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INVENTION
Patent of the Russian Federation RU2160723

METHOD OF PREPARING A COMPLEX MODIFICANT OF CONCRETE
AND INTEGRATED CONCRETE MODIFIER

The name of the inventor: Caprielov SS; Sheynfeld AV; Zhigulev N.F.
The name of the patent holder: OOO "Master Master Concrete"
Address for correspondence: 109428, Moscow, ul. 2-ya Institutskaya, 6, KTB NIIZhB, OOO "Enterprise Master Beaton", Caprielov SS.
Date of commencement of the patent: 1998.11.25

The invention relates to methods for preparing complex modifiers of concrete and to formulations of complex modifiers.

The technical task is to develop such a method for preparing a complex modifier and its compositions, in which the technological process (in particular, the drying operation of the slurry) would be shortened, the resulting modifier would have an increased plasticizing ability, and the concrete mixtures prepared using the resulting modifier would allow Get high strength concrete. A method for preparing a complex modifier of concrete comprising mixing a particulate silica-containing particulate mineral component with a chemical additive followed by drying and granulating the resulting mixture in a gas-air stream, the gas-cleaning products of furnaces melting crystalline silicon and / or silicon-containing alloys and / Coal, and / or rock; As a chemical additive, products based on organic acid salts are used, and natural gas combustion products and / or gases coming from furnaces melting silicon-containing alloys or coal-burning coal and using solid particles in an amount of no more than 2.5 G / n · m ³ , with the following ratio of the components of the resulting modifier, by weight : silica-containing particulate mineral component - 51.9 - 94.1 ; Chemical additive - 4,7 - 45,5 ; Water - the rest. In this case, the products of dry gas cleaning of furnaces melting crystalline silicon and / or ferrosilicon and / or ferrosilicochrome or silicocalcium and / or fly ash and / or kaolin are used as the dispersed mineral component. As a chemical additive, a plasticizer based on a polycondensate salt -naphthalenesulfonic acid and formaldehyde and / or a mixture thereof with nitro nitrophenylphosphonic acid and / or a complex nitrilotrimethylphosphonic acid salt and / or oxyethylenediphosphonic acid and / or disodium salt of ethylenediaminetetraacetic acid and / or a lignosulfonic acid salt plasticizer. In the complex modifier obtained from the initial mixture comprising a silica containing in an amount of not less than 50.7% by weight, the dispersed mineral component, the chemical additive and the water, dried and granulated in the gas-air flow, is solved in that a particulate mineral component is used The gas cleaning products of furnaces melting silicon-containing alloys and / or burning coal and / or rock, or a mixture of at least one of the above components with the gas cleaning product of furnaces melting ferrosilicon, and as a chemical additive it contains products based on Salts of organic acids with the following ratio of components, mass. % : Silica-containing particulate mineral component - 51.9-94.1 ; Chemical additive - 4,7-45,5 ; Water - the rest. In this case, as a particulate mineral component, it contains the products of dry gas cleaning of furnaces melting crystalline silicon and / or silicocalcium and / or ferrosilicochrome and / or fly ash and / or kaolin.

DESCRIPTION OF THE INVENTION

The invention relates to methods for preparing complex modifiers of concrete (complex additives) and to formulations of modifiers.

A method for the preparation of a complex modifier of concrete (complex additive) is known , which includes stirring microsilica ( 40-70 wt% ), a superplasticizer ( 4-9.5 wt% ) of nitrilotrimethylphosphoric acid ( 0.01-0.4 wt% ) and water (The remainder) to form a slurry, which is further dried in an air stream at 160-300 ^° C. , adjusting the moisture content of the product to 1-8% (RU, 2096389, 1997 ).

The closest to the technical essence and the achieved result is the method for preparing a complex modifier and a complex modifier comprising mixing microsilica (25-70 % by weight ) with a chemical additive ( 2-10% by weight ) and water (remaining) to obtain a suspension which undergoes Drying in a gas-air stream with a temperature of 120-270 ^° C at a flow rate of 3.0-15.0 m ³ / s . As a chemical additive, the method uses a plasticizer and / or its mixtures with a hardening regulator, air entraining, antifreeze additives. A product consisting of microsilica ( 77.2-94.0% by weight ), a chemical additive ( 4.7-15.7% by weight ) and water (the rest) is obtained ( RU, 2096372, 1997 ).

