CN104108952A - Method for preparing black ceramic pigment by using leather making sludge and product - Google Patents
Method for preparing black ceramic pigment by using leather making sludge and product Download PDFInfo
- Publication number
- CN104108952A CN104108952A CN201410312646.3A CN201410312646A CN104108952A CN 104108952 A CN104108952 A CN 104108952A CN 201410312646 A CN201410312646 A CN 201410312646A CN 104108952 A CN104108952 A CN 104108952A
- Authority
- CN
- China
- Prior art keywords
- oxide
- leather
- making mud
- colorant
- black
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Glass Compositions (AREA)
- Compositions Of Oxide Ceramics (AREA)
Abstract
The invention relates to a method for preparing black ceramic pigment by using leather making sludge and a product, which belongs to the technical field of preparation of pigment. According to the invention, the leather making sludge is washed and dried and then totally replaces chrome oxide as a raw material, and black ceramic pigment which can be used both for a base and a glaze and has obviously improved blackness can be prepared; thus, preparation procedures are simplified, a production period is shortened, and production cost is further reduced. According to the method, the leather making sludge is subjected to the pretreatment operation of calcining in a non-oxidizing atmosphere, ball milling, washing and drying and then used as a raw material; the prepared black ceramic pigment has increased usage temperature, an improved dyeing property and reduced application amount, and dissolving-out of a great amount of Cr6+ in the process of washing and usage does not exist.
Description
Technical field
The present invention relates to a kind of method and product that utilizes leather-making mud to prepare black ceramic colorant, belong to colorant preparing technical field.
Background technology
Black ceramic colorant is a kind of colorant very important in finishing material, and black glaze is with the extremely people's favor of its pure, dignified decorative effect.What generally prepare black pigment employing is coloring of crystal: the metal oxides such as chromium, iron, manganese, nickel, copper, cobalt form isomorphous mixed type spinel crystal.The oxidated cobalt price of black ceramic colorant price and remaining high, has to a certain degree limited production in enormous quantities and the application of black pigment.At present existing research and utilization chromium residue is prepared the method for black ceramic colorant base for: the industrial residue chromium mud at 950-1050 ℃ after calcining, ferric oxide and chromic oxide mixing, 1180-1250 ℃ calcine 1 hour, pulverize to obtain product.But the method, chromic oxide is not replaced by industrial residue chromium mud completely, and its cost is still higher, and blackness is lower.
Summary of the invention
A goal of the invention of the present invention is: provide a kind of and can further reduce production costs, product can base with also can glaze with and the method for preparing black ceramic colorant of quality better.
Another goal of the invention of object of the present invention is: provide a kind of aforesaid method prepared black ceramic colorant.
Leather-making mud is the solid waste obtaining after chrome tanned leather waste water alkaline chemical precipitation, is wherein rich in chromium; A kind of industrial residue chromium mud.In order further to reduce production costs, first contriver expects replacing chromic oxide as raw material completely with leather-making mud.But experiment is found, with leather-making mud, replace chromic oxide as raw material completely, adopt existing method lignin-sludge, utilize it to prepare black ceramic colorant and have following problem: blackness is lower, color is impure, unstable properties under hot conditions, tinctorial property is poor and washing use procedure in there is the problem of a large amount of Cr6+ strippings.
Contriver tests discovery after deliberation: after leather-making mud washing is dry, replace chromic oxide directly to use as raw material completely, can prepare can base with also can glaze with and the black ceramic colorant that obviously improves of blackness; So, simplify preparation section, shortened the production cycle, further reduced production cost.But there is unstable properties under hot conditions in this black ceramic colorant, tinctorial property is poor and wash the problem that has Cr6+ stripping in use procedure.And leather-making mud is used through be re-used as raw material after " calcining; then ball milling, washing, dry " this pretreatment operation under nonoxidizing atmosphere, prepared black ceramic colorant, its use temperature improves, tinctorial property improves, consumption reduces, and colorant can not exist a large amount of Cr6+ strippings in washing and use procedure.
The technical scheme that the present invention takes is:
Utilize leather-making mud to prepare a method for black ceramic colorant, raw material is through pulverizing, calcine to obtain product; Its improvements are: with the dried leather-making mud of washing, replace chromic oxide as raw material,
Or replace chromic oxide as raw material after leather-making mud pre-treatment; Described pre-treatment: calcine under nonoxidizing atmosphere, then ball milling, washing, dry.
