CN105540591B - The preparation method of multi items boron carbide micro powder - Google Patents
The preparation method of multi items boron carbide micro powder Download PDFInfo
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Abstract
The preparation method of multi items boron carbide micro powder, carry out according to the following steps：Boron carbide material is first carried out to one-level or two level crushes, then by classification and dry sieve operation break-down, you can obtain a variety of varigrained boron carbide micro powders.In the method, foreign peoples's medium is not introduced into crushing process, avoids caused a large amount of impurity in the production of general milling method; without carrying out pickling and the washing step in later stage again, substantial amounts of water resource and energy consumption are saved, has reduced production cost; environmental pollution is it also avoid simultaneously, is advantageous to environmental protection；And this method employs the mode of two-stage crushing, avoid raw material in general milling method and cross crushing, the wider phenomenon of particle size bands, improve the yield rate of product；In addition, this method flow is simple, with short production cycle, production efficiency is high, significantly reduces production cost.The inventive method has the advantages that simple for process, with short production cycle, product yield ratio is high, processing cost is low, environmental protection, saving water resource.
Description
Technical field
The invention belongs to the preparation method in the crushing technology field, more particularly to multi items boron carbide micro powder of superhard material.
Background technology
Boron carbide has that hardness high (Mohs' hardness 9.36), wearability is good, the low (2.52g/cm of density3) and fusing point height
Excellent specific properties such as (2450 DEG C), is widely used in the fields such as mechanical lapping, refractory material, engineering ceramics, nuclear industry and military affairs.
Boron carbide micro powder has the excellent specific properties such as specific surface area is big, chemism is high, respond is strong, fusing point and sintering temperature are low, on
Stating excellent specific property makes it be widely used in the fields such as fine ceramics, powder metallurgy, electronic technology and composite.Such as use carbon
It when changing boron Ultramicro-powder preparation engineering ceramics, can at a lower temperature, in the short period be sintered, obtain finer and close finer structures
Sintered body.
Because the hardness of boron carbide is very high (being only second to diamond and cubic boron nitride), being processed into for its micro mist is 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 air-flow powder
Broken method can obtain boron carbide micro powder, and it is few to bring impurity into, but there is high energy consumption, output capacity is low and amount of waste is big, cause to produce
Costly, raw material availability is relatively low.
It is still general milling method that the main method of large-scale production boron carbide micro powder, which is, at present.Its main technique is：Carbonization
Boron block → ball mill crushing → pickling impurity removal → plate compression → hydraulic classiciation → drying and dehydrating → finished product.General milling method has
The advantages that yield is high, technique is simple, but there is also production cycle length (being usually 18~30 days), product yield ratio it is low (30~
40%), high energy consumption, impurity (mainly Fe) content is high, especially also needs to carry out pickling impurity removal, water washing cleaning, causes water resource
Waste and environment pollution.
It follows that the production technology of comminution by gas stream and general milling method exist boron carbide raw material utilization rate it is relatively low,
Energy consumption is higher, output capacity is relatively low, the waste of water resource and the deficiencies of the pollution of environment.
The content of the invention
The present invention is for deficiency present in current boron carbide micro powder production technology, it is proposed that multi items boron carbide micro powder
Preparation method.The present invention production method be：Boron carbide raw material is passed through into vertical high energy outer circulation pulverizer or high energy autogenous tumbling mill
Carry out after one-level or two level crush, then by classification, dry screening and can obtain a variety of varigrained boron carbide micro powders, it is such as resistance to
Fiery material, hot pressed sintering material, granularity sand and grinding-material.
