Preparation method and system for alane and use of alane

Abstract

Provided are a preparation method and system for an alane and a use of the alane. The method comprises: preparation of triethylaluminum: using triethylaluminum as a seed and aluminum and hydrogen as raw materials to synthesize triethylaluminum by means of a direct synthesis method, wherein the newly synthesized triethylaluminum comprises triethylaluminum in an amount equal to the seed and triethylaluminum for alane synthesis; and preparation of alane: thermally decomposing the triethylaluminum for alane synthesis to obtain the alane, wherein the newly synthesized triethylaluminum in an amount equal to the seed is used as a new seed for new preparation of triethylaluminum. The present invention only consumes aluminum and hydrogen required for generating the alane during the preparation of alane, and other raw materials can achieve a balance between consumption and output during the production process, achieving recycling, low production costs, high safety performance, and low emissions.

Description

Preparation method, preparation system and application of alane TECHNICAL FIELD

[0001] The present application relates to the technical field of organic synthesis, and in particular to a preparation method, a preparation system and an application of alane. BACKGROUND

[0002] Alane (AlH3), also known as aluminum trihydride, is a high-energy material. Alane has a high hydrogen density (mass density of 10.08wt.% and volume density of 0.148 kg / L), a relatively low hydrogen release temperature and reaction enthalpy, and a high controllable hydrogen product purity, and thus is an ideal hydrogen storage material that can be matched with fuel cells.

[0003] However, alane has at least seven known polymorphs, a high synthesis difficulty, a controllable chemical property difficulty and a high production cost, so that the application range of alane as an energy product is very limited. Due to the thermodynamic characteristics of the reaction, the room temperature hydrogen equilibrium pressure of aluminum metal is at the level of 7 kbar (0.7 GPa), so only under a very high hydrogen pressure (>0.7 GPa), aluminum metal can directly react with hydrogen to generate alane, and such a reaction condition cannot be realized in industrial production, and the alane crystal produced by the direct reaction of high-pressure hydrogen and metal is difficult to realize controllability of properties.

[0004] At present, the synthesis of alane mostly adopts a liquid-phase organic chemical synthesis method and its variants, the principle of which is to use an excessive amount of lithium aluminum hydride to react with aluminum chloride in an anhydrous ether solvent to obtain an ether complex of alane, and then to obtain non-solvated alane by de-etherization and crystallization. For example, CN 106946224 A discloses a method for preparing alpha-aluminum trihydride by mixing lithium aluminum hydride and aluminum trihydride. Generally, a large amount of benzene solvent is used in combination to ensure the crystallization effect. Such a liquid-phase organic chemical synthesis method has a high yield and is relatively mature, but a large amount of lithium aluminum hydride and ether is required as raw materials, and the consumption of lithium leads to a high production cost and a safety hazard in the production process. In addition, the hydrogen gas that needs to be widely consumed is not a raw material required by the synthesis method, so if alane is used as a hydrogen supply material for fuel cells, the production method is difficult to achieve economy. TECHNICAL PROBLEM

[0005] In view of the technical features of the existing alane synthesis technology, how to reduce the preparation cost of alane and improve the production safety is a technical problem to be solved by those skilled in the art. TECHNICAL SOLUTION

[0006] To solve the above technical problems, the present application proposes the following technical solutions:

[0007] The first aspect of the present application provides an aluminum alkane preparation method, which comprises:

[0008] Preparation of triethylaluminum: triethylaluminum is synthesized by using direct synthesis method with triethylaluminum as seed and aluminum and hydrogen as raw materials; the newly synthesized triethylaluminum contains triethylaluminum equivalent to the seed and triethylaluminum for aluminum alkane synthesis;

[0009] Preparation of aluminum alkane: triethylaluminum for aluminum alkane synthesis is thermally decomposed to obtain aluminum alkane;

[0010] Preparation of triethylaluminum: triethylaluminum is synthesized by using direct synthesis method with triethylaluminum as seed and aluminum and hydrogen as raw materials; the newly synthesized triethylaluminum contains triethylaluminum equivalent to the seed and triethylaluminum for aluminum alkane synthesis;

[0011] In some embodiments, the preparation method of aluminum alkane comprises the following steps:

[0012] Preparation of diethylaluminum hydride: hydrogen and triethylaluminum as seed are added to aluminum suspension in a first reaction kettle to generate diethylaluminum hydride;

[0013] Preparation of triethylaluminum: the generated diethylaluminum hydride is added to a second reaction kettle, raw material ethylene is introduced into the second reaction kettle, and the newly synthesized triethylaluminum is generated by heating.