Experimental studies have found that: the variation of leather-making mud pretreatment condition, has a significant effect to the colourimetric number of black ceramic colorant, pulverizing complexity.
After leather-making mud is processed under nonoxidizing atmosphere below 1050 ℃, gained calcined material is easily pulverized; But, using this calcined material to use as raw material, prepared black ceramic raw material, its blackness is lower, black is impure, partially red.
After leather-making mud is processed under more than 1300 ℃ nonoxidizing atmosphere, gained calcined material is difficult to pulverize; Usining this calcined material uses as raw material, prepared black ceramic raw material, and its blackness is low, black is impure, partially reddish-brown.
After leather-making mud is processed under 1100-1300 ℃ of nonoxidizing atmosphere, gained calcined material is easily pulverized; Usining this calcined material uses as raw material, prepared black ceramic raw material, and its blackness is high, black is pure.
So, aforesaid method, preferred, described pre-treatment: preferably process 30 ~ 180min under 1100-1300 ℃ of nonoxidizing atmosphere.Aforesaid method, highly preferred pre-treatment is: process 60min for 1250 ℃.
In aforesaid method, the pulverizing of raw material, calcining adopt conventional processing means, and the present invention adopts: pulverized 300 orders, calcining temperature is 900-1300 ℃, and calcination time is 30-180min.
Aforesaid method, raw materials usedly also comprises metal oxide that determine according to black ceramic colorant crystal system to be prepared, beyond chromic oxide; The consumption of described leather-making mud is 10 ~ 60%.
Prepare the needed raw material of different crystal system black ceramic colorant different, at present, without cobalt black look ceramic pigment crystal system, comprise: Cr-Fe system, Ni-Cr-Fe system, Ni-Cr-Fe-Cu system, Ni-Cr-Fe-Mn system, the systems such as Ni-Cr-Fe-Mn-Cu.So, those skilled in the art can according to the crystal system of black ceramic colorant to be prepared determine select which kind of or which plant metal oxide and consumption thereof.So, aforesaid method, described metal oxide is one or more in nickel sesquioxide, cupric oxide, Manganse Dioxide, manganic oxide, manganous carbonate, ferrous sulfate, nickel protoxide and rare earth oxide.
Aforesaid method, described raw material is preferably:
25-70% leather-making mud, 30-75% ferric oxide;
Or, 30-50% leather-making mud, 20-50% ferric oxide, 10-30% nickel sesquioxide;
Or, 45-55% leather-making mud, 20% ferric oxide, 15-20% nickel sesquioxide, 10-15% cupric oxide;
Or, 30-60% leather-making mud, 20-40% ferric oxide, 5-25% nickel sesquioxide, 5-20% manganic oxide;
Or, 30-50% leather-making mud, 15-44% ferric oxide, 15-30% nickel sesquioxide, 1-10% manganic oxide, 10-30% cupric oxide.Better according to the quality of the prepared black ceramic colorant of this usage ratio.
Aforesaid method is different to the improvement degree of the black ceramic colorant quality of different crystal system; Wherein, maximum to the improvement degree of the mixed type spinel crystal black ceramic toner performance of Ni-Cr-Fe-Cu crystal system, the Ni-Cr-Fe-Cu crystal system black ceramic toner performance obtaining is best; Its raw material is: leather-making mud 45-55%, ferric oxide 20%, cupric oxide 10-15%, 15-20% nickel sesquioxide.Optimal proportion is: leather-making mud 50%, ferric oxide 20%, cupric oxide 15%, 15% nickel sesquioxide.
Raw material is different, calcining temperature, soaking time difference; Those skilled in the art can be according to selected raw material and consumption, corresponding calcining temperature and the time of adjusting while preparing black ceramic colorant.
A black ceramic colorant, adopts above-mentioned any one method to be prepared from.
Beneficial effect
Adopt this patent lignin-sludge curing chromic oxide of can purifying to greatest extent, meanwhile, avoid, after colorant calcining, washing
The stripping of a large amount of Cr6+ ions in journey, contaminate environment is wasted again chromium material;
With leather-making mud, replace chromic oxide completely, further reduce costs;
Simplify preparation section, thereby shorten the production cycle;
Prepared black ceramic colorant, blackness is high, colour purity just, good stability, can base with also can using by glaze.