One of preparation method of multi items boron carbide micro powder of the present invention, is carried out according to the following steps：
Step 1, in mass ratio, boron carbide material：Deionized water：Dispersant=1：(0.3~2)：(0.0~0.5), carry out
One-level crushes, and obtains D50=3~12 μm of one-level comminuting matters；
Step 2, one-level comminuting matter is squeezed into and cyclonic separation is carried out in cyclone, it is thin less than 15 μm of overflow to obtain granularity
Material and granularity are more than or equal to 15 μm of underflow coarse fodder；
Step 3, the processing of underflow coarse fodder：
(1) underflow coarse fodder is subjected to two level crushing, it is D to obtain granularity50=2.5~5 μm of two level comminuting matter；
(2) two level comminuting matter is subjected to sedimentation wet concentration, control the mass concentration of boron carbide in wet concentration slurry for 15~
30%, wet concentration temperature is 20~40 DEG C, and the sedimentation time is 4~12h, and it is D to select boron carbide wet concentration coarse fodder and granularity50=2~5 μm
Boron carbide finished product wet feed；
(3) by boron carbide finished product wet feed, screening is dried, it is D to obtain granularity50=2~5 μm of boron carbide hot pressed sintering material
Material；
(4) by boron carbide wet concentration coarse fodder, it is crushed to D50=2~5 μm, the two level comminuting matter as step 3 (1) circulates profit
With；
Step 4, the processing of overflow fines：
Overflow fines is dried, after ultrasound screening, obtains the boron carbide refractory material that granularity is less than 15 μm；Wherein,
Drying mode is spray drying：Spray drying ability is 80~200kg/h, 150~300 DEG C of drying temperature.
The two of the preparation method of the multi items boron carbide micro powder of the present invention, are carried out according to the following steps：
Step 1, in mass ratio, boron carbide material：Deionized water：Dispersant=1：(0.3~2)：(0.0~0.5), crush
Obtain the comminuting matter that granularity is 150~600 μm；
Step 2, comminuting matter is squeezed into centrifuge, in the case where centrifugal rotational speed is 2000~8000r/min, centrifuges, obtain
The finished product wet feed of coarse fodder slurry and granularity less than 400 μm to granularity more than or equal to 400 μm is starched；
Step 3, coarse fodder starch is broken to granularity less than 400 μm, the comminuting matter as step 1 recycles；
Step 4, finished product wet feed is starched and dries, sieves, obtain the boron carbide granularity sand that granularity is 150~400 μm；Drying side
Formula is microwave drying：Microwave frequency is 500~2000MHz, and power is 20~35kW, and drying capacity is 80~200kg/h.
The three of the preparation method of the multi items boron carbide micro powder of the present invention, are carried out according to the following steps：
Step 1, in mass ratio, boron carbide material：Deionized water：Dispersant=1：(0.3~2)：(0.0~0.5), powder
It is broken, obtain the comminuting matter that basic grain is 1~20 μm；
Step 2, comminuting matter is squeezed into and cyclonic separation is carried out in cyclone, obtain granularity less than 16 μm overflow fines and
Granularity is more than or equal to 16 μm of underflow coarse fodder；
Step 3, by boron carbide underflow coarse fodder, granularity is crushed to as 1~20 μm, and the comminuting matter as step 1 circulates profit
With；
Step 4, overflow fines is subjected to sedimentation wet concentration, the weight concentration for controlling wet concentration slurry is 15~30%, wet concentration temperature
Spend for 20~40 DEG C, the sedimentation time is 4~12h, and it is that 1.5~10 μm of boron carbide finished products are wet to select boron carbide wet concentration coarse fodder and granularity
Material；
Step 5, by boron carbide wet concentration coarse fodder, granularity is crushed to as 1~20 μm, and the comminuting matter as step 1 circulates profit
With；
Step 6, boron carbide finished product wet feed is dried and sieved, obtain boron carbide grinding-material；Wherein, dry mode is red
Outer forced air drying, drying condition are：Drying temperature is 60~100 DEG C, and drying capacity be 80~200kg/h, drying time for 6~
12h。
In the above method one, method two or method three, the equipment used is crushed as vertical high energy outer circulation pulverizer or height
Energy autogenous tumbling mill, both technical parameters are：Agitating paddle uses abrasive rubber and/or polyurethane material from mill and liner,
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；Crush
The dispersant used is KS5040, PVP-K90 or PEG.
In the above method one, method two or method three, described addition vertical high energy outer circulation pulverizer or high energy autogenous grinding
The boron carbide material of machine, by any two sections in varigrained three sections of materials or all three sections form, and granularity is 2 respectively~
1000 μm, 500~5000 μm, 1000~10000 μm, the purity of boron carbide material is all higher than 90%.
The boron carbide grinding-material obtained in the above method three is：W3.5 that basic grain is 1.5~3.5 μm, basic grain are
One kind in 3.5~5 μm of W5, the W7 that basic grain is 5~7 μm or the W10 that basic grain is 7~10 μm.
The yield rate of boron carbide product described in the above method one, method two or method three is 50 according to percentage by weight
~95%.
