CN106006658B - A kind of unpowered method for continuously synthesizing amorphous element boron - Google Patents
A kind of unpowered method for continuously synthesizing amorphous element boron Download PDFInfo
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- CN106006658B CN106006658B CN201510500484.0A CN201510500484A CN106006658B CN 106006658 B CN106006658 B CN 106006658B CN 201510500484 A CN201510500484 A CN 201510500484A CN 106006658 B CN106006658 B CN 106006658B
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 15
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 49
- 238000006243 chemical reaction Methods 0.000 claims abstract description 46
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000005554 pickling Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000010924 continuous production Methods 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 7
- 230000001902 propagating effect Effects 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 229910001018 Cast iron Inorganic materials 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 description 10
- 238000005265 energy consumption Methods 0.000 description 5
- ZOCHARZZJNPSEU-UHFFFAOYSA-N diboron Chemical compound B#B ZOCHARZZJNPSEU-UHFFFAOYSA-N 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 239000011777 magnesium Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 2
- 229910000851 Alloy steel Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002801 charged material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000026030 halogenation Effects 0.000 description 1
- 238000005658 halogenation reaction Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- -1 nuclear industry Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Physical Or Chemical Processes And Apparatus (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention discloses a kind of unpowered methods for continuously synthesizing amorphous element boron.Using homemade continuous high-temperature reacting furnace as synthesis device, using magnesium powder and diboron trioxide as raw material, self-propagating reaction is carried out under the conditions of 700-1200 DEG C, obtains purity in the amorphous element boron of 85-92%, and realize the unpowered continuous production of product under the high temperature conditions.By magnesium powder and diboron trioxide in mass ratio 1:1-1:After 3 are sufficiently mixed 2-4 hours, it charges material into multiple reaction vessels, reaction vessels are cast iron reaction utensil, the 3-5 reaction utensils equipped with material are put into high temperature furnace, after in-furnace temperature reaches setting temperature, heating is closed, continuous production is carried out by the heat of material self-propagating reaction in each reaction utensil, reacting rear material obtains partial size in 1-5 μm of amorphous element boron through pickling, washing, drying.
Description
Technical field
The invention discloses one kind using homemade continuous high-temperature reacting furnace as the unpowered continuous conjunction of synthesis device high temperature
At the method for amorphous element boron.
Background technique
Amorphous element boron is mainly used in metallurgy, electronics, medicine, ceramics, nuclear industry, chemical industry etc., with the shape of compound
Formula application is added in alloy as additional material.It can be used for the smelting of special steel alloy and the gas removing agent of molten steel, electronics
In industry in the ignitor of ignitron, the control rod in atomic pile and rocket high-energy fuel；It is the high-purity halogenation of manufacture
The important source material of boron is the raw material for producing a variety of borides；It can replace and save metal a large amount of valuable and that alkene is scarce；Boron and its
Compound also acts as the catalyst etc. of organic chemical reactions.With the continuous expansion of amorphous element boron application field and demand
Amount constantly expands, and high quality, low cost, the synthetic route of low energy consumption become the direction of scientific and technical personnel's research, currently, synthesis is without fixed
The method of shape element boron be interval self-spread synthesizing method, energy consumption is larger in the synthesis process, in process of production blow-on and
Energy waste is big in furnace shutting down process, increases the production cost of product.
Use magnesium powder and diboron trioxide for raw material the present invention provides a kind of, in homemade continuous high-temperature reacting furnace
It is continuously synthesized under the conditions of 700-1200 DEG C, has obtained amorphous element boron product.
Summary of the invention
The present invention is used as synthesis device using homemade continuous high-temperature reacting furnace, using magnesium powder and diboron trioxide as former
Material carries out self-propagating reaction under the conditions of 700-1200 DEG C, obtains purity in the amorphous element boron of 85-92%, and realize production
The unpowered continuous production of product under the high temperature conditions.By magnesium powder and diboron trioxide in mass ratio 1:1-1:3 to be sufficiently mixed 2-4 small
Shi Hou is charged material into multiple reaction vessels, and reaction vessels are cast iron reaction utensil, and the 3-5 reaction utensils equipped with material are put
Enter in high temperature furnace, after in-furnace temperature reaches setting temperature, closes heating, pass through material self-propagating reaction in each reaction utensil
Heat carries out continuous production, and it is amorphous in 85-92% in 1-5 μm, purity that reacting rear material through pickling, washing, drying obtains partial size
Element boron.
（1）Magnesium powder is used to react to have obtained without fixed in continuous high-temperature reacting furnace high temperature with diboron trioxide for raw material
Shape element boron, product purity is in 85-92%.
