CN110217803A - A kind of system and method preparing long brilliant grade primary oxidation boron - Google Patents
A kind of system and method preparing long brilliant grade primary oxidation boron Download PDFInfo
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- CN110217803A CN110217803A CN201910574693.8A CN201910574693A CN110217803A CN 110217803 A CN110217803 A CN 110217803A CN 201910574693 A CN201910574693 A CN 201910574693A CN 110217803 A CN110217803 A CN 110217803A
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910052796 boron Inorganic materials 0.000 title claims abstract description 29
- 230000003647 oxidation Effects 0.000 title claims abstract description 26
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims description 51
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 347
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 165
- 230000018044 dehydration Effects 0.000 claims abstract description 80
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 80
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000004327 boric acid Substances 0.000 claims abstract description 27
- 229910001873 dinitrogen Inorganic materials 0.000 claims abstract description 17
- 238000010438 heat treatment Methods 0.000 claims abstract description 17
- 238000012545 processing Methods 0.000 claims abstract description 14
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 43
- 229910052810 boron oxide Inorganic materials 0.000 claims description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 239000000463 material Substances 0.000 claims description 31
- 230000008569 process Effects 0.000 claims description 29
- VGTPKLINSHNZRD-UHFFFAOYSA-N oxoborinic acid Chemical compound OB=O VGTPKLINSHNZRD-UHFFFAOYSA-N 0.000 claims description 20
- 238000003860 storage Methods 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 19
- 238000007667 floating Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 230000000694 effects Effects 0.000 claims description 8
- 238000004090 dissolution Methods 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 5
- 235000021050 feed intake Nutrition 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000003708 ampul Substances 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 8
- 229960002645 boric acid Drugs 0.000 description 31
- 235000010338 boric acid Nutrition 0.000 description 31
- 239000000047 product Substances 0.000 description 11
- 239000013078 crystal Substances 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000010586 diagram Methods 0.000 description 8
- 238000002360 preparation method Methods 0.000 description 7
- 239000000428 dust Substances 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000004065 semiconductor Substances 0.000 description 5
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 4
- 229910011255 B2O3 Inorganic materials 0.000 description 4
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 230000036541 health Effects 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 238000011109 contamination Methods 0.000 description 3
- 238000010924 continuous production Methods 0.000 description 3
- 239000000498 cooling water Substances 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 230000002265 prevention Effects 0.000 description 3
- 238000006424 Flood reaction Methods 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000008400 supply water Substances 0.000 description 2
- 238000009423 ventilation Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- ZADPBFCGQRWHPN-UHFFFAOYSA-N boronic acid Chemical compound OBO ZADPBFCGQRWHPN-UHFFFAOYSA-N 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000012938 design process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B35/00—Boron; Compounds thereof
- C01B35/08—Compounds containing boron and nitrogen, phosphorus, oxygen, sulfur, selenium or tellurium
- C01B35/10—Compounds containing boron and oxygen
- C01B35/1027—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Drying Of Gases (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
A kind of system preparing long brilliant grade primary oxidation boron, comprising: primary dewatering furnace, second level dehydration furnace and the vacuum heat-preserving furnace being sequentially connected from top to bottom；Primary dewatering furnace is equipped with hopper, nitrogen inlet duct, decelerating motor, vacuum tube, thermometric TC, feeding switch and spiral hot wind air deflector；It is communicated by feeding switch with primary dewatering furnace at the top of second level dehydration furnace, is equipped with vacuum tube, thermometric TC, nitrogen inlet duct road, feeding switch, multistage flow damper and blower；Vacuum heat-preserving furnace roof portion is communicated by feeding switch with second level dehydration furnace, and spiral shape heating wire, thermometric TC, air gauge and vacuum tube are equipped with；Nitrogen gas processing equipment；Nitrogen gas processing equipment is equipped with booster pump, duct insert heater and nitrogen clean room；Nitrogen clean room is equipped with nitrogen outlet, is connected respectively with two nitrogen inlet duct roads by triple valve；Vacuum supervisor；Vacuum supervisor is equipped with condenser and filter core.The system can avoid foreign substance pollution, continuity is good, stability is high to the full and uniform dehydration of boric acid.
Description
Technical field
The present invention relates to boron oxide synthesis technical fields, are to be related to a kind of prepare to grow brilliant grade primary oxidation more specifically
The system and method for boron.
Background technique
In recent years, gallium arsenide semiconductor is in great demand in luminescent device and high-frequency element, in the industry company in addition to actively expanding production,
The promotion of crystal yields also pushes production capacity expansion to meet the market demand for very big.Currently, the crystal of domestic production GaAs is raw
Long yields is generally 70% hereinafter, there are obvious gaps up to 80% or more with the crystal growth yields of external the relevant technologies；
Therefore, exploitation new technology is to improve the crystal growth yields of GaAs, and then improves semiconductor crystal electrical property as ability
Field technique personnel technical problem urgently to be resolved.
As the important source material of arsenide gallium monocrystal growth, high-purity boron oxide has the crystal growth yields for improving GaAs
It plays an important role.But the dewatering process of starting boronic acid is very simple and crude in the preparation method of high-purity boron oxide in the prior art, tool
Body are as follows: by hydrolysis high-purity boracic acid mixed liquor successively through filtering, 100 DEG C of evaporation dryings, obtain primary dewatering high-purity boracic acid, then use
The flat stainless steel pallet sabot of 40cm × 30cm is successively cooled to through 110 DEG C~160 DEG C baking box baking 8h~14h, standings
Room temperature obtains dry high-purity boracic acid packaging and ties up；Although the technique equipment cost low (only use baking box), easy to operate,
It is to have the disadvantage in that
(1) time-consuming, and average baking time about 12 hours；(2) dehydration is uneven and insufficient, due to flat stainless steel support
The primary dewatering high-purity boracic acid inconvenience that disk is placed is stirred, and only leans on long-time baking dehydration, agglomeration part or material block internal anhydro are not
Sufficiently, expect outside block or the raw material of porous spot is then relatively dry；(3) foreign substance pollution hidden danger, since baking box fails shape
At vacuum environment, easily lead to the contaminant overstandards such as aluminium, iron, calcium under micro dust environment；Importantly, boric acid dehydration is insufficient
Caused subsequent technique defect, specifically includes:
1. boron oxide is lost serious when preparing long brilliant grade boric oxide, practical prior art is insufficient since boric acid is dehydrated,
It is bubbled in platinum crucible seriously, passes through measuring and calculating, boron oxide yield only has about 50%；2. the trace water mistake in subsequent finished product boron oxide
Amount leads to long brilliant process defect, and subsequent actual (tube) length crystalline substance grade boric oxide water content is more than code requirement in prior art
200ppm, up to 300~500ppm, manufacturing process Capability index CPK value is lower than 0.5 (normal value is 1.33 or more), due to having
Trace water is measured, the boron oxide comparison low moon 10%~15% of the long brilliant rate of crystal and import Sumitomo, also results in and is higher than comparison object
15% harmomegathus pipe, every month lead to 5~10 sets of burner hearth explosion damage (10,000 yuan or so of value) using prior art boron oxide,
And object Sumitomo boron oxide is compared without the explosion burner hearth phenomenon；3. not exclusively due to boric acid dehydration, subsequent prepare high-purity long brilliant grade
Boric acid volatilization is serious under hot conditions in the burner hearth of boron oxide, cause to pour workshop and 5 μ micro dust of packing shop up to 500,000~
2000000/cubic feet severely exceeds, and long-term sucking will endanger employee's occupational health.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of system and method for preparing long brilliant grade primary oxidation boron, energy
Enough realize to boric acid sufficiently, is uniformly dehydrated, and avoids foreign substance pollution, and continuous production is good, product stability is high.
