INVENTION
Patent of the Russian Federation RU2144552
A METHOD FOR PRODUCING SILICATE GLUE BOND

A METHOD FOR PRODUCING SILICATE ADHESIVE-BINDING. GLUE. KNOW HOW. INTRODUCTION. PATENT. TECHNOLOGIES.

INVENTION. A METHOD FOR PRODUCING SILICATE ADHESIVE-BINDING. Patent of the Russian Federation RU2144552

Applicant's name: Institute of Theoretical and Applied Mechanics SB RAS; Institute of Solid State Chemistry and Mineral Processing; Cherepanov Korniliy Alexandrovich
The name of the inventor: Cherepanov K.A .; Poluboyarov VA; Ushakova EP; Cherepanov A.N .; Cherepanov V.K.
The name of the patent holder: Institute of Theoretical and Applied Mechanics SB RAS; Institute of Solid State Chemistry and Mineral Processing; Cherepanov Korniliy Alexandrovich
Address for correspondence: 630128, Novosibirsk, Kutateladze St., 18, IHTST and MS of the SB RAS, Ushakova EP
Date of commencement of the patent: 1998.04.08

A method for the production of a silicate adhesive-binder is described, comprising the following: a silicon-containing amorphous material is subjected to a mechanochemical treatment in a 10-17% by weight solution of caustic soda at T: H = 1 :( 2.5-3.5) in a ball mill at a temperature of 25-50 ° C and atmospheric pressure for 4-8 hours . The method makes it possible to efficiently use the many-tonnage dust-like waste of ferrosilicon production - amorphous micro-silica and to obtain a silicate adhesive-adhesive used in chemical and other industries for the production of acid-resistant coatings, putties, mastics, in metallurgy and heat power engineering - in obtaining heat-resistant (dense and porous ) Of materials, in the construction industry - for gluing concrete products, bricks, natural stone, all sorts of finishing materials.

DESCRIPTION OF THE INVENTION

The invention relates to methods for producing silicate adhesives used in household chemicals, the building industry for bonding concrete products, bricks, natural stone, marble slabs, and for making putties, mastics, putties, heat-resistant and porous heat-insulating materials. It allows the efficient use of large-tonnage pulverized wastes of ferrosilicon production - amorphous microsilica.

A method for producing a glue-solution of the liquid sodium glass type is known, which includes treating silicon-containing wastes of ferrosilicon production with a solution of sodium hydroxide at a temperature of 20 ° -80 ° C. However, liquid glass is a true solution of inorganic polymer ( Na 2 SiO 3 ), which is an adhesive, but has relatively low adhesive properties and, in order to accelerate the curing process, requires a special curing agent ( RU 2044838, 20.11.92 ).

The inorganic adhesive bond of the type proposed occupies an intermediate position between the true solutions and the colloidal solutions. To a greater extent, it approaches colloidal, due to the presence in it of a certain amount of dispersed phase released into the solution during the process of condensation (polymerization) of a part of the solute in the form of a sol of SiO 2 .

Silicate bonding adhesives are usually obtained by modifying the liquid glass by introducing into it the sol-forming and stabilizing additives, as well as in the stage of obtaining the adhesive bond with the process of dissolving the silicon-containing materials ( MMSychev, Inorganic Adhesives, L., Chemistry, 99 ) .

For example, a method for activating a liquid glass is known, comprising the addition of an activating additive, which uses a sulfuric acid solution with a density of 1.14-1.15 g / cm2 , followed by stirring until the resulting gel of silicic acid is completely dissolved ( RU 2041178, August 9, 1995 ) .

The disadvantage of this method is that it is three-stage, since first you need to get a silicate-block, then a liquid glass, and then make its modification.

The closest technical solution chosen for the prototype is the method for producing the silicate bond adhesive by digesting the silicate block in an autoclave in the presence of highly disperse silica, the latter being introduced in an amount of 0.95 to 2.0 wt. H by 100 parts by weight. Silicate-clumps ( SU 331080, 07.09.72 ).

The known method has a number of disadvantages. Firstly, it is two-stage, since it requires the preliminary production of silicate-clod, and secondly, it is complex, requires high pressures, temperatures, and high power consumption.

The purpose of the invention is to simplify the process for producing adhesive binder, while reducing labor and energy costs, and to improve the performance characteristics of the product obtained.

The aim is achieved by the fact that silica containing an amorphous material is subjected to mechanochemical treatment in a 10-17% solution of sodium hydroxide in a ball mill at a ratio T: H = 1 :( 2.0-3.5) , where T is the amount of amorphous silica-containing material being loaded, M is the sodium hydroxide solution of the above concentrations, at a temperature of 25-50 ° C and atmospheric pressure for 4-10 hours .

As a silica-containing amorphous material, dusty wastes of ferrosilicon production are used.

