CN102153295A - Method for preparing Portland cement clinker - Google Patents
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- CN102153295A CN102153295A CN 201010109401 CN201010109401A CN102153295A CN 102153295 A CN102153295 A CN 102153295A CN 201010109401 CN201010109401 CN 201010109401 CN 201010109401 A CN201010109401 A CN 201010109401A CN 102153295 A CN102153295 A CN 102153295A
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Abstract
The invention relates to a method for preparing Portland cement clinker. The method comprises the following steps: proportionally mixing tetraethoxysilane, a calcium nitrate hydrate, an aluminium nitrate hydrate, a ferric nitrate hydrate, ethanol, nitric acid, hexamethylenetetramine, acetylacetone, deionized water and the like uniformly to obtain four kinds of mixed liquid, fully stirring the four kinds of mixed liquid respectively at the temperature of 50-70 DEG C until proper viscosity to obtain monomineral sols of the Portland cement clinker, then mixing the four monomineral sols in a mass ratio of (36-55):(24-40):(11-19):(20-31), ageing the mixture to form gel, carrying out heat treatment on the gel at the temperature of 1150-1200 DEG C for 4-6 hours and cooling the gel to the room temperature, thus obtaining the Portland cement clinker. Compared with the prior art, the method has the following advantages: the preparation process is simple; the reaction process is easy to control; and the product has high uniformity and purity and can be fired at the temperature lower than the temperature in the traditional methods.
Description
Technical field
The present invention relates to a kind of preparation method of inorganic materials, especially relate to a kind of preparation method of Portland clinker.
Background technology
In research during hydrated cementitious, in order to reduce unkownable factors as far as possible, usually with laboratory synthetic cement and grog simple ore thing as research object.Yet when synthesizing cement clinker mineral with the method for conventional high-temperature sintering reaction, desired reaction temperature height not only, and owing to usually adopt mineralizer etc. to reduce firing temperature or the Within Monominerals crystal that makes some crystal formation at room temperature can stable existence, can in cement clinker mineral, introduce other compositions.
In recent years, appearance along with various chemical processes, brought the revolution of cement clinker mineral synthetic method, they all attempt to overcome synthesis temperature height, the reaction shortcoming such as wayward of traditional solid-phase sintering method, make great efforts to have breakthrough at the aspect of performance of synthetic product.The chemical process of using aspect synthetic at the cement system mineral mainly contains: polymerization organic and inorganic synthesis method, hydrothermal synthesis method, combustion synthesis method and sol-gel method etc.Polymerization organic and inorganic synthesis method requires harshness for the polymer support that is adopted, hydrothermal synthesis method only is applicable to the synthetic silicate mineral, the Ca/Si=2 of especially Dicalcium Phosphate (Feed Grade), and control hydro-thermal synthetic product is difficulty relatively, and combustion synthesis method only is applicable to calcium aluminate and iron calcium aluminate.Sol-gel method is a kind of method of colloid chemistry, it uses liquid chemical reagent or colloidal sol to be raw material, metal alkoxide or inorganic salt are directly formed colloidal sol or form colloidal sol with fixed attention through separating through hydrolysis, make the solute polymeric gelization then, again organic composition is removed in gel drying, calcination, reached required inorganic materials at last.Preparation process comprises the preparation of colloidal sol, formation and gel drying and the heat treatment of gel.
Tradition adopts the synthetic cement clinker mineral of the method for high temperature sintering reaction.This method desired reaction temperature is higher than 1450 ℃; Reaction process is wayward, and free calcium oxide content is reduced to below 1%, needs just can finish through repeated multiple times grinding, powder compression and sintering; Because the simple ore thing crystal that usually adopts mineralizer (as cupric oxide, Calcium Fluoride (Fluorspan), calcium sulfate, phosphorus oxide, titanium oxide) to wait to reduce firing temperature or make some crystal formation at room temperature can stable existence, can in cement clinker mineral, introduce and remove the thing phase that designs the product.
