CN109705623A - A kind of preparation method of the Prussian blue pearlescent pigment of illusion-colour - Google Patents
A kind of preparation method of the Prussian blue pearlescent pigment of illusion-colour Download PDFInfo
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Abstract
A kind of preparation method of the Prussian blue pearlescent pigment of illusion-colour, its feature the following steps are included: prepare flake matrix material first, it is raw material with soluble zirconates, phosphoric acid and hydrofluoric acid, using conventional fine chemical-process, in atmospheric conditions, reaction temperature be 60~90 DEG C, the reaction time 2~4 hours, flake matrix material；Then the sodium hydroxide solution that titanium tetrachloride solution and concentration are 20~25% is added in system simultaneously, surface cladding is carried out to flake matrix material, 2 progress of flake matrix material surface cladding point, after first subsurface cladding, it is filtered, washs, calcines, obtained intermediate product are subjected to dispersion and carry out second of surface cladding；Then it is filtered, washs, filter cake is dried at 110~130 DEG C, calcining 1 hour is then carried out at 820~850 DEG C, obtains the Prussian blue pearlescent pigment of illusion-colour.
Description
Technical field
The present invention relates to a kind of preparation methods of the Prussian blue pearlescent pigment of illusion-colour.
Background technique
Prussian blue is the general name that six cyanogen close perferrite, is the complex of Fe (II), also referred to as milori blue or special grace
Boolean is blue.It is acidproof, alkaline-resisting, fast light, weather-proof in recent years since organic pigment phthalocyanine indigo plant has than Prussian blue more gay colours
Property is strong, has gradually replaced Prussian blue as important coating and coloring plastic pigment.It but is an example to pearlescent pigment
Outside, it because splitting and pearlescent pigment piece are poor to the absorption property of phthalocyanine blue, is easy from splitting or pearlescent pigment piece table
Face removing.And fine and close and tough and tensile coating can be obtained with Prussian blue cladding pearlescent pigment.
Pearlescent pigment is as a kind of reflecting effect pigment, and in ink, coating, the industrial applications such as plastics are more and more extensive, general
Logical interference series pearlescent pigment, due to only with transparent oxide cladding layers, going up at a certain angle inevitably only
Single glory effect can be presented, for example, yellow, red, purple, blue, green and other effects, this effect can no longer meet people to the need of color
It asks.Although there is the pearlescent pigment for coating organic mill base, since its stability is poor, easily decolourize, and application field is extremely narrow, not
It can be acceptable to the market well.So researching and developing a kind of polychrome, goniochromatic effect, high brightness, the pearlescent pigment of high stability is city
Field is required.
A kind of preparation method of the Prussian blue pearlescent pigment of illusion-colour, feature the following steps are included: prepare sheet base first
Then body material carries out surface cladding to flake matrix material；The preparation method of flake matrix material: reaction kettle is put into 3000 weights
The deionized water of part is measured, stirring is opened, the solid zirconium oxychloride of 200~250 parts by weight is added into reaction kettle, to solid oxygen chlorine
After change zirconium is completely dissolved, the hydrofluoric acid of 50~80 parts by weight is added into reaction kettle, hydrofluoric acid concentration is 41~42%, stirring 30
Minute, the phosphoric acid of 160~220 parts by weight is added into reaction kettle, phosphoric acid concentration is 90~93%, stirs 30 minutes, starts to rise
Temperature starts to keep the temperature when temperature reaches 60~90 DEG C, and soaking time 2~4 hours, after heat preservation, to temperature of reaction kettle nature
50 DEG C are cooled to hereinafter, be filtered, wash, obtains flake matrix material filter cake；
2 progress of flake matrix material surface cladding point, first time surface coating method: reaction kettle is put into going for 2200 parts by weight
Ionized water, open stirring, be added into reaction kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 78
At~82 DEG C, start to keep the temperature, the pH value of system is first adjusted to 1.8~2.0 with titanium tetrachloride solution, then by titanium tetrachloride solution
The sodium hydroxide solution for being 20~25% with concentration is added in reaction kettle simultaneously, and the pH value of system is remained in adition process
It is 900~950 parts by volume for the addition total amount to 1.8~2.0, titanium tetrachloride solution, controls titanium tetrachloride solution and 20~25%
Sodium hydroxide solution the addition time be 7~8 hours, addition finish heat preservation 30 minutes, open cooling water to reaction kettle carry out it is cold
But, when temperature is down to 50 DEG C hereinafter, be filtered, wash, the first subsurface cladding pearlescent pigment filter cake is obtained；Filter cake is existed
