CN109336105A - The continuous purifying technique and its device of Explosive detonation diamond - Google Patents
The continuous purifying technique and its device of Explosive detonation diamond Download PDFInfo
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- CN109336105A CN109336105A CN201811467870.4A CN201811467870A CN109336105A CN 109336105 A CN109336105 A CN 109336105A CN 201811467870 A CN201811467870 A CN 201811467870A CN 109336105 A CN109336105 A CN 109336105A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/25—Diamond
- C01B32/28—After-treatment, e.g. purification, irradiation, separation or recovery
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Abstract
The present invention relates to the continuous purifying techniques and its device of Explosive detonation diamond.The continuous purifying technique of Explosive detonation diamond, it is that the 95%-98% concentrated sulfuric acid is mixed into raw material slurry by detonation ash and purity, reaction kettle is injected from bottom or lower part by certain flow, 50%-60% perchlorate injects reaction kettle from reactor bottom according to material handling capacity, is mixed and oxidation reaction sufficiently occurs；Reactant, which is limited according to inlet amount and reaction kettle capacity from bottom or lower part, to be entered in next stage reaction kettle, supplements perchloric acid from next stage reactor bottom；Through series classification purification until material color becomes canescence from black and stops.Since present invention employs the methods continuously purified, it is uniform to purify obtained diamond dry powder finished product purity is high, quality, and to lack since every level-one purifies the addition more intermittent method of purification of perchloric acid, the process safety is reliable, economic and environment-friendly, perchloric acid utilization rate is high, and total dosage is reduced.
Description
Technical field
The present invention relates to a kind of purifying techniques of diamond, more particularly to a kind of company with explosive detonation diamond synthesis
Continuous purifying technique and its device.
Background technique
Explosive detonation diamond generallys use TNT (TNT), hexogen (RDX), Losec and opens up explosives and stones such as golden (HMX)
The carbon materials such as ink are raw material, and carry out detonation reaction in 1 closed container equipped with protection medium, make not oxidized freedom
Carbon atom is changed into nanometer or micron diamond under instantaneous superhigh-temperature and-pressure work, and detonation after the reaction was completed, collects and contains diamond
Detonation ash carry out purification processes.
Existing purification was all aoxidized using the method for pickling oxidation for removing amorphous carbon, graphite and other impurities
Cheng Caiyong perchloric acid-sulfuric acid (yellow wind thunder, Tong Yi etc., the artificially synthesizing diamond purification system with exhaust-gas treatment,
ZL200620133876.4), nitric acid-sulfuric acid (Xu Kang, Xue Qunji etc., the purification process of carbon-drop acid system, CN in diamond synthesis
1400162) or sulfuric acid-potassium permanganate (yellow wind thunder, Tong Yi, stone of washing, the method for purification of Nano diamond, CN1385366) combines
The method of oxidation.What these methods of purification were all made of is intermittent reaction, and oxidant (such as common perchloric acid) utilization rate is lower, is made
At waste, at the same increase harmful gas emission (Chen Hongwei, Quan Yi, move high-pressure process diamond synthesis technology in environment and peace
Full case study, safety and environment journal, the 2nd phase of volume 6, in April, 2006), aggravate post-processing load；Large-scale production just needs
Multiple reaction kettle parallel reactions are wanted, the purified reaction in each reaction kettle independently carries out, although the amount of reagent is by regulation ratio
Example addition, but factor can not be resisted since experimental facilities and operating error etc. are some, so that the final product quality in each reaction kettle is deposited
In small difference.Moreover, because reaction kettle quantity is more, energy consumption needed for the heating period is high, the heat loss that the stage of reaction is released
Also more, in summer sweltering heat weather, the heat of heating device and reaction releasing makes workshop temperature may be up to 40-50 DEG C, work
Make bad environments.
Summary of the invention
To overcome the shortcomings of above-mentioned method of purification, the invention proposes improved Explosive detonation purification of diamond methods, adopt
It with continuous method of purification, improves work efficiency, reduces the consumption of perchloric acid, decrease heat dissipation.