（2）In continuous high-temperature reacting furnace, by lighting material in reaction utensil one by one, the self- propagating of each material is released
Energy provides heat for system to realize continuous unpowered production, reduces energy consumption and production cost.
The technical scheme is that：A kind of unpowered method for continuously synthesizing amorphous element boron, steps are as follows：
(1) material mixes：In mass ratio 1:1-1:Magnesium powder is placed in batch mixer with diboron trioxide and mixes 2-4 hours by 3,
It is spare；
(2) unpowered continuously to synthesize amorphous element boron：Mixed material in step (1) is placed in reaction utensil, it will
No less than 3 reaction utensils are placed in continuous high-temperature reacting furnace, open heating, when in-furnace temperature is 700-1200 DEG C, are closed
Stove heating is reacted, the material in first reaction utensil is lighted, takes out the material in first reaction utensil after self- propagating while hot
It is put into second reaction utensil with material, after temperature is down to 700-1200 DEG C, lights the material in second reaction utensil, self- propagating
After take out material while hot and be put into the third reaction utensil with material, carry out continuous production slightly amorphous element in this way
Boron；
(3) pickling, washing and drying：Thick amorphous element boron after reaction is subjected to pickling with hydrochloric acid heating, washs 2-
10 hours crush, and filter thick amorphous element boron, then be washed with deionized, are dried to obtain fluffy brown ceramic powder,
As boron content 85-92%, the amorphous element boron that partial size is 1-5 μm.
The continuous high-temperature reacting furnace is that improved Muffle furnace is provided with more wherein being equipped with heating device in furnace body
A fire door.
The beneficial effects of the invention are as follows：It is produced, is solved among original technique using serialization high temperature synthesizer
The higher problem of production energy consumption of having a rest, in existing equipment production technology, production need to preheat reaction utensil material every time, increase the energy
Consumption, and continuous production some months can be achieved in this method, reduce production cost.
Detailed description of the invention
Attached drawing is continuous high temperature reacting furnace used in the present invention.
Specific embodiment
Below in conjunction with attached drawing and technical solution, a specific embodiment of the invention is further illustrated.
Embodiment 1
50 kilograms of magnesium powders and 100 kilograms of diboron trioxides are put into batch mixer and are sufficiently mixed 4 hours, by object after mixing
Material is added in 3 reaction utensils and is put into continuous high-temperature reacting furnace, is arranged 900 DEG C of in-furnace temperature, after temperature reaches set temperature
Heating is closed, material in first reaction utensil is lighted, reaction utensil is taken out after burning, and is put into one and is newly reacted equipped with material
Ware closes fire door, lights the second disk material after temperature reaches 900 DEG C, so recycles.Reacting rear material is through pickling, washing, mistake
Brown ceramic powder is obtained after filter drying, is amorphous element boron.
Embodiment 2
50 kilograms of magnesium powders and 100 kilograms of diboron trioxides are put into batch mixer and are sufficiently mixed 3 hours, by object after mixing
Material is added in 3 reaction utensils and is put into continuous high-temperature reacting furnace, is arranged 800 DEG C of in-furnace temperature, after temperature reaches set temperature
Heating is closed, material in first reaction utensil is lighted, reaction utensil is taken out after burning, and is put into one and is newly reacted equipped with material
Ware closes fire door, lights the second disk material after temperature reaches 800 DEG C, so recycles.Reacting rear material is through pickling, washing, mistake
Brown ceramic powder is obtained after filter drying, is amorphous element boron.
Embodiment 3
50 kilograms of magnesium powders and 150 kilograms of diboron trioxides are put into batch mixer and are sufficiently mixed 3 hours, by object after mixing
Material is added in 3 reaction utensils and is put into continuous high-temperature reacting furnace, is arranged 800 DEG C of in-furnace temperature, after temperature reaches set temperature
Heating is closed, material in first reaction utensil is lighted, reaction utensil is taken out after burning, and is put into one and is newly reacted equipped with material
Ware closes fire door, lights the second disk material after temperature reaches 800 DEG C, so recycles.Reacting rear material is through pickling, washing, mistake
Brown ceramic powder is obtained after filter drying, is amorphous element boron.