Summary of the invention
Purpose of the present invention be exactly provide in order to overcome the defective that above-mentioned prior art exists that a kind of purity height, preparation technology are simple, the reaction process preparation method of the Portland clinker of control easily.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of Portland clinker is characterized in that, this method is by sol-gel method mixing of analytical pure chemical reagent and ageing to be obtained gel, and the gained gel passes through high-temperature heat treatment again and is cooled to room temperature, promptly obtains Portland clinker.
This method specifically may further comprise the steps:
(1) with ethyl orthosilicate ((C
2H
5O)
4Si), calcium nitrate hydrate (Ca (NO
3)
24H
2O), ethanol (C
2H
5OH), nitric acid (HNO
3) be 1: 3.4 by weight: (10-30): (0.1-0.5) mix, obtain mixed liquor A, the control temperature is 50-70 ℃, fully stirs 8-10h, obtains the Within Monominerals Sol A;
(2) with ethyl orthosilicate ((C
2H
5O)
4Si), calcium nitrate hydrate (Ca (NO
3)
24H
2O), ethanol (C
2H
5OH), nitric acid (HNO
3) be 1: 2.27 by weight: (10-30): (0.1-0.6) mix, obtain mixed liquid B, the control temperature is 50-70 ℃, fully stirs 8-10h, obtains the Within Monominerals sol B;
(3) with aluminum nitrate hydrate (Al (NO
3)
39H
2O), calcium nitrate hydrate (Ca (NO
3)
24H
2O), hexamethylenetetramine ((CH
2)
6N
4), acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)), deionized water is 1: 0.94 by weight: (0.2-0.6): (0.08-0.16): (5-10) mix, obtain mixed liquor C, the control temperature is 50-70 ℃, fully stirs 10-12h, obtains Within Monominerals colloidal sol C;
(4) with aluminum nitrate hydrate (Al (NO
3)
39H
2O), calcium nitrate hydrate (Ca (NO
3)
24H
2O), ferric nitrate hydrate (Fe (NO
3)
3) 9H
2O), hexamethylenetetramine ((CH
2)
6N
4), acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)), deionized water is 1: 1.26: 1.08 by weight: (0.2-0.6): (0.08-0.16): (5-10) mix, obtain mixed liquor D, the control temperature is 50-70 ℃, fully stirs 10-12h, obtains Within Monominerals colloidal sol D;
(5) with simple ore thing Sol A, simple ore thing sol B, simple ore thing colloidal sol C and simple ore thing colloidal sol D according to weight ratio (36-55): (24-40): (11-19): (20-31) mix, the control bath temperature is 70-80 ℃, obtained gel in ageing 3-5 days, gel is placed high-temperature cracking furnace, controlled temperature is 1150-1200 ℃ and heat-treats 4-6h, is cooled to room temperature then and promptly gets Portland clinker.
Described tetraethoxy, nitrocalcite hydrate, aluminum nitrate hydrate, iron nitrate hydrate, hexamethylenetetramine, methyl ethyl diketone, ethanol and nitric acid are the analytical pure chemical reagent.
Described thermal treatment temp is 1150-1200 ℃.
Described heat treatment time is 4-6h.
Compared with prior art, the present invention by adjust and control solution in chemical reaction, obtain required composition and structure with suitable form, can prepare Portland clinker being lower than under the temperature of traditional method, product uniformity coefficient height, chemical uniformity is good, because in sol-gel process, colloidal sol is made by solution, so reach chemical ingredients unanimity between micelle in the micelle, and the purity height, wherein free calcium oxide content all is lower than 0.5%, and product granularity is little.Need not pass through sintering reaction in addition, than the easier preparation fine powder of conventional sintering method, gel grinds gained powder average grain diameter 2-4 μ m with agate mortar after Overheating Treatment, and preparation technology is simple, and course of reaction is easy to control, can finish preparation by once sintered.
