CN109054448A - A kind of compound blue ceramic pigment Cu2Y2O5-SiO2Preparation method - Google Patents
A kind of compound blue ceramic pigment Cu2Y2O5-SiO2Preparation method Download PDFInfo
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Abstract
The invention discloses a kind of compound blue ceramic pigment Cu2Y2O5‑SiO2Preparation method, mainly comprise the steps that 1) at room temperature, by Cu2Y2O5It is dispersed in by a certain percentage with dispersing agent in the mixed solution of the dehydrated alcohol of deionized water and 2-3 volume times, is ultrasonically treated 1h, obtains solution A；2) in deionized water by ethyl orthosilicate (TEOS) condition dispersion by a certain percentage, and ammonium hydroxide tune pH value is added dropwise, obtains solution B；3) solution B is added in solution A, is continuously stirred, after obtaining reddish-brown precipitation, compound blue ceramic pigment is can be obtained in centrifugation, dry, grinding；Have many advantages, such as that large specific surface area, high temperature resistant, chemical stability are good, bright in colour using the compound blue ceramic pigment of the method for the present invention preparation gained.
Description
Technical field
The present invention relates to ceramic paint technical fields, and in particular to a kind of compound blue ceramic pigment Cu2Y2O5-SiO2
Preparation method.
Background technique
Blue is a kind of color, it is a member in the three primary colors of RGB light, its wavelength is most in these three primary colors
It is short, it is 440~475 nanometers, belongs to short wavelength.Blue ceramic pigment is either used for ceramic illuminated, or as ceramics
The toner of color glaze or color embryo is all the indispensable ornament materials of ceramic decoration art.Traditional blue pigment includes toxic mostly
Heavy metal such as lead, chromium etc., serious influence is caused on environment and individual, and the pigment of traditional single performance cannot expire
The demand of sufficient all trades and professions.Simultaneously it is known that when scantling drops to after nanoscale, just have conventional material incomparable
Superior function.Therefore, the synthetic method for seeking green, obtains that size is small, good dispersion, granularity in relatively mild environment
The high-performance nano blue pigment being evenly distributed is imperative.
Common Nano-meter SiO_22It is a kind of unformed, nontoxic, white, tasteless powdered substance, there is high temperature resistant, chemistry
The characteristics of stability.It not only has particle size and density is smaller, large specific surface area, good dispersion etc. are as engineering material
Other than outstanding feature, but also because its size reaches nanometer scale to make it have and receive possessed by general nano material
Rice characteristic.Regardless of having its unique effect for testing still industry, for example as catalyst, pharmaceutical carrier, building coating
Additive, material settling out agent, and in Environment Science, it is also used to biologic medical, pollution processing, new high-tech material etc. and much leads
Domain.
Application No. is 201610665535.X patent applications to disclose a kind of preparation method of blue pigment modelled after an antique, belongs to Gu
Ceramic paint technical field.This method uses co-precipitation-hydrothermal synthesis method, and the pigment purity of preparation is high, crystalline condition is good,
But this method production cycle is long, and the addition of precipitating reagent may make local concentration excessively high, and it generates reunion or composition is not uniform enough,
It is unfavorable for being mass produced.
Summary of the invention
For the above technical problems, the present invention provides a kind of compound blue ceramic pigment Cu2Y2O5/SiO2
Preparation method, by SiO2With blue pigment Cu2Y2O5Carry out compound, synthesis, high temperature resistant, chemical stability at normal temperature
The environmentally friendly inorganic pigment of blue high, bright in colour.
The technical solution of the present invention is as follows: a kind of compound blue ceramic pigment Cu2Y2O5-SiO2Preparation method, it is main to wrap
Include following steps:
S1: at room temperature, by Cu2Y2O5Disperse in deionized water, to add 2-3 according to molar ratio 1:10 with dispersing agent
The dehydrated alcohol of times volume is ultrasonically treated 1-3h, obtains solution A；
S2: ethyl orthosilicate and dispersing agent are dispersed in deionized water, ammonium hydroxide to be added dropwise and adjusts solution according to molar ratio 2:1
PH value obtains solution B to 6-9；
S3: above-mentioned solution B is added in solution A, 20-60min is continuously stirred using magnetic stirring apparatus, is received using centrifuge
Collect bottom sediment, and sediment is cleaned with water and dehydrated alcohol；
S4: S3 products therefrom is placed in drying box, and dry 5-8h, grinds by grinding device under the conditions of 70-90 DEG C
Compound blue ceramic pigment can be obtained.
Further, the Cu in step S12Y2O5It is made by following steps:
1) by Cu (NO3)2·3H2O、Y(NO3)3·6H2O is added in the aqueous solution of glycine, is first stirred at 50-70 DEG C
It mixes to clarification；
2) 1) acquired solution in is heated to 100-120 DEG C, stirs 90-110min, solution occurs from climing in the process
Prolong combustion reaction and generates loose powder；
3) 2) gained powder is calcined under the conditions of 700-900 DEG C up to Cu2Y2O5Finished product.
Preferably, the calcination temperature of powder is 750-850 DEG C in step 3).
It is highly preferred that the calcination temperature of powder is 750 DEG C in step 3).
Further, the Cu (NO of addition3)2·3H2O、Y(NO3)3·6H2Respectively in terms of Cu, Y, glycine mole is O
2 times of the sum of Cu, Y mole.
Further, in step S1, any one in dispersing agent PVP, SDS, SDBS.
Further, in step S3, the mixing speed of magnetic stirring apparatus is 80-100r/min.