The drawback of the method is the duration and, correspondingly, the energy intensity of the drying process of the slurry from the moment it is fed to the drying unit to the final product and the resulting complex modifier has a relatively low plasticizing capacity.

The technical task is to develop such a method for preparing a complex modifier of concrete and its composition, in which the drying process of the slurry would be reduced, the resulting modifier would have an increased plasticizing ability, and the concrete mixtures prepared using the resulting modifier would produce higher strength concretes.

This object is achieved in such a manner that in the process for preparing a complex modifier of concrete comprising mixing the particulate silica-containing particulate mineral component with a chemical additive followed by drying and granulating the resulting mixture in a gas-air stream, the gas-cleaning products of furnaces melting crystalline silicon, And / or silicon-containing alloys and / or coal-burning and / or rock-bearing, organic acid-based products are used as a chemical additive, and natural gas combustion products and / or gases from furnaces are used as the gas-air stream, Melting of silicon-containing alloys or burning coal, and containing solid particles in an amount of not more than 2.5 g / n · m ³ , (hereinafter the concentration of particles in gases is given at normal temperature ( 20 ^° C ); G / n · m ³ ) with the following ratio of the components of the obtained modifier, mass% :

• The silica-containing particulate mineral component is 51.9 to 94.1
• The chemical additive - 4,7 - 45,5
• Water - Other

In this case, the products of dry gas cleaning of furnaces melting crystalline silicon and / or ferrosilicon and / or ferrosilicochrome and / or silococals and / or fly ash and / or kaolin are used as the dispersed mineral component.

As a chemical additive, a plasticizer based on a polycondensate salt Naphthalenesulfonic acid and formaldehyde and / or a mixture thereof with nitrilotrimethylphosphonic acid and / or a nitrilotrimethylphosphonic acid complex salt and / or oxyethylidenediphosphonic acid and / or disodium salt of ethylenediaminetetraacetic acid and / or a lignosulfonic acid salt plasticizer.

The task in view of the composition of the complex modifier obtained from the initial mixture comprising a silica-containing dispersed mineral component, a chemical additive and water is solved by the fact that as a particulate mineral component containing silica in an amount of not less than 50.7 wt. % , Use the gas cleaning products of ovens melting crystalline silicon and / or ferrosilicochrome and / or silicocalciums and / or burning coal and / or rock or a mixture of at least one of the above components with the gas cleaning product of furnaces smelting ferrosilicon, and As a chemical additive, it contains products based on salts of organic acids with the following ratio of components, mass% :

• The silica-containing particulate mineral component is 51.9 to 94.1
• The chemical additive - 4,7 - 45,5
• Water - Other

As a chemical additive, the modifier comprises a plasticizer based on a polycondensate salt Naphthalenesulfonic acid and formaldehyde and / or a mixture thereof with nitrilotrimethylphosphonic acid and / or a nitrilotrimethylphosphonic acid complex salt and / or oxyethylidenediphosphonic acid and / or disodium salt of ethylenediaminetetraacetic acid and / or a lignosulfonic acid salt plasticizer.

Complex modifier of concrete, including the product of gas cleaning of furnaces melting silicon-containing alloy-ferrosilicon, chemical additive based on salts of organic acids and water, characterized in that it contains components at the following ratio, by weight :

• The said product for gas cleaning of furnaces is 51.9 - 77.2
• Chemical additive - 15,8 - 45,5
• Water - Other

The complex modifier contains a plasticizer based on a polycondensate salt -naphthalenesulfonic acid and formaldehyde and / or lignosulfonic acid-based plasticizer, or a mixture of at least one of said plasticizers with nitrilotrimethylphosphonic acid and / or a nitrilotrimethylphosphoric acid complex salt and / or oxyethylidenediphosphonic acid and / or disodium salt of ethylenediaminetetraacetic acid .

A complex modifier of concrete comprising a silica-containing particulate mineral component, a chemical additive and water, characterized in that said dispersed mineral component contains at least 50.7% silica and is a product of gas cleaning of furnaces smelting ferrosilicon, and as a chemical additive It contains a mixture of a salt-based plasticizer Naphthalenesulfonic acid and formaldehyde and / or lignosulfonic acid-based plasticizer with a nitrilotrimethylphosphonic acid complex salt and / or oxyethylidene diphosphonic acid and / or disodium salt of ethylenediaminetetraacetic acid with the following component ratio, by weight :

• A dispersion component containing silica in an amount of at least 50.7% is 51.9 to 94.1
• The chemical additive - 4,7 - 15,7
• Water - Other

The invention reduces drying of the suspension and granulation.

