CN110078103A - A kind of calcium aluminium houghite and preparation method thereof - Google Patents
A kind of calcium aluminium houghite and preparation method thereof Download PDFInfo
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- CN110078103A CN110078103A CN201910445117.3A CN201910445117A CN110078103A CN 110078103 A CN110078103 A CN 110078103A CN 201910445117 A CN201910445117 A CN 201910445117A CN 110078103 A CN110078103 A CN 110078103A
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- calcium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/782—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen containing carbonate ions, e.g. dawsonite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/20—Two-dimensional structures
- C01P2002/22—Two-dimensional structures layered hydroxide-type, e.g. of the hydrotalcite-type
Abstract
The invention belongs to hydrotalcite-based compound preparation technical fields, and in particular to a kind of calcium aluminium houghite and preparation method thereof.The present invention provides a kind of preparation methods of calcium aluminium houghite, comprising the following steps: (1) mixes calcium source, silicon source, stabilizer and water, obtain mixed liquor and reacted, obtain intermediate slurries；Anion in the mixed liquor includes OH‑With cooperation anion；The cooperation anion includes Cl‑、F‑、SO4 2‑、NO3 ‑、PO4 3‑And HPO4 2‑One of or it is a variety of；(2) the intermediate slurries are mixed into crystallization with alkaline salt solution, obtains calcium aluminium houghite.The present invention follows " fast nucleation mechanism ", generates a kind of intermediate during the preparation process, avoids calcium ion, aluminium ion directly contacts with alkali soluble solution anion and generates CaCO3Equal impurity keep calcium aluminium houghite crystal phase obtained uniform, purity is high.
Description
Technical field
The invention belongs to hydrotalcite-based compound preparation technical fields, and in particular to a kind of calcium aluminium houghite and its preparation
Method.
Background technique
Calcium aluminium houghite is a kind of double-metal hydroxide with layer structure, and typical chemical formula is Ca4Al2
(OH)12(CO3)(H2O)5, with the Nomenclature Composition and Structure of Complexes, the properties such as controllable, alkaline, are widely used in PVC heat stabilizer, building, water
The fields such as pollution processing.
In the prior art, the methods of coprecipitation, hydro-thermal method, microwave process for synthesizing one can be used in the preparation of calcium aluminium houghite
Step is made.But during preparing calcium aluminium houghite using these methods, generalling use the soluble-salts such as calcium nitrate, aluminum nitrate is
Primary raw material, available calcium in this kind of raw material, aluminium element mass fraction be no more than 20%；And in preparation process, a side
Face is not followed " fast nucleation mechanism ", calcium ion radius and magnesium ion radius using conventional method synthesis calcium aluminium houghite
It differs larger, is difficult to replace the magnesium elements in hydrotalcite, CaCO3、Ca3Al2(OH)12It forms speed and is much larger than calcium aluminium houghite
Formation speed, on the other hand, CaCO3、Ca3Al2(OH)12Thermal stability be much larger than calcium aluminium houghite thermal stability, make
Stable CaCO is more readily formed in carbonate or hydroxyl and calcium, aluminium ion3、Ca3Al2(OH)12Impurity.Therefore the calcium aluminium of preparation
Houghite atom utilization is low, and the by-product of generation is more, and by-product separates difficulty with principal product calcium aluminium houghite, therefore obtains
Calcium aluminium houghite product purity is low, seriously affect the performance of calcium aluminium houghite.
Summary of the invention
In view of this, the present invention provides the purpose of the present invention is to provide a kind of calcium aluminium houghite and preparation method thereof
The purity is high of calcium aluminium houghite that is prepared of method, so that the utility value of calcium aluminium houghite is got a promotion, and technique
Simply.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical schemes:
The present invention provides a kind of preparation method of calcium aluminium houghite, comprising the following steps:
(1) calcium source, silicon source, stabilizer and water are mixed, obtains mixed liquor, the mixed liquor is reacted, is obtained
To intermediate slurries；
Anion in the mixed liquor includes OH-With cooperation anion；The cooperation anion includes Cl-、F-、
SO4 2-、NO3-、PO4 3-And HPO4 2-One of or it is a variety of；
(2) the intermediate slurries are mixed with alkaline salt solution, carries out crystallization, obtains calcium aluminium houghite.
