CN1594081A - Hydrated magnesium silicate and synthesis method thereof - Google Patents
Hydrated magnesium silicate and synthesis method thereof Download PDFInfo
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- CN1594081A CN1594081A CN 200410048770 CN200410048770A CN1594081A CN 1594081 A CN1594081 A CN 1594081A CN 200410048770 CN200410048770 CN 200410048770 CN 200410048770 A CN200410048770 A CN 200410048770A CN 1594081 A CN1594081 A CN 1594081A
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- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 title claims abstract description 83
- 239000000391 magnesium silicate Substances 0.000 title claims abstract description 80
- 229910052919 magnesium silicate Inorganic materials 0.000 title claims abstract description 79
- 235000019792 magnesium silicate Nutrition 0.000 title claims abstract description 79
- 238000001308 synthesis method Methods 0.000 title description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 108
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 63
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229910001868 water Inorganic materials 0.000 claims abstract description 37
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 229910052814 silicon oxide Inorganic materials 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 7
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 25
- 239000000377 silicon dioxide Substances 0.000 claims description 25
- 229910052681 coesite Inorganic materials 0.000 claims description 24
- 229910052906 cristobalite Inorganic materials 0.000 claims description 24
- 229910052682 stishovite Inorganic materials 0.000 claims description 24
- 229910052905 tridymite Inorganic materials 0.000 claims description 24
- 229910021487 silica fume Inorganic materials 0.000 claims description 15
- MOMKYJPSVWEWPM-UHFFFAOYSA-N 4-(chloromethyl)-2-(4-methylphenyl)-1,3-thiazole Chemical group C1=CC(C)=CC=C1C1=NC(CCl)=CS1 MOMKYJPSVWEWPM-UHFFFAOYSA-N 0.000 claims description 11
- 239000010881 fly ash Substances 0.000 claims description 11
- 235000019983 sodium metaphosphate Nutrition 0.000 claims description 11
- OQZCJRJRGMMSGK-UHFFFAOYSA-M potassium metaphosphate Chemical compound [K+].[O-]P(=O)=O OQZCJRJRGMMSGK-UHFFFAOYSA-M 0.000 claims description 4
- 229940099402 potassium metaphosphate Drugs 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 claims 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 abstract description 10
- 238000002441 X-ray diffraction Methods 0.000 description 25
- 238000006243 chemical reaction Methods 0.000 description 16
- 238000004455 differential thermal analysis Methods 0.000 description 15
- 239000011777 magnesium Substances 0.000 description 14
- 239000000047 product Substances 0.000 description 11
- 239000002994 raw material Substances 0.000 description 11
- 239000007795 chemical reaction product Substances 0.000 description 10
- 238000006703 hydration reaction Methods 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- 230000015572 biosynthetic process Effects 0.000 description 9
- 239000002893 slag Substances 0.000 description 7
- 238000002411 thermogravimetry Methods 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000002425 crystallisation Methods 0.000 description 6
- 230000008025 crystallization Effects 0.000 description 6
- 239000000499 gel Substances 0.000 description 6
- 230000036571 hydration Effects 0.000 description 6
- DGVMNQYBHPSIJS-UHFFFAOYSA-N dimagnesium;2,2,6,6-tetraoxido-1,3,5,7-tetraoxa-2,4,6-trisilaspiro[3.3]heptane;hydrate Chemical compound O.[Mg+2].[Mg+2].O1[Si]([O-])([O-])O[Si]21O[Si]([O-])([O-])O2 DGVMNQYBHPSIJS-UHFFFAOYSA-N 0.000 description 5
- 239000000347 magnesium hydroxide Substances 0.000 description 5
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000004570 mortar (masonry) Substances 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- 229910052839 forsterite Inorganic materials 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 239000011575 calcium Substances 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 3
- 238000002076 thermal analysis method Methods 0.000 description 3
- 238000001757 thermogravimetry curve Methods 0.000 description 3