Embodiment
The present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1
A kind of preparation method of Portland clinker, according to the formulated colloidal sol of table 1, concrete preparation method may further comprise the steps:
According to weight ratio with ethyl orthosilicate ((C
2H
5O)
4Si) 54.74 parts, calcium nitrate hydrate (Ca (NO
3)
24H
2O) 186.32 parts, ethanol (C
2H
5OH) 1239.65 parts, nitric acid (HNO
3) 17.57 parts of mixing, according to weight ratio with ethyl orthosilicate ((C
2H
5O)
4Si) 24.18 parts, calcium nitrate hydrate (Ca (NO
3)
24H
2O) 54.88 parts, ethanol (C
2H
5OH) 433.65 parts, nitric acid (HNO
3) 6.15 parts of mixing, according to weight ratio with aluminum nitrate hydrate (Al (NO
3)
39H
2O) 19.44 parts, calcium nitrate hydrate (Ca (NO
3)
24H
2O) 18.36 parts, hexamethylenetetramine ((CH
2)
6N
4) 8.50 parts, acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)) 2.38 parts, 107.00 parts of mixing of deionized water, according to weight ratio with aluminum nitrate hydrate (Al (NO
3)
39H
2O) 20.06 parts, calcium nitrate hydrate (Ca (NO
3)
24H
2O) 18.94 parts and ferric nitrate hydrate (Fe (NO
3)
3) 9H
2O) 21.61 parts, hexamethylenetetramine ((CH
2)
6N
4) 9.39 parts, acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)) 2.46 parts, 110.00 parts of mixing of deionized water, four kinds of mixed liquors are stirred well to proper viscosity respectively under 60 ℃, obtain Portland clinker Within Monominerals colloidal sol, then four kinds of Within Monominerals colloidal sols are mixed, after ageing, form gel, 1200 ℃ of lower heat treatments 4 hours, be cooled to room temperature and namely get Portland clinker, the mineral composition of grog is tricalcium silicate 60%, dicalcium silicate 20%, calcium aluminate 7%, calcium aluminoferrite 13%.
Embodiment 2
A kind of preparation method of Portland clinker, according to the formulated colloidal sol of table 1, concrete preparation method may further comprise the steps:
According to weight ratio with ethyl orthosilicate ((C
2H
5O)
4Si) 50.18 parts, calcium nitrate hydrate (Ca (NO
3)
24H
2O) 170.79 parts, ethanol (C
2H
5OH) 1136.35 parts, nitric acid (HNO
3) 16.11 parts of mixing, according to weight ratio with ethyl orthosilicate ((C
2H
5O)
4Si) 30.23 parts, calcium nitrate hydrate (Ca (NO
3)
24H
2O) 68.60 parts, ethanol (C
2H
5OH) 542.07 parts, nitric acid (HNO
3) 7.68 parts of mixing, according to weight ratio with aluminum nitrate hydrate (Al (NO
3)
39H
2O) 13.89 parts, calcium nitrate hydrate (Ca (NO
3)
24H
2O) 13.11 parts, hexamethylenetetramine ((CH
2)
6N
4) 6.07 parts, acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)) 1.70 parts, 80.00 parts of mixing of deionized water, according to weight ratio with aluminum nitrate hydrate (Al (NO
3)
39H
2O) 23.15 parts, calcium nitrate hydrate (Ca (NO
3)
24H
2O) 21.85 parts and ferric nitrate hydrate (Fe (NO
3)
3) 9H
2O) 24.94 parts, hexamethylenetetramine ((CH
2)
6N
4) 10.83 parts, acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)) 2.84 parts, 125.00 parts of mixing of deionized water, four kinds of mixed liquors are stirred well to proper viscosity respectively under 60 ℃, obtain Portland clinker Within Monominerals colloidal sol, then four kinds of Within Monominerals colloidal sols are mixed, after ageing, form gel, 1170 ℃ of lower heat treatments 4 hours, be cooled to room temperature and namely get Portland clinker, the mineral composition of grog is tricalcium silicate 55%, dicalcium silicate 25%, calcium aluminate 5%, calcium aluminoferrite 15%.
