CN105540591A - Method for preparing multi-variety boron carbide micro-powder - Google Patents
Method for preparing multi-variety boron carbide micro-powder Download PDFInfo
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Abstract
The invention provides a method for preparing multi-variety boron carbide micro-powder. The method comprises the following steps: conducting primary or secondary grinding on a boron carbide material, and conducting classifying, drying and screening steps to prepare multiple varieties of boron carbide micro-powder with different granularities. In the method, a heterogeneous medium is not introduced in the grinding process, generation of massive impurities in production by a conventional ball-mill method can be avoided, and a pickling or rinsing process in the later period is not required, so that massive water resource and energy consumption can be saved, production cost can be reduced, environmental pollution is avoided, and environmental protection is benefited; and a two-stage grinding mode is adopted, so that the phenomena of over-ground raw material and big granularity width in a conventional ball-mill method can be avoided, and the product yield can be improved. Furthermore, the method is simple in flow, short in production cycle and high in production efficiency, so that the production cost can be remarkably reduced. The method has the advantages of simple and feasible process, short production cycle, high product yield, low processing cost, environmental friendliness, water resource saving and the like.
Description
Technical field
The invention belongs to the crushing technology field of superhard material, particularly the preparation method of multi items boron carbide micro powder.
Background technology
Norbide has that hardness high (Mohs' hardness 9.36), wear resistance are good, the low (2.52g/cm of density
3) and the excellent specific property such as fusing point high (2450 DEG C), be widely used in the fields such as mechanical mill, refractory materials, engineering ceramics, nuclear industry and military affairs.Boron carbide micro powder has that specific surface area is large, chemically reactive is high, response capacity is strong, fusing point and the excellent specific property such as sintering temperature is low, and above-mentioned excellent specific property makes it be widely used in the fields such as fine ceramics, powder metallurgy, electronic technology and matrix material.Such as, when using norbide super-fine powder preparation engineering pottery, at a lower temperature, sinter in the short period, the sintered compact of finer and close finer structures can be obtained.
Due to the hardness of norbide very high (being only second to diamond and cubic boron nitride), its micro mist be processed into current technical barrier.Its main machining method is comminution by gas stream and general milling method at present.
The method that comminution by gas stream drives material to collide with each other by high velocity air obtains boron carbide micro powder.Although comminution by gas stream can obtain boron carbide micro powder, and it is few to bring impurity into, also exist that energy consumption is high, output capacity is low and amount of waste large, cause production cost expensive, raw material availability is lower.
The main method of current scale operation boron carbide micro powder is be still general milling method.Its main technique is: norbide block material → ball mill crushing → pickling impurity removal → filter press → hydraulic classification → drying and dehydrating → finished product.General milling method has the advantages such as output is high, technique is simple, but also there is the production cycle long (being generally 18 ~ 30 days), product yield ratio low (30 ~ 40%), energy consumption is high, impurity (mainly Fe) content is high, especially also need to carry out pickling impurity removal, water washing cleaning, cause the waste of water resources and the pollution of environment.
It can thus be appreciated that the production technique of comminution by gas stream and general milling method all exists that boron carbide raw material utilization ratio is on the low side, energy consumption is higher, output capacity is lower, the deficiency such as the waste of water resources and the pollution of environment.
Summary of the invention
The present invention is directed to the deficiency existed in current boron carbide micro powder production technique, propose the preparation method of multi items boron carbide micro powder.Production method of the present invention is: after boron carbide raw material is carried out one-level or two grade pulverization by vertical high energy outer circulation pulverizer or high energy autogenous mill, multiple varigrained boron carbide micro powder can be obtained, as refractory materials, hot pressed sintering material, granularity sand and abrasive substance again through classification, dry screening.
One of preparation method of multi items boron carbide micro powder of the present invention, carries out according to the following steps:
Step 1, in mass ratio, norbide material: deionized water: dispersion agent=1:(0.3 ~ 2): (0.0 ~ 0.5), carry out one-level pulverizing, obtain D
50=3 ~ 12 μm of first level flour broken materials;
Step 2, squeezes into first level flour broken material in swirler and carries out cyclonic separation, obtains granularity and is less than the underflow coarse fodder that the overflow fines of 15 μm and granularity are more than or equal to 15 μm;
Step 3, the process of underflow coarse fodder:
(1) underflow coarse fodder is carried out two grade pulverization, obtaining granularity is D
50the two grade pulverization material of=2.5 ~ 5 μm;
(2) two grade pulverization material is carried out sedimentation wet concentration, the mass concentration controlling norbide in wet concentration slip is 15 ~ 30%, and wet concentration temperature is 20 ~ 40 DEG C, and the settling time is 4 ~ 12h, selects norbide wet concentration coarse fodder and granularity is D
50the norbide finished product wet feed of=2 ~ 5 μm;
(3) by norbide finished product wet feed, dry screening, obtaining granularity is D
50the norbide hot pressed sintering material of=2 ~ 5 μm;
(4) by norbide wet concentration coarse fodder, D is crushed to
50=2 ~ 5 μm, the two grade pulverization Matter Transfer as step 3 (1) utilizes;
Step 4, the process of overflow fines:
After overflow fines being carried out drying, ultrasonic screening, obtain the norbide refractory materials that granularity is less than 15 μm; Wherein, drying mode is spraying dry: spray drying ability is 80 ~ 200kg/h, drying temperature 150 ~ 300 DEG C.
