CN106007724A - Method for preparing high-strength graphite and silicon carbide containing crucible for melting metal - Google Patents

28 Mar.,2024

 

The finished product that the formula of existing graphitic carbon SiClx special type crucible and technique produce is because being limited by production technology and the restriction of formula etc., causing produced product average life is 55 days, life-span is the shortest, and use and production cost constantly increase, the garbage produced also remains high, therefore, studying a kind of novel graphitic carbon SiClx special type crucible and production technology is current urgent problem, graphitic carbon SiClx special type crucible all has bigger purposes in each field of industrial chemistry.

Graphitic carbon SiClx special type crucible is mainly used in non-ferrous metals casting and Forging Technology, as recovery and the refine of noble metal, the corrosion-and high-temp-resistant product needed for plastics, pottery, glass, cement, rubber and medicine manufacture and the corrosion-resistant container needed for petro chemical industry field.

The invention has the beneficial effects as follows: the present invention uses the crucible that new crucible formula and new production technology produce, it is high temperature resistant, corrosion resistance is stronger, and the average life of crucible reaches 7-8 month, interiors of products even tissue zero defect, intensity are high, wall is relatively thin, good heat conductivity, plus appearance glazing layer and coating and repeated drying, repeatedly fire, on the one hand substantially increasing the corrosion resistance of product, on the other hand greatly reduce energy consumption, energy consumption saves about 30%.

Preferably, gas circuit blocking-up type labyrinth kiln bed described in described step (9) " drying " is specifically arranged above with insulating brick-layer at the cotton layer of sealing, in this insulating brick-layer, the insulating brick of one of insulating brick position forward and backward with it staggers setting, edge with forward and backward insulating brick staggers setting i.e. exactly, so can block gas circuit path, heat is stayed in kiln to greatest extent.

Preferably, in described step (2) " batch mixing " and described step (6) " rerolling ", the surrounding in blending bucket is respectively provided with pneumatic arch breaking apparatus, this pneumatic arch breaking apparatus is Pneumatic knocking hammer, constantly taps blending bucket, it is achieved blanking more thoroughly during blanking.

Preferably, this crucible includes major ingredient according to parts by weight: carborundum 45 parts, 25 parts of graphite, clay 27 parts, metallic silicon 3 parts;Adjuvant: wood pulp 0.25 part and glaze 0.775 part, wherein, bentonite 0.125 part, fire clay 0.05 part, 0.2 part of glass dust, feldspar powder 0.125 part, sodium carboxymethyl cellulose 0.075 part, 0.2 part of water in described glaze.

13) secondary is fired: the crucible impregnated is put into and carried out twice firing in kiln, and the firing time is 2 hours;

12) dipping: the crucible formed by a firing is sent into impregnating autoclave and carried out evacuation and pressure impregnation, evacuation, and impregnation liquid is delivered in impregnating autoclave by seal for pipe joints, dip time 45-60min;

11) once fire: the crucible of first-class glaze is sent into kiln and carried out once-firing, 28-30 hour firing time, effect is fired in order to improve, kiln inner bottom surface arranges one layer of band sealing effectiveness and gas circuit blocking-up type labyrinth kiln bed, this kiln bed bottom arranges one layer and seals cotton layer, being arranged above with one layer of heat preservation brick layer sealing cotton layer, this insulating brick-layer forms labyrinth kiln bed;

9) dry: carry out drying operation in the crucible feeding drying oven that step (8) cutting trims, dry temperature 120-150 DEG C, it is incubated 1-2 hour after drying, regulation system in air channel is set in drying oven, described air channel regulation system can the aluminium sheet of up-down adjustment be made up of several, this upper and lower adjustable aluminium sheet is arranged on two medial surface of described drying oven, and is set to air channel between each two aluminium sheet, reaches to regulate the purpose in air channel by the gap between aluminium sheet described in regulation each two;

8) cutting finishing: include Qie Gao and finishing crucible burr, cutting height is the height cutting out the crucible meeting requirement by cutting high machine, and is repaired by the burr after cutting;