Preferably, the cation in step (1) stabilizer includes H+、Na+、K+、NH4 +One of or it is a variety of.
Preferably, calcium source is calcium chloride, calcium sulfate, calcirm-fluoride, calcium nitrate, calcium oxide, hydroxide in the step (1)
One of calcium, calcium phosphate and calcium monohydrogen phosphate are a variety of；Silicon source is aluminium chloride, aluminium polychloride, aluminum sulfate, aluminum nitrate, three oxygen
Change one of two aluminium, aluminium hydroxide and aluminum phosphate or a variety of.
Preferably, the molar ratio of calcium constituent and aluminium element in silicon source is (1~5) in step (1) calcium source: 1；The calcium
In source calcium constituent with and mixed liquor in anion molar ratio be 1:(0.4~10).
Preferably, the temperature reacted in the step (1) is 60~200 DEG C, and the time is 0.1~4h.
Preferably, the solute in step (2) alkaline salt solution includes sodium carbonate, sodium bicarbonate, ammonium carbonate and carbonic acid
One of hydrogen ammonium is a variety of.
Preferably, the molar ratio of aluminium element is in the anion of solute and silicon source in step (2) alkaline salt solution
(0.4~1.0): 1.
Preferably, the temperature of crystallization is 60~200 DEG C in the step (2), and the time is 1~20h.
Preferably, in the step (2) after crystallization further include:
It will be filtered after the cooling of gained system, gained filtrate recycle carries out powder in step (1) after gained filtration cakes torrefaction
Broken processing obtains calcium aluminium houghite.
The present invention also provides the calcium aluminium houghites that preparation method described in above-mentioned technical proposal is prepared.
The present invention provides a kind of preparation methods of calcium aluminium houghite, comprising the following steps: (1) by calcium source, silicon source, steady
Determine agent and water mixing, obtains mixed liquor, the mixed liquor is reacted, obtain intermediate slurries；The mixed liquor
In anion include OH-With cooperation anion；The cooperation anion includes Cl-、F-、SO4 2-、NO3-、PO4 3-And HPO4 2-In
It is one or more；(2) the intermediate slurries are mixed with alkaline salt solution, carries out crystallization, obtains calcium aluminium houghite.
The present invention provides calcium and aluminium element using calcium source, silicon source as raw material, for calcium aluminium houghite, by be added stabilizer come
Change the forming feature of calcium aluminum hydrotalcite, two steps synthesize calcium aluminium houghite: calcium source, silicon source are reacted with stabilizer first, are generated
Stable intermediate；Alkaline salt solution is added on this basis, calcium aluminium houghite is made.The present invention first abides by during the preparation process
" fast nucleation mechanism " is followed, the OH in calcium source, silicon source and mixed liquor is utilized-A kind of centre is generated with cooperation anion
Body, then following " fast nucleation mechanism " again occurs intermediate and alkaline salt solution anion (such as carbonate or bicarbonate radical)
Reaction obtains calcium aluminium houghite；The present invention avoids calcium source, silicon source and alkaline salt solution by generating this mode of intermediate
In anion directly contact and generate CaCO3、Ca3Al2(OH)12Equal impurity keep calcium aluminium houghite crystal phase obtained uniform,
Purity is high.In the present invention, OH-First step reaction process is taken part in cooperation anion, but is dissolved out in second step reaction, instead
It can be used as containing the anion in mixed liquor (especially stabilizer) in filtrate after answering and prepare calcium aluminium houghite intermediate
Raw material, direct circulation utilize, and simple production process in whole preparation process, low energy consumption, without sewage discharge, and clean and environmental protection meets
Green chemical concept.