The beneficial effect of preparation method of the multi items boron carbide micro powder of the present invention is：
1st, in the present invention, vertical high energy outer circulation pulverizer or high energy autogenous tumbling mill are employed, foreign peoples's medium is not introduced into, keeps away
Exempt from caused a large amount of impurity (mainly Fe) in the production of general milling method, without carrying out pickling and the washing step in later stage again,
Substantial amounts of water resource and energy consumption have been saved, has reduced production cost, while it also avoid environmental pollution, has been advantageous to environmental protection；
2nd, in the present invention, the grinding mode of two-stage series connection is employed in method one, is avoided former caused by general milling
Expected to crush, the wider phenomenon of particle size bands, and substantially increased the yield rate (70~95%) of product；
3rd, in the present invention, direct wet concentration finished product during classification of sedimentation, the production cycle (2~5 days) is significantly shorten, is carried significantly
High production efficiency, reduces production cost.
4th, in the present invention, a variety of varigrained boron carbides can be obtained by adjusting grinding time and breaking method micro-
Powder, such as：Boron carbide refractory material (3~15 μm), boron carbide hot pressed sintering material (D50=2~5 μm), boron carbide granularity sand
(150~400 μm), boron carbide grinding-material, 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).
Brief description of the drawings
Fig. 1 is the flow chart of the preparation method one of the multi items boron carbide micro powder of the present invention；
Fig. 2 is the flow chart of the preparation method two of the multi items boron carbide micro powder of the present invention；
Fig. 3 is the flow chart of the preparation method three of the multi items boron carbide micro powder of the present invention.
Embodiment
Embodiment 1
The preparation method of multi items boron carbide micro powder, using method one, the equipment used is crushed as vertical high energy outer circulation
Pulverizer, its technical parameter are：Agitating paddle and liner use abrasive rubber and polyurethane material, and the rotating speed of pulverization cylinder is 400r/
min；The rotating speed of circulating barrel is 200r/min, grinding time 30h；Carry out according to the following steps：
Step 1, in mass ratio, boron carbide material：Deionized water=1：1, one-level crushing is carried out, obtains D50=3~8 μm one
Level comminuting matter；Wherein, boron carbide material is made up of varigrained two sections of materials, and the granularity of this two sections of boron carbides is respectively
2~1000 μm, 500~5000 μm, boron carbide feed purity is all higher than 90%；
Step 2, one-level comminuting matter is squeezed into cyclone and separated, obtain the overflow fines that granularity is 3~15 μm
It is D with granularity97=15~4000 μm of underflow coarse fodder；
Step 3, the processing of underflow coarse fodder：
(1) underflow coarse fodder is subjected to two level crushing, it is D to obtain granularity50=2.5~5 μm of two level comminuting matter；
(2) two level comminuting matter being subjected to sedimentation wet concentration, the mass concentration for controlling the boron carbide in wet concentration slurry is 15%,
Wet concentration temperature is 40 DEG C, sedimentation time 4h, and it is D to select boron carbide wet concentration coarse fodder and granularity50=2~5 μm of boron carbide finished product
Wet feed；
(3) by boron carbide finished product wet feed, screening is dried, it is D to obtain granularity50=2~5 μm of boron carbide hot pressed sintering material
Material；
(4) by boron carbide wet concentration coarse fodder, it is crushed to D50=2~5 μm, the two level comminuting matter as step 3 (1) circulates profit
With；
Step 4, the processing of overflow fines：
After the drying of overflow fines, ultrasound screening, the boron carbide refractory material that granularity is less than 15 μm is obtained；Wherein, dry
Mode is spray drying：Spray drying ability is 80kg/h, 150 DEG C of drying temperature.
The flow chart of the preparation method of the multi items boron carbide micro powder of the present embodiment is as shown in Figure 1.
The boron carbide refractory material of the present embodiment and total yield rate of boron carbide hot pressed sintering material are 70%.
