CN114230208B - High-strength cement and preparation method thereof - Google Patents

High-strength cement and preparation method thereof Download PDF

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CN114230208B
CN114230208B CN202210036890.6A CN202210036890A CN114230208B CN 114230208 B CN114230208 B CN 114230208B CN 202210036890 A CN202210036890 A CN 202210036890A CN 114230208 B CN114230208 B CN 114230208B
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cement
clinker
raw material
parts
strength cement
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CN114230208A (en
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段平娥
高小育
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Ningxia Shizuishan Saima Cement Co ltd
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Ningxia Shizuishan Saima Cement Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/24—Cements from oil shales, residues or waste other than slag
    • C04B7/243—Mixtures thereof with activators or composition-correcting additives, e.g. mixtures of fly ash and alkali activators
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/08—Fats; Fatty oils; Ester type waxes; Higher fatty acids, i.e. having at least seven carbon atoms in an unbroken chain bound to a carboxyl group; Oxidised oils or fats
    • C04B24/085—Higher fatty acids
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/10—Carbohydrates or derivatives thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
    • C04B24/121—Amines, polyamines
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
    • C04B24/124—Amides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/16—Sulfur-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/14—Cements containing slag
    • C04B7/147—Metallurgical slag
    • C04B7/153—Mixtures thereof with other inorganic cementitious materials or other activators
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/36—Manufacture of hydraulic cements in general
    • C04B7/38—Preparing or treating the raw materials individually or as batches, e.g. mixing with fuel
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/36—Manufacture of hydraulic cements in general
    • C04B7/38—Preparing or treating the raw materials individually or as batches, e.g. mixing with fuel
    • C04B7/42—Active ingredients added before, or during, the burning process
    • C04B7/421—Inorganic materials
    • C04B7/425—Acids or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/36—Manufacture of hydraulic cements in general
    • C04B7/38—Preparing or treating the raw materials individually or as batches, e.g. mixing with fuel
    • C04B7/42—Active ingredients added before, or during, the burning process
    • C04B7/428—Organic materials
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/52—Grinding aids; Additives added during grinding
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding

Abstract

The invention discloses high-strength cement and a preparation method thereof. The preparation method of the high-strength cement comprises the following steps: the cement prepared by the invention has good stability, water reduction rate and high strength, and the industrial wastes are recycled and used as raw materials, so that the water consumption is reduced, the resource utilization rate is improved, and the production cost is reduced.

Description

High-strength cement and preparation method thereof
Technical Field
The invention relates to the field of cement building materials, in particular to high-strength cement and a preparation method thereof.
Background
The cement industry is used as a traditional industry, and is a large resource, energy consumption user, carbon emission user and water resource consumption user. Since construction works generally require a large amount of cement, which is a high-cost material, most companies are trying to reduce the use of cement in the construction to reduce the overall cost. The strength of a building is determined by the cement ratio used, the particle size of the aggregate and the mineral composition. If the cement content is too low, the workability of the material may be adversely affected. In addition, the uneven distribution of cement in concrete also causes the structural performance of the concrete to be reduced, so that a large amount of water is required to ensure the fluidity of cement materials, so that the uneven distribution is avoided, and the utilization rate of cement is improved. Generally, on the premise of not increasing the cost, proper water reducing agents and accelerators are needed to prepare high-quality concrete materials (such as materials with good fluidity, low water consumption, quick setting time and high compressive strength). At present, the most widely used water reducer is a polycarboxylate type high-efficiency water reducer, but the water reducing effect of the polycarboxylate type water reducer is limited.
Chinese patent CN 109678439A provides a high fluidity cement concrete and a preparation method thereof, wherein the cement concrete comprises 500-600 parts of sulphoaluminate cement, 300-400 parts of fine sand, 250-300 parts of medium coarse sand, 100-120 parts of mineral powder, 15-25 parts of graphene oxide, 75-85 parts of hollow glass beads, 50-80 parts of gypsum, 33-49 parts of composite additive, 260-320 parts of water and 0.6-1.2 parts of concrete fiber; the cement concrete prepared by the method can effectively improve the fluidity and ensure the compression resistance, the impermeability and the frost resistance. However, the water reducing effect of the invention only depends on the water reducing agent in the composite additive, the water reducing effect is limited, the added graphene oxide has higher cost and narrow application range.
Chinese patent CN 110386793A discloses an ultra-retarding cement slurry with low water loss and high fluidity, which belongs to the technical field of slurry, and is characterized in that the cement slurry comprises the following components in parts by weight: 195-205 parts of cement, 780-820 parts of fly ash, 975-1025 parts of water, 146-154 parts of glycerin, 0.8-1.2 parts of sulfonated lignite resin, 1.3-1.7 parts of polycarboxylate superplasticizer and 0.8-1.2 parts of air entraining agent. The cement paste is prepared into a cementing body of cement paste by utilizing the retarding effect of the fly ash according to a specific proportion, so that the retarding time of the cement paste can be up to 45 hours under the high temperature condition of 40 ℃. On the premise of ensuring the retarding effect, the cement paste has high fluidity and low water loss by adjusting the mass ratio of the gel body to the water. However, the water reducing effect of the method depends on the polycarboxylate water reducer, and the cement has the defects of low strength and long setting period after setting.