The present invention provides a kind of systems for preparing long brilliant grade primary oxidation boron, comprising:
Primary dewatering furnace, second level dehydration furnace and the vacuum heat-preserving furnace being sequentially connected from top to bottom；
Primary dewatering furnace roof portion is equipped with hopper, the first nitrogen inlet duct and decelerating motor, and side wall is equipped with the first vacuum
Pipe and the first thermometric TC, bottom are equipped with the second thermometric TC and the first feeding switch, and inside is equipped with and first nitrogen inlet duct
The spiral hot wind air deflector communicated；
It is communicated by first feeding switch with the primary dewatering furnace at the top of the second level dehydration furnace, side wall is equipped with the
Two vacuum tubes and third thermometric TC, bottom are equipped with the second nitrogen inlet duct road and the second feeding switch, and inside is equipped with multistage unhurried current
Device and the blower communicated with second nitrogen inlet duct road；
Vacuum heat-preserving furnace roof portion is communicated by second feeding switch with the second level dehydration furnace, and inside is equipped with and passes through
The spiral shape heating wire of furnace body is worn, side wall is equipped with the 4th thermometric TC, air gauge third vacuum tube；
The nitrogen gas processing equipment being connected respectively with the first nitrogen inlet duct road and the second nitrogen inlet duct road；At the nitrogen
It manages device and is successively arranged booster pump, duct insert heater and nitrogen clean room along nitrogen flow direction；The nitrogen clean room is equipped with
Nitrogen outlet, the nitrogen outlet are connected with the first nitrogen inlet duct road and the second nitrogen inlet duct road respectively by triple valve；
The vacuum supervisor being connected respectively with the first vacuum tube, the second vacuum tube and third vacuum tube；The vacuum supervisor sets
There is condenser and the filter core of the condenser external is set.
Preferably, the spiral hot wind air deflector includes:
The nitrogen water conservancy diversion supervisor being arranged along the central axis of the primary dewatering furnace；The nitrogen water conservancy diversion supervisor and described first
Nitrogen inlet duct communicates；
Along the integrated stirring blade of nitrogen water conservancy diversion supervisor's spiral setting；
The disc type air outlet of nitrogen water conservancy diversion supervisor bottom is set；The bottom surface of the disc type air outlet is uniformly divided
The special-shaped flow-guiding mouth that be furnished with several air-out directions opposite with the mixing direction that nitrogen water conservancy diversion is responsible for.
Preferably, the multistage flow damper includes:
Several material storage dishes being arranged alternately from top to bottom along second level dehydration furnace inner wall two sides；
The material storage dish includes: disk body；The disk body edge is equipped with frame, and the other side of connection second level dehydration furnace inner wall is set
There is the discharge port of opening constriction；
It is connected with the disk body wedge shape overflow port by the discharge port for the constriction that is open；The wedge shape overflow port is along the discharging
Mouth opening is gradually wide；
The disk body of the wedge-shaped overflow port and the material storage dish being arranged below of the material storage dish being disposed over is vertically opposite；
The number of the material storage dish is 3~6.
Preferably, the blower includes:
Air-supply supervisor；
Several blowpipes of diverging setting around the air-supply supervisor；
The blowpipe bottom closing is around evenly distributed with the downward hole of several air-out directions, hole top
Tube body be equipped with Surface of Sphere mouth；
The floating ball being placed in each blowpipe；The floating ball can place the floating ball blowpipe on
Lower movement, and Surface of Sphere mouth will not be passed through.
Preferably, the spiral shape heating wire is encapsulated by quartz ampoule.
It is described by adopting the above technical scheme to be the present invention also provides a kind of method for preparing long brilliant grade primary oxidation boron
System, comprising the following steps:
A) in a nitrogen environment, boric acid raw material is subjected to primary dewatering at 95 DEG C~150 DEG C, obtains metaboric acid；It is described
The process of primary dewatering carries out under nitrogen hot wind water conservancy diversion；
B) under vacuum-pumping conditions, metaboric acid step a) obtained carries out second level dehydration at 220 DEG C~260 DEG C, obtains
To the boron oxide of molten condition；It is de- that the process of the second level dehydration carries out depth by multistage unhurried current under high temperature nitrogen air-supply
Water；
C) boron oxide of the obtained molten condition of step b) is subjected to vacuum heat-preserving, obtains long brilliant grade primary oxidation boron.
Preferably, the process of primary dewatering described in step a) specifically:
Boric acid raw material is stirred into 30min~60min at 95 DEG C~105 DEG C, 25rpm~35rpm；Then item is being vacuumized
140 DEG C~150 DEG C are warming up under part, temperature-rise period is stirred at 40rpm~60rpm；Continue to stir 90min~120min, obtain
To metaboric acid.
Preferably, the process of the dehydration of second level described in step b) specifically:
It is kept for 220 DEG C~260 DEG C under high temperature nitrogen air-supply, feeds intake while vacuumizing, metaboric acid dissolution passes through multistage slow
Gradually overflow carries out deep dehydration 1h~2h to stream, obtains the boron oxide of molten condition.
