CN106752098A - A kind of nano-calcium carbonate powder of ferrocene polyethyleneimine cross-linked polymer coating modification and preparation method thereof - Google Patents
A kind of nano-calcium carbonate powder of ferrocene polyethyleneimine cross-linked polymer coating modification and preparation method thereof Download PDFInfo
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- CN106752098A CN106752098A CN201610915011.1A CN201610915011A CN106752098A CN 106752098 A CN106752098 A CN 106752098A CN 201610915011 A CN201610915011 A CN 201610915011A CN 106752098 A CN106752098 A CN 106752098A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/182—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds
- C01F11/183—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by an additive other than CaCO3-seeds the additive being an organic compound
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- 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
- C09C3/08—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
- 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
- C09C3/10—Treatment with macromolecular organic compounds
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- 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
- C09C3/12—Treatment with organosilicon compounds
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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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 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
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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
- C01P2006/90—Other properties not specified above
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- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Paints Or Removers (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a kind of nano-calcium carbonate powder of ferrocene polyethyleneimine cross-linked polymer coating modification, the nano-calcium carbonate powder is prepared by carbonizatin method, with deionized water in preparation process, the composite solution that fluorocarbon surfactant is prepared is used as reaction medium, and add silane coupler kh550 to be modified treatment, so that the nano-calcium carbonate powder for preparing has good self-dispersing and certain hydrophobicity, pattern is more preferably, and in its surface grafting ferrocene polyethyleneimine cross-linked polymer, finally it is prepared for the nano-calcium carbonate powder with certain chemical property and adsorptivity, the use scope of calcium carbonate powder is further widened, make its functionalization.
Description
Technical field
The present invention relates to modified calcium carbonate technical field, more particularly to a kind of ferrocene-polyethyleneimine cross-linked polymer
Nano-calcium carbonate powder of coating modification and preparation method thereof.
Background technology
Calcium carbonate powder is a kind of very common inorganic material, and it is mainly used in papermaking, rubber, plastics, coating, oil
As reinforced filling in the products such as ink.Calcium carbonate powder surface polarity is high, hydrophilic oleophobic, with organic phase poor compatibility, easily rolls into a ball
Poly-, bad dispersibility does not reach gratifying filling-modified effect, it is necessary to carry out surface modification treatment to it, is made with improving it
With performance, there is that local reaction is modified, surface coating modification, high energy surface are modified and machinery changes using more method of modifying at present
Property method.
The surface coating modification of calcium carbonate is to carry out cladding treatment in calcium carbonate surface using organic or inorganic material, its energy
It is effective to improve the stability and dispersiveness for being wrapped by particle, there is more prominent advantage than other class method of modifying.《Shell
The interfacial characteristics research of glycan-adipic acid dual cladding modified calcium carbonate》One text is entered using adipic acid, shitosan to calcium carbonate
Row dual cladding, obtains with good dispersion, while introducing the unique performance of shitosan, has further widened calcium carbonate
Using scope, but cladding material easily comes off in process of lapping, causes the forfeiture of modified effect, therefore improve coating modification
Group and the problem that the adhesion of calcium carbonate is that industry compels to solve.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of ferrocene-polyethyleneimine crosslinking is poly-
Nano-calcium carbonate powder of compound coating modification and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of nano-calcium carbonate powder of ferrocene-polyethyleneimine cross-linked polymer coating modification, the nano-calcium carbonate powder
It is made up of the raw material of following weight portion：Calcium oxide 10-20, carbon dioxide（Technical pure）In right amount, fluorocarbon surfactant 0.01-
0.02nd, polyethyleneimine 2-3, ferrocene carboxaldehyde 0.5-1, silane coupler kh550 0.4-0.5, deionized water 100-200, nothing
Water-ethanol 50-80.