This is achieved through two factors:

• Use as a mineral component of both ultradispersed and coarse-dispersed materials of technogenic origin (dust of gas cleaning of furnaces melting silicon-containing alloys and fly ash) and treated rock (kaolin), and as a chemical additive - a complex of salts of organic acids,
• The use of flue gases (combustion products in natural gas furnaces) and gases emitted from furnaces containing solid particles as a gas-air stream.

The first factor allows, without increasing the viscosity of the suspension, to increase its concentration due to the less water-consuming pipe-spreading component or chemical additive, the second intensifies the drying and granulation process due to the presence of heated pulverous particles in the gaseous coolant.

Since the mineral component of the modifier consists of ultradisperse (particle sizes less than 1 μm) and coarsely dispersed (particle size 1-200 μm ) materials, one can expect it to be of less water demand. At a certain ratio between the mineral component and the chemical additive, this should contribute to an increase in the plasticizing capacity of the modifier in comparison with the prototype, which will also result in less water demand for concrete mixes and in increased strength of concrete, respectively. The presence of a polycondensate salt modifier in the composition -naphthalenesulfonic acid and formaldehyde, and lignosulfonate is intended to provide the plasticization of the cement system, and the organophosphorus compounds and the disodium salt of ethylenediaminetetraacetic acid to stabilize the suspension from the mineral component at the stage of preparation of the modifier, as well as for the long-term preservation of the consistency of the concrete mixtures in the concrete preparation stage. These effects on cement systems are greatly enhanced, because In the composition of the modifier, the balance between the mineral and organic components has been changed in the direction of increasing the latter.

Thus, the proposed method of preparation of the complex modifier, its composition, and the concrete mix allow to solve the task and meet the criteria "novelty" and "inventive level".

The method for preparing the complex modifier is carried out in the sequence that is set forth below.

The mixer is loaded with water, chemical additives, pulverized furnace gas cleaning products, in which crystalline silicon, ferrosilicon, ferrosilicochrome, fly ash and enriched kaolin are melted, which are mixed until a fluid and homogeneous suspension is obtained. The resulting slurry is fed to a drying unit in which it is dried and granulated. As a drying agent, combustion products are used in the furnaces of natural gas - flue gases or gases from furnaces melting ferroalloys or burning coal. The concentration of pulverized solid particles in gases leaving from furnaces melting ferroalloys and burning coal is 2.5 g / n · m ³ .

Example
Materials used for the preparation of the complex modifier, the characteristics of which are given below.

1. As mineral components:

   • Particles of spherical shape that are waste products of the production of silicon-containing alloys - products of dry gas cleaning of furnaces in which crystalline silicon ( Kp ) and ferroalloys are melted: low-percentage ferrosilicon ( FS ), ferrosilicochrom ( FSX) and silicocalcium ( UK ),

   • Fly ash, consisting of particles of spherical shape with a size of 1-200 microns , corresponding to GOST 25818-91 "Fly ash of thermal power plants for concrete,"

   • Kaolin, which is a dispersed material, corresponding to GOST 19607-74 "Kaolin enriched for the chemical industry".

   • A common feature of the listed materials is the predominance in their composition of silicon dioxide of an amorphous modification, the content of which is not less than 50.7% by weight ( see Table 1 ).

2. As chemical additives:

   • Superplasticizer brand C-3 based on the sodium salt of the condensation product -naphthalenesulfonic acid and formaldehyde, corresponding to TU 6-36-0204229-625-90 "Plasticiser C-3 ." Specifications. "

   • Technical lignosulfonate (LST) , which is the sodium salt of lignosulfonic acid with impurities corresponding to TU 13-0281036-029-94 "Technical lignosulfonate. Technical specifications".