Preferably, the temperature of vacuum heat-preserving described in step c) is 220 DEG C~250 DEG C.
Preferably, the step b) further include:
When obtaining the boron oxide of molten condition stops high temperature nitrogen air-supply, increasing high temperature nitrogen pressure rises to temperature
330 DEG C~380 DEG C, holding vacuumizes 2h~4h, improves reaction mass deep dehydration effect.
The present invention provides a kind of system and method for preparing long brilliant grade primary oxidation boron, which includes: from top to bottom
Primary dewatering furnace, second level dehydration furnace and the vacuum heat-preserving furnace being sequentially connected；Primary dewatering furnace roof portion is equipped with hopper, the first nitrogen
Gas air inlet pipe and decelerating motor, side wall are equipped with the first vacuum tube and the first thermometric TC, and bottom is equipped with the second thermometric TC and first and throws
Material switch, inside are equipped with the spiral hot wind air deflector communicated with first nitrogen inlet duct；It is logical at the top of the second level dehydration furnace
It crosses first feeding switch to communicate with the primary dewatering furnace, side wall is equipped with the second vacuum tube and third thermometric TC, and bottom is set
Have the second nitrogen inlet duct road and the second feeding switch, inside be equipped with multistage flow damper and with second nitrogen inlet duct road phase
Logical blower；Vacuum heat-preserving furnace roof portion is communicated by second feeding switch with the second level dehydration furnace, and inside is set
There is the spiral shape heating wire through furnace body, side wall is equipped with the 4th thermometric TC, air gauge and third vacuum tube；Respectively with the first nitrogen
The nitrogen gas processing equipment that air inlet pipeline and the second nitrogen inlet duct road are connected；The nitrogen gas processing equipment along nitrogen flow direction according to
It is secondary to be equipped with booster pump, duct insert heater and nitrogen clean room；The nitrogen clean room is equipped with nitrogen outlet, and the nitrogen outlet is logical
Triple valve is crossed to be connected with the first nitrogen inlet duct road and the second nitrogen inlet duct road respectively；Respectively very with the first vacuum tube, second
The vacuum supervisor that blank pipe is connected with third vacuum tube；The vacuum supervisor is equipped with condenser and the condenser external is arranged in
Filter core.Compared with prior art, system and method provided by the invention can realize boric acid and sufficiently, uniformly be dehydrated, and avoid different
Object pollution, and continuous production is good, product stability is high.The experimental results showed that system and method preparation provided by the invention
The purity of obtained long brilliant grade primary oxidation boron is 98% or more.
Meanwhile system whole process closing provided by the invention, be conducive to the prevention of product external contamination, the long crystalline substance of semiconductor is mentioned
Good raw material has been supplied, has been to improve crystal property and stability prerequisite；The process flow of encapsulation also well prevents micro-
Dust evaporate into air the problem of occupational health for damaging employee.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the system of the long brilliant grade primary oxidation boron of preparation provided in an embodiment of the present invention；
Fig. 2 is the structural schematic diagram of spiral hot wind air deflector in the embodiment of the present invention；
Fig. 3 is the structural schematic diagram of multistage flow damper in the embodiment of the present invention；
Fig. 4 is the structural schematic diagram of blower in the embodiment of the present invention.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described, it is clear that institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Every other embodiment obtained by those of ordinary skill in the art without making creative efforts, belongs to this hair
The range of bright protection.
The present invention provides a kind of systems for preparing long brilliant grade primary oxidation boron, comprising:
Primary dewatering furnace, second level dehydration furnace and the vacuum heat-preserving furnace being sequentially connected from top to bottom；
Primary dewatering furnace roof portion is equipped with hopper, the first nitrogen inlet duct and decelerating motor, and side wall is equipped with the first vacuum
Pipe and the first thermometric TC, bottom are equipped with the second thermometric TC and the first feeding switch, and inside is equipped with and first nitrogen inlet duct
The spiral hot wind air deflector communicated；
It is communicated by first feeding switch with the primary dewatering furnace at the top of the second level dehydration furnace, side wall is equipped with the
Two vacuum tubes and third thermometric TC, bottom are equipped with the second nitrogen inlet duct road and the second feeding switch, and inside is equipped with multistage unhurried current
Device and the blower communicated with second nitrogen inlet duct road；
Vacuum heat-preserving furnace roof portion is communicated by second feeding switch with the second level dehydration furnace, and inside is equipped with and passes through
The spiral shape heating wire of furnace body is worn, side wall is equipped with the 4th thermometric TC, air gauge and third vacuum tube；
The nitrogen gas processing equipment being connected respectively with the first nitrogen inlet duct road and the second nitrogen inlet duct road；At the nitrogen
It manages device and is successively arranged booster pump, duct insert heater and nitrogen clean room along nitrogen flow direction；The nitrogen clean room is equipped with
Nitrogen outlet, the nitrogen outlet are connected with the first nitrogen inlet duct road and the second nitrogen inlet duct road respectively by triple valve；
The vacuum supervisor being connected respectively with the first vacuum tube, the second vacuum tube and third vacuum tube；The vacuum supervisor sets
There is condenser and the filter core of the condenser external is set.
Referring to Fig. 1, Fig. 1 is the structural representation of the system of the long brilliant grade primary oxidation boron of preparation provided in an embodiment of the present invention
Figure；Wherein, 1 is primary dewatering furnace for 1, and 2 be second level dehydration furnace, and 3 be vacuum heat-preserving furnace, and 4 be hopper, and 5 be the first nitrogen air inlet
Pipe, 6 be decelerating motor, and 7 be the first vacuum tube, and 8 be the first thermometric TC, and 9 be the second thermometric TC, and 10 be the first feeding switch, 11
It is the second vacuum tube for spiral hot wind air deflector, 12,13 be third thermometric TC, and 14 be the second nitrogen inlet duct road, and 15 be second
Feeding switch, 16 be multistage flow damper, and 17 be blower, and 18 be spiral shape heating wire, and 19 be the 4th thermometric TC, and 20 be air pressure
Table, 21 be third vacuum tube, and 22 be nitrogen gas processing equipment, and 23 be booster pump, and 24 be duct insert heater, and 25 be nitrogen clean room,
26 be nitrogen outlet, and 27 be triple valve, and 28 are responsible for for vacuum, and 29 be condenser, and 30 be filter core；A is nitrogen, and b is to vacuumize, c
For cooling water.