Further, in step S3, complexing agent is added into the mixed solution of solution A and solution B in whipping process, is complexed
The preparation method of agent is by sodium hydroxide, phosphoric acid and methyl acid phosphate 3:2:1 hybrid reaction in molar ratio, and reaction solution by doing by spraying
It is dry to obtain partially polymerized intermediate powder, which is put into drying box and carries out polymerization reaction, polymerization reaction knot
Complexing agent finished product is obtained after beam；The temperature inside the box control is wherein dried at 180-270 DEG C, polymerization reaction time 8-15h.
Further, in step S3, antiwear assistant is added into the mixed solution of solution A and solution B in whipping process, it is resistance to
The raw material of milling aid include: by weight 3 parts of starch, 7 parts of distilled water, 9 parts of maleic anhydride, 6 parts of ammonium persulfate, 2 parts of styrene,
3 parts of aluminium chloride, 6 parts of potassium hydroxide, 1 part of bentonite, 9 parts of plant fiber, 2 parts of silane coupling agent；The preparation method of antiwear assistant
Are as follows: under nitrogen protection, starch, distilled water and maleic anhydride are uniformly mixed, then heat to 75 DEG C, keeps the temperature 1h, then plus
Entering ammonium persulfate to be uniformly mixed, addition styrene is uniformly mixed after stirring 25min, 45min is then stirred with 750r/min revolving speed,
95 DEG C are then heated to, extracts 30h, then in vacuum drying oven, 60 DEG C dry to constant weight, and are cooled to room temperature to obtain material A；By chlorine
Change aluminium, potassium hydroxide and water to be uniformly mixed, stirs evenly, be stored at room temperature 8d and obtain material B, then add swelling into material B
Soil and plant fiber are stored at room temperature 7d, and silane coupling agent is added and material A is uniformly mixed, with the stirring of 2800r/min revolving speed
50min then heats to 150 DEG C, and dry 6h, crushing after being cooled to room temperature can be obtained antiwear assistant finished product.
Further, in step S4, grinding device includes shell, level-one grinding assembly, secondary grinder component, power supply dress
It sets；Shell upper end is provided with feed hopper, shell lower end is provided with blanking port；Level-one grinding assembly includes that primary motor, level-one are ground
Grinding roller；Two-level grinding device includes secondary grinder stick, abrasive disk and Power Component, Power Component include secondary motor, eccentric wheel,
Oscillating rod；There are two level-one mixing rolls, and upper end, two level-ones are ground inside housings for two level-one mixing roll horizontal alignment settings
Roller surface is provided with multiple abrasive grains, and material blocking block, primary motor one are provided between two level-one mixing rolls and shell
Grade mixing roll provides power, and enclosure interior is provided with refining plate, and refining plate is located at two level-one mixing roll lower ends；Grind disk activity
Setting inside housings, is located at refining plate lower end, is provided with arc groove on abrasive disk, there are two arc grooves, on abrasive disk
It is provided through material-dropping hole, abrasive disk and shell contact position are provided with reset assembly, and there are two secondary grinder sticks, and two second levels are ground
The surface of frotton is provided with grinding protrusion, and the both ends of two secondary grinder sticks are movably set with connecting rod, four connecting rods
Upper end be movably set with movable plate, be connected with tension spring between two connecting rods of the left and right sides, connection be provided on movable plate
Ear, secondary motor provide power for eccentric wheel, and eccentric wheel is connect with engaging lug by oscillating rod, can by the rotation of eccentric wheel
To drive two secondary grinder sticks to roll on two arc grooves respectively；Power supply device is primary motor, secondary motor provides
Power supply.
Compared with prior art, beneficial effects of the present invention: the present invention is by Cu2Y2O5Blue pigment and SiO2It is compound, pass through
The advantage of the two is performed to most preferably, has synthesized Cu by the synergistic effect of the two2Y2O5-SiO2Nano composite ceramic pigment；This
The compound blue ceramic pigment of invention gained combines Cu2Y2O5And SiO2Excellent performance, have that bright in colour, high temperature is constant
The advantages that color.In addition, preparation method of the present invention is simple, raw material is easy to get, and synthesis temperature is low, and simple process is controllable, is suitable for scale
Production；And products obtained therefrom is low molecule, low toxicity even non-toxic organic object, without the toxic elements such as lead chromium, environmentally protective, product grain
Molecular dispersivity is good, even particle size distribution, and colour generation is good.
