UA45307C2 - METHOD OF MANUFACTURE OF METAL MAGNESIUM, METHOD OF MANUFACTURE OF MAGNESIUM OXIDE (VARIANTS) AND METHOD OF MANUFACTURE OF MATHENE MATHENIUM FLAMMABLE - Google Patents

Abstract

Metallic magnesium and pure magnesium oxide are produced by carbothermal reduction of starting materials such as magnesium oxide containing minor amounts of oxides of Fe, Si, Ca and Al, and/or magnesium silicate minerals, such as olivine, at subatmospheric pressure. Metallic magnesium is evaporated from a reduction zone and pure metallic magnesium and pure magnesium oxide are precipitated in a second condensation zone. Si is partly evaporated as SiO which is precipitated in a first condensation zone upstream the second condensation zone, partly converted to SiO and an alloy of Si and Fe in the reaction mixture. The starting materials may also be processed by a method wherein their magnesium component is converted to magnesium oxide in the reaction mixture, while the remaining components are converted to SiO and an alloy of Si and Fe. Au and valuable siderophilic elements may be recovered by leaching the alloy of Si and Fe.

Description

Description of the invention

The present invention relates to methods of processing a raw material selected from groups 2, consisting of magnesium oxide, containing a small amount of oxides Ee, Zi, Ca and Al, natural and industrially obtained magnesium silicate minerals and their osmosis, for example, olivine, by carbon-thermal reduction and methods of production of metallic magnesium, pure magnesium oxide (MoO) and refractory masses consisting of Mo, Ma 251054, and 5iC, by carbon-thermal recovery of the starting materials selected from the above groups,

In general, metallic magnesium is obtained by means of electrolytic and thermal methods. When using thermal methods, two groups of minerals/rocks are used as starting materials.

The first group, in which magnesium oxide is associated with carbon dioxide, includes, for example, a mineral! magnesite and dolomite. 19 The second group, in which magnesium oxide is associated with silicon dioxide, includes, for example, the mineral olivine.

Although a mineral! in the second group, for example, olivine is found in a large amount of deposits and has a high magnesium content, in industry, magnesite and dolomite are mainly used for the production of magnesium, i.e., the source material from the first group!

This is due to the fact that it was found that it is possible to remove and separate CO" from the members of the first group more easily than to remove and separate BIO" from the members of the second group!

In general, to remove 5iO" from the second group! White proposed two classes of methods: the wet method, in which ores are treated with strong mineral acids, and the direct method! recovery, in which the magnesium oxide component is ore! are restored and removed in the form of gaseous Ma.

Direct method! can be divided into two groups. In the first group of direct recovery methods, which were proposed only in connection with the recovery of metal oxides, i.e. not metal silicates, used Ho) reducing agents that form a gaseous reaction product containing oxygen, for example, reduction of MoaO with carbon as a reducing agent at atmospheric pressure and a temperature of 185070 leads to the formation of Mo and CO as a gaseous reaction product containing oxygen, or other methods were used carbon-thermal recovery, see, for example, OZ RBZ 2268779 in (ZEIREKT) and 05 RB 2582119 and 2582120 (NAMZOIKO). Ha")

When a mixture of magnesium silicate, for example, olivine (Mao xx Be,ziOd; ХО - 1), and carbon are heated to temperatures! in the interval from 13007 to 2200"C, the following reactions occur: o (1) (Mog-xgeh)ViOd(tv) with (14. x (14 2)) C(tv) "" y (2-x) Mastv) z (1 - 2x) BIO(g) (1 - x(1 z 2)) CO(g) k x"Vi,ge(1X(alloy 5i and Ee) Z (19 Mao»ziOd(tv) i Z C (tv) is" 2 Mao (tv)k5is(tv)" 2 SOsg) (173 Ma»ziOd(tv) i Z C(tv) is" " 20 2 Ma (p-5id(g)k Z SO(G ) with (1779 Ma»BiOd(tv) zhk 5 C(tv) "is" with 2 Ma (g -8is(g)n 4 SO(g) with (2) MoOtv) "S(tv) "" Ma( d) - СО(г) (3) БО(г) «С(тв) «и» II (тв/ж) «СО(г) (4) 5Ии (тв/ж) и- С(тв) «» 5IS(tv) "r" where: (tv), (h) and (d) denote the solid, liquid and gaseous phases, respectively.

At increased temperatures! and reduced pressures of the equilibrium, except for equilibrium (4), shift to the right. o Similar reactions occur with carbon-thermally reduced MoO, containing impurities, o 50, for example, oxides of Re, Z, Ca, and AI, which will later be referred to as "raw Moo".

Due to the formation of gaseous components Ma (g) and 5iO (g), movement of Ma and "I ZO" can occur within the limits of the reaction mixture, and Ma and 5iO can even be removed from it by evaporation.

Thus, solid Mo can be collected by condensation of vaporized metallic Ma in a separate condensation zone, i.e. in a condenser located at a distance from the reaction mixture.

The problem, inextricably linked to the first group of direct methods, is the possibility of a reverse reaction (see equation 2) between magnesium and the reaction product containing gaseous oxygen, by means of which magnesium is oxidized to magnesium oxide. This problem can be solved in the second group of direct methods using reducing agents that form a non-gaseous product! reactions, for example, during the reduction of magnesium-containing ores with silicon, aluminum, calcium carbide or silicon carbide.

Methods belonging to the second group of direct recovery methods, descriptions! described in a number of patents, for example, 2372571, 2379576, 2527722, 2527724 and 2570232 (NAM5OIIKO), and are also used in practice, for example, in the method of NAM5O|KOSa mentioned above, the methods of Riedeop and WoyIgapo (reaction between burning dolomite and ferrosilicon at temperature about 12007"C and under pressure) and in the 65 magnesium thermal method (recovery of calcined dolomite with ferrosilicon in the presence of aluminum oxide at a temperature of about 16007C and a pressure of 4KRa). In the methods related to the previous level of technology, other different solutions to the problem were proposed! avoiding the reverse reaction: in connection with the carbon-thermal reduction of MoaO, for example in the following way: to minimize the reverse reaction of the incoming gas obtained during the carbon-thermal reduced MoaO by: - instantaneous sharp cooling of the gas coming out of the carbon of the thermal zone, for example, shock cooling by injecting a cooling medium or by rapid adiabatic cooling nia, see, for example, 05 RB5 2582119 and 2582129 (NAMZOIKO), the description of the European patent application Mo 75836 (AMEKUH) and 05 RZ 4200264 (NOKI) or 70 - deposition of Mo under reduced pressure, see, for example, OE P5 49329 (KMORGEK) , 05 RZ 2257910 (KIKK) and Tgapzv. Ipvia Meep. Mega). 99. Mau-A!tsdivi 1990, pp. С1О5-СИ (M/LMAMO ей. ай).

During the carbon-thermal reduction of magnesium silicates, the amount of CO obtained increases compared to the amount of CO obtained during the carbon-thermal reduction of magnesium oxide, because CO is obtained not only during the reduction of MOoO, but also when 510 is reduced."

If during the carbon-thermal recovery Mod" 5iO; increase the pressure, increasing amounts of 5iO will evaporate from the reaction mixture, which will lead to an increase in the ratio of ZIO/Ma in the gas leaving the reaction mixture.

The closest in technical essence to the proposed method of obtaining metallic magnesium is the process (see US patent No. 4,437,886, class C22B 26/22), the essence of which is as follows. either a first amount of magnesium oxide, a second amount of a carbide-forming material, which is either a material selected from the group consisting of calcium, aluminum, boron, silicon, calcium oxide, aluminum oxide, boron oxide, and silicon oxide, or is a mixture of the two and more of these materials, and the mass of which is equal to 1095 and less than the mass! of the first amount and the third amount of carbon, which is at least equivalent to the molecular weight of magnesium oxide plus the material that forms the carbide, is heated in a reduction furnace at a pressure in the range from approximately 5 to 200 torr and a temperature of at least 1600°C. , which forms carbide, combines with carbon and i) forms carbide, which undergoes a reduction reaction occurring simultaneously with the reaction formed by carbon and reduces magnesium oxide, releasing magnesium vapors, which are quickly cooled by adiabatic expansion and form metallic magnesium, while - the carbide-forming material goes into the oxide form. The carbide-forming material is returned to the process and is repeatedly used to form carbide and restore new amounts of magnesium oxide.

However, the specified known method does not allow obtaining metallic magnesium of a sufficiently high degree of purity, since it does not allow to avoid contamination of the final product with MoO and C, and products obtained from 5IO". "IS

The first task that must be solved with the help of the present invention is to provide a carbon-thermal method for obtaining Mo from starting materials selected from the group consisting of magnesium oxide containing a small amount of He, 5i, Ca and A! oxides: natural and industrially obtained magnesium silicate materials and their mixtures, for example, olive oil when used, which "avoid contamination of the final magnesium product in c (I) Mass and C, obtained by means of the above-mentioned reverse reaction, and (II) condensation products obtained from 510, for example, Mo»ziO», zi, ZiS, 5iobo, etc. and According to the prior art, gray magnesium oxide, i.e. magnesium oxide containing impurities, for example, oxides of Re, Z, Ca, and AII, are obtained by calcining magnesium hydroxide, magnesium carbonate, or basic magnesium carbonate. Magnesium hydroxide is obtained on a large scale from sea water using a method in which Ma(OH)" is precipitated by adding calcium hydroxide. Precipitated magnesium hydroxide generally contains trace amounts of oxides B, Ca, ooZi, AI and Ge as impurities. These polluting impurities have a harmful effect on the behavior of magnesium oxide during 5-year sintering and during subsequent applications, which is why whites are taken! significant effort to remove these impurities, which led to high costs associated with processing.