A kind of preparation side of the nano-calcium carbonate powder of described ferrocene-polyethyleneimine cross-linked polymer coating modification
Method is comprised the following steps：
（1）During deionized water, fluorocarbon surfactant first put into reaction vessel successively, stirring mixing 20- under nitrogen atmosphere
System is heated to 80-85 DEG C after 30min, calcium oxide is and then added, grinding stirring digestion 2-3h forms calcium hydroxide slurry
Material, it is standby after ageing 10-15h；
（2）Agitating device is opened, to step（1）Silane coupler kh550 is added dropwise in the slurries of preparation, starts to lead to after completion of dropping
Carbon dioxide, stops ventilation when stabilizing to neutrality to system pH, continue to stir hybrid reaction 40-50min, and reaction terminates
System filtering afterwards, filtrate is scrubbed, vacuum drying, dispersion, obtain pre- modified nano calcium carbonate powder standby；
（3）The absolute ethyl alcohol of 10-15 weight powder is taken, ferrocene carboxaldehyde is added, stirring is completely dissolved to it, is configured to solution standby
With；
（4）In remainder amount absolute ethyl alcohol input reaction vessel, polyethyleneimine is subsequently added into, stirring puts into after being completely dissolved to it
Pre- modified nano calcium carbonate powder, ultrasonic disperse 40-50min is then added dropwise ferrocene carboxaldehyde alcoholic solution, and addition continues after finishing
Reaction 2-3h, then filtering, products therefrom is dried after washing, dispersion, obtains final product described modified nano calcium carbonate powder.
The present invention is prepared for nano-calcium carbonate powder using carbonizatin method, with deionized water, fluorocarbon surface in preparation process
The composite solution that activating agent is prepared adds silane coupler kh550 to be modified treatment as reaction medium so that preparation
Nano-calcium carbonate powder has a good self-dispersing and certain hydrophobicity, pattern more preferably, and its surface grafting ferrocene-
Polyethyleneimine cross-linked polymer, is finally prepared for the nano-calcium carbonate powder with certain chemical property and adsorptivity, enters
One step has widened the use scope of calcium carbonate powder, makes its functionalization.
Specific embodiment
A kind of nano-calcium carbonate powder of ferrocene polyethyleneimine cross-linked polymer coating modification, the nano-calcium carbonate calcium powder
Body is made up of the raw material of following weight portion：Calcium oxide 10, carbon dioxide（Technical pure）In right amount, fluorocarbon surfactant 0.01, poly-
Aziridine 2, ferrocene carboxaldehyde 0.5, silane coupler kh550 0.4, deionized water 100, absolute ethyl alcohol 50.
The embodiment modified nano calcium carbonate raw powder's production technology is comprised the following steps：
（1）During deionized water, fluorocarbon surfactant first put into reaction vessel successively, stirring mixing under nitrogen atmosphere
System is heated to 80 DEG C after 20min, calcium oxide is and then added, grinding stirring digestion 2h forms calcium hydroxide slurry, ageing
It is standby after 10h；
（2）Agitating device is opened, to step（1）Silane coupler kh550 is added dropwise in the slurries of preparation, starts to lead to after completion of dropping
Carbon dioxide, stops ventilation when stabilizing to neutrality to system pH, continue to stir hybrid reaction 40min, after reaction terminates
System is filtered, filtrate is scrubbed, vacuum drying, dispersion, obtain pre- modified nano calcium carbonate powder standby；
（3）The absolute ethyl alcohol of 10 weight powder is taken, ferrocene carboxaldehyde is added, stirring is completely dissolved to it, is configured to solution for standby；
（4）In remainder amount absolute ethyl alcohol input reaction vessel, polyethyleneimine is subsequently added into, stirring puts into after being completely dissolved to it
Pre- modified nano calcium carbonate powder, ultrasonic disperse 40min is then added dropwise ferrocene carboxaldehyde alcoholic solution, and addition continues anti-after finishing
2h is answered, then filtering, products therefrom is dried after washing, dispersion, obtains final product described modified nano calcium carbonate powder.
Obtained nano-calcium carbonate powder characteristic test result is：
Granularity D50：205nm；Viscosity：24.8mPa.s；Activation grade：100%；Oil factor：24.7；Settling volume：1.04ml/g.
