CN105778566A - Method for preparing pigment with manganese carbonate - Google Patents
Method for preparing pigment with manganese carbonate Download PDFInfo
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- CN105778566A CN105778566A CN201610111336.4A CN201610111336A CN105778566A CN 105778566 A CN105778566 A CN 105778566A CN 201610111336 A CN201610111336 A CN 201610111336A CN 105778566 A CN105778566 A CN 105778566A
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- manganese carbonate
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/0009—Pigments for ceramics
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/60—Optical properties, e.g. expressed in CIELAB-values
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for preparing pigment with manganese carbonate.The method includes the steps that manganese carbonate is subjected to surface modification processing, then the manganese carbonate obtained after surface modification treatment is subjected to decaying processing at the temperature of 30-50 DEG C, the decaying processing time is 48-60 hours, then the manganese carbonate obtained after decaying processing is mixed with an auxiliary material to form a mixture, the mixture is calcined to 1150 DEG C at the heating rate of 80-100 DEG C/h, then the calcined mixture is subjected to heat preservation for 1-2 hours at the temperature of 1130-1200 DEG C, and the pigment is obtained.The method for preparing the pigment with the manganese carbonate has the advantages that the sintering range of the prepared pigment becomes wider, and high temperature performance is good, and the pigment can be applied to high-end ceramic products.
Description
Technical field
The present invention relates to colorant production technology, particularly to a kind of method utilizing manganese carbonate to prepare colorant.
Background technology
Using manganese carbonate at present in ceramic pigment industry is that raw material is to produce colorant.This colorant mostly is pink look
Material, employing manganese carbonate of the prior art is that the method for the pink colorant of raw material production exists colorant firing range
Narrow, under 1250 DEG C of temperatures above environment use time glaze easily occur that pin hole, tinting strength, tinting power are weak and tone is inadequate
Bright-coloured problem, i.e. deposits the deficiency that using effect is the best in high temperature environments.Thus cannot be applied to high-end
In ceramic.
The Chinese invention patent of Patent No. 200710106267.9 discloses a kind of manganese doped corundum type pink coloring
The preparation method of material, the steps include: that (1) is by required aluminum nitrate, aluminium hydroxide, manganese nitrate and manganese carbonate four kinds
Raw material in molar ratio Mn: Al=0.15～0.20 ratio calculate the quality of each raw material used, allocated into
Volume ratio is in the solution of second alcohol and water of 30: 70；(2) mixed solution prepared is put into and spray gun feed liquor
In the container that pipe connects, and carrying out strong agitation, the air inlet at spray gun accesses 0.3～0.8kg/cm2Pressure
Compressed air；(3) leading portion at continuous oven is warmed up to 200 DEG C, and back segment is warmed up to 550 DEG C and keeps continuous oven two
Duan Wendu's is constant；(4) open spray gun to be sprayed to by mixed solution and be dried in stove and be atomized decomposition；(5) will
The powder that continuous oven afterbody is collected is calcined 3～4 hours in 900～1100 DEG C of high temperature furnaces, by per minute 5～
The speed of 10 DEG C cools to room temperature and i.e. obtains and required have additive Mn Alpha-alumina corundum type pink coloring material.
That is: use spray-wall interaction to combine calcine technology, with aluminum nitrate, aluminium hydroxide, manganese nitrate and manganese carbonate be
Raw material, is formed by calcining and has certain particle size and the method for pattern uniform corundum type ceramic powder red stain.
Simply, easily produce, prepare has additive Mn Α-aluminum oxide for this colorant low cost of manufacture, process control procedure
The advantage that corundum type ceramic powder red stain powder diameter is uniform, composition is controlled and purity is high.
The colorant that the preparation method of the manganese doped corundum type pink coloring material described in above-mentioned patent obtains does not overcomes look yet
The problem that material firing range is narrow and high-temperature behavior is the best.
