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Method of manufacturing vermiculite-based glass crystal material. RU patent 2250200.

IPC classes for russian patent Method of manufacturing vermiculite-based glass crystal material. RU patent 2250200. (RU 2250200):

C03C10/06 - Divalent metal oxide aluminosilicate crystalline phase, e.g. anorthite, slagcerams
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FIELD: glass article manufacture.

SUBSTANCE: process is accomplished by mixing vermiculite with limestone, reductive melting, separating silicate fraction of melt, and transferring it into X-ray amorphous state by pouring it into water and subsequent one-step heat treatment. In order to reduce heat treatment time, this operation is conducted under self-propagating crystallization conditions consisting in that elevated temperature wave front emerges owing to phase-transfer energy and it propagates at a velocity of 13 mm/min.

EFFECT: reduced heat treatment time.

 

The invention relates to the processing of non-metallic materials, in particular vermiculite, glass-ceramic materials that can be used in the construction industry, as well as in the aluminum industry as a refractory material for lining baths cells.

There is a way to obtain glass-ceramic materials by glass melting, casting it in a mold and crystallization of the resulting material in a muffle furnace with the aim of identifying crystalline phases [1] (Doucouliagos, Chewables, Mayakkam, Scharipova. “Glass for biocompatible glass-ceramic material”. A.S. 1742239 SU. Bull. No. 23 of 23.06.92 year). In this method, a powder mixture consisting of oxides SiO 2 , Al 2 O 3 , MgO, Fe 2 O 3 , MP 2 O 3 , Cao, P 2 O 5 2 O 3 , cook in corundum crucibles at temperatures 1380-1450°C for 1 h Impregnated glass cast in form and carry out the crystallization at a temperature of 850-1000°C for 1-2 hours Along with the crystallization of the glass in the form of solid samples is possible and heat treatment of the glass powders.

A known method of obtaining a glass-ceramic material [2] (Whibogyltv, Vmesto, Oahmofev. “Glass for shlakositalla”. A.S. 1123996 SU. Bull. No. 42 from 15.11.84) by melting glass comprising SiO 2 , Al 2 O 3 , Cao, MgO, Fe 2 O 3 , MnO, S -2 in a reducing environment at 1450±10°C for 2 h Heat treatment is conducted for a two-step mode by exposure in a given temperature range for 4 hours This method is chosen as the prototype for the maximum matching essential attributes. The disadvantages of the method include a multi-stage and duration of the heat treatment process, which limits the possibility of using this method.

The basis of the claimed invention is the task of developing a method of producing glass-ceramic material with a low heat treatment time on the basis of vermiculite, stable composition method of regenerative melting to expand the possibilities of their application as building and refractory materials in the aluminum industry.

The essence of the proposed method lies in the fact that the vermiculite is translated in the x-ray amorphous, stable composition of the state according to the method of [3] (EN 2132306, 6 03 11/00)by pre-adjusting the content of silicon oxide and calcium oxide in the initial charge to mass relationship SiO2 /Cao equal to the interval 1-2, and the carbon content up to 3 wt.%, melting in a reducing environment at a temperature of 1580-1610°With separate metal part of the melt containing iron, subsequent cooling of the silicate part of the melt in the mode of thermal shock shimmer in the water and get the x-ray amorphous, stable chemical composition, depleted iron material (inosilicate) of the following composition, wt.%: SiO 2 37,58; Al 2 O 3 11,34; Fe 2 O 3 0,05; SO 3 0,3; Cao 33,29; MgO 17,2; Na 2 O 0,16; K 2 O 0,08.

Thermographic study of inosilicate with redundancy enthalpy shows that at its transition from the amorphous state into the crystalline dissipation is more than half the value of the heat of fusion. After heating one of the edges of the sample from inosilicate to the temperature of crystallization it raises the local region of the crystallized phase, and along the sample covers the wave front of crystallization, i.e. samorasprostranyayushchiesya crystallization, supported by eye-catching in the crystallization zone of thermal energy of the phase transition.

Inosilicate is crushed to a particle size of 80 microns; the water is added in an amount of 10 wt.% more than 100 wt.% powder molded samples and placed in an oven, the heating which occurs to a temperature of 900°With a speed of 20°C/min and then cooled. At a temperature of 820°is the origin of the wave front of crystallization and its distribution along the sample with a speed of 13 mm/min While the temperature of the sample in the wave front increases by 200°compared with the temperature in the furnace. The rate of temperature change of the sample in the process of propagation of the wave front reaches 300°/min. Upon reaching 900°With the rate of change of temperature of the sample becomes equal to the rate of change of temperature in the furnace. This indicates the end of the process mode samorasprostranyayushchiisya crystallization. The total heat treatment time is 45 minutes. The proposed method of producing glass-ceramic material on the basis of vermiculite is illustrated with a specific example.

Example. 400 g of vermiculite enter 15 g of carbon, 167 g of limestone, is melted in a reducing environment at a temperature of 1580-1610°C. there Is a separation of the melt on the metal part containing iron, dropping to the bottom of the tank furnace, and the silicate portion which is cooled in the mode of thermal shock shimmer in the water with obtaining inosilicate. Inosilicate is crushed to a particle size of 80 μm, add 10 wt.% water in excess of 100 wt.% inosilicate, molded products, place it in the oven, which is heated at a rate of 20°C/min to a temperature of 900°C for 45 min and then cooled. The obtained glass-ceramic material has the following characteristics:

- density of 2.3 g/cm 3 ;

- compressive strength of 135 MPa;

- use temperature 1200°C.

A method of obtaining a glass-ceramic material on the basis of vermiculite by mixing it with lime, restorative melting, separation of the silicate part of the melt containing SiO 2 , Al 2 O 3 , Fe 2 O 3 , CaO, MgO, SO3 , Na 2 O, K 2 O, and its x-ray amorphous state, grinding to a particle size of 80 μm, molding and heat treatment, characterized in that to reduce the time of the heat treatment is performed in the mode samorasprostranyayushchiisya crystallization, which consists in the formation of the wave front of increased temperature due to the energy of the phase transition and its distribution along the sample with a speed of 13 mm/min in the following ratio, wt.%: SiO 2 37,58; Al 2 O 3 11,34; Fe 2 O 3 0,05; Cao 33,29; MgO 17,2; SO 3 0,3; Na 2 O 0,16; K 2 O 0,08.

 

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