Embodiment 2
The preparation method of multi items boron carbide micro powder, using method one, the equipment used is crushed as high energy autogenous tumbling mill, its skill
Art parameter is：Abrasive rubber is used from mill and liner, the rotating speed of pulverization cylinder is 650r/min；The rotating speed of circulating barrel is 300r/
Min, grinding time 20h, dispersant PVP-K90；Carry out according to the following steps：
Step 1, in mass ratio, boron carbide fill material：Deionized water：Dispersant=1：0.3：0.5, carry out first level flour
It is broken, obtain D50=8~200 μm of one-level comminuting matter；Wherein, boron carbide material is made up of varigrained two sections of materials,
The granularity of this two sections of boron carbides is 2~1000 μm, 1000~10000 μm respectively, and its purity is all higher than 90%；
Step 2, one-level comminuting matter is squeezed into cyclone and separated, obtain the overflow fines that granularity is 3~15 μm
It is D with granularity97=15~4000 μm of underflow coarse fodder；
Step 3, the processing of underflow coarse fodder：
(1) underflow coarse fodder is subjected to two level crushing, it is D to obtain granularity50=2.5~5 μm of two level comminuting matter；
(2) two level comminuting matter being subjected to sedimentation wet concentration, the mass concentration for controlling the boron carbide in wet concentration slurry is 30%,
Wet concentration temperature is 20 DEG C, sedimentation time 12h, and it is D to select boron carbide wet concentration coarse fodder and granularity50=2~5 μm of boron carbide finished product
Wet feed；
(3) by boron carbide finished product wet feed, screening is dried, it is D to obtain granularity50=2~5 μm of boron carbide hot pressed sintering material
Material；
(4) by boron carbide wet concentration coarse fodder, it is crushed to D50=2~5 μm, the two level comminuting matter as step 3 (1) circulates profit
With；
Step 4, the processing of overflow fines：
After the drying of overflow fines, ultrasound screening, the boron carbide refractory material that granularity is less than 15 μm is obtained；Wherein, dry
Mode is spray drying：Spray drying ability is 200kg/h, 300 DEG C of drying temperature.
The flow chart of the preparation method of the multi items boron carbide micro powder of the present embodiment is as shown in Figure 1.
The boron carbide refractory material of the present embodiment and total yield rate of boron carbide hot pressed sintering material are 75%.
Embodiment 3
The preparation method of multi items boron carbide micro powder, using method one, the equipment used is crushed as vertical high energy outer circulation
Pulverizer, its technical parameter are：Agitating paddle and liner use polyurethane material, and the rotating speed of pulverization cylinder is 800r/min；Circulating barrel
Rotating speed be 400r/min, grinding time 5h, dispersant PEG；Carry out according to the following steps：
Step 1, in mass ratio, boron carbide fill material：Deionized water：Dispersant=1：2：0.1, one-level crushing is carried out,
Obtain D50=200~4000 μm of one-level comminuting matter；Wherein, boron carbide material is made up of varigrained three sections of materials,
The granularity of this three sections of boron carbides is 2~1000 μm, 500~5000 μm respectively, and 1000~10000 μm, its purity is all higher than 90%；
Step 2, one-level comminuting matter is squeezed into cyclone and separated, obtain the overflow fines that granularity is 3~15 μm
It is D with granularity97=15~4000 μm of underflow coarse fodder；
Step 3, the processing of underflow coarse fodder：
(1) underflow coarse fodder is subjected to two level crushing, it is D to obtain granularity50=2.5~5 μm of two level comminuting matter；
(2) two level comminuting matter being subjected to sedimentation wet concentration, the mass concentration for controlling the boron carbide in wet concentration slurry is 20%,
Wet concentration temperature is 30 DEG C, sedimentation time 8h, and it is D to select boron carbide wet concentration coarse fodder and granularity50=2~5 μm of boron carbide finished product
Wet feed；
(3) by boron carbide finished product wet feed, screening is dried, it is D to obtain granularity50=2~5 μm of boron carbide hot pressed sintering material
Material；
(4) by boron carbide wet concentration coarse fodder, it is crushed to D50=2~5 μm, the two level comminuting matter as step 3 (1) circulates profit
With；
Step 4, the processing of overflow fines：
After the drying of overflow fines, ultrasound screening, the boron carbide refractory material that granularity is less than 15 μm is obtained；Wherein, dry
Mode is spray drying：Spray drying ability is 120kg/h, 220 DEG C of drying temperature.
The flow chart of the preparation method of the multi items boron carbide micro powder of the present embodiment is as shown in Figure 1.
The boron carbide refractory material of the present embodiment and total yield rate of boron carbide hot pressed sintering material are 78%.
