CN113603987B - Modified aluminum/fluorine-containing polymer compound and preparation method thereof - Google Patents
Modified aluminum/fluorine-containing polymer compound and preparation method thereof Download PDFInfo
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- CN113603987B CN113603987B CN202110859199.3A CN202110859199A CN113603987B CN 113603987 B CN113603987 B CN 113603987B CN 202110859199 A CN202110859199 A CN 202110859199A CN 113603987 B CN113603987 B CN 113603987B
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- 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
- C08J2327/12—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 fluorine atoms
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Abstract
The invention discloses a modified aluminum/fluorine-containing polymer compound, which consists of modified aluminum powder and a fluorine-containing polymer. Wherein the aluminum powder has a size of 50 nm-5 μm, a weight ratio of 90-70%, and a fluorine-containing polymer weight ratio of 10-30%. The invention can be used as a simple and effective criterion for the compatibility of the aluminum powder modified layer and the high molecular polymer and as a criterion for the adaptation of the explosive granulation process. And meanwhile, reference is provided for the design of the aluminum powder reactive material. The process is simple and easy to operate.
Description
Technical Field
The invention belongs to the field of energetic material composites, and particularly relates to a modified aluminum/fluorine-containing polymer composite for simply judging the compatibility of an aluminum powder surface modification layer and a fluorine-containing polymer and a preparation method thereof.
Background
The aluminum powder is added into the high-energy explosive due to high density and high combustion enthalpy, so that the reaction rate, detonation heat and other detonation properties of the mixed explosive are improved. The aluminum powder is coated by inorganic matters or organic matters, so that the dispersion and storage of the aluminum powder can be effectively improved, and the surface is prevented from being further oxidized. However, the coating layers are at the cost of sacrificing the energy density of the system, and no energy is contributed in the combustion and explosion process of the system, and researches show that fluorine is used as an oxidizing agent to replace oxygen to react with aluminum to generate AlF 3 The reaction can give off 13.31kcal/g of heat to generate Al 2 O 3 The exothermic heat of reaction was only 7.4 kcal/g. The mixture of fluoride and aluminum powder has been widely used as a high energy density material in nano thermite and reactive materials (mat. sci.2007,25, 95). Therefore, in the invention, GAP or PVDF is used for surface modification of aluminum powder, so that the nano-particles can be effectively passivatedThe aluminum powder and the coating layer can contribute energy to an energy-containing system and improve the reaction and energy release rate.
The aluminum-containing explosive is a multi-phase mixed material and comprises components such as a main explosive, aluminum powder, an adhesive and the like, so that in such a complex multi-interface system, the interface compatibility among the components has an important influence on the interface property of the composite material, and further the mechanical strength of the formed explosive column is changed. The interface work is calculated by utilizing the test contact angle, and the method is a common method for judging the interface compatibility of the components of the composite material. He et al performed Polydopamine (PDA) coating on the surface of main explosive TATB, and the compatibility of the explosive and fluoropolymer was characterized by measuring the contact angle between fluoropolymer solution and the grain and calculating the interfacial energy (j. mater. chem. a,2017, 5, 13499). Zeng et al tabletted fluoropolymers, tested the contact angles of water and diiodomethane on their surfaces, and calculated the corresponding interfacial work; the comparison of the values of the interfacial work shows that the TATB surface is subjected to grafting modification and then has the strongest interfacial action with the fluoropolymer, and a criterion is provided for mechanical enhancement (Polymers,2019,11, 1308). However, in testing the contact angle of compressed tablets, the interfacial contact angle obtained is not accurate due to the crushing of the particles by pressure, which makes the surface properties different from those of the particles before compression, and it is difficult to fully reflect the interfacial properties of the particles of the composite material. For direct testing of the contact angle of the Powder, there are currently two major types, Column wrapping or Washburn capitelliry rise (Powder Technology 2016,287,201). The two methods can only test the surface wetting condition of different solutions to the powder, cannot reflect the interfacial action condition of the polymer component and the polymer component, and even if the high polymer is dissolved to prepare the solution, the solvent exists and causes errors.
Bear lib et al disclose a method of chemical plating on the surface of a chemical polymer film to improve the surface energy of the polymer, but this approach is difficult to extend into the binder of energetic materials (CN 109576683A). The invention provides a method for chemical modification of the surface of aluminum powder, which can be used for preparing a mixed explosive in water and provides a support for preparing a fluorine-containing compound (ZL 201610478426.7).
