CN111171378A - Preparation method and application of carbon nano composite ferrosilicon powder - Google Patents
Preparation method and application of carbon nano composite ferrosilicon powder Download PDFInfo
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- CN111171378A CN111171378A CN202010102897.4A CN202010102897A CN111171378A CN 111171378 A CN111171378 A CN 111171378A CN 202010102897 A CN202010102897 A CN 202010102897A CN 111171378 A CN111171378 A CN 111171378A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
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- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C08K7/00—Use of ingredients characterised by shape
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2327/06—Homopolymers or copolymers of vinyl chloride
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2497/00—Characterised by the use of lignin-containing materials
- C08J2497/02—Lignocellulosic material, e.g. wood, straw or bagasse
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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Abstract
The invention discloses a preparation method and application of carbon nano composite ferrosilicon powder, wherein a chemical grafting method is adopted for processing the combination of nano materials such as carbon nano and the like and the ferrosilicon powder, so that the problems of difficult dispersion, easy agglomeration and poor long-term storage stability of the nano materials are effectively solved. The product obtained by the invention has bending strength, surface hardness and Vicat softening point which are basically superior to those of the traditional material under the approximate density.
Description
Technical Field
The invention relates to the technical field of modification of polymer composite materials, in particular to a preparation method and application of carbon nano composite ferrosilicon powder.
Background
Graphene is a polymer made of carbon atoms in sp2The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial. The ferrosilicon powder is an alkaline silicon-rich substance, the components of SiO2, CaO, MgO, FeO and the like contained in the ferrosilicon powder have a reinforcing effect, and the porous structure of the ferrosilicon powder has good adsorption performance. The nano material has the defects of difficult dispersion and easy agglomeration and has unstable long-term storage performance.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a preparation method and application of carbon nano composite ferrosilicon powder, which aims to solve the problems of difficult dispersion and easy agglomeration of carbon nano materials and long-term storage stability inspection.
In order to solve the technical problem, the invention discloses a preparation method of carbon nano composite ferrosilicon powder, which comprises the following steps:
mixing a carbon nano material and deionized water according to a mass ratio of 0.1-2: 100, adding a wetting dispersant with a mass ratio of 0.5-1%, and performing ultrasonic dispersion for 20-30 min in an ultrasonic dispersion mode;
taking ferrosilicon powder and neutralizing alkaline substances in the ferrosilicon powder;
step three, adding the ferrosilicon powder prepared in the step two into the mixture prepared in the step one;
step four, adding a coupling agent with the mass ratio of 0.2-0.8%, and stirring for 30-50 min at the temperature of 80-100 ℃;
and step five, carrying out water washing, suction filtration, drying and crushing treatment.
Further, the carbon nano material is graphene oxide, carbon nano tube or fullerene.
Further, in the step one, the wetting dispersant is any one or a mixture of a plurality of polyoxyethylene fatty acid ester, polyoxyethylene alkyl phenyl ether and polyoxyethylene succinate.
Further, the second step is to mix the ferrosilicon powder and the acid solution according to the mass ratio of 1-2: 1, and stir for 10-20 min at the temperature of 20-30 ℃.
Further, the stirred mixture was subjected to suction filtration.
Further, the acid solution is hydrochloric acid, sulfuric acid or nitric acid, and the pH value of the acid solution is 5.5-6.5.
Further, the coupling agent is a silane coupling agent.
Further, the coupling agent is vinyl silane, amino silane, epoxy silane, mercapto silane or methacryloxy silane.
Further, the single-layer rate of the graphene oxide is more than or equal to 80%.
The invention also discloses an application of the graphene composite ferrosilicon powder, which is prepared from the following components in parts by weight: 60-80 parts of polyvinyl chloride resin, 5-10 parts of natural bamboo fiber, 0.5-3 parts of cellulose nanocrystal, 0.5-3 parts of oxide nanocrystal, 0.5-3 parts of modified graphene oxide, 10-20 parts of carbon nano composite ferrosilicon powder, 3-10 parts of light calcium carbonate, 1-5 parts of calcium-zinc composite stabilizer, 0.3-5 parts of foaming agent, 0.1-0.3 part of accelerator and 1-5 parts of thermally reversible cross-linking agent.
