CN108192386A - It is a kind of to nitrogenize titanium nacreous preparation method - Google Patents
It is a kind of to nitrogenize titanium nacreous preparation method Download PDFInfo
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- CN108192386A CN108192386A CN201711389238.8A CN201711389238A CN108192386A CN 108192386 A CN108192386 A CN 108192386A CN 201711389238 A CN201711389238 A CN 201711389238A CN 108192386 A CN108192386 A CN 108192386A
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- reactor
- nitridation
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
- C09C1/0051—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings comprising a stack of coating layers with alternating low and high refractive indices, wherein the first coating layer on the core surface has the low refractive index
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
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Abstract
The present invention relates to a kind of methods that titanium nitride film cladding pearlescent pigment is prepared by vertical fluidized bed reactor, include the following steps：(1) charging exhaust；(2) heating ventilation；(3) nitridation reaction；(4) cooling exhaust.The present invention selects vertical fluidized bed reactor, pass through solids fluidised form technology, material is made to be in fluidization, increase the contact area of gas-particle two-phase, entire reaction system is made to be in substantially uniform state, the efficiency and homogeneity of nitridation reaction are greatly improved, so as to obtain a series of pearlescent pigments with unique visual effects.Compared to vapour deposition process directly in deposited on substrates titanium nitride film, the advantages that this method technique is more stable, reproducible, reactant is dangerous small, and manufactured nitridation titanium-type pearlescent pigment can inherit its raw material coated by titanium dioxide type pearlescent pigment film layer is smooth, crystal structure is uniform.
Description
Technical field：
Preparation method more particularly to one kind the present invention relates to a kind of pearlescent pigment pass through the preparation of vertical fluidized bed reactor
The method that titanium nitride film coats pearlescent pigment.
Background technology：
Pearly-lustre class pigment is a kind of material with extensive use in modern society.Pearl effect pigment cross section has class
It is similar to the physical arrangement of pearl：Kernel is the substance of low optical refractive index, and outer layer coats different types of high refractive index layer again.
Titanium nitride film, with different refractive index and color, with reference to the different thickness of film layer, can give thousand changes in nitrogen content difference
Ten thousand visual effects changed, although having titanium nitride powder coating or titanium nitride coating product at present, with micron order base material outsourcing
Progress is very limited in terms of covering pearlescent pigment made of titanium nitride film.
The pearlescent pigment method for preparing of mainstream is liquid phase deposition at present, can effectively be sunk by this method in substrate surface
Product metal or nonmetal oxide film layer, obtain gorgeous pearl effect, but liquid phase deposition can not effectively prepare metal nitrogen
Compound pearly-lustre.Vapour deposition process can directly prepare titanium nitride film：Physical vaporous deposition by reactive sputtering or can be penetrated
The mode of RF sputtering prepares titanium nitride film；Chemical vapour deposition technique can then pass through titanium tetrachloride/hydrogen/nitrogen or four chlorinations
Titanium/ammonia reaction system prepares titanium nitride film.But if vapor deposition is then difficult to realize applied to pearlescent pigment field：Object
Physical vapor deposition normal plane faces the difficult point that powder base material effectively disperses；And it is directly prepared in substrate surface using chemical vapour deposition technique
Pearlescent pigment faces the shortcomings of technique is unstable, and film layer is difficult to control.
Based on the above, a kind of preparation nitridation easily controllable, process is brief, process repeatability is strong, effect is good is found
The method of titanium film layer pearly-lustre is very valuable.
Invention content：
This patent selects vertical fluidized bed reactor, by solids fluidised form technology, is allowed to abundant with reaction gas
Contact, is compared thorough nitridation reaction, so as to obtain a series of pearlescent pigments with unique visual effects.This method has
There is the features such as easily controllable, process is brief, repeatable, effect is good.