The experimental results showed that the calcium aluminium houghite crystal phase obtained under the conditions of technical solution of the present invention is uniform, free from admixture is
Calcium aluminium houghite.
Detailed description of the invention
Fig. 1 is the XRD diagram of intermediate solid substance in 1 preparation process of the embodiment of the present invention；
Fig. 2 is the XRD diagram for the calcium aluminium houghite that the embodiment of the present invention 1~3 and comparative example 1 are prepared, and wherein A is real
Example 1 is applied, B is embodiment 2, and C is embodiment 3, and D is comparative example 1.
Specific embodiment
The present invention provides a kind of preparation methods of calcium aluminium houghite, comprising the following steps:
(1) calcium source, silicon source, stabilizer and water are mixed, obtains mixed liquor, the mixed liquor is reacted, is obtained
To intermediate slurries；
Anion in the mixed liquor includes OH-With cooperation anion；The cooperation anion includes Cl-、F-、
SO4 2-、NO3-、PO4 3-And HPO4 2-One of or it is a variety of；
(2) the intermediate slurries are mixed with alkaline salt solution, carries out crystallization, obtains calcium aluminium houghite.
In the present invention, if without specified otherwise, all components be commercial goods well known to those skilled in the art i.e.
It can.
The present invention mixes calcium source, silicon source, stabilizer and water, obtains mixed liquor, the mixed liquor is reacted,
Obtain intermediate slurries.In the present invention, the calcium source is preferably calcium chloride, calcium sulfate, calcirm-fluoride, calcium nitrate, calcium oxide, hydrogen
One of calcium oxide, calcium phosphate and calcium monohydrogen phosphate are a variety of.In the present invention, source of aluminium is preferably aluminium chloride, polymerization chlorine
Change one of aluminium, aluminum sulfate, aluminum nitrate, aluminum oxide, aluminium hydroxide and aluminum phosphate or a variety of.In the present invention, described
The molar ratio of calcium constituent and aluminium element in silicon source is preferably (1~5): 1, more preferably (1~4): 1 in calcium source.In the present invention,
The calcium source is preferably with or without the crystallization water.In the present invention, source of aluminium is preferably with or without the crystallization water.
In the present invention, the anion in the mixed liquor includes OH-With cooperation anion；The cooperation anion packet
Containing Cl-、F-、SO4 2-、NO3-、PO4 3-And HPO4 2-One of or it is a variety of.In the present invention, the cation in the stabilizer is excellent
Choosing includes H+、Na+、K+、NH4 +One of or it is a variety of.In the present invention, in the calcium source in calcium constituent and mixed liquor yin from
The molar ratio of son is preferably 1:(0.4~10), more preferably 1:(0.5~9.5).In the present invention, in the mixed liquor
Source of anions is in the calcium source, silicon source and stabilizer.In the present invention, the OH-It is to prepare in described with cooperation anion
The raw material of mesosome.The present invention is not particularly limited the dosage of the water, with can evenly dispersed calcium source, silicon source and stabilizer be
It is quasi-.The present invention passes through the molar ratio of calcium constituent and aluminium element in silicon source in control calcium source, calcium constituent and and mixed liquor in calcium source
The molar ratio of middle anion, and control OH-With cooperation anion-content, achieve the purpose that form intermediate.
The present invention is not particularly limited the mixing, by the way of mixing well known to those skilled in the art.
In the present invention, the temperature of the reaction is preferably 60~200 DEG C, and more preferably 65~195 DEG C；The time of the reaction is preferred
For 0.1~4h, more preferably 0.3~3.8h.The present invention makes stabilizer react with calcium source, silicon source under the above conditions, raw
At stable intermediate.
In the present invention, when cooperation anion is NO3 -When, the intermediate is a kind of 3CaOAl2O3·0.83Ca
(NO3)2·0.17Ca(OH)2·9.5H2O(Calcium Aluminum Oxide Nitrate Hydroxide Hydrate)
The compound of structure；When cooperating anion is other above-mentioned anion, the intermediate is NO in above-mentioned molecular formula3 -Become phase
Answer the structural compounds of anion.