[0014] In some embodiments, the preparation method of aluminum alkane comprises the following steps:

[0015] Preparation of triethylaluminum: the generated diethylaluminum hydride is added to a second reaction kettle, raw material ethylene is introduced into the second reaction kettle, and the newly synthesized triethylaluminum is generated by heating.

[0016] In some embodiments, the preparation method of aluminum alkane comprises the following steps:

[0017] In some embodiments, the preparation method of aluminum alkane comprises the following steps:

[0018] In some embodiments, the reaction conditions in the third reactor in the method for preparing aluminum hydride are as follows: the gas in the third reactor is hydrogen, the hydrogen pressure in the third reactor is 3-6 MPa after the third reactor is sealed, the reaction temperature is 150-180°C, and the reaction time is 6-10 hours.

[0019] The second aspect of the application also provides a system for preparing aluminum hydride, which uses the above method for preparing aluminum hydride, and comprises:

[0020] a first reactor and a second reactor for preparing triethylaluminum; triethylaluminum is synthesized by using direct synthesis method with triethylaluminum as seed; the newly synthesized triethylaluminum comprises triethylaluminum with the same molar mass as the seed and triethylaluminum for synthesizing aluminum hydride;

[0021] a third reactor for preparing aluminum hydride; aluminum hydride is obtained by thermal decomposition of triethylaluminum for synthesizing aluminum hydride;

[0022] a communication pipeline for communicating the first reactor and the second reactor, and for conveying the newly synthesized triethylaluminum with the same molar mass as the seed in the second reactor to the first reactor as a new seed for synthesizing triethylaluminum.

[0023] In some embodiments, the system for preparing aluminum hydride further comprises:

[0024] a gas separation device connected to the gas output end of the third reactor and in communication with the gas output end of the third reactor; the gas separation device is used for separating hydrogen and ethylene output by the third reactor;

[0025] a solvent purification and recycling system connected to the solvent output end of the third reactor and used for purifying the solvent and recycling the purified solvent.

[0026] In some embodiments, the system for preparing aluminum hydride further comprises:

[0027] a hydrogen purification and circulation system for purifying hydrogen; the hydrogen purification and circulation system comprises a plurality of first input ends and a plurality of first output ends; the plurality of first input ends are respectively connected to the hydrogen output end of the gas separation device and the hydrogen output end of the first reactor; the plurality of first output ends are respectively connected to the hydrogen input end of the first reactor and the hydrogen input end of the third reactor;

[0028] a plurality of first booster pumps correspondingly arranged at the first output ends; the first booster pumps increase the hydrogen pressure to a preset value before the hydrogen is delivered to the first reactor and the third reactor.

[0029] An ethylene purification circulation system for purifying ethylene, comprising a plurality of second input ends and a second output end; the second input ends are connected with ethylene output ends of the second reaction kettle and the gas separation device respectively; the second output end is connected with an ethylene input end of the second reaction kettle;

[0030] A second booster pump is correspondingly arranged at the second output end, and the second booster pump increases the ethylene gas pressure delivered to the second reaction kettle to a preset value;

[0031] After the reaction of the first reaction kettle, the second reaction kettle and the third reaction kettle ends, the residual hydrogen and ethylene are correspondingly delivered to the hydrogen purification circulation system and the ethylene purification circulation system for purification and recycling.

[0032] The third aspect of the present application also provides the application of the aluminum hydride prepared by the above preparation method as a hydrogen material for a fuel cell. Advantages

[0033] The aluminum hydride preparation method, preparation system and application thereof complete hydrogenation through a synthesis process of triethylaluminum, so that hydrogen enters the material system; under the action of a surfactant, triethylaluminum is pyrolyzed to synthesize aluminum hydride. The method completes the storage of hydrogen in the carrier metal aluminum through a chemical process, is suitable for synthesizing aluminum hydride for the purpose of hydrogen storage fuel, and can be used for the regeneration of aluminum powder left after the release of hydrogen from aluminum hydride. Meanwhile, the method does not need to use a large amount of lithium aluminum hydride and ether solvents, so that the cost can be obviously reduced, and the safety is higher.

