CN109503009A - A kind of modified magnesium sulfate cement and preparation method thereof - Google Patents
A kind of modified magnesium sulfate cement and preparation method thereof Download PDFInfo
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- CN109503009A CN109503009A CN201811491584.1A CN201811491584A CN109503009A CN 109503009 A CN109503009 A CN 109503009A CN 201811491584 A CN201811491584 A CN 201811491584A CN 109503009 A CN109503009 A CN 109503009A
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- magnesium sulfate
- magnesia
- sulfuric acid
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- flyash
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B9/00—Magnesium cements or similar cements
- C04B9/04—Magnesium cements containing sulfates, nitrates, phosphates or fluorides
Abstract
The present invention provides a kind of preparation method of modified magnesium sulfate cement, the method is as follows: (1) it is spare to weigh the concentrated sulfuric acid, superfined flyash, magnesia and water according to a certain percentage；(2) concentrated sulfuric acid is added in a certain amount of spare water and prepares dilution heat of sulfuric acid, superfined flyash is then added, stir to get activation modification superfined flyash；(3) the 10 ~ 20% of spare magnesia are slowly added into step (2) resulting mixture, adjusting stirring dissolves activated magnesia sufficiently, obtains flyash and Adlerika mixture；(4) a certain amount of additive is weighed (to be added in remaining water, be added to after stirring and dissolving at room temperature in the mixture that step (3) obtains, continuously add remaining magnesia, stir 30 ~ 60 min, obtain sticky magnesium sulfate water cement paste；The 28 days compression strength of magnesium sulfate cement that the present invention obtains is and easy to operate, low in cost up to 66.96 MPa, it is easy to accomplish industrialization.
Description
Technical field
The present invention relates to a kind of magnesium sulfate cement and preparation method thereof, particularly belong to one kind with activation modification superfined flyash
For the modification magnesium sulfate cement and preparation method thereof of filler.
Background technique
Magnesia-based cements have many advantages, such as fast solidifying, high-strength, wear-resisting, are the important supplement of ordinary portland cement, Devoting Major Efforts To Developing magnesium-based water
Mud is to the functional promotion of construction material, energy conservation and environmental protection, CO2Emission reduction, magnesium resource, which recycle etc., to be of great significance.Magnesia-based cements
It mainly include phosphorus-oxygen-magnesium cement, magnesia oxychloride cement and magnesium oxysulfide concrete, wherein magnesium oxysulfide concrete has and phosphorus-oxygen-magnesium cement and chlorine
The advantages that oxygen magnesium cement similar light, fast solidifying, early strong and wear-resisting, but the halogen moisture absorption, water-resistance are returned there is no magnesia oxychloride cement
The disadvantages of difference and chloride ion are to the strong corrosive of reinforcing bar, is the magnesium cement of most possible scale application.But magnesium oxysulfide water
The mechanical property of mud is poor, it is difficult to meet actual demand.
Flyash is large Industrial Solid Waste that coal-burning power plant generates, and is that silicon is widely applied since it is with pozzolanic properties
Mineral admixture in acid salt cement.In recent years, flyash also has relevant report as filler in the preparation of magnesium-based cementitious material.
Such as, patent CN106747240A proposes a kind of alkaline magnesium oxysulfide concrete and preparation method thereof, raw material mainly have light calcined magnesia,
Magnesium desulfurization byproduct epsom salt and flyash are conducive to insoluble crystalline substance due to using inorganic, organic assembling additive
The formation of palpus, improves the properties of magnesium oxysulfide concrete.Obtained 28 days maximum compression strengths of test block are up to 67.9 ~ 72.5
MPa, flexural strength is up to 19.5 MPa, and 120 days coefficient of softing are up to 0.88 ~ 0.95.