Claims (2)
1. the nano-calcium carbonate powder of a kind of ferrocene-polyethyleneimine cross-linked polymer coating modification, it is characterised in that this is received
Rice calcium carbonate powder is made up of the raw material of following weight portion：Calcium oxide 10-20, carbon dioxide（Technical pure）In right amount, fluorocarbon surface
Activating agent 0.01-0.02, polyethyleneimine 2-3, ferrocene carboxaldehyde 0.5-1, silane coupler kh550 0.4-0.5, deionization
Water 100-200, absolute ethyl alcohol 50-80.
2. the nano-calcium carbonate calcium powder of a kind of ferrocene-polyethyleneimine cross-linked polymer coating modification as claimed in claim 1
The preparation method of body, it is characterised in that its preparation method is comprised the following steps：
（1）During deionized water, fluorocarbon surfactant first put into reaction vessel successively, stirring mixing 20- under nitrogen atmosphere
System is heated to 80-85 DEG C after 30min, calcium oxide is and then added, grinding stirring digestion 2-3h forms calcium hydroxide slurry
Material, it is standby after ageing 10-15h；
（2）Agitating device is opened, to step（1）Silane coupler kh550 is added dropwise in the slurries of preparation, starts to lead to after completion of dropping
Carbon dioxide, stops ventilation when stabilizing to neutrality to system pH, continue to stir hybrid reaction 40-50min, and reaction terminates
System filtering afterwards, filtrate is scrubbed, vacuum drying, dispersion, obtain pre- modified nano calcium carbonate powder standby；
（3）The absolute ethyl alcohol of 10-15 weight powder is taken, ferrocene carboxaldehyde is added, stirring is completely dissolved to it, is configured to solution standby
With；
（4）In remainder amount absolute ethyl alcohol input reaction vessel, polyethyleneimine is subsequently added into, stirring puts into after being completely dissolved to it
Pre- modified nano calcium carbonate powder, ultrasonic disperse 40-50min is then added dropwise ferrocene carboxaldehyde alcoholic solution, and addition continues after finishing
Reaction 2-3h, then filtering, products therefrom is dried after washing, dispersion, obtains final product described modified nano calcium carbonate powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610915011.1A CN106752098A (en) | 2016-10-20 | 2016-10-20 | A kind of nano-calcium carbonate powder of ferrocene polyethyleneimine cross-linked polymer coating modification and preparation method thereof |
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| CN201610915011.1A CN106752098A (en) | 2016-10-20 | 2016-10-20 | A kind of nano-calcium carbonate powder of ferrocene polyethyleneimine cross-linked polymer coating modification and preparation method thereof |
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| CN201610915011.1A Pending CN106752098A (en) | 2016-10-20 | 2016-10-20 | A kind of nano-calcium carbonate powder of ferrocene polyethyleneimine cross-linked polymer coating modification and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113247936A (en) * | 2021-06-25 | 2021-08-13 | 安徽前江超细粉末科技有限公司 | Method for reducing energy consumption in production of nano calcium carbonate |
| CN117431123A (en) * | 2023-10-30 | 2024-01-23 | 众联晟通(苏州)科技有限公司 | Engine oil nozzle cleaning agent and preparation method thereof |
| CN117701089A (en) * | 2024-02-02 | 2024-03-15 | 山东信泰节能科技股份有限公司 | Composite liquid granite coating with high heat insulation performance |
-
2016
- 2016-10-20 CN CN201610915011.1A patent/CN106752098A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113247936A (en) * | 2021-06-25 | 2021-08-13 | 安徽前江超细粉末科技有限公司 | Method for reducing energy consumption in production of nano calcium carbonate |
| CN117431123A (en) * | 2023-10-30 | 2024-01-23 | 众联晟通(苏州)科技有限公司 | Engine oil nozzle cleaning agent and preparation method thereof |
| CN117701089A (en) * | 2024-02-02 | 2024-03-15 | 山东信泰节能科技股份有限公司 | Composite liquid granite coating with high heat insulation performance |
| CN117701089B (en) * | 2024-02-02 | 2024-04-26 | 山东信泰节能科技股份有限公司 | Composite liquid granite coating with high heat insulation performance |
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