Detailed description of the invention
Fig. 1 is Cu2Y2O5Under different calcination temperatures X-ray diffraction spectrogram (a:700 DEG C, b:750 DEG C, c:800 DEG C, d:
900℃)；
Fig. 2 be the matrix compound blue ceramic pigment different from SDS molar ratio X-ray diffraction spectrogram (a: matrix with
SDS molar ratio 1:5, b: matrix and SDS molar ratio 1:10)；
Fig. 3 is the X-ray diffraction spectrogram (a: base of the matrix compound blue ceramic pigment different from ethyl orthosilicate mole
Body and ethyl orthosilicate molar ratio 1:1, b: matrix and ethyl orthosilicate molar ratio 1:2)；
Fig. 4 is the X-ray diffraction spectrogram (a: surfactant of the different compound blue ceramic pigment of surfactant
SDBS, b: surfactant SDS)；
Fig. 5 is Cu2Y2O5SEM image (a:1 μm, b:100 μm :) under 750 DEG C of temperature calcinations；
Fig. 6 is the SEM image (a: matrix, b: after cladding) that matrix cladding front and back compares；
Fig. 7 be matrix and the different compound blue ceramic pigment of SDS molar ratio SEM image (a: ratio 1:5, b:
Ratio is 1:10)；
Fig. 8 be matrix and the different compound blue ceramic pigment of ethyl orthosilicate mole SEM image (a: ratio 1:
1, b: ratio 1:2)；
Fig. 9 is the SEM image (a:SDBS, b:SDS) of the different compound blue ceramic pigment of surfactant；
Figure 10 is the structural schematic diagram of grinding device of the invention；
Figure 11 is the structural schematic diagram of abrasive disk of the invention；
Figure 12 is the structural schematic diagram of eccentric wheel and oscillating rod of the invention；
Figure 13 is the structural schematic diagram of secondary grinder stick of the invention；
Wherein, 1- shell, 11- feed hopper, 12- blanking port, 2- level-one grinding assembly, 21- level-one mixing roll, 22- backgauge
Block, 23- refining plate, 3- secondary grinder component, 31- secondary grinder stick, 32- abrasive disk, 320- arc groove, 321- material-dropping hole,
33- reset assembly, 34- connecting rod, 340- tension spring, 35 movable plates, 350- engaging lug, 36- Power Component, 36- eccentric wheel, 362-
Oscillating rod.
Specific embodiment
Technical solution of the present invention is further discussed in detail with reference to embodiments, but protection scope of the present invention
It is not limited thereto.
Cu2Y2O5Preparation example 1:
3g glycine is dissolved in 100mL distilled water first, the Cu (NO of 2.42g is then added3)2·3H2O's and 3.83g
Y(NO3)3·6H2O is placed on stirring and dissolving on the magnetic stirring apparatus that set temperature is 50 DEG C, until dissolution obtains clarified solution (about completely
Need 20min)；100 DEG C of reaction 100min are then heated to, liquid is sticky in the process expands, and then releases gas, fast
Self-propagating combustion reaction occurs for speed, generates loose powder；Gained powder calcines 4h at 700 DEG C, i.e., blue nano dye
Cu2Y2O5。
Cu2Y2O5Preparation example 2:
3g glycine is dissolved in 100mL distilled water first, the Cu (NO of 2.42g is then added3)2·3H2O's and 3.83g
Y(NO3)3·6H2O is placed on stirring and dissolving on the magnetic stirring apparatus that set temperature is 60 DEG C, until dissolution obtains clarified solution (about completely
Need 20min)；110 DEG C of reaction 100min are then heated to, liquid is sticky in the process expands, and then releases gas, fast
Self-propagating combustion reaction occurs for speed, generates loose powder；Gained powder calcines 4h at 750 DEG C, i.e., blue nano dye
Cu2Y2O5。
Cu2Y2O5Preparation example 3:
3g glycine is dissolved in 100mL distilled water first, the Cu (NO of 2.42g is then added3)2·3H2O's and 3.83g
Y(NO3)3·6H2O is placed on stirring and dissolving on the magnetic stirring apparatus that set temperature is 60 DEG C, until dissolution obtains clarified solution (about completely
Need 20min)；110 DEG C of reaction 100min are then heated to, liquid is sticky in the process expands, and then releases gas, fast
Self-propagating combustion reaction occurs for speed, generates loose powder；Gained powder calcines 4h at 850 DEG C, i.e., blue nano dye
Cu2Y2O5。
Cu2Y2O5Preparation example 4:
3g glycine is dissolved in 100mL distilled water first, the Cu (NO of 2.42g is then added3)2·3H2O's and 3.83g
Y(NO3)3·6H2O is placed on stirring and dissolving on the magnetic stirring apparatus that set temperature is 70 DEG C, until dissolution obtains clarified solution (about completely
Need 20min)；120 DEG C of reaction 100min are then heated to, liquid is sticky in the process expands, and then releases gas, fast
Self-propagating combustion reaction occurs for speed, generates loose powder；Gained powder calcines 4h at 900 DEG C, i.e., blue nano dye
Cu2Y2O5。
Embodiment 1:
A kind of compound blue ceramic pigment Cu2Y2O5-SiO2Preparation method, mainly comprise the steps that
S1: at room temperature, by 0.2gCu2Y2O5It is dispersed in 80ml deionized water with 1.4gSDS according to molar ratio 1:10,
The dehydrated alcohol of 2 times of volumes is added, 1h is ultrasonically treated, obtains solution A；Wherein, Cu2Y2O5Using 1 gained of preparation example, addition
Cu (NO3)2·3H2O、Y(NO3)3·6H2For O respectively in terms of Cu, Y, glycine mole is 2 times of the sum of Cu, Y mole；
S2: 0.2g ethyl orthosilicate and SDS are dispersed in 50ml deionized water according to molar ratio 2:1, and ammonium hydroxide tune is added dropwise
Solution ph is saved to 6, obtains solution B；
S3: above-mentioned solution B is added in solution A, continuously stirs 20min using magnetic stirring apparatus, magnetic stirring apparatus stirs
Mixing speed is 80r/min, collects bottom sediment using centrifuge, and be respectively washed three to sediment with water and dehydrated alcohol
It is secondary；
S4: S3 products therefrom is placed in drying box, and dry 5h under the conditions of 70 DEG C can be obtained by grinding device grinding
To compound blue ceramic pigment.
