CN1023555C - Carbothermic process for preparing titanium boride powder - Google Patents
Carbothermic process for preparing titanium boride powder Download PDFInfo
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- CN1023555C CN1023555C CN 91106628 CN91106628A CN1023555C CN 1023555 C CN1023555 C CN 1023555C CN 91106628 CN91106628 CN 91106628 CN 91106628 A CN91106628 A CN 91106628A CN 1023555 C CN1023555 C CN 1023555C
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- 239000000843 powder Substances 0.000 title claims abstract description 38
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000010936 titanium Substances 0.000 title claims abstract description 19
- 229910052719 titanium Inorganic materials 0.000 title claims abstract description 19
- 238000004519 manufacturing process Methods 0.000 title abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- 238000000034 method Methods 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000005406 washing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 230000009467 reduction Effects 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 30
- 239000010439 graphite Substances 0.000 claims description 13
- 229910002804 graphite Inorganic materials 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 9
- 239000012774 insulation material Substances 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000004321 preservation Methods 0.000 claims description 6
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 238000012856 packing Methods 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 3
- 240000003936 Plumbago auriculata Species 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052782 aluminium Inorganic materials 0.000 abstract description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 9
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 abstract description 8
- 239000004327 boric acid Substances 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 8
- 239000004408 titanium dioxide Substances 0.000 abstract description 6
- 238000005868 electrolysis reaction Methods 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 229910033181 TiB2 Inorganic materials 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 description 14
- 239000004411 aluminium Substances 0.000 description 10
- 239000000203 mixture Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000010891 electric arc Methods 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 229910052810 boron oxide Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000000428 dust Substances 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 2
- 230000001174 ascending effect Effects 0.000 description 2
- 239000000571 coke Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- MOWNZPNSYMGTMD-UHFFFAOYSA-N oxidoboron Chemical class O=[B] MOWNZPNSYMGTMD-UHFFFAOYSA-N 0.000 description 2
- 239000002006 petroleum coke Substances 0.000 description 2
- 229910052573 porcelain Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 239000002918 waste heat Substances 0.000 description 2
- XDVOLDOITVSJGL-UHFFFAOYSA-N 3,7-dihydroxy-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound O1B(O)OB2OB(O)OB1O2 XDVOLDOITVSJGL-UHFFFAOYSA-N 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000010431 corundum Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000011982 device technology Methods 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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Abstract
The carbothermic process for preparing titanium boride powder is to mix titanium dioxide powder, boric acid powder and carbon powder in certain weight ratio, to obtain TiB through reduction and chemical combination reaction in the heat insulating area of resistance furnace2(ii) a The resulting TiB2Grinding, washing and drying to obtain finished TiB product2And (3) pulverizing. The titanium boride powder prepared by the method can utilize the residual heat of corresponding equipment and process, so that the method has the advantages of low product energy consumption, equipment investment saving, simple process flow, wide raw material source and low product cost (only the residual heat of other methods)One fifth to one tenth) and the like, and has wide popularization value in the aluminum electrolysis industry and other industries.
Description
The present invention is with to produce ti-based compound relevant.
The energy is the important factor of preparation aluminium electrolytic industry development.Along with the aluminium industrial expansion, require the carbon anode/cathode of aluminium cell is done corresponding the improvement, to reduce the power consumption of electrolytic process, be one of main direction of aluminium industrial development.Adopting titanium boride powder (making coated electrode or ceramic electrode) to improve the negative electrode of aluminium cell, is to make the aluminium electrolysis process saves energy, enhance productivity, prolong bath life, reduce one of effective way that fluoride salt consumes.Yet, how to produce titanium boride powder, generally in electric arc furnace, carbon tube furnace or other induction furnace, produced both at home and abroad with hydrogen shield or in vacuum system in the past.For example, India Harihara, M. etc. are in Trans SAEST1985 20(2～3), " producing the preliminary study of titanium boride in electric arc furnace " literary composition is disclosed in P85～88.This article claims: get TiO
21 part, B
2O
30.88 0.85～1.25 part of～1.75 parts, charcoal or acetylene carbon black (above umber all by weight, down with) were handled 60 minutes in electric arc furnace, obtained to contain Ti53.70～67.13, the product of B17.12～20.32.In November, 1967, U.S. Pat 3551428 proposed a kind ofly to produce TiB with carbon tube furnace
2Production method.This method is wetting with kerosene with 100 parts of titanium oxide, 92 parts of boron oxides, 75 parts in carbon, and then it being squeezed into tape spool is 6 inches right cylinder to bore dia, in the graphite boat of packing into, in the graphite sleeve of again graphite boat being packed into.Heat the graphite sleeve from the outside, when temperature of reaction is 1850～2250 ℃, just can make TiB
2Boron oxide excessive in the product is cleaned with hot water, can obtain TiB
2Content surpasses 95% product.Such as aforesaid method, low, the disposable building equipment investment of general production efficiency is big, energy consumption is high, production cost is high, is difficult to apply in aluminium electrolytic industry.