And high-purity magnesium oxide is obtained by melting magnesium oxide (Mo90) by electric arc melting.

In this method, which is described, for example, in Kadeh Kypaznats 1958, Nei 2, p. 91-104 (EIREI TASHEK et al.), Mao purification is achieved as a result of the migration of impurities through the liquid or gaseous phase into the directed 5v of the surface before and after cooling the molten MoO downloads.

After solidification, impurity particles! the hard block of Mao is removed by mechanical means. Thus, when this method is used, in addition to the inexhaustible high energy costs required for the melting of MoO, a relatively high ratio of production waste to product is obtained.

In addition, it is known to obtain a fine powder of magnesium oxide (periclase) suitable for the production of high-quality ceramics by a method in which metallic magnesium is evaporated at a temperature of 7007C or higher in a stream of inert gas and mixed with an oxygen-containing gas to ensure the flow of a reaction mixture in which steam! magnesium is oxidized to fine particles of magnesium oxide, which are collected from the reaction mixture, for example with the help of a filter, see the application of ZV (Great Britain) for patent Mo 2183622 (UO5NIBA). 65 The closest in technical essence to the proposed method of obtaining magnesium oxide is the method of obtaining fine-grained powder of magnesium oxide (see patent Great Britain Mo 2141701, class СО1Е

5/04) Its essence is that a fine-grained powder of high-density magnesium oxide is obtained using a process in which magnesium evaporates at a temperature of 7007"C or more in a stream of inert gas and mixes with a gas containing molecular oxygen, while the temperature the area of magnesium oxidation is regulated in the range from 800"C to 1600"C, and the values of the partial pressures of evaporated magnesium and oxygen in the area of magnesium oxidation are adjusted to a level of 0.09 atmospheres and less than a level that is 1/2 or more of the pressure of evaporated magnesium .

Disadvantages of known methods of production of magnesium oxide include the need to use expensive magnesium as a starting material. At the same time, the final product contains oxides of Са, си, АЙ у) M ге.

The second task to be solved by the method of the present invention is to provide a method of obtaining high-purity magnesium from inexpensive raw materials, while the high-purity magnesium oxide product does not essentially contain oxides of Ca, Z, AI and Ge.

It is well known that fireproof material! obtained by sintering olive powder at a temperature /5 V in the interval 15407 - 17107С under oxidizing conditions and at atmospheric pressure. In order to avoid the formation of low-melting phases, the content of calcium, aluminum and iron oxides in the original olivine should be low enough, usually less than 795 wt.

Eyop, my And, rarely 561-562, but even when these amounts of olivine are used, the resulting sintered product cannot be classified as a refractory material with high operational qualities.

BIS is an example of a refractory material with high operational qualities. It can be obtained in an electric furnace by reducing BIO 2 with carbon at a temperature of about 2200" - 240026.

Technical grade magnesium oxide can be burned, moreover, it is processed by sintering at temperatures up to 190072 degrees Celsius to obtain a hard-burned magnesium oxide, which is an important refractory material used in the production of steel.

The growing need for refractory materials with high operational qualities, used in modern steel production, has switched the market's needs to pure high-density sintered materials! The closest in terms of technical essence to the proposed method of processing raw materials is the process (see US patent No. 4,437,886, class C22B 26/22), the essence of which is as follows. at

A mixture of a first amount of magnesium oxide, a second amount of carbide-forming material, which itself is either a material selected from the group of materials consisting of calcium, aluminum, boron, silicon, calcium oxide, aluminum oxide, boron oxide, and silicon oxide, or is a mixture two or more o

Зз5 Of these materials, and the mass of which is equal to 1095 and less than the mass! of the first amount and the third amount of carbon, which is at least equivalent to the molecular weight of magnesium oxide plus the carbide-forming material, is heated in a reduction furnace at a pressure in the range from approximately 5 to 200 torr and a temperature of at least 1600"C The carbide-forming material combines with carbon and forms carbide, which undergoes a reduction reaction that occurs simultaneously with the carbon-induced reaction and reduces magnesium oxide, releasing magnesium vapor, which quickly cools by adiabatic expansion and forms metallic magnesium , at the same time, the carbide-forming material passes into the oxide form. The carbide-forming material is again returned to the process and repeatedly used to form carbide and restore new amounts of magnesium oxide.

The disadvantage of the known method of obtaining a refractory material is that it uses expensive sulfur. In addition, this method does not allow extracting valuable metallic elements contained in magnesium silicate rocks and minerals in low concentrations, for example, Mn, St, Mi, o Ai and members of the platinum group. oo The third problem that can be solved by the method of the present invention is to provide a simple and inexpensive method of obtaining refractory materials with high operational qualities, in which inexpensive sulfur selected from the group consisting of magnesium oxide containing

And a small amount of He, 5i, Ca and AI oxides, natural and industrially obtained magnesium silicate minerals; and their mixtures, for example olive.

In addition, it is desirable to provide a common method of processing members of the above-mentioned groups, which allows extracting valuable metallic elements contained in magnesium silicate rocks and minerals in low concentrations, for example, Mp, St, Mi, Am and members of the groups! platinum! (F, Description of the invention ka 1. Magnesium

It was found that the first problem can be solved with the help of the method of obtaining metallic magnesium, because by the ulerodothermal recovery of the starting material, selected from the group consisting of magnesium oxide, containing a small amount of He, 5i, Ca and AiY oxides; natural and industrially obtained magnesium silicate minerals and their mixtures, for example, olivine, which includes: - mixing of the starting material with carbon in the amount: at least Imol C/mol 5iO" plus at least Tmol C/mol BeO, plus at least 1 .3 moles C/mol Re2zhOz, plus at least 65 C/mol Mao Imol; - preferably in an amount of at least 2mol C/mol 5iO" plus at least Tmol C/mol

EeO, plus at least 1.3 mol C/mol Re»Oz, plus at least Tmol C/mol Mao; - especially in an amount of at least 3 mol C/mol 5iO" plus 1 mol C/mol Beo, plus 1.3mMole

C/mol Re»zhOz, plus TImol C/mol Mao; - preferably in an amount less than 4 moles C/mol 5iOo plus 2 moles C/mol ReO, plus 4 moles C/mol

Ee2O3z, plus 2 mol C/mol Moo; - heating the mixture in the reduction zone to temperatures of TT, in the range of 14007 - 1700C, preferably less than 15007"C, at pressure p, in the range of 0.01 - 1.75 kRa, preferably 0.2 - 1.1 kRa, in particular 0 ,3 - 0.7 kRa; - reduction of iron oxide contained in the source material in the reduction zone to iron; - reduction of silicon dioxide contained in the source material to BIO, which is partially transformed into 5iC and the alloy 5i and Re, "Zi, ZhBe" in the reduction zone, partially evaporates from the reduction zone and turns into 5iC, 5i and/or M9255iO, interacting with carbon in a separate 75 first condensation zone at a pressure of 0.01 - 1.1kRa, preferably 0.2 - О.8вкРа, in particular 0.3 - О.7кРА, at a temperature Tu more than;

Tntn7С- SIYA oot318 2109 ru - 19.92 where ri is reflected in kRa, and below (Tmin 7 1007С), preferably (Tuyn and 507), in particular (Tuyn 7 25"7С) and in any case below T,: - restoration of magnesium oxide of the starting material to gaseous metallic magnesium in the reduction zone; - evaporation of the aforementioned gaseous metallic magnesium from the reduction zone and condensation from gaseous metallic magnesium in a separate second condensation zone, located behind the first condensation zone, at a pressure within the interval 0.01 - 1 ,ykRa, preferably 0.2 - 0O,v8kRa, in particular 0.3 - 0.7kRa, at a temperature of at least 638"C, preferably in the range 2007 - 600"C, in particular in the range 2507 - 540"C ; и - removal of CO, formed by means of the above-mentioned recovery methods, from the second condensation zone and maintaining the pressure of the pump at pre-selected values of the ways of use of the pump; - by means of which the temperature gradient between the first condensation zone and the second condensation zone (СО is supported as large as possible; and ю - by means of which р» « ри « ру.

The main idea of the first aspect of the invention consists in regulated methods of transfer of gaseous magnesium and 5IIO by the carbon-thermal reaction of strong magnesium oxide and magnesium silicate minerals, i.e. regulation of the location of the formation of products and by-products by selecting the corresponding values and gradients of the following process parameters: pressure (values and gradient), temperatures (values and gradient) and the percentage of carbon in the sludge (values) in the reaction zone and in the first and second condensation zones . in c The vaporized material is extracted by condensation at low temperatures. Thus, the vaporized SiO (g) is essentially extracted in the form of 5i (tv) or 5iC (tv) in a suitably designed first condenser operating at a temperature lower than the temperature of the layer , and higher than the temperature (Tuin), where Mo (tv) can be formed by the reverse reaction corresponding to (2) Ma (g) and - CO (g) -" MO (tv) " C (tv). Evaporated Ma (g) can then be extracted in a suitably designed second condenser operating at a temperature lower than Tuin in the form of Ma (tv), while the reverse reaction (2) is avoided by working! at low pressure in by maintaining a large temperature gradient between the first and the second condenser. ("in 50 It is desirable to use 5 moles of carbon (C) or more for each molecule of olivine (Ma"5iO)), when the goal is to obtain pure Mao (tv) or MoO (tv), well separated from silicon-containing phases by carbon-thermal conversion of olivine .

