CN111908991A - alpha-AlH improvement3Method of thermal stabilization - Google Patents
alpha-AlH improvement3Method of thermal stabilization Download PDFInfo
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- CN111908991A CN111908991A CN202010699289.6A CN202010699289A CN111908991A CN 111908991 A CN111908991 A CN 111908991A CN 202010699289 A CN202010699289 A CN 202010699289A CN 111908991 A CN111908991 A CN 111908991A
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- C06B45/00—Compositions or products which are defined by structure or arrangement of component of product
- C06B45/18—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component
- C06B45/30—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component
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- C06B45/34—Compositions or products which are defined by structure or arrangement of component of product comprising a coated component the component base containing an inorganic explosive or an inorganic thermic component the coating containing an organic compound the compound being an organic explosive or an organic thermic component
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- C—CHEMISTRY; METALLURGY
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- C06B—EXPLOSIVES OR THERMIC COMPOSITIONS; MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES
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Abstract
The invention discloses a method for improving alpha-AlH3A method of thermal stability comprising treating alpha-AlH3Acid washing treatment is carried out, and then the acid-washed alpha-AlH is coated by the polymer containing the carbazolyl group3To increase alpha-AlH3Thermal stability of (2). The carbazole group-containing polymer is a single component or a mixed component of polyvinyl carbazole, poly (9-vinyl carbazole), poly (N-vinyl carbazole) and poly (N-ethyl-2-vinyl carbazole). Enhancement of alpha-AlH in the present invention3Method for further improving alpha-AlH thermal stability on the basis of acid pickling3Thermal stability, alpha-AlH treated by the process3Has lower decomposition rate and improved thermal stability. The method can be used as solid propellant fuel, the treatment process of the method is carried out at normal temperature, and the method is safe and reliable and is suitable for large-scale production.
Description
Technical Field
The invention belongs to the field of energetic materials, and particularly relates to a method for improving thermal stability of alpha-AlH 3.
Background
Hydrogen is introduced in the combustion process of the solid propellant, so that the average relative molecular mass of the fuel gas can be effectively reduced; meanwhile, the high combustion heat value of the hydrogen is beneficial to improving the temperature of the combustion chamber and the specific impulse. Aluminum trihydride is a light metal hydride with a relatively high hydrogen content, up to 10.08%, has a hydrogen storage density of 148g/L, twice that of liquid hydrogen (70.8g/L), has a higher heat of combustion value than aluminum powder, and is an ideal solid propellant fuel. At present, AlH3A total of 7 different crystal forms include: alpha, alpha', beta, gamma, beta, and zeta, wherein the thermodynamic property of the alpha crystal form is relatively stable, and the alpha crystal form is the only crystal form with application value in the formulation of the solid propellant. However, currently α -AlH is to be substituted3The solid propellant is applied to the solid propellant, and the decomposition phenomenon existing in the range of room temperature and the process temperature of the solid propellant needs to be solved.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and further improve the alpha-AlH on the basis of acid pickling passivation3The invention provides a method for improving the thermal stability of alpha-AlH 3.
In order to achieve the purpose, the invention discloses the following technical scheme:
alpha-AlH improvement3A method of thermal stability comprising treating alpha-AlH3Acid washing treatment is carried out, and then the acid-washed alpha-AlH is coated by the polymer containing the carbazolyl group3To increase alpha-AlH3Thermal stability of (2).
Further, the carbazole group-containing polymer is a single component or a mixed component of polyvinyl carbazole, poly (9-vinyl carbazole), poly (N-vinyl carbazole) and poly (N-ethyl-2-vinyl carbazole).
In particular, the alpha-AlH3The particle size of (A) is 200 nm-40 um.
Further, the acid washing treatment comprises the step of adding alpha-AlH3Adding into acid solution, stirring, filtering, cleaning and drying.
Further, the alpha-AlH after the acid pickling treatment is coated by the polymer containing the carbazolyl group3The method specifically comprises the following steps: dissolving a polymer containing carbazolyl group in an organic solvent to obtain a polymer solution system, and then carrying out acid washing treatment on the alpha-AlH3Dipping, stirring, filtering, washing and drying in the polymer solution system.
Further, the volume fraction of the acid solution is 5-10%.
Optionally, the cleaning solvent is one or more of ethanol, methanol, acetone and tetrahydrofuran.
Optionally, the organic solvent is one or more of benzene, toluene, chlorobenzene, chloroform, dichloromethane and tetrahydrofuran.
Specifically, the stirring is magnetic stirring, the stirring speed is 200-1000 rpm, and the stirring time is 2-12 hours;
the drying is freeze drying.