Summary of the invention
The technical problem to be solved is: provide a kind of colorant firing range width and high-temperature behavior good
Utilize the method that colorant prepared by manganese carbonate.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is:
A kind of method utilizing manganese carbonate to prepare colorant, carries out surface modification treatment by manganese carbonate, then by table
Manganese carbonate after the modification of face carries out old process under the conditions of 30-50 DEG C, and the time of described old process is
48-60h, then mixes the manganese carbonate after old process with auxiliary material, forms mixture, by described mixing
Thing is fired to 1150 DEG C with the heating rate of 80-100 DEG C/h by 0 DEG C, then will calcining after mixture in
1-2h it is incubated, it is thus achieved that described colorant under the conditions of 1130-1200 DEG C.
The beneficial effects of the present invention is:
(1) by manganese carbonate being carried out successively surface modification treatment and old process, and old process is coordinated
Condition design, can make the reactivity of manganese carbonate and dispersive property significantly improve；
(2) manganese carbonate that reactivity and dispersive property significantly improve is follow-up valid with the reaction of auxiliary material
Standby, make the firing range of the colorant (pink colorant) prepared broaden, and the colorant obtained is at height
Use under temperature environment, there is glaze and occur without that pin hole, tone be bright-coloured and the advantage of strong coloring force, therefore, this
The colorant that invention prepares can be applicable in high-end ceramic.
Detailed description of the invention
By describing the technology contents of the present invention in detail, being realized purpose and effect, give below in conjunction with embodiment
With explanation.
The design of most critical of the present invention is: manganese carbonate carries out surface modification treatment and old process successively,
The reactivity and the dispersive property that make manganese carbonate significantly improve, and then make the firing range of colorant broaden.
The present invention provides a kind of method utilizing manganese carbonate to prepare colorant, and manganese carbonate is carried out surface modification treatment,
Then the manganese carbonate after surface modification treatment is carried out under the conditions of 30-50 DEG C old process, described old process
Time be 48-60h, then the manganese carbonate after old process is mixed with auxiliary material, formed mixture,
Described mixture is fired to 1150 DEG C with the heating rate of 80-100 DEG C/h by 0 DEG C, then by after calcining
Mixture is incubated 1-2h under the conditions of 1130-1200 DEG C, it is thus achieved that described colorant.
The technology of the present invention is contemplated that:
First manganese carbonate is carried out surface modification treatment, the needs reacted according to concrete colorant so that it is obtained
Dispersed, active, formed and be prone to the material that colorant (such as pink colorant) reacts；Described surface modification
The method that the concrete grammar processed can use surface modification treatment of the prior art, such as, add surface and change
Property inorganic agent etc., if the manganese carbonate after surface modification treatment had dispersiveness, activity be prone to look
Material reaction, i.e. meets the demand of colorant reaction.BET multipoint method can also be used to measure at surface modification
The specific surface area of the manganese carbonate after reason, and carried out observing and controlling the granularity of manganese carbonate by laser particle analyzer；So
After will carry out old process after surface modification treatment, this old process advantage simple and flexible, environmental protection, do not have
Waste water and gas produces, and place and environmental condition are not had particular/special requirement, only there are certain requirements standing time,
Fully to improve reactivity and the dispersive property of manganese carbonate；Then mix with auxiliary material.In principle, only
If the raw material in addition to manganese carbonate in prepared by colorant all can be as the auxiliary material of the present invention.
Knowable to foregoing description, the beneficial effects of the present invention is:
(1) carry out surface modification treatment and old process successively by manganese carbonate, and coordinate the bar of old process
Part designs, and the reactivity of manganese carbonate and dispersive property can be made to significantly improve；
(2) manganese carbonate that reactivity and dispersive property significantly improve is follow-up valid with the reaction of auxiliary material
Standby, make the firing range of the colorant (pink colorant) prepared broaden, and the colorant obtained is at height
Use under temperature environment, there is glaze and occur without that pin hole, tone be bright-coloured and the advantage of strong coloring force, therefore, this
The colorant that invention prepares can be applicable in high-end ceramic.
