CN110550607B - alpha-AlH 3 flotation method and application thereof - Google Patents
alpha-AlH 3 flotation method and application thereof Download PDFInfo
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- CN110550607B CN110550607B CN201910865186.XA CN201910865186A CN110550607B CN 110550607 B CN110550607 B CN 110550607B CN 201910865186 A CN201910865186 A CN 201910865186A CN 110550607 B CN110550607 B CN 110550607B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/06—Hydrides of aluminium, gallium, indium, thallium, germanium, tin, lead, arsenic, antimony, bismuth or polonium; Monoborane; Diborane; Addition complexes thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B6/00—Hydrides of metals including fully or partially hydrided metals, alloys or intermetallic compounds ; Compounds containing at least one metal-hydrogen bond, e.g. (GeH3)2S, SiH GeH; Monoborane or diborane; Addition complexes thereof
- C01B6/34—Purification; Stabilisation
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- C—CHEMISTRY; METALLURGY
- C06—EXPLOSIVES; MATCHES
- C06D—MEANS FOR GENERATING SMOKE OR MIST; GAS-ATTACK COMPOSITIONS; GENERATION OF GAS FOR BLASTING OR PROPULSION (CHEMICAL PART)
- C06D5/00—Generation of pressure gas, e.g. for blasting cartridges, starting cartridges, rockets
Abstract
The invention relates to alpha-AlH3A flotation method and application thereof, belonging to the technical field of energetic materials. The invention utilizes alpha crystal form and non-alpha crystal form AlH3Different physical and chemical properties, surface adsorption property, crystal morphology property and other inherent properties, realizes AlH by means of the separation and purification function of ultrasonic waves and adopting specific flotation solution3AlH with medium alpha crystal form and non-alpha crystal form3High-efficiency separation is carried out to obtain high-quality alpha crystal form AlH3And non-alpha crystalline forms. Through impact sensitivity and friction sensitivity experiments, the separated high-quality alpha crystal form AlH is verified3Safety in application in composite high-energy solid propellant. The high-quality alpha crystal form AlH of the invention3High hydrogen content, based on high quality alpha crystal form AlH3The high-energy propellant has low slurry sensitivity.
Description
Technical Field
The invention relates to alpha-AlH3A flotation method and application thereof, belongs to the technical field of energetic materials, and more particularly relates to high-quality alpha-AlH applicable to the fields of propellants, explosives or other energetic materials3And liquid phase ultrasonic assisted flotation of high quality alpha-AlH3Increasing AlH3The method has applicability in the field of energetic materials.
Background
Aluminum trihydride (AlH)3) Also known as alane, is a promising high-energy additive for solid propellant formulations. According to theoretical calculations, AlH is used3The specific impulse of the solid propellant can be at least increased by 100N.s.kg instead of aluminum powder-1And the temperature of the combustion chamber and the ejected gas is lower than that of aluminum powder-containing propellant AlH3Releasing 10% of its own weight of H during decomposition2Effectively reducing the average molecular weight of the fuel gas, therefore, AlH3High-energy additives as solid propellants have become the focus of attention of researchers at home and abroad.
Depending on the synthesis method and reaction conditions, unsolvated AlH can be obtained3There are 7 different crystal forms, alpha', beta, gamma, delta, epsilon and xi. AlH of each crystal form3Have fixed atom arrangement modes, and therefore have unique thermodynamic properties. Practice proves that all separated crystal forms are most stable alpha-AlH3。β-AlH3And gamma-AlH3Can be converted into alpha-AlH at 91.0 ℃ and 100.7 ℃ respectively3However, they are not thermodynamically stable at normal temperature and have a decomposition rate much higher than that of α -AlH3. The alpha, delta, epsilon and xi crystal forms can not be converted into the alpha crystal form, the thermal stability is poor, and the thermal stability is obviously reduced due to the existence of a small amount of non-alpha crystal forms in the alpha crystal form. By mixing with waterThe reaction activity comparison shows that the alpha crystal form is relatively stable in water, the alpha' crystal form reacts violently with water, the beta and gamma crystal forms react relatively slowly, and the etherate crystal form catches fire when meeting water. Thus, only α -AlH3The crystal form has practical application value and is the only crystal form with application value in the formula of the solid propellant.