A kind of method that titanium nitride film cladding pearlescent pigment is prepared by vertical fluidized bed reactor, including following step
Suddenly：
(1) charging exhaust：50-200Kg coated by titanium dioxide type pearlescent pigments are fitted into vertical fluidized bed reactor, are made
Its free accumulation blasts nitrogen ammonia gas mixture body 5- on reactor bottom material bed by the blast cap for being mounted on reactor side
15min；
(2) heating ventilation：Infrared radiation heater is opened, is made in reactor cavity body with the rate of heat addition of 10-25 DEG C/min
Portion is kept the temperature after being warming up to reaction temperature.The blast cap mounted on reactor bottom is opened, is passed through and is preheated to reacting into reactor
The consistent nitrogen ammonia gas mixture body of temperature opens simultaneously the exhaust outlet of reactor head；
(3) nitridation reaction：Expect that the pearlescent pigment on bed suspends and start nitridation reaction 2-4h, nitridation reaction in after normal fluidisation
In be continually fed into the nitrogen ammonia gas mixture body consistent with reaction temperature；
(4) cooling exhaust：Stop infrared radiation heater heating, close reactor bottom blast cap, stopping is passed through ammonia, protects
It holds and is passed through nitrogen, close reactor head exhaust outlet and close entire reactor, reactor is beaten again after naturally cooling to room temperature
It opens top vent and opens blast cap and the unreacted residual nitrogen gas ammonia gas of air 5-15min discharges is blasted into reactor.It opens
It is titanium nacreous that discharge port takes out finished product nitridation.
Coated by titanium dioxide type pearlescent pigment in step (1) includes coated by titanium dioxide layer and base material, and base material includes day
Right mica, synthetic mica, silica, aluminium oxide etc., the thicknesses of layers of the coated by titanium dioxide type pearlescent pigment is 40-
150nm。
Step (1) is passed through the air in the mixed gas emptying reactor of nitrogen and ammonia.
The flow-rate ratio of nitrogen ammonia gas mixture body is 10 in step (1), (2):1-1:1.
Coated by titanium dioxide type pearlescent pigment influences the temperature of nitridation reaction as raw material, temperature tolerance.If step (1)
In coated by titanium dioxide type pearlescent pigment base material for natural mica, synthetic mica, step (2) reaction temperature be 750-850 DEG C；
If the coated by titanium dioxide type pearlescent pigment base material in step (1) is silica, aluminium oxide, step (2) reaction temperature is
750-950℃。
Step (3) pays close attention to the fluidised form of pearlescent pigment by form and decompression material taking mouth, and passes through sidewall of reactor
Depressurize sample tap sampling monitoring reactiveness.
Unreacted ammonia and other exhaust gas are discharged from reactor head exhaust outlet in step (4), after being sprayed by cold water
Dilute alkaline solution is made into, can be used for neutralizing the acid waste liquid of pearly-lustre producer, reduce environmental protection pressure.
Step (4) holding is passed through nitrogen protection nitride, in order to avoid by aoxidizing.
It is 80-95% that step (4) finished product, which nitrogenizes titanium nacreous yield,.
Advantage of the invention is that：
(1) fluidized-bed reactor makes material be in fluidization, so as to increase the contact area of gas-particle two-phase, makes entire anti-
System is answered to be in substantially uniform state, greatly improves the efficiency and homogeneity of nitridation reaction；
(2) compared to vapour deposition process directly in deposited on substrates titanium nitride film, this method technique is more stable, repeated
Well, reactant danger is small, and manufactured nitridation titanium-type pearlescent pigment can inherit its raw material-coated by titanium dioxide type pearly-lustre face
Expect the advantages that film layer is smooth, crystal structure is uniform.
