CN108864761A - It is a kind of to make the bright-coloured method for preparing colorant using manganese carbonate of colorant tone - Google Patents
It is a kind of to make the bright-coloured method for preparing colorant using manganese carbonate of colorant tone Download PDFInfo
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- CN108864761A CN108864761A CN201810376871.1A CN201810376871A CN108864761A CN 108864761 A CN108864761 A CN 108864761A CN 201810376871 A CN201810376871 A CN 201810376871A CN 108864761 A CN108864761 A CN 108864761A
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- manganese carbonate
- colorant
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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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- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of methods for preparing colorant using manganese carbonate, manganese carbonate is subjected to surface modification treatment, then the manganese carbonate after surface modification treatment is subjected to aging processing under the conditions of 30-50 DEG C, the time of the aging processing is 48-60h, then aging treated manganese carbonate is mixed with auxiliary material, form mixture, the mixture is fired to 1150 DEG C by 0 DEG C with the heating rate of 80-100 DEG C/h, then calcined mixture is kept the temperature under the conditions of 1130-1200 DEG C 1-2h, obtains the colorant.It is good with high-temperature behavior that the method for preparing colorant using manganese carbonate of the invention has the advantages that the firing range for the colorant for making to prepare broadens, and can be applied in high-end ceramic.
Description
This case is with the applying date on February 29th, 2016, application No. is 201610111336.4, a kind of entitled " utilization
The divisional application that the patent of invention of the method that manganese carbonate prepares colorant " carries out for female case.
Technical field
The present invention relates to colorant production technology, in particular to a kind of method for preparing colorant using manganese carbonate.
Background technique
Using manganese carbonate in ceramic pigment industry at present is raw material to produce colorant.The colorant is mostly pink colorant, existing
It is narrow with the presence of the method colorant firing range for using manganese carbonate to produce pink colorant for raw material in technology, at 1250 DEG C or more
Glaze paint is easy to appear the problem that pin hole, tinting strength, tinting power are weak and tone is not bright-coloured enough when using under temperature environment, that is, there is hot environment
The bad deficiency of lower using effect.Can not thus it be applied in high-end ceramic.
The Chinese invention patent of Patent No. 200710106267.9 discloses a kind of manganese doped corundum type pink coloring material
Preparation method, step are：(1) by four kinds of required aluminum nitrate, aluminium hydroxide, manganese nitrate and manganese carbonate raw materials Mn in molar ratio:
The ratio of Al=0.15~0.20 calculates the quality of each raw material used, is incorporated the second alcohol and water that volume ratio is 30: 70
In solution；(2) prepared mixed solution is put into the container connected with spray gun inlet tube, and stirred strongly, is being sprayed
The air inlet of rifle accesses 0.3~0.8kg/cm2The compressed air of pressure；(3) 200 DEG C are warming up in the leading portion of continuous oven, back segment
It is warming up to 550 DEG C and keeps the constant of two sections of temperature of continuous oven；(4) mixed solution is sprayed in furnace by unlatching spray gun is dried
It is decomposed with atomization；(5) powder for being collected into continuous oven tail portion is calcined 3~4 hours in 900~1100 DEG C of high temperature furnaces, by every
The speed of 5~10 DEG C of minute, which cools to, has additive Mn Alpha-alumina corundum type pink coloring material required for room temperature obtains.I.e.：
Using spray-wall interaction combination calcine technology, using aluminum nitrate, aluminium hydroxide, manganese nitrate and manganese carbonate as raw material, by calcining shape
At the method with certain particle size and corundum type ceramics pink coloring material of uniform morphology.The colorant manufacturing cost is low, technology controlling and process
Process is simple, easy to produce, the uniform, ingredient obtained with additive Mn Α-aluminium oxide corundum type ceramics pink coloring material powder diameter
Controllable and purity is high advantage.
The colorant that the preparation method of manganese doped corundum type pink coloring material described in above-mentioned patent obtains does not overcome colorant to burn yet
At the bad problem of narrow range and high-temperature behavior.