Embodiment 4
The preparation method of multi items boron carbide micro powder, using method two, the equipment used is crushed as high energy autogenous tumbling mill, its skill
Art parameter is：Agitating paddle and liner use abrasive rubber and polyurethane material, and the rotating speed of pulverization cylinder is 550r/min；Circulating barrel
Rotating speed is 250r/min, grinding time 22h, dispersant KS5040；Carry out according to the following steps：
Step 1, in mass ratio, boron carbide raw material：Deionized water：Dispersant=1：2：0.5, crush, obtain granularity as 150
~500 μm of comminuting matter；Wherein, boron carbide material is made up of varigrained two sections of materials, the grain of this two sections of boron carbides
Degree is 500~5000 μm respectively, and 1000~10000 μm, its purity is all higher than 90%；
Step 2, comminuting matter is squeezed into centrifuge, in the case where centrifugal rotational speed is 2000r/min, centrifuges, obtain granularity
D97=360~600 μm of coarse fodder slurry and the finished product wet feed that granularity is 150~360 μm are starched；
Step 3, coarse fodder starch is broken to granularity less than 400 μm, the comminuting matter as step 1 recycles；
Step 4, by the drying of finished product wet feed, screening, the boron carbide granularity sand that granularity is 150~400 μm is obtained；Drying mode
For microwave drying：The microwave frequency of microwave drying is 500MHz, power 20kW, drying capacity 80kg/h.
The flow chart of the preparation method of the multi items boron carbide micro powder of the present embodiment is as shown in Figure 2.
The yield rate of the boron carbide granularity sand of the present embodiment is 95%.
Embodiment 5
The preparation method of multi items boron carbide micro powder, using method two, the equipment used is crushed as high energy autogenous tumbling mill, its skill
Art parameter is：Polyurethane material is used from mill and liner, the rotating speed of pulverization cylinder is 800r/min；The rotating speed of circulating barrel is
400r/min, grinding time 5h, dispersant PEG；Carry out according to the following steps：
Step 1, in mass ratio, boron carbide raw material：Deionized water：Dispersant=1：1.2：0.4, crush, obtaining granularity is
200~600 μm of comminuting matter；Wherein, boron carbide material is formed by varigrained two sections, the granularity of this two sections of boron carbides
It is 50~1000 μm, 1000~10000 μm respectively, its purity is all higher than 90%；
Step 2, comminuting matter is squeezed into centrifuge, in the case where centrifugal rotational speed is 8000r/min, centrifuges, obtain granularity
D97=400~600 μm of coarse fodder slurry and the finished product wet feed that granularity is 200~400 μm are starched；
Step 3, coarse fodder starch is broken to granularity less than 400 μm, the comminuting matter as step 1 recycles；
Step 4, by the drying of finished product wet feed, screening, the boron carbide granularity sand that granularity is 200~400 μm is obtained；Drying mode
For microwave drying：The microwave frequency of microwave drying is 2000MHz, power 35kW, drying capacity 200kg/h.
The flow chart of the preparation method of the multi items boron carbide micro powder of the present embodiment is as shown in Figure 2.
The yield rate of the boron carbide granularity sand of the present embodiment is 90%.
Embodiment 6
The preparation method of multi items boron carbide micro powder, using method two, the equipment used is crushed as vertical high energy outer circulation
Pulverizer, its technical parameter are：Abrasive rubber is used from mill and liner, the rotating speed of pulverization cylinder is 400r/min；Circulating barrel
Rotating speed is 250r/min, grinding time 16h；Carry out according to the following steps：
Step 1, in mass ratio, boron carbide raw material：Deionized water=1：0.3, crush, it is 250~500 μm to obtain granularity
Comminuting matter；Wherein, by being formed in varigrained three sections of materials, the granularity of this three sections of boron carbides is respectively boron carbide material
2~400 μm, 500~800 μm, 1000~8000 μm, its purity is all higher than 90%；
Step 2, comminuting matter is squeezed into centrifuge, in the case where centrifugal rotational speed is 5000r/min, centrifuges, obtain granularity
D97=360~500 μm of coarse fodder slurry and the finished product wet feed that granularity is 150~360 μm are starched；
Step 3, coarse fodder starch is broken to granularity less than 400 μm, the comminuting matter as step 1 recycles；
Step 4, by the drying of finished product wet feed, screening, the boron carbide granularity sand that granularity is 150~360 μm is obtained；Drying mode
For microwave drying：The microwave frequency of microwave drying is 1200MHZ, power 28kW, drying capacity 150kg/h.