Embodiment 3
A kind of preparation method of Portland clinker, according to the formulated colloidal sol of table 1, concrete preparation method may further comprise the steps:
According to weight ratio with ethyl orthosilicate ((C
2H
5O)
4Si) 45.61 parts, calcium nitrate hydrate (Ca (NO
3)
24H
2O) 155.26 parts, ethanol (C
2H
5OH) 1033.04 parts, nitric acid (HNO
3) 14.65 parts of mixing, according to weight ratio with ethyl orthosilicate ((C
2H
5O)
4Si) 36.28 parts, calcium nitrate hydrate (Ca (NO
3)
24H
2O) 82.33 parts, ethanol (C
2H
5OH) 650.48 parts, nitric acid (HNO
3) 9.22 parts of mixing, according to weight ratio with aluminum nitrate hydrate (Al (NO
3)
39H
2O) 11.11 parts, calcium nitrate hydrate (Ca (NO
3)
24H
2O) 10.49 parts, hexamethylenetetramine ((CH
2)
6N
4) 4.86 parts, acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)) 1.36 parts, 65.00 parts of mixing of deionized water, according to weight ratio with aluminum nitrate hydrate (Al (NO
3)
39H
2O) 24.69 parts, calcium nitrate hydrate (Ca (NO
3)
24H
2O) 23.31 parts and ferric nitrate hydrate (Fe (NO
3)
3) 9H
2O) 26.60 parts, hexamethylenetetramine ((CH
2)
6N
4) 11.56 parts, acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)) 3.02 parts, 135.00 parts of mixing of deionized water, four kinds of mixed liquors are stirred well to proper viscosity respectively under 60 ℃, obtain Portland clinker Within Monominerals colloidal sol, then four kinds of Within Monominerals colloidal sols are mixed, after ageing, form gel, 1150 ℃ of lower heat treatments 4 hours, be cooled to room temperature and namely get Portland clinker, the mineral composition of grog is tricalcium silicate 50%, dicalcium silicate 30%, calcium aluminate 4%, calcium aluminoferrite 16%.
The prescription (weight ratio) of table 1 Portland clinker colloidal sol
Ethyl orthosilicate | The calcium nitrate hydrate | Ethanol | Nitric acid | The aluminum nitrate hydrate | The ferric nitrate hydrate | Hexamethylenetetramine | Acetylacetone,2,4-pentanedione | Deionized water |
Embodiment 1 | 78.92 | 278.49 | 1673.30 | 23.72 | 39.51 | 21.61 | 17.89 | 4.84 | 217.00 |
Embodiment 2 | 80.41 | 274.36 | 1678.41 | 23.80 | 37.04 | 24.94 | 16.90 | 4.54 | 205.00 |
Embodiment 3 | 81.89 | 271.39 | 1683.52 | 23.87 | 35.80 | 26.60 | 16.41 | 4.39 | 200.00 |
Embodiment 4
A kind of preparation method of Portland clinker, this method obtain gel by sol-gel method with mixing of analytical pure chemical reagent and ageing, and the gained gel passes through high-temperature heat treatment again and is cooled to room temperature, obtains Portland clinker.Specifically may further comprise the steps:
(1) with ethyl orthosilicate ((C
2H
5O)
4Si), calcium nitrate hydrate (Ca (NO
3)
24H
2O), ethanol (C
2H
5OH), nitric acid (HNO
3) be 1: 3.4: 10 by weight: 0.1 mixes, and obtains mixed liquor A, and the control temperature is 50 ℃, fully stirs 10h, obtains the Within Monominerals Sol A;
(2) with ethyl orthosilicate ((C
2H
5O)
4Si), calcium nitrate hydrate (Ca (NO
3)
24H
2O), ethanol (C
2H
5OH), nitric acid (HNO
3) be 1: 2.27: 10 by weight: 0.1 mixes, and obtains mixed liquid B, and the control temperature is 50 ℃, fully stirs 10h, obtains the Within Monominerals sol B;
(3) with aluminum nitrate hydrate (Al (NO
3)
39H
2O), calcium nitrate hydrate (Ca (NO
3)
24H
2O), hexamethylenetetramine ((CH
2)
6N
4), acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)), deionized water is 1: 0.94: 0.2 by weight: mix at 0.08: 5, obtain mixed liquor C, the control temperature is 70 ℃, fully stirs 10h, obtains Within Monominerals colloidal sol C;
(4) with aluminum nitrate hydrate (Al (NO
3)
39H
2O), calcium nitrate hydrate (Ca (NO
3)
24H
2O), ferric nitrate hydrate (Fe (NO
3)
3) 9H
2O), hexamethylenetetramine ((CH
2)
6N
4), acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)), deionized water is 1: 1.26: 1.08 by weight: mix at 0.6: 0.08: 5, obtain mixed liquor D, the control temperature is 70 ℃, fully stirs 10h, obtains Within Monominerals colloidal sol D;
(5) with simple ore thing Sol A, simple ore thing sol B, simple ore thing colloidal sol C and simple ore thing colloidal sol D according to weight ratio 36: 24: 19: 31 mix, the control bath temperature is 70 ℃, ageing obtained gel in 5 days, gel is placed high-temperature cracking furnace, controlled temperature is 1150 ℃ and heat-treats 6h, is cooled to room temperature then and promptly gets Portland clinker.