In order to seek the titanium boride powder production method that a kind of technology is simple, output is high, cost is low, be beneficial to wide popularization and application in aluminium electrolytic industry and other industry, special proposition the present invention.
The present invention produces the technical scheme of titanium boride powder, be that titanium dioxide powder, boric acid powder and carbon dust are mixed by certain weight ratio, the retort of then material being packed into also places the heat preservation zone of high temperature resistance furnace (as graphitizing furnace) to reduce combination reaction to make TiB
2Gained TiB
2After grinding, wash, drying, just make finished product TiB
2Powder.
For in industrial wide popularization and application, in conjunction with the accompanying drawings to producing TiB
2The embodiment of powder is described further.Fig. 1 is TiB
2Powder technological process of production figure.Employed raw material is titanium dioxide powder, boric acid powder and carbon dust, and its granularity requirements is respectively TiB
2＜43 μ m, H
3BO
3＜0.35mm, C＜0.075mm.Generally can adopt industrial pure material, optionally can improve the purity of various raw materials, with corresponding raising TiB
2The purity of powder product avoids impurity such as Fe, Si, Al, Ca to be brought into by raw material, but has also increased the cost of product simultaneously.
Produce TiB
2The principal reaction of powder is:
Can be by weight, at TiO
2: H
3BO
3: C=1: 1.6～3.0: in 0.75～0.90 the scope, the weight that takes by weighing corresponding material is prepared burden, and the material after will preparing burden by norm then carries out batch mixing.Because carbothermic method is produced TiB
2The reaction of powder is the solid state reaction process basically, and three kinds of raw material thorough mixing are even, to increase contact, helps being swift in response, carries out fully, so material must mix, black and white patch or look grain must not be arranged.Batch mixing can carry out in ball mill, feeds 30 kilograms for every batch, grinds can meet the demands in 1 hour.Look the big I of ball mill and increase or reduce charge amount.As produce used in electronic industry TiB
2Powder, the ball mill that can select for use corundum or lining to mould prevents that ferro element from bringing into.
The material that the mixes retort of can directly packing into also can place baking oven to control 150～240 ℃ temperature range inner drying a few hours, reinstalls retort after making boric acid become pyroboric acid.The retort structure adopts the graphite car to make plumbago crucible with cover as shown in Figure 2, and lid and crucible joining place car respectively have screw thread, are convenient to screwing hermetic, and certain internal pressure is arranged during heating, to reduce boric acid volatilization loss.Should spread the skim carbon dust in the retort bottom before the tinning, material answers layering to smash densification in fact during tinning.Should build cover immediately behind the charged, in time weighing charge amount and perform the preparation of shove charge.
Utilize the heat of the heat preservation zone of graphitizing furnace (or other high temperature resistance furnace) or simple coke oven to reduce combination reaction.After general elder generation installs the Graphite Electrodes base, sprinkle resistance material and push away concora crush real, select 1500～2100 ℃ heat preservation zone (being good especially), become number row to place Graphite Electrodes base top heat preservation zone (as shown in Figure 3) retort of filling material with 1700～1900 ℃.Repave after retort is laid and finished and cover insulation material (mixing) by coke grain and quartz sand.Should be noted that and worked as the retort placement location not at that time, will make material too high or too low, cause material burning or level of response to form half-cooked material inadequately because of temperature of reaction.When graphitizing furnace sent electricity, controlling its initial power and be 1000～1200 kilowatts, ascending power was 100～150 kilowatt-hours, send electricity can stop to send in about 46 hours.It is synchronous to adopt this law to produce production cycle of the reduction chemical combination reaction process of titanium boride powder and graphitizing furnace.When coming out of the stove, the rake open covering hangs out retort at the insulation material on top, imbeds in the standby cold insulation material, treats that it takes out retort again when being cooled to below 200 ℃.Retort is reusable 6～10 times like this.Show through test of many times, be equipped with above-mentioned material retort graphitizing furnace and the graphitizing furnace that is unkitted retort send electric current and powertrace in full accord; Retort and the material of adorning the ordinary production of graphitizing furnace and the quality of electrode product are not had any detrimentally affect.Therefore, adopt this law to produce titanium boride powder, can utilize the waste heat of graphitizing furnace, do not need extra many power supplies.
