CN102153295B - Method for preparing Portland cement clinker - Google Patents

Method for preparing Portland cement clinker Download PDF

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CN102153295B
CN102153295B CN 201010109401 CN201010109401A CN102153295B CN 102153295 B CN102153295 B CN 102153295B CN 201010109401 CN201010109401 CN 201010109401 CN 201010109401 A CN201010109401 A CN 201010109401A CN 102153295 B CN102153295 B CN 102153295B
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hydrate
monominerals
temperature
sol
gel
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CN102153295A (en
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刘贤萍
王培铭
陈红霞
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Tongji University
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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

A kind of preparation method of Portland clinker
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 the synthetic cement in laboratory and grog Within Monominerals as research object.Yet when synthesizing cement clinker mineral with the method for conventional high-temperature sintering reaction, not only desired reaction temperature is high, and owing to usually adopting 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, the shortcoming such as the synthesis temperature that they all attempt to overcome traditional solid-phase sintering method is high, reaction is wayward makes 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 adopts, hydrothermal synthesis method is only applicable to the synthetic silicate mineral, the Ca/Si=2 of especially Dicalcium Phosphate (Feed Grade), and control Hydrothermal Synthesis product is difficulty relatively, and combustion synthesis method is only applicable to calcium aluminate and calcium aluminoferrite.Sol-gel method is a kind of method of colloid chemistry, it uses liquid chemical reagent or colloidal sol to be raw material, with metal alkoxide or inorganic salt through being hydrolyzed direct formation colloidal sol or through separating the solidifying colloidal sol that forms, then make the solute polymeric gel, again organic composition is removed in gel drying, calcination, reached at last required inorganic materials.Preparation process comprises the preparation of colloidal sol, formation and gel drying and the thermal 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, make below the free calcium oxide content to 1%, needs just can finish through repeated multiple times grinding, powder compression and sintering; Because the Within Monominerals crystal that usually adopts mineralizer (such as cupric oxide, Calcium Fluoride (Fluorspan), calcium sulfate, phosphorus oxide, titanium oxide) etc. to reduce firing temperature or make some crystal formation at room temperature can stable existence, can introduce the phase except designing product in cement clinker mineral.
Summary of the invention
Purpose of the present invention is exactly to provide the preparation method that a kind of purity is high, preparation technology simple, reaction process is held manageable Portland clinker for the defective that overcomes above-mentioned prior art existence.
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, the method is by sol-gel method the 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, namely obtains Portland clinker.
The method specifically may further comprise the steps:
(1) with tetraethoxy ((C 2H 5O) 4Si), nitrocalcite 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 tetraethoxy ((C 2H 5O) 4Si), nitrocalcite 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), nitrocalcite hydrate (Ca (NO 3) 24H 2O), hexamethylenetetramine ((CH 2) 6N 4), methyl ethyl diketone ((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 solution 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), nitrocalcite hydrate (Ca (NO 3) 24H 2O), iron nitrate hydrate (Fe (NO 3) 3) 9H 2O), hexamethylenetetramine ((CH 2) 6N 4), methyl ethyl diketone ((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 solution D, the control temperature is 50-70 ℃, fully stirs 10-12h, obtains Within Monominerals colloidal sol D;
(5) with Within Monominerals Sol A, Within Monominerals sol B, Within Monominerals colloidal sol C and Within Monominerals 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, the control temperature is 1150-1200 ℃ and heat-treats 4-6h, then is cooled to room temperature and namely 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, the product uniformity coefficient is high, chemical uniformity is good, because in sol-gel process, colloidal sol is made by solution, so chemical composition is consistent in the micelle and between micelle, and purity is high, and its Free CaO content all is lower than 0.5%, and product granularity is little.Need not pass through sintering reaction in addition, more easily prepare fine powder than conventional sintering method, gel grinds gained powder median size 2-4 μ m with agate mortar after Overheating Treatment, and preparation technology is simple, and reaction process 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 tetraethoxy ((C 2H 5O) 4Si) 54.74 parts, nitrocalcite 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 tetraethoxy ((C 2H 5O) 4Si) 24.18 parts, nitrocalcite 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, nitrocalcite hydrate (Ca (NO 3) 24H 2O) 18.36 parts, hexamethylenetetramine ((CH 2) 6N 4) 8.50 parts, methyl