AlH in the early 60 s of the 20 th century3The application in military is evaluated and the AlH is found3The stability is poor, hydrogen is released during storage, the energy of the energetic material is reduced, and the preparation process and the safety performance of the energetic material are influenced. Especially, a small amount of non-alpha crystal form exists in the alpha crystal form, so that the thermal stability of the alpha crystal form is obviously reduced, and the safety of the energetic material system is further reduced. Existing AlH3The synthesis process, whether a liquid phase method or a solid phase method, is difficult to obtain a single alpha crystal form, and the existence of an impurity crystal form influences AlH3And further influences the practical application thereof. Many reports on AlH are reported3And stabilizing methods such as surface passivation, organic and inorganic coating, ion infiltration, and crystal transformation. Although these methods can improve AlH to some extent3Stability and safety of (2), but still does not substantially address AlH3Stability of (2).
AlH was synthesized as described above using the ether method3Due to alpha-form AlH3Sensitive to the raw material purity, the water content, the use and proportion of the cosolvent, the type and the dosage of the crystallization additive and other factors during synthesis, and non-alpha crystal form AlH often appears3And mainly takes alpha', beta and gamma crystal forms, and the appearance of the crystal forms is opposite to AlH3The thermodynamic stability and safety of the product under room temperature storage conditions are affected to different degrees. The presence of the impurity crystal form makes AlH3The alpha crystal form AlH has quick decomposition under the condition of room temperature storage, increases the friction sensitivity of the sample, particularly has obvious influence on the static sensitivity, and has better crystal form3Compared with the prior art, the difference of E50 is 5-10 times. The influence on the sensitivity of propellant slurry is more obvious, and AlH with poorer crystal form is added3Percussion of propellant slurryThe impact sensitivity and the friction sensitivity are increased rapidly, and the charging requirement is difficult to meet. Thus, an efficient method is used to minimize alpha-AlH3AlH of medium non-alpha crystal form3It is of great importance.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: overcomes the defects of the prior art and provides alpha-AlH3A flotation method and application thereof, wherein the method is used for separating the AlH produced in the industrialized production3AlH of alpha crystal form3And non-alpha crystal form AlH3And other impurities, which can increase AlH3The purity and stability of the medium alpha crystal form are improved, and high-quality alpha-AlH is obtained3And further reducing the mechanical sensitivity of a system after the alpha-AlH is mixed with the common components of the propellant, and realizing the practical application of the alpha-AlH in the high-energy solid propellant3And non-alpha crystal form AlH3Separating and increasing alpha-AlH3The crystal form purity of (1) and improves AlH3To realize an efficient and industrially easily applicable method for practical application in solid propellants, the high-quality alpha-AlH3The method for obtaining the alpha-AlH adopts a liquid phase ultrasonic auxiliary flotation method to prepare high-quality alpha-AlH3And is adsorbed on alpha-AlH by ultrasonic stripping3Non-alpha crystal form AlH on crystal3And other impurities, and use of alpha-AlH3Crystalline and non-alpha crystalline AlH3Different adsorption characteristics and sedimentation characteristics with the flotation solution, and alpha crystal form and non-alpha crystal form AlH3And other impurities are effectively separated, and AlH is improved3To thereby increase AlH3Hydrogen content of (2), solving AlH3And safety issues in energetic material applications.