In the invention, the addition of the magnesium triflate, combined with stachyose and triethylamine, enhances the electrostatic repulsive force and the steric hindrance effect between cements, and improves the water reducing rate and the mortar fluidity of the cements.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, the technical problems to be solved by the present invention are: (1) recycling industrial waste to prepare environment-friendly cement; (2) Solves the problem of insufficient cement strength caused by the incorporation of industrial wastes; (3) The water reducing rate of cement and the fluidity of mortar are improved, and water resources are saved.
In order to achieve the aim, the invention provides the high-strength cement and the preparation method thereof, the method adopts oil-based mud drill cuttings, electric furnace slag, fly ash, copper slag, red mud and other industrial wastes to reasonably match limestone, shale and dihydrate gypsum as main raw materials for producing cement, and adds grinding aid, magnesium triflate and reinforcing agent as functional substances, so that the prepared cement has good stability and water reduction rate and can be used as high-quality cement in strength.
In order to achieve the above object, the present invention adopts the following technical scheme:
the preparation method of the high-strength cement comprises the following steps of:
crushing of S1 raw materials: weighing 10-30 parts of oil-based mud drill cuttings, 80-100 parts of limestone, 10-20 parts of copper slag, 1-5 parts of shale and 1-5 parts of red mud, respectively crushing and uniformly mixing to obtain crushed raw materials;
grinding S2 raw materials: adding grinding aid into the crushed raw material prepared in the step S1 for fine grinding, and uniformly mixing to obtain fine ground raw material;
s3, preparation of clinker: uniformly stirring the finely ground raw material obtained in the step S2 with water and a sintering aid, pressing into a test cake, drying the test cake, calcining, and cooling to obtain clinker;
s4, preparation of cement: and (3) crushing and grinding the clinker prepared in the step (S3) with 20-40 parts of furnace slag, 20-40 parts of fly ash, 1-5 parts of magnesium triflate, dihydrate gypsum and reinforcing agent to obtain the high-strength cement.
The grinding aid is silicate cement grinding aid; preferably, the composition is one or two or more of triglycerol monolaurate, triglycerol monolaurate and N, N-dimethylformamide; further preferably, the grinding aid is triglyceryl monolaurate, and the addition amount of the grinding aid is 0.03-1% of the mass of the crushed raw material. The grinding aid added by the invention has stable quality and obvious effect, can reduce cement screen residue, avoid excessive grinding of particles, improve grinding efficiency, reduce grinding energy consumption, promote hydration of silicate minerals, improve cement activity and facilitate the improvement of later strength of cement.
The sintering aid is tetrasodium diphosphate and/or sodium lignin sulfonate. Preferably, the sintering aid is a mixture of tetrasodium diphosphate and sodium lignin sulfonate, and the mass ratio of the tetrasodium diphosphate to the sodium lignin sulfonate is 2-3:3-5. The addition amount of the sintering aid is 0.1-0.5% of the mass of the finely ground raw material.
The inventor found that by adding the mixture of the sintering aid tetra sodium diphosphate and the sodium lignin sulfonate, the reaction activation energy of the raw material is reduced, and Fe is strengthened 2 O 3 、SiO 2 、CaO、Al 2 O 3 Fe with enhanced reactivity at high temperature 2 O 3 、SiO 2 、CaO、Al 2 O 3 Can absorb the pollution gases such as sulfur dioxide, nitrogen oxides and the like generated in the combustion process, reduce the emission of the pollution gases such as sulfur dioxide, nitrogen oxides and the like, reduce the environmental pollution and simultaneously reduce the content of free calcium oxide in cement clinker.
Crushing in the step S1, namely crushing the raw materials until the average size is smaller than 2-3 mm;
the fineness of the finely ground raw materials in the step S2 is kept to be 10-15% of 80 mu m screen residue, and the 200 mu m screen residue is less than 1-1.5%;
in the step S3, the mass ratio of raw material to water is 1: 10-20 parts; the calcining step is that the temperature rising rate of the section of the lifting furnace at 0-950 ℃ is 5-10 ℃/min, the temperature is kept for 30-60 min at 950 ℃, the temperature rising rate of the section of the lifting furnace at 950-1300 ℃ is 3-5 ℃/min, the temperature keeping time at 1300 ℃ is 10-20 min, and the calcining is finished.
The mass of the dihydrate gypsum in the step S4 is 2-5% of the mass of the clinker; the fineness of the ground cement is kept to be less than 5-10% after 80 mu m screen residue.
The reinforcing agent is stachyose and/or triethylamine, and the addition amount is 0.01-0.05% of the clinker mass;
preferably, the enhancer is a mixture of stachyose and triethylamine in a mass ratio of 1:2-3.
The inventor finds that the mixture of the reinforcing agent stachyose and triethylamine improves the grinding assisting property of cement clinker, and hydration points are formed on the surface of cement, so that the formation of ettringite is promoted, the penetration of water in cement particles is accelerated, the hydrolysis of mineral phases of the cement clinker is promoted, the particle distribution of the cement is changed, the uniformity coefficient of the cement is increased, a relatively uniform and compact structure is formed, and the strength of the cement is enhanced, so that the cement is used as high-quality cement.