Patent CN106554160A, which is proposed, directly prepares rapid hardening magnesium oxysulfide concrete using the Waste Sulfuric Acid that concentration is 45 ~ 50%
Method, not only solve the processing of industrial waste sulfuric acid, also reduce the preparation of magnesium sulfate and its preparation link of solution, reduce
The production cost of magnesium oxysulfide concrete, prepared 28 days compression strength of cement are 32.3 ~ 65.3 MPa, flexural strength is 3.2 ~
12.6 MPa.Patent CN107473614A discloses a kind of water-fast highly resistance folding magnesium oxysulfide inorganic coagulation material and preparation method thereof,
Due to the incorporation of high-quality fly ash (containing 70% globular glass body), the heat of hydration and drying shrinkage of cementitious material are reduced, effectively
The performances such as impermeability, frost resistance, elasticity modulus, mechanics are improved, the flexural strength of 28 day age reaches 22-23 MPa, is made
Standard rubber sand test specimen water resistance with higher, coefficient of softing is suitable for being impregnated by water or in moist ring up to 0.90 or so
In the important feature in border.In modified magnesium oxysulfide concrete preparation method disclosed in patent CN102924038A, when with formic acid and formic acid
Salt be additive, using flyash as filler when, the compression strength of obtained cement briquette be respectively 69 and 73 MPa have it is excellent
Different mechanical property, alternative magnesia oxychloride cement is for producing the materials such as mortar, concrete, plate, craftwork.
But in above-mentioned preparation method reported in the literature, flyash is only a kind of common mine in magnesium-based cementitious material
Object filler, the performance boost of cementitious material is only limitted to fill it is closely knit, also without components such as apparent its surface-active aluminium, silicon in glue
Mechanism of action in gel material.Further to strengthen mechanism of action of the flyash in magnesium-based cementitious material, magnesium sulfate water is improved
The properties of mud need to develop new preparation method and process route.
Summary of the invention
The problem of the purpose of the present invention is to solve the novel processing steps of modified magnesium sulfate cement, provides one kind and changes
The preparation method of property magnesium sulfate cement.
The technical solution of this method is that a kind of Preparation Method of modified magnesium sulfate cement includes the following steps:
(1) it is 1:0.42 ~ 1.64:1.72 ~ 3.86 according to the mass ratio of the concentrated sulfuric acid, superfined flyash, activated magnesia, water:
3.48 ~ 4.75 to weigh a certain amount of concentrated sulfuric acid, superfined flyash, magnesia and water spare；
(2) concentrated sulfuric acid is added to the dilution heat of sulfuric acid of preparation 10 ~ 30% in a certain amount of spare water, superfined flyash is then added,
1 ~ 5 h is stirred at room temperature, obtains activation modification superfined flyash；
(3) the 10 ~ 20% of spare magnesia are added step-wise in step (2) resulting mixture, the stirring of the side Bian Tianjia is adjusted
Stirring rate is 100 ~ 500 r/min, stirs 0.5 ~ 2 h, continues 10 ~ 30 min of stirring after addition, make activated magnesia
Sufficiently dissolution, obtains flyash and Adlerika mixture；
(4) it is 0.5 ~ 2:100 according to additive and activated magnesia mass ratio, weighs a certain amount of additive and remaining water is added
In, it is added to after stirring and dissolving in the mixture that step (3) obtains at room temperature, 5 ~ 10 min of stirring mixing sufficiently, continuously adds
Remaining magnesia stirs 30 ~ 60 min, obtains sticky magnesium sulfate water cement paste；
(5) cement paste that (4) obtain is poured into three gang mould of standard stainless steel (40 × 40 × 40 mm), is placed in cement
60 s floating is vibrated on glue sand plain bumper, is demoulded after test specimen is conserved one day at room temperature, continues maintenance at room temperature to test
Age.
Additive is one of following substance: citric acid and citrate, tartaric acid and tartrate, phosphoric acid and phosphate
Class, sucrose, glucose etc.)
Preferably, in described (1) step, the concentration of dilution heat of sulfuric acid is 20 ~ 25%, and dilute sulfuric acid can be industrial waste sulfuric acid,
Preferably, in described (1) step, the partial size of superfined flyash is 1 ~ 5 μm.
Preferably, in described (1) step, the concentrated sulfuric acid, superfined flyash, activated magnesia, water mass ratio be 1:
0.42~1.64:2.15~3.43:3.48~4.75。
Preferably, in described (2) step, the additional amount of magnesia is controlled 15%.
Preferably, in described (3) step, additive optimization citric acid or sodium citrate.