Disclosure of Invention
The invention discloses a modified aluminum/fluorine-containing polymer compound and a preparation method thereof, aiming at the problem that the interfacial compatibility of components in an aluminum-containing explosive and a binder is difficult to visually characterize. The solvent is volatilized under the action of hot water and vacuum to form a film, the modified aluminum/fluorine-containing polymer compound is obtained, and the result of interfacial compatibility between the two is visually observed through an electron microscope. The method is expected to be widened to the range between other modified fine particles and high polymers, and provides a preliminary judgment basis for the interface matching of the components in the mixed material; the film prepared at the same time may provide a reference for the design of the aluminum powder reactive material.
In order to realize the purpose of the invention, the invention provides the following technical scheme:
a modified aluminum/fluorine-containing polymer compound comprises surface modified aluminum powder and fluorine-containing polymer, wherein the selected surface modified aluminum powder is spherical particle aluminum powder with the average size of 50 nm-5 mu m; the selected fluorine-containing polymer is a copolymer of vinylidene fluoride and chlorotrifluoroethylene; wherein the weight ratio of the aluminum powder is 90-70%, and the weight ratio of the fluorine-containing polymer is 10-30%.
The invention also discloses a preparation method of the modified aluminum/fluorine-containing polymer compound, which comprises the following steps: dispersing 90-70 wt% of modified aluminum powder in an organic solvent A, and performing ultrasonic treatment to form a suspension; dispersing 10-30 wt% of fluorine-containing polymer in the other part of organic solvent A, and magnetically stirring; mixing the above two materials, and stirring; and (3) dropwise adding the mixed solution on the surface of deionized water at a certain temperature, simultaneously carrying out vacuum treatment until the solvent is completely volatilized, forming a film by using the liquid drops, taking out and drying to obtain the modified aluminum/fluorine-containing polymer compound.
To successfully prepare the modified aluminum/fluorine-containing polymer composite, the following points need to be noted:
the ultrasonic time of the modified aluminum powder is controlled within 3min, so that the modified aluminum powder is fully dispersed, and a modified layer is not damaged as much as possible; preparing a binder mixed solution with a certain concentration by the fluorine-containing polymer before taking the fluorine-containing polymer, wherein the selected solvent is required to be consistent with a subsequent dispersion solvent A; during liquid taking, the mixed liquid is kept in a stirring state all the time, so that the aluminum powder is prevented from settling; controlling the liquid taking to be once for two drops as far as possible, and simultaneously paying attention to the fact that the vacuum is not too close to the water surface to prevent the liquid surface from being damaged; after the solvent is completely volatilized, the filter paper is cut into a certain angle or the film is taken by the silicon wafer, and after the film is dried in vacuum, the film can be separated from the filter paper.
In some embodiments, the aluminum powder surface modification layer is one of polyaziridine glycidyl ether (GAP), polyvinylidene fluoride (PVDF).
In some embodiments, the organic solvent a is one of ethyl acetate and butyl acetate.
In some embodiments, the ultrasound frequency is between 30kHz and 100 kHz.
In some embodiments, the temperature is 50-70 ℃.
In some embodiments, the magnetic stirring speed is 200rpm to 600rpm and the vacuum is 40mbar to 100 mbar.
Compared with the prior art, the invention has the beneficial effects that:
the modified aluminum/fluorine-containing polymer composite obtained by the invention is used as a means for preliminarily judging the interface compatibility of the two. The direct observation can be carried out through an electron microscope photo, if the interface interaction of the aluminum powder and the fluorine polymer film is strong, each aluminum powder particle is uniformly dispersed in the fluorine polymer film, and the contact area of the aluminum powder and the fluorine polymer film is increased; if the interface compatibility of the two is poor, the aluminum powder is agglomerated, and the aluminum powder on the surface of the fluoropolymer can be less.
Drawings
For a clearer explanation of the embodiments or technical solutions in the prior art of the present application, the drawings used in the description of the embodiments or prior art will be briefly described below, it is obvious that the drawings in the following description are only references to some embodiments in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a flow chart of the preparation of a modified aluminum/fluoropolymer composite according to the present invention;
FIG. 2 is an electron microscope image of the modified aluminum/fluorine-containing polymer composite of example 1 of the present invention;
FIG. 3 is an electron microscope image of modified aluminum/fluorine-containing polymer composite in example 3 of the present invention;
FIG. 4 is an electron micrograph of a modified aluminum/fluoropolymer composite according to example 5 of the present invention.
Detailed Description
The present invention will be further described with reference to the following examples, which are intended to illustrate only some, but not all, of the embodiments of the present invention. Based on the embodiments of the present invention, other embodiments used by those skilled in the art without any creative effort belong to the protection scope of the present invention.