- 238000009941 weaving Methods 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- 229910017625 MgSiO Inorganic materials 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052909 inorganic silicate Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000008247 solid mixture Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910017970 MgO-SiO2 Inorganic materials 0.000 description 1
- 241001460678 Napo <wasp> Species 0.000 description 1
- 239000004113 Sepiolite Substances 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- WYTGDNHDOZPMIW-RCBQFDQVSA-N alstonine Natural products C1=CC2=C3C=CC=CC3=NC2=C2N1C[C@H]1[C@H](C)OC=C(C(=O)OC)[C@H]1C2 WYTGDNHDOZPMIW-RCBQFDQVSA-N 0.000 description 1
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 229910021488 crystalline silicon dioxide Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000007416 differential thermogravimetric analysis Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000010459 dolomite Substances 0.000 description 1
- 229910000514 dolomite Inorganic materials 0.000 description 1
- 229910052634 enstatite Inorganic materials 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 238000010813 internal standard method Methods 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 235000012243 magnesium silicates Nutrition 0.000 description 1
- BBCCCLINBSELLX-UHFFFAOYSA-N magnesium;dihydroxy(oxo)silane Chemical compound [Mg+2].O[Si](O)=O BBCCCLINBSELLX-UHFFFAOYSA-N 0.000 description 1
- 239000002367 phosphate rock Substances 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- -1 rectenna Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 229910052624 sepiolite Inorganic materials 0.000 description 1
- 235000019355 sepiolite Nutrition 0.000 description 1
- 239000003469 silicate cement Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 235000019982 sodium hexametaphosphate Nutrition 0.000 description 1
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- FKHIFSZMMVMEQY-UHFFFAOYSA-N talc Chemical compound [Mg+2].[O-][Si]([O-])=O FKHIFSZMMVMEQY-UHFFFAOYSA-N 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- Catalysts (AREA)
Abstract
The invention provides a hydrated magnesium silicate and method for synthesizing the same, wherein the hydrated magnesium silicate has a structural formula of mMgO*SiO#-[2]*nH#-[2]O, wherein m=0.5-2.0, n=1-7, the hydrated magnesium silicate is prepared from magnesium oxide and silicon oxide at the presence of catalyst 20-75 deg. C and under 1 barometric pressure through mixing and reacting with water.
Description
Technical Field
The invention relates to hydrated magnesium silicate and a synthesis method thereof, in particular to the hydrated magnesium silicate synthesized at normal temperature and normal pressure and the synthesis method thereof.
Background
There are two types of magnesium silicate minerals present in nature: forsterite (Mg)2Si04) And magnesium metasilicate (MgSiO)3Also called enstatite, proenstatite, clinopodikite), eight kinds of hydrous magnesium silicates, such as serpentine, rectenna, sepiolite, etc.
At present, the conditions for artificially synthesizing magnesium silicate are high temperature and high pressure. E.g. MgO: SiO under hydrothermal conditions of 500 deg.C2The mixture of 2: 1 can be used for synthesizing forsterite (Mg)2SiO4) (ii) a In the ratio of MgO to SiO2Under the conditions of 1: 1 ratio and 1170 deg.C constant temperature (without mineralizer) for more than 50 hr, the clinoptiloenstatite (MgSiO) is formed3)。
Studies of aqueous solutions of magnesium oxide and silica at 75-350 ℃ have shown that: MgO/SiO at 75-100 deg.C2Magnesium oxide was completely bound at 0.75 h; and complete binding in less than 2 hours at 125-150 ℃. In this temperature range, MgO/SiO2The larger the ratio of (A) is, the longer the time for the magnesium oxide to be completely bound is. At the temperature of 125-150 ℃, MgO/SiO2The time for the magnesium oxide to be completely bound in the sample of 1.5 is 10 to 14 hours, while the MgO/SiO ratio is set to2When the time is 0.75, only 2 hours are needed. The magnesium silicate synthesized by the method has no gelling property and application prospect.
In summary, pure MgO and SiO2It is possible to form hydrous magnesium silicate from the raw material under saturated steam or superheated steam treatment conditions. So far, no research on the synthesis of hydrous magnesium silicate at room temperature has been reported.