Advantages of the present invention and effect compared with prior art: (1) present invention is used using dilution heat of sulfuric acid as reaction medium
" one kettle way ", directly by flyash activating, modified, Adlerika is prepared and the preparation of magnesium sulfate cementitious material is reacted at one
It is sequentially completed in kettle.Firstly, dilution heat of sulfuric acid as flyash activating modifying agent, at normal temperature performs etching fine coal gray surface
Activation, enters soluble surface aluminium and amorphous silicon in solution, and cellular is presented in surface topography, and active site increases；Secondly,
It is taken in technique and part (rather than all) magnesia is first added in sulfuric acid and mixture of fly ash to prepare magnesium sulfate molten
Liquid is gradually added remaining magnesia, is more advantageous to the generation of 517 phases, reduces magnesium hydroxide then after additive addition
It generates.(2) flyash that the present invention selects is superfine powder, and particle diameter distribution is about 1 ~ 10 μm, is crushed by supersonic speed steam,
On the one hand available micron-sized superfined flyash particle dramatically increases surface energy, gives full play to its pozzolanic properties；It is another
Aspect, fly ash grain fine, be conducive to surface etch activation degree improve and surface area increase, strengthen 517 phase gels with
Glue connection effect between fly ash grain, to improve the compression strength of magnesium sulfate cement.(3) enter solution in soluble aluminum and
Amorphous silicon can further occur with magnesium ion hydration reaction (as reacted shown in (1), (2)), generate insoluble aluminium (silicon)
Magnesium gelled product forms fine pore structure, further increases the compression strength of cement.
The principle of the invention is as follows:
Detailed description of the invention
Fig. 1 is aluminium, iron, calcium content in filtrate obtained by the sulfuric acid activated superfined flyash of 1 various concentration of embodiment.
Fig. 2 is the SEM figure of the sulfuric acid activated flyash of various concentration in superfined flyash (a) and embodiment 1, (b) 10% dilute sulphur
Acid, (c) 20% dilute sulfuric acid, (d) 30% dilute sulfuric acid.
Fig. 3 is the XRD diagram of the sulfuric acid activated flyash of various concentration in superfined flyash (a) and embodiment 1, (b) 10% dilute sulphur
Acid, (c) 20% dilute sulfuric acid, (d) 30% dilute sulfuric acid.
Fig. 4 is that embodiment 2,3,4 and comparative example 5 obtain the SEM figure of magnesium sulfate cement: mixing 10% activation fine coal in (a)
Ash, (b) in mix 20% activating fly ash, (c) in mix 30% activating fly ash, (d) not fly ash.
Fig. 5 is that embodiment 2,3,4 and comparative example 5 obtain the XRD diagram of magnesium sulfate cement: mixing 10% activation fine coal in (a)
Ash, (b) in mix 20% activating fly ash, (c) in mix 30% activating fly ash, (d) not fly ash.
From fig. 1, it can be seen that with the increase of dilute sulfuric acid concentration, aluminium, iron the amount of dissolution gradually increase, the amount of dissolution of calcium is reduced,
When dilute sulfuric acid concentration is 20%, the aluminium content in solution is up to 2 g/L or more.
As can be seen from Figure 2, when dilute sulfuric acid concentration is 20%, a large amount of honeycomb is presented in superfined flyash surface.
As can be seen from Figure 3, with the increase of dilute sulfuric acid concentration, the diffraction maximum of CaSO4 is gradually increased in modified coal ash.
From fig. 4, it can be seen that not fly ash when, obtain 517 phase crystal of shank shape；When volume is 10%, although crystal becomes
Carefully, short, but it is finer and close；When mixing 20%, crystal is elongated to attenuate；The intensity of corresponding test block increases to 66.96 by 43.16 MPa
MPa, but when volume is up to 30%, becomes cotton-shaped fine crystals, the strength reduction of test block to 49.88 MPa.
From fig. 5, it can be seen that the peak intensity of 517 phases gradually weakens with the interior increase for mixing activating fly ash.
Specific embodiment
Combined with specific embodiments below and attached drawing, the content that the present invention is further explained.