The technical solution of the invention is as follows:
alpha-AlH3A flotation process comprising the steps of:
s1: reacting AlH3Dispersing the crude product in a flotation solution to form a suspension A;
s2: ultrasonically pulverizing the suspension A with an ultrasonic pulverizer to obtain AlH3AlH of alpha crystal form in crude product3Surface and adsorbed non-alpha crystal form AlH3And other impurities are removed, and then stirring is carried out to ensure that AlH is3The crude product and the flotation solution fully react to form a suspension B;
s3: pouring the suspension B into a separating funnel, standing to naturally settle and stratify, recording the lower-layer solid as C and the upper-layer suspension as D, separating the lower-layer solid C from the upper-layer suspension D, washing, filtering and vacuum drying the lower-layer solid C to obtain alpha crystal form AlH3Carrying out suction filtration, washing and vacuum drying on the upper layer suspension D to obtain non-alpha crystal form AlH3And other impurity compounds.
In the step S1, AlH3The crude product is AlH produced by industrialized ether synthesis method3A crude product;
in the step S1, the flotation solution is one or a mixture of more than two of oleic acid, linoleic acid, linolenic acid and arachidonic acid;
in the step S1, AlH3The mass ratio of the crude product to the flotation solution is 1: 20-100;
in the step S2, the ultrasonic crushing power is 400-2000W, and the ultrasonic crushing time is 30-1800S;
in the step S2, the stirring speed is 200-1500r/min, and the stirring time is 30-300 min;
in the step S3, the standing time is 2-72 h;
in the step S3, the solvent used for washing is cyclohexane, n-hexane or ethyl acetate;
in the step S3, the vacuum drying temperature is 30-50 ℃, and the vacuum drying time is 6-48 h.
alpha-AlH3Use of alpha-AlH3The fuel is applied to the field of energetic materials such as propellant, explosive and the like.
Compared with the prior art, the invention has the advantages that:
(1) AlH based on industrial production3The post-treatment does not influence the preparation process of the industrial production, the separation technology is simple and efficient, and the industrial capability is continuous.
(2) ToEffectively reduces non-alpha crystal form AlH in the physical process3Content of not only improving AlH3Due to the removal of non-alpha-form AlH3And other impurities, AlH3Has a significantly increased or maintained AlH content as compared to the desensitization method by introducing other substances3The H content of (2).
(3) High quality AlH3The method has applicability in the field of energetic materials such as solid propellants, explosives and the like.
(4) The effect before and after flotation adopts H content and AlH3The impact sensitivity instrument and the friction sensitivity instrument of the slurry are evaluated to respectively test AlH3H content of (C) and based on AlH3Sample, high quality alpha-AlH3AlH of non-alpha crystal type3Sensitivity of high-energy propellant slurry.
(5) The invention utilizes alpha crystal form and non-alpha crystal form AlH3Different physical and chemical properties, surface adsorption property, crystal morphology property and other inherent properties, realizes AlH by means of the separation and purification function of ultrasonic waves and adopting specific flotation solution3AlH with medium alpha crystal form and non-alpha crystal form3High-efficiency separation is carried out to obtain high-quality alpha crystal form AlH3And non-alpha crystalline forms. Through impact sensitivity and friction sensitivity experiments, the separated high-quality alpha crystal form AlH is verified3Safety in application in composite high-energy solid propellant. The high-quality alpha crystal form AlH of the invention3High hydrogen content, based on high quality alpha crystal form AlH3The high-energy propellant has low slurry sensitivity.