Summary of the invention
The technical problem to be solved by the present invention is to：The utilization carbon that a kind of colorant firing range is wide and high-temperature behavior is good is provided
The method that sour manganese prepares colorant.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：
A method of colorant being prepared using manganese carbonate, manganese carbonate is subjected to surface modification treatment, it is then that surface is modified
Treated, and manganese carbonate carries out aging processing under the conditions of 30-50 DEG C, and the time of the aging processing is 48-60h, then will be old
Rotten treated that manganese carbonate is mixed with auxiliary material, formation mixture, by the mixture with the heating rate of 80-100 DEG C/h
1150 DEG C are fired to by 0 DEG C, calcined mixture is then kept the temperature into 1-2h under the conditions of 1130-1200 DEG C, obtains the color
Material.
The beneficial effects of the present invention are：
(1) by the way that manganese carbonate is successively carried out surface modification treatment and aging processing, and the condition of aging processing is cooperated to set
Meter, can be such that the reactivity of manganese carbonate and dispersion performance significantly improves；
(2) manganese carbonate that reactivity and dispersion performance significantly improve is prepared to be subsequent with reacting for auxiliary material, is made
The firing range of the colorant (pink colorant) prepared broadens, and the colorant obtained uses under high temperature environment, has
Glaze paint does not occur the advantages of bright-coloured pin hole, tone and strong coloring force, and therefore, the colorant that the present invention prepares can be applied to high-end
Ceramic in.
Specific embodiment
To explain the technical content, the achieved purpose and the effect of the present invention in detail, it is explained below in conjunction with embodiment.
The design of most critical of the present invention is：Manganese carbonate is successively subjected to surface modification treatment and aging processing, make carbonic acid
The reactivity and dispersion performance of manganese significantly improve, and then the firing range of colorant is made to broaden.
The present invention provides a kind of method for preparing colorant using manganese carbonate, manganese carbonate is carried out surface modification treatment, then
Manganese carbonate after surface modification treatment is subjected to aging processing under the conditions of 30-50 DEG C, the time of the aging processing is 48-
Then aging treated manganese carbonate is mixed with auxiliary material, forms mixture by 60h, by the mixture with 80-100 DEG C/
The heating rate of h is fired to 1150 DEG C by 0 DEG C, and calcined mixture is then kept the temperature 1-2h under the conditions of 1130-1200 DEG C,
Obtain the colorant.
Technical concept of the invention is：
Manganese carbonate is first subjected to surface modification treatment, according to the needs that specific colorant reacts, the dispersibility for having obtained it,
Activity forms the substance for being easy to colorant (such as pink colorant) reaction；The specific method of the surface modification treatment can be adopted
With method of surface modification treatment in the prior art, such as surface modification treatment agent is added etc., as long as surface modification treatment
Dispersibility that manganese carbonate afterwards has had, activity are simultaneously easy to colorant reaction, that is, meet the needs of colorant reaction.It can also adopt
The specific surface area of manganese carbonate after measuring surface modification treatment with BET multipoint method, and observed and controlled by laser particle analyzer
The granularity of manganese carbonate；Then by the aging processing of carry out after surface modification treatment, the aging processing advantage simple and flexible, environmental protection,
There is no waste water and gas generation, there is no particular/special requirement to place and environmental condition, only standing time there are certain requirements, sufficiently to mention
The reactivity and dispersion performance of high carbon acid manganese；Then it is mixed with auxiliary material.In principle, as long as in colorant preparation
Raw material other than manganese carbonate can be used as auxiliary material of the invention.
As can be seen from the above description, the beneficial effects of the present invention are：
(1) surface modification treatment and aging processing are successively carried out by manganese carbonate, and cooperate the condition design of aging processing,
The reactivity and dispersion performance that can make manganese carbonate significantly improve；
(2) manganese carbonate that reactivity and dispersion performance significantly improve is prepared to be subsequent with reacting for auxiliary material, is made
The firing range of the colorant (pink colorant) prepared broadens, and the colorant obtained uses under high temperature environment, has
Glaze paint does not occur the advantages of bright-coloured pin hole, tone and strong coloring force, and therefore, the colorant that the present invention prepares can be applied to high-end
Ceramic in.
Further, the granularity of the manganese carbonate is 10-12 μm.
Further, the auxiliary material is at least one of aluminium oxide, aluminium hydroxide, calcium phosphate and calcium chloride.
Further, treated that manganese carbonate is successively dried and ground by aging, then mixes with auxiliary material.It will be old
Rotten treated manganese carbonate dries 200-280min under the conditions of being 120-150 DEG C in temperature, then by aging treated manganese carbonate
The granularity for being ground to manganese carbonate be 3-4.5 μm.