It is dried at 110~130 DEG C, calcining 1 hour is then carried out at 820~850 DEG C, obtained illusion-colour and interfere blue pearlescent pigment,
The concentration of the titanium tetrachloride solution is 4.0 mol/Ls；
Second of surface coating method: reaction kettle is put into the deionized water of 2200 parts by weight, opens stirring, is added into reaction kettle
Above-mentioned first subsurface that obtains coats to obtain the blue pearlescent pigment of illusion-colour interference, starts to warm up, when temperature reaches 65~75 DEG C, opens
Begin to keep the temperature, the pH value of system is first adjusted to 4.0~4.5 with ammonium ferric sulfate solution, it is then that ammonium ferric sulfate solution and concentrated ammonia liquor is molten
Liquid is added in reaction kettle simultaneously, remained in adition process system pH value be to 4.0~4.5, ammonium ferric sulfate solution
Addition total amount is 160~180 parts by volume, and the addition time for controlling ammonium ferric sulfate solution and concentrated ammonia solution is 3~4 hours, is added
Potassium ferrocyanide is added with same method after entering, potassium ferrocyanide solution and concentrated ammonia solution are added to reaction simultaneously
The pH value that system is remained in kettle, in adition process is to 4.0~4.5, the addition total amount of potassium ferrocyanide solution is 120~
140 parts by volume, the addition time for controlling potassium ferrocyanide solution and concentrated ammonia solution is 2~3 hours, and addition finishes 30 points of heat preservation
Clock is opened cooling water and is cooled down to reaction kettle, and when temperature is down to 50 DEG C hereinafter, be filtered, wash, it is Prussian blue to obtain illusion-colour
Pearlescent pigment filter cake；Filter cake is dried at 110~130 DEG C, obtains the Prussian blue pearlescent pigment of illusion-colour；The sulfuric acid
The concentration of iron ammonium salt solution is 2.0 mol/Ls；The concentration of the potassium ferrocyanide solution is 1.5 mol/Ls.
Innovative point of the present invention: using soluble zirconates, phosphoric acid and hydrofluoric acid for raw material, using conventional fine chemical-process,
In atmospheric conditions, reaction temperature is 60~90 DEG C, the reaction time 2~4 hours, obtains flake matrix material, this synthesis side
Flake matrix material diameter and thickness that method obtains is uniformly and controllable, and 3~5 μm of flake matrix material diameter and thickness 50~
70nm keeps the performance of pigment more preferable.It is coated twice in addition, the present invention carries out intermediate washings, the pearlescent pigment color of preparation is fresher
It is gorgeous.
Summary of the invention
A kind of preparation method of the Prussian blue pearlescent pigment of illusion-colour, feature the following steps are included: prepare sheet base first
Then body material carries out surface cladding to flake matrix material；The preparation method of flake matrix material: reaction kettle is put into 3000 weights
The deionized water of part is measured, stirring is opened, the solid zirconium oxychloride of 200~250 parts by weight is added into reaction kettle, to solid oxygen chlorine
After change zirconium is completely dissolved, the hydrofluoric acid of 50~80 parts by weight is added into reaction kettle, hydrofluoric acid concentration is 41~42%, stirring 30
Minute, the phosphoric acid of 160~220 parts by weight is added into reaction kettle, phosphoric acid concentration is 90~93%, stirs 30 minutes, starts to rise
Temperature starts to keep the temperature when temperature reaches 60~90 DEG C, and soaking time 2~4 hours, after heat preservation, to temperature of reaction kettle nature
50 DEG C are cooled to hereinafter, be filtered, wash, obtains flake matrix material filter cake；
2 progress of flake matrix material surface cladding point, first time surface coating method: reaction kettle is put into going for 2200 parts by weight
Ionized water, open stirring, be added into reaction kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 78
At~82 DEG C, start to keep the temperature, the pH value of system is first adjusted to 1.8~2.0 with titanium tetrachloride solution, then by titanium tetrachloride solution
The sodium hydroxide solution for being 20~25% with concentration is added in reaction kettle simultaneously, and the pH value of system is remained in adition process
It is 900~950 parts by volume for the addition total amount to 1.8~2.0, titanium tetrachloride solution, controls titanium tetrachloride solution and 20~25%
Sodium hydroxide solution the addition time be 7~8 hours, addition finish heat preservation 30 minutes, open cooling water to reaction kettle carry out it is cold
But, when temperature is down to 50 DEG C hereinafter, be filtered, wash, the first subsurface cladding pearlescent pigment filter cake is obtained；Filter cake is existed
It is dried at 110~130 DEG C, calcining 1 hour is then carried out at 820~850 DEG C, obtained illusion-colour and interfere blue pearlescent pigment,
The concentration of the titanium tetrachloride solution is 4.0 mol/Ls；
Second of surface coating method: reaction kettle is put into the deionized water of 2200 parts by weight, opens stirring, is added into reaction kettle
