CN106967310B - Dedicated modified calcium carbonate of a kind of paint class and preparation method thereof - Google Patents
Dedicated modified calcium carbonate of a kind of paint class and preparation method thereof Download PDFInfo
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- CN106967310B CN106967310B CN201710312635.9A CN201710312635A CN106967310B CN 106967310 B CN106967310 B CN 106967310B CN 201710312635 A CN201710312635 A CN 201710312635A CN 106967310 B CN106967310 B CN 106967310B
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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
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/021—Calcium carbonates
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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
- 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
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
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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
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
- C01P2006/19—Oil-absorption capacity, e.g. DBP values
Abstract
The invention discloses a kind of preparation methods for painting the dedicated modified calcium carbonate of class, include the following steps: the preparation of (1) modifying agent: by mass percentage (90~95) by oleic acid, styrene and maleic anhydride: (5~9): (1~5) is put into reactor, after being stirred to react, it is cooling, the hydroquinone of product quality 0.03~0.1% is added to get modifying agent is arrived；(2) modifying agent is added modified in oxide spinel calcium, the oxide spinel calcium is powdered whiting or calcium carbonate mineral to get to the paint dedicated modified calcium carbonate of class.Product activation rate made from the method for the present invention is high, and the low and compatibility with high molecular polymer of oil factor is good.
Description
Technical field
The invention belongs to calcium carbonate modified fields, and in particular to a kind of dedicated modified calcium carbonate of paint class and its preparation side
Method.
Background technique
Calcium carbonate is a kind of cheap packing material, is had a wide range of applications in industries such as plastics, rubber, coating, papermaking.
But it is hydrophilic and oleophobic since its surface can be high, easily reunite, it is very poor with the compatibility of high molecular polymer.Therefore, it is being filled into
When high molecular polymer, it is modified to need to carry out it surface, to improve its dispersion and compatibility in the polymer, reduce at
This, improves performance.The modification technology of calcium carbonate is there are modification temperature height at present, and activation grade is insufficient, and oil factor is not low, and specificity is not
By force.Modification temperature is low, reduces energy consumption, and oil factor is low in the filling process, reduces high molecular polymer dosage and its performance
It is constant, it reduces costs.Many modifying agent sufficiently can not react cladding in calcium carbonate surface under cryogenic, so that living
Rate is not high.In the thorax of ring roll mill temperature be typically all be lower than 80 DEG C, therefore many modifying agent can not in milling apparatus with carbon
Sour calcium ore grinds modification together.Calcium carbonate modified method in terms of coating, we find following patent:
1, application number: 201610100450.7, denomination of invention: a kind of dedicated modified powdered whiting of paint and its system
Preparation Method and device, although product oil factor can be down to 17-20g oil/100g, during the preparation process, temperature of plate
It is 95-100 DEG C, temperature is higher, consumes energy larger, and the temperature of plate due to requiring is higher than 80 DEG C, can not be in milling apparatus
Modification is ground together with calcium carbonate mineral.
2, application number: 201610914887.4, a kind of denomination of invention: self-dispersing polymer-modified by maleic acid anhydride graft
Calcium carbonate powder and preparation method thereof, temperature of plate is 80-90 DEG C, is consumed energy larger, and the calcium carbonate that its method obtains
Powder oil factor is 0.42ml/g, is converted as unit of g/100g, is 42g/100g, and oil factor is higher.
3, application number: 201610914825.3, denomination of invention: a kind of erosion-resisting modified calcium carbonate powder and its preparation side
Method is modified although can be carried out grinding, and the calcium carbonate powder oil factor that its method obtains is 0.32ml/g, is converted with g/
100g is unit, is 32g/100g, and oil factor is higher.
Summary of the invention
Present invention aim to address above-mentioned technical problem, provide a kind of modification temperature be 50~80 DEG C, modifying agent can be with
The dedicated modified calcium carbonate of paint class of progress self-crosslinking and product oil factor lower than 20g/100g and its preparation side at such a temperature
Method.
To realize above-mentioned purpose, the technical solution of the present invention is as follows:
A kind of preparation method for painting the dedicated modified calcium carbonate of class, includes the following steps:
(1) preparation of modifying agent: by mass percentage (90~95) by oleic acid, styrene and maleic anhydride: (5~9): (1
~5) it is put into reactor, it is cooling after being stirred to react, the hydroquinone of product quality 0.03~0.1% is added to get to changing
Property agent；
(2) modifying agent is added in oxide spinel calcium and is modified, the oxide spinel calcium is powdered whiting or calcium carbonate mine
Stone to get to paint the dedicated modified calcium carbonate of class.