Experimental example 1
Three part of 10 g superfined flyash (1 ~ 5 μm) is weighed, the dilute sulfuric acid that 100 mL concentration are 10%, 20%, 30% is added separately to
In solution, it is separated by filtration after stirring 2 h at room temperature.Aluminium, iron, the calcium in filtrate are measured using ICP, the result is shown in Figure 1；It will
Obtained solid powder is washed with deionized to neutrality, after 105 DEG C of 3 ~ 5 h of drying, is characterized using SEM and XRD, knot
Fruit sees Fig. 2,3；Its specific surface area is measured using nitrogen absorption under low temperature, as a result the m of respectively 19,48 and 282/g。
Embodiment 1
It (1) is 1:0.42:2.15:3.69 according to the mass ratio of the concentrated sulfuric acid, superfined flyash (1 ~ 5 μm), activated magnesia, water
Weigh that concentrated sulfuric acid 58.80g, superfined flyash 24.96g, magnesia 126.05g and water 217.26g are spare, and (2) add the concentrated sulfuric acid
Enter into the spare water of 204.63g and prepare 20% dilution heat of sulfuric acid, superfined flyash is then added, stirs 2h at room temperature, is lived
Change modified superfine flyash；(3) 15% 18.91g of spare magnesia is slowly added into step (2) resulting mixture,
Adjusting stirring rate is 400 r/min, stirs 1.5 h, continues to stir 15 min after addition, keeps activated magnesia sufficiently molten
Solution, obtains flyash and Adlerika mixture；(4) it is 1:100 according to additive and activated magnesia mass ratio, weighs
1.26g citric acid is added in remaining water, is added to after stirring and dissolving in the mixture that step (3) obtains at room temperature, stirring 10
Min mixing sufficiently, continuously adds remaining magnesia, stirs 30min, obtains sticky magnesium sulfate water cement paste；(5) by (4)
Obtained cement paste is poured into three gang mould of standard stainless steel (40 × 40 × 40 mm), is placed on cement mortar plain bumper
60 s floating is vibrated, is demoulded after test specimen is conserved one day at room temperature, continuation was conserved at room temperature to 28 days, obtained magnesium sulfate water
The compression strength of mud test block is 53.39 MPa, carries out SEM and XRD characterization to the test block, sees Fig. 4 (a), Fig. 5 (a).
Embodiment 2
It (1) is 1:0.95:2.58:4.16 according to the mass ratio of the concentrated sulfuric acid, superfined flyash (1 ~ 5 μm), activated magnesia, water
Weigh that concentrated sulfuric acid 58.80g, superfined flyash 56.19g, magnesia 151.26g and water 244.44g are spare, and (2) add the concentrated sulfuric acid
Enter into the spare water of 204.63g and prepare 20% dilution heat of sulfuric acid, superfined flyash is then added, stirs 2 h at room temperature, obtains
Activation modification superfined flyash；3) 15% 22.69g of spare magnesia is slowly added into step (2) resulting mixture,
Adjusting stirring rate is 400 r/min, stirs 1.5 h, continues to stir 15 min after addition, keeps activated magnesia sufficiently molten
Solution, obtains flyash and Adlerika mixture；(4) it is 1:100 according to additive and activated magnesia mass ratio, weighs
1.51g citric acid is added in remaining water, is added to after stirring and dissolving in the mixture that step (3) obtains at room temperature, stirring 10
Min mixing sufficiently, continuously adds remaining magnesia, stirs 30min, obtains sticky magnesium sulfate water cement paste；(5) by (4)
Obtained cement paste is poured into three gang mould of standard stainless steel (40 × 40 × 40 mm), is placed on cement mortar plain bumper
60 s floating is vibrated, is demoulded after test specimen is conserved one day at room temperature, continuation was conserved at room temperature to 28 days.Obtain magnesium sulfate water
The compression strength of mud test block is 66.96MPa, carries out SEM and XRD characterization to the test block, sees Fig. 4 (b), Fig. 5 (b).