Above-mentioned first subsurface that obtains coats to obtain the blue pearlescent pigment of illusion-colour interference, starts to warm up, when temperature reaches 65~75 DEG C, opens
Begin to keep the temperature, the pH value of system is first adjusted to 4.0~4.5 with ammonium ferric sulfate solution, it is then that ammonium ferric sulfate solution and concentrated ammonia liquor is molten
Liquid is added in reaction kettle simultaneously, remained in adition process system pH value be to 4.0~4.5, ammonium ferric sulfate solution
Addition total amount is 160~180 parts by volume, and the addition time for controlling ammonium ferric sulfate solution and concentrated ammonia solution is 3~4 hours, is added
Potassium ferrocyanide is added with same method after entering, potassium ferrocyanide solution and concentrated ammonia solution are added to reaction simultaneously
The pH value that system is remained in kettle, in adition process is to 4.0~4.5, the addition total amount of potassium ferrocyanide solution is 120~
140 parts by volume, the addition time for controlling potassium ferrocyanide solution and concentrated ammonia solution is 2~3 hours, and addition finishes 30 points of heat preservation
Clock is opened cooling water and is cooled down to reaction kettle, and when temperature is down to 50 DEG C hereinafter, be filtered, wash, it is Prussian blue to obtain illusion-colour
Pearlescent pigment filter cake；Filter cake is dried at 110~130 DEG C, obtains the Prussian blue pearlescent pigment of illusion-colour；
The concentration of the ammonium ferric sulfate solution is 2.0 mol/Ls；
The concentration of the potassium ferrocyanide solution is 1.5 mol/Ls.
Specific embodiment
Embodiment 1
The preparation of flake matrix material: reaction kettle is put into the deionized water of 3000kg, opens stirring, is added into reaction kettle
The hydrofluoric acid that concentration is 41% is added into reaction kettle after solid zirconium oxychloride is completely dissolved for the solid zirconium oxychloride of 200kg
50kg is stirred 30 minutes, and the phosphatase 11 60kg that concentration is 90% is added into reaction kettle, stirs 30 minutes, starts to warm up, work as temperature
When reaching 60 DEG C, start to keep the temperature, soaking time 4 hours, after heat preservation, to temperature of reaction kettle naturally cool to 50 DEG C hereinafter,
It is filtered, washs, obtain flake matrix material filter cake；
Flake matrix material carries out the first subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, Xiang Fanying
Be added in kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 78 DEG C, start to keep the temperature, first use tetrachloro
Change titanium solution and the pH value of system is adjusted to 1.8, then adds the sodium hydroxide solution that titanium tetrachloride solution and concentration are 20% simultaneously
Enter into reaction kettle, remains that the pH value of system is to 1.8 in adition process, the addition total amount of titanium tetrachloride solution is 900
Rise, the concentration of titanium tetrachloride solution is 4.0 mol/Ls, control titanium tetrachloride solution and 20% sodium hydroxide solution addition when
Between be 7 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C hereinafter, carry out
It is filtered, washed, obtains the first subsurface cladding pearlescent pigment filter cake；Filter cake is dried at 110 DEG C, then at 820 DEG C
Under carry out calcining 1 hour, obtain illusion-colour and interfere blue pearlescent pigment；
Carry out the second subsurface cladding: reaction kettle is put into the deionized water of 2200 parts by weight, opens stirring, is added into reaction kettle
Above-mentioned first subsurface that obtains coats to obtain the blue pearlescent pigment of illusion-colour interference, starts to warm up, when temperature reaches 65 DEG C, starts to protect
The pH value of system is first adjusted to 4.0 with ammonium ferric sulfate solution, then ammonium ferric sulfate solution and concentrated ammonia solution is added simultaneously by temperature
The pH value that system is remained into reaction kettle, in adition process is to 4.0, and the addition total amount of ammonium ferric sulfate solution is 160 liters,
The concentration of ammonium ferric sulfate solution is 2.0 mol/Ls, and the addition time for controlling ammonium ferric sulfate solution and concentrated ammonia solution is 3 hours,
Potassium ferrocyanide is added with same method after addition, potassium ferrocyanide solution and concentrated ammonia solution are added to simultaneously anti-
It answers in kettle, remains that the pH value of system is to 4.0 in adition process, the addition total amount of potassium ferrocyanide solution is 120 liters, sub-
The concentration of potassium ferricyanide solution is 1.5 mol/Ls, and the addition time for controlling potassium ferrocyanide solution and concentrated ammonia solution is 2 small
When, addition finishes heat preservation 30 minutes, opens cooling water and cools down to reaction kettle, when temperature is down to 50 DEG C hereinafter, being filtered, washing
It washs, obtains the Prussian blue pearlescent pigment filter cake of illusion-colour；Filter cake is dried at 110 DEG C, obtains the Prussian blue pearly-lustre of illusion-colour
Pigment.
