonomer, vinylformic acid, vinylbenzene, methylpropene sodium sulfonate stirring and dissolving, obtain homogeneous solution, then add oxygenant, stir and obtain homogeneous solution;
3) by poly-for step 2) in institute obtain in homogeneous solution, disposable reductive agent and the chain-transfer agent mixture of adding, and continue stirring 3 ~ 4h, regulates pH to neutral, adds suitable deionized water, obtain the dispersion thickening material for phosphogypsum based self-leveling mortar.
By such scheme, described polyether macromonomer is prenol epoxy ethane-epoxy propane-oxyethane tri-block base ether, and its molecular structure is as follows:
By such scheme, the preparation method of prenol epoxy ethane-epoxy propane-oxyethane tri-block base ether is as follows:
A) prenol and sodium methoxide catalyst are uniformly mixed in encloses container, are warming up to 75 DEG C ~ 120 DEG C, and are incubated 0.5h;
B) be warmed up to 115 DEG C ~ 135 DEG C, within 1.5h, evenly add oxyethane, and be incubated 0.5h;
C) keep temperature-resistant, within 0.5h, evenly add propylene oxide, and be incubated 0.5h;
D) continue to be warmed up to 140 DEG C ~ 165 DEG C, within 1.5h, evenly add oxyethane, and be incubated 0.5h, obtain prenol epoxy ethane-epoxy propane-oxyethane tri-block base ether;
Wherein, step b), c), d) in oxyethane used: propylene oxide: the mol ratio of oxyethane is 60:3:60, sodium methylate consumption be prenol, oxyethane, propylene oxide total mass 0.5%.
By such scheme, described oxygenant is Potassium Persulphate, ammonium persulphate, tertbutyl peroxide any two or three mixes, and when being the mixing of two kinds, its mol ratio is 1:1, and when being the mixing of three kinds, its mol ratio is 1:1:1.
By such scheme, described reductive agent is sodium hypophosphite, S-WAT, L-AA any two or three mixes, and when being the mixing of two kinds, its mol ratio is 1:1, and when being the mixing of three kinds, its mol ratio is 1:1:1.
By such scheme, described chain-transfer agent is mercaptoethanol, thiohydracrylic acid mixture forms, and its mol ratio is 2:1.
Building-up reactions equation of the present invention is as follows:
A) pentenol epoxy ethane-epoxy propane-oxyethane tri-block base ether building-up reactions equation
B) thickening material building-up reactions equation is disperseed
Compared with commercially available conventional water reducing agents, beneficial effect of the present invention is:
1) the dispersion thickening material that prepared by the present invention can overcome phosphogypsum complicated component, the problem that impurity is more, has good adaptability to phosphogypsum based self-leveling mortar;
2) the dispersion thickening material that prepared by the present invention has larger sterically hindered, can well disperse phosphogypsum particle, make phosphogypsum based self-leveling mortar keep larger mobility, initial and 30min degree of mobilization can keep 150 ~ 180mm, and bleeding, segregation do not occur;
3) water-reducing rate of dispersion thickening material that prepared by the present invention can reach 27 ~ 30%, effectively can strengthen the intensity of phosphogypsum based self-leveling mortar, relatively do not mix the gravity flowing levelling mortar intensity of water reducer, the anti-crimping intensity of relative 1d can reach 155 ~ 206%, 144 ~ 159%, and the anti-crimping intensity of relative over dry can reach 134 ~ 155%, 146 ~ 156%.
Embodiment
For illustrating further content of the present invention, exemplifying following examples especially and the present invention is described in further detail.Embodiment provides by way of illustration, but is never only confined to content of the present invention.Protection scope of the present invention is as the criterion with claim specification sheets.
For a dispersion thickening material for phosphogypsum based self-leveling mortar, its molecular weight is 110000 ~ 260000, and its general structure is:
Wherein, a=20 ~ 45, b=10 ~ 20, c=15 ~ 35, d=10 ~ 30.