As further technical solution, oleic acid described above, styrene, maleic anhydride and hydroquinone quality percentage
Than for 95:6:1, the hydroquinone additive amount is the 0.1% of product quality.
As further technical solution, the temperature that the above is stirred to react is 45~60 DEG C, and being stirred to react the time is 3
~5h, cooling temperature are room temperature.
As further technical solution, modifying agent is added in calcium carbonate described in step (2) and is modified, is by granularity
Powdered whiting not less than 1250 mesh is added in mixed at high speed dispersion machine, and under the conditions of 50~80 DEG C, addition accounts for heavy carbonic acid
Calcareous amount is not higher than 1% modifying agent, is sufficiently mixed stirring crosslinking and coats 10~20 minutes to get the paint dedicated modified carbon of class is arrived
Sour calcium.
As further technical solution, between step (1) and step (2), the emulsifying step of modifying agent is also added,
Specifically by mass percentage 1:1, emulsifier is added into modifying agent；After to be modified dose emulsifies completely, then step (2) are carried out,
Modifying agent is added in calcium carbonate described in step (2) and is modified, is that the modifying agent after complete emulsification is added dropwise to exist with constant flow pump
Calcium carbonate mineral surface, the additive amount of modifying agent is the 0.6%~1.6% of calcium carbonate mineral quality after emulsification, is re-fed into grinding
The calcium carbonate not less than 1250 mesh is ground into machine to get to the paint dedicated modified calcium carbonate of class.
As further technical solution, emulsifier described above is made of sodium cetanesulfonate and water, and described 16
Sodium alkyl sulfonate accounts for the 0.1~1% of the water quality.
The dedicated modified calcium carbonate of paint class that made as described above method obtains, the activation rate of modified calcium carbonate are 92.8
~99.5%, oil factor is 15.3~19.8g/100g, and contact angle is 131~150 °.
Reaction principle of the invention are as follows: oleic acid, styrene and maleic anhydride of the invention all contains double bond, can be in low temperature
Lower carry out cross-linking reaction, while oleic acid, maleic anhydride can be modified calcium carbonate surface with calcium carbonate surface chemisorption.
Compared with prior art, the invention has the benefit that the method for the present invention uses oleic acid, styrene and maleic anhydride
It was both reduced as modifying agent so that calcium carbonate can carry out crosslinking cladding under low temperature (50~80 DEG C) according to specific proportion
Energy consumption, and grinding modification can be carried out to powdered whiting and calcium carbonate mineral, improve the utilization of raw material；Thus method obtains
Product activation rate is 92.8~99.5%, and oil factor is 15.3~19.8g/100g, and contact angle is 131~150 °, and activation rate is high,
The low and compatibility with high molecular polymer of oil factor is good.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited to
The range that embodiment indicates.
Embodiment 1:
A kind of preparation method for painting the dedicated modified calcium carbonate of class, includes the following steps:
(1) preparation of modifying agent: by oleic acid, styrene and maleic anhydride, 90:9:1 is put into reactor by mass percentage
In, it is cooling after being stirred to react, the hydroquinone of product quality 0.03% is added to get modifying agent is arrived；It is described to be stirred to react
Temperature is 60 DEG C, and being stirred to react the time is 3h, and cooling temperature is room temperature；
(2) 1000kg, granularity are added in mixed at high speed dispersion machine not less than the powdered whiting of 1250 mesh, in 50 DEG C of items
Under part, the modifying agent of powdered whiting quality 0.3% is added, is sufficiently mixed stirring crosslinking and coats 10 minutes to get paint class is arrived
Dedicated modified calcium carbonate.
Embodiment 2:
A kind of preparation method for painting the dedicated modified calcium carbonate of class, includes the following steps:
(1) preparation of modifying agent: by oleic acid, styrene and maleic anhydride, 90:5:5 is put into reactor by mass percentage
In, it is cooling after being stirred to react, the hydroquinone of product quality 0.1% is added to get modifying agent is arrived；It is described to be stirred to react
Temperature is 55 DEG C, and being stirred to react the time is 4h, and cooling temperature is room temperature；
(2) 1000kg, granularity are added in mixed at high speed dispersion machine not less than the powdered whiting of 1250 mesh, in 70 DEG C of items
Under part, the modifying agent of powdered whiting quality 0.6% is added, is sufficiently mixed stirring crosslinking and coats 15 minutes to get paint class is arrived
Dedicated modified calcium carbonate.