Disclosure of Invention
The invention aims to provide hydrated magnesium silicate and a synthesis method thereof.
The hydrated magnesium silicate provided by the invention has a structural formula of mMgO-SiO2·nH2O, wherein m is 0.5-2.0 and n is 1-7.
The hydrated magnesium silicate is prepared by reacting magnesium oxide and silicon oxide with water at 20-75 ℃ and 1 atmosphere under the action of a catalyst.
Wherein the silicon oxide is fly ash, silica fume or a combination thereof; the catalyst is sodium metaphosphate or potassium metaphosphate, and the dosage of the catalyst is 0.5 to 5 percent of the weight of the magnesium oxide and the silicon oxide.
In order to harden the hydrous magnesium silicate, the obtained hydrous magnesium silicate may be cured in an environment having a relative humidity of more than 90% or in water.
The hydrated magnesium silicate synthesized at normal temperature and normal pressure and the synthesis method thereof have mild reaction conditions, can complete the reaction at normal temperature and normal pressure to obtain the hydrated magnesium silicate, and have simple raw materials and wide sources. The mortar prepared on the basis of the hydrated magnesium silicate has high compressive strength and flexural strength and excellent performance, can partially replace the prior silicate series cement, and has wide application prospect.
Drawings
FIG. 1 is an X-ray diffraction pattern of MgO
FIG. 2 is an X-ray diffraction pattern of silica fume
FIG. 3 is an X-ray diffraction pattern of hydrous magnesium silicate
FIG. 4 is a thermogram spectrum of hydrous magnesium silicate (including thermal difference analysis DTA and thermogravimetric analysis TG)
FIG. 5 is an X-ray diffraction pattern of a product of hydrous magnesium silicate burned at 1000 deg.C
FIG. 6 shows 60% MgO + 40% SiO2X-ray diffraction patterns of 3-day, 7-day and 28-day hydration products
FIG. 7 is an X-ray diffraction pattern of a product of hydrous magnesium silicate burned at different temperatures
FIG. 8 shows 70% MgO + 30% SiO2Differential thermal analysis curves of reaction products at 50 ℃ and 75 ℃ with water
FIG. 9 shows 70% MgO + 30% SiO2X-ray diffraction pattern of reaction product of water at 50 ℃ and 75 DEG C
FIG. 10 shows 60% MgO + 40% SiO2Differential thermal analysis curves of reaction products at 50 ℃ and 75 ℃ with water
FIG. 11 shows 60% MgO + 40% SiO2X-ray diffraction pattern of reaction product of water at 50 ℃ and 75 DEG C
FIG. 12 shows 60% MgO + 40% SiO2DTA curve of 10 min to 6 h with water under the action of catalyst
FIG. 13 shows 60% MgO + 40% SiO2X-ray diffraction pattern of water addition for 10 min to 6 hours under the action of catalyst
FIG. 14 is an X-ray diffraction pattern of a raw material with a silica fume to magnesia ratio of 1: 1 and a half year hydrated sample thereof
FIG. 15 is a DTA curve of a sample half a year after hydration with a silica fume to magnesia ratio of 1: 1
Detailed Description
Under the action of catalyst, magnesium oxide and amorphous or weak crystalline silicon oxide are synthesized into hydrated magnesium silicatecontaining crystal water at normal temperature and normal pressure (5-75 deg.C and 1 atm).
The reaction formula is as follows:
the used MgO is a raw material containing magnesium oxide, which is prepared by calcining the phosphorite or dolomite; SiO 22The raw material is SiO2Silica fume or fly ash as main component; the catalyst is sodium metaphosphate. The generated hydrated magnesium silicate is a solid in an amorphous state and a weak crystalline state, the chemical composition of the hydrated magnesium silicate is not completely determined, and the hydrated magnesium silicate fluctuates along with the change of synthesis conditions, wherein m is 0.5-2.0, and n is 1-7.