The preparation method two of multi items boron carbide micro powder of the present invention, carries out according to the following steps:
Step 1, in mass ratio, norbide material: deionized water: dispersion agent=1:(0.3 ~ 2): (0.0 ~ 0.5), pulverize and obtain the comminuting matter that granularity is 150 ~ 600 μm;
Step 2, squeezes into whizzer by comminuting matter, and under centrifugal rotational speed is 2000 ~ 8000r/min, centrifugation, obtains the finished product wet feed slurry that coarse fodder is starched and granularity is less than 400 μm that granularity is more than or equal to 400 μm;
Step 3, is broken to granularity by coarse fodder starch and is less than 400 μm, as the comminuting matter recycle of step 1;
Step 4, by dry for finished product wet feed slurry, screening, obtains the norbide granularity sand that granularity is 150 ~ 400 μm; Drying mode is microwave drying: microwave frequency is 500 ~ 2000MHz, and power is 20 ~ 35kW, and drying power is 80 ~ 200kg/h.
The preparation method three of multi items boron carbide micro powder of the present invention, carries out according to the following steps:
Step 1, in mass ratio, norbide material: deionized water: dispersion agent=1:(0.3 ~ 2): (0.0 ~ 0.5), pulverize, obtain the comminuting matter that basic grain is 1 ~ 20 μm;
Step 2, squeezes into comminuting matter in swirler and carries out cyclonic separation, obtains granularity and is less than the underflow coarse fodder that the overflow fines of 16 μm and granularity are more than or equal to 16 μm;
Step 3, by norbide underflow coarse fodder, being crushed to granularity is 1 ~ 20 μm, as the comminuting matter recycle of step 1;
Step 4, carries out sedimentation wet concentration by overflow fines, and the weight concentration controlling wet concentration slip is 15 ~ 30%, and wet concentration temperature is 20 ~ 40 DEG C, and the settling time is 4 ~ 12h, selects norbide wet concentration coarse fodder and granularity is 1.5 ~ 10 μm of norbide finished product wet feeds;
Step 5, by norbide wet concentration coarse fodder, being crushed to granularity is 1 ~ 20 μm, as the comminuting matter recycle of step 1;
Step 6, by norbide finished product wet feed drying screening, obtains norbide abrasive substance; Wherein, dry mode is infrared forced air drying, and drying conditions is: drying temperature is 60 ~ 100 DEG C, and drying power is 80 ~ 200kg/h, and time of drying is 6 ~ 12h.
In aforesaid method one, method two or method three, pulverizing the equipment adopted is vertical high energy outer circulation pulverizer or high energy autogenous mill, both technical parameters are: stirring rake or adopt abrasive rubber and/or polyurethane material from mill and liner, and the rotating speed of pulverization cylinder is 400 ~ 800r/min; The rotating speed of circulating barrel is 200 ~ 400r/min, and grinding time is 5 ~ 30h; Pulverizing the dispersion agent adopted is KS5040, PVP-K90 or PEG.
In aforesaid method one, method two or method three, the described norbide material adding vertical high energy outer circulation pulverizer or high energy autogenous mill, be made up of any two sections or whole three sections in varigrained three sections of materials, granularity is 2 ~ 1000 μm, 500 ~ 5000 μm respectively, 1000 ~ 10000 μm, the purity of norbide material is all greater than 90%.
The norbide abrasive substance obtained in aforesaid method three is: the W5 that the W3.5 that basic grain is 1.5 ~ 3.5 μm, basic grain are 3.5 ~ 5 μm, the basic grain one that to be the W7 of 5 ~ 7 μm or basic grain be in the W10 of 7 ~ 10 μm.
The yield rate of the norbide product described in aforesaid method one, method two or method three is 50 ~ 95% according to weight percent.
The beneficial effect of the preparation method of multi items boron carbide micro powder of the present invention is:
1, in the present invention, have employed vertical high energy outer circulation pulverizer or high energy autogenous mill, do not introduce foreign peoples's medium, avoid during general milling method is produced a large amount of impurity (mainly Fe) produced, without the need to carrying out pickling and the washing step in later stage again, saving a large amount of water resourcess and energy consumption, having reduced production cost, it also avoid environmental pollution simultaneously, be conducive to protection of the environment;
2, in the present invention, have employed the grinding mode of two-stage series connection in method one, pulverizing crossed by the raw material produced when avoiding general milling, the phenomenon that particle size bands is wider, substantially increases the yield rate (70 ~ 95%) of product;
3, in the present invention, direct wet concentration finished product during classification of sedimentation, significantly shorten the production cycle (2 ~ 5 days), substantially increases production efficiency, reduces production cost.