In the present invention, the system of the long brilliant grade primary oxidation boron of the preparation includes that the primary being sequentially connected from top to bottom takes off
Water furnace (1), second level dehydration furnace (2) and vacuum heat-preserving furnace (3) and nitrogen gas processing equipment (22), vacuum supervisor (28).In this hair
In bright, the primary dewatering furnace (1) is used to carry out primary dewatering to boric acid raw material；The present invention is not special to the boric acid raw material
Limitation, using filtered hydrolysis high-purity boracic acid well known to those skilled in the art.
In the present invention, the furnace body of the primary dewatering furnace (1) is cone cylindrical cavity structure, and outside is insulating layer, can
Avoid heat loss.
In the present invention, hopper (4), the first nitrogen inlet duct (5) and the electricity that slows down are equipped at the top of the primary dewatering furnace (1)
Machine (6)；Hopper (4) the band vacuum, for being fed；First nitrogen inlet duct (5) is used to nitrogen being passed through primary dewatering
Furnace (1) furnace body；The decelerating motor (6) is used to provide stirring power for spiral hot wind air deflector (11).
In the present invention, primary dewatering furnace (1) side wall is equipped with the first vacuum tube (7) and the first thermometric TC (8)；It is described
The boil-off gas of primary dewatering is discharged for vacuumizing to primary dewatering furnace (1) in first vacuum tube (7)；Described first surveys
Warm TC (8) is for detecting furnace temperature, by detecting furnace temperature, adjusts duct insert heater (24) in due course to meet the requirement of production technology.
In the present invention, primary dewatering furnace (1) bottom is equipped with the second thermometric TC (9) and the first feeding switch (10)；
The second thermometric TC (9) is for detecting furnace temperature, by detecting furnace temperature, adjusts duct insert heater (24) in due course to meet production work
The requirement of skill；First feeding switch (10) is for feeding intake.
In the present invention, the spiral communicated with first nitrogen inlet duct (5) is equipped with inside the primary dewatering furnace (1)
Hot wind air deflector (11), structural schematic diagram is shown in Figure 2.In the present invention, the spiral hot wind air deflector (11) includes:
The nitrogen water conservancy diversion supervisor being arranged along the central axis of the primary dewatering furnace (1)；
Along the integrated stirring blade of nitrogen water conservancy diversion supervisor's spiral setting；
The disc type air outlet of nitrogen water conservancy diversion supervisor bottom is set.
In the present invention, the nitrogen water conservancy diversion supervisor communicates with first nitrogen inlet duct (5)；The disc type outlet air
Mouthful the bottom surface special-shaped flow-guiding mouth that be evenly distributed with several air-out directions opposite with the mixing direction that nitrogen water conservancy diversion is responsible for.
In the present invention, the spiral hot wind air deflector (11) is used for water conservancy diversion nitrogen, and nitrogen is by the first nitrogen inlet duct (5)
Through nitrogen water conservancy diversion, supervisor is finally sent out by disc type air outlet；And also there is stirring function under the effect of integrated stirring blade
Energy；In addition, the special-shaped flow-guiding mouth air-out direction and the mixing direction of nitrogen water conservancy diversion supervisor avoid particle on the contrary, can play
Shape boric acid blocks disc type air outlet, keeps supplying gas unobstructed.
The present invention ensures that primary dewatering particulate material can be stirred up and down using above-mentioned spiral hot wind air deflector (11), mentions significantly
High dehydration efficiency；And integral structure realizes water conservancy diversion and stirring simultaneously, strong guarantee primary dewatering furnace (1) heat utilization effect
Rate；Furthermore special-shaped flow-guiding mouth can effective guarantee stirring material when material will not be plugged air outlet.
In the present invention, de- by first feeding switch (10) and the primary at the top of the second level dehydration furnace (2)
Water furnace (1) communicates.In the present invention, the second level dehydration furnace (2) is used to feed intake that carry out second level de- to primary dewatering furnace (1)
Water.
In the present invention, the furnace body of the second level dehydration furnace (2) is cone cylindrical cavity structure, and outside is insulating layer, can
Avoid heat loss.
In the present invention, second level dehydration furnace (2) side wall is equipped with the second vacuum tube (12) and third thermometric TC (13)；Institute
The second vacuum tube (12) are stated for vacuumizing to second level dehydration furnace (2), while the boil-off gas of second level dehydration is discharged；The third
Thermometric TC (13) is for detecting furnace temperature, by detecting furnace temperature, adjusts duct insert heater (24) in due course to meet wanting for production technology
It asks.
In the present invention, second level dehydration furnace (2) bottom is equipped with the second nitrogen inlet duct road (14) and second and feeds intake out
It closes (15)；Second nitrogen inlet duct road (14) is used to nitrogen being passed through second level dehydration furnace (2) furnace body；Described second feeds intake out
(15) are closed for feeding intake.
In the present invention, be equipped with inside the second level dehydration furnace (2) multistage flow damper (16) and with second nitrogen into
The blower (17) that air pipe (14) communicates.
In the present invention, the structural schematic diagram of the multistage flow damper (16) is shown in Figure 3.In the present invention, described
Multistage flow damper (16) includes:
Several material storage dishes being arranged alternately from top to bottom along second level dehydration furnace (2) inner wall two sides；It feeds intake for accepting.
In the present invention, the material storage dish includes:
Disk body；The disk body edge is equipped with frame, and the other side of connection second level dehydration furnace (2) inner wall is equipped with opening constriction
Discharge port；
It is connected with the disk body wedge shape overflow port by the discharge port for the constriction that is open；The wedge shape overflow port is along the discharging
Mouth opening is gradually wide.
In the present invention, the wedge-shaped overflow port for the material storage dish being disposed over and the disk body for the material storage dish being arranged below hang down
It is straight opposite；The material storage dish to top layer in second level dehydration furnace (2) is accepted in feeding intake for primary dewatering furnace (1) first, is contracted by opening
Narrow discharge port control dissolved material runs underneath to next layer of material storage dish by wedge-shaped overflow port with less discharging overflow, with
This analogizes, and realizes and successively accepts；The wedge shape overflow port is open gradually wide along the discharge port, can expand material and thermal current
Contact area simultaneously extends it in the residence time of overflow port, is conducive to sufficiently be dehydrated.
In the present invention, the number of the material storage dish is preferably 3~6, more preferably 4；Multilayered structure is conducive to
The contact area to feed intake with the material storage dish of high temperature for increasing dissolution, is more advantageous to evaporation vapor.