The chemical reaction starts from the addition of water and can be completely carried out for a long time when MgO and SiO react2The chemical reaction is terminated when one of the reactants disappears. The higher the temperature, the faster the reaction rate.
Example 1 Synthesis of hydrous magnesium silicate
MgO is MgCO in the test3The fired product, its X-ray diffraction pattern is shown in FIG. 1. The silica fume is amorphous SiO2Its X-ray diffraction pattern is shown in FIG. 2. 0.5Kg each of MgO and silica fume was mixed and 30g (NaPO) was added3)6Then, the mixture was uniformly mixed with 0.5kg of water, and the mixture was cured for 1 day in an ambient temperature and pressure (20 ℃ C., 1 atm) environment with a relative humidity of more than 90%, and then cured for 28 days in deionized water at 20 ℃. Then, the mixture was ground in 2.5kg of water and filtered. The above operations of adding water, grinding and filtering are repeated once a day until MgO is nearly completely hydrated in 14 days to obtain the hydrated magnesium silicate.
The hydrous magnesium silicate thus obtained was analyzed by X-ray diffraction, and the results are shown in FIG. 3. It can be seen that the steamed bread-shaped dispersion peak of 2 theta at about 20-25 degrees is close to the characteristic peak of the silica fume, and the steamed bread peaks at other positions are the characteristic peaks of the hydrous magnesium silicate. It is thus demonstrated that magnesium silicate hydrate is amorphous, i.e., gel phase, and contains a small amount of weakly crystalline form due to the presence of several very weak diffraction peaks.
The hydrous magnesium silicate thus obtained was subjected to thermal analysis, and its thermogram is shown in FIG. 4, which contains Differential Thermal Analysis (DTA) and thermogravimetric analysis (TG). A large weight loss exists in the range of 50-350 ℃ on a thermogravimetric analysis curve, and a large endothermic valley (endothermic valley temperature of about 175 ℃) appears in the same temperature range on a differential thermal analysis curve, which means that the hydrated magnesium silicate loses bound water. A small weight loss and heat absorption valley (about 422 ℃ in the heat absorption valley temperature) in the range of 400-550 ℃, which is Mg (OH)2Losing the bound water. A sharp exothermic peak (exothermic peak temperature 846 ℃) exists on a differential thermal analysis curve in the range of 800-900 ℃, but no weight change exists on a thermogravimetric curve, which is the crystallization of non-static and weak crystalline substances of the dehydrated magnesium silicate hydrate into crystals, namely the crystallization peak of the magnesium silicate hydrate.
The resulting magnesium silicate hydrate was burned at 1000 ℃and the resulting product was analyzed by X-ray diffraction, as shown in FIG. 5. As can be seen from FIG. 5, the burned product contained only MgO and magnesium silicate (2 MgO. multidot.SiO)2) It was confirmed that the endothermic peak at 846 ℃ on the differential thermal curve is a crystallization peak of hydrous magnesium silicate.
Example 2 test of Normal temperature and pressure formation Process of hydrated magnesium silicate
0.6kg of MgO and 0.4kg of fly ash are taken, 20g of sodium hexametaphosphate is added as a catalyst to form a solid mixture, 0.4kg of water is added to be mixed with the solid mixture, the mixture is stirred uniformly and then is placed in air with the temperature of 20 ℃ and the relative humidity of more than 90 percent for curing for 1 day, and then the mixture is placed in water with the temperature of 20 ℃ for curing.
FIG. 6 is an X-ray diffraction pattern of samples cured for 3 days, 7 days, and 28 days from the addition of water. From the figure, it can be seen that the peak height of MgO decreased with time, while Mg (OH)2There is no significant increase in the peak indicating that a new gel phase, namely hydrated magnesium silicate, is present during hydration. As can be seen from fig. 6, the characteristic peak of MgO gradually decreases with time,and Mg (OH)2The characteristic peaks of (A) are not obviously increased, and the areas of the steamed bun-shaped peaks caused by the gel state and the weak crystalline state are greatly increased, which shows that the amorphous state and the weak junction are in the stageCrystalline hydrous magnesium silicate gels form in large quantities over time. But also considerable amounts of MgO and Mg (OH)2The chemical reaction is not yet completed.