Embodiment 3
It (1) is 1:1.64:3.43:4.75 according to the mass ratio of the concentrated sulfuric acid, superfined flyash (1 ~ 5 μm), activated magnesia, water
Weigh that concentrated sulfuric acid 58.80g, superfined flyash 96.33g, magnesia 201.68g and water 279.33g are spare, and (2) add the concentrated sulfuric acid
Enter into the spare water of 204.63g and prepare 20% dilution heat of sulfuric acid, superfined flyash is then added, stirs 2 h at room temperature, obtains
Activation modification superfined flyash；3) 15% 30.25g of spare magnesia is slowly added into step (2) resulting mixture,
Adjusting stirring rate is 400 r/min, stirs 1.5 h, continues to stir 15 min after addition, keeps activated magnesia sufficiently molten
Solution, obtains flyash and Adlerika mixture；(4) it is 1:100 according to additive and activated magnesia mass ratio, weighs
2.02g citric acid is added in remaining water, is added to after stirring and dissolving in the mixture that step (3) obtains at room temperature, stirring 10
Min mixing sufficiently, continuously adds remaining magnesia, stirs 30min, obtains sticky magnesium sulfate water cement paste；(5) by (4)
Obtained cement paste is poured into three gang mould of standard stainless steel (40 × 40 × 40 mm), is placed on cement mortar plain bumper
60 s floating is vibrated, is demoulded after test specimen is conserved one day at room temperature, continuation was conserved at room temperature to 28 days.Magnesium sulfate is obtained
The compression strength of cement briquette is 49.88MPa, carries out SEM and XRD characterization to the test block, sees Fig. 4 (c), Fig. 5 (c).
Comparative example 4
It (1) is that 1:2.58:3.48 weighs concentrated sulfuric acid 58.80g, magnesia according to the mass ratio of the concentrated sulfuric acid, activated magnesia, water
151.26g spare with water 204.63g；(2) concentrated sulfuric acid is added to the dilution heat of sulfuric acid of preparation 20% in the spare water of 204.63g, so
15% 22.69g of spare magnesia is slowly added into step (1) resulting mixture afterwards, adjusting stirring rate is 400
R/min stirs 1.5 h, continues to stir 15 min after addition, dissolves activated magnesia sufficiently, obtain flyash and sulphur
Sour magnesium solution mixture；(3) it is 1:100 according to additive and activated magnesia mass ratio, weighs 1.51g citric acid and be added to step
Suddenly in the mixture that (2) obtain, 10 min of stirring mixing sufficiently, continuously adds remaining magnesia, stirs 30min, glued
Thick magnesium sulfate water cement paste；(5) cement paste that (4) obtain is poured into three gang mould (40 × 40 × 40 of standard stainless steel
Mm it in), is placed on cement mortar plain bumper and vibrates 60 s floating, demoulded after test specimen is conserved one day at room temperature, continued in room
The lower maintenance of temperature was to 28 days.The compression strength for obtaining the magnesium sulfate cement of not fly ash is 43.16MPa, carries out SEM to the test block
And XRD characterization, see Fig. 4 (d), Fig. 5 (d).
Claims (7)
1. a kind of preparation method of modified magnesium sulfate cement, which is characterized in that step includes:
(1) it is 1:0.42 ~ 1.64:1.72 ~ 3.86 according to the mass ratio of the concentrated sulfuric acid, superfined flyash, activated magnesia, water:
3.48 ~ 4.75 to weigh a certain amount of concentrated sulfuric acid, superfined flyash, magnesia and water spare；
(2) concentrated sulfuric acid is added to be configured in a part of spare water 10 ~ 30% dilution heat of sulfuric acid, superfine powder is then added
Coal ash stirs 1 ~ 5 h at room temperature, obtains activation modification superfined flyash dilute sulfuric acid mixture；
(3) the 10 ~ 20% of spare magnesia are added step-wise in step (2) resulting mixture, when addition is stirred continuously, and adjusts
Section stirring rate is 100 ~ 500 r/min, stirs 0.5 ~ 2 h, continues 10 ~ 30 min of stirring after addition, make active oxidation
Magnesium sufficiently dissolves, and obtains flyash and Adlerika mixture；
(4) it is surplus to weigh a certain amount of additive addition for the ratio for being 0.5 ~ 2:100 according to additive and activated magnesia mass ratio
It in the spare water of remaining part point, is added to after stirring and dissolving in the mixture that step (3) obtains at room temperature, stirring 5 ~ 10 min mixing is filled
Point, remaining magnesia is continuously added, 30 ~ 60 min is stirred, obtains sticky magnesium sulfate water cement paste；
(5) cement paste that (4) obtain is poured into three gang mould of standard stainless steel (40 × 40 × 40 mm), is placed in cement
60 s floating is vibrated on glue sand plain bumper, is demoulded after test specimen is conserved one day at room temperature, continues maintenance at room temperature to test
Age.