Embodiment 5
A kind of preparation method of Portland clinker, this method obtain gel by sol-gel method with mixing of analytical pure chemical reagent and ageing, and the gained gel passes through high-temperature heat treatment again and is cooled to room temperature, promptly obtains Portland clinker.Specifically may further comprise the steps:
(1) with ethyl orthosilicate ((C
2H
5O)
4Si), calcium nitrate hydrate (Ca (NO
3)
24H
2O), ethanol (C
2H
5OH), nitric acid (HNO
3) be 1: 3.4: 30 by weight: 0.5 mixes, and obtains mixed liquor A, and the control temperature is 70 ℃, fully stirs 8h, obtains the Within Monominerals Sol A;
(2) with ethyl orthosilicate ((C
2H
5O)
4Si), calcium nitrate hydrate (Ca (NO
3)
24H
2O), ethanol (C
2H
5OH), nitric acid (HNO
3) be 1: 2.27: 30 by weight: 0.6 mixes, and obtains mixed liquid B, and the control temperature is 70 ℃, fully stirs 8h, obtains the Within Monominerals sol B;
(3) with aluminum nitrate hydrate (Al (NO
3)
39H
2O), calcium nitrate hydrate (Ca (NO
3)
24H
2O), hexamethylenetetramine ((CH
2)
6N
4), acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)), deionized water is 1: 0.94: 0.6 by weight: mix at 0.16: 10, obtain mixed liquor C, the control temperature is 50 ℃, fully stirs 12h, obtains Within Monominerals colloidal sol C;
(4) with aluminum nitrate hydrate (Al (NO
3)
39H
2O), calcium nitrate hydrate (Ca (NO
3)
24H
2O), ferric nitrate hydrate (Fe (NO
3)
3) 9H
2O), hexamethylenetetramine ((CH
2)
6N
4), acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)), deionized water is 1: 1.26: 1.08 by weight: mix at 0.6: 0.16: 10, obtain mixed liquor D, the control temperature is 50 ℃, fully stirs 12h, obtains Within Monominerals colloidal sol D;
(5) with simple ore thing Sol A, simple ore thing sol B, simple ore thing colloidal sol C and simple ore thing colloidal sol D according to weight ratio 55: 40: 11: 20 mix, the control bath temperature is 80 ℃, ageing obtained gel in 3 days, gel is placed high-temperature cracking furnace, controlled temperature is 1200 ℃ and heat-treats 4h, is cooled to room temperature then and promptly gets Portland clinker.
Claims (5)
1. the preparation method of a Portland clinker is characterized in that, this method is by sol-gel method mixing of analytical pure chemical reagent and ageing to be obtained gel, and the gained gel passes through high-temperature heat treatment again and is cooled to room temperature, promptly obtains Portland clinker.