To achieve the goals above, chemical principle is constant, and device upgrade is improved as continuous multi-stage purifying plant, should
Device can be accomplished continuously to feed, and material carries out again according to the capacity limit of reaction kettle automatically into next stage reaction kettle
Once oxidation purified reaction, until detonation ash becomes canescence, sampled to examine up to standard, stopping reaction, discharging washing and drying reaches
It is produced to streamlined.Independent intermittent reaction before is transformed into continous way reaction of high order by the device, is improved work efficiency,
Reaction kettle quantity needed for same reaction mass is few, so that the consumption of the heat and perchloric acid that release reaction is also reduced.
Detonation ash and purity are that the 95%-98% concentrated sulfuric acid is mixed into original by the continuous purifying technique of Explosive detonation diamond
Slurry material injects reaction kettle from bottom or lower part by certain flow, and 50%-60% perchlorate is according to material handling capacity from reaction
Reaction kettle is injected in bottom portion, is mixed and oxidation reaction sufficiently occurs；Reactant according to inlet amount and reaction kettle capacity limit from
Bottom or lower part enter in next stage reaction kettle, supplement perchloric acid from next stage reactor bottom；Through series classification purification until
Material color becomes canescence from black and stops.
Wherein total material proportion are as follows:
Detonation ash g: concentrated sulfuric acid ml=0.1-0.02, detonation ash g: perchloric acid ml=0.1-0.02.
The temperature of the oxidation reaction is 200-320 DEG C, wherein material pipe and storage tank between reaction kettle at different levels are all
It needs to carry out isothermal holding.
The time of the reaction refers to that material leaves afterbody reaction from into first order purified reaction device to reaction is completed
The residence time of device is 1-6 hours.
The perchloric acid is to bring reaction kettle by the small flow constriction air of high speed by Venturi tube, and the raw material slurry is logical
It crosses acid resistant diaphragm and is pumped into reaction kettle；The sour gas volatilized in the oxidation reaction process is gone after passing through condensing recovery liquid
Tail gas absorption.
The condensing recovery be made by the condenser pipe with condensate liquid outlet wherein gas enter negative pressure tail gas pipeline and do
Absorption processing, a part of liquid return to reaction kettle, another part export.Derived mainly condensed water, by controlling derived quantity
A part is returned to reaction kettle to adjust, and to guarantee the concentration of reaction mass, prevents excessively sticky influence stirring and flowing.
The material color becomes canescence from black and enters back into afterbody reaction kettle, does not add perchloric acid, directly
It is stirred to react.
The technique further includes the processing of material after purification, and the processing includes sedimentation separation and washing drying.
The sedimentation separation is that the material after purifying is introduced into subsider, is moved back away at the disposing mother liquor of upper layer wait be layered
Reason, lower layer are the pulpous state diamond dust after oxidation purification.
The washing drying is 6.0-7.0 to be washed pulpous state diamond dust repeatedly with distilled water to pH, is put into baking oven
It is middle to dry to get diamond dry powder is arrived.
The continuously purification device of Explosive detonation diamond, it is characterised in that: including the concatenated heating purified reaction of several grades
Kettle, there is agitating device inside the reaction kettle, and top is equipped with discharge port, grafting thermometer boss and the condensation for connecting condensing unit
Material inlet is arranged at recovery port, lower sides or bottom, and sewage draining exit and perchloric acid feed inlet, the perchloric acid feed inlet are arranged at bottom
It is fed by Venturi tube and is connected with perchloric acid holding vessel, wherein the material inlet of first order reaction kettle passes through acid resistant diaphragm
Pump is communicated with sour slurry storage tank, and the series connection is that the discharge port of upper level purified reaction kettle passes through acid resistant diaphragm pump and next stage
The material inlet of purified reaction kettle is connected.
On connecting line between discharge port and next stage the charging acid resistant diaphragm pump of the upper level purified reaction kettle, even
It is connected to dashpot.
Check-valves is housed between the diaphragm pump and reaction kettle.
There is heating tape in the middle part of the reaction kettle lateral wall.
The reaction kettle be quartz glass material, all pipe fittings connect with reaction kettle be quartz glass, babbit or
Polytetrafluoroethylene (PTFE) material.
The continuous purifying technique of the application, it is using continuous feed and the concatenated mode of multiple reaction kettles, previous stage is anti-
Answer the reaction product of kettle as the raw material of next stage reaction kettle, on the basis of previous stage purification, further add perchloric acid into
Then row purification obtains high-purity diamond by the way of sedimentation separation washing again until material becomes canescence from black
Dry powder.The present invention is purified by continuous multi-stage, and diamond dry powder finished product purity higher quality is uniform.