Embodiment 2:
A kind of compound blue ceramic pigment Cu2Y2O5-SiO2Preparation method, mainly comprise the steps that
S1: at room temperature, by 0.2gCu2Y2O5It is dispersed in 90ml deionized water with 1.4gPVP according to molar ratio 1:10,
The dehydrated alcohol of 2 times of volumes is added, 1h is ultrasonically treated, obtains solution A；Wherein, Cu2Y2O5Using 2 gained of preparation example, addition
Cu (NO3)2·3H2O、Y(NO3)3·6H2For O respectively in terms of Cu, Y, glycine mole is 2 times of the sum of Cu, Y mole；
S2: 0.2g ethyl orthosilicate and SDS are dispersed in 60ml deionized water according to molar ratio 2:1, and ammonium hydroxide tune is added dropwise
Solution ph is saved to 9, obtains solution B；
S3: above-mentioned solution B is added in solution A, continuously stirs 40min using magnetic stirring apparatus, magnetic stirring apparatus stirs
Mixing speed is 90r/min, collects bottom sediment using centrifuge, and be respectively washed three to sediment with water and dehydrated alcohol
It is secondary；
S4: S3 products therefrom is placed in drying box, and dry 6h under the conditions of 80 DEG C can be obtained by grinding device grinding
To compound blue ceramic pigment.
Embodiment 3:
A kind of compound blue ceramic pigment Cu2Y2O5-SiO2Preparation method, mainly comprise the steps that
S1: at room temperature, by 0.2gCu2Y2O5It is dispersed in 100ml deionized water with 0.7gSDS according to molar ratio 1:10,
The dehydrated alcohol of 3 times of volumes is added, 1h is ultrasonically treated, obtains solution A；Wherein, Cu2Y2O5Using 3 gained of preparation example, addition
Cu (NO3)2·3H2O、Y(NO3)3·6H2For O respectively in terms of Cu, Y, glycine mole is 2 times of the sum of Cu, Y mole；
S2: 0.2g ethyl orthosilicate and SDS are dispersed in 60ml deionized water according to molar ratio 2:1, and ammonium hydroxide tune is added dropwise
Solution ph is saved to 8, obtains solution B；
S3: above-mentioned solution B is added in solution A, continuously stirs 60min using magnetic stirring apparatus, magnetic stirring apparatus stirs
Mixing speed is 100r/min, collects bottom sediment using centrifuge, and be respectively washed three to sediment with water and dehydrated alcohol
It is secondary；
S4: S3 products therefrom is placed in drying box, and dry 7h under the conditions of 90 DEG C can be obtained by grinding device grinding
To compound blue ceramic pigment.
Embodiment 4:
A kind of compound blue ceramic pigment Cu2Y2O5-SiO2Preparation method, mainly comprise the steps that
S1: at room temperature, by 0.2gCu2Y2O5100ml deionized water is dispersed according to molar ratio 1:10 with 0.7gSDBS
In, the dehydrated alcohol of 3 times of volumes is added, 1h is ultrasonically treated, obtains solution A；Wherein, Cu2Y2O5Using 3 gained of preparation example, add
Cu (the NO added3)2·3H2O、Y(NO3)3·6H2For O respectively in terms of Cu, Y, glycine mole is 2 times of the sum of Cu, Y mole；
S2: 0.2g ethyl orthosilicate and SDS are dispersed in 60ml deionized water according to molar ratio 2:1, and ammonium hydroxide tune is added dropwise
Solution ph is saved to 8, obtains solution B；
S3: above-mentioned solution B is added in solution A, continuously stirs 60min using magnetic stirring apparatus, magnetic stirring apparatus stirs
Mixing speed is 100r/min, collects bottom sediment using centrifuge, and be respectively washed three to sediment with water and dehydrated alcohol
It is secondary；
S4: S3 products therefrom is placed in drying box, and dry 8h under the conditions of 90 DEG C can be obtained by grinding device grinding
To compound blue ceramic pigment.
Embodiment 5:
A kind of compound blue ceramic pigment Cu2Y2O5-SiO2Preparation method, mainly comprise the steps that
S1: at room temperature, by 0.2gCu2Y2O5It is dispersed in 80ml deionized water with 1.4gSDS according to molar ratio 1:10,
The dehydrated alcohol of 2 times of volumes is added, 1h is ultrasonically treated, obtains solution A；Wherein, Cu2Y2O5Using 1 gained of preparation example, addition
Cu (NO3)2·3H2O、Y(NO3)3·6H2For O respectively in terms of Cu, Y, glycine mole is 2 times of the sum of Cu, Y mole；
S2: 0.2g ethyl orthosilicate and SDS are dispersed in 50ml deionized water according to molar ratio 2:1, and ammonium hydroxide tune is added dropwise
Solution ph is saved to 8, obtains solution B；
S3: above-mentioned solution B is added in solution A, continuously stirs 20min using magnetic stirring apparatus, magnetic stirring apparatus stirs
Mixing speed is 100r/min, collects bottom sediment using centrifuge, and be respectively washed three to sediment with water and dehydrated alcohol
It is secondary；
S4: S3 products therefrom is placed in drying box, and dry 6h under the conditions of 70 DEG C can be obtained by grinding device grinding
To compound blue ceramic pigment.