After obtaining intermediate slurries, the present invention mixes the intermediate slurries with alkaline salt solution, carries out crystallization, obtains
Calcium aluminium houghite.In the present invention, the solute in the alkaline salt solution preferably includes sodium carbonate, sodium bicarbonate, ammonium carbonate
With one of ammonium hydrogen carbonate or a variety of.The present invention does not limit the concentration of the alkaline salt solution, using art technology
Alkaline salt solution concentration known to personnel.In the present invention, in the alkaline salt solution in the anion and silicon source of solute
The molar ratio of aluminium element is preferably (0.4~1.0): 1.
The present invention is not particularly limited the hybrid mode of the intermediate slurries and alkaline salt solution, using this field skill
Hybrid mode known to art personnel.
In the present invention, the temperature of the crystallization is preferably 60~200 DEG C, and more preferably 65~195 DEG C；The time of crystallization
For 1~20h, more preferably 1.5~19.5h.In the present invention, intermediate stable during the crystallization is converted to calcium aluminium
Houghite.
In the present invention, after the crystallization it is also preferable to include will gained system it is cooling after be filtered, gained filtrate recycle
In the preparation process of intermediate slurries, pulverization process is carried out after gained filtration cakes torrefaction, obtains calcium aluminium houghite.In the present invention
In, the final temperature of the cooling is preferably 100 DEG C hereinafter, more preferably 40~90 DEG C.Mode of the present invention to the cooling
It is not particularly limited, using the type of cooling well known to those skilled in the art.In the present invention, the filtering is preferably normal
Press filtration, filters pressing or suction filtration.The present invention is not particularly limited the mode of the drying and crushing, using those skilled in the art
The mode of well known drying and crushing.The present invention does not have particular/special requirement to the powder particle diameter of the crushing, described in meeting
Subject to the requirement of calcium aluminium houghite.
In the present invention, the filtrate is preferably back in the process for preparation of mixed liquor.In the present invention, the filtrate
To include OH-With the solution of cooperation anion, the cooperation anion includes Cl-、F-、SO4 2-、NO3 -、PO4 3-And HPO4 2-In
It is at least one.In the present invention, anion needed for the filtrate contains the reaction for preparing intermediate, during reuse, is not necessarily to
Additional addition cooperation anion again, that is, no longer need to additionally add stabilizer, advantageously reduce production cost.The present invention is preferably filtering
According to OH in the volume of filtrate and filtrate when liquid reuse-With the content adjustment calcium source and silicon source of cooperation anion, guarantee calcium source,
Silicon source, OH-With cooperation anion reaction, to generate intermediate.In the present invention, calcium constituent and aluminium in silicon source in the calcium source
The molar ratio of element is preferably (1~5): 1, more preferably (1~4): 1.In the present invention, calcium constituent and filtrate in the calcium source
The molar ratio of middle anion is preferably 1:(0.4~10), more preferably 1:(0.5~9.5).
The present invention also provides the calcium aluminium houghites that the preparation method as described in above technical scheme is prepared.In this hair
In bright, the interlayer anion of the calcium aluminium houghite is carbonate.
In order to further illustrate the present invention, below with reference to embodiment to calcium aluminium houghite provided by the invention and its preparation
Method is described in detail, but they cannot be interpreted as limiting the scope of the present invention.Obviously, described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
Embodiment 1
236.2g calcium nitrate tetrahydrate and 187.6g ANN aluminium nitrate nonahydrate are dissolved in 1000mL water, it is molten to be made into salt-mixture
Liquid, while 140g sodium hydroxide and 87.6g sodium chloride being dissolved in the water of 500mL, it is made into stabiliser solution, then by salt-mixture
Solution and stabiliser solution mixing, react 2h under the conditions of 130 DEG C, obtain intermediate slurries.
