CN1231415C - Preparation method of boron carbide ultramicropowder - Google Patents
Preparation method of boron carbide ultramicropowder Download PDFInfo
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- CN1231415C CN1231415C CN 03133314 CN03133314A CN1231415C CN 1231415 C CN1231415 C CN 1231415C CN 03133314 CN03133314 CN 03133314 CN 03133314 A CN03133314 A CN 03133314A CN 1231415 C CN1231415 C CN 1231415C
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- Prior art keywords
- ball
- fine powder
- super
- norbide
- cylinder
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- 229910052580 B4C Inorganic materials 0.000 title claims abstract description 5
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 title claims abstract description 5
- 238000002360 preparation method Methods 0.000 title claims description 6
- 239000000843 powder Substances 0.000 claims abstract description 30
- 238000000227 grinding Methods 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims abstract description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- 230000018044 dehydration Effects 0.000 claims description 11
- 238000006297 dehydration reaction Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 9
- 238000000498 ball milling Methods 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 6
- 238000003801 milling Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 3
- 235000012054 meals Nutrition 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 abstract description 11
- 239000012535 impurity Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 5
- 238000004062 sedimentation Methods 0.000 abstract description 4
- 238000000746 purification Methods 0.000 abstract 1
- 238000004904 shortening Methods 0.000 abstract 1
- 235000019580 granularity Nutrition 0.000 description 7
- 238000003756 stirring Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- 229910052796 boron Inorganic materials 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 239000006061 abrasive grain Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 238000005554 pickling Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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- Crushing And Grinding (AREA)
Abstract
The present invention relates to a technological process of preparing boron carbide ultra-fine powder, which belongs to the technical field of the superfine grinding technology of superhard material. The technological process is realized by combining three processes of circulating ball-grinding operation outside a cylinder, centrifugal sedimentation dewatering and purification, and anhydrous ethanol dispersion and vacuum drying at low temperature. After the superfine grinding operation of boron carbide, the grain size of the product can reach less than 2 mum, and impurities, including iron, free carbon, and the like in the raw material powder can be effectively removed. Thus, the purposes of shortening processing time and improving work efficiency so as to enhance production capacity and improve product quality are achieved.
Description
Affiliated technical field
The invention belongs to the ultrafine grinding process technology of superhard material.
Background technology
The norbide ultrafine powder has the characteristic of a lot of excellences, at high-technology field very big actual application value is arranged.It is big that the norbide super-fine powder has specific surface area, the chemically reactive height, and physics-chem characteristic such as response capacity is strong, and fusing point and sintering temperature are low, it plays a part very important at fine ceramics, powder metallurgy in the manufacturing of electronic technology, chemical industry, metallic substance.During for example with norbide super-fine powder preparation pottery, can be at a lower temperature, in the short time sintering, thereby obtain the effect of the sintered compact of finer and close careful weave construction.
Because norbide hardness is very high, the processing of its super-fine powder just becomes current technical barrier.Working method mainly contains (1) general milling method at present; (2) high-energy stirring ball mill method; (3) comminution by gas stream.High-energy stirring ball mill has the high advantage of crush efficiency, but ball milling, mill cylinder are required height, also has some problems on the technology, still is in the laboratory study stage so far.
Comminution by gas stream carries out after general milling is ground into certain particle size.Though comminution by gas stream can obtain super-fine powder, and the impurity of bringing into is few; But test points out that one time comminution by gas stream is difficult to obtain a large amount of super-fine powder, need pulverize repeatedly through 5-6 time just can reach granularity requirements.Comminution by gas stream needs a large amount of dust arrester installations, and the number of occurrence of pulverizing is many more, and energy expenditure is just high more, and the loss of being ground material will sharply increase.Comminution by gas stream prepares the norbide super-fine powder, and is also at the experimental stage at present, and the suitability for industrialized production that is unrealized.
Still the common wet ball grinding that really can enter commercial production scale prepares the technology of super-fine powder.It has advantages such as cost is low, output is big, preparation technology is simple, but exists impurity (mainly being iron) content height, and removal of impurities, sorting, dewatering time are long, many shortcomings such as other impurity in the raw material (as the uncombined carbon in the norbide) clearance is low.The present invention overcomes the new norbide super-fine powder complete processing that these shortcomings propose.
Summary of the invention
When a kind of particle diameter of material all can be called ultramicron at the several microns particles in the monoatomic broad range.The present invention a kind ofly is processed into the technology that granularity is lower than the super-fine powder of 2 μ m with norbide.Its technical process has adopted circulation ball-grinding outside of cylinder, centrifugal settling dehydration to purify and three kinds of complete processings of combining of dehydrated alcohol dispersion vacuum and low temperature oven dry as shown in drawings, has reached and has enhanced productivity, the purpose of improving the quality of products.