The samples cured for 28 days were heated to different temperatures and subjected to X-ray diffraction analysis, respectively, and an X-ray diffraction analysis pattern is shown in fig. 7. As can be seen from the figure, before 300 ℃, the hydrated magnesium silicate gel is dehydrated by heating, but the structure of the hydrated magnesium silicate gel still belongs to an amorphous phase and a weak crystalline phase, and the crystalline is not increased; mg (OH) is generated between 300 and 500 DEG C2Decomposing and dehydrating to generate MgO crystals so as to increase the diffraction peak of MgO; the crystallization of the hydrated magnesium silicate begins at about 800 ℃ corresponding to the thermal analysis curve of FIG. 4 to form forsterite (2 MgO. SiO)2) But in smaller amounts, lower crystallinity; above 800 deg.C, the forsterite amount increases, the crystal grows gradually, and the X-ray diffraction peak is sharpened. From the above analysis it can be determined that: under the condition of normal temperature and pressure and with catalyst, MgO and non-crystalline and weak crystalline SiO2The product of hydration reaction by adding water is mainly hydrated magnesium silicate mMgO SiO2·nH2O and magnesium hydroxide Mg (OH)2. When heated to above 800 ℃, the amorphous and weak crystalline hydrated magnesium silicate will crystallize to form 2 MgO-SiO2And (4) crystals.
Example 3 analysis of composition of hydrous magnesium silicate
Table 1 shows the composition of the reaction materials in the present example, which were mixed uniformly at room temperature, cured for 1 day at room temperature and pressure (20 ℃ C., 1 atm) with a relative humidity of more than 90%, and then cured in water for various periods of time, and samples were taken for analysis of the phase composition. The analysis method comprises the following steps: quantitatively determining the quantity of MgO crystals in a hydration reaction product by adopting an internal standard method of X-ray diffraction; quantitative determination of Mg (OH) by thermogravimetric analysis2The amount of water and the amount of water bound in the hydrous magnesium silicate; dissolving hydrous magnesium silicate, magnesium hydroxide and magnesium oxide with 15% acetic acid aqueous solution, and measuring from the filtered residueDetermination of unreacted SiO2The number of the cells. From these measurements, the amount and chemical composition of the hydrous magnesium silicate formed were calculated. The measurement and calculation results are shown in table 2. In the composition expression of hydrous magnesium silicate of Table 2, M represents MgO and S represents SiO2H represents H2O, subscripts represent the molar amount of each oxide. For example: m1.61SH1.71The composition of the hydrous magnesium silicate is represented by 1.61 mol of MgO and 1 mol of SiO2And 1.71 mol of H2O。
As can be seen from Table 2, the formation of the hydrous magnesium silicate is continuously carried out, and the formation amount of the hydrous magnesium silicate increases with the time; the composition of the hydrated magnesium silicate is not completely fixed and varies with the composition of the original material, the hydration time and the experimental conditions, wherein MgO/SiO2The ratio fluctuates between 0.5 and 2, H2O/SiO2Fluctuating between 1 and 7; mg (OH)2The amount of the MgO is related to the amount of MgO in the original mixture ratio; when Mg (OH) is present in the system2And SiO2When one disappears, the reaction product is not increased, and MgO or SiO in the original composition2Too little will cause the reaction to end at an earlier time, e.g., when MgO is 10% and SiO is present in the original mixture290% by weight, MgO and Mg (OH) within 28 days2All disappeared and the reaction was complete.