Magnesium triflate can cause electrostatic repulsion and steric hindrance effects. The electrostatic repulsion is due to-COO and-SO 3 The anions are cations (Ca 2+ ) And (5) adsorption. A large amount of anions are accumulated on the surface of the cement particles. The strong electrostatic repulsion between these anions repels the cement particles from each other. This breaks the flocculated structure of the cement, resulting in free water being released from the cement.
The steric hindrance effect is due to the fact that stachyose and triethylamine form a polymer molecule adsorption layer on the surface of the cement particles. As the polymer molecular content increases, the adsorption layer becomes thicker, preventing the formation of a cement flocculation structure. Therefore, the unique steric hindrance effect of stachyose and triethylamine makes the stachyose and triethylamine show stronger water-reducing capacity. On the other hand, after the water reducer is added into the cement, part of the water reducer is wrapped by the cement hydration product to form a composite layer. The higher negative charge density of magnesium triflate makes it easier to enter the composite layer, thereby reducing the required water reducing agent content. Therefore, the existence of the magnesium triflate increases electrostatic repulsive force between cements and steric hindrance effect, and further improves the water reducing rate and the mortar fluidity.
The explanation of some raw materials in the invention is as follows:
(1) Oil-based mud drill cuttings
The oil-based mud drill cuttings belong to oil-containing sludge, are residues which are difficult to treat, and are mainly characterized by a water-in-oil structure, wherein main minerals of the oil-based mud drill cuttings are dolomite, quartz and barium sulfate, and the barium sulfate content is high; the mud part contains various organic matters, mainly comprises long-chain hydrocarbon, has main carbon chain length of 11-28, and plays a role of mineralizer in a cement system. The oil-based mud drill cuttings used in the invention come from the southeast of Sichuan province, the water content of the oil-based mud drill cuttings is 15% +/-2%, the oil content is 20% +/-1%, and the radioactivity ira=0.194 is less than or equal to 1.0; ir=0.114 is less than or equal to 1.3, and meets the requirement of GB6566-2001 radionuclide limit for building materials for interior decoration.
(2) Limestone powder
The main component of the limestone is calcium carbonate, which is decomposed into calcium oxide and carbon dioxide at high temperature, and the ground limestone powder can accelerate the hydration of silicate cement, improve the pore structure of cement-based materials and harden the interface of cement paste, thereby improving the matrix strength.
(3) Slag of electric furnace
The electric furnace slag is solid waste discharged in the process of smelting metal by adopting an electric furnace, and the main components are oxides of calcium, iron, copper, silicon, magnesium, aluminum, manganese, phosphorus and the like, so that better gelling activity can be obtained under proper conditions, the electric furnace slag can be used as auxiliary gelling materials of cement and the like, the later strength of composite cement can not be reduced by doping the electric furnace slag, the microstructure of cement paste can be obviously improved, and the durability of cement can be improved.
(4) Fly ash
Fly ash, also known as fly ash or soot, is formed by burning and cooling pulverized coal at high temperature. Most of the materials are spherical, have smooth surfaces and smaller micropores, contain a large amount of oxides of silicon, iron, aluminum, calcium, magnesium, sodium, potassium and sulfur and various microelements, belong to a mixed material with pozzolanic property, have potential chemical activity, and the fly ash is singly mixed with water without hydraulic activity, but has Ca (OH) 2 Under the existing condition, the cement-like cementing material can be produced by reacting with water, has certain strength, has similarity with the chemical composition of clay in cement production, can be used as an additive for producing cement, can replace clay to be used as clinker for producing silicate cement, reduces electric energy consumption and carbon emission in cement production, improves the mixing amount of cement and reduces the production cost.
(5) Copper slag
Copper slag is slag produced in copper smelting process, belongs to one kind of nonferrous metal slag, and contains Fe, cu, zn, pb, co, ni and other valuable metals and small amount of noble metals. Can replace iron powder as mineralizer in cement manufacture and can be used as iron correction agent to produce Portland cement.
(6) Shale
Shale is a tiny particle formed by hardening clay substances, is easy to break into obvious rock stratum, and takes clay minerals (kaolinite, hydromica and the like) as main materials, and has chemical components of SiO 2 The content is 45-80%, al 2 O 3 The content is 12 to 25 percent, fe 2 O 3 The content is 2-10%, and the CaO content is 0.2-12%.
(7) Red mud
The red mud is an industrial solid waste discharged when alumina is extracted in the aluminum production industry, has large hidden ferric oxide amount and similar appearance to red mud, and is called red mud, and the main component is SiO 2 、 Al 2 O 3 、CaO、Fe 2 O 3 Etc.
(8) Dihydrate gypsum
The dihydrate gypsum, namely the gypsum, is the dihydrate of calcium sulfate, is an important constituent material of cement, not only can play a role in retarding, but also can serve as a sulfate excitant for improving the activity of the cement, and meanwhile SO in the cement 3 The amount of the content can directly affect the strength of the cement.