The flow chart of the preparation method of the multi items boron carbide micro powder of the present embodiment is as shown in Figure 2.
The yield rate of the boron carbide granularity sand of the present embodiment is 92%.
Embodiment 7
The preparation method of multi items boron carbide micro powder, using method three, the equipment used is crushed as high energy autogenous tumbling mill, its skill
Art parameter is：Agitating paddle and liner use polyurethane material, and the rotating speed of pulverization cylinder is 800r/min；The rotating speed of circulating barrel is
400r/min, grinding time 5h, dispersant KS5040；Carry out according to the following steps：
Step 1, in mass ratio, boron carbide raw material：Deionized water：Dispersant=1：1.6：0.25, crush, obtain basic grain
For 1~6 μm of comminuting matter；Wherein, boron carbide material is made up of varigrained two sections of materials, the grain of this two sections of boron carbides
Degree is 2~600 μm, 2000~5000 μm respectively, and its purity is all higher than 90%；
Step 2, comminuting matter is squeezed into and cyclonic separation is carried out in cyclone, obtain granularity less than 4 μm overflow fines and
Granularity is more than or equal to 4 μm of underflow coarse fodder；
Step 3, by boron carbide underflow coarse fodder, granularity is crushed to as 1~20 μm, and the comminuting matter as step 1 circulates profit
With；
Step 4, overflow fines is subjected to sedimentation wet concentration, the weight concentration for controlling wet concentration slurry is 15%, and wet concentration temperature is
20 DEG C, sedimentation time 12h, it is 1.5~3.5 μm of boron carbide finished product wet feeds to select boron carbide wet concentration coarse fodder and basic grain；
Step 5, by boron carbide wet concentration coarse fodder, granularity is crushed to as 1~20 μm, and the comminuting matter as step 1 circulates profit
With；
Step 6, boron carbide finished product wet feed is dried and sieved, obtain boron carbide grinding-material W3.5；Wherein, dry mode
For infrared forced air drying, drying condition is：Drying temperature is 60 DEG C, drying capacity 80kg/h, drying time 12h.
The flow chart of the preparation method of the multi items boron carbide micro powder of the present embodiment is as shown in Figure 3.
The boron carbide grinding-material W3.5 of the present embodiment yield rate is 72%.
Embodiment 8
The preparation method of multi items boron carbide micro powder, using method three, the equipment used is crushed as vertical high energy outer circulation
Pulverizer, its technical parameter are：Abrasive rubber and polyurethane material are used from mill and liner, the rotating speed of pulverization cylinder is 400r/
min；The rotating speed of circulating barrel is 200r/min, grinding time 30h, dispersant PVP-K90；Carry out according to the following steps：
Step 1, in mass ratio, boron carbide raw material：Deionized water：Dispersant=1：1.2：0.15, crush, obtain basic grain
For 4~8 μm of comminuting matter；Wherein, boron carbide material is made up of varigrained two sections of materials, the grain of this two sections of boron carbides
Degree is 2~100 μm, 1000~5000 μm respectively, and its purity is all higher than 90%；
Step 2, comminuting matter is squeezed into and cyclonic separation is carried out in cyclone, obtain granularity less than 6 μm overflow fines and
Granularity is more than or equal to 6 μm of underflow coarse fodder；
Step 3, by boron carbide underflow coarse fodder, granularity is crushed to as 1~20 μm, and the comminuting matter as step 1 circulates profit
With；
Step 4, overflow fines is subjected to sedimentation wet concentration, the weight concentration for controlling wet concentration slurry is 30%, and wet concentration temperature is
40 DEG C, sedimentation time 6h, it is 3.5~5 μm of boron carbide finished product wet feeds to select boron carbide wet concentration coarse fodder and basic grain；
Step 5, by boron carbide wet concentration coarse fodder, granularity is crushed to as 1~20 μm, and the comminuting matter as step 1 circulates profit
With；
Step 6, boron carbide finished product wet feed is dried and sieved, obtain boron carbide grinding-material W5；Wherein, dry mode is
Infrared forced air drying, drying condition are：Drying temperature is 100 DEG C, drying capacity 200kg/h, drying time 6h.
The flow chart of the preparation method of the multi items boron carbide micro powder of the present embodiment is as shown in Figure 3.