4, in the present invention, multiple varigrained boron carbide micro powder is obtained by adjustment grinding time and breaking method, as: norbide refractory materials (3 ~ 15 μm), norbide hot pressed sintering material (D50=2 ~ 5 μm), norbide granularity sand (150 ~ 400 μm), norbide abrasive substance, as W3.5 (basic grain is 1.5 ~ 3.5 μm), W5 (basic grain is 3.5 ~ 5 μm), W7 (basic grain is 5 ~ 7 μm), W10 (basic grain is 7 ~ 10 μm).
Accompanying drawing explanation
Fig. 1 is the schema of the preparation method one of multi items boron carbide micro powder of the present invention;
Fig. 2 is the schema of the preparation method two of multi items boron carbide micro powder of the present invention;
Fig. 3 is the schema of the preparation method three of multi items boron carbide micro powder of the present invention.
Embodiment
Embodiment 1
The preparation method of multi items boron carbide micro powder, employing method one, pulverizing the equipment adopted is vertical high energy outer circulation pulverizer, and its technical parameter is: stirring rake and liner adopt abrasive rubber and polyurethane material, and the rotating speed of pulverization cylinder is 400r/min; The rotating speed of circulating barrel is 200r/min, and grinding time is 30h; Carry out according to the following steps:
Step 1, in mass ratio, norbide material: deionized water=1:1, carries out one-level pulverizing, obtains D
50=3 ~ 8 μm of first level flour broken materials; Wherein, norbide material is made up of varigrained two sections of materials, and the granularity of these two sections of norbides is 2 ~ 1000 μm, 500 ~ 5000 μm respectively, and norbide feed purity is all greater than 90%;
Step 2, squeezes into first level flour broken material in swirler and is separated, and to obtain granularity be the overflow fines of 3 ~ 15 μm and granularity is D
97the underflow coarse fodder of=15 ~ 4000 μm;
Step 3, the process of underflow coarse fodder:
(1) underflow coarse fodder is carried out two grade pulverization, obtaining granularity is D
50the two grade pulverization material of=2.5 ~ 5 μm;
(2) two grade pulverization material is carried out sedimentation wet concentration, the mass concentration controlling the norbide in wet concentration slip is 15%, and wet concentration temperature is 40 DEG C, and the settling time is 4h, selects norbide wet concentration coarse fodder and granularity is D
50the norbide finished product wet feed of=2 ~ 5 μm;
(3) by norbide finished product wet feed, dry screening, obtaining granularity is D
50the norbide hot pressed sintering material of=2 ~ 5 μm;
(4) by norbide wet concentration coarse fodder, D is crushed to
50=2 ~ 5 μm, the two grade pulverization Matter Transfer as step 3 (1) utilizes;
Step 4, the process of overflow fines:
After the drying of overflow fines, ultrasonic screening, obtain the norbide refractory materials that granularity is less than 15 μm; Wherein, drying mode is spraying dry: spray drying ability is 80kg/h, drying temperature 150 DEG C.
The schema of the preparation method of the multi items boron carbide micro powder of the present embodiment as shown in Figure 1.
The norbide refractory materials of the present embodiment and total yield rate of norbide hot pressed sintering material are 70%.
Embodiment 2
The preparation method of multi items boron carbide micro powder, employing method one, pulverizing the equipment adopted is high energy autogenous mill, and its technical parameter is: adopt abrasive rubber from mill and liner, the rotating speed of pulverization cylinder is 650r/min; The rotating speed of circulating barrel is 300r/min, and grinding time is 20h, and dispersion agent is PVP-K90; Carry out according to the following steps:
Step 1, in mass ratio, norbide fill material: deionized water: dispersion agent=1:0.3:0.5, carries out one-level pulverizing, obtains D
50the first level flour broken material of=8 ~ 200 μm; Wherein, norbide material is made up of varigrained two sections of materials, and the granularity of these two sections of norbides is 2 ~ 1000 μm, 1000 ~ 10000 μm respectively, and its purity is all greater than 90%;
Step 2, squeezes into first level flour broken material in swirler and is separated, and to obtain granularity be the overflow fines of 3 ~ 15 μm and granularity is D
97the underflow coarse fodder of=15 ~ 4000 μm;
Step 3, the process of underflow coarse fodder:
(1) underflow coarse fodder is carried out two grade pulverization, obtaining granularity is D
50the two grade pulverization material of=2.5 ~ 5 μm;
(2) two grade pulverization material is carried out sedimentation wet concentration, the mass concentration controlling the norbide in wet concentration slip is 30%, and wet concentration temperature is 20 DEG C, and the settling time is 12h, selects norbide wet concentration coarse fodder and granularity is D
50the norbide finished product wet feed of=2 ~ 5 μm;
(3) by norbide finished product wet feed, dry screening, obtaining granularity is D
50the norbide hot pressed sintering material of=2 ~ 5 μm;
(4) by norbide wet concentration coarse fodder, D is crushed to
50=2 ~ 5 μm, the two grade pulverization Matter Transfer as step 3 (1) utilizes;
Step 4, the process of overflow fines:
After the drying of overflow fines, ultrasonic screening, obtain the norbide refractory materials that granularity is less than 15 μm; Wherein, drying mode is spraying dry: spray drying ability is 200kg/h, drying temperature 300 DEG C.
