Classifications

• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B32/00—Carbon; Compounds thereof
  • C01B32/90—Carbides
  • C01B32/914—Carbides of single elements
  • C01B32/956—Silicon carbide
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
  • C01B32/00—Carbon; Compounds thereof
  • C01B32/90—Carbides
  • C01B32/914—Carbides of single elements
  • C01B32/956—Silicon carbide
  • C01B32/963—Preparation from compounds containing silicon
  • C01B32/97—Preparation from SiO or SiO2
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
  • C01P2006/00—Physical properties of inorganic compounds
  • C01P2006/80—Compositional purity

Definitions

• the present invention relates to a carbonaceous powder having the following particle size,
• the present invention relates to a method for producing ⁇ -type silicon carbide at a temperature of / 6 S0'C or lower by further reacting with carbon.
• ⁇ -type silicon carbide has its chemical and physical properties.
• Binders Materials ⁇ Binders, deoxidizers for metallurgy, abrasives for polishing, high temperature
• silicon carbide is produced by a gas phase reaction using a unique apparatus. Suitable raw materials for the gas phase reaction are relatively expensive, but are also hydrolyzed in air. Since it is easily produced, and the yield of ⁇ -type silicon carbide by the gas phase reaction is generally low, there is a disadvantage in the production method in that the product must be expensive.
• the average particle diameter of this method is from 3 to ⁇ im because of its relatively large particle diameter.
• the reaction rate is extremely slow in the following because of the use of the raw material of the resilient force, and an extremely high temperature above the melting point of the resilient force (about / 7/0) is required for economical production.
• an operation method that intentionally leaves unreacted silicon and carbon in the reaction product to prevent sticking of the mixture material due to silicon monoxide generated during the reaction. Must be taken, and additional operations are required to reduce the yield of ⁇ -type silicon carbide and later to remove them. I need it.
• the present invention uses the following force of the particle size, and by using / 0 to be less than 0, most of them at relatively low temperature.
• the aim is to produce type silicon carbide with high efficiency.
• Shi Li force (Si0 2) and carbon (G) whether we reactions silicon carbide (SiG) is Ru is generated is generally (1) formula, type silicon carbide Ru is produced in a temperature range of the present invention .
• Si0 2 + 30 -SiC + 200 (1)
• the main reaction in equation (1) is based on the reaction shown in equation (2).
• silicon monoxide (SiO) produced from the reaction with, reacts with the surrounding carbon to produce /? Type silicon carbide. .
• generation of ⁇ -type silicon carbide by using formulas ( 2 ) and) as the main reactions has been confirmed by the present inventors' tests.
• silicon monoxide To produce ⁇ -type silicon carbide, silicon monoxide must be obtained from the reaction system.
• the present invention provides a coal having a particle size of oim or less.
• Material powder and fine powder of Ofi or less are used as raw materials.
• a method for preparing ultrafine ⁇ -type silicon carbide is provided.
• the raw material powder of the present invention has a particle size of / 0 "m or less.
• the particle size of the silica is unreacted due to its use.
• the most preferred carbon raw material is a carbon black, which has a high reaction rate and is operationally advantageous.
• the reaction than intends follow the MiKakeue (1), subjecting the raw material of carbon and sheet re forces described above, the mixture was uniformly mixed in earthenware pots by ing and J in CZSi0 2 molar ratio in the reaction Is good. If the mole ratio deviates significantly from J, unreacted residues are included, and the grade of silicon carbide is deteriorated, which is not preferable.
• An industrial advantage is that, according to the invention, it is possible to operate at temperatures below / / crc.
• the reaction of the above mixture raw material generates carbon monoxide gas.Therefore, it is difficult to remove the mixture outside the system while keeping the inside of the equipment in a reduced E state. It is convenient for easily proceeding. Therefore, it is advantageous to carry out the reaction while evacuating the vacuum, and by adopting this method, the reaction temperature can be lowered to 00.
• the preferred temperature range is 00 ⁇ / O'C in vacuum evacuation, / 0 ⁇ in inert atmosphere. ⁇ / 0 ° C, 0 ° C, and fine ⁇ -type silicon carbide with uniform grain size can be obtained with high quality. Operating at temperatures higher than / 6S0 ° C is not advantageous because the objectives of the present invention can be achieved up to a temperature of I "0.C.
• the particles of the silicon carbide type are provided. According to the study of the present inventors, the particles of the silicon carbide type are provided.