2. the preparation method of modified magnesium sulfate cement according to claim 1, it is characterised in that:
Flyash described in step (1) is the superfined flyash as made from supersonic speed steam pulverizer, particle size range is 1 ~
10 μm。
3. the preparation method of modified magnesium sulfate cement according to claim 1, it is characterised in that:
Activated magnesia described in step (2) be by Qinghai Salt Lake bischofite after recrystallizing directly it is pyrogenically prepared, either
It is made by brine method, is also possible to magnesite calcining and is made.
4. the preparation method of modified magnesium sulfate cement according to claim 1, it is characterised in that: additive is following substance
One of, citric acid, citrate, tartaric acid and tartrate, phosphoric acid and phosphoric acid salt, sucrose, glucose etc..
5. the preparation method of modified magnesium sulfate cement according to claim 2, it is characterised in that: in described (1) step,
The partial size of superfined flyash is 1 ~ 5 μm.
6. the preparation method of modified magnesium sulfate cement according to claim 1, it is characterised in that: in described (3) step,
The additional amount of magnesia is controlled 15%.
7. the preparation method of modified magnesium sulfate cement according to claim 4, it is characterised in that: the additive is preferred
Citric acid or sodium citrate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110218011A (en) * | 2019-07-26 | 2019-09-10 | 南乐县美誉达建材有限公司 | A kind of technique of industrial waste sulfuric acid production plate |
| CN110357467A (en) * | 2019-07-15 | 2019-10-22 | 辽宁科大中驰镁建材科技有限公司 | A kind of modification magnesium sulfate cement and preparation method thereof that resistant to sea water corrodes |
| CN113698171A (en) * | 2021-09-08 | 2021-11-26 | 山西大学 | Surface-hydrophobic modified magnesium-based fly ash porous sound absorption material and preparation method thereof |
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| US4749413A (en) * | 1985-06-17 | 1988-06-07 | E. I. Du Pont De Nemours And Company | Phosphate cement including fly ash for high-strength concrete-like products |
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| CN102515824A (en) * | 2011-11-30 | 2012-06-27 | 南京航空航天大学 | Super-light foam cement concrete and preparation method thereof |
| CN106554160A (en) * | 2016-11-10 | 2017-04-05 | 沈阳化工大学 | A kind of method that utilization Waste Sulfuric Acid directly prepares rapid hardening magnesium oxysulfide concrete |
| CN106565118A (en) * | 2016-11-01 | 2017-04-19 | 郑文薏 | Modified magnesium cement |
| CN106747240A (en) * | 2016-12-29 | 2017-05-31 | 内蒙古中鼎工正环保有限公司 | A kind of alkaline magnesium oxysulfide concrete and preparation method thereof |
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| US4749413A (en) * | 1985-06-17 | 1988-06-07 | E. I. Du Pont De Nemours And Company | Phosphate cement including fly ash for high-strength concrete-like products |
| CN1431042A (en) * | 2003-01-17 | 2003-07-23 | 中唯炼焦技术国家工程研究中心有限责任公司 | Modified adsorbent of fly ash and method for treating waste water by using absorbent |
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| CN110357467A (en) * | 2019-07-15 | 2019-10-22 | 辽宁科大中驰镁建材科技有限公司 | A kind of modification magnesium sulfate cement and preparation method thereof that resistant to sea water corrodes |
| CN110218011A (en) * | 2019-07-26 | 2019-09-10 | 南乐县美誉达建材有限公司 | A kind of technique of industrial waste sulfuric acid production plate |
| CN113698171A (en) * | 2021-09-08 | 2021-11-26 | 山西大学 | Surface-hydrophobic modified magnesium-based fly ash porous sound absorption material and preparation method thereof |
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| CN109503009B (en) | 2021-05-14 |
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