The reaction will occur in accordance with (1) Ma925510, (tv) i- 5С (tv) -» 2Ma (g) k- BIS (tv) - 4СО (g). 59 This ensures the complete evaporation of magnesium and the maximum content of silicon in the layer in the form of carbide

HF) silicon (and Bi, be, when iron is present). Thus, the amount of ZO (g), which will be 7 condensed in the form of 5Ii (tv) or 5iIS in the first condenser, will probably be very insignificant.

The present invention, concerning the production of pure Mao (tv), is based on the purification of the gas phase formed by carbon-thermal processing of magnesium silicate materials and rocks, as well as 60 contaminated magnesium oxide, by condensation of the evaporated 5iO (g) in the form of 5i (tv) or 5iC ( tv) in a suitably designed first capacitor. This is most effectively carried out by the formation of IS (tv) corresponding to (335 2C -, viC and CO at a temperature higher than Tuin, where Mas (tv) can be formed by the reverse reaction between Ma (g) and CO b5 (7). with the help of the following equation (laboratory of the KR):

Cumin - -32217 (2 109 (Robosch) - 19.92371 - 273.15

As mentioned above, Bio interacts with carbon in the first condensation zone. The mentioned zone is advantageously given the shape of a single pipe or it is filled in the form of a set of parallel pipes filled with chemically active carbon or covered with chemically active carbon.

The starting materials suitable for use in the above-mentioned method are: - gray magnesium oxide, i.e. magnesium oxide containing a small amount of impurities, for example oxide Ee, 5i, Sam AI, - silicate! magnesium, i.e. natural and industrial production of magnesium silicate minerals. 70 Magnesium oxide sulfur contains calcined (heat-treated at a temperature of approximately 100072) compounds obtained from magnesite, brucite, kieserite, or similar industrially obtained materials, for example, spent furnace lining filled with periclase, or filter sawdust from magnesite-burning factories.

Gray magnesium oxide contains more than 5095 MoO, in particular, more than 8095 Ma9O. Preferably, the content of 75 CaO will be less than 195, in particular less than 0.595,

Preferably, the content of alkali metals will be less than 195, in particular, less than 0.395 in terms of oxide.

Preferably, the sum of the second volatile elements, for example 5 and SI, and metals such as 7p, Ca, Na, etc., will be less than 195, in particular less than 0.595.

Slick! magnesium include natural or calcined (heat-treated at a temperature of 10007C) silicate mineral, for example, olivine, serpentine, vermiculite, anthophyllite, cumingtonite, znstatite, pyrope, spinel, and similar industrially obtained compounds containing Ma as the main component, which is determined! below

Preferably silicate! magnesium contain more than 2595 Mo, in particular more than 4095 Ma. si

Preferably, the content of SAC is less than 195, in particular less than 0.595. at

Preferably, the content of alkali metals is less than 195, in particular, less than 395 in terms of oxide!.

If the AI2O5z content is higher than 3905, the reaction temperature in the reduction zone must be less than 155072 to avoid the formation of aluminum carbide. -

Preferably, the sum of other volatile elements, for example Z and SI and metals, such as 7p, Ca, Na, etc., added is less than 195, in particular less than 0.595. at

Slick! magnesium, in addition, include natural rocks consisting of more than 5095 silicates. and magnesium, which is higher, preferably more than 8095, in particular rocks consisting of more than 9095 silicates, and industrial waste, rich high-quality magnesium silicate, for example, the use of forsterite furnace lining. h;E

In this context, the term "carbon" includes material rich in carbon, for example, anthracite, carbon black, and coke.

This material is rich in carbon! in general, the following composition: "carbon content" 9095 shsh with ash "290 ts volatile component! "890 p" Preferably: carbon content "9695 ash "195 c" volatile component! "390 s Preferably: carbon content" 98.595 (95) ash "0.595 o 50 volatile components! "195 "I The starting material is preferably ground to an average particle size of less than 45 mm.

The carbon-rich material preferably has an average particle size of about 100 nm. The reaction mixture is preferably introduced into the reduction zone in the form of briquettes having a porosity of about 57905.

A large temperature gradient between the first and second condensation zones can be obtained by means of quenching methods proposed for use in the carbon-thermal processing method,

F, which is described in the description of the patent discussed above. according to the preferred options: - a large temperature gradient between the first and second condensation zones is provided by means of rapid cooling, which includes the introduction of gas from the first condensation zone into the dispersing nozzle operating under conditions of insufficient expansion, the ejection of the mixed gas through the dispersing nozzle and the creation of an opportunity for mixed gas expands adiabatically at supersonic speed, as a result of which the coefficient of expansion in the nozzle is selected in the range of 12.5 - 2, preferably in the range of 12.5 - 6; 65 - the silicon dioxide component of the starting material is converted in the reaction mixture essentially at 5°C by using added carbon in the amount taken in the interval C - 4 Ammol C/mol ZO 5" plus 1

- 2 moles of C/molBes, plus C - 4 moles of C/mol Re2»O3z plus 1 - 2 moles of C/mol Mao; - the temperature gradient between the reduction zone and the first condensation zone is maintained as large as possible; - magnesium oxide containing small amounts of He, 5i, Ca and AI oxides is used as the starting material; - olive oil is used as a starting material; - when the content of AI2Oz in the initial reaction mixture is more than 195 wt., T. less than 15507; -"8i,Re" and metallic iron are separated from the rest in the reduction zone by traditional methods, 7/0, for example, by magnetic or electrostatic separation or flotation, after which A and transition elements), for example, Mp, St, AI, and metal from the platinum group are extracted generally accepted methods, for example, leaching and - IS, formed in the reduction zone and the first condensation zone, are extracted in the form of a by-product from the residue, respectively, in the reduction zone and the first condensation zone.

The extracted 5iC is a microproduct of high purity.

Magnesium, depending on the conditions in the second condensation zone, can be deposited in the form of macrocrystals, as well as in the form of a pyrophoric mass, which can be melted and formed into ingots by generally accepted methods. 2. Magnesium oxide

In addition, it was found that the second problem can be solved by the method of obtaining pure magnesium oxide by carbon-thermal reduction of the starting material, selected from the group consisting of magnesium oxide containing small amounts of He, 5i, Ca and Al oxides; natural and industrially obtained magnesium silicate minerals; in their mixtures, for example, olive oil, which includes; - mixing of the starting material with carbon in the amount of at least Imole C/mol ZiO" plus at least thymol C/mol Reo, plus at least Zmol

C/mol Re»Oz, plus at least Thymol C/mol Mao; o - preferably in an amount of at least 2mol C/mol 5iO» plus at least Tmol C/mol

EeO, plus at least Zmol C/mol Be2O3z, plus at least imol C/mol MdO; in particular, in the amount of at least 5% Zmol C/mol 5iO" plus iImol C/mol BeO, plus Zmol C/mol Be2O3, plus

Lmol C/mol MoO; preferably in an amount less than 4 moles C/mol ZiOo plus 2 moles C/mol Geo, plus 4 moles C/mol Re2»Oz, plus 2 moles C/mol Mao. o - heating the mixture in the reduction zone to temperatures! T, in the interval 14002 - 17009C, preferably (With less than 15002C, at pressurized p, in the interval 0.01 - 10 (-16381..(T,- 273) and 10.03) kRa, and preferably « 0, 2 - 10 (-16381.. (Tu 273)7 x 10.03) kRa, in particular 0.3 - 1.75 kRa; " - reduction of the iron oxide component in the reaction mixture to iron; - reduction of the silicon dioxide component of the starting material to 5iO, which is partially converted to 5iC in the reduction zone by the alloy ZiS, Re, and/or M925iO, by interaction with carbon z" in a separate first condensation zone at a pressure p/, where ri x p, and at a temperature T/ higher , than

Tinss-- ZM 2735 mountains -19.92 and where ri is expressed in kRa, and lower than (Tmin 7 10022), preferably (Tuyn and 5022), in particular (Tuyn and 1 25"С), and in any case it is lower T,; c - reduction of the magnesium oxide component of the starting material, at least partial gaseous metallic magnesium in the reduction zone; o - evaporation of gaseous metallic magnesium from the reduction zone and interaction of gaseous metallic magnesium with CO, formed in the reduction zone, to ModO and С , and precipitation of these reaction products in the form of a mixture of carbon and magnesium oxide in a separate oxidation zone and a condensation zone, located behind the first condensation zone, at a pressure of ro, where ro x ri and at a temperature of To

In the interval from 6382 to T., preferably from 6502C to TT. - 50, in particular from 8002 to 100025; - removal of a mixture of carbon and magnesium oxide from the zone of oxidation and condensation and removal of carbon from

F) removed product, for example by oxidation; and ka - the removal of that part of CO, which was formed as a result of the above-mentioned methods of reduction, is not consumed during the reaction with MoO, from the oxidation and condensation zone and maintaining the pressure of p 25 at pre-selected values by using a pump; - by means of which ro x ri x ru.