(6) High-quality alpha-AlH3Flotation method, AlH prepared by industrialized ether synthesis3The crude product is used as a starting material, and industrial AlH is separated by a liquid-phase ultrasonic-assisted flotation method at normal temperature3AlH of alpha crystal form in crude product3And non-alpha crystal form AlH3And other impurities to obtain high-quality alpha-AlH3. The method comprises the following steps: s1: AlH prepared by industrialized ether synthesis method3Dispersing the crude product in a certain amount of flotation solvent to form suspension A; s2: ultrasonically crushing the suspension A for a certain time by using an ultrasonic crusher at a certain ultrasonic power to ensure that AlH is obtained3AlH of alpha crystal form in crude product3Non-alpha crystal form AlH of surface3And other impurities are separated from the surface of the suspension, and the suspension is stirred for a certain time at a certain stirring speed to form suspension B; s3: pouring the suspension B into a separating funnel, standing for a certain time to allow the suspension B to naturally settle and stratify, recording the lower-layer solid as C and the upper-layer suspension as D, separating C and D, and then respectively carrying out suction filtration, washing and vacuum drying to obtain the high-quality alpha-AlH3And non-alpha crystal form AlH3And other impurities. The method has simple process, easy operation and convenient industrial production, and the adoption of simple liquid-phase ultrasonic-assisted flotation can improve the industrial AlH3Middle alpha-AlH3Crystal purity and hydrogen content, and the flotation solution adopted can slowly react with AlH3Reaction is carried out to form a passivation layer, so that AlH can be effectively improved3The heat stability of the crude product is improved, and then AlH is effectively improved3Safety in application in the field of energetic materials such as propellants.
Drawings
FIG. 1 is AlH3SEM image of crude product;
FIG. 2 shows AlH of alpha crystal form3SEM picture of (1);
FIG. 3 shows non-alpha crystal form AlH3SEM image of (d).
Detailed Description
High-quality alpha-AlH3Flotation method for AlH prepared by industrialized ether synthesis method3Non-alpha crystal form AlH often appears in crude products3And other impurities, by using AlH of different crystal forms3The alpha crystal form AlH is enabled to be in a higher ultrasonic stripping effect by adopting an ultrasonic crusher3Surface adsorbed non-alpha crystal form AlH3And separating other impurities. Pairing alpha crystal form and non-alpha crystal form AlH by means of flotation solution3And other impurities with different adsorption capacities to realize alpha crystal form and non-alpha crystal form AlH3Accurately screening to obtain high-quality alpha-AlH3Increasing AlH3Stability and safety in application in energetic materials such as propellant.
High-quality alpha-AlH3The flotation method comprises the following steps:
s1, reacting AlH at normal temperature3Is configured to be suspendedLiquid A, specifically AlH prepared by industrial ether synthesis3Placing the crude product in a beaker, and preparing AlH with the mass ratio of 1: 20-1: 1003-flotation slurry, stirred for a certain time, let AlH3Completely wetting to obtain suspension A;
s2, ultrasonically crushing the suspension A for a certain time by an ultrasonic crusher at a certain power to ensure that AlH3AlH of alpha crystal form in crude product3Non-alpha crystal form AlH of surface3And other impurities are separated, and then the mixture is stirred for a certain time at a certain speed to ensure that the AlH is3Fully reacting with a flotation solvent to form a suspension B;
s3, pouring the suspension B into a separating funnel, standing for a certain time to allow the suspension B to naturally settle and separate, recording the lower-layer solid as C and the upper-layer suspension as D, separating C and D, and then respectively carrying out suction filtration, washing and vacuum drying to obtain the high-quality alpha-AlH3And non-alpha crystal form AlH3And other impurities.
The solvent used in the step S1 is one or two of oleic acid, linoleic acid, linolenic acid and arachidonic acid.
In the step S1, the stirring speed is 200r/min-1500r/min, and the preferred stirring speed is 400r/min-800 r/min.
The ultrasonic power used in the step S2 is 400W-2000W, and the ultrasonic mode may be one time of long time ultrasonic or multiple times of short time ultrasonic.
The ultrasonic time of the step S2 is 30S-1800S, and the preferable ultrasonic time is 120S-600S.
In the step S2, the stirring speed is 200r/min-1500r/min, the preferred stirring speed is 400r/min-1000r/min, the stirring time is 10min-360min, and the preferred stirring time is 30min-120 min.