   • Nitrilotrimethylphosphonic acid ( NTP ), N ( CH2PO3H2 ) ₃ , corresponding to TU 6-095283-83 "Nitrilotrimethylphosphonic acid is pure." Specifications. "

   • Oxyethylidenediphosphonic acid (OEDP), CH ₃ C (OH) (PO ₃ H ₂ ) ₂ , corresponding to TU 6-09-5372-87 "1-hydroxyethylidenediphosphonic acid MA (OEDP-MA) is pure." Specifications . "

   • Disodium salt of ethylenediaminetetraacetic acid (Trilon B), C ₁₀ H ₁₄ Na ₂ O ₈ · 2H ₂ O , corresponding to GOST 10652-73 "Ethylenediamine - N, N.N ', N' , - tetraacetic acid disodium salt, 2 - aqueous Disodium ethylenediamine salt - N, N, N ', N', tetraacetic acid, Trilon B) .

   • Complex salt (AMFO) consisting of a mixture of the ammonium salt of nitrilotrimethylphosphonic acid (95%), N (CH ₂ PO ₃ ) ₃ H ₃ (NH ₄ ) ₃ , corresponding to TU 6-09-20-195-91 "Amifol . ", And oxyethylidenediphosphonic acid - OEDP (5%) .

From the above materials in a high-speed mixer, aqueous suspensions were prepared which were fed to a drying unit. The ratio between the mineral components of the suspension and the chemical additive ranged from 51.9: 45.5 to 94.1: 4.7 .

Suspensions were sprayed with nozzles and subjected to drying by a counter-gas-air flow acting as a drying agent. Three types of drying agent were used: flue gases (TG) - combustion products in natural gas furnaces, at a temperature of 120-270 ^o C and a flow rate of 2.5-8.0 m ³ / s , gases emanating from furnaces melting silicon-containing alloys (KG) , the concentration of dust particles is 0.1-2.0 g / n · m ³ , temperature 140-180 ^° C with a flow rate of 4.0-15.0 m ³ / s , gases emanating from the furnaces of thermal power plants, In which coal (UG) is burnt , the concentration of particles is 0.4-2.5 g / N · m ³ , temperature 120-170 ^° C with a flow rate of 8.0-15.0 m ³ / s .

The suspension was dried in a 35 m ^{3 unit} with an inert carrier. The duration of drying was predetermined by the need to ensure the moisture content of the finished product within the range of 0-5% . Samples of the prototype modifier were prepared by the same method, using as a mineral component microsilica to which Kp sample corresponds, as a chemical additive - a mixture of C-3 and NTP , as a drying agent - flue gas (TG) .

The characteristics of the obtained modifier samples with the parameters of their preparation technology are given in Table. 2 , from which it follows that the proposed method allows to reduce the drying time in comparison with the prototype by 27-52% . Reduction of the drying time, as noted above, is associated with a complex effect of a number of factors: using as a drying agent particles containing heated dust particles (leaving from furnaces smelting ferroalloys and burning coal), using as fly ash, kaolin, dust-like as a mineral component Wastes of production of silicon-containing alloys and their mixtures, as well as using plasticizers in combination with complexones (NTF, OEDF, AMFO, Trilon B) as chemical additives.

With the use of the obtained modifier samples (with the exception of samples N 5 and N 22 , which do not solve the set task in terms of reducing the drying time), concrete mixtures were prepared. As a binder used portland cement M500 D5 (GOST 10178) , as fillers - quartz sand with M _cr = 2.0 (GOST 8736) and granite rubble fr. 5-20 mm (GOST 8267) . The proportion of sand in the aggregate mixture Was 0.37-0.40 . The mobility of concrete mixtures was estimated by the cone draft in accordance with GOST 10181.1 , and the strength of concrete at the age of 28 days. Normal storage - according to the results of testing samples-cubes 10x10x10 cm according to GOST 10180 . The characteristics of the resulting concrete, depending on the composition of the modifiers and their dosages, are given in Table. 3 .

From the information presented in it, it follows that the concrete mixtures prepared using the modifier obtained by the proposed method differ by an increased mobility of 28-33% (compare samples NN 1 and 6 , a and NN 2 and 8 ), and the concretes are increased by 15-22% strength with a similar prototype mobility and composition of the concrete mixture (compare samples NN 1 and 7 , a and NN 2 and 9 ).

Summarizing the data presented in Table. 2 and tab. 3 materials, we can draw the following conclusions:

- the proposed method of preparation of the modifier makes it possible to obtain a high-quality product with a shorter duration of the technological process than in the prototype,

- complex modifier, obtained by the proposed method, allows to produce more plastic concrete mixtures and high strength concrete.