Embodiment 6:
A kind of compound blue ceramic pigment Cu2Y2O5-SiO2Preparation method, mainly comprise the steps that
S1: at room temperature, by 0.2gCu2Y2O5It is dispersed in 90ml deionized water with 1.4gSDS according to molar ratio 1:10,
The dehydrated alcohol of 2 times of volumes is added, 1h is ultrasonically treated, obtains solution A；Wherein, Cu2Y2O5Using 2 gained of preparation example, addition
Cu (NO3)2·3H2O、Y(NO3)3·6H2For O respectively in terms of Cu, Y, glycine mole is 2 times of the sum of Cu, Y mole；
S2: 0.2g ethyl orthosilicate and SDS are dispersed in 60ml deionized water according to molar ratio 2:1, and ammonium hydroxide tune is added dropwise
Solution ph is saved to 9, obtains solution B；
S3: above-mentioned solution B is added in solution A, continuously stirs 40min using magnetic stirring apparatus, magnetic stirring apparatus stirs
Mixing speed is 100r/min, collects bottom sediment using centrifuge, and be respectively washed three to sediment with water and dehydrated alcohol
It is secondary；
S4: S3 products therefrom is placed in drying box, and dry 6h under the conditions of 80 DEG C can be obtained by grinding device grinding
To compound blue ceramic pigment.
Embodiment 7:
A kind of compound blue ceramic pigment Cu2Y2O5-SiO2Preparation method, mainly comprise the steps that
S1: at room temperature, by 0.2gCu2Y2O5It is dispersed in 90ml deionized water with 1.4gSDS according to molar ratio 1:10,
The dehydrated alcohol of 2 times of volumes is added, 1h is ultrasonically treated, obtains solution A；Wherein, Cu2Y2O5Using 2 gained of preparation example, addition
Cu (NO3)2·3H2O、Y(NO3)3·6H2For O respectively in terms of Cu, Y, glycine mole is 2 times of the sum of Cu, Y mole；
S2: 0.2g ethyl orthosilicate and SDS are dispersed in 60ml deionized water according to molar ratio 2:1, and ammonium hydroxide tune is added dropwise
Solution ph is saved to 9, obtains solution B；
S3: above-mentioned solution B is added in solution A, continuously stirs 40min using magnetic stirring apparatus, magnetic stirring apparatus stirs
Mixing speed is 100r/min, collects bottom sediment using centrifuge, and be respectively washed three to sediment with water and dehydrated alcohol
It is secondary；Complexing agent is added in whipping process into the mixed solution of solution A and solution B, the preparation method of complexing agent is by hydroxide
3:2:1 hybrid reaction, reaction solution obtain partially polymerized intermediate by spray drying in molar ratio for sodium, phosphoric acid and methyl acid phosphate
The intermediate powder is put into drying box and carries out polymerization reaction by powder, and complexing agent finished product is obtained after polymerization reaction；Wherein
Dry the temperature inside the box control is at 180 DEG C, polymerization reaction time 8h；
S4: S3 products therefrom is placed in drying box, and dry 6h under the conditions of 80 DEG C can be obtained by grinding device grinding
To compound blue ceramic pigment.
Embodiment 8:
A kind of compound blue ceramic pigment Cu2Y2O5-SiO2Preparation method, mainly comprise the steps that
S1: at room temperature, by 0.2gCu2Y2O5It is dispersed in 90ml deionized water with 1.4gSDS according to molar ratio 1:10,
The dehydrated alcohol of 2 times of volumes is added, 1h is ultrasonically treated, obtains solution A；Wherein, Cu2Y2O5Using 2 gained of preparation example, addition
Cu (NO3)2·3H2O、Y(NO3)3·6H2For O respectively in terms of Cu, Y, glycine mole is 2 times of the sum of Cu, Y mole；
S2: 0.2g ethyl orthosilicate and SDS are dispersed in 60ml deionized water according to molar ratio 2:1, and ammonium hydroxide tune is added dropwise
Solution ph is saved to 9, obtains solution B；
S3: above-mentioned solution B is added in solution A, continuously stirs 40min using magnetic stirring apparatus, magnetic stirring apparatus stirs
Mixing speed is 100r/min, collects bottom sediment using centrifuge, and be respectively washed three to sediment with water and dehydrated alcohol
It is secondary；Complexing agent is added in whipping process into the mixed solution of solution A and solution B, the preparation method of complexing agent is by hydroxide
3:2:1 hybrid reaction, reaction solution obtain partially polymerized intermediate by spray drying in molar ratio for sodium, phosphoric acid and methyl acid phosphate
The intermediate powder is put into drying box and carries out polymerization reaction by powder, and complexing agent finished product is obtained after polymerization reaction；Wherein
Dry the temperature inside the box control is at 200 DEG C, polymerization reaction time 10h；
S4: S3 products therefrom is placed in drying box, and dry 6h under the conditions of 80 DEG C can be obtained by grinding device grinding
To compound blue ceramic pigment；Grinding device includes shell 1, level-one grinding assembly 2, secondary grinder component 3, power supply device；
1 upper end of shell is provided with feed hopper 11,1 lower end of shell is provided with blanking port 12；Level-one grinding assembly 2 includes primary motor, one
Grade mixing roll 21；Two-level grinding device 3 includes secondary grinder stick 31, abrasive disk 32 and Power Component 36, and Power Component 36 includes
Secondary motor, eccentric wheel 361, oscillating rod 362；There are two level-one mixing rolls 21, two 21 horizontal alignment of level-one mixing roll settings
In 1 inner upper end of shell, two 21 surfaces of level-one mixing roll are provided with multiple abrasive grains, two level-one mixing rolls 21 and shell
Material blocking block 22 is provided between body 1, primary motor is that level-one mixing roll 21 provides power, and shell 1 is internally provided with refining plate 23,
Refining plate 23 is located at two 21 lower ends of level-one mixing roll；Abrasive disk 32 is movably arranged on inside shell 1, is located under refining plate 23
It holds, is provided with arc groove 320 on abrasive disk 32, there are two arc grooves 320, is provided through material-dropping hole on abrasive disk 32
321, abrasive disk 32 and shell contact position are provided with reset assembly 33, and there are two secondary grinder sticks 31, two secondary grinder sticks 31
Surface be provided with grinding protrusion, the both ends of two secondary grinder sticks 31 are movably set with connecting rod 34, four connecting rods
34 upper end is movably set with movable plate 35, is connected with tension spring 340 between two connecting rods 34 of the left and right sides, on movable plate 35
It is provided with engaging lug 350, secondary motor is that eccentric wheel 361 provides power, and eccentric wheel 361 and engaging lug 350 pass through oscillating rod 362
Connection, by the rotation of eccentric wheel 361, can drive two secondary grinder sticks 31 to roll on two arc grooves 320 respectively；
Power supply device is primary motor, secondary motor provides power supply.