Embodiment 2
The preparation of flake matrix material: reaction kettle is put into the deionized water of 3000kg, opens stirring, is added into reaction kettle
The hydrofluoric acid that concentration is 42% is added into reaction kettle after solid zirconium oxychloride is completely dissolved for the solid zirconium oxychloride of 250kg
80kg is stirred 30 minutes, and the phosphoric acid 220kg that concentration is 93% is added into reaction kettle, stirs 30 minutes, starts to warm up, work as temperature
When reaching 90 DEG C, start to keep the temperature, soaking time 2 hours, after heat preservation, to temperature of reaction kettle naturally cool to 50 DEG C hereinafter,
It is filtered, washs, obtain flake matrix material filter cake；
Flake matrix material carries out the first subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, Xiang Fanying
Be added in kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 82 DEG C, start to keep the temperature, first use tetrachloro
Change titanium solution and the pH value of system is adjusted to 2.0, then adds the sodium hydroxide solution that titanium tetrachloride solution and concentration are 21% simultaneously
Enter into reaction kettle, remains that the pH value of system is to 2.0 in adition process, the addition total amount of titanium tetrachloride solution is 950
Rise, the concentration of titanium tetrachloride solution is 4.0 mol/Ls, control titanium tetrachloride solution and 21% sodium hydroxide solution addition when
Between be 8 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C hereinafter, carry out
It is filtered, washed, obtains the first subsurface cladding pearlescent pigment filter cake；Filter cake is dried at 130 DEG C, then at 850 DEG C
Under carry out calcining 1 hour, obtain illusion-colour and interfere blue pearlescent pigment；
Carry out the second subsurface cladding: reaction kettle is put into the deionized water of 2200 parts by weight, opens stirring, is added into reaction kettle
Above-mentioned first subsurface that obtains coats to obtain the blue pearlescent pigment of illusion-colour interference, starts to warm up, when temperature reaches 75 DEG C, starts to protect
The pH value of system is first adjusted to 4.5 with ammonium ferric sulfate solution, then ammonium ferric sulfate solution and concentrated ammonia solution is added simultaneously by temperature
The pH value that system is remained into reaction kettle, in adition process is to 4.5, and the addition total amount of ammonium ferric sulfate solution is 180 liters,
The concentration of ammonium ferric sulfate solution is 2.0 mol/Ls, and the addition time for controlling ammonium ferric sulfate solution and concentrated ammonia solution is 4 hours,
Potassium ferrocyanide is added with same method after addition, potassium ferrocyanide solution and concentrated ammonia solution are added to simultaneously anti-
It answers in kettle, remains that the pH value of system is to 4.5 in adition process, the addition total amount of potassium ferrocyanide solution is 140 liters, sub-
The concentration of potassium ferricyanide solution is 1.5 mol/Ls, and the addition time for controlling potassium ferrocyanide solution and concentrated ammonia solution is 3 small
When, addition finishes heat preservation 30 minutes, opens cooling water and cools down to reaction kettle, when temperature is down to 50 DEG C hereinafter, being filtered, washing
It washs, obtains the Prussian blue pearlescent pigment filter cake of illusion-colour；Filter cake is dried at 130 DEG C, obtains the Prussian blue pearly-lustre of illusion-colour
Pigment.