Compared with the prior art, the invention can obtain the following technical effects:
(1) the surface of the ferrosilicon powder is activated by adopting a coupling agent, so that the ferrosilicon powder is effectively combined with graphene oxide, and the problems that the graphene nano material is difficult to disperse, easy to agglomerate and poor in long-term storage stability are solved.
(2) The carbon nano tube with the one-dimensional structure, the graphene with the two-dimensional structure and the fullerene with the three-dimensional structure are adopted to be compounded simultaneously, so that the toughness of a polymer finished product is not influenced when the filler is added in a large amount during the processing of the polymer, and the adding range is wide.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example one
A preparation method of carbon nano composite ferrosilicon powder comprises the following steps:
mixing graphene oxide with a monolayer rate of 80% and deionized water according to a mass ratio of 0.1:100, adding a wetting dispersant with a mass ratio of 0.5%, and performing ultrasonic dispersion for 20min in an ultrasonic dispersion manner;
neutralizing alkaline substances in the ferrosilicon powder;
step three, adding the ferrosilicon powder prepared in the step two into the mixture prepared in the step one;
step four, adding a coupling agent with the mass ratio of 0.2%, and stirring for 30min at the temperature of 80 ℃;
and step five, carrying out water washing, suction filtration, drying and crushing treatment.
Wherein the coupling agent is vinyl silane.
Example two
A preparation method of graphene composite ferrosilicon powder comprises the following steps:
mixing graphene oxide with a monolayer rate of 85% with deionized water according to a mass ratio of 2:100, adding a wetting dispersant with a mass ratio of 1%, and performing ultrasonic dispersion for 30min in an ultrasonic dispersion manner;
neutralizing alkaline substances in the ferrosilicon powder;
step three, adding the ferrosilicon powder prepared in the step two into the mixture prepared in the step one;
step four, adding a coupling agent with the mass ratio of 0.8%, and stirring for 50min at the temperature of 100 ℃;
and step five, carrying out water washing, suction filtration, drying and crushing treatment.
The coupling agent is aminosilane.
EXAMPLE III
A preparation method of graphene composite ferrosilicon powder comprises the following steps:
step one, mixing graphene oxide with a monolayer rate of 93% with deionized water according to a mass ratio of 1:100, adding a wetting dispersant with a mass ratio of 0.73%, and performing ultrasonic dispersion for 25min in an ultrasonic dispersion mode;
neutralizing alkaline substances in the ferrosilicon powder;
step three, adding the ferrosilicon powder prepared in the step two into the mixture prepared in the step one;
step four, adding a coupling agent with the mass ratio of 0.65%, and stirring for 38min at the temperature of 86 ℃;
and step five, carrying out water washing, suction filtration, drying and crushing treatment.
The coupling agent is epoxy silane.
Example four
The difference from the first embodiment is that: the carbon nano tube replaces graphene oxide.
EXAMPLE five
The difference from the first embodiment is that: the fullerene replaces the graphene oxide.
EXAMPLE six
In example 1, the wetting dispersant is polyoxyethylene fatty acid ester, the ferrosilicon powder and hydrochloric acid are mixed according to the mass ratio of 1:1, the pH value of the hydrochloric acid is 5.5, and the mixture is stirred for 10min at the temperature of 20 ℃. And performing suction filtration treatment on the stirred mixture.
In addition: the coupling agent is mercaptosilane.
EXAMPLE seven
In example 1, the wetting dispersant is polyoxyethylene alkyl phenyl ether, the ferrosilicon powder and sulfuric acid are mixed according to the mass ratio of 2:1, the pH value of the sulfuric acid is 6.5, and the mixture is stirred for 20min at the temperature of 30 ℃. And performing suction filtration treatment on the stirred mixture.