Embodiment 9:
A kind of compound blue ceramic pigment Cu2Y2O5-SiO2Preparation method, mainly comprise the steps that
S1: at room temperature, by 0.2gCu2Y2O5It is dispersed in 90ml deionized water with 1.4gSDS according to molar ratio 1:10,
The dehydrated alcohol of 2 times of volumes is added, 1h is ultrasonically treated, obtains solution A；Wherein, Cu2Y2O5Using 2 gained of preparation example, addition
Cu (NO3)2·3H2O、Y(NO3)3·6H2For O respectively in terms of Cu, Y, glycine mole is 2 times of the sum of Cu, Y mole；
S2: 0.2g ethyl orthosilicate and SDS are dispersed in 60ml deionized water according to molar ratio 2:1, and ammonium hydroxide tune is added dropwise
Solution ph is saved to 9, obtains solution B；
S3: above-mentioned solution B is added in solution A, continuously stirs 40min using magnetic stirring apparatus, magnetic stirring apparatus stirs
Mixing speed is 100r/min, collects bottom sediment using centrifuge, and be respectively washed three to sediment with water and dehydrated alcohol
It is secondary；Complexing agent is added in whipping process into the mixed solution of solution A and solution B, the preparation method of complexing agent is by hydroxide
3:2:1 hybrid reaction, reaction solution obtain partially polymerized intermediate by spray drying in molar ratio for sodium, phosphoric acid and methyl acid phosphate
The intermediate powder is put into drying box and carries out polymerization reaction by powder, and complexing agent finished product is obtained after polymerization reaction；Wherein
Dry the temperature inside the box control is at 270 DEG C, polymerization reaction time 15h；To the mixed solution of solution A and solution B in whipping process
Middle addition antiwear assistant, the raw material of antiwear assistant include: 3 parts of starch, 7 parts of distilled water, 9 parts of maleic anhydride, over cure by weight
6 parts of sour ammonium, 2 parts of styrene, 3 parts of aluminium chloride, 6 parts of potassium hydroxide, 1 part of bentonite, 9 parts of plant fiber, 2 parts of silane coupling agent；
Antiwear assistant the preparation method comprises the following steps: under nitrogen protection, starch, distilled water and maleic anhydride being uniformly mixed, then heated to
75 DEG C, keep the temperature 1h, then be added ammonium persulfate be uniformly mixed, stir 25min after be added styrene be uniformly mixed, then with
750r/min revolving speed stirs 45min, then heats to 95 DEG C, extracts 30h, then in vacuum drying oven, 60 DEG C dry to constant weight, cold
But material A is obtained to room temperature；Aluminium chloride, potassium hydroxide and water are uniformly mixed, stirred evenly, 8d is stored at room temperature and obtains material B,
Then bentonite and plant fiber are added into material B, is stored at room temperature 7d, and silane coupling agent is added and material A is uniformly mixed, with
2800r/min revolving speed stirs 50min, then heats to 150 DEG C, dry 6h, crushing after being cooled to room temperature can be obtained wear-resisting help
Agent finished product；
S4: S3 products therefrom is placed in drying box, and dry 6h under the conditions of 80 DEG C can be obtained by grinding device grinding
To compound blue ceramic pigment；Grinding device includes shell 1, level-one grinding assembly 2, secondary grinder component 3, power supply device；
1 upper end of shell is provided with feed hopper 11,1 lower end of shell is provided with blanking port 12；Level-one grinding assembly 2 includes primary motor, one
Grade mixing roll 21；Two-level grinding device 3 includes secondary grinder stick 31, abrasive disk 32 and Power Component 36, and Power Component 36 includes
Secondary motor, eccentric wheel 361, oscillating rod 362；There are two level-one mixing rolls 21, two 21 horizontal alignment of level-one mixing roll settings
In 1 inner upper end of shell, two 21 surfaces of level-one mixing roll are provided with multiple abrasive grains, two level-one mixing rolls 21 and shell
Material blocking block 22 is provided between body 1, primary motor is that level-one mixing roll 21 provides power, and shell 1 is internally provided with refining plate 23,
Refining plate 23 is located at two 21 lower ends of level-one mixing roll；Abrasive disk 32 is movably arranged on inside shell 1, is located under refining plate 23
It holds, is provided with arc groove 320 on abrasive disk 32, there are two arc grooves 320, is provided through material-dropping hole on abrasive disk 32
321, abrasive disk 32 and shell contact position are provided with reset assembly 33, and there are two secondary grinder sticks 31, two secondary grinder sticks 31
Surface be provided with grinding protrusion, the both ends of two secondary grinder sticks 31 are movably set with connecting rod 34, four connecting rods
34 upper end is movably set with movable plate 35, is connected with tension spring 340 between two connecting rods 34 of the left and right sides, on movable plate 35
It is provided with engaging lug 350, secondary motor is that eccentric wheel 361 provides power, and eccentric wheel 361 and engaging lug 350 pass through oscillating rod 362
Connection, by the rotation of eccentric wheel 361, can drive two secondary grinder sticks 31 to roll on two arc grooves 320 respectively；
Power supply device is primary motor, secondary motor provides power supply.