The standing time in the step S3) is 2-72h, and the preferable time is 6-24 h.
The solvent used for washing in the step S3 is cyclohexane, n-hexane, ethyl acetate and the like, the vacuum drying temperature is 30-50 ℃, and the vacuum heat preservation time is 6-48 h.
High-quality alpha-AlH3The application in propellants and explosives.
The following examples are provided to better illustrate the effects of the present invention, but the present invention is not limited to the following examples.
Example 1
alpha-AlH3The flotation method comprises the following steps:
step 1: weighing 5g of AlH3Placing the crude product in a 500mL beaker, accurately measuring 250mL oleic acid, magnetically stirring at 400r/min for 60min to obtain AlH3The crude product was completely wetted with oleic acid to give suspension A.
Step 2: carrying out ultrasonic treatment on the suspension A for 120s by using an ultrasonic crusher at 600W ultrasonic power, and then stirring for 240min at the stirring speed of 800rmp/min to obtain a suspension B;
and step 3: standing the suspension B in a separating funnel for 24h, layering, respectively performing suction filtration on the lower-layer solid C and the upper-layer suspension D, washing with n-hexane for several times, and keeping the temperature in a vacuum drying oven at 50 ℃ for 24 hours to respectively obtain off-white powder AlH3-C3.78g and AlH3-D1.13g。
Reacting AlH3Crude product and obtained AlH3-C and AlH3D H content test and AlH of basic formula3Impact and friction sensitivities of/AP/Cl-20/H-16/other auxiliaries, the results show: AlH3Crude product, AlH3-C and AlH3-hydrogen content of D9.944%, 9.957% and 9.102%, respectively; as received AlH3The impact sensitivity of the crude product/AP/CL-20/H-16/other auxiliary agent system is: 4.6J, 96% of friction sensitivity, AlH3The impact sensitivity of the-C/AP/CL-20/H-16/other auxiliary agent system is 7.4J, and the friction sensitivity is 44%; AlH3The impact sensitivity of the-D/AP/CL-20/H-16/other auxiliary system was 4.1J and the friction sensitivity was 88%.
Example 2
alpha-AlH3The flotation method comprises the following steps:
step 1: weighing 5g of AlH3Placing the crude product in a 500mL beaker, accurately measuring 500mL linoleic acid, and stirring with 200r/min magnetic stirring for 360min to obtain AlH3The crude product was completely wetted with linoleic acid to give suspension A.
Step 2: and (4) carrying out ultrasonic treatment on the suspension A for 30s by using an ultrasonic crusher at 2000W ultrasonic power, and then stirring for 360min at a stirring speed of 200rmp/min to obtain a suspension B.
And step 3: standing the suspension B in a separating funnel for 72h, layering, respectively performing suction filtration on the lower-layer solid C and the upper-layer suspension D, washing with n-hexane for several times, and keeping the temperature in a vacuum drying oven at 30 ℃ for 72h to respectively obtain off-white powder AlH3-C4.12g and AlH3-D0.86g。
And 4, step 4: all-in-one AlH3、AlH3-C and AlH3D H content test and AlH of basic formula3Impact and friction sensitivities of/AP/CL-20/H-16/other adjuvants, the results show: as received AlH3Crude product, AlH3-C and AlH3-hydrogen content of D9.944%, 9.969% and 8.926%, respectively; as received AlH3The impact sensitivity of the crude product/AP/CL-20/H-16/other auxiliary agent system is: 4.6J, 96% of friction sensitivity, AlH3The impact sensitivity of the-C/AP/CL-20/H-16/other auxiliary agent system is 8.0J, and the friction sensitivity is 36%; AlH3The impact sensitivity of the-D/AP/CL-20/H-16/other auxiliary system is 4.2J and the friction sensitivity is 100%.