Embodiment 4
50 kilograms of magnesium powders and 100 kilograms of diboron trioxides are put into batch mixer and are sufficiently mixed 3 hours, by object after mixing
Material is added in 3 reaction utensils and is put into continuous high-temperature reacting furnace, is arranged 700 DEG C of in-furnace temperature, after temperature reaches set temperature
Heating is closed, material in first reaction utensil is lighted, reaction utensil is taken out after burning, and is put into one and is newly reacted equipped with material
Ware closes fire door, lights the second disk material after temperature reaches 700 DEG C, so recycles.Reacting rear material is through pickling, washing, mistake
Brown ceramic powder is obtained after filter drying, is amorphous element boron.
Produce comparison table
| Embodiment | Boron content % | Free boron（B2O3）% | Granularity（d50, μm） |
| Embodiment 1 | 87.9 | 0.05 | 1.5 |
| Embodiment 2 | 90.7 | 0.08 | 3.6 |
| Embodiment 3 | 90.2 | 0.15 | 4.9 |
| Embodiment 4 | 91.5 | 0.15 | 2.8 |
Claims (2)
1. a kind of unpowered method for continuously synthesizing amorphous element boron, which is characterized in that steps are as follows：
(1) material mixes：In mass ratio 1:1-1:Magnesium powder is placed in batch mixer with diboron trioxide and mixes 2-4 hours by 3, standby
With；
(2) unpowered continuously to synthesize amorphous element boron：Mixed material in step (1) is placed in reaction utensil, it will be many
It is placed in continuous high-temperature reacting furnace in 3 reaction utensils, opens heating, when in-furnace temperature is 700-1200 DEG C, close reaction
Stove heating, lights the material in first reaction utensil, and the material taken out in first reaction utensil while hot after self- propagating is put into
Second reaction utensil with material after temperature is down to 700-1200 DEG C, lights the material in second reaction utensil, and self- propagating terminates
It takes out material while hot afterwards and is put into reaction utensil of the third with material, carry out continuous production slightly amorphous element boron in this way；
(3) pickling, washing and drying：Heating in hydrochloric acid is added in thick amorphous element boron after reaction and carries out pickling, washs 2-
10 hours crush, and filter thick amorphous element boron, then be washed with deionized, are dried to obtain fluffy brown ceramic powder,
As boron content 85-92%, the amorphous element boron that partial size is 1-5 μm.
2. the method according to claim 1, wherein the continuous high-temperature reacting furnace is improved Muffle
Furnace is provided with multiple fire doors in furnace body wherein being equipped with heating device.
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| CN201510500484.0A CN106006658B (en) | 2015-08-14 | 2015-08-14 | A kind of unpowered method for continuously synthesizing amorphous element boron |
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| CN106006658A CN106006658A (en) | 2016-10-12 |
| CN106006658B true CN106006658B (en) | 2018-11-27 |
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| CN115784819A (en) * | 2022-11-29 | 2023-03-14 | 天元航材(营口)科技股份有限公司 | Preparation method of amorphous element boron for high-energy boron-containing oxygen-deficient propellant |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863662A (en) * | 2010-07-15 | 2010-10-20 | 武汉工程大学 | Method for preparing nano boron powder |
| CN102491358A (en) * | 2011-12-13 | 2012-06-13 | 吉林九安硼业有限责任公司 | Novel method for preparing amorphous boron powder in tube furnace by taking cut magnesium powder as reducing agent |
| KR20160053831A (en) * | 2014-11-05 | 2016-05-13 | 하나에이엠티 주식회사 | Preparation Method of Boron particles by using Self-propagating High-temperature Synthesis(SHS) |
-
2015
- 2015-08-14 CN CN201510500484.0A patent/CN106006658B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101863662A (en) * | 2010-07-15 | 2010-10-20 | 武汉工程大学 | Method for preparing nano boron powder |
| CN102491358A (en) * | 2011-12-13 | 2012-06-13 | 吉林九安硼业有限责任公司 | Novel method for preparing amorphous boron powder in tube furnace by taking cut magnesium powder as reducing agent |
| KR20160053831A (en) * | 2014-11-05 | 2016-05-13 | 하나에이엠티 주식회사 | Preparation Method of Boron particles by using Self-propagating High-temperature Synthesis(SHS) |
Non-Patent Citations (1)
| Title |
|---|
| 镁热还原法制备无定形硼粉与工业化;潘波涛;《中国优秀硕士论文数据库》;20051231;第17页 * |
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Application publication date: 20161012 Assignee: Zhongguancun Technology Leasing Co.,Ltd. Assignor: Tianyuan aviation materials (Yingkou) Technology Co.,Ltd. Contract record no.: X2021980014334 Denomination of invention: A method for continuous synthesis of amorphous element boron without power Granted publication date: 20181127 License type: Exclusive License Record date: 20211208 |
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