Embodiment proportioning is as shown in table 1, and specific implementation process is as follows:
1) by polyether macromonomer, vinylformic acid, vinylbenzene, methylpropene sodium sulfonate stirring and dissolving, obtain homogeneous solution, then add oxygenant, stir and obtain homogeneous solution;
2) by poly-for step 1) in institute obtain in homogeneous solution, disposable reductive agent and the chain-transfer agent mixture of adding, and continue to stir 3h, regulates pH to neutral, adds suitable deionized water, obtain the dispersion thickening material for phosphogypsum based self-leveling mortar.
Wherein, polyether macromonomer is prenol epoxy ethane-epoxy propane-oxyethane tri-block base ether, and its molecular structure is as follows:
Its preparation method is as follows:
A) prenol and sodium methoxide catalyst are uniformly mixed in encloses container, are warming up to 75 DEG C ~ 120 DEG C, and are incubated 0.5h;
B) be warmed up to 115 DEG C ~ 135 DEG C, within 1.5h, evenly add oxyethane, and be incubated 0.5h;
C) keep temperature-resistant, within 0.5h, evenly add propylene oxide, and be incubated 0.5h;
D) continue to be warmed up to 140 DEG C ~ 165 DEG C, within 1.5h, evenly add oxyethane, and be incubated 0.5h, obtain prenol epoxy ethane-epoxy propane-oxyethane tri-block base ether.
Wherein, step b), c), d) in oxyethane used: propylene oxide: the mol ratio of oxyethane is 60:3:60, sodium methylate consumption be prenol, oxyethane, propylene oxide total mass 0.5%.
Described oxygenant is Potassium Persulphate, ammonium persulphate, tertbutyl peroxide any two or three mixes, when being the mixing of two kinds, its mol ratio is 1:1 (embodiment 1-6), and when being the mixing of three kinds, its mol ratio is 1:1:1 (embodiment 7-12).
Described reductive agent is sodium hypophosphite, S-WAT, L-AA any two or three mixes, when being the mixing of two kinds, its mol ratio is 1:1 (embodiment 1-6), and when being the mixing of three kinds, its mol ratio is 1:1:1 (embodiment 7-12).
Described chain-transfer agent is mercaptoethanol, thiohydracrylic acid mixture forms, and its mol ratio is 2:1.
One kind, table 1 is for the dispersion thickening material proportioning of phosphogypsum based self-leveling mortar
The proportioning of phosphogypsum based self-leveling mortar is as shown in table 2, and (embodiment) a kind of effect of the dispersion thickening material for phosphogypsum based self-leveling mortar of synthesizing is as shown in table 3 as stated above.
The proportioning of table 2 phosphogypsum based self-leveling mortar
| Phosphogypsum/g | Breeze/g | Cement/g | Sand/g | Water/g | Retardant/g | Water reducer/g |
| 450 | 115 | 45 | 900 | 260 | 11.25 | 22.5 |
Table 3 disperses thickening material effect
Note: in experiment cement used be new No. 42.5,01, the P.O of China used be commercially available conventional water reducing agents.
Evaluation to the product of above 14 embodiments:
The test of phosphogypsum based self-leveling mortar is carried out according to JC/T 1023-2007 " gypsum base gravity flowing levelling mortar " regulation.As can be seen from the table, compared with commercially available conventional water reducing agents, adopt dispersion thickening material of the present invention, its water-reducing rate, degree of mobilization and intensity are all greatly improved, water-reducing rate can reach 27 ~ 30%, degree of mobilization can keep 150 ~ 180mm, and the anti-crimping intensity of 1d can reach 5 ~ 7MPa, 14 ~ 17MPa, and the anti-crimping intensity of over dry can reach 13 ~ 15MPa, 30 ~ 32MPa.Relative to the blank mortar strength of not mixing water reducer, the anti-crimping intensity of 1d can reach 155 ~ 206%, 144 ~ 159%, and the anti-crimping intensity of over dry can reach 134 ~ 155%, 146 ~ 156%.Therefore dispersion thickening material of the present invention can solve that phosphogypsum based self-leveling mortar exists water tolerance, intensity reduces and keep the problem such as high workability, and has good adaptability.