Further, the granularity of described manganese carbonate is 10-12 μm.
Further, during described auxiliary material is aluminum oxide, aluminium hydroxide, calcium phosphate and calcium chloride at least
A kind of.
Further, the manganese carbonate after old process dried successively and ground, then mixing with auxiliary material
Close.Manganese carbonate after old process is dried under the conditions of temperature is 120-150 DEG C 200-280min, then by old
The granularity being ground to manganese carbonate of the manganese carbonate after rotten process is 3-4.5 μm.
Seen from the above description, the manganese carbonate after old process can be dried successively and grind, preferably
The granularity being ground to manganese carbonate is 3-4.5 μm, makes the specific surface area of manganese carbonate increase, in order to filling of reaction
Divide and carry out.
Further, the mixture after insulation is cooled down.Mixture after insulation is ground successively,
Washing and drying.
Seen from the above description, can carry out cooling down by the mixture after insulation, grind, wash and drying etc.
Subsequent treatment, it is thus achieved that be prone to preservation, the colorant of required specification.
Further, the mixture after calcining is incubated 1.5h under the conditions of 1160 DEG C.
Seen from the above description, the above-mentioned setting for preferred heat-retaining condition, have and make preparation process material anti-
Should technique effect completely.
Embodiments of the invention one are:
A kind of method utilizing manganese carbonate to prepare colorant, carries out surface modification by the manganese carbonate that granularity is 10 μm
Process, then the manganese carbonate after surface modification treatment is carried out under the conditions of 30 DEG C old process, described old
Process time be 48h, then the manganese carbonate after old process is dried successively and is ground, then with auxiliary
Raw material mixes, and described auxiliary material is the mixture of aluminum oxide, aluminium hydroxide, calcium phosphate and calcium chloride.Will
Manganese carbonate after old process dries 200min under the conditions of temperature is 120 DEG C, then by the carbon after old process
The granularity being ground to manganese carbonate of acid manganese is 3 μm；Described auxiliary material is.Form mixture, by described mixed
Compound is fired to 1150 DEG C with the heating rate of 80 DEG C/h by 0 DEG C, then by the mixture after calcining in 1130 DEG C
Under the conditions of be incubated 1h, will insulation after mixture carry out successively cooling down, grind, wash and drying, it is thus achieved that institute
State colorant.
Embodiments of the invention two are:
A kind of method utilizing manganese carbonate to prepare colorant, carries out surface modification by the manganese carbonate that 12 μm granularities are
Process, then the manganese carbonate after surface modification treatment is carried out under the conditions of 50 DEG C old process, described old
Process time be 60h, then the manganese carbonate after old process is dried successively and is ground, then with auxiliary
Raw material mixes, and described auxiliary material is the mixture of aluminum oxide, aluminium hydroxide, calcium phosphate and calcium chloride.Will
Manganese carbonate after old process dries 280min under the conditions of temperature is 150 DEG C, then by the carbon after old process
The granularity being ground to manganese carbonate of acid manganese is 4.5 μm；Described auxiliary material is.Form mixture, by described
Mixture is fired to 1150 DEG C with the heating rate of 100 DEG C/h by 0 DEG C, then will calcining after mixture in
It is incubated 2h under the conditions of 1200 DEG C, carries out successively cooling down, grind, wash and drying by the mixture after insulation,
Obtain described colorant.