The schema of the preparation method of the multi items boron carbide micro powder of the present embodiment as shown in Figure 1.
The norbide refractory materials of the present embodiment and total yield rate of norbide hot pressed sintering material are 75%.
Embodiment 3
The preparation method of multi items boron carbide micro powder, employing method one, pulverizing the equipment adopted is vertical high energy outer circulation pulverizer, and its technical parameter is: stirring rake and liner adopt polyurethane material, and the rotating speed of pulverization cylinder is 800r/min; The rotating speed of circulating barrel is 400r/min, and grinding time is 5h, and dispersion agent is PEG; Carry out according to the following steps:
Step 1, in mass ratio, norbide fill material: deionized water: dispersion agent=1:2:0.1, carries out one-level pulverizing, obtains D
50the first level flour broken material of=200 ~ 4000 μm; Wherein, norbide material is made up of varigrained three sections of materials, and the granularity of these three sections of norbides is 2 ~ 1000 μm, 500 ~ 5000 μm respectively, and 1000 ~ 10000 μm, its purity is all greater than 90%;
Step 2, squeezes into first level flour broken material in swirler and is separated, and to obtain granularity be the overflow fines of 3 ~ 15 μm and granularity is D
97the underflow coarse fodder of=15 ~ 4000 μm;
Step 3, the process of underflow coarse fodder:
(1) underflow coarse fodder is carried out two grade pulverization, obtaining granularity is D
50the two grade pulverization material of=2.5 ~ 5 μm;
(2) two grade pulverization material is carried out sedimentation wet concentration, the mass concentration controlling the norbide in wet concentration slip is 20%, and wet concentration temperature is 30 DEG C, and the settling time is 8h, selects norbide wet concentration coarse fodder and granularity is D
50the norbide finished product wet feed of=2 ~ 5 μm;
(3) by norbide finished product wet feed, dry screening, obtaining granularity is D
50the norbide hot pressed sintering material of=2 ~ 5 μm;
(4) by norbide wet concentration coarse fodder, D is crushed to
50=2 ~ 5 μm, the two grade pulverization Matter Transfer as step 3 (1) utilizes;
Step 4, the process of overflow fines:
After the drying of overflow fines, ultrasonic screening, obtain the norbide refractory materials that granularity is less than 15 μm; Wherein, drying mode is spraying dry: spray drying ability is 120kg/h, drying temperature 220 DEG C.
The schema of the preparation method of the multi items boron carbide micro powder of the present embodiment as shown in Figure 1.
The norbide refractory materials of the present embodiment and total yield rate of norbide hot pressed sintering material are 78%.
Embodiment 4
The preparation method of multi items boron carbide micro powder, adopts method two, and pulverizing the equipment adopted is high energy autogenous mill, and its technical parameter is: stirring rake and liner adopt abrasive rubber and polyurethane material, and the rotating speed of pulverization cylinder is 550r/min; The rotating speed of circulating barrel is 250r/min, and grinding time is 22h, and dispersion agent is KS5040; Carry out according to the following steps:
Step 1, in mass ratio, boron carbide raw material: deionized water: dispersion agent=1:2:0.5, pulverizes, obtains the comminuting matter that granularity is 150 ~ 500 μm; Wherein, norbide material is made up of varigrained two sections of materials, and the granularity of these two sections of norbides is 500 ~ 5000 μm respectively, and 1000 ~ 10000 μm, its purity is all greater than 90%;
Step 2, squeezes into whizzer by comminuting matter, and under centrifugal rotational speed is 2000r/min, centrifugation, obtains granularity D
97the coarse fodder slurry of=360 ~ 600 μm and granularity are the finished product wet feed slurry of 150 ~ 360 μm;
Step 3, is broken to granularity by coarse fodder starch and is less than 400 μm, as the comminuting matter recycle of step 1;
Step 4, finished product wet feed is dry, screening, obtains the norbide granularity sand that granularity is 150 ~ 400 μm; Drying mode is microwave drying: the microwave frequency of microwave drying is 500MHz, and power is 20kW, and drying power is 80kg/h.