TABLE 1 composition of raw materials for the synthesis of hydrous magnesium silicate (unit: kg)
| Numbering | MgO | SiO2 | (NaPO3)6 | Water (W) |
| 1 | 90 | 10 | 2 | 40 |
| 2 | 80 | 20 | 2 | 40 |
| 3 | 70 | 30 | 2 | 40 |
| 4 | 60 | 40 | 2 | 40 |
| 5 | 50 | 50 | 2 | 40 |
| 6 | 40 | 60 | 2 | 40 |
| 7 | 30 | 70 | 2 | 40 |
| 8 | 20 | 80 | 2 | 40 |
| 9 | 10 | 90 | 2 | 40 |
TABLE 2 analysis results of the amount of hydration product and the composition of the hydrated magnesium silicate
| Weaving machine Number (C) | Amount of formation of hydrous magnesium silicate (wt%) | Hydrated magnesium silicate composition (molar ratio) | Mg(OH)2Amount of production (wt%) | |||
| 3 days | 28 days | 3 days | 28 days | 3 days | 28 days | |
| 1 | 25.88 | 34.03 | M1.61SH1.71 | M1.83SH3.65 | 24.69 | 57.96 |
| 2 | 27.77 | 37.98 | M1.12SH1.28 | M1.60SH2.73 | 22.09 | 42.10 |
| 3 | 30.37 | 44.50 | M1.07SH1.44 | M1.82SH3.59 | 16.76 | 36.27 |
| 4 | 31.84 | 43.03 | M1.51SH1.54 | M1.41SH2.36 | 14.09 | 35.00 |
| 5 | 34.29 | 43.29 | M1.10SH1.42 | M0.94SH3.06 | 11.43 | 26.28 |
| 6 | 26.30 | 46.89 | M0.94SH1.94 | M1.61SH3.03 | 10.90 | 20.60 |
| 7 | 22.72 | 37.56 | M1.07SH1.16 | M0.92SH2.01 | 6.62 | 14.90 |
| 8 | 15.15 | 31.48 | M1.15SH2.88 | M1.20SH2.43 | 4.67 | 5.39 |
| 9 | 11.84 | 21.02 | M1.57SH5.74 | M0.86SH2.12 | 2.58 | 0.00 |
Example 4 speed of Synthesis of magnesium silicate hydrate
The reactants were prepared according to the raw materials numbered 1, 2, 3 and 4 in Table 1, and cured at 25 deg.C, 50 deg.C and 75 deg.C, respectively. Tables 3 to 5 show data of X-ray diffraction analysis (XRD), thermogravimetric analysis (TG) and Differential Thermal Analysis (DTA) of samples taken at various times of curing at different temperatures after adding water, and Table 6 shows the composition of hydrous magnesium silicate measured at 60 days. Fig. 8 and 9 are a differential thermal analysis curve and an X-ray diffraction pattern of the hydration reaction product of sample No. 3, respectively, and fig. 10 and 11 are a differential thermal analysis curve and an X-ray diffraction pattern of the hydration reaction product of sample No. 4, respectively.
From these data, it can be seen that the reaction rate increases with increasing temperature. Wherein MgO accounts for 60% and SiO2Sample No. 4, which accounts for 40%, shows Mg (OH) during hydration at a curing temperature of 75 DEG C)2And 60 days later MgO and Mg (OH)2Completely disappears, and the hydrated magnesium silicate is completely generated. Even if the reaction is carried out at 75 ℃, the product is still amorphous and weakly crystalline hydrous magnesium silicate, and the crystallization degree is still very low and almost gelatinous.