The boron carbide grinding-material W5 of the present embodiment yield rate is 80%.
Embodiment 9
The preparation method of multi items boron carbide micro powder, using method three, the equipment used is crushed as vertical high energy outer circulation
Pulverizer, its technical parameter are：Agitating paddle uses 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, grinding time 15h；Carry out according to the following steps：
Step 1, in mass ratio, boron carbide raw material：Deionized water=1：2, crush, obtain the powder that basic grain is 5~10 μm
Broken material；Wherein, boron carbide material is made up of varigrained three sections of materials, and the granularity of this three sections of boron carbides is 100 respectively
~500 μm, 1000~3000 μm, 2000~60000 μm, its purity is all higher than 90%；
Step 2, comminuting matter is squeezed into and cyclonic separation is carried out in cyclone, obtain granularity less than 8 μm overflow fines and
Granularity is more than or equal to 8 μm of underflow coarse fodder；
Step 3, by boron carbide underflow coarse fodder, granularity is crushed to as 1~20 μm, and the comminuting matter as step 1 circulates profit
With；
Step 4, overflow fines is subjected to sedimentation wet concentration, the weight concentration for controlling wet concentration slurry is 25%, and wet concentration temperature is
30 DEG C, sedimentation time 4h, it is 5~7 μm of boron carbide finished product wet feeds to select boron carbide wet concentration coarse fodder and basic grain；
Step 5, by boron carbide wet concentration coarse fodder, granularity is crushed to as 1~20 μm, and the comminuting matter as step 1 circulates profit
With；
Step 6, boron carbide finished product wet feed is dried and sieved, obtain boron carbide grinding-material W7；Wherein, dry mode is
Infrared forced air drying, drying condition are：Drying temperature is 80 DEG C, drying capacity 120kg/h, drying time 8h.
The flow chart of the preparation method of the multi items boron carbide micro powder of the present embodiment is as shown in Figure 3.
The boron carbide grinding-material W7 of the present embodiment yield rate is 85%.
Embodiment 10
The preparation method of multi items boron carbide micro powder, using method three, the equipment used is crushed as vertical high energy outer circulation
Pulverizer or high energy autogenous tumbling mill, its technical parameter are：Polyurethane material is used from mill and liner, the rotating speed of pulverization cylinder is
550r/min；The rotating speed of circulating barrel is 400r/min, grinding time 10h, dispersant KS5040；Carry out according to the following steps：
Step 1, in mass ratio, boron carbide raw material：Deionized water：Dispersant=1：0.3：0.5, crush, obtain basic grain
For 7~15 μm of comminuting matter；Wherein, boron carbide material in varigrained two sections of materials by forming, this two sections of boron carbides
Granularity be 50~1000 μm, 1000~10000 μm respectively, its purity is all higher than 90%；
Step 2, comminuting matter is squeezed into and cyclonic separation is carried out in cyclone, obtain granularity less than 13 μm overflow fines and
Granularity is more than or equal to 13 μm of underflow coarse fodder；
Step 3, by boron carbide underflow coarse fodder, granularity is crushed to as 1~20 μm, and the comminuting matter as step 1 circulates profit
With；
Step 4, overflow fines is subjected to sedimentation wet concentration, the weight concentration for controlling wet concentration slurry is 20%, and wet concentration temperature is
32 DEG C, sedimentation time 8h, it is 7~10 μm of boron carbide finished product wet feeds to select boron carbide wet concentration coarse fodder and basic grain；
Step 5, by boron carbide wet concentration coarse fodder, granularity is crushed to as 1~20 μm, and the comminuting matter as step 1 circulates profit
With；
Step 6, boron carbide finished product wet feed is dried and sieved, obtain boron carbide grinding-material W10；Wherein, dry mode
For infrared forced air drying, drying condition is：Drying temperature is 60 DEG C, drying capacity 180kg/h, drying time 10h.
The flow chart of the preparation method of the multi items boron carbide micro powder of the present embodiment is as shown in Figure 3.
The boron carbide grinding-material W10 of the present embodiment yield rate is 88%.