The schema of the preparation method of the multi items boron carbide micro powder of the present embodiment as shown in Figure 2.
The yield rate of the norbide granularity sand of the present embodiment is 95%.
Embodiment 5
The preparation method of multi items boron carbide micro powder, adopts method two, and pulverizing the equipment adopted is high energy autogenous mill, and its technical parameter is: adopt polyurethane material from mill and liner, the rotating speed of pulverization cylinder is 800r/min; The rotating speed of circulating barrel is 400r/min, and grinding time is 5h, and dispersion agent is PEG; Carry out according to the following steps:
Step 1, in mass ratio, boron carbide raw material: deionized water: dispersion agent=1:1.2:0.4, pulverizes, obtains the comminuting matter that granularity is 200 ~ 600 μm; Wherein, norbide material forms by varigrained two sections, and the granularity of these two sections of norbides is 50 ~ 1000 μm, 1000 ~ 10000 μm respectively, and its purity is all greater than 90%;
Step 2, squeezes into whizzer by comminuting matter, and under centrifugal rotational speed is 8000r/min, centrifugation, obtains granularity D
97the coarse fodder slurry of=400 ~ 600 μm and granularity are the finished product wet feed slurry of 200 ~ 400 μm;
Step 3, is broken to granularity by coarse fodder starch and is less than 400 μm, as the comminuting matter recycle of step 1;
Step 4, finished product wet feed is dry, screening, obtains the norbide granularity sand that granularity is 200 ~ 400 μm; Drying mode is microwave drying: the microwave frequency of microwave drying is 2000MHz, and power is 35kW, drying power 200kg/h.
The schema of the preparation method of the multi items boron carbide micro powder of the present embodiment as shown in Figure 2.
The yield rate of the norbide granularity sand of the present embodiment is 90%.
Embodiment 6
The preparation method of multi items boron carbide micro powder, adopts method two, and pulverizing the equipment adopted is vertical high energy outer circulation pulverizer, and its technical parameter is: adopt abrasive rubber from mill and liner, the rotating speed of pulverization cylinder is 400r/min; The rotating speed of circulating barrel is 250r/min, and grinding time is 16h; Carry out according to the following steps:
Step 1, in mass ratio, boron carbide raw material: deionized water=1:0.3, pulverizes, obtains the comminuting matter that granularity is 250 ~ 500 μm; Wherein, norbide material forms by varigrained three sections of materials, and the granularity of these three sections of norbides is 2 ~ 400 μm, 500 ~ 800 μm respectively, and 1000 ~ 8000 μm, its purity is all greater than 90%;
Step 2, squeezes into whizzer by comminuting matter, and under centrifugal rotational speed is 5000r/min, centrifugation, obtains granularity D
97the coarse fodder slurry of=360 ~ 500 μm and granularity are the finished product wet feed slurry of 150 ~ 360 μm;
Step 3, is broken to granularity by coarse fodder starch and is less than 400 μm, as the comminuting matter recycle of step 1;
Step 4, finished product wet feed is dry, screening, obtains the norbide granularity sand that granularity is 150 ~ 360 μm; Drying mode is microwave drying: the microwave frequency of microwave drying is 1200MHZ, and power is 28kW, and drying power is 150kg/h.
The schema of the preparation method of the multi items boron carbide micro powder of the present embodiment as shown in Figure 2.
The yield rate of the norbide granularity sand of the present embodiment is 92%.
Embodiment 7
The preparation method of multi items boron carbide micro powder, employing method three, pulverizing the equipment adopted is high energy autogenous mill, and its technical parameter is: stirring rake and liner adopt polyurethane material, and the rotating speed of pulverization cylinder is 800r/min; The rotating speed of circulating barrel is 400r/min, and grinding time is 5h, and dispersion agent is KS5040; Carry out according to the following steps:
Step 1, in mass ratio, boron carbide raw material: deionized water: dispersion agent=1:1.6:0.25, pulverizes, obtains the comminuting matter that basic grain is 1 ~ 6 μm; Wherein, norbide material is made up of varigrained two sections of materials, and the granularity of these two sections of norbides is 2 ~ 600 μm, 2000 ~ 5000 μm respectively, and its purity is all greater than 90%;
Step 2, squeezes into comminuting matter in swirler and carries out cyclonic separation, obtains granularity and is less than the underflow coarse fodder that the overflow fines of 4 μm and granularity are more than or equal to 4 μm;
Step 3, by norbide underflow coarse fodder, being crushed to granularity is 1 ~ 20 μm, as the comminuting matter recycle of step 1;
Step 4, carries out sedimentation wet concentration by overflow fines, and the weight concentration controlling wet concentration slip is 15%, and wet concentration temperature is 20 DEG C, and the settling time is 12h, selects norbide wet concentration coarse fodder and basic grain is 1.5 ~ 3.5 μm of norbide finished product wet feeds;
Step 5, by norbide wet concentration coarse fodder, being crushed to granularity is 1 ~ 20 μm, as the comminuting matter recycle of step 1;
Step 6, by norbide finished product wet feed drying screening, obtains norbide abrasive substance W3.5; Wherein, dry mode is infrared forced air drying, and drying conditions is: drying temperature is 60 DEG C, and drying power is 80kg/h, and time of drying is 12h.