Seen from the above description, can treated that manganese carbonate is successively dried and ground by aging, be preferably ground to
The granularity of manganese carbonate is 3-4.5 μm, increases the specific surface area of manganese carbonate, in order to the abundant progress of reaction.
Further, the mixture after heat preservation is cooled down.Mixture after heat preservation is successively ground, wash and
Drying.
Seen from the above description, the mixture after heat preservation can be carried out the subsequent place such as cooling down, grind, wash and dry
Reason obtains the colorant of specification that be easy to save, required.
Further, calcined mixture is kept the temperature into 1.5h under the conditions of 1160 DEG C.
Seen from the above description, the above-mentioned setting for preferred heat-retaining condition, having keeps preparation process material reaction complete
Technical effect.
The embodiment of the present invention one is：
A method of colorant being prepared using manganese carbonate, the manganese carbonate that granularity is 10 μm is subjected to surface modification treatment, so
The manganese carbonate after surface modification treatment is subjected to aging processing under the conditions of 30 DEG C afterwards, the time of the aging processing is 48h, so
Treated that manganese carbonate is successively dried and ground by aging afterwards, then mixes with auxiliary material, and the auxiliary material is oxidation
Aluminium, aluminium hydroxide, calcium phosphate and calcium chloride mixture.It is dried under the conditions of being 120 DEG C in temperature by aging treated manganese carbonate
Dry 200min, then by the granularity for being ground to manganese carbonate of aging treated manganese carbonate be 3 μm；The auxiliary material is.It is formed
The mixture is fired to 1150 DEG C by 0 DEG C with the heating rate of 80 DEG C/h by mixture, then by calcined mixture in
1h is kept the temperature under the conditions of 1130 DEG C, the mixture after heat preservation is successively carried out cooling down, grind, wash and drying, obtains the colorant.
The embodiment of the present invention two is：
A method of colorant being prepared using manganese carbonate, the manganese carbonate for being by 12 μm of granularities carries out surface modification treatment, so
The manganese carbonate after surface modification treatment is subjected to aging processing under the conditions of 50 DEG C afterwards, the time of the aging processing is 60h, so
Treated that manganese carbonate is successively dried and ground by aging afterwards, then mixes with auxiliary material, and the auxiliary material is oxidation
Aluminium, aluminium hydroxide, calcium phosphate and calcium chloride mixture.It is dried under the conditions of being 150 DEG C in temperature by aging treated manganese carbonate
Dry 280min, then by the granularity for being ground to manganese carbonate of aging treated manganese carbonate be 4.5 μm；The auxiliary material is.Shape
The mixture is fired to 1150 DEG C by 0 DEG C with the heating rate of 100 DEG C/h, then by calcined mixing by resulting mixture
Object keeps the temperature 2h under the conditions of 1200 DEG C, the mixture after heat preservation is successively carried out cooling down, grind, wash and drying, described in acquisition
Colorant.
The embodiment of the present invention three is：
A method of colorant being prepared using manganese carbonate, the manganese carbonate for being by 11 micron granularities carries out surface modification treatment,
Then the manganese carbonate after surface modification treatment being subjected to aging processing under the conditions of 40 DEG C, the time of the aging processing is 55h,
Then treated that manganese carbonate is successively dried and ground by aging, then mixes with auxiliary material, and the auxiliary material is oxygen
Change the mixture of aluminium, aluminium hydroxide, calcium phosphate and calcium chloride.By aging treated manganese carbonate under the conditions of temperature is 135 DEG C
240min is dried, then by the granularity for being ground to manganese carbonate of aging treated manganese carbonate is 4 μm；The auxiliary material is.Shape
The mixture is fired to 1150 DEG C by 0 DEG C with the heating rate of 90 DEG C/h, then by calcined mixture by resulting mixture
1.5h is kept the temperature under the conditions of 1180 DEG C, the mixture after heat preservation is successively carried out cooling down, grind, wash and drying, described in acquisition
Colorant.