In addition, it was found that the second problem can also be solved by the method of producing pure magnesium oxide by the carbon-thermal reduction of the starting material, selected from the groups consisting of magnesium oxide, containing an insignificant amount of oxides of He, Z, Ca, and Al, native and 65 industrially obtained magnesium silicate minerals, and their mixtures, for example, olive oil, which includes; - mixing of the starting material with carbon in the amount of at least imol C/mol 5iO" plus at least thymol C/mol Geo, plus at least Zmol C/mol Ge»Oz plus at least mol

C/mol ModO; preferably in an amount of at least 2 mol C/mol 5iO" plus at least Thymol

C/mol of ReO, plus at least Zmole C/mol of Re»Oz, plus at least Tmol C/mol of ModO; in particular

In the amount of at least Zmol C/mol BIO" plus mol C/mol Geo, plus Zmol C/mol Re2Oz, plus 1 mol C/mol Mao; preferably in an amount less than 4 moles C/mol ZiOo plus 2 moles C/mol GBeo, plus 4 moles C/mol Be»zhOz plus 2 moles C/mol Mao; - heating the mixture in the reduction zone to temperatures! T, in the interval 1400 - 170092С, preferably less than 15002С, at pressure p, in the interval 0.01 - 10 (-16381..(Т, - 273) and 10.03) kPa, preferably 0.2 - 10 (- 16381.. (Tu 273)7 and 10.03) kRa, in particular 0.3 - 1.75 kRa; - restoration of the iron-oxide component of the source material in the reduction zone to iron; - reduction of the silicon dioxide component of the starting material to 5iO, which is partially converted in the reduction zone of 5iC into an alloy of 5iC and Re, "5i,He" is partially evaporated from the reduction zone and converted into ZiS, and/or Ma»5iO; by interaction with carbon in a separate first condensation zone at a pressure p», where ru « p, and at a temperature higher than

Tinss-- ZM 2735 mountains -19.92 where ri is reflected in kRa, and below (Tuyn 7 10022), preferably (Tuyn y 502), in particular (Tuyn 7 2590) and in any case below T,; c - reduction of the magnesium oxide component of the starting material, at least partially, to (C) gaseous metallic magnesium in the reduction zone; - vaporization of the aforementioned gaseous metallic magnesium from the reduction zone and interaction of gaseous metallic magnesium with separately added oxygen-containing gas, for example molecular oxygen, air, CO, CO, NoO and their mixtures, to the formation of magnesium oxide and precipitation of magnesium oxide in a separate oxidation zone and condensation, located after the first zone (av) of condensation, under pressure p», where ro « ri, and at a temperature To in the interval from 6382 to T3, preferably from 65022 to Tu - 50, in particular from 8002C to 100020; - removal of magnesium oxide from the oxidation and condensation zone and, if necessary, removal of carbon from the removed product by oxidation; и « - removal of gases formed during the above-mentioned processes of reduction and oxidation from oxidation and condensation zones and maintenance of pressure р at pre-selected values by using a pump; - by means of which ro « ri « rr «

The main idea of the second aspect of the present invention is essentially the same as that of the first aspect.

The evaporated material is extracted by condensation at low temperatures. Thus, ;" the evaporated 5iO (g) can be extracted in the form of 5i (tv) in the first condenser designed in a corresponding manner, operating at a temperature below the temperature! layer and higher than the temperature (T min), where MaO (tv) can be formed by means of the reverse reaction in accordance with: .

Evaporated Ma (g) can then be extracted in a suitably designed second and th condenser operating at a temperature lower than Tuin, or in the form of MoO (tv) mixed with C (tv) in

Ge) in accordance with the reverse reaction given above, or in the form of Mo (tv), when molecular oxygen, air, CO, H2oO are separately added to their mixture. o It is desirable to use 5 moles of carbon (C) or more for each mole of olivine (Ma925iO)), when the goal of "I is to obtain pure Ma (tv) or MoO (tv), well separated from silicon-containing phases by carbon-thermal conversion of olivine.

The reaction will occur in accordance with: (1) Ma925510, (tv) i- 5С (tv) -» 2Ma (g) k BIS (tv) - 4СО (g)

That ensures complete evaporation of magnesium and maximum retention of silicon in the layer in the form of carbide i) silicon (and "5i, Re", when iron is present). Thus, the amount of 510 (tv), which is condensed in the form of Z (tv) or IC in the first condenser, will probably be very insignificant.

The present invention, related to the production of pure MoO (tv), is based on the purification of the gas phase formed during carbon-thermal processing of magnesium silicate minerals and rocks, as well as contaminated magnesium oxide by condensation of evaporated 5iO (g) in the form of 5i (tv) or 5iC (tv ) in the first capacitor designed with the corresponding edge. This is most effectively carried out by the formation of IS (tv) in accordance with: (335 2C -, viC and CO 65 at a temperature higher than TUuyn, where Mao (tv) can be formed by the reverse reaction between Ma (g) and CO (7). Darkness determined using the following equation (Robsh in kRa):

Cumin - -32217 (2 109 (Robosch) - 19.9237! -273.15

As mentioned above, 5IO interacts with carbon in the first condensation zone. The mentioned zone is advantageously filled in the form of a single pipe or in the form of multiple parallel pipes made of chemically active carbon or coated with chemically active carbon.

The starting materials suitable for use in the above-mentioned method are: - gray magnesium oxide, i.e. magnesium oxide containing a small amount of impurities, for example oxide Ee, 5i, Sai di - silicate! magnesium, i.e. natural or industrial production of magnesium silicate minerals.

Magnesium oxide sulfur involves calcination (heat treatment at a temperature of approximately 100072) of the compound, obtaining it from magnesite, brucite, kieserite, or similar industrially obtained material, for example, spent furnace lining filled with periclase, and filter sawdust from magnesite roasting factories.

Magnesium oxide sulfur contains more than 8095 Mo, in particular, more than 8095 MaO. Preferably 75 content of Sas will be less than 195, in particular less than 0.595.

Preferably, the content of alkali metals will be less than 195, in particular, less than 0.395 in terms of oxide.

Preferably, the sum of other volatile elements, for example 5 and SI, and metals such as 7p, Ca, Re, etc., will be less than 195, in particular less than 0.595.

Slick! magnesium include natural or calcined (heat-treated at a temperature of 10007) silicate mineral, for example, olivine, serpentine, vermiculite, anthophyllite, cumingtonite, znstatite, pyrope, spinel and similar industrially obtained compounds containing Ma as the main component, which is determined! below

Preferably silicate! magnesium contain more than 2595 ModO, in particular more than 4095 MaO. si

Preferably, the content of SAC is less than 195, in particular less than 0.595. at

Preferably, the content of alkali metals is less than 195, in particular, less than 0.395 in terms of oxide.

If the AI2O5z content is higher than 3905, the reaction temperature in the reduction zone should be less than 15507С in order to avoid the formation of aluminum carbide. -

Preferably, the sum of small volatile elements, for example 5 and SI, and metals such as 2p, Ca, Na, etc., should be less than 1905, in particular less than 0.595. at

Magnesium silicates, in addition, include natural rocks consisting of more than 5095 silicates, which we will determine! more, preferably from more than 8095, in particular, rock, consisting of more than 9095 silicates, and industrial waste, rich in magnesium silicate of high quality, for example, the use of forsterite furnace lining. h;E

In the present context, the term "carbon" includes material rich in carbon, for example anthracite, carbon black in coke.

This is a carbon-rich material! in general, the following composition: "carbon content" 9095 shsh with ash "2 c volatile component! "890 p" Preferably: carbon content "9695 ash "195 c" volatile component! "390 s Preferably: carbon content" 98.595 (95) ash "0.595 o 50 volatile components! "195 "I The starting material is preferably ground to an average particle size of less than 45 mm.

The carbon-rich material preferably has an average particle size of about 100 nm. The reaction mixture is preferably introduced into the reduction zone in the form of briquettes having a porosity of about 57905.

According to the preferred options: - the silicon dioxide component of the starting material is converted in the reaction mixture essentially at 5°C

F, by using added carbon in the amount taken in the interval C - 4 mmol C/mol 510 5» plus 1 co - 2 moles C/molBes, plus C - 4 moles C/mol Re2»O3z plus 1 - 2 moles C/mol Mao; - the temperature gradient between the recovery zone and the first condensation zone is maintained as large as possible; - magnesium oxide containing small amounts of He, 5i, Ca and AI oxides is used as the starting material; - olive oil is used as a starting material; - when the content of AI2Oz in the initial reaction mixture is more than 195 wt., T. less than 15507; 65 -"8i,Re" and metallic iron are separated from the rest in the reduction zone by traditional methods, for example, by magnetic or electrostatic separation or flotation, after which A and a transition element), for example, Mp, Cg, AI, and the metal is extracted from the platinum pear by generally accepted methods , for example, by leaching and - IS, formed in the reduction zone and the first condensation zone, are extracted as a by-product from the residue, respectively, in the reduction zone and the first condensation zone.

The extracted 5iC is a microproduct of high purity. 3. Processing of magnesium silicates.

