CN1498870A - Gelatinization material of phosphoaluminic salt system - Google Patents
Gelatinization material of phosphoaluminic salt system Download PDFInfo
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- CN1498870A CN1498870A CNA021357714A CN02135771A CN1498870A CN 1498870 A CN1498870 A CN 1498870A CN A021357714 A CNA021357714 A CN A021357714A CN 02135771 A CN02135771 A CN 02135771A CN 1498870 A CN1498870 A CN 1498870A
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- phosphoaluminic
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- sosoloid
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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
- C04B7/00—Hydraulic cements
- C04B7/32—Aluminous cements
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Abstract
A cementing material is a cement whose main components are calcium phosphoaluminate, calcium aluminate and calcium phosphate. Its clinker contains such chemical components (wt%) as CaO (30-60), Al2O3 (17-50), SiO2 (1-15), P2O5 (10-30), Fe2O3 (1-8) and MgO (1-7). Its advantages are high and early strength, high refractory nature, and high compatibility with existing cement.
Description
(1) technical field
The invention belongs to the inorganic materials scientific domain, particularly a kind of gelling material of energy hydration and hardening.
(2) background technology
At present, the domestic and international used cement of construction work is all based on traditional silicate cement.The cement annual production of China has reached 6.4 hundred million tons (meters in 2002), near 1/3 of Gross World Product.As developing country, the sustainable development of Chinese national economy will have significantly the demand of cement and increases, and will reach more than 800,000,000 tons to the annual requirement of China's cement in 2010.The Cement industry Development patterns of quantitative expansion can make China's energy, resource and environment can't bear the heavy load.The industry that current China Cement industry still is high consumption, poor efficiency, Environmental compatibility is poor, environmental cost is high.
Along with the development of modern construction engineering to high stratification, undergroundization, large span, heavy load, ocean direction, the emerge in multitude of Highrise buildings, large bridge, airport and high-grade highway, more and more higher to concrete requirement, the shortcoming of traditional silicate cement shows gradually, its hydration and hardening is slow, goods from great, easily produce alkali-aggregate reaction, poor durability, and defective such as function singleness can not adapt to growing modernization project needs.
For many years, the cement scientific worker is in the research of being devoted to chemistry of cement and cement industry both at home and abroad, but be the silicate cement of principal phase and mostly, and utilize industrial residue, its objective is to cut down the consumption of energy, reduce CO its super-refinement based on transforming with the tricalcium silicate mineral
2Discharging, preparation high-grade concrete.But they still are silicate system all the time.At present, China's special cement output only accounts for 1.6% of cement total amount, and developed country accounts for 5%-10% in the world.Wherein the high grade produced of China (＞60MPa) cement only accounts for 0.13% of manufacture of cement total amount, and developed country accounts for 4%-8% in the world.China's unshape refractory accounts for 30% (aluminate cement that wherein is used for unshape refractory only has 100,000 tons/year) of refractory materials total amount, and by contrast, developed country accounts for about 70% in the world.As seen, China's special cement output can not satisfy the special engineering demand at present, and the high-strength cement critical shortage.Therefore, invent a kind of high-strength, fast hard, low alkali, function more, not only can adapt to the needs of modern construction engineering with the good novel architecture gelling material of Environmental compatibility, and meet the requirement of the strategy of sustainable development.
Gelling material is one of large Material Used.At present, the hydraulic cementing materials of home and abroad widespread production and use mainly contains silicates, aluminate class, and a spot of sulplo-aluminate class that grows up in the eighties in 20th century, does not have the aluminophosphates gelling material.The phosphoric acid salt agglutinate is arranged in relating to phosphatic prior art, and it can be divided into acidifying sclerosis and hydration and hardening.About the phosphoric acid salt gelling material, since the early 1980s leaf, relevant report has appearred in succession, for example: Sugama, T.and Kukacka, L.E..Magnesium monophosphatecements derived from magnesium diammonium phosphate solutionCement and Concrete Research, the trimagnesium phosphate of 1983 13:407-416 report, Silsbee, M.R.et.al..Low temperature (＜300 ℃) phosphate ceramics fromreactive aluminas.1991, the aluminum phosphate of Materials Research Society SymposiumProceedings 179:49-58 report, binding agents such as zinc phosphate and calcium phosphate.Why be called " binding agent ", be because these materials mainly are acid-alkali cement, it condenses and sclerosis is to be caused by the oxide compound of ammonium or alkali-metal phosphoric acid salt or poly-phosphate and Mg and Zn etc. or salts reaction, they are mainly used in does high-temperature refractory, because its long-term mechanical property loss is so can not be used for engineering construction; 1986, Brown, W.E.and Chow, L.C..Anew calcium phosphate water setting cement.1986, American CeramicSociety, Westerville, OH, USA:352-359 has reported the calcium-phosphate cement of the hydraulicity, and this cement normally produces hydroxyapatite by the reaction of the calcium phosphate of two kinds of different basicity and causes setting and harden.