Compared with the prior art, the invention has the beneficial effects that:
1. the sintering aid with special proportion is added in the raw material calcining process, so that the reaction activation energy of the raw material is reduced, and Fe generated in the raw material calcining process is intensified 2 O 3 、SiO 2 、CaO、Al 2 O 3 Fe with enhanced reactivity at high temperature 2 O 3 、SiO 2 、CaO、Al 2 O 3 Can absorb the pollution gases such as sulfur dioxide, nitrogen oxides and the like generated in the combustion process, reduce the emission of the pollution gases such as sulfur dioxide, nitrogen oxides and the like, reduce the environmental pollution and simultaneously reduce the content of free CaO in cement clinker.
2. The mixture of the reinforcing agent stachyose and triethylamine is used in the cement preparation process, so that the dispersibility of cement clinker is improved, hydration points are formed on the surface of cement, thereby promoting the formation of ettringite, accelerating the penetration of water in cement particles, promoting the hydrolysis of mineral phases of the cement clinker, changing the particle distribution of cement, increasing the uniformity coefficient of cement, forming a relatively uniform and compact structure, enhancing the strength of cement and reaching the strength required by engineering construction.
3. The addition of the magnesium triflate can increase electrostatic repulsive force and steric hindrance effect between cements, and improve water reducing rate and mortar fluidity.
4. The cement prepared by the method has good stability, utilizes a large amount of industrial waste, reduces the pollution to the environment and reduces the cost of cement production.
Detailed Description
The invention is further illustrated by means of the following examples, which are not intended to limit the scope of the invention. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
The comparative example and the examples of the present invention have the following parameters of part of raw materials:
oil-based mud drill cuttings from the luzhou sun 10H-40 drilling platform.
Limestone: caCO purchased from Qingshan building materials Co.Ltd 3 95%, 53.73%, 2.0%, 0.56% and 32.8g/cm of bulk density 3 The color is gray, and the size is 1-3cm.
Copper slag: the main chemical composition is SiO 2 27.59% CaO, 5.26% MgO, 2.2% Al 2 O 3 The content is 5.26 percent, fe 2 O 3 The content is 59.16%.
Shale: purchased from Shijia Feiji mineral products limited company, has the appearance of sheet, the grade of first grade and the product number of 078.
Red mud: the processing plant of the Hemsleya amabilis mineral products is in powder form, the product number is h858558, and the grade is first grade.
Magnesium triflate: molecular weight of Shanghai long root chemical Co., ltd.): 322.44, cas number: 60871-83-2.
Electric furnace slag: loss on ignition of 1.04%, siO 2 The content is 20.67%, al 2 O 3 The content is 6.35 percent, fe 2 O 3 The content is 38.97%, the CaO content is 23.87%, and the MgO content is 4.47%.
The fly ash is class II fly ash, and is purchased from Wuhan yang power plant, and has specific surface area 449m 2 /kg。
The dihydrate gypsum is purchased from Hezhou City and Foundation building materials Co., ltd, has the flexural strength of 2.35MPa, the standard consistency of 95.23%, the expansion coefficient of 6.3, the initial setting time of 3.45 minutes and the final setting time of 59.36 minutes.
Comparative example 1
A preparation method of high-strength cement comprises the following steps:
crushing of S1 raw materials: respectively crushing 20g of oil-based mud drill cuttings, 100g of limestone, 10g of copper slag, 5g of shale and 5g of red mud by using a jaw crusher, and uniformly mixing to obtain crushed raw materials, wherein the average size of the crushed raw materials is less than 1.5 mm;
grinding S2 raw materials: adding 7g of triglyceryl monolaurate into the crushed raw material prepared in the step S1 for fine grinding, and uniformly mixing to obtain fine ground raw material, wherein the fineness of the fine ground raw material is kept to be 10% after 80 mu m screen residue and below 1% after 200 mu m screen residue;
s3, preparation of clinker: stirring the finely ground raw material prepared in the step S2 with 1500g of water, adding the mixture into a tabletting mold, using a TYE-300 type pressure tester to carry for 10S with 11KN to obtain a test cake, drying the test cake in a drying oven at 80 ℃ for 10h, then placing the test cake in a SJF-1600 lifting furnace for calcination, setting the heating rate of a section at the temperature of 0-950 ℃ to be 10 ℃/min, keeping the temperature of the section at the temperature of 950 ℃ to be 30min, the heating rate of the section at the temperature of 950-1300 ℃ to be 5 ℃/min, and keeping the temperature of the section at the temperature of 1300 ℃ to be 10min, and ending the calcination; cooling the clinker to 30 ℃ to obtain clinker;
s4, preparation of cement: crushing and grinding the clinker prepared in the step S3, 20g of electric furnace slag, 30g of fly ash and dihydrate gypsum uniformly to obtain high-strength cement; the addition amount of the dihydrate gypsum is 2.5% of the clinker mass.
