CN107345085A - A kind of preparation method of organic matrix filling Fe2O3 doping calcium carbonate - Google Patents
A kind of preparation method of organic matrix filling Fe2O3 doping calcium carbonate Download PDFInfo
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- CN107345085A CN107345085A CN201710600128.5A CN201710600128A CN107345085A CN 107345085 A CN107345085 A CN 107345085A CN 201710600128 A CN201710600128 A CN 201710600128A CN 107345085 A CN107345085 A CN 107345085A
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- Prior art keywords
- calcium carbonate
- fe2o3 doping
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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
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention discloses a kind of preparation method of organic matrix filling Fe2O3 doping calcium carbonate, the calcium carbonate of the present invention is particularly suitable for application as the packing material of polymer, it can be compatible well with polymer after surface organic is handled, its dispersiveness with polymer can be improved, effectively reduce reunion, improve the stability_intensity of calcium carbonate and polymer composites, the calcium carbonate of the present invention also passes through Fe2O3 doping, impart the preferable magnetic of calcium carbonate, its feature is enhanced, expands its use range.
Description
Technical field
The invention belongs to Material Field, and in particular to a kind of preparation method of organic matrix filling Fe2O3 doping calcium carbonate.
Background technology
Calcium carbonate is a kind of highly important functional inorganic filling, is widely used in plastics, rubber, coating and makes
The industrial circles such as paper.In the application field of calcium carbonate, most products belong to the category of polymer, such as plastics, rubber, gluing
Agent, coating etc., and occupy the important market share.Modifying agent serves important function to the performance of nano-calcium carbonate and application.
For example, the addition of dispersant can reduce the reunion of nano particle, dispersiveness is improved, the addition of surface modifier can improve nanometer
Compatibility of the calcium carbonate in polymeric system.The application of dispersant and surface modifier for nano-calcium carbonate as can be seen here is
It is vital.However, the addition of dispersant and surface modifier so that nano-calcium carbonate temperature is diminished significantly using window,
Reason is that conventional dispersant and coupling agent are easily decomposes at high temperature, bubble, cracking, defect, deformation etc. is caused, so as to influence
Outward appearance, heat resistance and the mechanical property of material；
More and more extensive with the application of composite, the effect of the raw material of traditional simple function is also constantly by composite
Substitution, it is well known that the function of calcium carbonate is a lot, also very extensive in the utilization of every field, but if being assigned magnetic,
Its use range, application number can be strengthened：A kind of 201510054453.7 magnetic of the nano-calcium carbonate of grafting and activating containing maleic anhydride
Also related in property polyethylene powder coating and preparation method thereof and assign calcium carbonate to magnetic, it is to carry out nano-calcium carbonate
Oxygen activation processing, and in its surface grafting maleic anhydride, then it is equal to impart material for the spherical ferroferric oxide magnetic powder of dopen Nano
Even magnetic, the thus invention is that modified nano-calcium carbonate is simply common with nanometer spherical ferroso-ferric oxide in fact
It is mixed, it is then added in polythene material, is and the purpose of the present invention in order to realize the dispersiveness in polythene material uniformly
It is the calcium carbonate material for preparing magnetic, is to be effectively combined calcium carbonate and magnetic material, stable composite is made, without
It is that simple blending is uniform；
Magnetic nano-particle not only has 4 basic effects possessed by common nano-particle, can also be with magnetic-particle material
Composition change and abnormal magnetic property is presented, such as superparamagnetism, high-coercive force, low Curie temperature and high magnetic susceptibility spy
Property.Preparing to solve magnetic material, particle coagulation, agglomeration easily occur during separation, post processing and storage,
Offspring is formed, particle diameter becomes big, etc. technical problem, needs to be modified the surface of magnetic nanoparticle, improve it
Dispersiveness, so as to apply obstacle efficiently against magnetic composite.
The content of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of organic matrix filling Fe2O3 doping
The preparation method of calcium carbonate.
To achieve the above object, the present invention uses following technical scheme：
A kind of preparation method of organic matrix filling Fe2O3 doping calcium carbonate, it is characterised in that comprise the following steps：
（1）Ferrocene is taken, is added in the deionized water of 40-50 times of its weight, adds trimethylolpropane, rise temperature is
50-60 DEG C, add to phenoxy benzoic acid, insulated and stirred 1-2 hours, filtering, precipitation is washed, air drying, obtains carboxylated
Iron；
（2）Calcium carbonate is taken, is added in the dichloromethane of 7-9 times of its weight, ultrasonic 3-5 minutes, adds triethylamine, stirring is equal
It is even, obtain calcium carbonate pre-dispersed liquid；
（3）Above-mentioned carboxylated iron is added in calcium carbonate pre-dispersed liquid, stirred, is passed through nitrogen, at room temperature stirring reaction
7-8 hours, solvent is distilled off, dries 2-3 hours at 50-60 DEG C of vacuum, obtains Fe2O3 doping amination calcium carbonate；
（4）Oleic acid is taken, is added in the deionized water of 70-100 times of its weight, stirs, adds above-mentioned Fe2O3 doping amination carbon
Sour calcium, rise temperature are 60-70 DEG C, insulated and stirred 3-5 hours, filtering, precipitation are washed, air drying, produced described organic
Fe2O3 doping calcium carbonate is used in matrix filling；
Described ferrocene, trimethylolpropane, it is 4- to the weight ratio of phenoxy benzoic acid, calcium carbonate, triethylamine, oleic acid
7:1-2:3-5:70-80:3-4:1-2。
Advantages of the present invention：
Calcium carbonate is modified by the present invention by triethylamine, with carboxylated iron blended cross linking, obtains Fe2O3 doping amination calcium carbonate, Ran Houtong
Oleic acid processing is crossed, obtains the Fe2O3 doping calcium carbonate of surface organic；
The calcium carbonate of the present invention is particularly suitable for application as the packing material of polymer, and it can be with after surface organic is handled
Polymer is compatible well, it is possible to increase its dispersiveness with polymer, effectively reduces reunion, improves calcium carbonate and polymer
The stability_intensity of composite, calcium carbonate of the invention also by Fe2O3 doping, impart the preferable magnetic of calcium carbonate, enhanced
Its feature, expand its use range.