Example 3
alpha-AlH3The flotation method comprises the following steps:
step 1: weighing 5g of AlH3Placing the crude product in 500mL beaker, accurately measuring 100mL linolenic acid, and magnetically stirring at 1500r/min for 30min to obtain AlH3The crude product is completely wetted by linolenic acid to obtain suspension A.
Step 2: and (4) carrying out ultrasonic treatment on the suspension A for 1200s by using an ultrasonic crusher at the ultrasonic power of 400W, and then stirring for 180min at the stirring speed of 600rmp/min to obtain suspension B.
And step 3: standing the suspension B in a separating funnel for 8h, layering, respectively performing suction filtration on the lower-layer solid C and the upper-layer suspension D, washing with cyclohexane for several times, and keeping the temperature in a vacuum drying oven at 40 ℃ for 24h to respectively obtain off-white powder AlH3-C4.28g and AlH3-D0.68g。
Step (ii) of4: all-in-one AlH3、AlH3-C and AlH3D H content test and AlH of basic formula3Impact and friction sensitivities of/AP/CL-20/H-16/other adjuvants, the results show: as received AlH3Crude product, AlH3-C and AlH3-hydrogen content of D9.944%, 9.978% and 8.838%, respectively; as received AlH3The impact sensitivity of the crude product/AP/CL-20/H-16/other auxiliary agent system is: 4.6J, 96% of friction sensitivity, AlH3The impact sensitivity of the-C/AP/CL-20/H-16/other auxiliary agent system is 9.4J, and the friction sensitivity is 32%; AlH3The impact sensitivity of the-D/AP/CL-20/H-16/other auxiliary system is 4.1J, and the friction sensitivity is 96%.
Example 4
alpha-AlH3The flotation method comprises the following steps:
step 1: weighing 5g of AlH3Placing the crude product in 500mL beaker, accurately measuring 150mL oleic acid and 150mL linoleic acid, and stirring with magnetic force of 800r/min for 30min to obtain AlH3The crude product was completely wetted with oleic acid to give suspension A.
Step 2: and (3) carrying out ultrasonic treatment on the suspension A by an ultrasonic crusher at 800W ultrasonic power for 180s, then carrying out ultrasonic treatment at 600rmp/min for 30min, then carrying out ultrasonic treatment at 800W ultrasonic power for 120s, and carrying out ultrasonic treatment at 600rmp/min for 30min to obtain a suspension B.
And step 3: standing the suspension B in a separating funnel for 24h, layering, respectively performing suction filtration on the lower-layer solid C and the upper-layer suspension D, washing with ethyl acetate for several times, and keeping the temperature in a vacuum drying oven at 40 ℃ for 12h to respectively obtain off-white powder AlH3-C3.52g and AlH3-D1.45g。
And 4, step 4: all-in-one AlH3、AlH3-C and AlH3D H content test and AlH of basic formula3Impact and friction sensitivities of/AP/CL-20/H-16/other adjuvants, the results show: as received AlH3Crude product, AlH3-C and AlH3-hydrogen content of D9.944%, 9.985% and 8.188%, respectively; as received AlH3The impact sensitivity of the crude product/AP/CL-20/H-16/other auxiliary agent system is: 4.6J, friction sensitivity96% of AlH3The impact sensitivity of the-C/AP/CL-20/H-16/other auxiliary agent system is 9.8J, and the friction sensitivity is 20%; AlH3The impact sensitivity of the-D/AP/CL-20/H-16/other auxiliary system was 4.5J and the friction sensitivity was 76%.
Example 5
alpha-AlH3The flotation method comprises the following steps:
step 1: weighing 5g of AlH3Placing the crude product in 500mL beaker, accurately measuring 200mL arachidonic acid, and magnetically stirring at 500r/min for 60min to obtain AlH3The crude product was completely wetted with arachidonic acid to give suspension A.
Step 2: and (4) carrying out ultrasonic treatment on the suspension A for 300s by using an ultrasonic crusher at the ultrasonic power of 1000W, and then stirring for 240min at the stirring speed of 600rmp/min to obtain a suspension B.