Reaction mass of the present invention is all fed from reaction kettle lower part, from upper outlet, to increase oxidant perchloric acid and quilt
The time of contact of oxidation material and contact area improve reaction efficiency and perchloric acid utilization rate, while multistage purification reacts, so that
Form is added using multiple spot step by step in oxidant perchloric acid, keeps reaction is lasting to carry out, improves the utilization rate of perchloric acid, reduce
The dosage of perchloric acid, while a small amount of multiple addition, avoid heat caused by being added at one time and gather release risk.
Reaction kettle series required for the present invention is determined by reaction system production capacity and charging rate, generally will entirely be purified anti-
It should control into 1-3 hours and complete (refer to material from enter the time for leaving purification system).
After material becomes canescence from black, do not worry and carry out sedimentation separation, material can be entered into afterbody
In reaction kettle, perchloric acid is not added, reaction temperature is kept, serves and consolidate the extent of reaction.
Since the diamond dry powder finished product purity is high, the quality that present invention employs the method continuously purified, purify are equal
One, and the more intermittent method of purification of perchloric acid is added to lack since every level-one purifies, the process safety is reliable, economic ring
It protects, perchloric acid utilization rate is high, and total dosage is reduced.
Detailed description of the invention
Fig. 1 is the device of the invention structural schematic diagram,
Fig. 2 is the structural schematic diagram of reaction kettle in apparatus of the present invention,
Each label lists as follows in figure: 1. agitating devices, 2. condensing units, 3. reaction kettles, 4. heating tapes, the storage of 5. wintercherry material
Deposit tank, 6. diaphragm pumps, 7. perchloric acid holding vessels, 8. Venturi tubes, 9. air pumps, 10. thermometers, 11. dashpots, 12. discharge ports,
13. thermometer boss, 14. agitating device interfaces, 15. are condensed back to closing in, 16. material inlets, 17. perchloric acid feed inlets, 18.
Sewage draining exit.
Specific embodiment
Of the invention is described further with reference to the accompanying drawings and examples.
As shown in Figure 1 and Figure 2, the continuously purification device of Explosive detonation diamond of the invention, it is characterised in that: if including
The concatenated heating purified reaction kettle 3 of grade is done, there is agitating device interface 14 inside the reaction kettle 3, top is equipped with discharge port 12, inserts
The thermometer boss 13 of jointing temp meter 10 is condensed back to closing in 15 with connection condensing unit 2, and agitating device 1 is connect by agitating device
Mouth 14 accesses inside reaction kettles 3；Reaction kettle lower sides have material inlet 16, and sewage draining exit 18 and perchloric acid feed inlet are arranged at bottom
17, the perchloric acid feed inlet 17 is fed and is connected with perchloric acid holding vessel 7 by Venturi tube 8, and Venturi tube 8 is by air pump 9
The small flow constriction air of high speed bring reaction kettle 3 into, wherein the material inlet 16 of first order reaction kettle pass through acid resistant diaphragm pump 6
It is communicated with sour slurry storage tank 5, the series connection is that dashpot 11 will be connect under the discharge port 12 of upper level purified reaction kettle 3 by resistance to
Sour diaphragm pump 6 is connected with the material inlet 16 of next stage purified reaction kettle 3；There is heating in the middle part of 3 lateral wall of reaction kettle
Band 4.
It is preferred that being equipped with check-valves (not shown) between the diaphragm pump and reaction kettle.
The bottom of reaction kettle 3 can also be arranged in material inlet 16.
The reaction kettle be quartz glass material, all pipe fittings connect with reaction kettle be quartz glass, babbit or
Polytetrafluoroethylene (PTFE) material.
The present invention uses continuously purification device, using the concatenated mode of multiple reaction kettles, by the outlet of previous stage reaction kettle with
The material inlet of next stage reaction kettle is connected, and on the basis of previous stage purification, further adds perchloric acid into secondary purification, phase
When improving the utilization rate of perchloric acid, reduce heat and gather discharge, improve safety in a small amount of multiple purification mode.
Reaction kettle material selection quartz glass, connecting piece material are all made of quartz glass, babbit or polytetrafluoroethylene (PTFE).