Compared with the prior art, the invention has the following technical effects:
enhancement of alpha-AlH in the present invention3Method for further improving alpha-AlH thermal stability on the basis of acid pickling3Thermal stability, alpha-AlH treated by the process3Has lower decomposition rate and better thermal stability. The method can be used as solid propellant fuel, the treatment process of the method is carried out at normal temperature, and the method is safe and reliable and is suitable for large-scale production.
The present invention will be described in further detail with reference to specific embodiments.
Drawings
FIG. 1 shows the present inventionMethod for treating alpha-AlH3SEM topography of (a).
FIG. 2 acid-washed alpha-AlH3/Al2O3X-ray powder diffraction pattern of (a).
FIG. 3 alpha-AlH treated by the present method3/Al2O3Thermal stability curve at 60 ℃ for/PVK.
Detailed Description
Any modification of the structure, change of the ratio or adjustment of the size of the structure should still fall within the scope of the present disclosure without affecting the function and the purpose of the present disclosure.
The invention provides a method for improving alpha-AlH by coating with a polymer containing carbazolyl group3A method of thermal stability. The carbazole group has good electron-donating ability and is beneficial to alpha-AlH3Al in the crystal lattice3+Produces complexation, thereby inhibiting the catalytic decomposition process. In addition, the polymer containing carbazolyl group generally has better thermal stability, hydrophobicity and chemical stability, and not only can improve alpha-AlH3The compatibility of the alpha-AlH can also be obviously improved, and the alpha-AlH is beneficial to promoting the thermal stability of the alpha-AlH3Research on the practical application of the solid propellant.
"alpha-AlH" in the present invention3/Al2O3"means alpha-AlH3After acid washing treatment, dilute hydrochloric acid and alpha-AlH3Surface reaction at alpha-AlH3In situ formation of Al on the surface2O3。
"alpha-AlH" in the present invention3/Al2O3the/PVK' refers to alpha-AlH subjected to acid washing treatment and then coated with carbazolyl-group-containing polymer after acid washing treatment3In this case, alpha-AlH3Containing Al2O3And two coating layers of PVK, Al2O3The occupation ratio of the two coating layers to PVK is small.
The function of the added carbazole group polymer is in alpha-AlH3/Al2O3A coating layer is formed on the surface to improve alpha-AlH3Thermal stability of (a);
"coating" means coating in alpha-AlH3alpha-AlH obtained after acid washing treatment3/Al2O3The surface is coated with a layer of carbazole group-containing polymer, wherein, during preparation, the carbazole group-containing polymer and alpha-AlH3Acid-washing the alpha-AlH3/Al2O3The mass ratio of (1) to (5).
The improvement of alpha-AlH of the invention3A method of thermal stability comprising treating alpha-AlH3Acid washing treatment is carried out, and then the acid-washed alpha-AlH is coated by the polymer containing the carbazolyl group3To increase alpha-AlH3Thermal stability of (2).
The method comprises the step of magnetically stirring a solution system by an IKA magnetic stirrer (RH digital), wherein the stirring speed is 200-1000 rpm, and the stirring time is 2-12 h.
alpha-AlH for use in the invention3Other experimental materials were purchased from alatin reagent, inc, provided by the seian recent chemical research institute. The average molecular weight of the carbazole-based polymer is about 90000.
Example 1:
this example discloses an improvement of alpha-AlH3A method of thermal stability comprising treating alpha-AlH3Acid washing treatment is carried out, and then the acid-washed alpha-AlH is coated by the polymer containing the carbazolyl group3To increase alpha-AlH3Thermal stability of (2).
The acid washing treatment comprises the step of adding alpha-AlH3Adding the mixture into acid solution, stirring, filtering, cleaning and drying in sequence to obtain alpha-AlH3/Al2O3。
alpha-AlH coated with carbazolyl-group-containing polymer and subjected to acid pickling treatment3The method specifically comprises the following steps: dissolving a polymer containing carbazolyl group in an organic solvent to obtain a polymer solution system, and then carrying out acid washing treatment on the alpha-AlH3Dipping, stirring, filtering, washing and drying in the polymer solution system.
The carbazole group-containing polymer is a single component or a mixed component of polyvinyl carbazole, poly (9-vinyl carbazole), poly (N-vinyl carbazole) and poly (N-ethyl-2-vinyl carbazole).
In this example, the acid solution was diluted hydrochloric acid, and the carbazole group-containing polymer was poly (9-vinylcarbazole).
(1) Preparing a dilute hydrochloric acid solution with the volume fraction of 10%; taking alpha-AlH synthesized by a wet method3Adding into dilute hydrochloric acid solution, stirring, filtering, washing with ethanol for 3 times, and freeze drying to obtain off-white powder sample, i.e. alpha-AlH3/Al2O3。
Al2O3In alpha-AlH3Surface in-situ formation; and has protection effect and can improve the thermal stability of the alpha-AlH 3.