Embodiments of the invention three are:
A kind of method utilizing manganese carbonate to prepare colorant, carries out surface modification by the manganese carbonate that 11 micron granularities are
Process, then the manganese carbonate after surface modification treatment is carried out under the conditions of 40 DEG C old process, described old
Process time be 55h, then the manganese carbonate after old process is dried successively and is ground, then with auxiliary
Raw material mixes, and described auxiliary material is the mixture of aluminum oxide, aluminium hydroxide, calcium phosphate and calcium chloride.Will
Manganese carbonate after old process dries 240min under the conditions of temperature is 135 DEG C, then by the carbon after old process
The granularity being ground to manganese carbonate of acid manganese is 4 μm；Described auxiliary material is.Form mixture, by described mixed
Compound is fired to 1150 DEG C with the heating rate of 90 DEG C/h by 0 DEG C, then by the mixture after calcining in 1180 DEG C
Under the conditions of be incubated 1.5h, will insulation after mixture carry out successively cooling down, grind, wash and drying, it is thus achieved that
Described colorant.
Embodiments of the invention four are:
Manganese carbonate of the present invention produces the method for pink colorant, comprises the following steps:
1) surface modification treatment of carbonic acid manganese powder: by the carbonic acid manganese powder that granularity is 10-12 μm, by reaction
Still be modified process, formed a kind of good dispersion, activity good, be prone to pink colorant reaction material；
2) old process: to step 1) material of gained carries out old process under 30-50 DEG C of environment, old
The process time is 48-60 hour, grinds to form fine powder standby after then drying, and the granularity of described fine powder is 3-4.5
μm；
3) prepare sample: weigh step 2) manganese carbonate and the aluminum oxide of gained, aluminium hydroxide, calcium phosphate and
Calcium chloride (other auxiliary materials of pink colorant) is fully mixed evenly, and loads special saggar, at electricity high temperature
Carry out calcination processing in stove, at the uniform velocity heat up in 0 DEG C to 1150 DEG C, about 80 DEG C of-100 DEG C/h of dresses of heating rate
Alms bowl heating and calcining 10 hours, insulation 1.5 hours when reaching 1160 DEG C of at the uniform velocity heating up, take after cooling down
Go out, grind washing and dry, then carry out pink color development contrast.
The colorant of the acquisition of embodiment one to embodiment four is respectively adopted BET multipoint method and carries out specific surface area survey
Amount, and the specific surface area of measurement is contrasted, the most as shown in table 1 before processing；Table 1 is embodiment
The specific surface area of the colorant that one to embodiment four obtains and contrast table before treatment.
Table 1
According to table 1, the specific surface area of the colorant that embodiment one to embodiment four obtains is tool compared with before process
It is significantly improved.
The colorant obtaining embodiment one to embodiment four detects its firing range respectively, and by measurement
Firing range contrasts, the most as shown in table 2 before processing；Table 1 is the look of embodiment one to four
The firing range of material and contrast table before treatment.
Table 2
As shown in Table 2, the firing range of the colorant that embodiment one to four obtains has compared with before process
More apparent increase.
Colorant embodiment one to embodiment four obtained carries out color development experiment respectively, and structure is as shown in table 3,
Table 3 is the colorant high temperature color development value of chromatism of embodiment one to embodiment four acquisition and contrast table before treatment.
Table 3
As shown in Table 3, the high temperature color development value of chromatism of the colorant that embodiment one to embodiment four obtains shows relatively
Be significantly improved before processing effect.
The specific surface area that the present invention is increased effectively by manganese carbonate surface modification and old process, improves carbonic acid
The reactivity of manganese, dispersive property are good, increase colorant firing range, use glaze to occur without under hot environment
Pin hole, tone are bright-coloured, strong coloring force, may apply in high-end ceramic.
In sum, the method utilizing manganese carbonate to prepare colorant that the present invention provides has the look making to prepare
The advantage that the firing range of material broadens and high-temperature behavior is good, can be applicable in high-end ceramic.
The foregoing is only embodiments of the invention, not thereby limit the scope of the claims of the present invention, every profit
The equivalents made by description of the invention content, or directly or indirectly it is used in relevant technical field,
The most in like manner it is included in the scope of patent protection of the present invention.