In addition, it was found that the third problem can be solved by processing the source material selected from the group consisting of magnesium oxide, containing small amounts of oxides Re, Z, Ca 7/0. M AiYi; natural and industrially obtained magnesium silicate minerals; and their mixtures, for example olivine, which includes: - mixing of the starting material with carbon in the amount of at least Imol C/mol ZiO" plus at least thymol C/mol Reo, plus at least Zmol

C/mol Re»Oz, plus at least Thymol C/mol Mao; 15 - preferably in an amount of at least 2mol C/mol 5iO" plus at least Tmol C/mol

BeO, plus at least Zmol C/mol Be2O3z, plus at least TiTmol C/mol ModO; in particular, in the amount of at least 1 mol C/mol 5iO" plus 1 mol C/mol Geo, plus 1 mol C/mol Re2Oz, plus 1 mol C/mol Mao; preferably in an amount less than 4 moles C/mol ZiOo plus 2 moles C/mol GBeo, plus 4 moles C/mol Re2»Oz, plus 2 moles C/mol Mao. 20 - heating the mixture in the reaction zone to temperatures! t; in the interval 1400 - 18007C, preferably less than 1700"C, at pressure p, in the interval (-16381.. (Tu - 27337 j 10.03) - 10 (-17043.. (Tu 2737 i - 10.75) kRa is preferably at 1700 - 17507 and about 101 kRa (Tatm), by means of which: the iron oxide component of the starting material is reduced in the reaction mixture to iron, the silicon dioxide component of the starting material is, at least partially, converted in the reaction zone into 5IiS and the ZS alloy, Be and "5i,Re" the magnesium oxide component of the starting material is converted at least partially into magnesium oxide (periclase): - removal of the essentially completely converted mixture as a final product from the reaction/che zone; o - removal of CO formed by the above-mentioned methods recovery, from the reaction zone and maintaining the pressure of Ro in the reaction zone with the pre-selected means "(9) using a pump; and if desired, precipitation of a mixture of MoaO, Mao"5iO", 5i and 5iC when gas is removed from the reaction and daughters! in a separate condensation zone, located in front of the pump, at a pressure of 100 °C, and at a temperature in the range of 800 - "KG 150072" and extraction of the mentioned precipitated material.

The starting materials suitable for use in the above-mentioned method are: - gray magnesium oxide, i.e. magnesium oxide containing a small amount of impurities, for example, "oxide Ee, 5i, Sai AI, - silicate! magnesium, i.e. natural and industrial production of magnesium silicate minerals. o) with sulfur magnesium oxide contains calcined (heat treatment at a temperature of approximately "» 100072) compounds obtained from magnesite, brucite, kyserite, or similar industrially obtained "material, for example, spent furnace lining filled with periclase, or filter sawdust from magnesite calcining factories.

Gray magnesium oxide contains more than 5095 MoO, in particular, more than 8095 Ma9O. Preferably, the content of CAO will be less than 195, in particular, less than 0.590, with Preferably the content of alkali metals will be less than 195, in particular, less than 0.395 in terms of oxide! similar 7p, Sa, Na, etc., at 20 will be less than 195, in particular less than 0.595.

Slick! magnesium include natural or calcined (heat-treated at a temperature of 10007C) silicate minerals, for example, olivine, serpentine, vermiculite, anthophyllite, cumingtonite, znstatite, pyrope, spinel, and similar industrial production of compounds containing Mao as the main component, which are determined below

Preferably silicate! magnesium contain more than 2595 Mo, in particular more than 4095 Ma.

GF! Preferably, the content of SAC is less than 195, in particular less than 0.595.

Preferably, the content of alkali metals is less than 190, in particular, less than 395 in terms of O per oxide!.

If the content of AI2O5z is higher than 3905, the reaction temperature in the reduction zone should be less than 60 15502 in order to avoid the formation of aluminum carbide.

Preferably, the sum of other volatile elements, for example Z and SI and metals, such as 7p, Ca, Na, etc., added is less than 195, in particular less than 0.595.

Slick! magnesium, in addition, include natural rocks consisting of more than 5095 magnesium silicates, which are defined higher, preferably more than 8095, in particular rocks consisting of more than 9095 silicates, and industrial waste rich in high-quality magnesium silicate , for example, the use of forsterite furnace lining.

In this context, the term "carbon" includes material rich in carbon, for example, anthracite, carbon black, and coke.

This material is rich in carbon! in general, they have the following composition: carbon content » 9095 ash «2 volatile component! "890

Preferably: 70 carbon content » 9695 ash content «19 volatile component! "390

Preferably: carbon content » 98.595 ash «0.595 volatile component! "190

The raw material is preferably crushed to an average particle size of less than 45 mm.

The carbon-rich material preferably has an average particle size of about 100 nm. Reactive manure is preferably introduced into the recovery zone in the form of briquettes with a porosity of about 57905.

According to the first preferred option, the starting material is mixed with carbon: - in the amount of 2.9 - Z, Zmola C/mol 5iO" plus 1.0 - 1.3mol C/mol Geo, plus 3.0 - Z 4mol C/mol Re"2O"z, plus 0.0 - 0.25 mol C/mol Mo, - preferably in the amount of 2.9 - 3.2 mol C/mol 5iO", plus 1.0 - 12 mol C/mol Reo, plus 3.0 - sch

3.2 mol C/mol Re2Oz, plus 0.0 - 0.2 mol C/mol Mao, - in particular, in the amount of 2.9 - 1 mol C/mol 5iO" plus 1.0 - 1.05 mol C/mol Reo, plus 3.0 - Z, 1 mole o

C/mol Re»Oz, plus 0.0 - O,Bmol C/mol Mao,

In accordance with the second preferred options: - the reaction temperature T is maintained in the interval 14002 - 15002С, and Mao and Md»ziO; deposited in the zone of condensation by injection of oxygen-containing gas, for example, molecular oxygen, air, CO,

SO, But and their mixtures; o - magnesium oxide is used as the starting material, containing a small amount of He, 5i, Ca, and AI oxides; - olive oil is used as a starting material; that) - when the content of AI2Oz in the initial reaction mixture is more than 195 wt., T. less than 15507; "g -"8i,Re" and metallic iron are separated from the rest in the reduction zone by traditional methods, for example, magnetic or electrostatic separation or flotation, after which A and transition elements, for example Mp, Cg, AI, and metal from the platinum group are extracted by generally accepted methods , for example, by leaching and "- Z8IS, formed in the reduction zone and the first condensation zone, are extracted as a by-product -pv) from the residue, respectively, in the reduction zone and the first condensation zone. - MadO, formed in the reduction zone and the first condensation zone, is extracted as a by-product from the residue in the reduction zone and the first condensation zone.

In the following, the invention is also described with reference to the drawings, in which: Fig. 1 shows the laboratory-scale experimental apparatus used for the experiments presented in examples 1 - 5: Fig. 2 shows the laboratory-scale experimental apparatus used for the experiments , representations in example 6; 2) Fig. 3 shows the apparatus for carbon-thermal processing of magnesium silicate minerals and rocks; Fig. 4 shows photographic images of the reacted layer of material from Example 1, obtained by "M" on a scanning electron microscope; Fig. 5 shows photographic images of magnesium columnar crystals from Example 5 obtained on a scanning electron microscope; Fig. b shows diagrams illustrating the passage of Mao (tv) from the layer of MoO, which has passed into the vapor phase, as a function of reduced pressure during carbonothermic transformation of olivine 613 at 1508 - iF) 2"s (examples 1, 4 and 8). Fig. 1 shows the laboratory-scale experimental apparatus used for the experiments presented in examples 1 - 55, which has an electrically heated chamber furnace 1, because it is designed for 1600 °C, only thermal insulation is shown, furnace chamber 2, thermocouple C for measuring furnace temperatures, a millivoltmeter 4, connection with thermocouple 3, reactor and tube 6 of the condenser, consisting of a graphite tube with a closed end, located in a tube of aluminum oxide with a closed end, having a plug b at the end of the tube 5 of the reactor, the first condensate 7 at the heated end of the tube 5 of the condenser and the second condensate 8 at the cold end of the condenser tube 5, pressure switch 9 for regulating gas pressure in the reactor and condenser tube 5, pneumatic valve 10, regulated by the pressure switch 9, dust filter 11, vacuum pump 12, gas tank 13 for collecting exhaust gas from the reactor/ condenser tubes 5, and CO monitor 14.

Fig. 2 shows the laboratory-scale experimental apparatus used for the 7/0 experiments presented in example 6, having: electrically heated furnace 1, designed for 1600 °C, for heating the reactor part/reactor condenser tube, electrically heated furnace 2, designed for 1400 "C, for heating the first part of the reactor condenser/condenser tube, electrically heated furnace C, designed for 1200"C, for heating the second part of the reactor condenser/condenser tube, thermal insulation 4, between the three elements of the furnace, the reactor and the condenser tube, consisting of graphite a tube with a closed end located inside a tube made of aluminum oxide with a closed end, having part b of the reaction chambers at the end of the tube 5 2 of the reactor, and the first part 7 of the tube 8 of the condenser, and the second part 8 of the tube 5 of the condenser, a particle filter 9 for collecting M9O-C powder formed in the second part 8 of the tube 5 of the condenser, the vacuum-tight removable cover 10, and the vacuum tube 1 1, leading to the pneumatic valve, regulated by a pressure switch, between the condenser and the vacuum pumps.

Fig. 3 shows the apparatus for the carbon-thermal processing of magnesium silicate minerals and rocks, which has a vacuum closed system 1 for loading a granulated sulfur mixture located on top of an electrically heated furnace 2, calculated at least at 1400 °C, and preferably at 18007 °C, with a graphite lining for carbon-thermal processing of the sulfur mixture, a vacuum closed system C for unloading the final layer of material from the furnace 2, with an electrically heated first condenser 4 with a temperature control system for maintaining a constant temperature in the range from 10007 to 15007"С, which has a carbon lining and containing chemically active carbon in a form suitable for the formation of ZS by interaction with "g"

The second capacitor 5 is electrically heated by the ZO component of the gas phase generated in the furnace 2 to obtain a fine powder of MadO or metallic magnesium.

To obtain a fine Mao powder, the second condenser is equipped with a temperature control system "to maintain a constant temperature!" in the range from 600" to 15007С and a filtration system for the collection of fine particles and optionally a system for the regulated introduction of oxygen-containing gas.