26.5g natrium carbonicum calcinatum is dissolved in 500mL water, sodium carbonate liquor is obtained, then by intermediate slurries and carbonic acid
After sodium solution mixing, the crystallization 14h under the conditions of 160 DEG C is filtered after being subsequently cooled to 80 DEG C, collects gained filtrate recycle in centre
The preparation of somaplasm liquid, gained filter cake crushed after being dried under the conditions of 60 DEG C obtain calcium aluminium houghite.
The intermediate slurries of embodiment 1 are filtered, are dried and milled processed, intermediate solid substance are obtained, to this
Intermediate solid substance carries out XRD test, and test results are shown in figure 1.
Embodiment 2
74g calcium hydroxide and 39g aluminium hydroxide are added in the filtrate recycled to 1800mL embodiment 1, it is steady in the filtrate
The anion concentration for determining agent is 2.72mol/L, reacts 3h under the conditions of 110 DEG C, obtains intermediate slurries.
21g sodium bicarbonate is dissolved in 500mL water, sodium bicarbonate solution is obtained, then by intermediate slurries and bicarbonate
After sodium solution mixing, gained filtrate recycling, reuse are collected in the crystallization 10h under the conditions of 140 DEG C, filters pressing after being subsequently cooled to 80 DEG C
In the preparation of intermediate slurries, gained filter cake crushed after being dried under the conditions of 60 DEG C is crushed, and obtains calcium aluminium houghite.
Embodiment 3
It is added in the filtrate recycled to 1820mL embodiment 2,56g calcium oxide and 25.5g aluminum oxide in the filtrate
The anion concentration of stabilizer is 2.36mol/L, reacts 4h under the conditions of 130 DEG C, obtains intermediate slurries.
26.5g sodium carbonate is dissolved in the water of 500mL, sodium carbonate liquor is obtained, then by intermediate slurries and sodium carbonate
After solution mixing, under the conditions of 150 DEG C crystallization 8h, filters pressing after being subsequently cooled to 80 DEG C is collected gained filtrate recycling, is back to
The preparation of mesosome slurries, gained filter cake crushed after being dried under the conditions of 60 DEG C crush, and obtain calcium aluminium houghite.
Comparative example 1
Using hydrotalcite traditional preparation methods, 236.2g calcium nitrate tetrahydrate and 187.6g ANN aluminium nitrate nonahydrate are dissolved in
In 1000mL water, it is made into mixing salt solution；140g sodium hydroxide and 26.5g natrium carbonicum calcinatum are dissolved in the water of 1000mL, matched
At mixed ammonium/alkali solutions；Then mixing salt solution and mixed ammonium/alkali solutions are mixed, 2h is reacted under the conditions of 130 DEG C, then at 160 DEG C of items
The lower crystallization 14h of part, filters pressing after being subsequently cooled to 80 DEG C, gained filter cake crushed after being dried under the conditions of 60 DEG C crush, and obtain calcium
Aluminium houghite.
XRD detection is carried out to the calcium aluminium houghite of Examples 1 to 3 and comparative example 1, testing result is as shown in Figure 2.
A curve in comparison diagram 1 and Fig. 2 it is found that the main feature diffraction maximum of intermediate is mobile toward low-angle direction simultaneously,
Thus deducibility first step reaction forms the intermediate different from final product calcium aluminium hydrotalcite-like compound.It can be seen by Fig. 2
Out, the product calcium aluminium houghite that the embodiment of the present invention obtains, crystal phase is uniform, free from admixture, purity is high；And what comparative example 1 obtained
In product in addition to generating calcium aluminium houghite, also with CaCO3、Ca3Al2(OH)12Equal impurity generate, and calcium aluminium houghite is pure
It spends low.