TABLE 3 XRD Peak height (cps)
| Weaving machine Number (C) | MgO(2.1_) | Mg(OH)2(4.77_) | ||||||||||||||||
|
25 | 50℃ | 75℃ |
25 | 50℃ | 75℃ | |||||||||||||
| 3d | 7d | 60d | 3d | 7d | 60d | 3d | 7d | 60d | 3d | 7d | 60d | 3d | 7d | 60d | 3d | 7d | 60d | |
| 1 | 3352 | 1730 | 1428 | 2559 | 1693 | 831 | 1429 | 1257 | 910 | 1528 | 1403 | 2652 | 1161 | 1161 | 2459 | 1222 | 1554 | 2122 |
| 2 | 3304 | 1426 | 1532 | 2379 | 2063 | 962 | 2550 | 1370 | 951 | 1344 | 1015 | 1750 | 757 | 747 | 1338 | 995 | 1072 | 1207 |
| 3 | 3641 | 2332 | 1317 | 2260 | 2139 | 713 | 1867 | 862 | 957 | 993 | 803 | 933 | 541 | 654 | 864 | 727 | 395 | 1235 |
| 4 | 3754 | 2583 | 1103 | 1394 | 1726 | 914 | 1741 | 772 | Is free of | 642 | 603 | 478 | 300 | 384 | 432 | 315 | 236 | Is free of |
TABLE 4 thermogravimetric analysis results
| Weaving machine Number (C) | Water loss (%) | Mg(OH)2Loss (%) | ||||||||||
| 50℃ |
75 | 50℃ | 75℃ | |||||||||
| 3d | 7d | 60d | 3d | 7d | 60d | 3d | 7d | 60d | 3d | 7d | 60d | |
| 1 | 4.99 | 6.37 | 5.49 | 5.66 | 6.05 | 5.94 | 18.64 | 21.27 | 21.16 | 20.06 | 21.35 | 20.84 |
| 2 | 8.09 | 7.99 | 7.68 | 7.16 | 6.88 | 7.58 | 14.99 | 15.88 | 16.22 | 15.55 | 17.92 | 17.92 |
| 3 | 7.91 | 10.16 | 9.28 | 8.79 | 7.56 | 8.04 | 12.10 | 14.15 | 12.79 | 12.41 | 13.80 | 16.34 |
| 4 | 9.41 | 11.14 | 12.06 | 9.11 | 7.55 | 10.5 | 9.88 | 9.18 | 9.16 | 10.34 | 11.57 | Is free of |
TABLE 5 peak height of crystallization of magnesium silicate at 840 ℃ in differential thermal analysis curve (. mu.V/mg)
| Numbering | 50℃ | 75℃ | ||||
| 3d | 7d | 60d | 3d | 7d | 60d | |
| 1 | 0.095 | 0.075 | 0.110 | 0.096 | 0.090 | 0.092 |
| 2 | 0.255 | 0.240 | 0.248 | 0.323 | 0.205 | 0.190 |
| 3 | 0.214 | 0.239 | 0.267 | 0.221 | 0.202 | 0.220 |
| 4 | 0.182 | 0.267 | 0.256 | 0.265 | 0.286 | 0.670 |
TABLE 6 chemical composition Change of hydrated magnesium silicate formed after 60 days of reaction
| Numbering | 25℃ | 50℃ | 75℃ |
| 1 | M1.39SH2.72 | M1.47SH4.54 | M2.05SH5.1 |
| 2 | M1.39SH2.65 | M1.38SH3.1 | M1.6SH3.2 |
| 3 | M1.31SH2.23 | M1.56SH2.63 | M1.41SH2.2 |
| 4 | M1.19SH1.89 | M1.11SH2.24 | M2.1SH1.8 |
The earliest products of sample No. 4 of table 1 after adding water were measured by thermal analysis, fig. 12 is a differential thermal analysis curve of the samples at 10 minutes, 30 minutes and 6 hours, and fig. 13 is an X-ray diffraction pattern of the samples at 10 minutes, 30 minutes and 6 hours. As can be seen, the reaction of the mixture with water started to form Mg (OH) on MgO2And simultaneously forming hydrated magnesium silicate, and gradually increasing reaction products along with the time.
0.5kg of silica fume and 0.5kg of MgO respectively, 20g of sodium metaphosphate and 0.5kg of water are added to form hydrated magnesium silicate, the X-ray diffraction spectrum of the raw materials and the sample after the raw materials are hydrated for half a year is shown in figure 14, and the differential thermal analysis curve ofthe product after the reaction for half a year is shown in figure 15. It can be seen that the reaction is already close to completion and no new reaction product is formed.