Claims (8)
1. one kind utilizes the method that colorant prepared by manganese carbonate, it is characterised in that manganese carbonate is carried out surface modification
Process, then the manganese carbonate after surface modification treatment is carried out under the conditions of 30-50 DEG C old process, described old
The rotten time processed is 48-60h, is then mixed with auxiliary material by the manganese carbonate after old process, is formed mixed
Compound, is fired to 1150 DEG C with the heating rate of 80-100 DEG C/h by 0 DEG C by described mixture, then will forge
Mixture after burning is incubated 1-2h under the conditions of 1130-1200 DEG C, it is thus achieved that described colorant.
The method utilizing manganese carbonate to prepare colorant the most according to claim 1, it is characterised in that described
The granularity of manganese carbonate is 10-12 μm.
The method utilizing manganese carbonate to prepare colorant the most according to claim 1, it is characterised in that described
Auxiliary material is at least one in aluminum oxide, aluminium hydroxide, calcium phosphate and calcium chloride.
The method utilizing manganese carbonate to prepare colorant the most according to claim 1, it is characterised in that by old
Manganese carbonate after rotten process is dried successively and grinds, then mixes with auxiliary material.
The method utilizing manganese carbonate to prepare colorant the most according to claim 4, it is characterised in that by old
Manganese carbonate after rotten process dries 200-280min under the conditions of temperature is 120-150 DEG C, then by after old process
The granularity being ground to manganese carbonate of manganese carbonate be 3-4.5 μm.
The method utilizing manganese carbonate to prepare colorant the most according to claim 1, it is characterised in that will protect
Mixture after temperature cools down.
7. according to utilizing, described in claim 1 or 6, the method that manganese carbonate prepares colorant, it is characterised in that
Mixture after insulation is ground successively, washes and dries.
The method utilizing manganese carbonate to prepare colorant the most according to claim 1, it is characterised in that will forge
Mixture after burning is incubated 1.5h under the conditions of 1160 DEG C.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610111336.4A CN105778566B (en) | 2016-02-29 | 2016-02-29 | A kind of method that colorant is prepared using manganese carbonate |
| CN201810377479.9A CN108864762B (en) | 2016-02-29 | 2016-02-29 | Method for preparing pigment by using manganese carbonate and capable of enabling pigment to have strong coloring power |
| CN201810376871.1A CN108864761B (en) | 2016-02-29 | 2016-02-29 | Method for preparing pigment by using manganese carbonate and capable of enabling pigment to be bright in color tone |
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| CN201610111336.4A CN105778566B (en) | 2016-02-29 | 2016-02-29 | A kind of method that colorant is prepared using manganese carbonate |
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| CN201810376871.1A Division CN108864761B (en) | 2016-02-29 | 2016-02-29 | Method for preparing pigment by using manganese carbonate and capable of enabling pigment to be bright in color tone |
| CN201810377479.9A Division CN108864762B (en) | 2016-02-29 | 2016-02-29 | Method for preparing pigment by using manganese carbonate and capable of enabling pigment to have strong coloring power |
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| CN201810377479.9A Active CN108864762B (en) | 2016-02-29 | 2016-02-29 | Method for preparing pigment by using manganese carbonate and capable of enabling pigment to have strong coloring power |
| CN201610111336.4A Active CN105778566B (en) | 2016-02-29 | 2016-02-29 | A kind of method that colorant is prepared using manganese carbonate |
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| CN201810377479.9A Active CN108864762B (en) | 2016-02-29 | 2016-02-29 | Method for preparing pigment by using manganese carbonate and capable of enabling pigment to have strong coloring power |
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Also Published As
| Publication number | Publication date |
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| CN108864762A (en) | 2018-11-23 |
| CN108864761B (en) | 2020-09-01 |
| CN108864761A (en) | 2018-11-23 |
| CN108864762B (en) | 2020-06-02 |
| CN105778566B (en) | 2018-05-18 |
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