Calcium aluminium houghite purity is high provided by the invention, improves hydrotalcite it can be seen from embodiment and comparative example
Utility value；Simple process simultaneously, realizes filtrate recycling and reusing, not only reduces waste and dirt caused by discharging of waste liquid
Dye, and reduce the additive amount of stabilizer and water；Calcium aluminium houghite by-product is few, separation is simple, is not necessarily in the preparation later period
Massive laundering reduces production cost, has extremely strong environmental protection characteristic and high economic value.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of calcium aluminium houghite, comprising the following steps:
(1) calcium source, silicon source, stabilizer and water are mixed, obtains mixed liquor, the mixed liquor is reacted, obtained
Mesosome slurries；
Anion in the mixed liquor includes OH-With cooperation anion；The cooperation anion includes Cl-、F-、SO4 2-、
NO3 -、PO4 3-And HPO4 2-One of or it is a variety of；
(2) the intermediate slurries are mixed with alkaline salt solution, carries out crystallization, obtains calcium aluminium houghite.
2. preparation method according to claim 1, which is characterized in that the cation in step (1) stabilizer includes H+、Na+、K+、NH4 +One of or it is a variety of.
3. preparation method according to claim 1, which is characterized in that calcium source is calcium chloride, sulfuric acid in the step (1)
One of calcium, calcirm-fluoride, calcium nitrate, calcium oxide, calcium hydroxide, calcium phosphate and calcium monohydrogen phosphate are a variety of；Source of aluminium is chlorine
Change one of aluminium, aluminium polychloride, aluminum sulfate, aluminum nitrate, aluminum oxide, aluminium hydroxide and aluminum phosphate or a variety of.
4. preparation method according to any one of claims 1 to 3, which is characterized in that calcium member in step (1) calcium source
The molar ratio of element and aluminium element in silicon source is (1~5): 1；In the calcium source calcium constituent with and mixed liquor in anion mole
Than for 1:(0.4~10).
5. preparation method according to claim 1, which is characterized in that the temperature reacted in the step (1) is 60~200
DEG C, the time is 0.1~4h.
6. preparation method according to claim 1, which is characterized in that the solute packet in step (2) alkaline salt solution
Include one of sodium carbonate, sodium bicarbonate, ammonium carbonate and ammonium hydrogen carbonate or a variety of.
7. preparation method according to claim 1 or 6, which is characterized in that solute in step (2) alkaline salt solution
The molar ratio of aluminium element is (0.4~1.0) in anion and silicon source: 1.
8. preparation method according to claim 1, which is characterized in that the temperature of crystallization is 60~200 in the step (2)
DEG C, the time is 1~20h.
9. preparation method according to claim 1, which is characterized in that in the step (2) after crystallization further include:
It will be filtered after the cooling of gained system, gained filtrate recycle carries out at crushing after gained filtration cakes torrefaction in step (1)
Reason, obtains calcium aluminium houghite.
10. the calcium aluminium houghite that preparation method described in any one is prepared according to claim 1~9.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110898783A (en) * | 2019-11-15 | 2020-03-24 | 江苏隆昌化工有限公司 | Preparation method of inorganic layered supramolecular material |
| CN113045231A (en) * | 2021-03-26 | 2021-06-29 | 沈阳建筑大学 | Calcium-aluminum hydrotalcite structure geopolymer cement based on microwave curing and preparation method thereof |
| CN114516651A (en) * | 2022-03-28 | 2022-05-20 | 北京化工大学 | Calcium-aluminum hydrotalcite with 3D structure and preparation method and application thereof |
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| CN105347310A (en) * | 2015-11-23 | 2016-02-24 | 北京化工大学 | Method for preparing high-purity calcium-based hydrotalcite |
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| CN110898783A (en) * | 2019-11-15 | 2020-03-24 | 江苏隆昌化工有限公司 | Preparation method of inorganic layered supramolecular material |
| CN113045231A (en) * | 2021-03-26 | 2021-06-29 | 沈阳建筑大学 | Calcium-aluminum hydrotalcite structure geopolymer cement based on microwave curing and preparation method thereof |
| CN114516651A (en) * | 2022-03-28 | 2022-05-20 | 北京化工大学 | Calcium-aluminum hydrotalcite with 3D structure and preparation method and application thereof |
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