[0034] The aluminum hydride preparation method, preparation system and application thereof consume only raw materials aluminum and hydrogen in the whole preparation method, and other substances participating in the reaction can be generated in equal amounts in the preparation process, and can be recycled in the preparation process of aluminum hydride. Indirectly, aluminum and hydrogen are used as raw materials to produce aluminum hydride, the production process is controllable, the raw material utilization efficiency is high, and the emission is reduced. Industrial production has high safety factor, low production cost, and can realize large-scale batch production. BRIEF DESCRIPTION OF DRAWINGS

[0035] Fig. 1 is a first flowchart of the aluminum hydride preparation method according to the present application;

[0036] Fig. 2 is a second flowchart of the aluminum hydride preparation method according to the present application;

[0037] Fig. 3 is a structural schematic diagram of the aluminum hydride preparation system according to the present application;

[0038] Fig. 4 is an XRD diagram of the aluminum hydride prepared by the aluminum hydride preparation method according to the present application in Example 1 and Example 2;

[0039] Figure 5 is a TEM image of aluminum ane prepared by the aluminum ane preparation method described in Example 1 of the present invention;

[0040] Figure 6 is a TEM image of aluminum ane prepared using the aluminum ane preparation method described in Example 2 of this invention. The best embodiment of the present invention

[0041] Preferred exemplary embodiments of the present invention will now be described in detail with reference to the accompanying drawings. This detailed description should not be considered as a limitation of the present invention, but rather as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0042] It should be understood that the terminology used in this invention is merely for describing particular embodiments and is not intended to limit the invention. Furthermore, with respect to numerical ranges in this invention, it should be understood that the upper and lower limits of the range and each intermediate value between them are specifically disclosed. Any stated value or intermediate value within a stated range, as well as each smaller range between any other stated value or intermediate value within said range, are also included in this invention. The upper and lower limits of these smaller ranges may be independently included or excluded from the range.

[0043] Unless otherwise stated, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. While only preferred methods and materials have been described herein, any methods and materials similar or equivalent to those described herein may be used in the implementation or verification of this invention. All references to this specification are incorporated by way of citation to disclose and describe methods and / or materials associated with those references. In the event of any conflict with any incorporated reference, the content of this specification shall prevail.

[0044] The terms "comprising," "including," "having," "containing," etc., used in this document are open-ended, meaning they include but are not limited to. The term "and / or" as used in this document includes any or all of the stated items. Unless otherwise stated, % refers to a percentage by mass or volume.

[0045] As shown in Figures 1 and 2, the present invention provides a method for preparing aluminum alkane, comprising:

[0046] The preparation of triethylaluminum includes:

[0047] Preparation of diethylaluminum hydride: In the first reaction vessel, hydrogen and triethylaluminum as a seed are added to an aluminum suspension to generate diethylaluminum hydride;

[0048] First Reactor:

[0049] Preparation of triethylaluminum: all the diethylaluminum hydride generated in the first reaction kettle is added into the second reaction kettle, raw material ethylene is introduced into the second reaction kettle, and new synthesized triethylaluminum is generated by heating.

[0050] Second reaction kettle:

[0051] Preparation of aluminum hydride: in the third reaction kettle, aluminum hydride is obtained by thermal decomposition of triethylaluminum for aluminum hydride synthesis under the action of a surfactant, and new ethylene is generated;

[0052] Third reaction kettle:

[0053] The total reaction of the three reaction kettles is:

[0054] In the second reaction kettle, the amount of is equal to the amount of consumed in the first reaction kettle and the third reaction kettle, and the amount of generated in the third reaction kettle is equal to the amount of consumed in the second reaction kettle, that is, in the entire preparation process of aluminum hydride, only raw materials aluminum and hydrogen are consumed, and other raw materials can be generated in the preparation process. Recycle.

[0055] In the above scheme, the aluminum suspension preparation process is prepared by fully mixing aluminum powder and solvent at room temperature. The solvent is a solvent that does not dissolve aluminum hydride, and further, the solvent is an alkane solvent that can dissolve the selected surfactant, such as cyclohexane, dodecane.