ethyl diketone ((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, nitrocalcite hydrate (Ca (NO 3) 24H 2O) 18.94 parts and iron nitrate hydrate (Fe (NO 3) 3) 9H 2O) 21.61 parts, hexamethylenetetramine ((CH 2) 6N 4) 9.39 parts, methyl ethyl diketone ((CH 3CO) 2CH (AcAcH)) 2.46 parts, 110.00 parts of mixing of deionized water, four kinds of mixed solutions 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 thermal treatments 4 hours, be cooled to room temperature and namely get Portland clinker, the mineral composition of grog is tricalcium silicate 60%, Dicalcium Phosphate (Feed Grade) 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 tetraethoxy ((C 2H 5O) 4Si) 50.18 parts, nitrocalcite 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 tetraethoxy ((C 2H 5O) 4Si) 30.23 parts, nitrocalcite 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, nitrocalcite hydrate (Ca (NO 3) 24H 2O) 13.11 parts, hexamethylenetetramine ((CH 2) 6N 4) 6.07 parts, methyl ethyl diketone ((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, nitrocalcite hydrate (Ca (NO 3) 24H 2O) 21.85 parts and iron nitrate hydrate (Fe (NO 3) 3) 9H 2O) 24.94 parts, hexamethylenetetramine ((CH 2) 6N 4) 10.83 parts, methyl ethyl diketone ((CH 3CO) 2CH (AcAcH)) 2.84 parts, 125.00 parts of mixing of deionized water, four kinds of mixed solutions 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 thermal treatments 4 hours, be cooled to room temperature and namely get Portland clinker, the mineral composition of grog is tricalcium silicate 55%, Dicalcium Phosphate (Feed Grade) 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 tetraethoxy ((C 2H 5O) 4Si) 45.61 parts, nitrocalcite 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 tetraethoxy ((C 2H 5O) 4Si) 36.28 parts, nitrocalcite 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, nitrocalcite hydrate (Ca (NO 3) 24H 2O) 10.49 parts, hexamethylenetetramine ((CH 2) 6N 4) 4.86 parts, methyl ethyl diketone ((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, nitrocalcite hydrate (Ca (NO 3) 24H 2O) 23.31 parts and iron nitrate hydrate (Fe (NO 3) 3) 9H 2O) 26.60 parts, hexamethylenetetramine ((CH 2) 6N 4) 11.56 parts, methyl ethyl diketone ((CH 3CO) 2CH (AcAcH)) 3.02 parts, 135.00 parts of mixing of deionized water, four kinds of mixed solutions 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 thermal treatments 4 hours, be cooled to room temperature and namely get Portland clinker, the mineral composition of grog is tricalcium silicate 50%, Dicalcium Phosphate (Feed Grade) 30%, calcium aluminate 4%, calcium aluminoferrite 16%.
The prescription (weight ratio) of table 1 Portland clinker colloidal sol
Tetraethoxy The nitrocalcite hydrate Ethanol Nitric acid The aluminum nitrate hydrate The iron nitrate hydrate Hexamethylenetetramine Methyl ethyl diketone 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, the method obtain gel by sol-gel method with the 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 tetraethoxy ((C 2H 5O) 4Si), nitrocalcite 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 tetraethoxy ((C 2H 5O) 4Si), nitrocalcite 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), nitrocalcite hydrate (Ca (NO 3) 24H 2O), hexamethylenetetramine ((CH 2) 6N 4), methyl ethyl diketone ((CH 3CO) 2CH (AcAcH)), deionized water is 1: 0.94: 0.2 by weight: mix at 0.08: 5, obtain mixed solution 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), nitrocalcite hydrate (Ca (NO 3) 24H 2O), iron nitrate hydrate (Fe (NO 3) 3) 9H 2O), hexamethylenetetramine ((CH 2) 6N 4), methyl ethyl diketone ((CH 3CO) 2CH (AcAcH)), deionized water is 1: 1.26: 1.08 by weight: mix at 0.6: 0.08: 5, obtain mixed solution D, the control temperature is 70 ℃, fully stirs 10h, obtains Within Monominerals colloidal sol D;
(5) with Within Monominerals Sol A, Within Monominerals sol B, Within Monominerals colloidal sol C and Within Monominerals 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, the control temperature is 1150 ℃ and heat-treats 6h, then is cooled to room temperature and namely gets Portland clinker.
Embodiment 5
A kind of preparation method of Portland clinker, the method obtain gel by sol-gel method with the 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, namely obtains Portland clinker.Specifically may further comprise the steps:
(1) with tetraethoxy ((C 2H 5O) 4Si), nitrocalcite 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 tetraethoxy ((C 2H 5O) 4Si), nitrocalcite 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), nitrocalcite hydrate (Ca (NO 3) 24H 2O), hexamethylenetetramine ((CH 2) 6N 4), methyl ethyl diketone ((CH 3CO) 2CH (AcAcH)), deionized water is 1: 0.94: 0.6 by weight: mix at 0.16: 10, obtain mixed solution 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), nitrocalcite hydrate (Ca (NO 3) 24H 2O), iron nitrate hydrate (Fe (NO 3) 3) 9H 2O), hexamethylenetetramine ((CH 2) 6N 4), methyl ethyl diketone ((CH 3CO) 2CH (AcAcH)), deionized water is 1: 1.26: 1.08 by weight: mix at 0.6: 0.16: 10, obtain mixed solution D, the control temperature is 50 ℃, fully stirs 12h, obtains Within Monominerals colloidal sol D;
(5) with Within Monominerals Sol A, Within Monominerals sol B, Within Monominerals colloidal sol C and Within Monominerals 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, the control temperature is 1200 ℃ and heat-treats 4h, then is cooled to room temperature and namely gets Portland clinker.