Embodiment 3
The preparation of flake matrix material: reaction kettle is put into the deionized water of 3000kg, opens stirring, is added into reaction kettle
The hydrogen fluorine that concentration is 41.5% is added into reaction kettle after solid zirconium oxychloride is completely dissolved for the solid zirconium oxychloride of 230kg
Sour 60kg is stirred 30 minutes, and the phosphatase 11 80kg that concentration is 91% is added into reaction kettle, stirs 30 minutes, starts to warm up, work as temperature
Degree starts to keep the temperature, soaking time 3 hours when reaching 70 DEG C, after heat preservation, to temperature of reaction kettle naturally cool to 50 DEG C with
Under, it is filtered, washs, obtain flake matrix material filter cake；
Flake matrix material carries out the first subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, Xiang Fanying
Be added in kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 80 DEG C, start to keep the temperature, first use tetrachloro
Change titanium solution and the pH value of system is adjusted to 1.9, then adds the sodium hydroxide solution that titanium tetrachloride solution and concentration are 25% simultaneously
Enter into reaction kettle, remains that the pH value of system is to 1.9 in adition process, the addition total amount of titanium tetrachloride solution is 910
Rise, the concentration of titanium tetrachloride solution is 4.0 mol/Ls, control titanium tetrachloride solution and 25% sodium hydroxide solution addition when
Between be 7.5 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C hereinafter, into
Row is filtered, washed, and obtains the first subsurface cladding pearlescent pigment filter cake；Filter cake is dried at 120 DEG C, then 830
Calcining 1 hour is carried out at DEG C, is obtained illusion-colour and is interfered blue pearlescent pigment；
Carry out the second subsurface cladding: reaction kettle is put into the deionized water of 2200 parts by weight, opens stirring, is added into reaction kettle
Above-mentioned first subsurface that obtains coats to obtain the blue pearlescent pigment of illusion-colour interference, starts to warm up, when temperature reaches 70 DEG C, starts to protect
The pH value of system is first adjusted to 4.2 with ammonium ferric sulfate solution, then ammonium ferric sulfate solution and concentrated ammonia solution is added simultaneously by temperature
The pH value that system is remained into reaction kettle, in adition process is to 4.2, and the addition total amount of ammonium ferric sulfate solution is 170 liters,
The concentration of ammonium ferric sulfate solution is 2.0 mol/Ls, and the addition time for controlling ammonium ferric sulfate solution and concentrated ammonia solution is 3.5 small
When, potassium ferrocyanide is added with same method after addition, potassium ferrocyanide solution and concentrated ammonia solution are added simultaneously
The pH value that system is remained into reaction kettle, in adition process is to 4.2, and the addition total amount of potassium ferrocyanide solution is 130
It rises, the concentration of potassium ferrocyanide solution is 1.5 mol/Ls, controls the addition time of potassium ferrocyanide solution and concentrated ammonia solution
It is 2.5 hours, addition finishes heat preservation 30 minutes, opens cooling water and cools down to reaction kettle, when temperature is down to 50 DEG C hereinafter, carrying out
It is filtered, washed, obtains the Prussian blue pearlescent pigment filter cake of illusion-colour；Filter cake is dried at 120 DEG C, obtains illusion-colour Prussia
Blue pearlescent pigment.
Embodiment 4
The preparation of flake matrix material: reaction kettle is put into the deionized water of 3000kg, opens stirring, is added into reaction kettle
The hydrogen fluorine that concentration is 41.8% is added into reaction kettle after solid zirconium oxychloride is completely dissolved for the solid zirconium oxychloride of 240kg
Sour 75kg is stirred 30 minutes, and the phosphoric acid 215kg that concentration is 92.8% is added into reaction kettle, stirs 30 minutes, starts to warm up, when
When temperature reaches 85 DEG C, start to keep the temperature, soaking time 2.5 hours, after heat preservation, naturally cools to 50 DEG C to temperature of reaction kettle
Hereinafter, being filtered, washing, flake matrix material filter cake is obtained；
Flake matrix material carries out the first subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, Xiang Fanying
Be added in kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 82 DEG C, start to keep the temperature, first use tetrachloro
Change titanium solution and the pH value of system is adjusted to 2.0, then adds the sodium hydroxide solution that titanium tetrachloride solution and concentration are 22% simultaneously
Enter into reaction kettle, remains that the pH value of system is to 2.0 in adition process, the addition total amount of titanium tetrachloride solution is 940
Rise, the concentration of titanium tetrachloride solution is 4.0 mol/Ls, control titanium tetrachloride solution and 22% sodium hydroxide solution addition when
Between be 7 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C hereinafter, carry out
It is filtered, washed, obtains the first subsurface cladding pearlescent pigment filter cake；Filter cake is dried at 128 DEG C, then at 845 DEG C
Under carry out calcining 1 hour, obtain illusion-colour and interfere blue pearlescent pigment；