7) compressing: isostatic pressing machine hopper sent into by the material of rerolling, send in isostatic pressing machine after charging, jolt ramming, evacuation, matting in a mold and suppress;

5) second batch: again transported by the material in hopper and carry out second batch to proportioning machine, adds the carborundum of remaining 50% in material during second batch, sends into batch mixer through the material of second batch and again carries out batch mixing;

4) crushing and screening: Crushing & Screening Machineries carries out precrushing, impact breaker crushes again in the material entrance of dried cake, sieve through 60 mesh sieve subsets simultaneously, material particles more than 0.25mm return to again to be circulated precrushing, more broken, sieve again, the screening material less than 0.25mm is to hopper;

2) batch mixing: after preparing raw material in batch mixer, blanking is to buffering in hopper, batch mixing is carried out in raw material in buffering hopper is promoted to blending bucket by bucket elevator again, at bucket elevator feed opening, deironing apparatus is set, and priming apparatus is set in blending bucket, adding water while stirring, amount of water is 10L/min;

1) feed proportioning: carborundum, graphite, clay, metallic silicon are respectively put in respective batch hopper by driving, PLC program automatically controls and by ratio requirement, each material is carried out blanking weighs, blanking is controlled by operated pneumatic valve, at least two LOAD CELLS is set bottom each batch hopper, material after weighing is put in batch mixer by automatic moveable carriage machine, wherein first addition is its total amount the 50% of carborundum;

Problem for above-mentioned existence, it is desirable to provide the smelting metal preparation method of high strength graphite silicon carbide crucible, the product prepared in the method is high temperature resistant, corrosion-resistant, use mission long, and energy-conservation, reduction of discharging can be accomplished during producing, environmental protection, the recycling rate of garbage is high, and resource is recycled to greatest extent.

In order to make those of ordinary skill in the art be better understood on technical scheme, below in conjunction with embodiment, technical scheme is further described.

Embodiment:The smelting metal preparation method of high strength graphite silicon carbide crucible, this crucible includes major ingredient according to parts by weight: carborundum 45 parts, 25 parts of graphite, clay 27 parts, metallic silicon 3 parts;Adjuvant: wood pulp 0.25 part and glaze 0.775 part, bentonite 0.125 part, fire clay 0.05 part, 0.2 part of glass dust, feldspar powder 0.125 part, sodium carboxymethyl cellulose 0.075 part, 0.2 part of water in described glaze.

Carborundum: be commonly called as corundum, molecular weight is 40.1, and sterling is clear crystal, industrial goods because of impure and in furvous, density is 3.06~3.2g/cm3, refractive index is 2.65, and fusing point 2700 DEG C has high rigidity, high thermal stability and semiconductive;

Graphite: for iron black, steel grey, metallic luster is opaque, fusing point 3850 DEG C, boiling point 4827 DEG C, and density is 2.25g/cm2, corrosion-resistant, it is difficult to reaction with soda acid etc., as antiwear additive and lubriation material, makes crucible, electrode, pencil-lead etc.;

Clay: main component is kaolinite, accounts for the 80-90% of total amount, next to that hydromuscovite and quartz.Also has minority with gibbsite as main component.In clay, dioxide-containing silica is 43-55%, and iron sesquioxide is 1-3.5%, and aluminium sesquioxide is 20-25%, and titanium dioxide is 0.8-1.2%;In the present invention, clay used does not contains fluoride;

Metallic silicon: belong to technical grade, silicone content is more than 97%, for the amorphous non-metal powder of pitchy, fusing point 1410 DEG C, boiling point 2355 DEG C, water insoluble, hydrochloric acid, nitric acid etc.;This project is used has good welding performance for silicon copper, and is not likely to produce spark when impacting, and has explosion prevention function, can be used for making storage tank;

Wood pulp: lignosulphonic acid magnesium 10-20%, aqueous solution 30-40%, dry 30-60%.