After the retort cooling, the taking-up product of uncapping again.After selection, the part substandard products return batching.Qualified product is ground to the granularity less than 0.15mm, uses 60～100 ℃ hot wash three times again.The liquid-solid ratio of each washing is 6～8: 1, and the most handy hydrochloric acid of washing is adjusted into 4～5 with the pH value of washing lotion for the first time, helps removing superfluous boron oxide.Product after the washing toasts through filtering to send in the baking oven after doing.Baking material temperature is controlled at 140～280 ℃.Product after the oven dry is finished product TiB
2Powder.
The present invention and carbon tube furnace or electric arc oven process are produced titanium boride relatively, following advantage is arranged: (1) this law has been sought the suitable high temperature service that reacts required, utilize the waste heat of relevant device technology to produce qualified titanium boride powder, thereby saved facility investment and electric energy additive decrementation; (2) utilize the insulation material secluding air to come the protective reaction jar, do not need hydrogen, rare gas element or vacuum protection; (3) adopt the oxide compound carbothermic method, raw material sources are wide, low price; (4) quality product meets the requirement of electrolysis of aluminum or other industry, and can be adjusted according to user's needs; (5) output height, the production cost of this law production titanium boride powder are low, only are 1/5th to 1/10th of other method through adjusting workshop cost; (6) production technique is simple, and production process is easy to grasp; (7) production process is not polluted relevant device, product and environment.
Description of drawings:
Fig. 1 is a process flow sheet of producing titanium boride powder;
Fig. 2 is a retort right section synoptic diagram;
Fig. 3 is TiB
2Reduction combination reaction shove charge synoptic diagram, wherein: 1 is retort; 2 is resistance material; 3 is graphite electrode stock; 4 is insulation material; 5 is furnace wall;
Fig. 4 send electric current and powertrace measured drawing for graphitizing furnace: ordinate zou is an electric current (1 * 10
4A), power (1 * 10
3Kw); X-coordinate be electric power feeding time (hour); Dotted line is a current curve; Solid line is a powertrace;
Fig. 5 is the X-ray thing phase diffracting spectrum of titanium boride powder.
Example 1: according to technical scheme of the present invention, when implement in first factory greying workshop, get 5.40 kilograms of the titanium dioxide (＜43 μ m) of anatase titanium dioxide metallurgical grade, the industrial boric acid powder (＜0.35mm) 12.00 kilograms, petroleum coke powder (＜0.075mm) 4.65 kilograms, adopt manual batch mixing that above-mentioned three kinds of raw materials are mixed, the aluminium dish and place baking oven to toast of then it being packed into.Oven temperature slowly rises to 230 ℃, storing time 4 hours from 100 ℃.The material of oven dry is contained in two retort and places 2
#In the insulation bed of material of graphitizing furnace, send electricity until burning till synchronously with graphite electrode stock.Electric power feeding time is 50 hours, accumulative total power consumption 103380kwh, and current consumption is consistent with other heat, and the working of a furnace is normal.It is all excellent after two retort are taken out.The product that takes out in the retort behind the naturally cooling makes thick TiB through check
24.69 kilogram (carbon containing 2.42% contains oxygen 0.36%); Substandard products 0.35 kilogram (carbon containing 5.71% contains oxygen 2.78%) can be done returning charge.The thick TiB that makes
2Adopt ball mill be milled to＜0.15mm after, with 80～95 ℃ filtered water washings three times, after filter is dried with TiB
2Powder placed 200～230 ℃ baking oven dry 3 hours.Make TiB thus
24.50 kilograms in powder.Product carries out the thing identification of phases (X-ray diffraction is illustrated in Fig. 5) through the full-automatic diffractometer of the D-500 of Siemens type X-ray, distinguishes that products obtained therefrom is TiB
2, be Ti66.04% through chemical analysis product composition (wt%), B29.34%, C2.11, O0.31, Fe0.33, Si0.69, Al0.67, Ca0.28.