And step 3: standing the suspension B in a separating funnel for 6h, layering, respectively carrying out suction filtration on a lower-layer solid C and an upper-layer suspension D, washing for a plurality of times by adopting cyclohexane, and carrying out heat preservation in a vacuum drying oven at 40 ℃ for 24 to respectively obtain offwhite powder AlH3-C3.82g and AlH3-D1.08g。
And 4, step 4: all-in-one AlH3、AlH3-C and AlH3D H content test and AlH of basic formula3Impact and friction sensitivities of/AP/CL-20/H-16/other adjuvants, the results show: as received AlH3Crude product, AlH3-C and AlH3-hydrogen content of D9.944%, 9.968% and 8.582%, respectively; as received AlH3The impact sensitivity of the crude product/AP/CL-20/H-16/other auxiliary agent system is: 4.6J, 96% of friction sensitivity, AlH3The impact sensitivity of the-C/AP/CL-20/H-16/other auxiliary agent system is 8.3J, and the friction sensitivity is 48%; AlH3The impact sensitivity of the-D/AP/CL-20/H-16/other auxiliary system was 4.1J and the friction sensitivity was 92%.
Example 6
alpha-AlH3The flotation method comprises the following steps:
step 1: weighing 5g of AlH3Placing the crude product in a 500mL beaker, accurately measuring 300mL of oleic acid, and magnetically stirring for 300mi at 200r/minn is AlH3The crude product was completely wetted with oleic acid to give suspension A.
Step 2: and (4) carrying out ultrasonic treatment on the suspension A for 120s by using an ultrasonic crusher at 2000W ultrasonic power, and then stirring for 240min at a stirring speed of 600rmp/min to obtain a suspension B.
And step 3: standing the suspension B in a separating funnel for 6h, layering, respectively performing suction filtration on the lower layer solid C and the upper layer suspension D, washing with n-hexane for several times, and keeping the temperature in a vacuum drying oven at 50 ℃ for 24 to respectively obtain off-white powder AlH3-C3.45g and AlH3-D1.52g。
And 4, step 4: all-in-one AlH3、AlH3-C and AlH3D H content test and AlH of basic formula3Impact and friction sensitivities of/AP/CL-20/H-16/other adjuvants, the results show: as received AlH3Crude product, AlH3-C and AlH3-hydrogen content of D9.944%, 9.981% and 8.652%, respectively; as received AlH3The impact sensitivity of the crude product/AP/CL-20/H-16/other auxiliary agent system is: 4.6J, 96% of friction sensitivity, AlH3The impact sensitivity of the-C/AP/CL-20/H-16/other auxiliary agent system is 9.9J, and the friction sensitivity is 36%; AlH3The impact sensitivity of the-D/AP/CL-20/H-16/other auxiliary system was 4.3J and the friction sensitivity was 84%.
Example 7
alpha-AlH3The flotation method comprises the following steps:
step 1: weighing 5g of AlH3Placing the crude product in 500mL beaker, accurately measuring 100mL oleic acid and 100mL linolenic acid, and stirring with magnetic force of 400r/min to obtain AlH3The crude product is completely wetted by oleic acid and linolenic acid to obtain suspension A.
Step 2: and (4) carrying out ultrasonic treatment on the suspension A for 300s by using an ultrasonic crusher at the ultrasonic power of 1000W, and then stirring for 360min at the stirring speed of 600rmp/min to obtain suspension B.