Accompanying drawing explanation
Fig. 1 is the XRD figure of embodiment 2 colorant products;
Fig. 2 is the sample pictures of embodiment 2;
Fig. 3 is the XRD figure of embodiment 2,3,4 colorant products.
Embodiment
According to the mode of table 1, prepare raw material A 1-A6:
A1 | Wash dried leather-making mud |
A2 | After leather-making mud pulverizing is dry, under 1250 ℃ of nonoxidizing atmospheres, temperature calcining 60min obtains calcined material, and this calcined material is powdery; By calcinate ball milling, washing, dry; |
A3 | After leather-making mud pulverizing is dry, under 1100 ℃ of nonoxidizing atmospheres, temperature calcining 60min obtains calcined material, and this calcined material is powdery; By calcinate ball milling, washing, dry; |
A4 | After leather-making mud pulverizing is dry, under 1300 ℃ of nonoxidizing atmospheres, temperature calcining 60min obtains calcined material, and this calcined material is powdery; By calcinate ball milling, washing, dry; |
A5 | After leather-making mud pulverizing is dry, under 1000 ℃ of nonoxidizing atmospheres, temperature calcining 60min obtains calcined material, and this calcined material is powdery; By calcinate ball milling, washing, dry; |
A6 | After leather-making mud pulverizing is dry, under 1350 ℃ of nonoxidizing atmospheres, temperature calcining 60min obtains calcined material, and this calcined material is powdery; By calcinate ball milling, washing, dry; |
A7 | Leather-making mud is pulverized, is dried, then at 1050 ℃ of conventional calcining 60min |
embodiment 1
By mass percentage by 50% A1,20% ferric oxide, 15% cupric oxide, 15% nickel sesquioxide through wet ball grinding mix, cross 300 mesh sieves, dry after, high-temperature calcination, calcining temperature is 1220 ℃, is incubated 30 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment.The black ceramic colorant colourimetric number data determination result of preparation is as follows: L
*=29.42 a
*=1.78 b
*=1.31; Colorant has a large amount of hexavalent chromium strippings in washing process, far away higher than national standard;
Adding 8% above-mentioned black pigment is in frit in commercial barium, adds 1% carboxymethyl cellulose, through wet-milling, crosses 300 mesh sieves, obtains ceramic glaze.This glaze is imposed on ceramic model, and through 1200 ℃ of high-temperature calcinations, insulation 30min, obtains the partially red glaze layer of black.Glaze produces the defects such as bubble, pinprick.
embodiment 2
By mass percentage by 50% A2,20% ferric oxide, 15% cupric oxide, 15% nickel sesquioxide through wet ball grinding mix, cross 300 mesh sieves, dry after, high-temperature calcination, calcining temperature is 1220 ℃, is incubated 30 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment.The black ceramic colorant colourimetric number data determination result of preparation is as follows: L
*=23.96 a
*=0.72 b
*=0.68; Colorant has a small amount of hexavalent chromium stripping in washing process, lower than national standard;
From Fig. 1, can go out, the black pigment of embodiment 2 preparations is by NiFe
2o
4, Cr
2niO
4, NiCrFeO
4, CuCr
2o
4deng mixing spinel type crystalline phase, form, this black pigment belongs to isomorphous mixed type spinel colorant.As can be seen from Figure 2, the black ceramic colorant product that adopts this example to prepare, blackness is high, and color is pure;
Adding 6% above-mentioned black pigment is in frit in commercial barium, adds 1% carboxymethyl cellulose, through wet-milling, crosses 300 mesh sieves, obtains ceramic glaze.This glaze is imposed on ceramic model, and through 1250 ℃ of high-temperature calcinations, insulation 30min, obtains the pure glaze layer of black.Glaze is without bubble, pinprick, cracking phenomena.
embodiment 3
By mass percentage by 50% A3,20% ferric oxide, 15% cupric oxide, 15% nickel sesquioxide through wet ball grinding mix, cross 300 mesh sieves, dry after, high-temperature calcination, calcining temperature is 1220 ℃, is incubated 30 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment.The black ceramic colorant colourimetric number data determination result of preparation is as follows: L
*=25.76 a
*=1.21 b
*=1.27; Colorant has a small amount of hexavalent chromium stripping in washing process, lower than national standard;
Adding 6% above-mentioned black pigment is in frit in commercial barium, adds 1% carboxymethyl cellulose, through wet-milling, crosses 300 mesh sieves, obtains ceramic glaze.This glaze is imposed on ceramic model, and through 1250 ℃ of high-temperature calcinations, insulation 30min, obtains the pure glaze layer of black.Glaze is without bubble, pinprick, cracking phenomena.