[0056] In the above scheme, in the reaction kettle 3, the concentration of the surfactant is 0.3 mM to 6 mM; in some embodiments, the concentration of the surfactant is 0.3 mM, 0.5 mM, 1 mM, 1.5 mM, 2 mM, 2.5 mM, 3 mM, 3.5 mM, 4 mM, 4.5 mM, 5 mM, 5.5 mM or 6 mM.

[0057] The surfactant is a long-chain surfactant that can effectively stabilize the aluminum hydride generated by the decomposition of triethylaluminum, such as sodium dodecyl sulfate SDS, cetyltrimethylammonium bromide CTAB or sodium triacetoxyborohydride STAB.

[0058] In the above scheme, the reaction conditions in the first reaction kettle are: the gas in the first reaction kettle is hydrogen, the internal hydrogen pressure of the first reaction kettle after sealing is 6 MPa to 10 MPa, the reaction temperature is 100°C to 150°C, and the reaction time is 2h to 6h.

[0059] In some embodiments, the reaction conditions in the first reaction kettle are:

[0060] The hydrogen pressure inside the first reactor after sealing is 6 MPa, 7 MPa, 8 MPa, 9 MPa or 10 MPa;

[0061] The reaction temperature inside the first reactor is 100°C, 110°C, 120°C, 125°C, 130°C, 140°C or 150°C;

[0062] The reaction time inside the first reactor is 2 h, 3 h, 4 h, 5 h or 6 h.

[0063] In some embodiments, the reaction conditions inside the second reactor are:

[0064] The ethylene pressure inside the second reactor after sealing is 0.4 MPa, 0.5 MPa, 0.6 MPa, 0.7 MPa, 0.8 MPa, 0.9 MPa or 1 MPa;

[0065] The reaction temperature inside the second reactor is 60°C, 70°C, 75°C, 80°C, 90°C or 100°C;

[0066] The reaction time inside the second reactor is 5 h, 6 h, 6.5 h, 7 h or 8 h.

[0067] In the above scheme, the reaction conditions in the third reactor are:

[0068] The hydrogen pressure inside the third reactor after sealing is 3 MPa, 4 MPa, 4.5 MPa, 5 MPa or 6 MPa;

[0069] The reaction temperature inside the third reactor is 150°C, 160°C, 165°C, 170°C, 175°C or 180°C;

[0070] The reaction time inside the third reactor is 6 h, 7 h, 7.5 h, 8 h, 9 h or 10 h.

[0071] As shown in FIG. 3, the second aspect of the present application further provides a system for preparing aluminum hydride, which uses the above preparation method, and the system comprises:

[0072] A first reactor, raw materials: triethylaluminum (seed), hydrogen, and aluminum and solvent prepared into a suspension; internal gas: hydrogen; final product: diethylaluminum hydride and solvent not involved in the reaction;

[0073] A first communication pipeline, which communicates the first reactor and the second reactor; the communication pipeline transports the final product in the first reactor to the second reactor;

[0074] The second reactor, raw material: diethylaluminum hydride and ethylene generated in the first reactor react to generate newly synthesized triethylaluminum; internal gas: ethylene; final product: liquid product, the liquid product including triethylaluminum and solvent; wherein, the amount of triethylaluminum contained in 2 / 3 of the liquid product is the same as the amount of triethylaluminum as seed in the first reactor, the 2 / 3 of the liquid product is transported to the first reactor for cyclic production, and the remaining 1 / 3 of the liquid product is transported to the third reactor for production of alane;

[0075] The second connecting pipeline is connected to the second reactor and the third reactor, and the remaining 1 / 3 of the liquid product is transported to the third reactor for production of alane;

[0076] The third connecting pipeline is connected to the second reactor and the first reactor, and the 2 / 3 of the liquid product is transported to the first reactor for cyclic production;

[0077] The third reactor, raw material: triethylaluminum; internal gas: hydrogen; final product: alane, hydrogen and ethylene;

[0078] The gas separation device connected to the gas output end of the third reactor is in communication with the gas output end of the third reactor; the gas separation device is used to separate hydrogen and ethylene output by the third reactor;

[0079] The solvent purification and recycling system connected to the solvent output end of the third reactor is used to purify the solvent and recycle it.