(3) summary of the invention
The object of the present invention is to provide a kind of dependence to generate crystal with gelling property and the common interlacing hydrated product system of gel and make member produce setting and harden, make it have the gelling material of early strong, high-strength and high-temperature flame-proof.
The object of the present invention is achieved like this:
The invention discloses a kind of gelatinization material of phosphoaluminic salt system, is a kind of cement that mainly contains phosphorus calcium aluminate and calcium phosphate composition, and the main chemical compositions content (W%) of its grog is:
CaO?????30-60????????Al
2O
3??17-50
SiO
2???1-15?????????P2O5?????10-30
Fe
2O
3?1-8??????????MgO??????1-7
Gelatinization material of phosphoaluminic salt system of the present invention forms a kind of ternary phosphorus calcium aluminate sosoloid crystalline phase (existing called after LH in the cement clinker
SsPhase), LH
SsThe crystalline structure of phase belong to etc. axle (cube) crystallographic system, three main diffraction patterns of its X-ray diffraction are d=0.3723-0.3754nm, 0.2629-0.2650nm and 0.2147-0.2160nm, its main chemical compositions content is: CaO (1-X-Y) Al
2O
3XSiO
2YP
2O
5, X=0.146-0.206, Y=0.048-0.081.
Gelatinization material of phosphoaluminic salt system of the present invention has independently clinker mineral system of as described below oneself: ternary phosphorus calcium aluminate sosoloid (existing called after LH
SsPhase), calcium aluminate sosoloid and calcium phosphate sosoloid mutually and an amount of vitreum, the essential mineral component content is (w/%):
Ternary phosphorus calcium aluminate sosoloid (LH
SsPhase) 20-70
Calcium aluminate sosoloid phase 10-60
Calcium phosphate sosoloid phase 10-60
Vitreum 0-15
Gelatinization material of phosphoaluminic salt system of the present invention has height, strong feature early in order to make it, and the content of its essential mineral (W/%) is:
Ternary phosphorus calcium aluminate sosoloid (LH
SsPhase) 20-40
Calcium aluminate sosoloid phase 30-60
Calcium phosphate sosoloid phase 10-40
Vitreum 0-15
Gelatinization material of phosphoaluminic salt system of the present invention has high temperature resistant feature in order to make it, and the content of its essential mineral (W/%) is:
Ternary phosphorus calcium aluminate sosoloid (LH
SsPhase) 40-70
Calcium aluminate sosoloid phase 10-40
Calcium phosphate sosoloid phase 25-60
Vitreum 0-15
Gelatinization material of phosphoaluminic salt system of the present invention, described gelatinization material of phosphoaluminic salt system
Its raw material is mainly derived from mineral stone lime stone, phosphatic rock and the aluminium alum.
1. the theoretical basis of aluminophosphates gelling material of the present invention:
The aluminophosphates mineral are the very stable mineral of nature, and it extensively is present in land, the seabed, also find to have the aluminophosphates mineral in the biological fossil in up to ten thousand years.From the angle of chemistry, radius is little, present the amphoteric cation compound can have good aquation, Hardenability; Consider [the PO in the crystalline structure from the crystal chemistry angle
4] to [SiO
4] and [AlO
4], and [AlO
6] and [MgO
6] double replacement degree height between waiting, again because of [PO
4] the two keys of P=O in the building stone, make the phosphor aluminate cement mineral have very high hydration activity and help phosphor aluminate cement and silicate cement compound.The applicant notices that the natural phosphate mineral of a century, stable existence in thousand have good water tolerance, characteristic such as weather-proof, resistance to chemical attack.Be subjected to the inspiration of the Nature, and invented gelatinization material of phosphoaluminic salt system.