XRD test
The lower Cu synthesized is calcined to different temperatures2Y2O5XRD analysis is carried out, as shown in Figure 1, it is known that: 700 DEG C have miscellaneous peak,
750 DEG C, 800 DEG C and 900 DEG C of diffraction maximum and standard diagram corresponds, and illustrates to have synthesized Cu2Y2O5, excellent based on comprehensively considering
Selecting calcination temperature is 750 DEG C.
Under the same terms, the influence of preferred substrate and dispersive agent ratio to product, as shown in Fig. 2, both comparisons characteristic peak,
Using Scherrer formula D=0.89 λ/β cos θ obtain target product average grain diameter be respectively 72.75nm (1:5), 54.54nm (1:
10).It follows that: it is more excellent process conditions that the ratio of matrix and SDS, which are 1: 10,.
Under the same terms, preferred substrate and influence of the ethyl orthosilicate molar ratio to product, as shown in figure 3, matrix with just
The XRD diagram of two ratios of silester is pure phase, but ratio is high for the peak value of 1: 1 characteristic peak, according to Scherrer formula meter
Calculating average grain diameter is respectively 72.76nm (1:1), 54.57nm (1:2).So the ratio of matrix and ethyl orthosilicate be 1: 2 be compared with
Excellent result.
Under the same terms, influence of the preferred dispersants type to product obtains mesh with Scherrer formula D=0.89 λ/β cos θ
Product average grain diameter is marked, surfactant is the average grain diameter D=54.57nm of SDBS, and surfactant is the average grain diameter of SDS
D=48.48nm illustrates that the cladding product prepared using SDS is better than SDBS.SEM test
Micro-structural test is carried out to product by scanning electron microscope, from fig. 5, it can be seen that 20000 under 750 DEG C of calcination temperatures
With the Cu of 50000 amplification factors2Y2O5With preferable dispersibility, particle size distribution is uniform, and pattern is in near-spherical.Fig. 6 can be with
Find out, obviously more evenly, shape is closer spherical for size than before for the particle after coating.As seen from Figure 7, expand simultaneously
In 50000 times of SEM figure, it is 1: 5 that the grain diameter of ratio 1: 10, which is significantly less than ratio, thus conclude that matrix with
The ratio of surfactant has biggish specific surface area for 1: 10, is more excellent result.From figure 8, it is seen that ratio is 1: 2
It is 1: 1 that grain diameter, which is slightly less than ratio, and ratio 1: 2 has more small size particles, and specific surface area is bigger, it was demonstrated that matrix
It is preferable for the effect of 1: 2 cladding with ethyl orthosilicate ratio, it is a more excellent condition.From fig. 9, it can be seen that the crystal grain ruler of the two
Very little size is not much different, but the granular size of SDS is more uniform, and surface does not have kick, more smooth compared to SDBS, institute
It is preferably condition using SDS as surfactant.
Coloration test
(Cu resulting to experiment2Y2O5) blue ceramic pigment progress coloration test, as a result it see the table below.
Cu2Y2O5Color coordinates schematic diagram
As seen from table, Cu2Y2O5Matrix when increasing to 900 DEG C by 700 DEG C with temperature, L value is gradually increased, gradually by
33.02, which increase to 42.88, L, indicates light and shade (brightness), and chromatic value is gradually increased, and illustrates that product is brighter.With the increase of temperature,
The value of a is smaller and smaller, indicates that sample is greener；B value is smaller and smaller, illustrates that matrix is more and more blue.Wherein, L* is brightness, and L* is bigger
Indicate that product colour is brighter；A* is red green changing value, and a* is bigger, and expression product colour is redder；B* is champac changing value, and b* is bigger
Indicate that product colour is more yellow.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify to technical solution documented by previous embodiment or equivalent replacement of some of the technical features；And
These are modified or replaceed, the spirit and model of technical solution of the embodiment of the present invention that it does not separate the essence of the corresponding technical solution
It encloses.
Claims (10)
1. a kind of compound blue ceramic pigment Cu2Y2O5-SiO2Preparation method, which is characterized in that mainly comprise the steps that
S1: at room temperature, by Cu2Y2O5Disperse in deionized water, to add 2-3 times of body according to molar ratio 1:10 with dispersing agent
Long-pending dehydrated alcohol is ultrasonically treated 1-3h, obtains solution A；
S2: ethyl orthosilicate and dispersing agent are dispersed in deionized water, ammonium hydroxide to be added dropwise and adjusts solution ph according to molar ratio 2:1
To 6-9, solution B is obtained；
S3: above-mentioned solution B being added in solution A, continuously stirs 20-60min using magnetic stirring apparatus, collects bottom using centrifuge
Portion's sediment, and sediment is cleaned with water and dehydrated alcohol；
S4: S3 products therefrom is placed in drying box, and dry 5-8h, grinds by grinding device under the conditions of 70-90 DEG C
Obtain compound blue ceramic pigment.