Technical scheme of the present invention is achieved in that
The first cylinder outer circulation wet ball grinding technology that adopts is to be the boron carbide raw material of 30 μ m-44 μ m with granularity, adds the DC dispersion agent of entry and 0.3%, and ore milling concentration is 55-65%, is driven in the agitated ball mill with pump.The filling ratio of abrading-ball is 65%, and ratio of grinding media to material remains (2.5-4.5) in the ball mill cylinder: 1, and the ball amount kept 1: 1 with the ratio of total stuff amount.In the mechanical milling process, slip is squeezed into from the bottom of ball mill by recycle pump, is discharged in the circulation basin by ball mill top.Through 8-12 hour circulation ball-grinding outside of cylinder, raw meal particle size was levigate extremely less than 4 μ m.
Circulation ball-grinding outside of cylinder has prolonged the ball milling cycle, has increased the feeding quantity in the one-period, has saved charging, discharging time, has avoided in the stirring ball-milling process in the ball milling cylinder because of stirring the dead angle that produces not in place material evenly being ground, and grinds epigranular.Compare with general milling operation reaching and improve two times of work efficiency under the situation of same abrasive grain.
Material behind ball milling contains the iron contamination of the 10-20% that has an appointment, need carry out chemical subtraction.This has just entered the technological process that centrifugal settling dehydration of the present invention purifies.Under agitation condition, add hydrochloric acid or sulfuric acid etc. according to iron content and the excessive 6-12% of acid-respons stoichiometric number.Stirred 1 hour, natural subsidence 12 hours makes iron enter into solution with the ionic form.Supernatant liquor is extracted out, and remaining slip is put into the centrifugal settling water extracter and is washed twice, each washing time 40 minutes.In dehydration, utilize the density difference of norbide and uncombined carbon that uncombined carbon is further separated.Can be in dehydration most of separated the removing of uncombined carbon in norbide.Further purified the norbide super-fine powder.Shortened the washing dehydration time greatly, each washing can be saved 11 hours, improved 12 times of work efficiency.Norbide super-fine powder after the washing is added subsider, adopt conventional settling process classification, granularity accounts for 30% of the total amount that feeds intake less than the super-fine powder of 2 μ m.With the granularity of classification of sedimentation less than the qualified super-fine powder slurries of 2 μ m, after being pumped into centrifugal settling water extracter dehydrating and removing impurities matter, material cake moisture about 20%; Greater than the slip of 2 μ m also through return after the centrifugal settling dehydration circulation ball-grinding outside of cylinder machine again row grind.
If directly particle diameter is sent to oven dry less than the material cake of 2 μ m, will make powder produce caking, do not meet the requirement of user to the powder shatter value, the present invention proposes the technology that dehydrated alcohol disperses, vacuum and low temperature is dried for addressing this problem.Be that the dehydrated alcohol that adds the 20%-40% of inventory in the norbide ultra micro powder cake after the centrifugal settling dehydration carries out moistening dispersion, put into vacuum drying oven then; The vacuum tightness of control vacuum drying oven is lower than 0.095MPa, and drying temperature is 90-120 ℃ dried more than 4 hours, can obtain not having the super-fine powder of caking.
Not dry and hard, the good dispersity of norbide super-fine powder by the present invention's processing obtains brings convenience to the users.Production efficiency improves 2 times than ordinary method, and yield is greater than 90%, and purity improves.
Description of drawings
Fig. 1 is norbide super-fine powder preparation flow figure.
Embodiment
The raw material of selecting for use is the norbide meal of 30 μ m-44 μ m granularities, free carbon content 2.72%.This raw material 200kg is added in the circulation bucket, add dispersion agent 0.3%, add water 100kg and stir, squeeze in the agitated ball mill with recycle pump.Ball filling ratio 65%, ratio of grinding media to material is 3: 1 in the cylinder, ore milling concentration 55%, circulation ball-grinding outside of cylinder 11 hours.To grind the back feed liquid and squeeze into pickling tank, add the 20kg vitriol oil, stir sedimentation 12 hours 1 hour.Supernatant liquor is put into neutralization tank.The bottom slurry is put into the centrifugal settling water extracter, add water washing, liquid-solid ratio is 1.5.Start whizzer, norbide is deposited on the centrifuge drum wall, and uncombined carbon is suspended in the water in the material, and water is extracted out with suction pipe.Washed twice like this, washing lotion acidity can reach pH=6～6.5.Each washing time 40 minutes.The norbide that is deposited on the rotatory drum wall is moved into subsider, adding water stirred 30 minutes, sedimentation 10 hours, extract middle part suspension to the centrifugal settling water extracter after the dehydration, norbide ultra micro powder cake is taken out, put into Stainless Steel Disc, after adding 40kg ethanol is done the moistening dispersion of dispersion agent, put into vacuum drying oven.At vacuum tightness 0.095MPa, temperature was dried 5 hours down for 100 ℃, promptly obtained loose non-caking high-quality norbide super-fine powder product.
The product chemical analysis results:
B
4C:95.6% B
Always: 77.5% B
2O
3: 0.2% C
Always: 22.12%
C
Trip: 1.4% Fe
2O
3: 0.5%
The product granularity detected result:
Median diameter: 0.84 μ m
State diameter: 1.19 μ m
Specific surface area: 19.64m
2/ g.