In addition: the coupling agent is methacryloxy silane.
Example eight
In example 1, the wetting dispersant is polyoxyethylene succinate, the ferrosilicon powder and nitric acid are mixed according to the mass ratio of 1.5:1, the pH value of the nitric acid is 5.9, and the mixture is stirred for 16min at the temperature of 26.5 ℃. And performing suction filtration treatment on the stirred mixture.
Example nine
60 parts of polyvinyl chloride resin, 5 parts of natural bamboo fiber, 0.5 part of cellulose nanocrystal, 0.5 part of oxide nanocrystal, 1 part of modified graphene oxide, 20 parts of graphene composite ferrosilicon powder, 5 parts of light calcium carbonate, 3 parts of calcium-zinc composite stabilizer, 0.3 part of foaming agent, 0.1 part of accelerator and 2 parts of thermoreversible crosslinking agent.
The preparation process comprises the following steps:
carrying out surface treatment on natural bamboo fibers;
banburying cellulose nanocrystals, oxide nanocrystals, modified graphene oxide and graphene composite ferrosilicon powder;
polyvinyl chloride, natural bamboo fiber with treated surface, light calcium carbonate, calcium-zinc composite stabilizer, foaming agent, accelerant and thermal reversible cross-linking agent are put into a high-speed mixer to be mixed for 30 minutes, then the mixture enters a double screw extruder to be extruded at 130 ℃ to be mixed, extruded and foamed, and the mixture is cooled and shaped by a die.
Example ten
70 parts of polyvinyl chloride resin, 10 parts of natural bamboo fiber, 1 part of cellulose nanocrystal, 0.5 part of oxide nanocrystal, 2 parts of modified graphene oxide, 10 parts of graphene composite ferrosilicon powder, 3 parts of light calcium carbonate, 1 part of calcium-zinc composite stabilizer, 1 part of foaming agent, 0.1 part of accelerator and 2 parts of thermoreversible crosslinking agent.
The preparation process comprises the following steps:
carrying out surface treatment on natural bamboo fibers;
banburying cellulose nanocrystals, oxide nanocrystals, modified graphene oxide and graphene composite ferrosilicon powder;
putting polyvinyl chloride, natural bamboo fiber with treated surface, light calcium carbonate, calcium-zinc composite stabilizer, foaming agent, accelerant and thermal reversible cross-linking agent into a high-speed mixer for mixing for 26 minutes, then putting the mixture into a double screw extruder for extruding at 180 ℃ for mixing, extruding and foaming, and cooling and shaping the mixture by a die.
EXAMPLE eleven
80 parts of polyvinyl chloride resin, 8 parts of natural bamboo fiber, 2 parts of cellulose nanocrystalline, 1 part of oxide nanocrystalline, 0.5 part of modified graphene oxide, 20 parts of graphene composite ferrosilicon powder, 3 parts of light calcium carbonate, 2 parts of calcium-zinc composite stabilizer, 1 part of foaming agent, 0.12 part of accelerator and 1 part of thermoreversible crosslinking agent.
The preparation process comprises the following steps:
carrying out surface treatment on natural bamboo fibers;
banburying cellulose nanocrystals, oxide nanocrystals, modified graphene oxide and graphene composite ferrosilicon powder;
putting polyvinyl chloride, natural bamboo fiber with treated surface, light calcium carbonate, calcium-zinc composite stabilizer, foaming agent, accelerant and thermal reversible cross-linking agent into a high-speed mixer for mixing for 35 minutes, then carrying out double-screw extrusion at 163 ℃ for mixing, extruding and foaming, and cooling and shaping through a die.
The conventional material was compared to the material prepared in example nine, example ten and example eleven with the following properties:
from the above table, it can be seen that the bending strength, surface hardness and vicat softening point of the product obtained by the present invention are substantially superior to those of the conventional material at the similar density.