embodiment 4
By mass percentage by 50% A4,20% ferric oxide, 15% cupric oxide, 15% nickel sesquioxide through wet ball grinding mix, cross 300 mesh sieves, dry after, high-temperature calcination, calcining temperature is 1220 ℃, is incubated 30 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment.The black ceramic colorant colourimetric number data determination result of preparation is as follows: L
*=25.83 a
*=1.28 b
*=1.25; Colorant has a small amount of hexavalent chromium stripping in washing process, lower than national standard;
Adding 6% above-mentioned black pigment is in frit in commercial barium, adds 1% carboxymethyl cellulose, through wet-milling, crosses 300 mesh sieves, obtains ceramic glaze.This glaze is imposed on ceramic model, and through 1250 ℃ of high-temperature calcinations, insulation 30min, obtains the pure glaze layer of black.Glaze is without bubble, pinprick, cracking phenomena.
embodiment 5
By mass percentage by 50% A5,20% ferric oxide, 15% cupric oxide, 15% nickel sesquioxide through wet ball grinding mix, cross 300 mesh sieves, dry after, high-temperature calcination, calcining temperature is 1220 ℃, is incubated 30 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment.The black ceramic colorant colourimetric number data determination result of preparation is as follows: L
*=28.31 a
*=1.44 b
*=1.69; Colorant has a small amount of hexavalent chromium stripping in washing process, lower than national standard;
Adding 8% above-mentioned black pigment is in frit in commercial barium, adds 1% carboxymethyl cellulose, through wet-milling, crosses 300 mesh sieves, obtains ceramic glaze.This glaze is imposed on ceramic model, and through 1250 ℃ of high-temperature calcinations, insulation 30min, obtains the slightly reddish brown glaze layer of black.Illustrate that its blackness of this colorant is low, black is impure, partially reddish-brown look.
embodiment 6
By mass percentage by 50% A6,20% ferric oxide, 15% cupric oxide, 15% nickel sesquioxide through wet ball grinding mix, cross 300 mesh sieves, dry after, high-temperature calcination, calcining temperature is 1220 ℃, is incubated 30 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment.The black ceramic colorant colourimetric number data determination result of preparation is as follows: L
*=27.68 a
*=1.65 b
*=1.89; Colorant has a small amount of hexavalent chromium stripping in washing process, lower than national standard;
Adding 6% above-mentioned black pigment is in frit in commercial barium, adds 1% carboxymethyl cellulose, through wet-milling, crosses 300 mesh sieves, obtains ceramic glaze.This glaze is imposed on ceramic model, and through 1250 ℃ of high-temperature calcinations, insulation 30min, obtains the slightly reddish brown glaze layer of black, illustrates that its blackness of this colorant is low, black is impure, partially red.
embodiment 7
By mass percentage by 50% A7,20% ferric oxide, 15% cupric oxide, 15% nickel sesquioxide through wet ball grinding mix, cross 300 mesh sieves, dry after, high-temperature calcination, calcining temperature is 1220 ℃, is incubated 30 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment.The black ceramic colorant colourimetric number data determination result of preparation is as follows: L
*=28.72 a
*=1.68 b
*=1.65; Colorant has a large amount of hexavalent chromium strippings in washing process;
Adding 8% above-mentioned black pigment is in frit in commercial barium, adds 1% carboxymethyl cellulose, through wet-milling, crosses 300 mesh sieves, obtains ceramic glaze.This glaze is imposed on ceramic model, and through 1230 ℃ of high-temperature calcinations, insulation 30min, obtains the slightly reddish brown glaze layer of black, illustrates that its blackness of this colorant is low, black is impure, partially red, and the defects such as bubble, pinprick appear in glaze.
embodiment 8
By mass percentage by 45% A2,20% ferric oxide, 15% cupric oxide, 20% nickel sesquioxide through wet ball grinding mix, cross 300 mesh sieves, dry after, high-temperature calcination, calcining temperature is 1200 ℃, is incubated 30 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment.The black ceramic colorant colourimetric number data determination result of preparation is as follows: L
*=24.57 a
*=1.11 b
*=1.09.