• the practice of the present invention is to adopt a method in which silicon monoxide produced in the reaction stage of the mixture is not dissipated as much as possible from the substances involved in the reaction. It is an indispensable requirement. In order to prevent escape, it is necessary to collect gaseous silicon monoxide that has not reacted with carbon in the reactant in a temperature range where silicon monoxide condenses. is there . This is achieved by intermittently heating the mixture. In other words, the temperature distribution in the reaction tube consists of a hot part, a high temperature part, and a low temperature part.
• the direction of movement of silicon monoxide can be adjusted by the direction of vacuum evacuation and the direction of airflow in the atmosphere.
• it is effective to guide the reaction product in the direction of removal.
• a specific example is shown by the method using the screw conveyor shown in FIG.
• the inside of the device is evacuated and the outside of the mixture is fed into the reaction tube J, which is heated by the heating element 2 on the outside, from the raw material supply port to the screw conveyor. It is supplied more continuously.
• the gaseous silicon monoxide generated by the reaction of the raw material moves from the hot zone to the hot zone, where it reacts with the residual carbon to form ⁇ -type silicon carbide.
• the unreacted silicon monoxide moves in the direction of the vacuum exhaust, condenses in the hot zone located thereabove, is collected in the reaction product, and is recovered from the product recovery port. .
• the mixture is stirred and mixed by a conveyor, and operations such as pulverization are performed.
• the generated silicon carbide is separated from the surface of the carbon particles, and the carbon particles are separated.
• FIG. 1 is a schematic diagram of an apparatus for performing the method of the present invention.
• the evacuation direction was the direction in which the reaction products were removed.
• the mixture When flowing argon gas, the mixture was allowed to flow from the inlet ⁇ to the outlet side. Regardless of whether the reaction tube was vertical or horizontal, no significant difference was found in the composition of the reaction product.
• the test results are shown in Table ⁇ 2.
• the yield of ⁇ -SiC is J or less, which indicates that the yield of ⁇ -SiC is lower than that of the present invention.
• the reaction product is produced when the raw material mixture is reacted in a powdered state, and when the mixture is reacted as a molded product having a size of 2 to dew by adding about% of a phenol resin. No significant difference was found in the composition of the product. However, the molded body was able to prevent the powder from scattering, and was easy to handle in all steps.
• the silica component is indicated as SiOx because it contains silicon monoxide.
• Example 1 The reaction product obtained in Example 1 was remixed with a ball mill, pulverized, and then passed through the reaction tube again under the same heating conditions. The number of times these operations were repeated and the composition of the recovered reaction product are shown in Table 2 in comparison with the results of Example 1.
• the quality of ⁇ -type silicon carbide is significantly improved. Thus, the effect of the method of the present invention is remarkably exhibited.
• composition of reaction product (% by weight)
• composition of reaction product (% by weight)
• the mixture was sent through a small hole.
• a rotor with the same face is attached to the mixture inlet side of the disc, and the same port is used to roll the reactant after passing through the small hole. It is loaded in close contact with the disc.
• the mixture is transported through the reaction tube by the screw conveyor, but the mixing and pulverization operations are added by this equipment.
• the position of the reaction product type silicon carbide was remarkably improved.
• Table J summarizes the test results obtained by using this device and operating under the same conditions as ⁇ / in Table /. These results are not substantially different from the results of Example 2.
• the obtained ⁇ -type silicon carbide has a reaction temperature around 0-0 brub ⁇ O. OS- ⁇ , at around / 600'C.
• the raw material having the particle size described in Example 1 was used as a molding aid, and 2 to 2% of a liquid phenol resin was added, and the mixture was formed into aggregates having a size of from 2 to dragon. . Even when pitch was used as a molding aid, there was almost no difference in the test results, but in any case, the carbonization rate of these molding aids was measured in advance, and G / S i0. It was made to be J in molar ratio.
• the silicon carbide produced by the method of the present invention is used as a filler for refractories, a binder, a deoxidizer for metallurgy, an abrasive for polishing, and an abrasive for high temperatures.
• the demand for pigments and raw materials for sintering is wide.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Inorganic Chemistry (AREA)
• Carbon And Carbon Compounds (AREA)

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• 1979
  • 1979-12-14 JP JP16164179A patent/JPS5684310A/ja active Pending
• 1980
  • 1980-12-12 US US06/293,218 patent/US4368181A/en not_active Expired - Lifetime
  • 1980-12-12 DE DE19803050136 patent/DE3050136C2/de not_active Expired
  • 1980-12-12 GB GB8123775A patent/GB2076385B/en not_active Expired
  • 1980-12-12 WO PCT/JP1980/000305 patent/WO1981001699A1/ja not_active Ceased

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