Claims (1)
1, a kind of preparation method of norbide super-fine powder is characterized in that this method is purified by circulation ball-grinding outside of cylinder, centrifugal settling dehydration and dehydrated alcohol disperses three steps in sequence operations of vacuum and low temperature oven dry to realize:
1. circulation ball-grinding outside of cylinder, adopt the boron carbide raw material of 30-44 μ m, the dispersion agent that adds entry and 0.3%, ore milling concentration is 55-65%, the filling ratio of abrading-ball is 65%, and ratio of grinding media to material keeps 2.5-4.5 than 1 in the ball mill cylinder, and ball amount and total stuff amount were than 1: 1, through 8-12 hour circulation ball-grinding outside of cylinder, raw meal particle size was levigate extremely less than 4 μ m;
2. the centrifugal settling dehydration purifies, through the material behind the ball milling under agitation condition, add hydrochloric acid or sulfuric acid according to iron and the excessive 6-12% of acid-respons stoichiometric number, stirred 1 hour, natural subsidence 12 hours, the super-fine powder slip that settles down is put into the centrifugal settling water extracter carry out twice washing, to remove de-iron and uncombined carbon; Super-fine powder slip classification in subsider after the washing is obtained norbide super-fine powder less than 2 μ m, in the centrifugal settling water extracter, dewater then, obtain the norbide ultra micro powder cake of granularity less than 2 μ m;
3. dehydrated alcohol disperses the vacuum and low temperature oven dry, and the material cake after dehydration adds the dehydrated alcohol of quality of material 20-40% and makes dispersion agent, puts into vacuum drying oven, and oven dry is more than 4 hours under vacuum tightness is lower than 0.095MPa, temperature 90-120 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03133314 CN1231415C (en) | 2003-05-19 | 2003-05-19 | Preparation method of boron carbide ultramicropowder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03133314 CN1231415C (en) | 2003-05-19 | 2003-05-19 | Preparation method of boron carbide ultramicropowder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1460640A CN1460640A (en) | 2003-12-10 |
| CN1231415C true CN1231415C (en) | 2005-12-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 03133314 Expired - Fee Related CN1231415C (en) | 2003-05-19 | 2003-05-19 | Preparation method of boron carbide ultramicropowder |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101823714A (en) * | 2010-05-21 | 2010-09-08 | 牡丹江金钢钻碳化硼有限公司 | Preparation method of boron carbide powder with high specific surface area |
| CN102735025A (en) * | 2011-04-12 | 2012-10-17 | 陆宏卿 | Healing sponge drying process |
| CN102432014B (en) * | 2011-10-17 | 2013-08-28 | 宁波伏尔肯机械密封件制造有限公司 | Preparation method of submicron carbonized boron powder |
| CN104475213A (en) * | 2014-11-10 | 2015-04-01 | 张藜泷 | Method for preparing ultra-fine Hetian jade powder |
| CN105693250B (en) * | 2016-01-22 | 2018-08-28 | 东北大学 | A method of preparing boron carbide Ultramicro-powder with sapphire smooth grinding slug |
| CN105540591B (en) * | 2016-02-03 | 2018-03-06 | 东北大学 | The preparation method of multi items boron carbide micro powder |
| CN108101059A (en) * | 2018-02-10 | 2018-06-01 | 潍坊锐能新材料技术有限公司 | A kind of production technology and process units of ultra tiny boron carbide micro powder |
| CN109482288B (en) * | 2018-11-28 | 2020-11-20 | 中建材（合肥）粉体科技装备有限公司 | Method for measuring particle size distribution of fine powder in material bed extrusion crushing material cake |
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2003
- 2003-05-19 CN CN 03133314 patent/CN1231415C/en not_active Expired - Fee Related
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| CN1460640A (en) | 2003-12-10 |
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Owner name: DALIAN JIALIDE NEW MATERIALS CO., LTD.; NORTHEAST Free format text: FORMER OWNER: DALIAN JUXIN SUPERHARD MATERIALS CO., LTD.; NORTHEASTERN UNIVERSITY Effective date: 20070824 |
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Owner name: DUNHUA ZHENGXING ABRASIVE CO., LTD.; NORTHEASTERN Free format text: FORMER OWNER: DALIAN JIALIDE NEW MATERIALS CO., LTD.; NORTHEASTERN UNIVERSITY Effective date: 20080613 |
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Effective date of registration: 20080613 Address after: 4, industrial road, development zone, Dunhua, Jilin Province, zip code: 133700 Co-patentee after: Northeastern University Patentee after: Abrasives Co., Ltd. Dunhua Zheng Xing Address before: Liaoning province Dalian Dalian Development Zone wins Zhenjiang village village zip code: 116100 Co-patentee before: Northeastern University Patentee before: Dalian jialide New Material Co., Ltd. |
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Granted publication date: 20051214 Termination date: 20120519 |