Example 2: adopt technical scheme of the present invention, when implement in second aluminium manufacturer greying workshop, get 13.40 kilograms of titanium dioxide powders (enamel level＜43 μ m), the industrial boric acid powder (＜0.35mm) 29.00 kilograms, petroleum coke powder (＜0.075mm) 11.40 kilograms, adopt the ball mill batch mixing, above-mentioned raw materials is divided into ball milling twice, ground 1 hour at every turn.The material of ball milling mixing is directly dressed up two jars (compactings) and placed 4
#In the insulation bed of material of graphitizing furnace, send electricity synchronously with graphite electrode stock, 1200 kilowatts of initial powers, 100～150 kilowatts of ascending powers, electric power feeding time 46 hours send electric current consistent with the graphitizing furnace that is unkitted retort with powertrace, and the working of a furnace is normal.At first taking out two retort when coming out of the stove also in time imbeds in the standby cold insulation material.Material is taken out in the cooling back, and manually selection makes thick TiB
210.82 kilogram (carbon containing 1.62% contains oxygen 0.44%), 1.56 kilograms of substandard products (carbon containing 5.98% contains oxygen 2.34%), work done in the manner of a certain author is returned batching.Thick TiB
2Through grind, sieve (＜0.15mm),, filter and driedly be placed in the baking oven (about 200 ℃ of controlled temperature) drying 3 hours with 70～100 ℃ three times (liquid-solid ratio 7: 1) of filtered water washing, claim finished product TiB
210.22 kilograms in powder is regarded as TiB through material phase analysis
2, Chemical Composition (wt%) is: Ti65.77, B29.21, C1.59O0.44, Fe0.38, Si0.67, Al0.68, Ca0.32.
Example 3: after proportioning is determined in the laboratory, take by weighing titanium dioxide (chemical pure) 200 grams, boric acid powder (chemical pure) 480 grams, activated carbon (chemical pure, granular, Beijing activated carbon factory energetically produces) 170 grams, adopt manual that three kinds of raw materials ground and mixed in porcelain mortar is even, then material is packed into porcelain dish and place baking oven to toast, temperature slowly rise to 220 ℃ from 100 ℃, and temperature-rise period amounts to 5 hours; Take out material and be respectively charged into 1
#, 2
#, 3
#, 4
#Retort, every canned material 150 grams (50 grams of surplusing are approximately expected), put into deposit in the moisture eliminator standby.Adopt horizontal carbon tube furnace, feed hydrogen shield, the reaction times is 1 hour, according to heat and temperature difference, produces corresponding TiB
2Product.Remove 4
#The jar product is formed outside the glossiness lump, and the product of all the other each jars is all more loose.Product is after being ground to 0.15mm, use 60～100 ℃ distilled water wash three times respectively, the washing liquid-solid ratio is 7: the pH value that 1(wherein washs for the first time with hydrochloric acid adjustment washing lotion is 4～4.5), filter respectively in the baking oven that is placed on 220～240 ℃ after doing and toasted 3 hours, products therefrom is taken a sample respectively and is carried out chemical analysis, the thing identification of phases and true specific gravity mensuration, and it the results are shown in table one.
After table 1 is seen literary composition
Can find out from table one, under the situation of identical proportioning, with 2
#, 3
#Retort, promptly temperature of reaction in the time of 1800 to 1900 ℃, products obtained therefrom the best.
Fig. 5 is the X-ray thing phase diffracting spectrum of titanium boride.X-coordinate (on) scale is shown, ordinate zou illustrates intergranular apart from the position; X-coordinate (descending) indicate sample position, intergranular apart from, highly, relative intensity, it is listed in table two respectively.
After table two is seen literary composition.