And step 3: standing the suspension B in a separating funnel for 12h, layering, respectively performing suction filtration on the lower layer solid C and the upper layer suspension D, washing with n-hexane for several times, and keeping the temperature in a vacuum drying oven at 40 ℃ for 24 hours to obtainOff-white powder AlH3-C3.84g and AlH3-D1.08g。
And 4, step 4: all-in-one AlH3、AlH3-C and AlH3D H content test and AlH of basic formula3Impact and friction sensitivities of/AP/CL-20/H-16/other adjuvants, the results show: as received AlH3Crude product, AlH3-C and AlH3-hydrogen content of D9.944%, 9.967% and 8.752%, respectively; as received AlH3The impact sensitivity of the crude product/AP/CL-20/H-16/other auxiliary agent system is: 4.6J, 96% of friction sensitivity, AlH3The impact sensitivity of the-C/AP/CL-20/H-16/other auxiliary agent system is 9.5J, and the friction sensitivity is 28%; AlH3The impact sensitivity of the-D/AP/CL-20/H-16/other auxiliary system is 4.2J and the friction sensitivity is 100%.
Example 8
alpha-AlH3The flotation method comprises the following steps:
step 1: weighing 5g of AlH3Placing the crude product in a 500mL beaker, accurately measuring 250mL of oleic acid, and stirring with magnetic force of 400r/min to obtain AlH3The crude product was completely wetted with oleic acid to give suspension A.
Step 2: and (4) carrying out ultrasonic treatment on the suspension A for 600s by using an ultrasonic crusher at the ultrasonic power of 800W, and then stirring for 300min at the stirring speed of 600rmp/min to obtain suspension B.
And step 3: standing the suspension B in a separating funnel for 12h, layering, respectively performing suction filtration on the lower layer solid C and the upper layer suspension D, washing with n-hexane for several times, and keeping the temperature in a vacuum drying oven at 40 ℃ for 12h to respectively obtain off-white powder AlH3-C3.48g and AlH3-D1.35g。
And 4, step 4: all-in-one AlH3、AlH3-C and AlH3D H content test and AlH of basic formula3Impact and friction sensitivities of/AP/CL-20/H-16/other adjuvants, the results show: as received AlH3Crude product, AlH3-C and AlH3-hydrogen content of D9.944%, 9.972% and 8.578%, respectively; as received AlH3The impact sensitivity of the crude product/AP/CL-20/H-16/other auxiliary agent system is: 4.6J, rubSensitivity 96% AlH3The impact sensitivity of the-C/AP/CL-20/H-16/other auxiliary agent system is 8.3J, and the friction sensitivity is 48%; AlH3The impact sensitivity of the-D/AP/CL-20/H-16/other auxiliary system was 4.1J and the friction sensitivity was 92%.
The above-mentioned embodiments are further illustrative of the present invention, but it should not be construed that the scope of the present invention is limited to the embodiments. All the technologies realized based on the above contents belong to the scope of the present invention.
Claims (2)
1. alpha-AlH3A flotation process, characterized in that the process comprises the steps of:
s1: reacting AlH3Dispersing the crude product in a flotation solution to form a suspension A;
s2: ultrasonically crushing the suspension A by using an ultrasonic crusher, and then stirring to obtain a suspension B;
s3: pouring the suspension B into a separating funnel, standing and layering, taking the lower layer solid as C and the upper layer suspension as D, separating the lower layer solid C from the upper layer suspension D, washing, filtering and vacuum drying the lower layer solid C to obtain the alpha crystal form AlH3；
In the step S1, AlH3The crude product is AlH produced by industrialized ether synthesis method3The crude product is a flotation solution which is one or a mixture of more than two of oleic acid, linoleic acid, linolenic acid and arachidonic acid, and AlH3The mass ratio of the crude product to the flotation solution is 1: 20-100;
in the step S2, the ultrasonic pulverization power is 400-;
in the step S3, the standing time is 2-72h, the solvent used for washing is cyclohexane, n-hexane or ethyl acetate, the vacuum drying temperature is 30-50 ℃, and the vacuum drying time is 6-48 h.
2. An alpha-AlH obtained according to claim 13The application of (2), which is characterized in that: alpha-AlH3Use as fuel in propellants or explosivesThe field of energetic materials.
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