Example 1
A preparation method of high-strength cement comprises the following steps:
crushing of S1 raw materials: respectively crushing 20g of oil-based mud drill cuttings, 100g of limestone, 10g of copper slag, 5g of shale and 5g of red mud by using a jaw crusher, and uniformly mixing to obtain crushed raw materials, wherein the average size of the crushed raw materials is less than 1.5 mm;
grinding S2 raw materials: adding 7g of triglyceryl monolaurate into the crushed raw material prepared in the step S1 for fine grinding, and uniformly mixing to obtain fine ground raw material, wherein the fineness of the fine ground raw material is kept to be 10% after 80 mu m screen residue and below 1% after 200 mu m screen residue;
s3, preparation of clinker: stirring the finely ground raw material obtained in the step S2 with 1500g of water and a sintering aid, adding the mixture into a tabletting mold, using a TYE-300 type pressure testing machine to carry out load keeping for 10S with 11KN to obtain a test cake, placing the test cake into a drying oven at 80 ℃ for drying for 10h, placing the test cake into a SJF-1600 lifting furnace for calcination, setting the heating rate of a section at the temperature of 0-950 ℃ to be 10 ℃/min, preserving the heat at the temperature of 950 ℃ to 30min, setting the heating rate of a section at the temperature of 950-1300 ℃ to be 5 ℃/min, preserving the heat at the temperature of 1300 ℃ to be 10min, and ending the calcination; cooling the clinker to 30 ℃ to obtain clinker; the sintering aid is tetrasodium diphosphate, and the addition amount of the sintering aid is 0.5% of the mass of the finely ground raw material.
S4, preparation of cement: crushing and grinding the clinker prepared in the step S3, 20g of electric furnace slag, 30g of fly ash and dihydrate gypsum uniformly to obtain high-strength cement; the addition amount of the dihydrate gypsum is 2.5% of the clinker mass.
Example 2
A preparation method of high-strength cement comprises the following steps:
crushing of S1 raw materials: respectively crushing 20g of oil-based mud drill cuttings, 100g of limestone, 10g of copper slag, 5g of shale and 5g of red mud by using a jaw crusher, and uniformly mixing to obtain crushed raw materials, wherein the average size of the crushed raw materials is less than 1.5 mm;
grinding S2 raw materials: adding 7g of triglyceryl monolaurate into the crushed raw material prepared in the step S1 for fine grinding, and uniformly mixing to obtain fine ground raw material, wherein the fineness of the fine ground raw material is kept to be 10% after 80 mu m screen residue and below 1% after 200 mu m screen residue;
s3, preparation of clinker: stirring the finely ground raw material obtained in the step S2 with 1500g of water and a sintering aid, adding the mixture into a tabletting mold, using a TYE-300 type pressure testing machine to carry out load keeping for 10S with 11KN to obtain a test cake, placing the test cake into a drying oven at 80 ℃ for drying for 10h, placing the test cake into a SJF-1600 lifting furnace for calcination, setting the heating rate of a section at the temperature of 0-950 ℃ to be 10 ℃/min, preserving the heat at the temperature of 950 ℃ to 30min, setting the heating rate of a section at the temperature of 950-1300 ℃ to be 5 ℃/min, preserving the heat at the temperature of 1300 ℃ to be 10min, and ending the calcination; cooling the clinker to 30 ℃ to obtain clinker; the sintering aid is sodium lignin sulfonate, and the addition amount of the sintering aid is 0.5% of the mass of the finely ground raw material.
S4, preparation of cement: crushing and grinding the clinker prepared in the step S3, 20g of electric furnace slag, 30g of fly ash and dihydrate gypsum uniformly to obtain high-strength cement; the addition amount of the dihydrate gypsum is 2.5% of the clinker mass.
Example 3
A preparation method of high-strength cement comprises the following steps:
crushing of S1 raw materials: respectively crushing 20g of oil-based mud drill cuttings, 100g of limestone, 10g of copper slag, 5g of shale and 5g of red mud by using a jaw crusher, and uniformly mixing to obtain crushed raw materials, wherein the average size of the crushed raw materials is less than 1.5 mm;
grinding S2 raw materials: adding 7g of triglyceryl monolaurate into the crushed raw material prepared in the step S1 for fine grinding, and uniformly mixing to obtain fine ground raw material, wherein the fineness of the fine ground raw material is kept to be 10% after 80 mu m screen residue and below 1% after 200 mu m screen residue;
s3, preparation of clinker: stirring the finely ground raw material obtained in the step S2 with 1500g of water and a sintering aid, adding the mixture into a tabletting mold, using a TYE-300 type pressure testing machine to carry out load keeping for 10S with 11KN to obtain a test cake, placing the test cake into a drying oven at 80 ℃ for drying for 10h, placing the test cake into a SJF-1600 lifting furnace for calcination, setting the heating rate of a section at the temperature of 0-950 ℃ to be 10 ℃/min, preserving the heat at the temperature of 950 ℃ to 30min, setting the heating rate of a section at the temperature of 950-1300 ℃ to be 5 ℃/min, preserving the heat at the temperature of 1300 ℃ to be 10min, and ending the calcination; cooling the clinker to 30 ℃ to obtain clinker; the sintering aid is a mixture of tetrasodium diphosphate and sodium lignin sulfonate with a mass ratio of 2:3, and the addition amount of the sintering aid is 0.5% of the mass of the finely ground raw material.