Embodiment 1
With reference to Fig. 1, Fig. 2:
(1) match reaction solution:
Material and specification: detonation ash --- dry powder；The concentrated sulfuric acid --- 95~98% chemical pure or industrial goods；Perchloric acid ---
70~72% chemistry are pure.
(2) feed intake reaction:
Detonation ash and the concentrated sulfuric acid are proportionally mixed into slurry in sour slurry storage tank 5, according to certain flow benefit
It is pumped into autoclave body 3 from material inlet 16 with diaphragm pump 6, the control of flow is set according to the treating capacity of material and the capacity of reaction kettle
It is fixed；Perchlorate utilizes perchloric acid feed inlet 17 of the Venturi tube 8 from reactor bottom by perchloric acid holding vessel 7 according to material ratio
Injection, the dispersion mixing device 1 by being connected to agitating device interface 14 stir the mixture for uniformly, sufficiently generation oxidation reaction；
The temperature being plugged in the 10 feedback response kettle of thermometer in thermometer boss 13, to be controlled entirely by adjusting heating tape 4
The reaction temperature of purification process；The sour gas of the gas and volatilization that generate in reaction process, which passes through, is condensed back to the cold of closing in 15
Solidifying device 2 is handled；Mixed material can be limited according to feed rate and reaction kettle capacity from discharge port 12 into dashpot to be passed through again
Diaphragm pump 6 is pumped into next stage purifying plant；Successively series classification purifies, until material color becomes canescence from black, at this time
Reach the afterbody of reaction (afterbody does not add perchloric acid)；Reaction stop or at the end of can pass through reactor bottom
Sewage draining exit 18 carries out blowdown cleaning.
(3) sedimentation separation
The material of end of reaction is introduced into subsider, band layering moves back away the processing of upper layer disposing mother liquor, and lower layer is oxidation
Pulpous state diamond dust after purification；
(4) washing and drying
Pulpous state diamond dust distilled water is washed repeatedly to pH is 6.0~7.0, is put into baking oven and dries to get arriving
Diamond dry powder.
The above description is only an embodiment of the present invention, not thereby limits the scope of the patents of the invention, all to utilize this hair
Structures or the equivalent process transformation such as made by bright specification and accompanying drawing content, are applied directly or indirectly in other relevant technologies
Field is included within the scope of the present invention.
Specific implementation process citing:
1. stock and ingredient:
Detonation ash (g): the concentrated sulfuric acid (ml)=0.3,
Detonation ash (g): perchloric acid (ml)=0.3；
Concentrated sulfuric acid concentration 95%, perchloric acid concentration 55%.
2. reactor prepares:
Single 50 liters of reactor volume, 35 liters of effecting reaction volume, the series connection of 5 order reaction kettles, each reaction kettle electric heating function
Rate 3KW.
3. feed intake reaction:
First first reaction kettle is added with 0.5 liter/min of flow in detonation ash and concentrated sulfuric acid slurry, reaches reaction in material
Kettle volume 1/3 when begin to warm up, temperature is initially added into perchloric acid when reaching 200 DEG C, flow control at 0.137 liter/min, temperature
Degree stops heating when rising to 250 DEG C, maintains kettle temperature by reaction heat, and by thermometric and temperature-controlling system regulation heating rhythm；High chlorine
Acid is only added in preceding 4 reaction kettles, and the 5th reaction kettle is the heat preservation consolidation phase, and perchloric acid is not added.
4. response time history controls:
Detonation ash and concentrated sulfuric acid slurry are about 6 from the residence time for entering first reaction kettle to the 5th reaction kettle of outflow
A hour, according to the intermediate sampling of reaction and outlet sampling observation analysis as a result, appropriate adjustment slurry flow and perchloric acid flow, with
Subject to purification result is up to standard.
It is compared with the prior art:
The technical indicator comparison of continuous processing and batch technology of the invention (is shown in Table 1, with continuous processing 250KG detonation ash
Production capacity carry out process check.)
The comparison of the key technical indexes of 1 continuous processing of table and batch technology
Continuous processing of the invention and batch technology comparing result as can be seen from Table 1, continuous processing are constituting purification life
It produces and all has a clear superiority on the indices of cost, the overall cost 20-30% of detonation purification of diamond can be greatly reduced.