Sodium carboxymethyl cellulose: outward appearance is that pure strain is white or slightly yellow fibrous powder or granule, is dissolved in water, aqueous alkali, ammonia and cellulose solution, insoluble in organic solution, the colourless amorphous article of mineral oil.Can be as powerful emulsifying agent for water/oil, oil/water system, it is also possible to as thickening agent and stabilizer.

The smelting metal preparation method of high strength graphite silicon carbide crucible, comprises the following steps:

1) feed proportioning: carborundum, graphite, clay, metallic silicon are respectively put in respective batch hopper by driving, PLC program automatically controls and by ratio requirement, each material is carried out blanking weighs, blanking is controlled by operated pneumatic valve, at least two LOAD CELLS is set bottom each batch hopper, material after weighing is put in batch mixer by automatic moveable carriage machine, wherein first addition is its total amount the 50% of carborundum, during feeding intake, configuration solves bag preventer, reduces the generation of the dust that feeds intake;Adding of material feeds intake for indirect type, proportioning machine has certain dust to overflow during work, dust generation amount is 5/10000ths of dosage, special outfit vacuum cleaner carries out purified treatment, hopper upper side arranges collection QI KOU and collects the dust of the middle generation that feeds intake, processed by sack cleaner after collection, dust-collecting efficiency is 95%, and then discharged by aiutage again, owing to graphite is lighter, the batch hopper of graphite is individually prepared sack cleaner and is processed, dust-collecting efficiency is 95%, the dust collected the most directly returns to graphite storehouse, dust after airborne cleaner unit is collected adds in batch mixer again, reach the purpose of material recycle;

2) batch mixing: after preparing raw material in batch mixer, blanking is to buffering in hopper, batch mixing is carried out in raw material in buffering hopper is promoted to blending bucket by bucket elevator again, at bucket elevator feed opening, deironing apparatus is set, deironing apparatus is mainly arranged on three magnet tube at bucket elevator feed opening, by magnet tube, the ferrum in batch mixing is removed, improve the purity of batch mixing, and priming apparatus is set in blending bucket, add water while stirring, amount of water is 10L/min, batch mixing has certain dust to overflow during work, dust carries out purified treatment by vacuum cleaner, add water and material can be made quickly to lump mixing;

3) batch mixing is dried: the wet feed after batch mixing is dried in drying plant, dry temperature 120-150 DEG C, remove moisture removal, drying plant uses drying oven, drying oven uses natural gas as combustion medium, taking out natural cooling after drying completely, the material after cooling can be sent into subsequent processing and carry out crushing and screening pelletize again;

4) crushing and screening: the material of dried cake enters Crushing & Screening Machineries and carries out precrushing, impact breaker crushes again, precrushing is that the material of caking is first broken into coarse granule, impact breaker is broken again is that coarse granule is then broken into fine grained, sieve through 60 mesh sieve subsets simultaneously, material particles more than 0.25mm returns to again be circulated precrushing, crush again, sieve again, the screening material less than 0.25mm is to hopper, crushing and screening process has certain dust and overflows, purified treatment is carried out by vacuum cleaner, dust-collecting efficiency is 95%, waste gas after process is discharged by aiutage;

5) second batch: again transported by the material meeting granularity requirements in hopper and carry out second batch to proportioning machine, adds the carborundum of remaining 50% in material during second batch, sends into batch mixer through the material of second batch and again carries out batch mixing;

The present invention's is that carborundum is divided into two parts carry out dispensing, batch mixing, so ensure that dispensing, batch mixing uniform, ensure that the crucible produced has the performances such as high rigidity, high thermal stability and semiconductive, and this dispensing method for mixing of the present invention to solve dispensing batch mixing in prior art uneven, the problem that the crucible quality of production is relatively low;

6) rerolling: secondary stirring batch mixing process, blending bucket arranges the special solution liquid-adding device with viscosity, special solution is weighed by weighing bucket and adds in blending bucket, special solution adds wood pulp, the interpolation temperature of wood pulp is at 18-20 DEG C, because wood pulp has higher viscosity, it is possible to increase the mixed adhesive strength of material, enter the intensity improving crucible further, extend its service life;