embodiment 9
By mass percentage by 55% A2,20% ferric oxide, 10% cupric oxide, 15% nickel sesquioxide through wet ball grinding mix, cross 300 mesh sieves, dry after, high-temperature calcination, calcining temperature is 1250 ℃, is incubated 30 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment.The black ceramic colorant colourimetric number data determination result of preparation is as follows: L
*=24.12 a
*=1.08 b
*=1.05.
embodiment 10
By mass percentage by 40-50%A2 and 50-60% ferric oxide; After wet ball grinding mixes, sieves, is dried, high-temperature calcination, calcining temperature is 1200 ℃, is incubated 60 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment; Its colourimetric number data determination result is as follows: L
*=24.57-25.1 a
*=1.75-1.81 b
*=1.74-1.89;
By mass percentage by 40-50%A6 and 50-60% ferric oxide; After wet ball grinding mixes, sieves, is dried, high-temperature calcination, calcining temperature is 1200 ℃, is incubated 60 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment; Its colourimetric number data determination result is as follows: L
*=30.13-31.27 a
*=1.69-1.75 b
*=1.66-1.73.
embodiment 11
By mass percentage by 30-50%A2,30-40% ferric oxide and 10-30% nickel sesquioxide; After wet ball grinding mixes, sieves, is dried, high-temperature calcination, calcining temperature is 1220 ℃, is incubated 60 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment; Its colourimetric number data determination result is as follows: L
*=21.6-22.89 a
*=0.46-1.13 b
*=1.12-2.71;
By mass percentage by 30-50%A6,30-40% ferric oxide and 10-30% nickel sesquioxide; After wet ball grinding mixes, sieves, is dried, high-temperature calcination, calcining temperature is 1220 ℃, is incubated 60 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment; Its colourimetric number data determination result is as follows: L
*=24.18-25.69 a
*=1.83-2.56 b
*=0.56-1.89.
embodiment 12
By mass percentage by 30-60%A2,20-40% ferric oxide, 5-25% nickel sesquioxide and 5-20% manganic oxide; After wet ball grinding mixes, sieves, is dried, high-temperature calcination, calcining temperature is 1250 ℃, is incubated 60 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment; Its colourimetric number data determination result is as follows: L
*=21.87-21.96 a
*=1.65-1.84 b
*=1.81-1.92;
By mass percentage by 30-60%A6,20-40% ferric oxide, 5-25% nickel sesquioxide, 5-20% manganic oxide; After wet ball grinding mixes, sieves, is dried, high-temperature calcination, calcining temperature is 1250 ℃, is incubated 60 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment; Its colourimetric number data determination result is as follows: L
*=23.83-24.96 a
*=2.87-2.99 b
*=1.06-1.37.
embodiment 13
By mass percentage by 30-50%A2,15-50% ferric oxide, 15-30% nickel sesquioxide, 1-10% manganic oxide, 10-30% cupric oxide; After wet ball grinding mixes, sieves, is dried, high-temperature calcination, calcining temperature is 1250 ℃, is incubated 60 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment; Its colourimetric number data determination result is as follows: L
*=24.49-25.13 a
*=1.42-1.57 b
*=1.97-2.31;
By mass percentage by 30-50%A6,15-44% ferric oxide, 15-30% nickel sesquioxide, 1-10% manganic oxide, 10-30% cupric oxide; After wet ball grinding mixes, sieves, is dried, high-temperature calcination, calcining temperature is 1230 ℃, is incubated 60 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment; Its colourimetric number data determination result is as follows: L
*=26.79-27.65 a
*=1.60-1.98 b
*=1.28-1.75.
comparative example
By mass percentage by 50% the leather-making mud without washing, 20% ferric oxide, 15% cupric oxide, 15% nickel sesquioxide through wet ball grinding mix, cross 300 mesh sieves, dry after, high-temperature calcination, calcining temperature is 1220 ℃, is incubated 30 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment.The black ceramic colorant colourimetric number data determination result of preparation is as follows: L
*=32.35 a
*=1.95 b
*=1.73; Colorant has a large amount of hexavalent chromium strippings in washing process.
comparative example 2
After leather-making mud pulverizing is dry, under 1250 ℃ of nonoxidizing atmospheres, temperature calcining 60min obtains calcined material; By mass percentage by 50% calcined material, 20% ferric oxide, 15% cupric oxide, 15% nickel sesquioxide through wet ball grinding mix, cross 300 mesh sieves, dry after, high-temperature calcination, calcining temperature is 1220 ℃, is incubated 30 minutes; Again by the first coarse crushing of the colorant after calcining, then in small, broken bits, the washing of ball milling, dry after, obtain without cobalt black look ceramic pigment.The black ceramic colorant colourimetric number data determination result of preparation is as follows: L
*=29.42 a
*=0.94 b
*=1.03; Colorant has a small amount of hexavalent chromium stripping in washing process, lower than national standard.