In addition, the frame at the disk body edge is preferably set to arc-shaped, the area of material storage dish can be further increased, favorably
It is come into full contact in feeding intake with material storage dish.
In the present invention, the blower (17) communicates with second nitrogen inlet duct road (14)；Its structural schematic diagram
It is shown in Figure 4.
In the present invention, the blower (17) includes:
Air-supply supervisor；The air-supply supervisor communicates with second nitrogen inlet duct road (14)；
Several blowpipes of diverging setting around the air-supply supervisor；The blowpipe bottom closing, surrounding
It is evenly distributed with the downward hole of several air-out directions, the tube body above hole is equipped with Surface of Sphere mouth；
The floating ball being placed in each blowpipe；The floating ball can place the floating ball blowpipe on
Lower movement, and Surface of Sphere mouth will not be passed through.In the present invention, the floating ball is preferably the stainless steel ball of hollow structure.
In the present invention, blowpipe is entered by air-supply supervisor from the second nitrogen inlet duct road (14) high temperature nitrogen, and
It is sent out by hole；Floating ball is located at blowpipe bottom at this time；After the boron oxide of molten condition is continuously increased, hot wind is closed
When (high temperature nitrogen), floating ball floats to Surface of Sphere mouth, overflows so that the boron oxide of melting be avoided to be responsible for adverse current to air-supply；Also,
At this point, start booster pump (23) and heat up, until high temperature nitrogen can depress to floating ball under blower (17) air outlet, it can
Lower furnace bottom reaction mass viscosity, improves reaction mass deep dehydration effect.
In the present invention, the second level dehydration furnace (2) passes through multistage flow damper (16) effectively by the material of dissolution in foot
Pyroreaction and dehydration are carried out under enough time and bigger contact area；And it can be in multiple furnace temperature in conjunction with blower (17)
Condition carries out deep dehydration by the way that floating ball is mobile.
In the present invention, de- by second feeding switch (15) and the second level at the top of the vacuum heat-preserving furnace (3)
Water furnace (2) communicates.In the present invention, the vacuum heat-preserving furnace (3) is used to carry out vacuum heat-preserving to the boron oxide of molten condition.
In the present invention, the furnace body of the vacuum heat-preserving furnace (3) is cylinder, and both ends are hemisphere face, and outside is insulating layer,
It can be avoided heat loss.
In the present invention, the spiral shape heating wire (18) through furnace body is equipped with inside the vacuum heat-preserving furnace (3), it can be maximum
Thermal energy is utilized to limit, and keeps furnace body internal oxidition boron heated sufficiently and uniform；The spiral shape heating wire (18) preferably passes through stone
The encapsulation of English pipe.
In the present invention, it is true to be equipped with the 4th thermometric TC (19), air gauge (20) and third for vacuum heat-preserving furnace (3) side wall
Blank pipe (21)；The 4th thermometric TC (19), by the furnace temperature of detection, adjusts spiral shape heating wire for detecting furnace temperature in due course
(18) power is to meet the requirement of production technology；The air gauge (20) is for detecting furnace pressure；The third vacuum tube (21) is used
It is vacuumized in vacuum heat-preserving furnace (3), while the boil-off gas of vacuum heat-preserving is discharged.
The present invention maintains the molten condition of boron oxide using vacuum heat-preserving furnace (3), obtains long brilliant grade primary oxidation boron, and
Effectively pollution of the prevention conventional heater to long brilliant grade boric oxide, also improves utilization efficiency of heat energy；The vacuum heat-preserving furnace (3)
To boron oxide is prevented, application provides good feed states in next step for secondary water suction resurgence and entrance in air environment；It is heavier
It wants, the boron oxide that can be realized molten condition has the longer holding time, it ensure that the continuity of the design process flow,
Enable the boron oxide of the molten condition to pass through discharge port and transfer out at any time further to be applied.
In the present invention, the nitrogen gas processing equipment (22) respectively with the first nitrogen inlet duct road (5) and the second nitrogen into
Air pipe (14) is connected；For providing high-purity (high temperature) nitrogen.The present invention is not particularly limited the source of the nitrogen, uses
Industrial nitrogen well known to those skilled in the art.
In the present invention, the nitrogen gas processing equipment (22) is successively arranged booster pump (23), air duct along nitrogen flow direction
Heater (24) and nitrogen clean room (25)；The booster pump (23) is used to provide power for nitrogen conveying；The air duct heating
Device (24) uses hot air apparatus well known to those skilled in the art, can heat for nitrogen；The tune of the duct insert heater (24)
Warm range is 100 DEG C~800 DEG C, meets the heating of the required nitrogen of boric acid Dewatering reaction and supplies gas；The nitrogen purification
The preferably efficient air-supply filtration equipment for clarifying in room (25), is used for nitrogen purge gas；It is placed on duct insert heater (24), is conducive to nitrogen
The filtering for the metal microparticle that micro dust and duct insert heater (24) generate in gas, eliminates foreign polluted product.
In the present invention, the nitrogen clean room (25) is equipped with nitrogen outlet (26), and the nitrogen outlet (26) passes through three
Port valve (27) is connected with the first nitrogen inlet duct road (5) and the second nitrogen inlet duct road (14) respectively.
In the present invention, the vacuum supervisor (28) is true with the first vacuum tube (7), the second vacuum tube (12) and third respectively
Blank pipe (21) is connected；It is vacuumized by vacuum pump.In the present invention, vacuum supervisor (28) be equipped with condenser (29) and
The filter core (30) external in the condenser (29) is set；The condenser (29) is by cooling water to the first vacuum tube (7), the
The boil-off gas (boric acid, steam of high temperature etc.) that two vacuum tubes (12) and third vacuum tube (21) conveying come is condensed, thus
Realize the enrichment to high temperature boric acid and vapor gaseous mixture dirt；The external filter core (30) of the condenser (29) is for filtering
Gas dirt.
System and method provided by the invention can realize boric acid and sufficiently, uniformly be dehydrated, and avoid foreign substance pollution, and raw
Production continuity is good, product stability is high.In addition, system whole process closing provided by the invention, is conducive to the pre- of product external contamination
It is anti-, good raw material is provided to the long crystalline substance of semiconductor, is to improve crystal property and stability prerequisite；The process flow of encapsulation
Also the problem of micro dust evaporate into air the occupational health for damaging employee is well prevented.