(2) 100mg of Poly (9-vinylcarbazole) (Poly (9-vinylcarbazole), PVK) is dispersed in a chloroform solvent and stirred to dissolve; then 300mg of alpha-AlH is taken3/Al2O3Adding the alpha-AlH into the solution, stirring and dispersing the solution for 4 to 12 hours, filtering the solution, cleaning the solution for 3 times by using trichloromethane, and finally freeze-drying the solution to obtain an off-white powder sample, namely the alpha-AlH3/Al2O3PVK. The stirring speed is 200-1000 rpm.
In the preparation raw materials in this example, poly (9-vinylcarbazole) and α -AlH3/Al2O3The mass ratio of (A) to (B) may be 1 (1-5). In this embodiment, 1:3 is selected.
Example 2
Same as example 1, except that poly (9-vinylcarbazole) and α -AlH3The mass ratio of (1) to (5) and the volume fraction of the dilute hydrochloric acid solution is 8%.
Example 3:
(1) preparing a dilute hydrochloric acid solution with the volume fraction of 5%; taking alpha-AlH synthesized by a wet method3Adding into dilute hydrochloric acid solution, stirring, filtering, washing with ethanol for 3 times, and freeze drying to obtain off-white powder sample, i.e. alpha-AlH3/Al2O3。
(2) Dispersing 200mg of poly (N-ethyl-2-vinylcarbazole) in a trichloromethane solvent, and stirring for dissolving; then 500mg of alpha-AlH is taken3/Al2O3Adding the mixture into the solution, stirring and dispersing for 2-6 h, filtering and cleaning for 3 times by using trichloromethane, and finally freeze-drying to obtain an off-white powder sample, namely alpha-AlH3/Al2O3PVK. The stirring speed is 200-1000 rpm.
Example 4:
the carbazole group-containing polymer was selected from polyvinylcarbazole, polyvinylcarbazole and α -AlH as in example 13/Al2O3The mass ratio of (A) to (B) is 1:2, and the volume fraction of the dilute hydrochloric acid solution is 6%.
Example 5
The carbazole group-containing polymer was selected from polyvinylcarbazole, polyvinylcarbazole and α -AlH as in example 13/Al2O3The mass ratio of (A) to (B) is 1:4, and the volume fraction of the dilute hydrochloric acid solution is 9%.
Treatment of alpha-AlH by the method of the invention3The characterization results of the morphology structure and the thermal stability are as follows:
example 1 alpha-AlH coated with Pickling and PVK3The SEM picture is shown in FIG. 1, which is a square particle shape and is formed by alpha-AlH3Compared with the appearance, the appearance is not obviously changed.
FIG. 2 shows the acid-washed alpha-AlH3(α-AlH3/Al2O3) The X-ray powder diffraction pattern of (A) can be seen from which is alpha-AlH after acid washing3The diffraction pattern of (2) and its standard card (PDF #71-2421, space group)
) The consistency indicates that the acid washing process does not change the alpha-AlH3A crystalline form of (a).
Thermal stability characterization experiments were performed under vacuum at 60 ℃, as shown in fig. 3: as can be seen, the acid-washed alpha-AlH3/Al2O3As a control, the thermal stability, measured as the percentage decomposition, of the alpha-AlH treated by the method of the invention at the same constant temperature time3/Al2O3the/PVK has a lower decomposition rate, indicating a better thermal stability, alpha-AlH3/Al2O3The decomposition rate of/PVK is lower than 10%, and only acid-washed alpha-AlH3/Al2O3The decomposition rate of (A) is as high as 45%.
Example 6
The carbazolyl-group-containing polymer was selected from poly (9-vinylcarbazole), poly (9-vinylcarbazole) and alpha-AlH as in example 13/Al2O3The mass ratio of (1) to (1) and the volume fraction of the dilute hydrochloric acid solution is 6%.
Example 7
The carbazolyl-group-containing polymer was selected from poly (9-vinylcarbazole), poly (9-vinylcarbazole) and alpha-AlH as in example 13/Al2O3The mass ratio of (1) to (1) and the volume fraction of the dilute hydrochloric acid solution is 5%.
Example 8
The carbazole group-containing polymer was selected from polyvinylcarbazole, polyvinylcarbazole and α -AlH as in example 13/Al2O3The mass ratio of (A) to (B) is 1:3, and the volume fraction of the dilute hydrochloric acid solution is 5%.
Example 9
The carbazole group-containing polymer was selected from poly (n-vinylcarbazole), poly (n-vinylcarbazole) and α -AlH as in example 13/Al2O3The mass ratio of (1) to (1) and the volume fraction of the dilute hydrochloric acid solution is 9%.
Example 10
The carbazole group-containing polymer was selected from poly (N-ethyl-2-vinylcarbazole), poly (N-ethyl-2-vinylcarbazole) and α -AlH, as in example 13/Al2O3The mass ratio of (A) to (B) is 1:5, and the volume fraction of the dilute hydrochloric acid solution is 10%.