For the production of metallic magnesium, the second condenser is equipped with a regulation system;" temperature for maintaining a constant temperature in the range from 2007 to 6507"С and a system for collecting condensed metal.

The apparatus also has a zone of large temperature gradient b, located between the first condenser 4 and the second condenser 5. This zone can be designed in the form of a dispersing nozzle for supersonic adiabatic cooling of the vase passing from the first condenser 4 to the second condenser 5. In conclusion the apparatus has a cyclone 7 for the deposition of particles entrained by the exhaust gas from the second condenser 5, a filter 8 for fine particles, and a vacuum pump 9, which makes it possible to maintain a pressure in the range of 10 - 105Ra in the furnace 2, in the first condenser 4 and in the second condenser 5, and the vacuum closed system 10 for unloading metallic magnesium formed in the second capacitor, Fig. 4 shows photographic images of the reacted layer of the material from example 1, obtained

F, on a scanning electron microscope (methodology 1: 150672, Robshch/Rravn - 0.79; 320min). Co. A) Review (Mo 5359/01),

B) Micron size sorting of ModO and 5iC crystals together with a 5-micron "5i,Re" droplet, as a close-up view (Mo 5357/01),

Fig. 5 shows photographic images of columnar magnesium crystals from example 5, obtained on a scanning electron microscope (methodology 1: 151072, Robshch/Rravn - 0.029; 115MIN).

Crystal! Ma was formed by precipitation from the vapor phase in the coldest part of the condenser ( ; 6507С). 65 A) Review (Mo 5300/01).

C) Close-up (Mo 5299/01).

Fig. b6 shows diagrams illustrating the output of MoO (tv) from the layer, and MoO that has passed into the vapor phase, as a function of reduced pressure during carbonothermic transformed olivine 613 at 1508 -

Z"C (Example 1, 4 and 5).

In the future, the main idea of the present invention will also be explained with reference to fig.b.

Product! Reactions formed during appropriate heating of mixtures, for example, olivine (Ma»25iOd) and carbon (C) depend on the molar ratio between the reactants and the gas pressure during processing. For example, a mixture of olivine pitch (M95510O45) and carbon pitch (C) can react in accordance with reaction (1) or (1") depending on the total gas pressure. 70 (7) Ma92551iO, (tv) - ZS(tv) -» 2MaO(tv) k zis(tv) - 2СОg) (2) Ma925iO, (tv) and ZS(tv) -» 2Ma(g) - 5id(g) - ZSO g)

Ma25iO4 and Zmolami with at 1400 - 17507 " o,

Thermodynamic calculations show that reaction (1) will occur from left to right in the temperature range from 14007"С to 17507"С, if the partial pressure СО(Псо) is less than or equal to the pressure (nRa) determined by equation (a) in table A. At thermodynamic equilibrium, the simultaneous partial pressures of all the other important types of gas Ma(g), zF(g), O (g) included in the reaction are determined by equations (b), (c) and (4) in Table A. From the by means of the partial pressure of the main types of gas and the mass balance of the reactions involved, it is possible to calculate the total pressure of the gas (Prvn), the composition and amount of volatile material and the final composition of the layer for i - the equilibrium transformation of Ma »5iO); (tv) in MoO (tv) and ZiS (tv) in accordance with equation (1), while it is possible to calculate the minimum excess of added carbon necessary for the formation of an equilibrium amount of Ma (g) and ZO (g). The total equilibrium pressure of the gas Prvn multiplied in this way can be represented as follows: u (Prvn) - -17043 t i 10.705

If the total pressure of the steam (Robsch) of the existing gas phase! above the reaction mixture is higher than Pravn; the reaction will not occur.

Under equilibrium conditions (Rorsch/Rravn) 7 1, the multiple output of MOO (tv) from the layer changes from 86.495 at 14007С to 91.895 at 170070.

When the production becomes lower than P, further evaporation of the charge will occur in accordance with reaction 40. (17 and the input of MOO (tv) and 5IS (tv) into the layer will decrease. Thus, when the pressure is constantly reduced below v) with Eq reaction (1" ) becomes more and more significant compared to reaction (1). "» Experience! show that reaction (17) is the predominant one when (P obch/Pequn) 5 0.7, and that the input of MoO (tv) from the layer (reaction 1) is x 5906 when (Pobch/Pequn) 5 0.2 (fig. b ), i.e. during processing, the olive evaporates more than 9595 Ma.

It should be understood that although the nominal temperature of the furnace, which is used to calculate the Ro equation (1508 54. 27C in Fig.b) is equal to the actual temperature of the layer when (Robosch/Pequn) » 1, this case is not the case when the general pressure decreases and steam formation becomes predominant. Under these conditions, evaporation leads to the cooling of the layer to temperatures) when R is equal to the pressure of the gas at steady evaporated, or to temperatures when vapor formation decreases due to kinetic reasons (he av | 20 1400"С; example 3). At the nominal temperatures of the furnace more than 150072 and (Robsh/Pravn); t 0.1, the rate of evaporation will be largely regulated by the rate at which heat is supplied. So, in general, it is similar to what happens during sublimation processes. Under these conditions, the nominal temperature of the furnace reflects the rate of heating supply, not the temperature of the layer. Thus, a temperature equal to 15087C leads to Robsh x TkRa (Robsh/Pravn); with 0.1. Example 4, 5 and b are typical examples of what happens when the same Robushch and nominal furnace temperature in the range from 14007C to 175075.

GF) Try the following! describe the preferred option in more detail! the method invented

GF for the conversion of magnesium silicates (for example, olivine) c

A) refractory mass consisting of periclase, silicon carbide and optionally forsterite enriched with magnesium oxide; because B) the separation of metallic magnesium and silicon carbide is good;

C) magnesium oxide and silicon carbide are well separated.

The chemical composition and physical data of the sulfur used in examples 1-b are given in Table 1.

The composition and physical data of the granulated carbon-forsterite mixtures obtained from this sulfur and used in experiments are presented in Table 2. 65 Experiments! carried out in accordance with the following methods.

Methodology 1

Laboratory-scale experimental equipment used in this part of the work! for carbon-thermal transformation at temperatures between 12007 and 15007C and pressures between 0.4 - 10kRa of the briquetted sulfur mixture shown in Fig.1.

Loads of known mass were placed in a reactor/condenser, a graphite tube with a closed end, located inside an aluminum oxide tube with a closed end. Then the reactor/condenser was evacuated, filled with Ag to the desired pressure and introduced into the preheated furnace at a rate corresponding to the heating rate of about 50"C/min. To maintain a constant pressure in the reactor/condenser during the carbon-thermal reactions, a pneumatic valve was used, located in front of with a vacuum pump that regulated the pressure. Then the gas released in the process was collected and the concentration of CO was checked.

After carbon-thermal treatment, the product! reactions in the layer and various fractions, condensed from the vapor phase, were separately collected, weighed and analyzed by XKO (X-ray diffraction), TO 7/5 (thermogravimetry) and ZEM/EOzZ (scanning electron microscopy/EO5).

Methodology 2

Laboratory-scale experimental equipment used in this part of the work! for the carbon-thermal conversion at a temperature of 15102C and a pressure of 1.1 kRa of the briquetted sulfur mixture, shown in Fig.2.

Loads of known mass were placed in a reactor/condenser, a graphite tube with a closed end, located inside an aluminum oxide tube with a closed end. Then the reactor/condenser was evacuated, filled with Ag to the desired pressure and introduced into the preheated section of the furnace at a rate corresponding to a heating rate of about 502С/min. To maintain a constant pressure in the reactor/condenser during the carbon-thermal reaction, a pneumatic valve was used, located in front of the vacuum pump, which regulated the pressure. Then the gas released in the process was collected and CO concentration was boiled. at

After carbon-thermal treatment, the product! reactions in the layer and various fractions condensed from the vapor phases were separately collected, weighed and analyzed by KKO, TO and ZEM/EU5. cha zo

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A) Preparation of refractory masses consisting of perclase (Mo9O), silicon carbide (ZiS) and traces of forsterite (Mo25iO)), enriched with magnesium oxide

Example 1

In this experiment, 11.2 g of carbon-olive briquettes of mixture A (Table 2) were processed in accordance with method 1 at 15062C and a gas pressure (Robsch) of 10.4kRa for 320 minutes.

The pressure (Robsch) was set equal to 0.84 of the equilibrium gas pressure (B equal), as was calculated from thermodynamic data. The end of the reaction was determined after 320 minutes by means of a gradual decrease in the release of CO, which was determined in the entered exhaust gas. high school

Analytical data of the phase composition of the reacted layer in the precipitated products in the condenser are given in Table 3.

The reacted layer consisted of highly porous briquettes of a greenish color. Present phases! sorted by size into MoO, 5iC, droplets of "5i,ge" and insignificant remnants of Ma»ziO; (see fig. 4).

The input of Mao (TV) from the layer was 6790. They were crushed. A part of the transformed material of the layer was crushed and the "Bee" droplets were removed with a magnet. On the basis of the spatial distribution of phases and the total weight of the samples, it was established that more than 9595 wt. of the original 8.6295 wt. white iron oxides were removed in this way. co

The BEM/EOZ analysis shows that the transition element (St, Mn, Mi, and RO), which are found in the following amounts in olivine 613, is concentrated in the "5Zi,Be" droplets. The semi-quantitative analysis of EO5 M shows the average concentration in the "5i,Re" droplets : 29 oves. St, 0.39 oves. MP, Zdoves. Mi and 0.19 oves. RI. "

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Example 2.