The schema of the preparation method of the multi items boron carbide micro powder of the present embodiment as shown in Figure 3.
The yield rate of the norbide abrasive substance W3.5 of the present embodiment is 72%.
Embodiment 8
The preparation method of multi items boron carbide micro powder, employing method three, pulverizing the equipment adopted is vertical high energy outer circulation pulverizer, and its technical parameter is: adopt abrasive rubber and polyurethane material from mill and liner, the rotating speed of pulverization cylinder is 400r/min; The rotating speed of circulating barrel is 200r/min, and grinding time is 30h, and dispersion agent is PVP-K90; Carry out according to the following steps:
Step 1, in mass ratio, boron carbide raw material: deionized water: dispersion agent=1:1.2:0.15, pulverizes, obtains the comminuting matter that basic grain is 4 ~ 8 μm; Wherein, norbide material is made up of varigrained two sections of materials, and the granularity of these two sections of norbides is 2 ~ 100 μm, 1000 ~ 5000 μm respectively, and its purity is all greater than 90%;
Step 2, squeezes into comminuting matter in swirler and carries out cyclonic separation, obtains granularity and is less than the underflow coarse fodder that the overflow fines of 6 μm and granularity are more than or equal to 6 μm;
Step 3, by norbide underflow coarse fodder, being crushed to granularity is 1 ~ 20 μm, as the comminuting matter recycle of step 1;
Step 4, carries out sedimentation wet concentration by overflow fines, and the weight concentration controlling wet concentration slip is 30%, and wet concentration temperature is 40 DEG C, and the settling time is 6h, selects norbide wet concentration coarse fodder and basic grain is 3.5 ~ 5 μm of norbide finished product wet feeds;
Step 5, by norbide wet concentration coarse fodder, being crushed to granularity is 1 ~ 20 μm, as the comminuting matter recycle of step 1;
Step 6, by norbide finished product wet feed drying screening, obtains norbide abrasive substance W5; Wherein, dry mode is infrared forced air drying, and drying conditions is: drying temperature is 100 DEG C, and drying power is 200kg/h, and time of drying is 6h.
The schema of the preparation method of the multi items boron carbide micro powder of the present embodiment as shown in Figure 3.
The yield rate of the norbide abrasive substance W5 of the present embodiment is 80%.
Embodiment 9
The preparation method of multi items boron carbide micro powder, employing method three, pulverizing the equipment adopted is vertical high energy outer circulation pulverizer, and its technical parameter is: stirring rake or adopt abrasive rubber from mill and liner, and the rotating speed of pulverization cylinder is 650r/min; The rotating speed of circulating barrel is 350r/min, and grinding time is 15h; Carry out according to the following steps:
Step 1, in mass ratio, boron carbide raw material: deionized water=1:2, pulverizes, obtains the comminuting matter that basic grain is 5 ~ 10 μm; Wherein, norbide material is made up of varigrained three sections of materials, and the granularity of these three sections of norbides is 100 ~ 500 μm, 1000 ~ 3000 μm respectively, and 2000 ~ 60000 μm, its purity is all greater than 90%;
Step 2, squeezes into comminuting matter in swirler and carries out cyclonic separation, obtains granularity and is less than the underflow coarse fodder that the overflow fines of 8 μm and granularity are more than or equal to 8 μm;
Step 3, by norbide underflow coarse fodder, being crushed to granularity is 1 ~ 20 μm, as the comminuting matter recycle of step 1;
Step 4, carries out sedimentation wet concentration by overflow fines, and the weight concentration controlling wet concentration slip is 25%, and wet concentration temperature is 30 DEG C, and the settling time is 4h, selects norbide wet concentration coarse fodder and basic grain is 5 ~ 7 μm of norbide finished product wet feeds;
Step 5, by norbide wet concentration coarse fodder, being crushed to granularity is 1 ~ 20 μm, as the comminuting matter recycle of step 1;
Step 6, by norbide finished product wet feed drying screening, obtains norbide abrasive substance W7; Wherein, dry mode is infrared forced air drying, and drying conditions is: drying temperature is 80 DEG C, and drying power is 120kg/h, and time of drying is 8h.
The schema of the preparation method of the multi items boron carbide micro powder of the present embodiment as shown in Figure 3.
The yield rate of the norbide abrasive substance W7 of the present embodiment is 85%.