Claims (15)
1. detonation ash and purity are that the 95%-98% concentrated sulfuric acid is mixed into raw material by the continuous purifying technique of Explosive detonation diamond
Slurry injects reaction kettle from bottom or lower part by certain flow, and 50%-60% perchlorate is according to material handling capacity from reaction kettle
Reaction kettle is injected in bottom, is mixed and oxidation reaction sufficiently occurs；Reactant is limited according to inlet amount and reaction kettle capacity the bottom of from
Portion or lower part enter in next stage reaction kettle, supplement perchloric acid from next stage reactor bottom；Through series classification purification until object
Material color becomes canescence from black and stops.
2. continuous purifying technique according to claim 1, wherein total material proportion are as follows:
Detonation ash g: concentrated sulfuric acid ml=0.1-0.02, detonation ash g: perchloric acid ml=0.1-0.02.
3. continuous purifying technique according to claim 1, the temperature of the oxidation reaction is 200-320 DEG C, wherein at different levels
Material pipe and storage tank between reaction kettle require to carry out isothermal holding.
4. continuous purifying technique according to claim 1, the time of the reaction refers to that material is anti-from first order purification is entered
It answers device to leave the residence time of afterbody reactor to completion reaction, is 1-6 hours.
5. continuous purifying technique according to claim 1, the perchloric acid is by Venturi tube by the small flow pressure of high speed
Contracting air brings reaction kettle into, and the raw material slurry is pumped into reaction kettle by acid resistant diaphragm；It volatilizees in the oxidation reaction process
Sour gas out removes tail gas absorption after passing through condensing recovery liquid.
6. continuous purifying technique according to claim 5, the condensing recovery is the condensation by having condensate liquid outlet
Pipe make wherein gas enter negative pressure tail gas pipeline and do absorption processing, a part of liquid returns to reaction kettle, a part export, to guarantee
The concentration of reaction mass prevents excessively sticky influence stirring and flowing.
7. continuous purifying technique according to claim 1, the material color becomes canescence from black and enters back into finally
In first order reaction kettle, perchloric acid is not added, is directly stirred to react.
8. continuous purifying technique according to claim 1, the technique further includes the processing of material after purification, the processing
Including sedimentation separation and washing drying.
9. continuous purifying technique according to claim 8, the sedimentation separation is that the material after purifying introduces subsider
In, the processing of upper layer disposing mother liquor is moved back away wait be layered, lower layer is the pulpous state diamond dust after oxidation purification.
10. continuous purifying technique according to claim 9, the dry washing is by pulpous state diamond dust distilled water
Washing is 6.0-7.0 to pH repeatedly, is put into baking oven and dries to get diamond dry powder is arrived.
11. the continuously purification device of Explosive detonation diamond, it is characterised in that: including the concatenated heating purified reaction of several grades
Kettle, there is agitating device inside the reaction kettle, and top is equipped with discharge port, grafting thermometer boss and the condensation for connecting condensing unit
Material inlet is arranged at recovery port, lower sides or bottom, and sewage draining exit and perchloric acid feed inlet, the perchloric acid feed inlet are arranged at bottom
It is fed by Venturi tube and is connected with perchloric acid holding vessel, wherein the material inlet of first order reaction kettle passes through acid resistant diaphragm
Pump is communicated with sour slurry storage tank, and the series connection is that the discharge port of upper level purified reaction kettle passes through acid resistant diaphragm pump and next stage
The material inlet of purified reaction kettle is connected.
12. continuously purification device according to claim 11, it is characterised in that: the discharging of the upper level purified reaction kettle
On connecting line between mouth and next stage charging acid resistant diaphragm pump, it is connected with dashpot.
13. continuously purification device according to claim 11, it is characterised in that: be equipped between the diaphragm pump and reaction kettle
Check-valves.
14. continuously purification device according to claim 11, it is characterised in that: have heating in the middle part of the reaction kettle lateral wall
Band.
15. continuously purification device according to claim 11, it is characterised in that: the reaction kettle is quartz glass material,
All pipe fittings connecting with reaction kettle are quartz glass, babbit or polytetrafluoroethylene (PTFE) material.
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| CN112221406A (en) * | 2020-12-09 | 2021-01-15 | 佛山市普力达科技有限公司 | Full-grade silicone adhesive continuous production system |
| WO2023277474A1 (en) * | 2021-06-30 | 2023-01-05 | 주식회사 에스더블유케미컬즈 | High purity nanodiamond, and preparation method thereof |
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