Embodiment 3:
A kind of preparation method for painting the dedicated modified calcium carbonate of class, includes the following steps:
(1) preparation of modifying agent: by oleic acid, styrene and maleic anhydride, 95:6:1 is put into reactor by mass percentage
In, it is cooling after being stirred to react, the hydroquinone of product quality 0.1% is added to get modifying agent is arrived；It is described to be stirred to react
Temperature is 45 DEG C, and being stirred to react the time is 3h, and cooling temperature is room temperature；
(2) 1000kg, granularity are added in mixed at high speed dispersion machine not less than the powdered whiting of 1250 mesh, in 80 DEG C of items
Under part, the modifying agent of powdered whiting quality 0.8% is added, is sufficiently mixed stirring crosslinking and coats 20 minutes to get paint class is arrived
Dedicated modified calcium carbonate.
Embodiment 4:
A kind of preparation method for painting the dedicated modified calcium carbonate of class, includes the following steps:
(1) preparation of modifying agent: by oleic acid, styrene and maleic anhydride, 95:6:1 is put into reactor by mass percentage
In, it is cooling after being stirred to react, the hydroquinone of product quality 0.1% is added to get modifying agent is arrived；It is described to be stirred to react
Temperature is 60 DEG C, and being stirred to react the time is 5h, and cooling temperature is room temperature；
(2) emulsification of modifying agent: 1:1 by mass percentage adds emulsifier into modifying agent, and the emulsifier is by 16
Sodium alkyl sulfonate and water composition, the sodium cetanesulfonate account for the 0.1% of the water quality；
It (3) is that the modifying agent behind calcium carbonate mineral surface, emulsification is added dropwise in the modifying agent constant flow pump after complete emulsification
Additive amount is the 0.6% of calcium carbonate mineral quality, is re-fed into and is ground into calcium carbonate not less than 1250 mesh in grinder to get arriving
Paint the dedicated modified calcium carbonate of class.
Embodiment 5:
A kind of preparation method for painting the dedicated modified calcium carbonate of class, includes the following steps:
(1) preparation of modifying agent: by oleic acid, styrene and maleic anhydride, 95:6:1 is put into reactor by mass percentage
In, it is cooling after being stirred to react, the hydroquinone of product quality 0.1% is added to get modifying agent is arrived；It is described to be stirred to react
Temperature is 60 DEG C, and being stirred to react the time is 5h, and cooling temperature is room temperature；
(2) emulsification of modifying agent: 1:1 by mass percentage adds emulsifier into modifying agent, and the emulsifier is by 16
Sodium alkyl sulfonate and water composition, the sodium cetanesulfonate account for the 0.5% of the water quality；
It (3) is that the modifying agent behind calcium carbonate mineral surface, emulsification is added dropwise in the modifying agent constant flow pump after complete emulsification
Additive amount is the 1.2% of calcium carbonate mineral quality, is re-fed into and is ground into calcium carbonate not less than 1250 mesh in grinder to get arriving
Paint the dedicated modified calcium carbonate of class.
Embodiment 6:
A kind of preparation method for painting the dedicated modified calcium carbonate of class, includes the following steps:
(1) preparation of modifying agent: by oleic acid, styrene and maleic anhydride, 95:6:1 is put into reactor by mass percentage
In, it is cooling after being stirred to react, the hydroquinone of product quality 0.1% is added to get modifying agent is arrived；It is described to be stirred to react
Temperature is 60 DEG C, and being stirred to react the time is 5h, and cooling temperature is room temperature；
(2) emulsification of modifying agent: 1:1 by mass percentage adds emulsifier into modifying agent, and the emulsifier is by 16
Sodium alkyl sulfonate and water composition, the sodium cetanesulfonate account for the 1% of the water quality；
It (3) is that the modifying agent behind calcium carbonate mineral surface, emulsification is added dropwise in the modifying agent constant flow pump after complete emulsification
Additive amount is the 1.6% of calcium carbonate mineral quality, is re-fed into and is ground into calcium carbonate not less than 1250 mesh in grinder to get arriving
Paint the dedicated modified calcium carbonate of class.
The dedicated modified calcium carbonate product index of paint class prepared by embodiment 1-6 is as shown in table 1:
Table 1
Table 1 illustrates that product activation rate produced by the present invention is high, and the low and compatibility with high molecular polymer of oil factor is good.