CLAIM

1. A process for the preparation of a complex modifier of concrete, comprising mixing a particulate silica-containing particulate mineral component with a chemical additive and water, followed by drying and granulating the resulting mixture in a gas-air flow, characterized in that the particulate mineral component is used for the gas cleaning products of furnaces melting crystalline silicon and / or Silicon-containing alloys and / or coal-burning and / or rock-burning coal, organic acid-based products are used as a chemical additive, and natural gas combustion products and / or gases from furnaces melting silicon-containing alloys or burning Coal, and containing solid particles in an amount of not more than 2.5 g / n · m ³ , with the following ratio of the components of the resulting modifier, :

   • The silica-containing particulate mineral component is 51.9 to 94.1

   • The chemical additive - 4,7 - 45,5

   • Water - Other

2. A method of preparing a complex modifier according to claim 1, characterized in that a plasticizer based on a polycondensate salt is used as a chemical additive Naphthalenesulfonic acid and formaldehyde, and / or a mixture thereof with nitrilotrimethylphosphonic acid and / or a complex salt of nitrilotrimethylphosphonic acid and / or oxyethylidenediphosphonic acid and / or disodium salt of ethylenediaminetetraacetic acid and / or a lignosulfonic acid salt plasticizer.

3. A complex modifier of concrete comprising a silica-containing dispersed mineral component, a chemical additive and water, characterized in that said particulate mineral component comprises at least 50.7% by weight of silica and is a rock and / or a gas cleaning product of furnaces melting Crystalline silicon and / or ferrosilicochrome and / or silicocalcium and / or coal burners, or a mixture of at least one of the above components with the gas cleaning product of furnaces smelting ferrosilicon and, as a chemical additive, it contains salt-based products Organic acids with the following ratio of comonents, mass% :

   • A dispersion component containing silica in an amount of not less than 50.7% by weight is 51.9 to 94.1%

   • The chemical additive - 4,7 - 45,5

   • Water - Other

4. A complex modifier according to claim 3, characterized in that, as salts of organic acids, it contains a plasticizer based on a polycondensate salt Naphthalenesulfonic acid and formaldehyde and / or a lignosulfonic acid salt plasticizer or a mixture of at least one of the said nitrilotrimethylphosphonic acid plasticizers and / or nitrilotrimethylphosphonic acid complex salt and / or oxyethylidenediphosphonic acid and / or disodium salt Ethylenediaminetetraacetic acid.

5. Complex modifier of concrete, including the product of gas cleaning of furnaces melting silicon-containing alloy-ferrosilicon, chemical additive based on salts of organic acids and water, characterized in that it contains components at the following ratio, mass% :

   • The said product for gas cleaning of furnaces is 51.9 - 77.2

   • Chemical additive - 15,8 - 45,5

   • Water - Other

6. Комплексный модификатор по п.5, отличающийся тем, что в качестве солей органических кислот он содержит пластификатор на основе соли поликонденсата - нафталинсульфокислоты и формальдегида и/или пластификатор на основе соли лигносульфоновой кислоты или смесь, по крайней мере, одного из указанных пластификаторов с нитрилотриметилфосфоновой кислотой, и/или с комплексной солью нитрилотриметилфосфоновой кислоты, и/или с оксиэтилидендифосфоновой кислотой, и/или с динатриевой солью этилендиаминтетрауксусной кислоты.

7. Комплексный модификатор бетона, включающий содержащий диоксид кремния дисперсный минеральный компонент, химическую добавку и воду, отличающийся тем, что указанный дисперсный минеральный компонент содержит диоксид кремния в количестве не менее 50,7% и является продуктом газоочистки печей, выплавляющих ферросилиций, а в качестве химической добавки он содержит смесь пластификатора на основе соли -нафталинсульфокислоты и формальдегида и/или пластификатора на основе соли лигносульфоновой кислоты с комплексной солью нитрилотриметилфосфоновой кислоты, и/или с оксиэтилидендифосфорной кислотой, и/или с динатриевой солью этилендиаминтетрауксусной кислоты при следующем соотношении компонентов, мас.% :

   • Дисперсный компонент, содержащий диоксид кремния в количестве не менее 50,7% - 51,9 - 94,1

   • Химическая добавка - 4,7 - 15,7

   • Вода - Остальноеи

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Дата публикации 25.11.2006гг

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