2. a kind of compound blue ceramic pigment Cu according to claim 12Y2O5-SiO2Preparation method, feature exists
In Cu described in step S12Y2O5It is made by following steps:
1) by Cu (NO3)2·3H2O、Y(NO3)3·6H2O is added in the aqueous solution of glycine, first stirred at 50-70 DEG C to
Clarification；
2) 1) acquired solution in is heated to 100-120 DEG C, stirs 90-110min, self- propagating combustion occurs for solution in the process
It burns reaction and generates loose powder；
3) 2) gained powder is calcined under the conditions of 700-900 DEG C up to Cu2Y2O5Finished product.
3. a kind of compound blue ceramic pigment Cu according to claim 22Y2O5-SiO2Preparation method, feature exists
In the calcination temperature of powder described in step 3) is 750-850 DEG C.
4. a kind of compound blue ceramic pigment Cu according to claim 32Y2O5-SiO2Preparation method, feature exists
In the calcination temperature of powder described in step 3) is 750 DEG C.
5. a kind of compound blue ceramic pigment Cu according to claim 22Y2O5-SiO2Preparation method, feature exists
In the Cu (NO of addition3)2·3H2O、Y(NO3)3·6H2For O respectively in terms of Cu, Y, glycine mole is the sum of Cu, Y mole
2 times.
6. a kind of compound blue ceramic pigment Cu according to claim 12Y2O5-SiO2Preparation method, feature exists
In, in step S1, any one in dispersing agent PVP, SDS, SDBS.
7. a kind of compound blue ceramic pigment Cu according to claim 12Y2O5-SiO2Preparation method, feature exists
In in step S3, the mixing speed of the magnetic stirring apparatus is 80-100r/min.
8. a kind of compound blue ceramic pigment Cu according to claim 12Y2O5-SiO2Preparation method, feature exists
In complexing agent, the preparation side of the complexing agent is added in whipping process into the mixed solution of solution A and solution B in step S3
Method is that 3:2:1 hybrid reaction, reaction solution obtain part by spray drying in molar ratio by sodium hydroxide, phosphoric acid and methyl acid phosphate
The intermediate powder is put into drying box and carries out polymerization reaction by the intermediate powder of polymerization, obtains network after polymerization reaction
Mixture finished product；The temperature inside the box control is wherein dried at 180-270 DEG C, polymerization reaction time 8-15h.
9. a kind of compound blue ceramic pigment Cu according to claim 12Y2O5-SiO2Preparation method, feature exists
In complexing agent, the preparation side of the complexing agent is added in whipping process into the mixed solution of solution A and solution B in step S3
Method is that 2:1:3 hybrid reaction, reaction solution obtain part by spray drying in molar ratio by phosphoric acid hydrogen, methyl acid phosphate and sodium oxide molybdena
The intermediate powder is put into drying box and carries out polymerization reaction by the intermediate powder of polymerization, obtains network after polymerization reaction
Mixture finished product；The temperature inside the box control is wherein dried at 180-270 DEG C, polymerization reaction time 8-15h.
10. a kind of compound blue ceramic pigment Cu according to claim 12Y2O5-SiO2Preparation method, feature exists
In in step S4, the grinding device includes shell (1), level-one grinding assembly (2), secondary grinder component (3), power supply device；
Shell (1) upper end is provided with feed hopper (11), shell (1) lower end is provided with blanking port (12)；The level-one grinding assembly
It (2) include primary motor, level-one mixing roll (21)；The two-level grinding device (3) includes secondary grinder stick (31), abrasive disk
(32) and Power Component (36), the Power Component (36) include secondary motor, eccentric wheel (361), oscillating rod (362)；It is described
There are two level-one mixing rolls (21), and two level-one mixing roll (21) horizontal alignments are arranged in shell (1) inner upper end, two level-ones
Mixing roll (21) surface is provided with multiple abrasive grains, is provided with backgauge between two level-one mixing rolls (21) and shell (1)
Block (22), the primary motor are that level-one mixing roll (21) provide power, and shell (1) is internally provided with refining plate (23), described
Refining plate (23) is located at two level-one mixing roll (21) lower ends；The abrasive disk (32) is movably arranged on shell (1) inside, is located at
Refining plate (23) lower end is provided with arc groove (320) on abrasive disk (32), and there are two the arc grooves (320), abrasive disk
(32) it is provided through on material-dropping hole (321), abrasive disk (32) and shell contact position are provided with reset assembly (33), the second level
There are two grinding rods (31), and the surface of two secondary grinder sticks (31) is provided with grinding protrusion, two secondary grinder sticks (31)
Both ends be movably set with connecting rod (34), the upper end of four connecting rods (34) is movably set with movable plate (35), left
It is connected with tension spring (340) between two connecting rods (34) of right two sides, is provided with engaging lug (350) on the movable plate (35),
The secondary motor is that the eccentric wheel (361) provide power, and eccentric wheel (361) and engaging lug (350) pass through the oscillating rod
(362) it connects, by the rotation of eccentric wheel (361), two secondary grinder sticks (31) can be driven respectively in two arc grooves
(320) it is rolled on；The power supply device is primary motor, secondary motor provides power supply.
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| Application Number | Priority Date | Filing Date | Title |
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| Application Number | Priority Date | Filing Date | Title |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105175012A (en) * | 2015-08-21 | 2015-12-23 | 华北水利水电大学 | Spinel type composite ultrafine blue ceramic pigment and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105175012A (en) * | 2015-08-21 | 2015-12-23 | 华北水利水电大学 | Spinel type composite ultrafine blue ceramic pigment and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| RACU, AV等: ""Rapid combustion synthesis of Cu2Y2O5 as a precursor for CuYO2 delafossite"", 《MATERIALS TODAY COMMUNICATIONS》 * |
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