Above-described embodiment is only further described the purpose of the present invention, technical scheme and beneficial effects specific
A example, present invention is not limited to this.All any modification, equivalent substitution and improvement done within the scope of disclosed by the invention
Deng being all included in the scope of protection of the present invention.
Claims (5)
1. a kind of preparation method for painting the dedicated modified calcium carbonate of class, which comprises the steps of:
(1) preparation of modifying agent: by mass percentage (90~95) by oleic acid, styrene and maleic anhydride: (5~9): (1~5)
It is put into reactor, it is cooling after being stirred to react, the hydroquinone of product quality 0.03~0.1% is added to get modifying agent is arrived；
(2) modifying agent is added it is modified in oxide spinel calcium, it is described modifying agent is added it is modified in calcium carbonate, be by granularity not
Oxide spinel calcium less than 1250 mesh is added in mixed at high speed dispersion machine, and under the conditions of 50~80 DEG C, addition accounts for oxide spinel calcium
Of low quality to be sufficiently mixed stirring crosslinking in 1% modifying agent and coat 10~20 minutes, the oxide spinel calcium is heavy carbonic acid
Calcium or calcium carbonate mineral are to get to the paint dedicated modified calcium carbonate of class.
2. a kind of preparation method for painting the dedicated modified calcium carbonate of class according to claim 1, it is characterised in that: described to stir
The temperature for mixing reaction is 45~60 DEG C, and being stirred to react the time is 3~5h, and cooling temperature is room temperature.
3. a kind of preparation method for painting the dedicated modified calcium carbonate of class according to claim 1, it is characterised in that: in step
(1) between step (2), the emulsifying step of modifying agent is also added, specifically by mass percentage 1:1 adds into modifying agent
Add emulsifier；After to be modified dose emulsifies completely, then step (2) are carried out, modifying agent is added in calcium carbonate described in step (2)
It is modified, it is that the modifying agent constant flow pump after complete emulsification is added dropwise in oxide spinel calcium surface, the additive amount of modifying agent after emulsification
It is the 0.6%~1.6% of the calcareous amount of oxide spinel, is re-fed into and is ground into calcium carbonate not less than 1250 mesh in grinder to get arriving
Paint the dedicated modified calcium carbonate of class.
4. a kind of preparation method for painting the dedicated modified calcium carbonate of class according to claim 3, it is characterised in that: the cream
Agent is made of sodium cetanesulfonate and water, and the sodium cetanesulfonate accounts for the 0.1~1% of the water quality.
5. the dedicated modified calcium carbonate of paint class that the preparation method as described in any one of Claims 1 to 4 obtains, feature exist
It is 92.8 ~ 99.5% in: the activation rate of its modified calcium carbonate, oil factor is 15.3~19.8g/100g, contact angle is 131~
150°。
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109135342A (en) * | 2018-09-28 | 2019-01-04 | 贺州钟山县双文碳酸钙新材料有限公司 | Paint-emulsion paint modified calcium carbonate |
| CN109627805B (en) * | 2019-01-15 | 2021-04-30 | 广西大学 | Preparation method and application of modified nano calcium carbonate |
| CN109762632B (en) * | 2019-01-15 | 2021-12-10 | 广西碳酸钙产业化工程院有限公司 | High-performance composite calcium sulfonate-based lubricating grease containing calcium carbonate and preparation method thereof |
| CN113372618B (en) * | 2021-07-31 | 2022-04-01 | 广东联塑科技实业有限公司 | Modified calcium carbonate and preparation method thereof, PVC pipe material containing modified calcium carbonate and PVC pipe |
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| CN1597531A (en) * | 2004-07-21 | 2005-03-23 | 华南理工大学 | Modified nanometer calcium carbonate and its preparation method |
| CN101671494A (en) * | 2009-09-19 | 2010-03-17 | 张家界恒亮新材料科技有限公司 | Surface modified calcium carbonate and preparation method thereof |
| CN106590042A (en) * | 2016-10-20 | 2017-04-26 | 青阳县永诚钙业有限责任公司 | Calcium carbonate powder modified by grafting of self dispersible polymer-maleic anhydride and preparation method thereof |
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| CN101671494A (en) * | 2009-09-19 | 2010-03-17 | 张家界恒亮新材料科技有限公司 | Surface modified calcium carbonate and preparation method thereof |
| CN106590042A (en) * | 2016-10-20 | 2017-04-26 | 青阳县永诚钙业有限责任公司 | Calcium carbonate powder modified by grafting of self dispersible polymer-maleic anhydride and preparation method thereof |
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