S4, preparation of cement: crushing and grinding the clinker prepared in the step S3, 20g of electric furnace slag, 30g of fly ash and dihydrate gypsum uniformly to obtain high-strength cement; the addition amount of the dihydrate gypsum is 2.5% of the clinker mass.
Test example 1
Cement clinker free calcium oxide (f) CaO ) Is determined by: according to the glycol method in GB/T176-2008 "analysis of Cement chemical composition", the content of free calcium oxide in cement clinker samples prepared in comparative example 1 and examples 1-3 is determined by titration with a benzoic acid-absolute ethanol standard titration solution by a free calcium oxide determinator. The test results are shown in table 1:
table 1: determination of free calcium oxide of Cement clinker
Free calcium oxide (f) CaO ) Content (%)
Comparative example 1 1.96
Example 1 0.82
Example 2 0.78
Example 3 0.64
The content of free calcium oxide is an important index for measuring the quality of cement, and can directly influence the stability of cement clinker, so that the stability of cement is further influenced, and the content of the free calcium oxide in the cement clinker produced by a general vertical kiln is less than or equal to 1.0 percent and is qualified. From the above results, it can be seen that the cement clinker prepared by adding the sintering aid has stability within the acceptable range.
Example 4
A preparation method of high-strength cement comprises the following steps:
crushing of S1 raw materials: respectively crushing 20g of oil-based mud drill cuttings, 100g of limestone, 10g of copper slag, 5g of shale and 5g of red mud by using a jaw crusher, and uniformly mixing to obtain crushed raw materials, wherein the average size of the crushed raw materials is less than 1.5 mm;
grinding S2 raw materials: adding 7g of triglyceryl monolaurate into the crushed raw material prepared in the step S1 for fine grinding, and uniformly mixing to obtain fine ground raw material, wherein the fineness of the fine ground raw material is kept to be 10% after 80 mu m screen residue and below 1% after 200 mu m screen residue;
s3, preparation of clinker: stirring the finely ground raw material obtained in the step S2 with 1500g of water and a sintering aid, adding the mixture into a tabletting mold, using a TYE-300 type pressure testing machine to carry out load keeping for 10S with 11KN to obtain a test cake, placing the test cake into a drying oven at 80 ℃ for drying for 10h, placing the test cake into a SJF-1600 lifting furnace for calcination, setting the heating rate of a section at the temperature of 0-950 ℃ to be 10 ℃/min, preserving the heat at the temperature of 950 ℃ to 30min, setting the heating rate of a section at the temperature of 950-1300 ℃ to be 5 ℃/min, preserving the heat at the temperature of 1300 ℃ to be 10min, and ending the calcination; cooling the clinker to 30 ℃ to obtain clinker; the sintering aid is a mixture of tetrasodium diphosphate and sodium lignin sulfonate with a mass ratio of 2:3, and the addition amount of the sintering aid is 0.5% of the mass of the finely ground raw material.
S4, preparation of cement: crushing and grinding the clinker prepared in the step S3, 20g of electric furnace slag, 30g of fly ash, dihydrate gypsum and reinforcing agent uniformly to obtain high-strength cement; the addition amount of the dihydrate gypsum is 2.5% of the clinker mass; the reinforcing agent is stachyose, and the addition amount of the reinforcing agent is 0.03% of the mass of clinker.
Example 5
A preparation method of high-strength cement comprises the following steps:
crushing of S1 raw materials: respectively crushing 20g of oil-based mud drill cuttings, 100g of limestone, 10g of copper slag, 5g of shale and 5g of red mud by using a jaw crusher, and uniformly mixing to obtain crushed raw materials, wherein the average size of the crushed raw materials is less than 1.5 mm;
grinding S2 raw materials: adding 7g of triglyceryl monolaurate into the crushed raw material prepared in the step S1 for fine grinding, and uniformly mixing to obtain fine ground raw material, wherein the fineness of the fine ground raw material is kept to be 10% after 80 mu m screen residue and below 1% after 200 mu m screen residue;
s3, preparation of clinker: stirring the finely ground raw material obtained in the step S2 with 1500g of water and a sintering aid, adding the mixture into a tabletting mold, using a TYE-300 type pressure testing machine to carry out load keeping for 10S with 11KN to obtain a test cake, placing the test cake into a drying oven at 80 ℃ for drying for 10h, placing the test cake into a SJF-1600 lifting furnace for calcination, setting the heating rate of a section at the temperature of 0-950 ℃ to be 10 ℃/min, preserving the heat at the temperature of 950 ℃ to 30min, setting the heating rate of a section at the temperature of 950-1300 ℃ to be 5 ℃/min, preserving the heat at the temperature of 1300 ℃ to be 10min, and ending the calcination; cooling the clinker to 30 ℃ to obtain clinker; the sintering aid is a mixture of tetrasodium diphosphate and sodium lignin sulfonate with a mass ratio of 2:3, and the addition amount of the sintering aid is 0.5% of the mass of the finely ground raw material.
S4, preparation of cement: crushing and grinding the clinker prepared in the step S3, 20g of electric furnace slag, 30g of fly ash, dihydrate gypsum and reinforcing agent uniformly to obtain high-strength cement; the addition amount of the dihydrate gypsum is 2.5% of the clinker mass; the reinforcing agent is triethylamine, and the addition amount of the reinforcing agent is 0.03% of the clinker mass.