Claims (7)
1. for a dispersion thickening material for phosphogypsum based self-leveling mortar, it is characterized in that, its molecular weight is 110000 ~ 260000, and its general structure is:
Wherein, a=20 ~ 45, b=10 ~ 20, c=15 ~ 35, d=10 ~ 30.
2. the preparation method of the dispersion thickening material for phosphogypsum based self-leveling mortar according to claim 1, is characterized in that, include following steps:
1) starting material are chosen: by the chain-transfer agent of the polyether macromonomer of 45 ~ 65wt%, 15 ~ 35wt% vinylformic acid, 7 ~ 25wt% vinylbenzene, 10 ~ 30% methylpropene sodium sulfonates, the oxygenant of 1.0 ~ 1.5wt%, the reductive agent of 1.0 ~ 1.5wt% and 0.5 ~ 1.0wt%, each component total amount is 100% above, chooses starting material;
2) by described polyether macromonomer, vinylformic acid, vinylbenzene, methylpropene sodium sulfonate stirring and dissolving, obtain homogeneous solution, then add oxygenant, stir and obtain homogeneous solution;
3) by poly-for step 2) in institute obtain in homogeneous solution, disposable reductive agent and the chain-transfer agent mixture of adding, and continue stirring 3 ~ 4h, regulates pH to neutral, adds suitable deionized water, obtain the dispersion thickening material for phosphogypsum based self-leveling mortar.
3. the preparation method of the dispersion thickening material for phosphogypsum based self-leveling mortar according to claim 2, it is characterized in that: described polyether macromonomer is prenol epoxy ethane-epoxy propane-oxyethane tri-block base ether, and its molecular structure is as follows:
4. the preparation method of the dispersion thickening material for phosphogypsum based self-leveling mortar according to claim 3, is characterized in that: the preparation method of prenol epoxy ethane-epoxy propane-oxyethane tri-block base ether is as follows:
A) prenol and sodium methoxide catalyst are uniformly mixed in encloses container, are warming up to 75 DEG C ~ 120 DEG C, and are incubated 0.5h;
B) be warmed up to 115 DEG C ~ 135 DEG C, within 1.5h, evenly add oxyethane, and be incubated 0.5h;
C) keep temperature-resistant, within 0.5h, evenly add propylene oxide, and be incubated 0.5h;
D) continue to be warmed up to 140 DEG C ~ 165 DEG C, within 1.5h, evenly add oxyethane, and be incubated 0.5h, obtain prenol epoxy ethane-epoxy propane-oxyethane tri-block base ether;
Wherein, step b), c), d) in oxyethane used: propylene oxide: the mol ratio of oxyethane is 60:3:60, sodium methylate consumption be prenol, oxyethane, propylene oxide total mass 0.5%.
5. the preparation method of the dispersion thickening material for phosphogypsum based self-leveling mortar according to claim 2, it is characterized in that: described oxygenant is Potassium Persulphate, ammonium persulphate, tertbutyl peroxide any two or three mixes, when being the mixing of two kinds, its mol ratio is 1:1, when being the mixing of three kinds, its mol ratio is 1:1:1.
6. the preparation method of the dispersion thickening material for phosphogypsum based self-leveling mortar according to claim 2, it is characterized in that: described reductive agent is sodium hypophosphite, S-WAT, L-AA any two or three mixes, when being the mixing of two kinds, its mol ratio is 1:1, when being the mixing of three kinds, its mol ratio is 1:1:1.
7. the preparation method of the dispersion thickening material for phosphogypsum based self-leveling mortar according to claim 2, it is characterized in that: described chain-transfer agent is mercaptoethanol, thiohydracrylic acid mixture forms, its mol ratio is 2:1.
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| CN101786824A (en) * | 2010-02-26 | 2010-07-28 | 北京新中岩建材科技有限公司 | Plastic retaining type polyether assemblage carboxylic acid high-performance water reducing agent and preparation method thereof |
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