Specific embodiment：
Embodiment 1：
100Kg mica titanium nacreous materials is taken to be fitted into vertical fluidized bed reactor, make its free accumulation in reactor bottom
Expect on bed.Then the mixed gas 10 minutes of nitrogen and ammonia is blasted by the blast cap for being mounted on reactor side to empty reactor
In air, the ratio of nitrogen and ammonia is 6:1.Infrared radiation heater makes reactor cavity with the rate of heat addition of 18 DEG C/min
Inside is kept the temperature after being warming up to 800 DEG C of reaction temperature of setting.It is opened later by being mounted on the blast cap of reactor bottom into reactor
Begin to be passed through the nitrogen ammonia gas mixture body for being preheated to 800 DEG C, the two ratio is 6:1, and open simultaneously the exhaust of reactor head
Mouthful.Pearlescent pigment on material bed suspends melts beginning nitridation reaction in normal stream, reactor cavity temperature and nitrogen in reaction process
Ammonia gas mixture temperature is held at 800 DEG C, and nitridation reaction maintains 2.5 hours altogether, passes through sidewall of reactor during reaction
Depressurize sample tap sampling monitoring reactiveness.Stop infrared radiation heater heating after nitridation reaction, close reactor bottom
Portion's blast cap, stopping are passed through ammonia, and holding is passed through nitrogen, close reactor head exhaust outlet and close entire reactor, reactor
Be again turned on top vent after naturally cooling to room temperature and open blast cap blasted into reactor air 15min discharge unreacted
Residual nitrogen gas ammonia gas, residual nitrogen gas ammonia gas after discharge is made into dilute alkaline solution through cold water spray.Open discharge port take out into
Product nitrogenize titanium nacreous 88Kg.
Embodiment 2：
80Kg coated by titanium dioxide aluminum oxide base material pearlescent pigments is taken to be fitted into vertical fluidized bed reactor, make its free heap
Product is on reactor bottom material bed.Then the mixed gas 8 for nitrogen and ammonia being blasted by the blast cap for being mounted on reactor side is divided
For clock to empty the air in reactor, the ratio of nitrogen and ammonia is 8:1.Infrared radiation heater is with the heating speed of 23 DEG C/min
Rate makes to keep the temperature after being warming up to 900 DEG C of reaction temperature of setting inside reactor cavity.Later by being mounted on the wind of reactor bottom
Cap starts to be passed through the nitrogen ammonia gas mixture body for being preheated to 900 DEG C into reactor, and the two ratio is 8:1, and open simultaneously anti-
Answer the exhaust outlet at the top of device.Pearlescent pigment on material bed suspends melts beginning nitridation reaction in normal stream, reactor in reaction process
Cavity temperature and nitrogen ammonia gas mixture temperature are held at 900 DEG C, and nitridation reaction maintains 2 hours altogether, passes through during reaction
The decompression sample tap sampling monitoring reactiveness of sidewall of reactor.Stop infrared radiation heater heating after nitridation reaction,
Reactor bottom blast cap is closed, stopping is passed through ammonia, and holding is passed through nitrogen, closes reactor head exhaust outlet and closes entire anti-
Device, reactor is answered to be again turned on top vent after naturally cooling to room temperature and open blast cap to blast air into reactor
10min discharges unreacted residual nitrogen gas ammonia gas, and the residual nitrogen gas ammonia gas after discharge is made into dilute alkaline solution through cold water spray.It opens
It opens discharge port and takes out the titanium nacreous 70Kg of finished product nitridation.
Embodiment 3：
160Kg coated by titanium dioxide silica base material pearlescent pigments is taken to be fitted into vertical fluidized bed reactor, make it certainly
By being piled up on reactor bottom material bed.Then the mixed gas of nitrogen and ammonia is blasted by the blast cap for being mounted on reactor side
To empty the air in reactor, the ratio of nitrogen and ammonia is 4 within 12 minutes:1.Infrared radiation heater is added with 15 DEG C/min's
Hot rate makes to keep the temperature after being warming up to 870 DEG C of reaction temperature of setting inside reactor cavity.Later by being mounted on reactor bottom
Blast cap start to be passed through the nitrogen ammonia gas mixture body for being preheated to 800 DEG C into reactor, the two ratio is 4:1, and beat simultaneously
Open the exhaust outlet of reactor head.It is in normally to melt beginning nitridation reaction that pearlescent pigment on material bed, which suspends, in reaction process
Reactor cavity temperature and nitrogen ammonia gas mixture temperature are held at 870 DEG C, and nitridation reaction maintains 3.5 hours altogether, reaction
The decompression sample tap sampling monitoring reactiveness that period passes through sidewall of reactor.Stop infrared radiation heating after nitridation reaction
Device heats, and closes reactor bottom blast cap, and stopping is passed through ammonia, and holding is passed through nitrogen, closes reactor head exhaust outlet and seals
Close entire reactor, reactor is again turned on top vent after naturally cooling to room temperature and opens blast cap blasting into reactor
Air 15min discharges unreacted residual nitrogen gas ammonia gas, and the residual nitrogen gas ammonia gas after discharge is made into diluted alkaline molten through cold water spray
Liquid.It opens discharge port and takes out the titanium nacreous 140Kg of finished product nitridation.