2. the characteristics of Fa Ming gelatinization material of phosphoaluminic salt system
The present invention is a kind of novel hydration and hardening aluminophosphates gelling material.Material of the present invention adopts raw mineral materials Wingdale, phosphatic rock and alumina, levigate forming after high temperature burns till.Relying on pulverized powder to mix generation with water has the crystal of gelling property and the common interlacing hydrated product system of gel and makes member generation setting and harden.This material has oneself independently mineral composition system, that is: the ternary phosphorus calcium aluminate sosoloid that is designed and synthesized by the contriver (existing called after LH
SsPhase), calcium aluminate sosoloid and calcium phosphate sosoloid are mutually and an amount of vitreum.
Gelling material of the present invention, its slurry self early strengthening and high strengthening, hydrated product is stable, and later strength is sustainable growth still.By different proportionings and technology, can have multi-functional, as: early strong, high-strength; Compound and high-temperature flame-proof etc. with silicate cement.Its basic mechanical design feature index following (by existing GB):
1. strong, high strong type early: 12 hours ultimate compression strength 40-60MPa; 3 days ultimate compression strength 60-80MPa, 28 days ultimate compression strength＞80MPa, long-term behaviour is stable;
2. compound: good with the silicate cement composite performance, mix a small amount of compoundly with the 425# silicate cement, can improve the intensity of compound system, the alkalescence of reduction silicate cement is greatly improved the weather resistance of cement concrete.
3. high-temperature flame-proof type: the hydraulicity, 1500～1700 ℃ of use temperatures.
Aluminophosphates gelling material of the present invention is from physicochemical principle, organically combines the good and high advantage of aluminium mineral material hydration rate of phosphate mineral weather resistance.Basicity low (＜0.5%) in the system, the aquation system does not contain free SO
3, no ettringite crystalline phase and no Ca (OH)
2Hydrated product.Freeze proof, the anti-carbonization of cement slurry and excellent performance such as impervious can be avoided alkali-aggregate reaction, have the IMAGE energy.The mineral that this system's cement adopts the nature richness to deposit are main raw material, adopt the production unit of existing traditional portland and technical process to produce basically.
Aluminophosphates gelling material of the present invention be a kind of high-quality, low consumption, efficient, with the good Sustainable development kind of Environmental compatibility, it is raw materials used be extensively Wingdale, phosphatic rock, the bauxitic clay of existence of nature; Firing temperature low (about 1350-1400 ℃), and CO
2Quantity discharged is about the 50%-65% that traditional portland is produced.Structure that phosphorus calcium aluminate phase in the grog, calcium phosphate reach the calcium aluminate phase mutually and formation kinetics thereof are restricting the hydration rate and the performance of this system cement.
3. the performance of the gelatinization material of phosphoaluminic salt system of being invented
3.1 mechanical property
Table 1. phosphor aluminate cement glue sand test specimen folding strength (MPa)
Folding strength
Water/gray scale
12h 1 day 3 days 7 days 28 days
0.39-0.42???4.0-7.0??5.0-8.0??6.0-8.5??6.5-9.0???7-＞9.0
Table 2. phosphor aluminate cement glue sand test specimen ultimate compression strength (MPa)
Ultimate compression strength
Water/gray scale
12h 1 day 3 days 7 days 28 days
0.39-0.42???30-45????45-65?????55-70????60-80???70-＞80
3.2 physicals
Table 3. phosphor aluminate cement physicals
Time of coagulation (minute) stable specific surface area cement cement slurry
Property fineness proportion
Cm is boiled in initial set final set
2/ g (200 g/cm
3The pH value
The 3h mesh screen residue)
60-140 100-180 stabilizes 3000-4000 3.0-5.5 2.90 11.0-12.5
4. raw material sources of the present invention
The gelatinization material of phosphoaluminic salt system of being invented, its main chemical compositions derives from Wingdale respectively, phosphatic rock and bauxitic clay.The compositing range such as the table 4. of three kinds of raw mineral materialss
The main chemical constitution (w/%) of table 4 raw material
| Mineral | L.O.I. | ??SiO 2 | ????Al 2O 3 | ????Fe 2O 3 | ????CaO | ????MgO | ??P 2O 5 |
| Alumina | 10.5- 15.5 | ??1.0- ??13.0 | ????61.0- ????78.0 | ????0.7- ????12.0 | ????0.5- ????3.5 | ????0.1- ????2.0 | |
| Wingdale | 42.0- 43.0 | ??1.0- ??5.0 | ????0.1- ????1.0 | ????0.1- ????1.0 | ????45.0- ????54.5 | ????0.5- ????4.0 | |
| Phosphatic rock | 3.0- 7.5 | ??1.0- ??5.0 | ????1.0- ????3.0 | ????0.1- ????2.0 | ????40.0- ????55.0 | ????0.3- ????3.0 | ????27.0- ????36.0 |
Select suitable mineral stone lime stone, phosphatic rock and bauxitic clay for use.Cooperate and homogenizing according to needed chemical constitution, levigate after, through high temperature 1350-1450 calcining, the conventional high reactivity of the grog that burns till gained and 0-15% is mixed the cement of making behind material and an amount of adjustable solidification agent mix grinding.PH value=the 11.0-12.5 of slurry.Under the condition that need not ultra-fine and admixture hardening accelerator, its high and sustainable growth of intensity in 1 day-28 days, its longterm strength is high and stable, and its ultimate compression strength is more than 100MPa after 1 year.