It is described by adopting the above technical scheme to be the present invention also provides a kind of method for preparing long brilliant grade primary oxidation boron
System, comprising the following steps:
A) in a nitrogen environment, boric acid raw material is subjected to primary dewatering at 95 DEG C~150 DEG C, obtains metaboric acid；It is described
The process of primary dewatering carries out under nitrogen hot wind water conservancy diversion；
B) under vacuum-pumping conditions, metaboric acid step a) obtained carries out second level dehydration at 220 DEG C~260 DEG C, obtains
To the boron oxide of molten condition；It is de- that the process of the second level dehydration carries out depth by multistage unhurried current under high temperature nitrogen air-supply
Water；
C) boron oxide of the obtained molten condition of step b) is subjected to vacuum heat-preserving, obtains long brilliant grade primary oxidation boron.
The present invention carries out primary dewatering at 95 DEG C~150 DEG C first in a nitrogen environment, by boric acid raw material, obtains inclined boron
Acid.The present invention is not particularly limited the source of the nitrogen, using industrial nitrogen well known to those skilled in the art.This
Invention is not particularly limited the boric acid raw material, is using filtered hydrolysis high-purity boracic acid well known to those skilled in the art
It can.
In the present invention, the process of the primary dewatering carries out under nitrogen hot wind water conservancy diversion；The present invention preferably leads to nitrogen
Spiral hot wind air deflector (11) is crossed to primary dewatering furnace (1) ventilation 5min~10min, keeps the dry dustless state of burner hearth.At this
In invention, the process of the primary dewatering is preferred specifically:
Boric acid raw material is stirred into 30min~60min at 95 DEG C~105 DEG C, 25rpm~35rpm；Then item is being vacuumized
140 DEG C~150 DEG C are warming up under part, temperature-rise period is stirred at 40rpm~60rpm；Continue to stir 90min~120min, obtain
To metaboric acid；
More preferably:
Boric acid raw material is stirred into 30min~60min at 100 DEG C, 30rpm；Then it is warming up to 140 under vacuum-pumping conditions
DEG C~150 DEG C, temperature-rise period is stirred at 40rpm~60rpm；Continue to stir 90min~120min, obtains metaboric acid.
Boric acid raw material is realized that moisture is evaporated by the present invention at 95 DEG C~105 DEG C, is reacted and is generated at 140 DEG C~150 DEG C
Metaboric acid (HBO2), play the role of further being dehydrated.
After obtaining the metaboric acid, the present invention under vacuum-pumping conditions, the metaboric acid that step a) is obtained 220 DEG C~
Second level dehydration is carried out at 260 DEG C, obtains the boron oxide of molten condition.In the present invention, the process of the second level dehydration is in high temperature
Nitrogen air-supply is lower to carry out deep dehydration by multistage unhurried current.In the present invention, the process of the second level dehydration is preferred specifically:
It is kept for 220 DEG C~260 DEG C under high temperature nitrogen air-supply, feeds intake while vacuumizing, metaboric acid dissolution passes through multistage slow
Gradually overflow carries out deep dehydration 1h~2h to stream, obtains the boron oxide of molten condition；
More preferably:
It is kept for 230 DEG C~240 DEG C under high temperature nitrogen air-supply, feeds intake while vacuumizing, metaboric acid dissolution passes through multistage slow
Gradually overflow carries out deep dehydration 1h~2h to stream, obtains the boron oxide of molten condition.
The present invention realizes product reaction by the way that the boric acid of above-mentioned different conditions is dehydrated segmentation in different dehydration furnaces
Control for Kiln Temperature, it is ensured that product reaction effectively control, to guarantee abundant, uniformly dehydration.
In the present invention, the process of second level dehydration it is also preferable to include:
When obtaining the boron oxide of molten condition stops high temperature nitrogen air-supply, increasing high temperature nitrogen pressure rises to temperature
330 DEG C~380 DEG C, holding vacuumizes 2h~4h, improves reaction mass deep dehydration effect.The present invention uses above-mentioned blower
(17), the boron oxide of melting gradually floods institute's hole of blower (17) lower part air outlet, and so far, viscid reactant will be sent
Stainless steel floating ball in wind device (17) floats, and withstands Surface of Sphere mouth in pipeline；Increasing high temperature nitrogen pressure at this time rises to temperature
330 DEG C~380 DEG C, holding vacuumizes 2h~4h, improves reaction mass deep dehydration effect.
After obtaining the boron oxide of the molten condition, the boron oxide of obtained molten condition is carried out vacuum guarantor by the present invention
Temperature obtains long brilliant grade primary oxidation boron.In the present invention, the temperature of the vacuum heat-preserving is preferably 220 DEG C~250 DEG C.
The present invention provides a kind of system and method for preparing long brilliant grade primary oxidation boron, which includes: from top to bottom
Primary dewatering furnace, second level dehydration furnace and the vacuum heat-preserving furnace being sequentially connected；Primary dewatering furnace roof portion is equipped with hopper, the first nitrogen
Gas air inlet pipe and decelerating motor, side wall are equipped with the first vacuum tube and the first thermometric TC, and bottom is equipped with the second thermometric TC and first and throws
Material switch, inside are equipped with the spiral hot wind air deflector communicated with first nitrogen inlet duct；It is logical at the top of the second level dehydration furnace
It crosses first feeding switch to communicate with the primary dewatering furnace, side wall is equipped with the second vacuum tube and third thermometric TC, and bottom is set
Have the second nitrogen inlet duct road and the second feeding switch, inside be equipped with multistage flow damper and with second nitrogen inlet duct road phase
Logical blower；Vacuum heat-preserving furnace roof portion is communicated by second feeding switch with the second level dehydration furnace, and inside is set
There is the spiral shape heating wire through furnace body, side wall is equipped with the 4th thermometric TC, air gauge and third vacuum tube；Respectively with the first nitrogen
The nitrogen gas processing equipment that air inlet pipeline and the second nitrogen inlet duct road are connected；The nitrogen gas processing equipment along nitrogen flow direction according to
It is secondary to be equipped with booster pump, duct insert heater and nitrogen clean room；The nitrogen clean room is equipped with nitrogen outlet, and the nitrogen outlet is logical
Triple valve is crossed to be connected with the first nitrogen inlet duct road and the second nitrogen inlet duct road respectively；Respectively very with the first vacuum tube, second
The vacuum supervisor that blank pipe is connected with third vacuum tube；The vacuum supervisor is equipped with condenser and the condenser external is arranged in
Filter core.Compared with prior art, system and method provided by the invention can realize boric acid and sufficiently, uniformly be dehydrated, and avoid different
Object pollution, and continuous production is good, product stability is high.The experimental results showed that system and method preparation provided by the invention
The purity of obtained long brilliant grade primary oxidation boron is 98% or more.