The embodiment of the present invention four is：
The method that manganese carbonate of the present invention produces pink colorant, includes the following steps：
1) surface modification treatment of carbonic acid manganese powder：The carbonic acid manganese powder for being 10-12 μm by granularity, is modified by reaction kettle
Processing forms the substance that a kind of good dispersion, activity is good, is easy to pink colorant reaction；
2) aging processing：Aging processing, aging processing time are carried out under 30-50 DEG C of environment to the resulting substance of step 1)
It is 48-60 hours, is ground into that fine powder is spare after then drying, the granularity of the fine powder is 3-4.5 μm；
3) sample is prepared：Weigh the resulting manganese carbonate of step 2) and aluminium oxide, aluminium hydroxide, calcium phosphate and calcium chloride (peach
Red stain other auxiliary materials) sufficiently it is mixed evenly, it is packed into dedicated saggar, calcination processing is carried out in electric high temperature furnace, 0 DEG C is extremely
It at the uniform velocity heats up in 1150 DEG C, about 80 DEG C of 10 hours of -100 DEG C/h of dress alms bowl heating and calcinings of heating rate, at the uniform velocity heating reach
1.5 hours are kept the temperature at 1160 DEG C, are taken out after cooling down, then grinding washing drying carries out pink color development comparison.
BET multipoint method is respectively adopted in the colorant of the acquisition of embodiment one to example IV and carries out specific surface area measurement, and
It will be compared before the specific surface area and processing of measurement, it is specific as shown in table 1；Table 1 is what embodiment one was obtained to example IV
The specific surface area and the contrast table before processing of colorant.
Table 1
According to table 1, the specific surface area for the colorant that embodiment one is obtained to example IV has bright compared with before processing
It is aobvious to improve.
Its firing range detected respectively to the colorant that embodiment one to example IV obtains, and by the firing temperature of measurement
It is compared before degree range and processing, it is specific as shown in table 2；Table 1 be embodiment one to four colorant firing range with
Contrast table before processing.
Table 2
As shown in Table 2, the firing range for the colorant that embodiment one to four obtains has more apparent compared with before processing
Increase.
The colorant that embodiment one to example IV obtains is subjected to color development experiment respectively, structure is as shown in table 3, and table 3 is real
Contrast table before applying the colorant high temperature color development value of chromatism and processing that example one to example IV obtains.
Table 3
As shown in Table 3, the high temperature color development value of chromatism for the colorant that embodiment one is obtained to example IV is shown relative to processing
Before be significantly improved effect.
The present invention handles effectively increased specific surface area with aging by the way that manganese carbonate surface is modified, improves the anti-of manganese carbonate
It answers activity, dispersion performance good, increases colorant firing range, do not occur that pin hole, tone be bright-coloured, coloring under hot environment using glaze paint
Power is strong, can be applied in high-end ceramic.
In conclusion the method provided by the invention for preparing colorant using manganese carbonate has the burning for the colorant for making to prepare
At the advantage that it is good with high-temperature behavior that range broadens, can be applied in high-end ceramic.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalents made by bright description are applied directly or indirectly in relevant technical field, are similarly included in this hair
In bright scope of patent protection.
Claims (1)
1. one kind can make the bright-coloured method for preparing colorant using manganese carbonate of colorant tone, which is characterized in that carry out manganese carbonate
Then manganese carbonate after surface modification treatment is carried out aging processing, the aging place by surface modification treatment under the conditions of 40 DEG C
The time of reason is 55h, then mixes aging treated manganese carbonate with auxiliary material, formation mixture, by the mixture
1150 DEG C are fired to by 0 DEG C with the heating rate of 90 DEG C/h, then keeps the temperature calcined mixture under the conditions of 1180 DEG C
Mixture after heat preservation is successively ground, washed and is dried by 1.5h, obtains the colorant；
The granularity of the manganese carbonate is 11 μm；
Dry 240min under the conditions of being 135 DEG C in temperature by aging treated manganese carbonate, then by aging treated manganese carbonate
The granularity for being ground to manganese carbonate be 4 μm, then mixed with auxiliary material；The auxiliary material is aluminium oxide, aluminium hydroxide, phosphoric acid
Calcium or calcium chloride.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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|---|---|---|---|
| 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 |
| 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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| CN201610111336.4A Division CN105778566B (en) | 2016-02-29 | 2016-02-29 | A kind of method that colorant is prepared using manganese carbonate |
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| CN201610111336.4A Active CN105778566B (en) | 2016-02-29 | 2016-02-29 | A kind of method that colorant is prepared using manganese carbonate |
| 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 |
|---|---|
| CN105778566B (en) | 2018-05-18 |
| CN105778566A (en) | 2016-07-20 |
| CN108864762A (en) | 2018-11-23 |
| CN108864762B (en) | 2020-06-02 |
| CN108864761B (en) | 2020-09-01 |
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