Claims (9)
1. utilize leather-making mud to prepare a method for black ceramic colorant, raw material is through pulverizing, calcine to obtain product; It is characterized in that: with the dried leather-making mud of washing, replace chromic oxide as raw material,
Or replace chromic oxide as raw material after leather-making mud pre-treatment; Described pre-treatment: calcine then ball milling washing, dry under nonoxidizing atmosphere.
2. according to power, require the method described in 1, it is characterized in that, under nonoxidizing atmosphere, calcining temperature is 1060-1300 ℃, and the time is 30-180min.
3. according to power, require the method described in 2, it is characterized in that, process 60min for 1250 ℃.
4. according to power, require the method described in 1, it is characterized in that, raw material pulverizing is crossed 300 orders, and calcining temperature is 900-1300 ℃, and calcination time is 30-180min.
5. according to power, require the method described in 1, it is characterized in that, raw materials usedly also comprise metal oxide that determine according to black ceramic colorant crystal system to be prepared, beyond chromic oxide; The consumption of described leather-making mud is 10 ~ 60%.
6. according to power, require the method described in 1, it is characterized in that, described metal oxide is one or more in nickel sesquioxide, cupric oxide, Manganse Dioxide, manganic oxide, manganous carbonate, ferrous sulfate, nickel protoxide and rare earth oxide.
7. according to power, require the method described in 1, it is characterized in that, described raw material is:
25-70% leather-making mud, 30-75% ferric oxide;
Or, 30-50% leather-making mud, 20-50% ferric oxide, 10-30% nickel sesquioxide;
Or, 45-55% leather-making mud, 20% ferric oxide, 15-20% nickel sesquioxide, 10-15% cupric oxide;
Or, 30-60% leather-making mud, 20-40% ferric oxide, 5-25% nickel sesquioxide, 5-20% manganic oxide;
Or, 30-50% leather-making mud, 15-44% ferric oxide, 15-30% nickel sesquioxide, 1-10% manganic oxide, 10-30% cupric oxide.
8. according to power, require the method described in 7, it is characterized in that, leather-making mud 50%, ferric oxide 20%, cupric oxide 15%, 15% nickel sesquioxide.
9. one kind adopts the black ceramic colorant that in claim 1-8 prepared by the method described in any one.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201410312646.3A CN104108952A (en) | 2014-07-03 | 2014-07-03 | Method for preparing black ceramic pigment by using leather making sludge and product |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201410312646.3A CN104108952A (en) | 2014-07-03 | 2014-07-03 | Method for preparing black ceramic pigment by using leather making sludge and product |
Publications (1)
Publication Number | Publication Date |
---|---|
CN104108952A true CN104108952A (en) | 2014-10-22 |
Family
ID=51705965
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201410312646.3A Pending CN104108952A (en) | 2014-07-03 | 2014-07-03 | Method for preparing black ceramic pigment by using leather making sludge and product |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN104108952A (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106045321A (en) * | 2016-06-01 | 2016-10-26 | 佛山市高明区海帝陶瓷原料有限公司 | Method for preparing black glaze pigment with nickel-containing waste materials and black glaze pigment |
CN109231959A (en) * | 2018-08-15 | 2019-01-18 | 陕西科技大学 | A kind of preparation method using leather sludge production exterior wall tile |
CN111662570A (en) * | 2020-05-25 | 2020-09-15 | 武汉科技大学 | Mixed spinel type black ceramic pigment and preparation method thereof |
CN111662571A (en) * | 2017-12-12 | 2020-09-15 | 佛山市大千色釉料有限公司 | Preparation method of ceramic pigment |
CN113999044A (en) * | 2021-11-12 | 2022-02-01 | 郑州磨料磨具磨削研究所有限公司 | Porous ceramic plate and preparation method thereof |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102992808A (en) * | 2012-12-14 | 2013-03-27 | 赞皇县高砂陶瓷材料有限公司 | Method for preparing black ceramic pigment for blank by use of chromium-containing waste residue and product prepared by same |
-
2014
- 2014-07-03 CN CN201410312646.3A patent/CN104108952A/en active Pending