Embodiment 10
The preparation method of multi items boron carbide micro powder, employing method three, pulverizing the equipment adopted is vertical high energy outer circulation pulverizer or high energy autogenous mill, and its technical parameter is: adopt polyurethane material from mill and liner, the rotating speed of pulverization cylinder is 550r/min; The rotating speed of circulating barrel is 400r/min, and grinding time is 10h, and dispersion agent is KS5040; Carry out according to the following steps:
Step 1, in mass ratio, boron carbide raw material: deionized water: dispersion agent=1:0.3:0.5, pulverizes, obtains the comminuting matter that basic grain is 7 ~ 15 μm; Wherein, norbide material forms by varigrained two sections of materials, and the granularity of these two sections of norbides is 50 ~ 1000 μm, 1000 ~ 10000 μm respectively, and its purity is all greater than 90%;
Step 2, squeezes into comminuting matter in swirler and carries out cyclonic separation, obtains granularity and is less than the underflow coarse fodder that the overflow fines of 13 μm and granularity are more than or equal to 13 μm;
Step 3, by norbide underflow coarse fodder, being crushed to granularity is 1 ~ 20 μm, as the comminuting matter recycle of step 1;
Step 4, carries out sedimentation wet concentration by overflow fines, and the weight concentration controlling wet concentration slip is 20%, and wet concentration temperature is 32 DEG C, and the settling time is 8h, selects norbide wet concentration coarse fodder and basic grain is 7 ~ 10 μm of norbide finished product wet feeds;
Step 5, by norbide wet concentration coarse fodder, being crushed to granularity is 1 ~ 20 μm, as the comminuting matter recycle of step 1;
Step 6, by norbide finished product wet feed drying screening, obtains norbide abrasive substance W10; Wherein, dry mode is infrared forced air drying, and drying conditions is: drying temperature is 60 DEG C, and drying power is 180kg/h, and time of drying is 10h.
The schema of the preparation method of the multi items boron carbide micro powder of the present embodiment as shown in Figure 3.
The yield rate of the norbide abrasive substance W10 of the present embodiment is 88%.
Claims (7)
1. a preparation method for multi items boron carbide micro powder, is characterized in that, carries out according to the following steps:
Step 1, in mass ratio, norbide material: deionized water: dispersion agent=1:(0.3 ~ 2): (0.0 ~ 0.5), carry out one-level pulverizing, obtain D
50=3 ~ 12 μm of first level flour broken materials;
Step 2, squeezes into first level flour broken material in swirler and is separated, and obtains granularity and is less than the underflow coarse fodder that the overflow fines of 15 μm and granularity are more than or equal to 15 μm;
Step 3, the process of underflow coarse fodder:
(1) underflow coarse fodder is carried out two grade pulverization, obtaining granularity is D
50the two grade pulverization material of=2.5 ~ 5 μm;
(2) two grade pulverization material is carried out sedimentation wet concentration, wherein wet concentration pulp density is 15 ~ 30wt%, and wet concentration temperature is 20 ~ 40 DEG C, and the settling time is 4 ~ 12h, selects norbide wet concentration coarse fodder and granularity is D
50the norbide finished product wet feed of=2 ~ 5 μm;
(3) by norbide finished product wet feed, dry screening, obtaining granularity is D
50the norbide hot pressed sintering material of=2 ~ 5 μm;
(4) by norbide wet concentration coarse fodder, D is crushed to
50=2 ~ 5 μm, the two grade pulverization Matter Transfer as step 3 (1) utilizes;
Step 4, the process of overflow fines: after overflow fines being carried out drying, ultrasonic screening, obtains the norbide refractory materials that granularity is less than 15 μm; Wherein, drying mode is spraying dry: spray drying ability is 80 ~ 200kg/h, drying temperature 150 ~ 300 DEG C.
2. a preparation method for multi items boron carbide micro powder, is characterized in that, carries out according to the following steps:
Step 1, in mass ratio, norbide material: deionized water: dispersion agent=1:(0.3 ~ 2): (0.0 ~ 0.5), pulverize and obtain the comminuting matter that granularity is 150 ~ 600 μm;
Step 2, squeezes into whizzer by comminuting matter, and under centrifugal rotational speed is 2000 ~ 8000r/min, centrifugation, obtains the finished product wet feed slurry that coarse fodder is starched and granularity is less than 400 μm that granularity is more than or equal to 400 μm;
Step 3, is broken to granularity by coarse fodder starch and is less than 400 μm, as the comminuting matter recycle of step 1;
Step 4, by dry for finished product wet feed slurry, screening, obtains the norbide granularity sand that granularity is 150 ~ 400 μm; Drying mode is microwave drying: microwave frequency is 500 ~ 2000MHz, and power is 20 ~ 35kW, and drying power is 80 ~ 200kg/h.