2. the preparation method of a kind of Portland clinker according to claim 1 is characterized in that, this method specifically may further comprise the steps:
(1) with ethyl orthosilicate ((C
2H
5O)
4Si), calcium nitrate hydrate (Ca (NO
3)
24H
2O), ethanol (C
2H
5OH), nitric acid (HNO
3) be 1: 3.4 by weight: (10-30): (0.1-0.5) mix, obtain mixed liquor A, the control temperature is 50-70 ℃, fully stirs 8-10h, obtains the Within Monominerals Sol A;
(2) with ethyl orthosilicate ((C
2H
5O)
4Si), calcium nitrate hydrate (Ca (NO
3)
24H
2O), ethanol (C
2H
5OH), nitric acid (HNO
3) be 1: 2.27 by weight: (10-30): (0.1-0.6) mix, obtain mixed liquid B, the control temperature is 50-70 ℃, fully stirs 8-10h, obtains the Within Monominerals sol B;
(3) with aluminum nitrate hydrate (Al (NO
3)
39H
2O), calcium nitrate hydrate (Ca (NO
3)
24H
2O), hexamethylenetetramine ((CH
2)
6N
4), acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)), deionized water is 1: 0.94 by weight: (0.2-0.6): (0.08-0.16): (5-10) mix, obtain mixed liquor C, the control temperature is 50-70 ℃, fully stirs 10-12h, obtains Within Monominerals colloidal sol C;
(4) with aluminum nitrate hydrate (Al (NO
3)
39H
2O), calcium nitrate hydrate (Ca (NO
3)
24H
2O), ferric nitrate hydrate (Fe (NO
3)
3) 9H
2O), hexamethylenetetramine ((CH
2)
6N
4), acetylacetone,2,4-pentanedione ((CH
3CO)
2CH (AcAcH)), deionized water is 1: 1.26: 1.08 by weight: (0.2-0.6): (0.08-0.16): (5-10) mix, obtain mixed liquor D, the control temperature is 50-70 ℃, fully stirs 10-12h, obtains Within Monominerals colloidal sol D;
(5) with simple ore thing Sol A, simple ore thing sol B, simple ore thing colloidal sol C and simple ore thing colloidal sol D according to weight ratio (36-55): (24-40): (11-19): (20-31) mix, the control bath temperature is 70-80 ℃, obtained gel in ageing 3-5 days, gel is placed high-temperature cracking furnace, controlled temperature is 1150-1200 ℃ and heat-treats 4-6h, is cooled to room temperature then and promptly gets Portland clinker.
3. the preparation method of a kind of Portland clinker according to claim 2, it is characterized in that described tetraethoxy, nitrocalcite hydrate, aluminum nitrate hydrate, iron nitrate hydrate, hexamethylenetetramine, methyl ethyl diketone, ethanol and nitric acid are the analytical pure chemical reagent.
4. the preparation method of a kind of Portland clinker according to claim 2 is characterized in that, described thermal treatment temp is 1150-1200 ℃.
5. the preparation method of a kind of Portland clinker according to claim 2 is characterized in that, described heat treatment time is 4-6h.
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Cited By (2)
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---|---|---|---|---|
CN106220005A (en) * | 2016-07-26 | 2016-12-14 | 武汉大学 | A kind of method utilizing sol-gel technique to prepare ultra-dispersed high pure state nano cement |
CN114315194A (en) * | 2021-12-20 | 2022-04-12 | 武汉大学 | High-reactivity aluminum-containing cement clinker powder and preparation method and application thereof |
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《中国博士学位论文全文数据库,工程科技I辑》 20080715 朱晓燕 煅烧条件对高胶凝性水泥熟料的烧成和阿特晶体结构的影响 , * |
Cited By (4)
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CN106220005A (en) * | 2016-07-26 | 2016-12-14 | 武汉大学 | A kind of method utilizing sol-gel technique to prepare ultra-dispersed high pure state nano cement |
CN106220005B (en) * | 2016-07-26 | 2017-11-10 | 武汉大学 | A kind of method that ultra-dispersed high pure state nano cement is prepared using sol-gel technique |
CN114315194A (en) * | 2021-12-20 | 2022-04-12 | 武汉大学 | High-reactivity aluminum-containing cement clinker powder and preparation method and application thereof |
CN114315194B (en) * | 2021-12-20 | 2022-12-30 | 武汉大学 | High-reactivity aluminum-containing cement clinker powder and preparation method and application thereof |
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