Claims (6)
1. a kind of nitrogenize titanium nacreous preparation method, it is characterised in that includes the following steps：
(1) charging exhaust：50-200Kg coated by titanium dioxide type pearlescent pigments are fitted into vertical fluidized bed reactor, make it certainly
By being piled up on reactor bottom material bed, nitrogen ammonia gas mixture body 5-15min is blasted by the blast cap for being mounted on reactor side；
(2) heating ventilation：Infrared radiation heater is opened, makes to rise inside reactor cavity with the rate of heat addition of 10-25 DEG C/min
It is kept the temperature after temperature to reaction temperature.The blast cap mounted on reactor bottom is opened, is passed through and is preheated to and reaction temperature into reactor
Consistent nitrogen ammonia gas mixture body opens simultaneously the exhaust outlet of reactor head；
(3) nitridation reaction：Expect that the pearlescent pigment on bed suspends and start nitridation reaction 2-4h in after normal fluidisation, held in nitridation reaction
It is continuous to be passed through the nitrogen ammonia gas mixture body consistent with reaction temperature；
(4) cooling exhaust：Stop infrared radiation heater heating, close reactor bottom blast cap, stopping is passed through ammonia, keeps logical
Enter nitrogen, close reactor head exhaust outlet and close entire reactor, reactor is again turned on pushing up after naturally cooling to room temperature
Portion's exhaust outlet simultaneously opens blast cap air 5-15min is blasted into reactor and discharge unreacted residual nitrogen gas ammonia gas.Open discharging
It is titanium nacreous that mouth takes out finished product nitridation.
2. a kind of titanium nacreous preparation method of nitridation according to claim 1, it is characterised in that：The step (1)
In coated by titanium dioxide type pearlescent pigment thicknesses of layers for 40-150nm, including coated by titanium dioxide layer and base material.
3. a kind of titanium nacreous preparation method of nitridation according to claim 2, it is characterised in that：The base material includes
Natural mica, synthetic mica, silica, aluminium oxide.
4. a kind of titanium nacreous preparation method of nitridation according to claim 3, it is characterised in that：If base material is day
Right mica, synthetic mica, step (2) reaction temperature are 750-850 DEG C；If base material is silica, aluminium oxide, step (2)
Reaction temperature is 750-950 DEG C.
5. a kind of titanium nacreous preparation method of nitridation according to claim 1, it is characterised in that：The step (1),
(2) flow-rate ratio of nitrogen ammonia gas mixture body is 10 in:1-1:1.
6. a kind of titanium nacreous preparation method of nitridation according to claim 1, it is characterised in that：The step (4)
It is 80-95% that finished product, which nitrogenizes titanium nacreous yield,.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711389238.8A CN108192386A (en) | 2017-12-20 | 2017-12-20 | It is a kind of to nitrogenize titanium nacreous preparation method |
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| CN201711389238.8A CN108192386A (en) | 2017-12-20 | 2017-12-20 | It is a kind of to nitrogenize titanium nacreous preparation method |
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| CN108192386A true CN108192386A (en) | 2018-06-22 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724396A (en) * | 2019-09-24 | 2020-01-24 | 河北欧克新型材料股份有限公司 | Temperature-resistant black pearlescent pigment and preparation method thereof |
-
2017
- 2017-12-20 CN CN201711389238.8A patent/CN108192386A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110724396A (en) * | 2019-09-24 | 2020-01-24 | 河北欧克新型材料股份有限公司 | Temperature-resistant black pearlescent pigment and preparation method thereof |
| CN110724396B (en) * | 2019-09-24 | 2021-10-01 | 河北欧克新型材料股份有限公司 | Temperature-resistant black pearlescent pigment and preparation method thereof |
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Application publication date: 20180622 |
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