Essential distinctive features of the claimed technical solution are:

  • Silica-containing amorphous material is subjected to mechanochemical treatment in 10 - 17% by weight. Solution of sodium hydroxide in a ball mill;
  • Mechanochemical activation is carried out at a ratio of T: H = (2.0 - 3.5) ;
  • Mechanochemical treatment is carried out at a temperature of 25 ° -50 ° C. and atmospheric pressure for 4-10 hours .

A particular distinguishing feature of the claimed technical solution is:

  • As a silica-containing amorphous material, dusty wastes of ferrosilicon production are used.

Comparison of the claimed technical solution with the prototype made it possible to establish the conformity of the claimed technical solution with the "novelty".

The set of essential distinctive features allows to achieve the set goal, and to conclude that the claimed technical solution meets the criterion of "inventive level".

As a silica-containing amorphous material, dusty wastes of ferrosilicon production are used, for example, of the following composition (wt.%): SiO 2 = 92.8; CaO = 2.32; MgO = 1.28; Al 2 O 3 = 0.94; MnO = 0.28; Fe 2 O 3 = 1.82; C = 0.56 and having a density of about 0.2 g / cm 3 .

The caustic soda is used as an alkaline component. The amount of water is dispensed from the predetermined ratio of the solid and liquid phases of the prepared suspension.

The claimed method is illustrated by the examples given in the table.

Example 1 (by prototype)
The autoclave is loaded with 450 kg of silicate blocks, 1500 liters of water and 9 kg of silica-containing pulverized waste. The mixture is heated to 120 ° C. under a pressure of 2 atm. And maintained at this temperature for 8-10 hours to obtain a solution with a specific gravity of 1.17 g / cm 3 . The solution is filtered and evaporated to a specific gravity of 1.45 g / cm 3 , cooled and left to stand until a clear solution is obtained. According to XRF data ( X-ray phase analysis), the resulting adhesive contains up to 15% of the SiO2 sol .

Example 2
According to the claimed method, 15 liters of water, 2.7 kg of caustic soda and 6 kg of fly ash from the production of ferrosilicon are fed into a ball mill filled with 1/3 steel balls. During the mixing process, the contents of the ball mill are heated to 50 ° C. and subjected to mechanochemical treatment for 8 hours. The resulting glue-binder is poured into a storage tank. The yield of the finished product is 100% .

All the examples necessary to justify the claimed method, as well as the properties of the adhesive according to the prototype and the claimed method, are given in the table.

In appearance, the glue is a solution of dark gray color with a density of 1.3 - 1.45 g / cm 3 and a pH of about 10 , containing in its composition about 20-25% of the SiO 2 sol and 80% of Na 2 SO 3 according to RFA . It has a long shelf life, does not require a special hardener. The adhesive joint retains its performance when heated up to 1400 ° C.

As can be seen from the table, when using an alkali slurry with a lower concentration when preparing a slurry, if the claimed T: F ratio is not respected, and the temperature and time parameters of the method realization, a glue-binder with reduced characteristics, i.e., with reduced adhesive capacity, is obtained.

A METHOD FOR PRODUCING SILICATE ADHESIVE-BINDING. Patent of the Russian Federation RU2144552

With prolonged machining ( example 10 ), a glue-paste with a low adhesive capacity is formed due to the high viscosity due to dilatancy.

With an increase in the temperature of the adhesive binder above 50 ° C, there is no improvement in its characteristics, hence, it is impractical ( Example 11 ).

When the content of the solution is increased, that is, at T: H = 1: 4 and higher, the adhesive adhesive obtained is not stable (stratified upon storage).

If the reaction time of the initial components is lower than the declared limits, the reaction does not go to the end, the product is not homogeneous, and when the concentration of alkali is reduced below 10 the product is neither homogeneous nor stable.

Thus, the adhesive-binder with the necessary physicochemical properties is obtained due to the combination of the claimed distinctive features.

The proposed method is more simple in technological and technical execution, does not require high temperatures and pressures, is more economically and environmentally efficient and allows to obtain the final product with higher service and operational characteristics.

CLAIM

  1. A method for producing a silicate adhesive binder comprising the use of a silica-containing amorphous material, characterized in that the silica-containing amorphous material is subjected to a mechanochemical treatment in 10 to 17 wt. % Solution of caustic sodium in a ball mill at a ratio of T: H = 1: ( 2.0-3.5 ) , where T is the amount of amorphous silica-containing material being loaded, M is a solution of caustic sodium of these concentrations, at a temperature of 25-50 ° C and Atmospheric pressure for 4-10 hours .

  2. The method of claim 1, wherein the silica-containing amorphous material is a dust-derived waste of ferrosilicon production.

print version
Date of publication 11.11.2006гг