Carry out the second subsurface cladding: reaction kettle is put into the deionized water of 2200 parts by weight, opens stirring, is added into reaction kettle
Above-mentioned first subsurface that obtains coats to obtain the blue pearlescent pigment of illusion-colour interference, starts to warm up, when temperature reaches 68 DEG C, starts to protect
The pH value of system is first adjusted to 4.3 with ammonium ferric sulfate solution, then ammonium ferric sulfate solution and concentrated ammonia solution is added simultaneously by temperature
The pH value that system is remained into reaction kettle, in adition process is to 4.3, and the addition total amount of ammonium ferric sulfate solution is 168 liters,
The concentration of ammonium ferric sulfate solution is 2.0 mol/Ls, and the addition time for controlling ammonium ferric sulfate solution and concentrated ammonia solution is 3.2 small
When, potassium ferrocyanide is added with same method after addition, potassium ferrocyanide solution and concentrated ammonia solution are added simultaneously
The pH value that system is remained into reaction kettle, in adition process is to 4.3, and the addition total amount of potassium ferrocyanide solution is 128
It rises, the concentration of potassium ferrocyanide solution is 1.5 mol/Ls, controls the addition time of potassium ferrocyanide solution and concentrated ammonia solution
It is 2.4 hours, addition finishes heat preservation 30 minutes, opens cooling water and cools down to reaction kettle, when temperature is down to 50 DEG C hereinafter, carrying out
It is filtered, washed, obtains the Prussian blue pearlescent pigment filter cake of illusion-colour；Filter cake is dried at 118 DEG C, obtains illusion-colour Prussia
Blue pearlescent pigment.
Embodiment 5
The preparation of flake matrix material: reaction kettle is put into the deionized water of 3000kg, opens stirring, is added into reaction kettle
The hydrogen fluorine that concentration is 41.6% is added into reaction kettle after solid zirconium oxychloride is completely dissolved for the solid zirconium oxychloride of 225kg
Sour 70kg is stirred 30 minutes, and the phosphoric acid 200kg that concentration is 92% is added into reaction kettle, stirs 30 minutes, starts to warm up, work as temperature
Degree starts to keep the temperature, soaking time 3 hours when reaching 80 DEG C, after heat preservation, to temperature of reaction kettle naturally cool to 50 DEG C with
Under, it is filtered, washs, obtain flake matrix material filter cake；
Flake matrix material carries out the first subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, Xiang Fanying
Be added in kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 78 DEG C, start to keep the temperature, first use tetrachloro
Change titanium solution and the pH value of system is adjusted to 1.8, then adds the sodium hydroxide solution that titanium tetrachloride solution and concentration are 24% simultaneously
Enter into reaction kettle, remains that the pH value of system is to 1.8 in adition process, the addition total amount of titanium tetrachloride solution is 930
Rise, the concentration of titanium tetrachloride solution is 4.0 mol/Ls, control titanium tetrachloride solution and 24% sodium hydroxide solution addition when
Between be 7 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C hereinafter, carry out
It is filtered, washed, obtains the first subsurface cladding pearlescent pigment filter cake；Filter cake is dried at 122 DEG C, then at 835 DEG C
Under carry out calcining 1 hour, obtain illusion-colour and interfere blue pearlescent pigment；
Carry out the second subsurface cladding: reaction kettle is put into the deionized water of 2200 parts by weight, opens stirring, is added into reaction kettle
Above-mentioned first subsurface that obtains coats to obtain the blue pearlescent pigment of illusion-colour interference, starts to warm up, when temperature reaches 72 DEG C, starts to protect
The pH value of system is first adjusted to 4.1 with ammonium ferric sulfate solution, then ammonium ferric sulfate solution and concentrated ammonia solution is added simultaneously by temperature
The pH value that system is remained into reaction kettle, in adition process is to 4.1, and the addition total amount of ammonium ferric sulfate solution is 177 liters,
The concentration of ammonium ferric sulfate solution is 2.0 mol/Ls, and the addition time for controlling ammonium ferric sulfate solution and concentrated ammonia solution is 3.7 small
When, potassium ferrocyanide is added with same method after addition, potassium ferrocyanide solution and concentrated ammonia solution are added simultaneously
The pH value that system is remained into reaction kettle, in adition process is to 4.1, and the addition total amount of potassium ferrocyanide solution is 133
It rises, the concentration of potassium ferrocyanide solution is 1.5 mol/Ls, controls the addition time of potassium ferrocyanide solution and concentrated ammonia solution
It is 2.7 hours, addition finishes heat preservation 30 minutes, opens cooling water and cools down to reaction kettle, when temperature is down to 50 DEG C hereinafter, carrying out
It is filtered, washed, obtains the Prussian blue pearlescent pigment filter cake of illusion-colour；Filter cake is dried at 122 DEG C, obtains illusion-colour Prussia
Blue pearlescent pigment.