7) compressing: isostatic pressing machine hopper sent into by the material of rerolling, send in isostatic pressing machine after charging, jolt ramming, evacuation, matting in a mold and suppress, the bottom of mould arranges vibrator, after mold bottom increases vibrator, that vibrates is more solid, the density be combineding with each other between material is higher, and raw material has a small amount of dust spilling during putting into mould and carries out purified treatment by vacuum cleaner;

8) cutting finishing: include Qie Gao and finishing crucible burr, cutting height is the height cutting out the crucible meeting requirement by cutting high machine, and is repaired by the burr after cutting, and the dust that the process of cutting finishing produces carries out purified treatment by vacuum cleaner;

9) dry: carrying out drying operation in the crucible feeding drying oven that step (8) cutting trims, dry temperature 120-150 DEG C, be incubated 1-2 hour after drying, this drying oven is natural gas heat-conducting oil furnace, and crucible proper alignment is in drying oven;Regulation system in air channel is set in drying oven, described air channel regulation system can the aluminium sheet of up-down adjustment be made up of several, this upper and lower adjustable aluminium sheet is arranged on two medial surface of described drying oven, and it is set to air channel between each two aluminium sheet, reach to regulate the purpose in air channel by the gap between aluminium sheet described in regulation each two, every piece of aluminium sheet two ends arrange draw-in groove, and aluminium sheet can move up and down in draw-in groove, regulation air channel size;

10) glazing: glaze adds water formulated by proportioning through bentonite, fire clay, glass dust, feldspar powder, sodium carboxymethyl cellulose, bentonite 0.125 part, fire clay 0.05 part, 0.2 part of glass dust, feldspar powder 0.125 part, sodium carboxymethyl cellulose 0.075 part, 0.2 part of water, manual brushing glazing is used during glazing, glaze charging basket produces waste water in cleaning, this waste water enters plant area's sedimentation tank and precipitates, supernatant enters development zone drainage system, precipitating sludge dries rear crush cycle and uses, environmental protection, liquid waste processing is effective;

11) once fire: the crucible of first-class glaze is sent into kiln and carried out once-firing, 28-30 hour firing time, burned crucible becomes special cermacis product, i.e. crucible, firing effect to improve, arrange one layer of band sealing effectiveness and gas circuit blocking-up type labyrinth kiln bed in kiln inner bottom surface, this kiln bed bottom arranges one layer and seals cotton layer, being arranged above with one layer of heat preservation brick layer sealing cotton layer, this insulating brick-layer forms labyrinth kiln bed;Gas circuit blocking-up type labyrinth kiln bed is specifically arranged above with insulating brick-layer at the cotton layer of sealing, in this insulating brick-layer, one of insulating brick with its before, the insulating brick of rear position staggers setting, it is exactly i.e. with front, the edge of rear insulating brick staggers setting, so can block gas circuit path, heat is stayed in kiln to greatest extent, gas circuit is blocked between every two blocks of insulating bricks, gas can not be from the gap on ground to leaking outside, can only upwards " overflow ", it is fired in heat is all concentrated on kiln, reduce the thermal loss in sintering procedure, save the energy, and improve and fire efficiency, shorten the firing time;

12) dipping: the crucible formed by a firing is sent into impregnating autoclave and carried out evacuation and pressure impregnation, 0.5MPa pressurize 30min, evacuation, and impregnation liquid is delivered in impregnating autoclave by seal for pipe joints, dip time 45-60min;

13) secondary is fired: the crucible impregnated is put into and carried out twice firing in kiln, and the firing time is 2 hours;

14) coating: the crucible surface application water paint acrylic resin water paint that twice firing is good;

15) finished product is gone out: coating carries out dry tack free after completing, warehouse-in packaging after being dried.

The novel process of the present invention has more than been shown and described; skilled person will appreciate that of the industry; the present invention is not restricted to the described embodiments; the principle that the present invention is simply described described in above-described embodiment and description; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements both fall within scope of the claimed invention, and claimed scope is defined by appending claims and equivalent thereof.

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