Example 6
A preparation method of high-strength cement comprises the following steps:
crushing of S1 raw materials: respectively crushing 20g of oil-based mud drill cuttings, 100g of limestone, 10g of copper slag, 5g of shale and 5g of red mud by using a jaw crusher, and uniformly mixing to obtain crushed raw materials, wherein the average size of the crushed raw materials is less than 1.5 mm;
grinding S2 raw materials: adding 7g of triglyceryl monolaurate into the crushed raw material prepared in the step S1 for fine grinding, and uniformly mixing to obtain fine ground raw material, wherein the fineness of the fine ground raw material is kept to be 10% after 80 mu m screen residue and below 1% after 200 mu m screen residue;
s3, preparation of clinker: stirring the finely ground raw material obtained in the step S2 with 1500g of water and a sintering aid, adding the mixture into a tabletting mold, using a TYE-300 type pressure testing machine to carry out load keeping for 10S with 11KN to obtain a test cake, placing the test cake into a drying oven at 80 ℃ for drying for 10h, placing the test cake into a SJF-1600 lifting furnace for calcination, setting the heating rate of a section at the temperature of 0-950 ℃ to be 10 ℃/min, preserving the heat at the temperature of 950 ℃ to 30min, setting the heating rate of a section at the temperature of 950-1300 ℃ to be 5 ℃/min, preserving the heat at the temperature of 1300 ℃ to be 10min, and ending the calcination; cooling the clinker to 30 ℃ to obtain clinker; the sintering aid is a mixture of tetrasodium diphosphate and sodium lignin sulfonate with a mass ratio of 2:3, and the addition amount is 0.5% of the mass of the finely ground raw material;
s4, preparation of cement: crushing and grinding the clinker prepared in the step S3, 20g of electric furnace slag, 30g of fly ash, dihydrate gypsum and reinforcing agent uniformly to obtain high-strength cement; the addition amount of the dihydrate gypsum is 2.5% of the clinker mass; the mass ratio of the reinforcing agent is 1: 2. the addition amount of the mixture of stachyose and triethylamine is 0.03 percent of the mass of clinker.
Example 7
A preparation method of high-strength cement comprises the following steps:
crushing of S1 raw materials: respectively crushing 20g of oil-based mud drill cuttings, 100g of limestone, 10g of copper slag, 5g of shale and 5g of red mud by using a jaw crusher, and uniformly mixing to obtain crushed raw materials, wherein the average size of the crushed raw materials is less than 1.5 mm;
grinding S2 raw materials: adding 7g of triglyceryl monolaurate into the crushed raw material prepared in the step S1 for fine grinding, and uniformly mixing to obtain fine ground raw material, wherein the fineness of the fine ground raw material is kept to be 10% after 80 mu m screen residue and below 1% after 200 mu m screen residue;
s3, preparation of clinker: stirring the finely ground raw material obtained in the step S2 with 1500g of water and a sintering aid, adding the mixture into a tabletting mold, using a TYE-300 type pressure testing machine to carry out load keeping for 10S with 11KN to obtain a test cake, placing the test cake into a drying oven at 80 ℃ for drying for 10h, placing the test cake into a SJF-1600 lifting furnace for calcination, setting the heating rate of a section at the temperature of 0-950 ℃ to be 10 ℃/min, preserving the heat at the temperature of 950 ℃ to 30min, setting the heating rate of a section at the temperature of 950-1300 ℃ to be 5 ℃/min, preserving the heat at the temperature of 1300 ℃ to be 10min, and ending the calcination; cooling the clinker to 30 ℃ to obtain clinker; the sintering aid is a mixture of tetrasodium diphosphate and sodium lignin sulfonate with a mass ratio of 2:3, and the addition amount is 0.5% of the mass of the finely ground raw material;
s4, preparation of cement: crushing and grinding the clinker prepared in the step S3, 20g of furnace slag, 30g of fly ash, 3g of magnesium triflate, dihydrate gypsum and reinforcing agent, and uniformly mixing to obtain environment-friendly high-strength cement; the addition amount of the dihydrate gypsum is 2.5% of the clinker mass; the mass ratio of the reinforcing agent is 1:2, and the addition amount of the mixture of stachyose and triethylamine is 0.03 percent of the mass of clinker.
Test example 2
Cement strength test: the preparation of the cement mortar is carried out according to the national standard GB/T17671-1999 'cement mortar strength test', the cement mortar molding is carried out according to the GB/T175-2007 'general Portland Cement', one part of cement and three parts of Chinese ISO standard sand are proportioned according to the water cement ratio of 0.5, after molding for 24 hours, the mold is removed, the mold is put into water with the temperature of 20+/-1 ℃ for curing, and the 3d and 28d flexural strength and the compressive strength of the mold are measured. The test results are shown in table 2:
table 2: strength of cement mortar
Figure BDA0003468803830000141
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Figure BDA0003468803830000151
The use of high strength grade cement to prepare high grade concrete in engineering is beneficial to reducing cost and improving durability of concrete, and as can be seen from the data in Table 2, the strength of cement prepared by adding the reinforcing agent can reach the strength requirement of silicate cement with 62.5 strength grade. The possible reasons are that the reinforcing agent improves the dispersibility of the cement and accelerates the penetration of water inside the cement particles, promoting C 3 S, the particle distribution of cement is changed, and meanwhile, the hydration speed of cement is delayed, so that the distribution of hydration products such as C-S-H of solution around cement particles is more uniform, the grid structure is more compact, and finally, the internal structure of cement is more compact, thereby improving the strength of cement.