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102992808A (en) * | 2012-12-14 | 2013-03-27 | 赞皇县高砂陶瓷材料有限公司 | Method for preparing black ceramic pigment for blank by use of chromium-containing waste residue and product prepared by same |
Non-Patent Citations (2)
Title |
---|
叶昌等: "利用铬盐废渣生产陶瓷色料的研究", 《中国陶瓷》, vol. 41, no. 4, 31 August 2005 (2005-08-31), pages 33 - 36 * |
韩松等: "制革污泥的处理方法与资源化", 《上海电力学院学报》, vol. 28, no. 2, 30 April 2012 (2012-04-30) * |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106045321A (en) * | 2016-06-01 | 2016-10-26 | 佛山市高明区海帝陶瓷原料有限公司 | Method for preparing black glaze pigment with nickel-containing waste materials and black glaze pigment |
CN111662571A (en) * | 2017-12-12 | 2020-09-15 | 佛山市大千色釉料有限公司 | Preparation method of ceramic pigment |
CN111662571B (en) * | 2017-12-12 | 2021-09-03 | 佛山市大千色釉料有限公司 | Preparation method of ceramic pigment |
CN109231959A (en) * | 2018-08-15 | 2019-01-18 | 陕西科技大学 | A kind of preparation method using leather sludge production exterior wall tile |
CN111662570A (en) * | 2020-05-25 | 2020-09-15 | 武汉科技大学 | Mixed spinel type black ceramic pigment and preparation method thereof |
CN113999044A (en) * | 2021-11-12 | 2022-02-01 | 郑州磨料磨具磨削研究所有限公司 | Porous ceramic plate and preparation method thereof |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN102260078B (en) | Zirconia ceramic and preparation method thereof | |
CN104108952A (en) | Method for preparing black ceramic pigment by using leather making sludge and product | |
CN108047763B (en) | Ceramic pigment and preparation method thereof | |
CN102992808A (en) | Method for preparing black ceramic pigment for blank by use of chromium-containing waste residue and product prepared by same | |
CN101696125A (en) | Method for preparing cobalt-free black ceramic pigment by using copper ore tailings and product manufactured by using same | |
CN100455630C (en) | Method for preparing nanometer cobalt blue dye | |
CN109456617B (en) | Black ceramic pigment and preparation method thereof | |
CN109111760A (en) | A kind of alumina ceramic of black color toner and its preparation method and application | |
CN103980005B (en) | Preparation method of blue-and-white material with Kangxi blue-and-white color development effect and blue-and-white porcelain product decorated by blue-and-white material | |
CN102910892A (en) | Black ceramic plate prepared by natural minerals and extracted vanadium tailings and preparation method of black ceramic plate | |
CN102617116A (en) | Method for preparing ceramic black materials by utilizing industrial slag | |
CN102617188B (en) | Method for preparing split-phase black fancy glaze by utilizing industrial slag | |
CN103601244A (en) | Preparation method of molybdenum bismuth vanadate yellow pigment | |
CN105198392A (en) | Method for preparing black cobalt-free ceramic pigment for billets from steel slag and product decorated by black cobalt-free ceramic pigment for billets | |
CN109266040B (en) | High-temperature red ceramic pigment and preparation method thereof | |
CN110982303A (en) | Method for preparing copper-chromium black toner by promoting solid-phase sintering by using V-Mn and application thereof | |
CN106046857A (en) | Method for preparing black ceramic pigment with cobalt-and-manganese waste materials and black ceramic pigment | |
CN104108953B (en) | A kind of production method that can reduce the green ceramic colorant of production cost | |
CN101544406B (en) | Method for producing red iron oxide pigment | |
CN108862385A (en) | The control method of partial size in a kind of production of chrome oxide green | |
CN111039324A (en) | Copper-chromium black and preparation method thereof | |
CN105692704A (en) | Preparation method of temperature-resistant iron oxide yellow | |
CN1137941C (en) | Preparing process of iron oxide red pigment for high-temperature ceramic with iron-containing industrial sludge | |
CN110128850B (en) | Method for preparing mixed-phase spinel type black ceramic hybrid pigment by using oil shale semicoke | |
CN103553147B (en) | Preparation method of high-stability spinel black toner |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C12 | Rejection of a patent application after its publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20141022 |