Example 1
As shown in figure 1, 0.18g of modified aluminum powder with the average diameter of 50nm (the modified layer is GAP) is ultrasonically dispersed in 10ml of butyl acetate for 3 min; 0.5g of fluoropolymer binder A (the concentration is 4%, actually 0.02g) is added into 10ml of butyl acetate, and the mixture is magnetically stirred at the rotating speed of 200 rpm; pouring the aluminum powder suspension into the fluoropolymer solution, and keeping magnetic stirring at the rotating speed of 300 rpm; and (3) dropwise adding about 1ml of mixed solution on the surface of deionized water at 70 ℃, carrying out vacuum treatment at 40mbar until the solvent is completely volatilized, taking out the film by using clean filter paper, and drying at 60 ℃ in vacuum to obtain the modified aluminum/fluorine-containing polymer compound with the weight ratio of 9: 1.
Example 2
As shown in figure 1, 0.16g of modified aluminum powder with the average diameter of 200nm (the modified layer is GAP) is ultrasonically dispersed in 10ml of butyl acetate for 2 min; 1g of fluoropolymer adhesive A (the concentration is 4 percent, actually 0.04g) is added into 10ml of butyl acetate and stirred by magnetic force, and the rotating speed is 300 rpm; pouring the aluminum powder suspension into the fluoropolymer solution, and keeping magnetic stirring at the rotating speed of 500 rpm; and (3) dropwise adding about 1ml of mixed solution on the surface of deionized water at 70 ℃, carrying out vacuum treatment at 60mbar until the solvent is completely volatilized, taking out the film by using clean filter paper, and drying at 60 ℃ in vacuum to obtain the modified aluminum/fluorine-containing polymer compound with the weight ratio of 8: 2.
Example 3
As shown in fig. 1, 0.14g of modified aluminum powder with an average diameter of 3 μm (the modified layer is GAP) is ultrasonically dispersed in 10ml of butyl acetate for 1 min; adding 1.5g of fluoropolymer adhesive A (the concentration is 4 percent, actually 0.04g) into 10ml of butyl acetate, and magnetically stirring at the rotating speed of 300 rpm; pouring the aluminum powder suspension into the fluoropolymer solution, and keeping magnetic stirring at the rotating speed of 600 rpm; and (3) dropwise adding about 1ml of mixed solution on the surface of deionized water at 70 ℃, carrying out vacuum treatment at 100mbar until the solvent is completely volatilized, taking out the film by using clean filter paper, and drying at 60 ℃ in vacuum to obtain the modified aluminum/fluorine-containing polymer compound with the weight ratio of 7: 1.
Example 4
As shown in figure 1, 0.18g of modified aluminum powder with the average diameter of 50nm (the modified layer is GAP) is ultrasonically dispersed in 10ml of ethyl acetate for 3 min; adding 0.5g of fluoropolymer binder B (the concentration is 4 percent, and the actual concentration is 0.02g) into 10ml of ethyl acetate, and magnetically stirring at the rotating speed of 200 rpm; pouring the aluminum powder suspension into the fluoropolymer solution, and keeping magnetic stirring at the rotating speed of 400 rpm; and (3) dropwise adding about 1ml of mixed solution on the surface of deionized water at 60 ℃, carrying out vacuum treatment at 40mbar until the solvent is completely volatilized, taking out the film by using clean filter paper, and drying at 60 ℃ in vacuum to obtain the modified aluminum/fluorine-containing polymer compound with the weight ratio of 9: 1.
Example 5
Example 5 is a blank control with aluminum powder as the raw material without surface modification.
Taking 0.16g of raw material aluminum powder with the average diameter of 50nm to be ultrasonically dispersed in 10ml of butyl acetate for 1 min; 1g of fluoropolymer adhesive A (the concentration is 4 percent, actually 0.04g) is added into 10ml of butyl acetate, and the mixture is magnetically stirred at the rotating speed of 200 rpm; pouring the aluminum powder suspension into the fluoropolymer solution, and keeping magnetic stirring at the rotating speed of 350 rpm; and (3) dropwise adding about 1ml of mixed solution on the surface of deionized water at 70 ℃, carrying out vacuum treatment at 70mbar until the solvent is completely volatilized, taking out the film by using clean filter paper, and drying at 60 ℃ in vacuum to obtain the modified aluminum/fluorine-containing polymer compound with the weight ratio of 8: 2.