Embodiment 6
The preparation of flake matrix material: reaction kettle is put into the deionized water of 3000kg, opens stirring, is added into reaction kettle
The hydrofluoric acid that concentration is 42% is added into reaction kettle after solid zirconium oxychloride is completely dissolved for the solid zirconium oxychloride of 230kg
68kg is stirred 30 minutes, and the phosphatase 11 90kg that concentration is 92% is added into reaction kettle, stirs 30 minutes, starts to warm up, work as temperature
When reaching 75 DEG C, start to keep the temperature, soaking time 4 hours, after heat preservation, to temperature of reaction kettle naturally cool to 50 DEG C hereinafter,
It is filtered, washs, obtain flake matrix material filter cake；
Flake matrix material carries out the first subsurface cladding: reaction kettle is put into the deionized water of 2200kg, opens stirring, Xiang Fanying
Be added in kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 81 DEG C, start to keep the temperature, first use tetrachloro
Change titanium solution and the pH value of system is adjusted to 2.0, then adds the sodium hydroxide solution that titanium tetrachloride solution and concentration are 22% simultaneously
Enter into reaction kettle, remains that the pH value of system is to 2.0 in adition process, the addition total amount of titanium tetrachloride solution is 920
Rise, the concentration of titanium tetrachloride solution is 4.0 mol/Ls, control titanium tetrachloride solution and 22% sodium hydroxide solution addition when
Between be 7 hours, addition finish heat preservation 30 minutes, open cooling water and reaction kettle cooled down, when temperature be down to 50 DEG C hereinafter, carry out
It is filtered, washed, obtains the first subsurface cladding pearlescent pigment filter cake；Filter cake is dried at 130 DEG C, then at 820 DEG C
Under carry out calcining 1 hour, obtain illusion-colour and interfere blue pearlescent pigment；
Carry out the second subsurface cladding: reaction kettle is put into the deionized water of 2200 parts by weight, opens stirring, is added into reaction kettle
Above-mentioned first subsurface that obtains coats to obtain the blue pearlescent pigment of illusion-colour interference, starts to warm up, when temperature reaches 71 DEG C, starts to protect
The pH value of system is first adjusted to 4.4 with ammonium ferric sulfate solution, then ammonium ferric sulfate solution and concentrated ammonia solution is added simultaneously by temperature
The pH value that system is remained into reaction kettle, in adition process is to 4.4, and the addition total amount of ammonium ferric sulfate solution is 172 liters,
The concentration of ammonium ferric sulfate solution is 2.0 mol/Ls, and the addition time for controlling ammonium ferric sulfate solution and concentrated ammonia solution is 3.3 small
When, potassium ferrocyanide is added with same method after addition, potassium ferrocyanide solution and concentrated ammonia solution are added simultaneously
The pH value that system is remained into reaction kettle, in adition process is to 4.4, and the addition total amount of potassium ferrocyanide solution is 138
It rises, the concentration of potassium ferrocyanide solution is 1.5 mol/Ls, controls the addition time of potassium ferrocyanide solution and concentrated ammonia solution
It is 2.8 hours, addition finishes heat preservation 30 minutes, opens cooling water and cools down to reaction kettle, when temperature is down to 50 DEG C hereinafter, carrying out
It is filtered, washed, obtains the Prussian blue pearlescent pigment filter cake of illusion-colour；Filter cake is dried at 126 DEG C, obtains illusion-colour Prussia
Blue pearlescent pigment.