Example 11
The carbazolyl-group-containing polymer is selected from poly (9-vinylcarbazole) and poly (N-ethyl-2-vinylcarbazole) in the same manner as in example 1, the mass ratio of the poly (9-vinylcarbazole) to the poly (N-ethyl-2-vinylcarbazole) is 1:1, and the poly (9-vinylcarbazole) to the poly (N-ethyl-2-vinylcarbazole) to alpha-AlH3/Al2O3The mass ratio of (1: 1: 2) and the volume fraction of the dilute hydrochloric acid solution is 8%.
Example 12
The carbazolyl-group-containing polymer was selected from poly (9-vinylcarbazole), polyvinylcarbazole and poly (N-ethyl-2-vinyl-carbazole) in the same manner as in example 1Carbazole), the mass ratio of poly (9-vinyl carbazole), polyvinyl carbazole and poly (N-ethyl-2-vinyl carbazole) is 1:1:1, and the carbazole group-containing polymer and alpha-AlH3/Al2O3The mass ratio of (1) to (2) and the volume fraction of the dilute hydrochloric acid solution is 8%.
The objects, technical solutions and advantages of the present invention are further described in the above embodiments, it should be noted that the above embodiments are merely preferred embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
The preferred embodiments of the present disclosure are described in detail with reference to the accompanying drawings, however, the present disclosure is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present disclosure within the technical idea of the present disclosure, and these simple modifications all belong to the protection scope of the present disclosure.
It should be noted that, in the foregoing embodiments, various features described in the above embodiments may be combined in any suitable manner, and in order to avoid unnecessary repetition, various combinations that are possible in the present disclosure are not described again.
In addition, any combination of the various embodiments of the present disclosure can be made, and the same should be considered as the inventive content of the present disclosure, as long as the combination does not depart from the spirit of the present disclosure.
Claims (9)
1. alpha-AlH improvement3A method of thermal stability comprising para-alpha-AlH3Acid washing treatment is carried out, and then the acid-washed alpha-AlH is coated by the polymer containing the carbazolyl group3To increase alpha-AlH3Thermal stability of (2).
2. The method of claim 1 for increasing alpha AlH3The method for thermal stability is characterized in that the carbazole group-containing polymer is polyvinylcarbazole,Poly (9-vinylcarbazole), poly (N-vinylcarbazole) and poly (N-ethyl-2-vinylcarbazole) as single components or as mixed components.
3. The method of claim 1 for increasing alpha AlH3A method for thermal stabilization, characterized in that said α -AlH3The particle size of (A) is 200 nm-40 um.
4. The method of claim 1 for increasing alpha AlH3The method for thermal stability is characterized in that the acid washing treatment comprises the step of adding alpha-AlH3Adding into acid solution, stirring, filtering, cleaning and drying.
5. The method of claim 1 for increasing alpha AlH3The method for thermal stability is characterized in that the carbazolyl-group-containing polymer is used for coating the alpha-AlH subjected to acid washing treatment3The method specifically comprises the following steps: dissolving a polymer containing carbazolyl group in an organic solvent to obtain a polymer solution system, and then carrying out acid washing treatment on the alpha-AlH3Dipping, stirring, filtering, washing and drying in the polymer solution system.
6. The method of claim 4 for increasing alpha AlH3The method for thermal stability is characterized in that the volume fraction of the acid solution is 5-10%.
7. The method of claim 4 for increasing alpha AlH3The method for thermal stability is characterized in that the cleaning solvent is one or more of ethanol, methanol, acetone and tetrahydrofuran.
8. The method of claim 5 for increasing alpha AlH3The method for thermal stability is characterized in that the organic solvent is one or more of benzene, toluene, chlorobenzene, trichloromethane, dichloromethane and tetrahydrofuran.
9. According to claim4 or 5 by increasing alpha-AlH3The method for thermal stability is characterized in that the stirring is magnetic stirring, the stirring speed is 200-1000 rpm, and the stirring time is 2-12 h; the drying is freeze drying.
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Cited By (3)
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| CN112441863A (en) * | 2020-11-27 | 2021-03-05 | 湖北航天化学技术研究所 | ADN/AlH3Composite microspheres, preparation method and solid propellant containing microspheres |
| CN113670770A (en) * | 2021-09-16 | 2021-11-19 | 湖北航天化学技术研究所 | AlH-containing catalyst3Propellant thermal decomposition detection method |
| CN117247309A (en) * | 2023-09-22 | 2023-12-19 | 湖北航天化学技术研究所 | Stabilization modification method for aluminum trihydride |
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| CN117247309A (en) * | 2023-09-22 | 2023-12-19 | 湖北航天化学技术研究所 | Stabilization modification method for aluminum trihydride |
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