Test example 3
And (3) measuring the water reducing rate of the rubber sand:
the preparation of the cement sand is carried out according to the national standard GB/T17671-1999 cement mortar strength test, and the cement sand water reduction rate test is measured by referring to the adaptability detection method of the concrete admixture specified in the concrete admixture homogeneity test method of GB/T8077-2012. Firstly, measuring the water consumption of the reference sand fluidity, then measuring the water consumption of the additive-doped sand fluidity, and calculating to obtain the sand water reduction rate.
The cement mortar water reduction rate (%) is calculated according to the following formula:
cement mortar water reduction rate= (M0-M1)/m0×100
Wherein:
m0 is water consumption in grams (g) when the standard sand fluidity is (180+/-5) mm;
m1-water consumption in grams (g) when the cement sand fluidity of the sample cement is (180+/-5) mm;
the test results of the test pieces are shown in Table 3.
Table 3: water reduction rate of cement mortar
Experimental protocol Rubber sand water reduction rate (%)
Comparative example 1 13
Example 1 15
Example 2 17
Example 3 18
Example 4 20
Example 5 21
Example 6 22
Example 7 25
It can be seen from Table 3 that the water reducing effect of example 7 is best, probably due to electrostatic repulsion and steric hindrance effects that magnesium triflate can cause. The electrostatic repulsion is due to the fact that the-COO and-SO 3 anions in the gum sand are attached to the cations (Ca 2+ ) And (5) adsorption. A large amount of anions are accumulated on the surface of the cement particles. The strong electrostatic repulsion between these anions repels the cement particles from each other. This breaks down the flocculation structure of the cement, leading toSo that free water is released from the cement. Further steric hindrance is due on the one hand to the fact that stachyose and triethylamine form a polymer molecular adsorption layer on the surface of the cement particles. With the increase of the polymer molecular content, the adsorption layer becomes thicker, plays a role in supporting and dispersing, and prevents the formation of a cement flocculation structure. On the other hand, after the water reducer is added into the cement, part of the water reducer is wrapped by the cement hydration product to form a composite layer. The higher negative charge density of magnesium triflate makes it easier to enter the composite layer, thereby reducing the required water reducing agent content. Therefore, the existence of the magnesium triflate increases electrostatic repulsive force and steric hindrance effect between cements, improves the water reducing rate of the sample cement, and improves the adhesiveness of concrete.

Claims (7)

1. The preparation method of the high-strength cement is characterized by comprising the following steps of:
crushing of S1 raw materials: weighing 10-30 parts of oil-based mud drill cuttings, 80-100 parts of limestone, 10-20 parts of copper slag, 1-5 parts of shale and 1-5 parts of red mud, respectively crushing and uniformly mixing to obtain crushed raw materials;
grinding S2 raw materials: adding grinding aid into the crushed raw material prepared in the step S1 for fine grinding, and uniformly mixing to obtain fine ground raw material;
s3, preparation of clinker: uniformly stirring the finely ground raw material obtained in the step S2 with water and a sintering aid, pressing into a test cake, drying the test cake, calcining, and cooling to obtain clinker;
s4, preparation of cement: crushing and grinding the clinker prepared in the step S3, 20-40 parts of furnace slag, 20-40 parts of fly ash, 1-5 parts of magnesium triflate, dihydrate gypsum and reinforcing agent, and uniformly mixing to obtain high-strength cement;
the sintering aid is a mixture of tetrasodium diphosphate and sodium lignin sulfonate, and the mass ratio of the tetrasodium diphosphate to the sodium lignin sulfonate is 2-3:3-5;
the reinforcing agent is a mixture of stachyose and triethylamine in a mass ratio of 1:2-3.
2. A method of preparing a high strength cement according to claim 1, wherein: the grinding aid is one or two or more than two of triglycerol monolaurate, triglycerol monolaurate and N, N-dimethylformamide.
3. A method of preparing a high strength cement according to claim 1, wherein: the addition amount of the grinding aid is 0.03-1% of the mass of the crushed raw material.
4. A method of preparing a high strength cement according to claim 1, wherein: the addition amount of the sintering aid is 0.1-0.5% of the mass of the finely ground raw material.
5. A method of preparing a high strength cement according to claim 1, wherein: the mass of the dihydrate gypsum in the step S4 is 2-5% of the mass of the clinker.
6. A method of preparing a high strength cement according to claim 1, wherein: the addition amount of the reinforcing agent is 0.01-0.05% of the clinker mass.
7. A high strength cement prepared by the method of preparing a high strength cement according to any one of claims 1 to 6.
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