Claims (1)
1. a kind of preparation method of the Prussian blue pearlescent pigment of illusion-colour, feature the following steps are included: prepare flaky matrix first
Then material carries out surface cladding to flake matrix material；The preparation method of flake matrix material: reaction kettle is put into 3000 weight
The deionized water of part opens stirring, the solid zirconium oxychloride of 200~250 parts by weight is added into reaction kettle, to solid oxychlorination
After zirconium is completely dissolved, the hydrofluoric acid of 50~80 parts by weight is added into reaction kettle, hydrofluoric acid concentration is 41~42%, stirs 30 points
The phosphoric acid of 160~220 parts by weight is added into reaction kettle for clock, and phosphoric acid concentration is 90~93%, stirs 30 minutes, starts to warm up,
When temperature reaches 60~90 DEG C, start to keep the temperature, it is soaking time 2~4 hours, naturally cold to temperature of reaction kettle after heat preservation
But to 50 DEG C hereinafter, be filtered, wash, flake matrix material filter cake is obtained；
2 progress of flake matrix material surface cladding point, first time surface coating method: reaction kettle is put into going for 2200 parts by weight
Ionized water, open stirring, be added into reaction kettle it is above-mentioned obtain flake matrix material filter cake, start to warm up, when temperature reaches 78
At~82 DEG C, start to keep the temperature, the pH value of system is first adjusted to 1.8~2.0 with titanium tetrachloride solution, then by titanium tetrachloride solution
The sodium hydroxide solution for being 20~25% with concentration is added in reaction kettle simultaneously, and the pH value of system is remained in adition process
It is 900~950 parts by volume for the addition total amount to 1.8~2.0, titanium tetrachloride solution, controls titanium tetrachloride solution and 20~25%
Sodium hydroxide solution the addition time be 7~8 hours, addition finish heat preservation 30 minutes, open cooling water to reaction kettle carry out it is cold
But, when temperature is down to 50 DEG C hereinafter, be filtered, wash, the first subsurface cladding pearlescent pigment filter cake is obtained；Filter cake is existed
It is dried at 110~130 DEG C, calcining 1 hour is then carried out at 820~850 DEG C, obtained illusion-colour and interfere blue pearlescent pigment,
The concentration of the titanium tetrachloride solution is 4.0 mol/Ls；
Second of surface coating method: reaction kettle is put into the deionized water of 2200 parts by weight, opens stirring, is added into reaction kettle
Above-mentioned first subsurface that obtains coats to obtain the blue pearlescent pigment of illusion-colour interference, starts to warm up, when temperature reaches 65~75 DEG C, opens
Begin to keep the temperature, the pH value of system is first adjusted to 4.0~4.5 with ammonium ferric sulfate solution, it is then that ammonium ferric sulfate solution and concentrated ammonia liquor is molten
Liquid is added in reaction kettle simultaneously, remained in adition process system pH value be to 4.0~4.5, ammonium ferric sulfate solution
Addition total amount is 160~180 parts by volume, and the addition time for controlling ammonium ferric sulfate solution and concentrated ammonia solution is 3~4 hours, is added
Potassium ferrocyanide is added with same method after entering, potassium ferrocyanide solution and concentrated ammonia solution are added to reaction simultaneously
The pH value that system is remained in kettle, in adition process is to 4.0~4.5, the addition total amount of potassium ferrocyanide solution is 120~
140 parts by volume, the addition time for controlling potassium ferrocyanide solution and concentrated ammonia solution is 2~3 hours, and addition finishes 30 points of heat preservation
Clock is opened cooling water and is cooled down to reaction kettle, and when temperature is down to 50 DEG C hereinafter, be filtered, wash, it is Prussian blue to obtain illusion-colour
Pearlescent pigment filter cake；Filter cake is dried at 110~130 DEG C, obtains the Prussian blue pearlescent pigment of illusion-colour；
The concentration of the ammonium ferric sulfate solution is 2.0 mol/Ls；
The concentration of the potassium ferrocyanide solution is 1.5 mol/Ls.
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| CN102181176A (en) * | 2011-06-03 | 2011-09-14 | 杭州弗沃德精细化工有限公司 | Process for preparing iron blue with fantastic color effect |
| CN102260421A (en) * | 2011-06-08 | 2011-11-30 | 四川大学 | Magic-color nacreous aluminum powder pigment and preparation method thereof |
| CN102443285A (en) * | 2011-09-05 | 2012-05-09 | 福州坤彩精化有限公司 | Prussian blue pearlescent pigment and preparation method thereof |
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2019
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102181176A (en) * | 2011-06-03 | 2011-09-14 | 杭州弗沃德精细化工有限公司 | Process for preparing iron blue with fantastic color effect |
| CN102260421A (en) * | 2011-06-08 | 2011-11-30 | 四川大学 | Magic-color nacreous aluminum powder pigment and preparation method thereof |
| CN102443285A (en) * | 2011-09-05 | 2012-05-09 | 福州坤彩精化有限公司 | Prussian blue pearlescent pigment and preparation method thereof |
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| 袁潇等: "磷酸锆碟片粒径对提高二氧化钛悬浮液分散稳定性的影响", 《功能材料》 * |
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