Example 5 use of hydrated magnesium silicate
The raw materials are magnesium oxide, silica fume, fly ash, high calcium fly ash, slag powder, phosphorous slag powder, zeolite powder, steel slag powder and metakaolin, hydrated magnesium silicate containing different admixtures is prepared according to the proportion shown in the table 7, wherein the water dosage is 0.45Kg, and then the hydrated magnesium silicate is mixed with 2.5Kg of sand to prepare mortar, the performance of the mortar is measured according to the conventional method, and the performance is shown in the table 7.
TABLE 7 Performance testing of hydrated magnesium silicate cements
| Sample numbering | 1 | 2 | 3 | 4 | 5 | |
| Wood material Material Group of Become into kg | Magnesium oxide | 60 | 40 | 60 | 42 | 30 |
| Silicon oxide | Silica fume 18 | Fly ash 25
| The amount of the silica fume 10 is such that, fly ash 10 | Silica fume 15 | Fly ash 30 | |
| Active mineral admixture |
|
| Metakaolin 19 | | | |
| Calcareous raw material | High calcium flyash 2 | Steel slag powder 10 | 0 | | Lime 2 | |
| Catalyst and process for preparing same | Sodium metaphosphate 1 | Sodium metaphosphate 3 | Potassium metaphosphate 2 | Sodium metaphosphate 4 | Sodium metaphosphate 1 | |
| Property of (2) Can be used for Measuring Test for | 28d flexural strength MPa | 8.58 | 7.03 | 8.21 | 7.65 | 3.47 |
| 28d compressive strength MPa | 72.2 | 65.3 | 71.3 | 63.6 | 35.1 | |
| Flow-down time (seconds) | 19 | 22 | 34 | 12 | 16 | |
| Water content for standard consistency% | 0.30 | 0.33 | 0.31 | 0.32 | 0.29 | |
| Initial setting time h: min | 2:30 | 2:15 | 7:45 | 2:45 | 3:30 | |
| The final setting time h: min | 3:25 | 3:20 | 9:00 | 4:15 | 4:40 | |
As can be seen from the above table, the mortar prepared by the hydrated magnesium silicate material has the compressive strength of 30-80 MPa in 28 days, the flexural strength of 3-10 MPa in 28 days and the setting time of 1-15 hours, and has good performance compared with the common silicate cement mortar.
Claims (9)
1. A hydrated magnesium silicate with the structural formula of mMgO-SiO2·nH2O, wherein m is 0.5-2.0 and n is 1-7.
2. The hydrous magnesium silicate of claim 1 prepared by reacting magnesium oxide and silicon oxide with water at 20-75 ℃ and 1 atmosphere in the presence of a catalyst.
3. The hydrous magnesium silicate of claim 2, characterized in that: the silicon oxide is fly ash, silica fume or the combination thereof.
4. The hydrous magnesium silicate of claim 2 or 3, characterized in that: the catalyst is sodium metaphosphate or potassium metaphosphate.
5. The hydrous magnesium silicate of claim 4, characterized in that: the weight of the sodium metaphosphate or the potassium metaphosphate is 0.5 to 5 percent of the weight of the magnesium oxide and the silicon oxide.
6. A process for synthesizing hydrated magnesium silicate features that magnesium oxide and silicon oxide are used as catalystUnder the action of the agent, the mixture reacts with water at the temperature of 20-75 ℃ and under 1 atmosphere to obtain the compound with the structural formula of mMgO-SiO2·nH2Hydrated magnesium silicate of O, wherein m is 0.5-2.0 and n is 1-7.
7. The method of synthesizing hydrous magnesium silicate of claim 6 wherein: the resulting hydrous magnesium silicate requires curing in an environment or water having a relative humidity of greater than 90%.
8. The method of synthesizing hydrous magnesium silicate as claimed in claim 6 or 7, characterized by comprising: the catalyst is sodium metaphosphate.
9. The method of synthesizing a hydrous magnesium silicate as claimed in claim 8, wherein: the sodium metaphosphate accounts for 0.5 to 5 percent of the weight of the magnesium oxide and the silicon oxide.
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