Described gelatinization material of phosphoaluminic salt system has multifunctionality.As: resistance to elevated temperatures, but its working temperature can be up to 1500-1600 ℃; Good and silicate cement composite performance etc.425# silicate cement before complex cement glue sand test specimen 1 day and 3 days ultimate compression strength are more compound improves 20-40%, 28 days raising 7-14MPa.
Described gelatinization material of phosphoaluminic salt system has good weather resistance, as good frost resistance, anti-carbonization, and resist chemical, ability such as impervious and anti-steel bar corrosion.
Aluminophosphates of the present invention has the feature of early strong, high-strength and high-temperature flame-proof, and with existing cement good consistency is arranged.
(5) embodiment
Embodiment 1
Select suitable mineral stone lime stone, phosphatic rock and bauxitic clay for use.Cooperate and homogenizing according to needed chemical constitution, levigate after, through high temperature 1350-1400 ℃ calcining, the grog that burns till gained is regrinded into fine powder, mixes with water, amount of water is so that the slurry degree of mobilization is controlled at 118 ± 2mm for suiting.The main chemical constitution of its raw material is as shown in table 5.The chemical ingredients of raw material and grog is shown in table 6 and table 7.Phosphor aluminate cement glue sand test specimen intensity is as shown in table 8.
The main chemical constitution (w/%) of table 5 raw material
Mineral
L.O.I.???SiO
2??Al
2O
3?Fe
2O
3CaO??????MgO????P
2O
5
14.41????12.87???66.05???0.90????0.67????0.12
Alum
15.41????2.46????72.18???1.08????3.03????1.58
Soil
14.10????21.22???52.32???8.28????3.11????0.79
Stone 42.28 4.09 0.20 0.22 45.27 3.75
Ash 42.27 3.36 0.15 0.19 52.33 1.31
Stone 42.91 1.34 0.67 0.18 53.59 0.66
Phosphorus 3.36 2.89 1.20 1.28 50.38 1.44 35.27
Ash 7.35 9.53 2.19 0.87 46.50 0.68 29.58
Stone 5.66 4.71 1.47 0.18 53.48 1.90 34.18
2. embodiment 2
Form as embodiment 1 described production technique and raw material, the raw material of its phosphor aluminate cement, grog and cement mortar test specimen intensity are shown in table 6, table 7 and table 8.
The chemical ingredients of table 6. raw material (w/%)
L.O.I.??SiO
2?Al
2O
3?Fe
2O
3?CaO???MgO???P
2O
5
Example 1 20.36 5.20 37.44 1.42 24.34 2.41 8.27
Example 2 26.86 0.90 12.94 0.57 38.06 1.04 19.15
Example 3 18.82 8.86 23.61 2.51 27.38 1.80 15.37
The chemical ingredients of table 7. grog and mineralogical composition (w/%)
L.O.I.??SiO
2?Al
2O
3?Fe
2O
3?CaO???MgO???P
2O
5
Example 1 0.14 6.53 46.99 1.78 30.55 3.02 10.38
Example 2 0.37 1.23 17.69 0.78 52.06 1.42 26.20
Example 3 0.20 11.02 29.39 3.12 34.08 2.24 19.13
3. embodiment 3
Form as embodiment 1 described technology and raw material, the raw material of its aluminophosphates, grog and cement mortar test specimen intensity are shown in table 6, table 7 and table 8.