Table one: under differing temps, product chemical analysis and true specific gravity analytical results
Ti B C O true specific gravity
1
＃1700℃ 64.67 28.83 3.97 1.26 4.17
2
＃1800℃ 66.62 29.17 2.21 0.56 4.38
3
＃1900℃ 67.04 30.03 1.68 0.35 4.47
4
＃2100℃ 66.77 30.02 2.08 0.31 4.45
Table two: titanium boride powder X-ray thing phase diffracting spectrum data
Sequence number position intergranular is apart from height relative intensity (%)
1????26，567????3.3523????122????8.0
2????27.604????3.2286????117????7.7
3????34.140????2.6240????187????12.2
4????35.104????2.5542????72????4.7
5????44.510????2.0338????1527????100.0
6????57.025????1.6136????962????63.0
7????61.132????1.5147????254????16.6
8????68.300????1.3721????396????25.9
9????71.989????1.3106????95????6.2
10????78.705????1.2147????89????5.8
11????88.395????1.1049????181????11.9
Claims (9)
1, a kind of method of producing titanium boride powder is characterized in that adopting by weight TiO
2: H
3BO
3: C=1: 1.6～3.0: the material of 0.75～0.90 proportioning, through mixing the retort of packing into, with the material layering compacting, will cover then and the crucible screwing hermetic, place the heat preservation zone of 1500～2100 ℃ of resistance furnaces (as graphitizing furnace) to reduce combination reaction and make thick TiB
2, be finished product TiB through grinding, wash, drying again
2Powder.
2, in accordance with the method for claim 1, it is characterized in that the granularity of selected material, be respectively TiO
2＜43 μ m, H
3BO
3＜0.35mm, C＜0.075mm can select the purity of corresponding raw material for use according to the requirement of quality product.
3, in accordance with the method for claim 1, it is characterized in that raw materials used weight ratio, with TiO
2: H
3BO
3: C=1: 2.16～2.40: 0.84～0.86 proportioning is good.
4, in accordance with the method for claim 1, it is characterized in that batch mixing adopts ball milling or handwork, the material that the mixes retort of can directly packing into, or in 150～240 ℃ baking oven, toast a few hours.
5, in accordance with the method for claim 1, it is characterized in that retort adopts the graphite car to make plumbago crucible with cover, lid and crucible interface are with being threaded.
6, in accordance with the method for claim 1, it is characterized in that the retort that will fill material places graphitizing furnace top heat preservation zone, it is good selecting 1700～1900 ℃ zone.
7, in accordance with the method for claim 1, it is characterized in that retort hung out and imbed in the cold standby insulation material.
8, in accordance with the method for claim 1, it is characterized in that taking out the product of reduction combination reaction when grinding to form less than 0.15mm, filtration hot water with 60～100 ℃, by 1: 7 solid-to-liquid ratio washing three times, or after adjusting the pH value and be 4～5 filtration hot wash once with hydrochloric acid, use 60～100 ℃ twice of filtration hot wash again.
9, in accordance with the method for claim 1, it is characterized in that will washing product filter do after, place 140～280 ℃ baking oven baking 3 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91106628 CN1023555C (en) | 1991-02-05 | 1991-02-05 | Carbothermic process for preparing titanium boride powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 91106628 CN1023555C (en) | 1991-02-05 | 1991-02-05 | Carbothermic process for preparing titanium boride powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1061010A CN1061010A (en) | 1992-05-13 |
| CN1023555C true CN1023555C (en) | 1994-01-19 |
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|---|---|---|---|
| CN 91106628 Expired - Fee Related CN1023555C (en) | 1991-02-05 | 1991-02-05 | Carbothermic process for preparing titanium boride powder |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| UA97819C2 (en) * | 2006-11-01 | 2012-03-26 | Рио Тинто Алкан Интернешнл Лимитед | Metal boride precursor mixture, process for its preparation and carbon composite material, containing it |
| CN101817538A (en) * | 2010-04-16 | 2010-09-01 | 东北大学 | Method for preparing titanium boride by arc melting method |
| CN102583422B (en) * | 2012-03-07 | 2013-02-27 | 深圳市新星轻合金材料股份有限公司 | Cyclic preparation method for producing titanium boride by taking potassium-based titanium boron villiaumite mixture as intermediate raw material and synchronously producing potassium cryolite |
| CN102583421B (en) * | 2012-03-07 | 2013-01-23 | 深圳市新星轻合金材料股份有限公司 | Circulated preparation method for producing titanium boride and sodium cryolite synchronously by adopting mixture of sodium-based titanium boron villiaumite as intermediate raw material |
| CN107082435A (en) * | 2016-05-11 | 2017-08-22 | 泰丰新素材（大连）有限公司 | The preparation method of titanium boride |
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1991
- 1991-02-05 CN CN 91106628 patent/CN1023555C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1061010A (en) | 1992-05-13 |
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