The beneficial technical effects of the invention are as follows:
(1) the surface of the ferrosilicon powder is activated by adopting a coupling agent, so that the ferrosilicon powder is effectively combined with graphene oxide, and the problems that the graphene nano material is difficult to disperse, easy to agglomerate and poor in long-term storage stability are solved.
(2) The carbon nano tube with the one-dimensional structure, the graphene with the two-dimensional structure and the fullerene with the three-dimensional structure are adopted to be compounded simultaneously, so that the toughness of a polymer finished product is not influenced when the filler is added in a large amount during the processing of the polymer, and the adding range is wide.
Claims (10)
1. A preparation method of carbon nano composite ferrosilicon powder is characterized by comprising the following steps:
mixing a carbon nano material and deionized water according to a mass ratio of 0.1-2: 100, adding a wetting dispersant with a mass ratio of 0.5-1%, and performing ultrasonic dispersion for 20-30 min in an ultrasonic dispersion mode;
taking ferrosilicon powder and neutralizing alkaline substances in the ferrosilicon powder;
step three, adding the ferrosilicon powder prepared in the step two into the mixture prepared in the step one;
step four, adding a coupling agent with the mass ratio of 0.2-0.8%, and stirring for 30-50 min at the temperature of 80-100 ℃;
and step five, carrying out water washing, suction filtration, drying and crushing treatment.
2. The method for preparing carbon nano composite ferrosilicon powder according to claim 1, wherein the method comprises the following steps: the carbon nano material is graphene oxide, a carbon nano tube or fullerene.
3. The method for preparing carbon nano composite ferrosilicon powder according to claim 1, wherein the method comprises the following steps: in the step one, the wetting dispersant is any one or a mixture of more of polyoxyethylene fatty acid ester, polyoxyethylene alkyl phenyl ether and polyoxyethylene succinate.
4. The method for preparing carbon nano composite ferrosilicon powder according to claim 1, wherein the method comprises the following steps: and step two, specifically, mixing the ferrosilicon powder and the acid solution according to the mass ratio of 1-2: 1, and stirring for 10-20 min at the temperature of 20-30 ℃.
5. The method for preparing carbon nano composite ferrosilicon powder according to claim 4, wherein the method comprises the following steps: and performing suction filtration treatment on the stirred mixture.
6. The method for preparing carbon nano composite ferrosilicon powder according to claim 4, wherein the method comprises the following steps: the acid solution is hydrochloric acid, sulfuric acid or nitric acid, and the pH value of the acid solution is 5.5-6.5.
7. The method for preparing carbon nano composite ferrosilicon powder according to claim 1, wherein the method comprises the following steps: the coupling agent is a silane coupling agent.
8. The method for preparing carbon nano composite ferrosilicon powder according to claim 7, wherein the method comprises the following steps: the coupling agent is vinyl silane, amino silane, epoxy silane, mercapto silane or methacryloxy silane.
9. The method for preparing carbon nano composite ferrosilicon powder according to claim 2, wherein the method comprises the following steps: the single-layer rate of the graphene oxide is more than or equal to 80%.
10. Use of the carbon nanocomposite ferrosilicon powder of any one of claims 1 to 9, wherein: the preparation is carried out according to the following weight: 60-80 parts of polyvinyl chloride resin, 5-10 parts of natural bamboo fiber, 0.5-3 parts of cellulose nanocrystal, 0.5-3 parts of oxide nanocrystal, 0.5-3 parts of modified graphene oxide, 10-20 parts of carbon nano composite ferrosilicon powder, 3-10 parts of light calcium carbonate, 1-5 parts of calcium-zinc composite stabilizer, 0.3-5 parts of foaming agent, 0.1-0.3 part of accelerator and 1-5 parts of thermally reversible cross-linking agent.
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2020
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| WO2020221987A1 (en) * | 2019-04-30 | 2020-11-05 | !Obac Limited | Heated floor or wall coating system |
| CN110041644A (en) * | 2019-05-08 | 2019-07-23 | 上海擎木新材料科技有限公司 | The multiple dimensioned composite filled thermal reversion crosslinked PVC material of one kind and preparation method |
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