Table 8. phosphor aluminate cement glue sand test specimen intensity (MPa)
Water/folding strength ultimate compression strength
1 day 3 days 7 days 28 days 12h of gray scale 12h 1 day 3 days 7 days 28 days
Example 1 0.42 6.3 7.6 8.3 8.9 9.2 44.7 62.3 70.0 82.2 91.6
Example 2 0.39 5.2 6.1 7.9 7.9 8.4 38.2 54.7 66.1 67.0 79.5
Example 3 0.41 4.9 5.0 6.5 6.5 7.2 30.0 45.5 55.8 59.3 73.9
Claims (7)
1. a gelatinization material of phosphoaluminic salt system is a kind of cement that mainly contains phosphorus calcium aluminate, calcium aluminate and calcium phosphate composition, it is characterized in that: the main chemical compositions content (W%) of grog is:
CaO???????30-60??????Al
2O
3????17-50
SiO
2?????1-15???????P
2O
5?????10-30
Fe
2O
3???1-8????????MgO????????1-7
2. gelatinization material of phosphoaluminic salt system according to claim 1 is characterized in that: formed a kind of ternary phosphorus calcium aluminate sosoloid crystalline phase (existing called after LH in the cement clinker
SsPhase), LH
SsThe crystalline structure of phase belong to etc. axle (cube) crystallographic system, main diffraction pattern scope of tool X-ray diffraction is: d=0.3723-0.3754nm, 0.2629-0.2650nm and 0.2147-0.2160nm, its main chemical compositions content is: CaO (1-X-Y) Al
2O
3XSiO
2YP
2O
5, wherein: X-0.146-0.206, Y-0.048-0.081.
3. gelatinization material of phosphoaluminic salt system according to claim 1 and 2 is characterized in that: described gelatinization material of phosphoaluminic salt system has oneself independently clinker mineral system: ternary phosphorus calcium aluminate sosoloid (existing called after LH
SsPhase), calcium aluminate sosoloid and calcium phosphate sosoloid mutually and an amount of vitreum, essential mineral component content (w/%) is:
Ternary phosphorus calcium aluminate sosoloid (LH
SsPhase) 20-70
Calcium aluminate sosoloid phase 10-60
Calcium phosphate sosoloid phase 10-60
Vitreum 0-15
4. gelatinization material of phosphoaluminic salt system according to claim 3 is characterized in that: described gelatinization material of phosphoaluminic salt system, and essential mineral component content (W/%) is:
Ternary phosphorus calcium aluminate sosoloid (LH
SsPhase) 20-40
Calcium aluminate sosoloid phase 30-60
Calcium phosphate sosoloid phase 10-40
Vitreum 0-15
5. gelatinization material of phosphoaluminic salt system according to claim 3 is characterized in that: described gelatinization material of phosphoaluminic salt system, and essential mineral component content (W/%) is:
Ternary phosphorus calcium aluminate sosoloid (LH
SsPhase) 40-70
Calcium aluminate sosoloid phase 10-40
Calcium phosphate sosoloid phase 25-60
Vitreum 0-15
6. gelatinization material of phosphoaluminic salt system according to claim 1 and 2 is characterized in that: its raw material of described gelatinization material of phosphoaluminic salt system is mainly derived from mineral stone lime stone, phosphatic rock and bauxitic clay.
7. gelatinization material of phosphoaluminic salt system according to claim 3 is characterized in that: its raw material of described gelatinization material of phosphoaluminic salt system is mainly derived from mineral stone lime stone, phosphatic rock and bauxitic clay.
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| CN104140216A (en) * | 2014-06-24 | 2014-11-12 | 济南大学 | High-iron phosphoaluminate cement clinker |
| CN104803567A (en) * | 2015-02-14 | 2015-07-29 | 广州市正源环境工程有限公司 | Sludge modifier, and method used for preparing subgrade soil from sludge via modification |
| CN105502981A (en) * | 2015-12-15 | 2016-04-20 | 济南大学 | Modified calcium aluminophosphate mineral |
| CN105502982A (en) * | 2015-12-22 | 2016-04-20 | 济南大学 | Barium-containing phosphoaluminate cement |
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| CN115784653A (en) * | 2022-12-20 | 2023-03-14 | 江苏容汇通用锂业股份有限公司 | Preparation method of phosphoaluminate cement clinker and phosphoaluminate cement clinker |
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