In this experiment, 12.6 g of carbon-olive briquettes of mixture A (Table 2) were processed according to the method at a temperature of 15802C and a gas pressure (Robsch) of 31.3kRa for 260 minutes.

The pressure (Robsch) was set equal to 0.97 mm of the equilibrium pressure of the gas (R equal), as it was calculated from thermodynamic data. The end of the reaction was determined after 260 minutes by means of a gradual decrease in the introduction of CO, which was determined in the injected exhaust gas.

The reacted layer consisted of highly porous briquettes of a greenish color. Present phases! sorted by size into ModO, ZyS, "Zi,ge" droplets and insignificant remnants of Ma»5iO;. The material in the form of steam was not analyzed in detail. The output of MOO (tv) from the layer was 82,965.

Example C

In this experiment, 13.5 g of carbon-olive briquettes of mixture A (table 2) were processed in accordance with method 1 at 14052C and compressed gas (Robsch) of 3.4kRa for 180 minutes.

The pressure (Robsch) was equal to 0.97 of the equilibrium gas pressure (P equal), as was calculated from 7/0 thermodynamic data.

After 180 minutes, the experiment was stopped, despite the fact that the release of CO was still observed, which was determined in the exhaled exhaust gas.

The observed weight loss was 18.795 wt., including MoO, which was not extracted.

The reacted layer consisted of highly porous briquettes of black-green color. The 75 facies present were olivine (39905 wt), periclase (1795 wt), ZnS (1195 wt), "zi,Re" (395 wt), and carbon (1190 wt).

The Mao input (tv) from the layer was 44906, while the unreacted olivine contained about 5095 of the initial Mao content.

In addition, studies of the briquettes of mixture A (Table 8) using OTA/TO (differential thermal analysis/thermogravimetry) by Mieg showed that when a high-pressure argon flow was used to remove the gaseous products of the reaction (calculated: (Robsch - Rag) / Equation from 0, 97), at a temperature of 120090 there was very little interaction. After 120 minutes, the total weight loss was only 490 weight. and formation of periclase (ModO) was not observed.

B) Obtaining well-separated metallic magnesium (Ma) and silicon carbide (5iC) Ha

Example 4

In this experiment, 15 g of carbon-olive briquettes of mixture A (table 2) were processed in accordance with i) method 1 at 15102C and pressurized gas (Robsch) of 1.1kRa for 103 minutes.

The pressure (Robsch) was set equal to 0.079 of the equilibrium gas pressure (P equal), as was calculated from thermodynamic data. The end of the reaction was determined after 103 minutes by means of a gradual decrease in the release of CO, which was determined in the evaporated exhaust gas.

Analytical data of the phase composition of the conducting layer and precipitation products in the condenser can be found in Table 4.

The final layer of the material consisted mainly of "Zi, Be" droplets together with an insignificant amount of perclase (MoC), traces of 5IiC, however, it did not contain forsterite. at

Due to the low pressure and the molar ratio between Mao, 25 and O., and carbon equal to 1:3, most of the silicon and magnesium from olivine 613 in the sulfur mixture quickly evaporated according to the reaction:

Ma25iO, (tv) k ZS (tv) -» 2Ma (g) - BIO (g) - ZSO (g).

Silicon was again deposited in the form of 5iC in the most heated part of the condenser (1480 - 20"C) together with periclase (Mos) and a certain amount of forsterite formed by the reverse reaction.

The output of metallic magnesium, formed in the coldest part of the condenser ("650"C), was 28905 wt. Metallic magnesium contained about 4.495 wt, periclase (Mo90) as the main impurity. Example 5 » In this experiment, 9.4 g of carbon - olive oil briquettes of mixture A (table 2) were processed in accordance with method 1 at 1510"7C and a gas pressure (Working) of 0.4kRa for 115 minutes.

The pressure (Robsch) was chosen equal to 0.029 of the equilibrium pressure of the gas (P equal), as it was calculated from the thermodynamic data. The end of the reaction was determined after 115 minutes by means of a gradual decrease in the introduction of CO, which was determined in the injected exhaust gas.

Analytical data of the phase composition of the reacting layer and precipitation products in the condenser are shown in Table 5. 20 The final layer of the material consisted mainly of "5i, Re" droplets and a small amount of is.

Due to the low pressure and the molar ratio between the Ma 2505 part of olivine and carbon, "m equal to 1 : C, most of the silicon and magnesium from olivine 613 in the sulfur mixture quickly evaporated in accordance with the reaction:

Ma25iO, (tv) k ZS (tv) -» 2Ma (g) - BIO (g) - ZSO (g). 29 Silicon was redeposited, mainly in the form of Z, in the most heated part of the capacitor (13007)

GF! together with forsterite, formed by reverse reaction, a small amount of periclase (Mo) and traces of 51C. The yield of metallic magnesium formed in the coldest part of the condenser (650°C) was 74.695. Magnesium was precipitated in the form of columnar crystals (Fig. 5). Metallic magnesium contained about 4.995 wt. 60 of periclase (MoO) as the main impurity. Temperature | 00000000 69100000 65 0pressure/111111111111111111

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Example 6

What. In this experiment, 14.2 g of carbon-olive briquettes of mixture A (Table 2) were processed in accordance with method 2 at 15102C and a gas pressure (Working pressure) of 1.1kRa for 120 minutes.

The pressure (Robsch) was set equal to 0.079 of the equilibrium pressure of the gas (P equal), as it was calculated from thermodynamic data. The end of the reaction was determined after 120 minutes by means of a gradual

ГФ) reduction of CO release, which was determined in the boiled exhaust gas.

Analytical data of the phase composition of the conducting layer and precipitation products in the condenser are given in Table 6.

The final layer of material consisted of 5iC, "Zi,Re" droplets and a small amount of final carbon. 60 The single phase detected in capacitor 1, kept at 1360"С, was 51С.

The material collected from condenser P, held at 800"C, was a fine black powder consisting of periclase (MoC) and carbon (C). The carbon was removed by heating the powder to 800"C in air for 5 hours.

The resulting powder was blem, and the only phase detected by X-ray diffraction (XRD) was periclase (Mo90). The output of periclase was 9595 wt.

In the above experiments, olivine was used as the starting material. Like the result! can be obtained with other magnesium silicate minerals and gray magnesium oxide. and

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Claims (28)