3. a preparation method for multi items boron carbide micro powder, is characterized in that, carries out according to the following steps:
Step 1, in mass ratio, norbide material: deionized water: dispersion agent=1:(0.3 ~ 2): (0.0 ~ 0.5), pulverize, obtain the comminuting matter that basic grain is 1 ~ 20 μm;
Step 2, squeezes into comminuting matter in swirler and carries out cyclonic separation, obtains granularity and is less than the underflow coarse fodder that the overflow fines of 16 μm and granularity are more than or equal to 16 μm;
Step 3, by norbide underflow coarse fodder, being crushed to granularity is 1 ~ 20 μm, as the comminuting matter recycle of step 1;
Step 4, carries out sedimentation wet concentration by overflow fines, and the weight concentration controlling wet concentration slip is 15 ~ 30%, and wet concentration temperature is 20 ~ 40 DEG C, and the settling time is 4 ~ 12h, selects norbide wet concentration coarse fodder and granularity is 1.5 ~ 10 μm of norbide finished product wet feeds;
Step 5, by norbide wet concentration coarse fodder, being crushed to granularity is 1 ~ 20 μm, as the comminuting matter recycle of step 1;
Step 6, by norbide finished product wet feed drying screening, obtains norbide abrasive substance; Wherein, dry mode is infrared forced air drying, and drying conditions is: drying temperature is 60 ~ 100 DEG C, and drying power is 80 ~ 200kg/h, and time of drying is 6 ~ 12h.
4. the preparation method of multi items boron carbide micro powder according to claim 3, it is characterized in that, in described step 6, the norbide abrasive substance obtained is: the W5 that the W3.5 that basic grain is 1.5 ~ 3.5 μm, basic grain are 3.5 ~ 5 μm, the basic grain one that to be the W7 of 5 ~ 7 μm or basic grain be in the W10 of 7 ~ 10 μm.
5. the preparation method of the multi items boron carbide micro powder according to claim 1,2 or 3, it is characterized in that, the equipment that described pulverizing adopts is vertical high energy outer circulation pulverizer or high energy autogenous mill, both technical parameters are: stirring rake or adopt abrasive rubber and/or polyurethane material from mill and liner, and the rotating speed of pulverization cylinder is 400 ~ 800r/min; The rotating speed of circulating barrel is 200 ~ 400r/min, and grinding time is 5 ~ 30h, and pulverizing the dispersion agent adopted is KS5040, PVP-K90 or PEG.
6. the preparation method of multi items boron carbide micro powder according to claim 5, it is characterized in that, the described norbide material adding vertical high energy outer circulation pulverizer or high energy autogenous mill, be made up of any two sections or whole three sections in varigrained three sections of materials, granularity is 2 ~ 1000 μm, 500 ~ 5000 μm respectively, 1000 ~ 10000 μm, the purity of norbide material is all greater than 90%.
7. the preparation method of the multi items boron carbide micro powder according to claim 1,2 or 3, is characterized in that, the yield rate of described norbide product is 50 ~ 95% according to weight percent.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108373332A (en) * | 2018-03-21 | 2018-08-07 | 北京清核材料科技有限公司 | A kind of boron carbide ceramics slurry for ultrasonic wave batch mixing |
| CN108622900A (en) * | 2018-06-29 | 2018-10-09 | 江苏可润光电科技有限公司 | A kind of device and method of recycling boron carbide |
| CN111233479A (en) * | 2020-01-25 | 2020-06-05 | 大连正兴磨料有限公司 | Preparation method of high-purity, high-density and large-size boron carbide ceramic |
| CN113773805A (en) * | 2021-09-17 | 2021-12-10 | 开封贝斯科超硬材料有限公司 | Dry-wet combined production process for superhard material grinding material |
| CN115974084A (en) * | 2023-01-07 | 2023-04-18 | 中硼科技(威海)有限公司 | Preparation method of high-purity boron carbide powder for core |
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| CN1460640A (en) * | 2003-05-19 | 2003-12-10 | 大连巨鑫超硬材料有限公司 | Preparation method of boron carbide ultramicropowder |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108373332A (en) * | 2018-03-21 | 2018-08-07 | 北京清核材料科技有限公司 | A kind of boron carbide ceramics slurry for ultrasonic wave batch mixing |
| CN108622900A (en) * | 2018-06-29 | 2018-10-09 | 江苏可润光电科技有限公司 | A kind of device and method of recycling boron carbide |
| CN111233479A (en) * | 2020-01-25 | 2020-06-05 | 大连正兴磨料有限公司 | Preparation method of high-purity, high-density and large-size boron carbide ceramic |
| CN111233479B (en) * | 2020-01-25 | 2022-05-06 | 大连正兴磨料有限公司 | Preparation method of high-purity, high-density and large-size boron carbide ceramic |
| CN113773805A (en) * | 2021-09-17 | 2021-12-10 | 开封贝斯科超硬材料有限公司 | Dry-wet combined production process for superhard material grinding material |
| CN115974084A (en) * | 2023-01-07 | 2023-04-18 | 中硼科技(威海)有限公司 | Preparation method of high-purity boron carbide powder for core |
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