Claims (5)
1. a kind of preparation method of multi items boron carbide micro powder, it is characterised in that carry out according to the following steps：
Step 1, in mass ratio, boron carbide material：Deionized water：Dispersant=1：（0.3~2）：（0.0~0.5）, carry out first level flour
It is broken, obtain D50=3 ~ 12 μm of one-level comminuting matters；
Step 2, one-level comminuting matter is squeezed into cyclone and separated, obtain overflow fines and granularity of the granularity less than 15 μm
Underflow coarse fodder more than or equal to 15 μm；
Step 3, the processing of underflow coarse fodder：
（1）Underflow coarse fodder is subjected to two level crushing, it is D to obtain granularity50=2.5 ~ 5 μm of two level comminuting matter；
（2）Two level comminuting matter is subjected to sedimentation wet concentration, wherein wet concentration pulp density is 15 ~ 30wt%, and wet concentration temperature is 20 ~ 40
DEG C, the sedimentation time is 4 ~ 12h, and it is D to select boron carbide coarse fodder and granularity50=2 ~ 5 μm of boron carbide finished product wet feed；
（3）By boron carbide finished product wet feed, screening is dried, it is D to obtain granularity50=2 ~ 5 μm of boron carbide hot pressed sintering material；
（4）By boron carbide coarse fodder, D50=2 ~ 5 μm are crushed to, are used as step 3（1）Two level comminuting matter recycle；
Step 4, the processing of overflow fines：Overflow fines is dried, after ultrasound screening, obtains the carbonization that granularity is less than 15 μm
Boron refractory material；Wherein, drying mode is spray drying：Spray drying ability is 80 ~ 200kg/h, drying temperature 150 ~ 300
℃。
2. a kind of preparation method of multi items boron carbide micro powder, it is characterised in that carry out according to the following steps：
Step 1, in mass ratio, boron carbide material：Deionized water：Dispersant=1：（0.3~2）：（0.0~0.5）, crush, obtain base
This grain is 1 ~ 20 μm of comminuting matter；
Step 2, comminuting matter is squeezed into and cyclonic separation is carried out in cyclone, obtain overflow fines and granularity of the granularity less than 16 μm
Underflow coarse fodder more than or equal to 16 μm；
Step 3, by boron carbide underflow coarse fodder, granularity is crushed to as 1 ~ 20 μm, the comminuting matter as step 1 recycles；
Step 4, overflow fines is subjected to sedimentation wet concentration, control wet concentration slurry weight concentration be 15 ~ 30%, wet concentration temperature be 20 ~
40 DEG C, the sedimentation time is 4 ~ 12h, and it is 1.5 ~ 10 μm of boron carbide finished product wet feeds to select boron carbide coarse fodder and granularity；
Step 5, by boron carbide coarse fodder, granularity is crushed to as 1 ~ 20 μm, the comminuting matter as step 1 recycles；
Step 6, boron carbide finished product wet feed is dried and sieved, obtain boron carbide grinding-material；Wherein, dry mode is infrared drum
Air-dried dry, drying condition is：Drying temperature is 60 ~ 100 DEG C, and drying capacity is 80 ~ 200kg/h, and drying time is 6 ~ 12h.
3. the preparation method of multi items boron carbide micro powder according to claim 2, it is characterised in that in the step 6, obtain
To boron carbide grinding-material be：W3.5 that basic grain is 1.5 ~ 3.5 μm, the W5 that basic grain is 3.5 ~ 5 μm, basic grain are 5 ~ 7 μ
M W7, the W10 that basic grain is 7 ~ 10 μm.
4. the preparation method of multi items boron carbide micro powder according to claim 1 or 2, it is characterised in that described crushing
The equipment used is for vertical high energy outer circulation pulverizer or high energy autogenous tumbling mill, both technical parameters：Agitating paddle or autogenous grinding
Disk and liner use abrasive rubber and/or polyurethane material, and the rotating speed of pulverization cylinder is 400 ~ 800r/min；The rotating speed of circulating barrel is
200 ~ 400r/min, grinding time are 5 ~ 30h, crush the dispersant used as KS5040, PVP-K90 or PEG.
5. the preparation method of multi items boron carbide micro powder according to claim 4, it is characterised in that described addition is vertical
The boron carbide material of high energy outer circulation pulverizer or high energy autogenous tumbling mill, be by any two sections in varigrained three sections of materials or
All three sections of compositions, granularity is 2 ~ 1000 μm, 500 ~ 5000 μm respectively, and 1000 ~ 10000 μm, the purity of boron carbide material is big
In 90%.
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