The formula of the invention Go) IS) 1. The method of obtaining metallic magnesium by carbon-thermal reduction of the original material 32, selected from the group consisting of magnesium oxide, containing a small amount of oxides of Ge, 5i, Ca, and Al, natural and industrially obtained magnesium silicate minerals and their mixtures, for example, olivine, distinguished by , which mix the original material with carbon in the amount of 1-4 moles C/mol ZiO" plus 1-2 moles C/mol ReoO, plus 3 moles C/mol Re 203, plus 1-2 moles C/mol ModO, heat the mixture in recovery zone to temperatures! T, in the interval 14007-1700"С, at a pressure p, in the interval 40 0.01-1.75kRa, reduce the iron oxide component of the starting material in the reduction zone to 3 c of iron, reduce the silicon dioxide component of the starting material to 500, which is partially are converted in the reduction zone to 51iC and the alloy 5i and Re, "5i,ge", is partially evaporated from the reduction zone and converted to 5IiC, Z or M925iO, by reaction with carbon in a separate first condensation zone at a pressure of r. in the interval 0.01 -1.1 kRa at a temperature of T. more than 45 °C - up to CY Y -81315, sl giv r,-19.92 here expressed in kRa, but below T,, reduce the magnesium oxide component of the starting material in the reduction zone to gaseous metallic magnesium, vaporize gaseous metallic ("c") 50 magnesium from the reduction zone and condense gaseous metallic magnesium in a separate second condensation zone, located behind the first condensation zone, under pressure interval of 0.01-1.1 kRa, at a temperature To» less than bZVa C, and remove CO, formed by means of the above-mentioned reduction processes, from the second condensation zone and maintain the pressure po at a pre-selected value by using a pump, by means of which the temperature gradient between The first condensation zone and the second condensation zone are supported as much as possible, and also by means of what is called "r". " Mr. 2. The method of obtaining pure magnesium oxide by carbon-thermal reduction of the starting material, selected from the group consisting of magnesium oxide containing a small amount of oxides of Re, Z, Ca and Al, natural and industrially obtained magnesium silicate minerals and their mixtures, for example, olivine, distinguished by mixing the starting material with carbon in the amount of 1-4 moles C/mol ZiO" plus 1-2 moles C/mol ReO, plus 3 moles C/mol Re 203, plus 1-2 moles C/mol ModO, heating the mixture in recovery zone to temperatures! T, in the interval 14008 -1700 in C at pressure p, in the interval b5 to 1-1 di-tezet "st; katz nov) b reduce the iron oxide component of the starting material in the reaction mixture to iron, reduce the silicon dioxide component of the starting material to 510, which partially are converted in the reduction zone to 5ZiS and the alloy of Bi and Re "Bi, Ge", are partially evaporated from the reduction zone and converted to 5iS, Zi and/or Ma»5iO by reaction with carbon in a separate first condensation zone under pressurized ri, where ri. - ry at a temperature T. higher than -32217 tyu TinneS t inn ТZ, 2Io9 Р, -19.92 where ri is expressed in kRa, but below T,, reduce the magnesium oxide component of the starting material in the reduction zone, at least partially , to gaseous metallic magnesium, evaporate gaseous metallic magnesium from the 75 reduction zone and act on gaseous metallic magnesium CO, formed in the reduction zone, to MdO and C and precipitate this product! reactions in the form of cm of carbon and magnesium oxide in a separate oxidation zone and condensation zone, located behind the first condensation zone, under pressure, where ро: рі and at a temperature T" in the interval from 638 C to Tu, remove the mixture of carbon and magnesium oxide from the oxidation zone and condensation and remove carbon from the removed product, for example, by oxidation, and remove the part of CO formed by the above-mentioned reduction methods, which was not consumed during the reaction with Ma, from the zone of oxidation and condensation, and maintain the pressure po at preselected values by using a pump, by means of which re « ri « g. se C. The method of obtaining pure magnesium oxide by carbon-thermal reduction of the starting material, selected from the group consisting of magnesium oxide, containing a small amount of (o) oxides of Ee, Z, Ca, and Al, natural and industrially obtained magnesium silicate minerals and their mixtures, for example, olivine, which is distinguished by the fact that the starting material is mixed with carbon in the amount of 1-4 moles C/mol ZiO" plus 1-2 moles C/mol ReO, plus 3 moles C/mol Re 203, plus 1-2 moles C/mol ModO, heated - with the mixture in the recovery zone to the temperatures! T, in the interval 14008 -1700 in C at pressure p, in the interval (ав) . pldi-ezvist st, katzro oz Kha, c reduce the iron oxide component of the starting material in the reaction mixture to iron, and reduce the silicon dioxide component of the starting material to 510, which is partially converted into Zo in the reduction zone in 5iC and the alloy Bi and Ee "Vi,he ", partially evaporate from the reduction zone and " turn into ЗИиС, Зи and/or М92551О; by interaction with carbon in a separate first condensation zone at a pressure p,, where p: ri and a temperature T. higher than t -0Й отв, their 400 "min 2Йо9 Р, -19.92 С с where rch is expressed in kRa and below T,, :z" reduce the magnesium oxide component of the starting material, at least partially, in the reduction zone to gaseous metallic magnesium, evaporate gaseous metallic 415 magnesium from the reduction zone and act on gaseous metallic magnesium separately by adding an oxygen-containing gas, for example, air, CO" , СО, НОО and their mixtures, to magnesium oxide and precipitate magnesium oxide in a separate zone of oxidation and condensation, under pressurized water, where Рори, and at a temperature of То in the interval from 6З8ВАС to ТУ, remove magnesium oxide from the oxidation zone and condensation and, if necessary, remove carbon from the removed product by oxidation and remove gases formed by the above-mentioned reduction and oxidation processes, and maintain pressure р 2 with pre-selected values by using a pump, by means of which " " "m раз ре ре. 4. The method of obtaining a refractory material based on magnesium oxide by processing the starting material selected from the group consisting of magnesium oxide, containing a small amount of 22 oxides of Ee, Zi, Ca and Al, which are natural in industrially obtained magnesium silicate minerals and their mixtures, Ф! for example, olivine, distinguished by the fact that the starting material is mixed with carbon in the amount of 1-4 moles of C/mol of ZiO" plus 1-2 moles of C/mol of ReO, plus 3 moles of C/mol of Re 203, plus 1-2 moles of C/mol of ModO, heat the mixture in the reduction zone to temperatures! T, in the interval 1400 8 -1800 in C at pressure p, in the interval bo udi-tezvi "(Tteka?z ria oz), hole "(Tekotz ro tv) o 1 by means of which the iron oxide component of the starting material is reduced in the reaction mixture to iron , the silicon dioxide component of the starting material is, at least partially, transformed in the reaction zone into ZiC and the alloy of Zi and Re "5i,Be" the magnesium oxide component of the starting material is transformed, 65 at least partially, into magnesium oxide (periclase), removed essentially completely the transformed mixture as a final product from the reaction zone, remove CO, formed by means of the above-mentioned reduction methods, from the reaction zone and maintain the pressure p in the reaction zone at pre-selected values by using a pump and, if desired, precipitate a mixture of Ma, Ma»»5iO ;, Zi and ZiS from the gas removed from the reaction zone in a separate condensation zone located in front of the pump, at pressurized p; 5007C and extraction of precipitated material. 5. The method according to one of claims 1, 2, C or 4, characterized by the fact that carbon is preferably vibrated in the amount of 2 mol C/mol ZiO" plus Tmol C/mol Reo, plus Zmol C/mol BGe2zhOz, plus imol C/mol MOO , in particular in the amount of Zmol C/mol ZiOo plus Tmol C/mol BReO, plus Zmol C/mol BGe2»Oz, plus mol 70 C/imole ModO, preferably in the amount of 4 mol C/mol 5iO»o plus 2 mol C/mol Geo , plus 4mol C/mol Ee2O3z, plus 2mol C/mol Mao. b. The method according to one of items 1, 2, or C, characterized by the fact that the temperature T is preferably less than 150070. 7. The method according to claim 1, characterized by the fact that the pressure p is preferably 0.2-1.1, in particular 0.3-0.7kRa. 8. The method according to one of items 2 or 3, characterized by the fact that the pressure p, preferably 2-1 di-tezet "(tu ko? |) no dz) rya 9. The method according to claim 4, characterized by the fact that the temperature T is preferably less than 1700760. 10. The method according to claim 4, characterized by the fact that the pressure p is equal to 101 kRa (Tatm). 11. The method according to item 100 is characterized in that the water pressure is preferably 0.2-0.8, in particular 0.3-0.7kRa. 12. The method according to one of items 1, 2 or 3, characterized by the fact that the temperature T 4 is lower (Tuyn1007C), preferably (Tmin720C), in particular (Tumint257C). 13. The method according to claim 1, characterized by the fact that the pressure is preferably 0.2-0.8 kRa, in particular Ga 0.3-0.7 kRa. 14. The method according to claim 1, characterized by the fact that the temperature T is preferably in the range of 200-600, in particular 250-540. 15. The method according to one of items 2 or 3, characterized by the fact that the temperature To is in the interval preferably from 6507 to TT. - 50"C, in particular from 800" to 100070. rch- 16. The method according to claim 1, characterized by the fact that a large temperature gradient between the first and second condensation zones is provided by rapid cooling, which includes the introduction of gas from the first condensation zones into a dispersing nozzle operating under conditions of insufficient expansion, ejection from the mixed gas through the dispersing nozzle and creating an opportunity for the mixed gas to expand adiabatically at supersonic speed, by means of which the coefficient of expansion in the nozzle vibrates in the interval 12.5-2, in particular 12.5-6. "Her 17. The method according to one of items 71, 2 or 3, characterized by the fact that the silicon dioxide component of the starting material is converted in the reaction mixture to essentially 5iC by using added carbon in the amount of 3-dmol C/mol of ZIO 3 plus 1-2 mol C/mol BeO, plus 3-dmol C/mol Re 203, plus 1-2 moles C/mol Mao. 18. The method according to one of items 1, 2 or 3, characterized by the fact that the temperature gradient between the reduction zone and the first condensation zone is maintained as large as possible. and" 19. The method according to one of items 1, 2 or 3, characterized by the fact that magnesium oxide is used as the starting material, containing a small amount of oxides of He, 5i, Sai AI. 20. The method according to one of items 71, 2 or 3, characterized by the fact that olive oil is used as the starting material "". 21. The method according to one of items 1, 2 or 3, characterized by the fact that when the content of AI2O3 in the reaction mixture is more than 195 wt., T, less than 155070. 22, The method according to one of items 71, 2 or 3, characterized by the fact that "5i,Re" and metallic iron are separated from the residue in the reaction zone by traditional methods, for example, by magnetic or electrostatic separation or flotation, after which A!y and transition elements, for example, Mn, St, Mi and "I metal; from the platinum group, are extracted by ordinary methods, for example, by leaching. 23. The method according to one of items 1, 2 or 3, characterized by the fact that ZIIS formed in the reduction zone and the first condensation zone are extracted as a by-product from the residue in the reduction zone and the first condensation zone, respectively. 24. The method according to one of clauses 2 or 3, characterized by the fact that the temperature To is in the interval from iF) 6507 to Tu - 50, in particular from 800" to 100070. 25. The method according to one of items 2 or 3, characterized by the fact that the temperature gradient between the first condensation zone and the oxidation and condensation zone is maintained as large as possible. 26. The method according to claim 4, characterized by the fact that the starting material is mixed with carbon in the amount of 2.9-3.3 moles C/mol ZO 3 plus 1.0-1.3 moles C/mol ReO, plus 3.0-3А4 moles C /mol Re 203, plus 0.0-0.25 mol C/mol Mao, preferably in the amount of 2.9-3.2 mol C/mol 5IO 2 plus 1.0-14.2 mol C/mol Beo, plus 3, 0-3.2 mol C/mol Re2Oz, plus 0.0-0.2 mol C/mol Mo, in particular in the amount of 2.9-3 mol C/mol ZO 25 65 plus 1.0-1.05 mol C/mol Rheo, plus 3.0-3, mol C/mol Be2Oz, plus 0.0-0.15 mol C/mol MoO. 27. The method according to claim 4, characterized by the fact that the temperature of the reaction T K is maintained in the interval 14007-15007С, and in the condensation zone by injecting oxygen-containing gas, for example, molecular oxygen, air, CO», CO, NOO in their mixtures, precipitate Mo and Mo»5iO». 28. The method according to claim 4, characterized by the fact that ModO, formed in the reduction zone and the first condensation zone, is extracted as a by-product from the residue, respectively, in the reduction zone and the first condensation zone. c schi 6) i- «c) (ze) IS) « - with . and? sh» 1 (95) Ge Sho that has) 60 b5