Meanwhile system whole process closing provided by the invention, be conducive to the prevention of product external contamination, the long crystalline substance of semiconductor is mentioned
Good raw material has been supplied, has been to improve crystal property and stability prerequisite；The process flow of encapsulation also well prevents micro-
Dust evaporate into air the problem of occupational health for damaging employee.
In order to further illustrate the present invention, it is described in detail below by following embodiment.
Embodiment 1
The structural schematic diagram of the system of the long brilliant grade primary oxidation boron of the preparation that the embodiment of the present invention 1 provides is shown in Figure 1；
Wherein, 1 is primary dewatering furnace for 1, and 2 be second level dehydration furnace, and 3 be vacuum heat-preserving furnace, and 4 be hopper, and 5 be the first nitrogen inlet duct, 6
It is the first vacuum tube for decelerating motor, 7,8 be the first thermometric TC, and 9 be the second thermometric TC, and 10 be the first feeding switch, and 11 be spiral shell
Hot wind air deflector is revolved, 12 be the second vacuum tube, and 13 be third thermometric TC, and 14 be the second nitrogen inlet duct road, and 15 feed intake for second
Switch, 16 be multistage flow damper, and 17 be blower, and 18 be spiral shape heating wire, and 19 be the 4th thermometric TC, and 20 be air gauge, 21
It is nitrogen gas processing equipment for third vacuum tube, 22,23 be booster pump, and 24 be duct insert heater, and 25 be nitrogen clean room, and 26 be nitrogen
Gas outlet, 27 be triple valve, and 28 are responsible for for vacuum, and 29 be condenser, and 30 be filter core；A is nitrogen, and b is to vacuumize, and c is cooling
Water.
The course of work for preparing long brilliant grade primary oxidation boron using above system is as follows:
(1) metering of filtered hydrolysis high-purity boracic acid raw material is launched and arrives hopper (4), then be added portionwise by hopper (4)
Primary dewatering furnace (1), adds to 3kg；Then nitrogen is passed through into spiral hot wind air deflector (11) to primary dewatering furnace (1) ventilation 5min
~10min keeps the dry dustless state of burner hearth；
Start duct insert heater (24), the furnace temperature of primary dewatering furnace (1) made to reach 100 DEG C, keep 100 ± 5 DEG C of 30min~
60min；Starting decelerating motor (6) keeps spiral hot wind air deflector (11) to stir at low speed state, high purity boron at 30rpm in the process
Granulates material stirs from bottom to top under the action of spiral hot wind air deflector (11)；The process mainly completes hydrolysed filtrate
High-purity boracic acid raw material absorption moisture evaporated in 100 DEG C of normal pressure states；First thermometric TC (8) thermometric can be passed through in operational process
The furnace body thermometric variation of observation in every 10 minutes, adjusts duct insert heater (24) heat supply temperature, it is ensured that primary dewatering furnace (1) in due course
Furnace temperature meet the requirements；
Starting vacuum pump vacuumizes primary dewatering furnace (1) by vacuum supervisor (28), adjusts duct insert heater (24) function
Rate makes the furnace temperature of primary dewatering furnace (1) reach 140 DEG C~150 DEG C；Spiral hot wind air deflector (11) is persistently kept in temperature-rise period
The stirring at 40rpm~60rpm runs 90min~120min；The process, which is mainly reacted, generates metaboric acid (HBO2),
Specific reaction equation are as follows: H3BO3=HBO2+H2O。
(2) by nitrogen through blower (17) to second level dehydration furnace (1) ventilate 5min~10min, keep burner hearth drying it is dustless
State；
Start duct insert heater (24), the furnace temperature of second level dehydration furnace (2) is made to rise to 230 DEG C~240 DEG C, keeps 30min, really
It is uniform to protect multistage flow damper (16) temperature in burner hearth；Then first feeding switch (10) of primary dewatering furnace (1) bottom is opened,
With the inventory of 200g/min by metaboric acid (HBO2) put into second level dehydration furnace (2)；It feeds intake while starting vacuum pump and pass through very
Sky supervisor (28) vacuumizes second level dehydration furnace (2)；
Metaboric acid (HBO2) put into second level dehydration furnace (2) after, successively slowly flowed down through multistage flow damper (16)；The process
Deep dehydration is mainly carried out, and gradually purifies water and generates boron oxide (what is do not reacted completely partially is still metaboric acid), it is specific anti-
Answer formula are as follows: 2HBO2=B2O3+H2O；
In 1h~2h dissolution, gradually to furnace bottom, the boron oxide of melting gradually floods blower (17) lower part to 3kg raw material for overflow
Institute's hole of air outlet, so far, viscid reactant floats the stainless steel floating ball in blower (17), withstands pipeline inner circle
Spherical surface mouth；Start booster pump (23) at this time, be continuously heating to 330 DEG C~380 DEG C, until high temperature nitrogen can be by stainless steel floating ball pressure
Under blower (17) air outlet, holding vacuumizes 2h~4h；The process can lower furnace bottom reaction mass viscosity, mention
High reaction mass deep dehydration effect obtains the boron oxide of molten condition, purity 98%.
(3) starting vacuum pump vacuumizes vacuum heat-preserving furnace (3) by vacuum supervisor (28)；Pass through spiral shape heating wire again
(18) 220 DEG C~250 DEG C are warming up to；Then second feeding switch (15) of second level dehydration furnace (2) bottom is opened, by step
(2) boron oxide of the molten condition obtained puts into vacuum heat-preserving furnace (3) vacuum heat-preserving, obtains long brilliant grade primary oxidation boron；Out
High-purity boron oxide is used to prepare after material.
The above description of the disclosed embodiments, enables those skilled in the art to implement or use the present invention.It is right
A variety of modifications of these embodiments will be readily apparent to those skilled in the art, and as defined herein one
As principle can realize in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention will
It will not be intended to be limited to the embodiments shown herein, and be to fit to consistent with the principles and novel features disclosed herein
Widest scope.