Embodiment
Embodiment 1
A kind of organic matrix filling preparation method of Fe2O3 doping calcium carbonate, comprises the following steps：
（1）Ferrocene is taken, is added in the deionized water of 40 times of its weight, adds trimethylolpropane, rise temperature is 60 DEG C,
Add to phenoxy benzoic acid, insulated and stirred 1 hour, filtering, precipitation is washed, air drying, obtains carboxylated iron；
（2）Calcium carbonate is taken, is added in the dichloromethane of 7 times of its weight, ultrasound 3 minutes, triethylamine is added, stirs,
Obtain calcium carbonate pre-dispersed liquid；
（3）Above-mentioned carboxylated iron is added in calcium carbonate pre-dispersed liquid, stirred, is passed through nitrogen, at room temperature stirring reaction 7
Hour, solvent is distilled off, is dried 2 hours at 60 DEG C of vacuum, obtains Fe2O3 doping amination calcium carbonate；
（4）Oleic acid is taken, is added in the deionized water of 100 times of its weight, stirs, adds above-mentioned Fe2O3 doping amination carbonic acid
Calcium, rise temperature are 60 DEG C, insulated and stirred 5 hours, filtering, precipitation are washed, air drying, produce the organic matrix filling
With Fe2O3 doping calcium carbonate；
Described ferrocene, trimethylolpropane, the weight ratio to phenoxy benzoic acid, calcium carbonate, triethylamine, oleic acid are 4:
1:5:80:3：1.
Claims (1)
1. a kind of preparation method of organic matrix filling Fe2O3 doping calcium carbonate, it is characterised in that comprise the following steps：
（1）Ferrocene is taken, is added in the deionized water of 40-50 times of its weight, adds trimethylolpropane, rise temperature is
50-60 DEG C, add to phenoxy benzoic acid, insulated and stirred 1-2 hours, filtering, precipitation is washed, air drying, obtains carboxylated
Iron；
（2）Calcium carbonate is taken, is added in the dichloromethane of 7-9 times of its weight, ultrasonic 3-5 minutes, adds triethylamine, stirring is equal
It is even, obtain calcium carbonate pre-dispersed liquid；
（3）Above-mentioned carboxylated iron is added in calcium carbonate pre-dispersed liquid, stirred, is passed through nitrogen, at room temperature stirring reaction
7-8 hours, solvent is distilled off, dries 2-3 hours at 50-60 DEG C of vacuum, obtains Fe2O3 doping amination calcium carbonate；
（4）Oleic acid is taken, is added in the deionized water of 70-100 times of its weight, stirs, adds above-mentioned Fe2O3 doping amination carbon
Sour calcium, rise temperature are 60-70 DEG C, insulated and stirred 3-5 hours, filtering, precipitation are washed, air drying, produced described organic
Fe2O3 doping calcium carbonate is used in matrix filling；
Described ferrocene, trimethylolpropane, it is 4- to the weight ratio of phenoxy benzoic acid, calcium carbonate, triethylamine, oleic acid
7:1-2:3-5:70-80:3-4:1-2。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710600128.5A CN107345085A (en) | 2017-07-21 | 2017-07-21 | A kind of preparation method of organic matrix filling Fe2O3 doping calcium carbonate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710600128.5A CN107345085A (en) | 2017-07-21 | 2017-07-21 | A kind of preparation method of organic matrix filling Fe2O3 doping calcium carbonate |
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| CN107345085A true CN107345085A (en) | 2017-11-14 |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104559327A (en) * | 2015-01-27 | 2015-04-29 | 华东理工大学 | Surface modified nano calcium carbonate with core-shell structure and preparation method thereof |
| CN104629519A (en) * | 2015-02-02 | 2015-05-20 | 芜湖市宝艺游乐科技设备有限公司 | Magnetic polyethylene powder coating containing maleic anhydride grafted activated nano calcium carbonate and preparation method of polyethylene powder coating |
| CN106590048A (en) * | 2016-10-20 | 2017-04-26 | 青阳县永诚钙业有限责任公司 | Nano-titanium-dioxide-coated modified calcium carbonate powder and preparation method thereof |
-
2017
- 2017-07-21 CN CN201710600128.5A patent/CN107345085A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104559327A (en) * | 2015-01-27 | 2015-04-29 | 华东理工大学 | Surface modified nano calcium carbonate with core-shell structure and preparation method thereof |
| CN104629519A (en) * | 2015-02-02 | 2015-05-20 | 芜湖市宝艺游乐科技设备有限公司 | Magnetic polyethylene powder coating containing maleic anhydride grafted activated nano calcium carbonate and preparation method of polyethylene powder coating |
| CN106590048A (en) * | 2016-10-20 | 2017-04-26 | 青阳县永诚钙业有限责任公司 | Nano-titanium-dioxide-coated modified calcium carbonate powder and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 陶晓敏 等: ""二茂铁酰胺类金属有机三阶非线性光学材料的合成"", 《功能材料》 * |
| 高敬民: ""纳米SiO2改性核壳型氟碳乳液的制备及水性绿色涂料的性能研究"", 《中国优秀硕士学位论文全文数据库（工程科技I辑）》 * |
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Application publication date: 20171114 |