Claims (2)

1. the preparation method of a Portland clinker is characterized in that, the method is by sol-gel method the 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, namely obtains Portland clinker;
The method specifically may further comprise the steps:
(1) with tetraethoxy (C 2H 5O) 4Si, nitrocalcite hydrate Ca (NO 3) 24H 2O, ethanol C 2H 5OH, nitric acid HNO 3Be 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 tetraethoxy (C 2H 5O) 4Si, nitrocalcite hydrate Ca (NO 3) 24H 2O, ethanol C 2H 5OH, nitric acid HNO 3Be 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, nitrocalcite hydrate Ca (NO 3) 24H 2O, hexamethylenetetramine (CH 2) 6N 4, methyl ethyl diketone (CH 3CO) 2CH (AcAcH), deionized water are 1: 0.94 by weight: (0.2-0.6): (0.08-0.16): (5-10) mix, obtain mixed solution 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, nitrocalcite hydrate Ca (NO 3) 24H 2O, iron nitrate hydrate Fe (NO 3) 3) 9H 2O, hexamethylenetetramine (CH 2) 6N 4, methyl ethyl diketone (CH 3CO) 2CH (AcAcH), deionized water are 1: 1.26: 1.08 by weight: (0.2-0.6): (0.08-0.16): (5-10) mix, obtain mixed solution D, the control temperature is 50-70 ℃, fully stirs 10-12h, obtains Within Monominerals colloidal sol D;
(5) with Within Monominerals Sol A, Within Monominerals sol B, Within Monominerals colloidal sol C and Within Monominerals 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, the control temperature is 1150-1200 ℃ and heat-treats 4-6h, then is cooled to room temperature and namely gets Portland clinker.
2. the preparation method of a kind of Portland clinker according to claim 1, 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.
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