Claims (10)
1. a kind of system for preparing long brilliant grade primary oxidation boron, comprising:
Primary dewatering furnace, second level dehydration furnace and the vacuum heat-preserving furnace being sequentially connected from top to bottom；
Primary dewatering furnace roof portion be equipped with hopper, the first nitrogen inlet duct and decelerating motor, side wall be equipped with the first vacuum tube and
First thermometric TC, bottom are equipped with the second thermometric TC and the first feeding switch, and inside is equipped with and communicates with first nitrogen inlet duct
Spiral hot wind air deflector；
It is communicated by first feeding switch with the primary dewatering furnace at the top of the second level dehydration furnace, it is true that side wall is equipped with second
Blank pipe and third thermometric TC, bottom are equipped with the second nitrogen inlet duct road and the second feeding switch, inside be equipped with multistage flow damper and
The blower communicated with second nitrogen inlet duct road；
Vacuum heat-preserving furnace roof portion is communicated by second feeding switch with the second level dehydration furnace, and inside, which is equipped with, runs through furnace
The spiral shape heating wire of body, side wall are equipped with the 4th thermometric TC, air gauge and third vacuum tube；
The nitrogen gas processing equipment being connected respectively with the first nitrogen inlet duct road and the second nitrogen inlet duct road；The nitrogen treatment dress
It sets and is successively arranged booster pump, duct insert heater and nitrogen clean room along nitrogen flow direction；The nitrogen clean room is equipped with nitrogen
Outlet, the nitrogen outlet are connected with the first nitrogen inlet duct road and the second nitrogen inlet duct road respectively by triple valve；
The vacuum supervisor being connected respectively with the first vacuum tube, the second vacuum tube and third vacuum tube；The vacuum supervisor is equipped with cold
Condenser and the filter core that the condenser external is set.
2. system according to claim 1, which is characterized in that the spiral hot wind air deflector includes:
The nitrogen water conservancy diversion supervisor being arranged along the central axis of the primary dewatering furnace；The nitrogen water conservancy diversion supervisor and first nitrogen
Air inlet pipe communicates；
Along the integrated stirring blade of nitrogen water conservancy diversion supervisor's spiral setting；
The disc type air outlet of nitrogen water conservancy diversion supervisor bottom is set；The bottom surface of the disc type air outlet is evenly distributed with
Several air-out directions special-shaped flow-guiding mouth opposite with the mixing direction that nitrogen water conservancy diversion is responsible for.
3. system according to claim 1, which is characterized in that it is described multistage flow damper include:
Several material storage dishes being arranged alternately from top to bottom along second level dehydration furnace inner wall two sides；
The material storage dish includes: disk body；The disk body edge is equipped with frame, and the other side of connection second level dehydration furnace inner wall, which is equipped with, opens
The discharge port of mouth constriction；
It is connected with the disk body wedge shape overflow port by the discharge port for the constriction that is open；The wedge shape overflow port is opened along the discharge port
Mouth is gradually wide；
The disk body of the wedge-shaped overflow port and the material storage dish being arranged below of the material storage dish being disposed over is vertically opposite；
The number of the material storage dish is 3~6.
4. system according to claim 1, which is characterized in that the blower includes:
Air-supply supervisor；
Several blowpipes of diverging setting around the air-supply supervisor；
The blowpipe bottom closing, is around evenly distributed with the downward hole of several air-out directions, the pipe above hole
Body is equipped with Surface of Sphere mouth；
The floating ball being placed in each blowpipe；The floating ball can place the floating ball blowpipe on move down
It is dynamic, and Surface of Sphere mouth will not be passed through.
5. system according to claim 1, which is characterized in that the spiral shape heating wire is encapsulated by quartz ampoule.
6. a kind of method for preparing long brilliant grade primary oxidation boron, which is characterized in that system described in claim 1 is used, including
Following steps:
A) in a nitrogen environment, boric acid raw material is subjected to primary dewatering at 95 DEG C~150 DEG C, obtains metaboric acid；The primary
The process of dehydration carries out under nitrogen hot wind water conservancy diversion；
B) under vacuum-pumping conditions, metaboric acid step a) obtained carries out second level dehydration at 220 DEG C~260 DEG C, is melted
Melt the boron oxide of state；The process of the second level dehydration carries out deep dehydration by multistage unhurried current under high temperature nitrogen air-supply；
C) boron oxide of the obtained molten condition of step b) is subjected to vacuum heat-preserving, obtains long brilliant grade primary oxidation boron.
7. according to the method described in claim 6, it is characterized in that, the process of primary dewatering described in step a) specifically:
Boric acid raw material is stirred into 30min~60min at 95 DEG C~105 DEG C, 25rpm~35rpm；Then under vacuum-pumping conditions
140 DEG C~150 DEG C are warming up to, temperature-rise period is stirred at 40rpm~60rpm；Continue to stir 90min~120min, obtain partially
Boric acid.
8. according to the method described in claim 6, it is characterized in that, the process of the dehydration of second level described in step b) specifically:
Kept for 220 DEG C~260 DEG C under high temperature nitrogen air-supply, feed intake while vacuumizing, metaboric acid dissolution by it is multistage flow slowly by
It walks overflow and carries out deep dehydration 1h~2h, obtain the boron oxide of molten condition.
9. according to the method described in claim 6, it is characterized in that, the temperature of vacuum heat-preserving described in step c) be 220 DEG C~
250℃。
10. according to the described in any item methods of claim 6~9, which is characterized in that the step b) further include:
When obtaining the boron oxide of molten condition stops high temperature nitrogen air-supply, increasing high temperature nitrogen pressure makes temperature rise to 330 DEG C
~380 DEG C, holding vacuumizes 2h~4h, improves reaction mass deep dehydration effect.
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| JP2007238371A (en) * | 2006-03-08 | 2007-09-20 | Nippon Denko Kk | Apparatus and method for manufacturing boron oxide |
| CN103523793A (en) * | 2013-10-08 | 2014-01-22 | 清远先导材料有限公司 | Method for preparing anhydrous boron oxide |
| CN108622912A (en) * | 2018-07-11 | 2018-10-09 | 广东先导先进材料股份有限公司 | The production method of high temperature covering agent grade boric oxide |
| CN210419269U (en) * | 2019-06-28 | 2020-04-28 | 广东先导先进材料股份有限公司 | System for preparing long-crystal-grade primary boron oxide |
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