As can be seen from comparison of electron microscope photographs, in the examples 1 to 4, the aluminum powder subjected to surface modification treatment can be well dispersed on the surface of the fluoropolymer film, and the size of the aluminum powder has little influence on the uniformity of the composite, as shown in FIGS. 2 to 3; in example 5, the mixed solution is difficult to volatilize to form a complete film without surface modification during the preparation process, and the film has many holes mainly due to poor interface compatibility between the raw aluminum powder and the fluoropolymer, as shown in fig. 4. Therefore, the modified aluminum/fluorine polymer film prepared by the method has reference significance for preliminarily judging the interfacial compatibility of the aluminum powder and the high-molecular binder in the aluminum-containing explosive.
Although the invention has been described herein with reference to the illustrated embodiments thereof, which are intended to be the only preferred embodiments of the invention, it is not intended that the invention be limited thereto, since many other modifications and embodiments will be apparent to those skilled in the art and will be within the spirit and scope of the principles of this disclosure.
Claims (2)
1. A modified aluminum/fluorine-containing polymer compound is characterized in that: the paint comprises surface modified aluminum powder and a fluorine-containing polymer, wherein the selected surface modified aluminum powder is spherical particle aluminum powder with the average size of 50 nm-5 mu m; the selected fluorine-containing polymer is a copolymer of vinylidene fluoride and chlorotrifluoroethylene; wherein the weight ratio of the aluminum powder is 90-70%, and the weight ratio of the fluorine-containing polymer is 10-30%; the preparation method comprises the following steps:
dispersing 90-70 wt% of modified aluminum powder in an organic solvent A, and performing ultrasonic treatment to form a suspension, wherein the ultrasonic treatment time is controlled within 3 min; dispersing 10-30 wt% of a fluorine-containing polymer in another part of the organic solvent A, and magnetically stirring; mixing the above two materials, and stirring; dropwise adding the mixed solution on the surface of deionized water at the temperature of 50-70 ℃, simultaneously performing vacuum treatment until the solvent is completely volatilized, forming a film by liquid drops, taking out and drying to obtain a modified aluminum/fluorine-containing polymer compound; wherein the aluminum powder surface modification layer is one of polyaziridine glycidyl ether (GAP) and polyvinylidene fluoride (PVDF); the organic solvent A is one of ethyl acetate and butyl acetate; the ultrasonic frequency is 30 kHz-100 kHz; the magnetic stirring speed is 200rpm to 600rpm, and the vacuum degree is 40mbar to 100 mbar.
2. A preparation method of a modified aluminum/fluorine-containing polymer compound is characterized by comprising the following steps: the method comprises the following steps: dispersing 90-70 wt% of modified aluminum powder in an organic solvent A, and performing ultrasonic treatment to form a suspension, wherein the ultrasonic treatment time is controlled within 3 min; dispersing 10-30 wt% of a fluorine-containing polymer in another part of the organic solvent A, and magnetically stirring; mixing the above two materials, and stirring; dropwise adding the mixed solution on the surface of deionized water at the temperature of 50-70 ℃, simultaneously performing vacuum treatment until the solvent is completely volatilized, forming a film by using the liquid drops, taking out and drying to obtain a modified aluminum/fluorine-containing polymer compound; wherein the aluminum powder surface modification layer is one of polyaziridine glycidyl ether (GAP) and polyvinylidene fluoride (PVDF); the organic solvent A is one of ethyl acetate and butyl acetate; the ultrasonic frequency is 30 kHz-100 kHz; the magnetic stirring speed is 200 rpm-600 rpm, and the vacuum degree is 40 mbar-100 mbar.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070113939A1 (en) * | 2002-12-23 | 2007-05-24 | Chan May L | High energy blast explosives for confined spaces |
| CN106116995A (en) * | 2016-06-24 | 2016-11-16 | 中国工程物理研究院化工材料研究所 | The method press-fiting aluminum composition modeling powder is prepared in a kind of aqueous suspension |
| CN109293463A (en) * | 2018-12-13 | 2019-02-01 | 中国工程物理研究院化工材料研究所 | A kind of method of aluminium powder surface self-activation |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070113939A1 (en) * | 2002-12-23 | 2007-05-24 | Chan May L | High energy blast explosives for confined spaces |
| CN106116995A (en) * | 2016-06-24 | 2016-11-16 | 中国工程物理研究院化工材料研究所 | The method press-fiting aluminum composition modeling powder is prepared in a kind of aqueous suspension |
| CN109293463A (en) * | 2018-12-13 | 2019-02-01 | 中国工程物理研究院化工材料研究所 | A kind of method of aluminium powder surface self-activation |
Non-Patent Citations (1)
| Title |
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| "基于表面改性铝粉的含铝炸药水悬浮制备及其性能研究";夏红 等;《广东化工》;20200915;第47卷(第17期);第29-31页 * |
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