[0080] In some embodiments, the gas separation device can adopt a gas module separation device, a pressure swing adsorption device, a low-temperature distillation device, etc., wherein the gas module separation device can adopt a palladium-based metal membrane, a carbon molecular sieve membrane (CMSM), an electrochemical hydrogen pump membrane (EHPM) and an ionic liquid (IL) membrane to separate hydrogen from the mixed gas of hydrogen and ethylene.

[0081] The hydrogen purification and circulation system is used to purify hydrogen; it includes a plurality of first input ends and a plurality of first output ends; the plurality of first input ends are respectively connected to the hydrogen output end of the gas separation device, the hydrogen output end of the first reactor; the plurality of first output ends are respectively connected to the hydrogen input end of the first reactor and the hydrogen input end of the third reactor;

[0082] The plurality of first booster pumps are correspondingly arranged at the first output ends, and the first booster pumps increase the pressure of the hydrogen transported to the first reactor and the third reactor to a preset value.

[0083] An ethylene purification circulation system for purifying ethylene, comprising a plurality of second input ends and a second output end; the second input ends are connected with ethylene output ends of the second reactor and the gas separation device respectively; the second output end is connected with an ethylene input end of the second reactor;

[0084] A second booster pump is correspondingly arranged at the second output end, and the second booster pump increases the ethylene gas pressure delivered to the second reactor to a preset value;

[0085] After the first reactor, the second reactor and the third reactor are reacted, the residual hydrogen and ethylene are correspondingly delivered to the hydrogen purification circulation system and the ethylene purification circulation system for purification and recycling.

[0086] In a third aspect, the application also provides an application of the aluminum hydride prepared by the above preparation method as a hydrogen supply material for a fuel cell. The aluminum hydride preparation method provided by the application consumes aluminum and hydrogen as raw materials, hydrogen as one of the raw materials, hydrogen directly enters the production process and is finally converted into aluminum hydride, and the storage of hydrogen in the carrier metal aluminum is completed, which is suitable for synthesizing aluminum hydride for the purpose of hydrogen-loaded fuel.

[0087] The following is a preferred embodiment of the application:

[0088] Embodiment 1

[0089] This embodiment prepares aluminum hydride according to the following steps, and the specific steps are as follows:

[0090] 1. 54 g of aluminum powder and 18 L of cyclohexane are added to the first reactor, and the mixture is fully mixed at room temperature to form a suspension. 914 g of triethylaluminum is added to the aluminum powder suspension, and the reactor is sealed after fully mixing and stirring;

[0091] 2. The first reactor is vacuumed, and then 10 MPa of hydrogen pressure is filled into the first reactor. The reactor is heated to 130°C and kept for 5 hours;

[0092] 3. After the reaction is completed, the temperature is reduced to room temperature, the residual hydrogen in the first reactor is recovered, and the liquid product is introduced into the second reactor;

[0093] 4. The second reactor is vacuumed, and then 0.5 MPa of ethylene is filled into the second reactor. The temperature is raised to 80°C and kept for 6 hours to obtain a liquid product;

[0094] 5. After the reaction is completed, the temperature is reduced to room temperature, the residual ethylene in the second reactor is recovered, 2 / 3 of the liquid product is used as a new triethylaluminum seed, and the remaining 1 / 3 of the liquid product is introduced into the third reactor for decomposition;

[0095] 6. Add 4 g CTAB to the third reactor containing the triethylaluminum to be decomposed, and charge 6 MPa of hydrogen pressure, then raise the temperature of the third reactor 3 to 160°C and maintain for 8 hours;

[0096] 7. After the reaction is completed, reduce to room temperature, and recover the gas in the reactor; filter the solid-liquid mixture after the reaction, collect the solid product, wash repeatedly with anhydrous ethanol for three times, and then place in a vacuum dryer at 50°C to obtain 58 g of product aluminum hydride. Yield: 98%, purity: 96%. (The synthesized aluminum hydride contains a small amount of surfactant)

[0097] Example 2

[0098] 1. Add 54 mg of aluminum powder and 18 mL of cyclohexane to the first reactor, mix thoroughly at room temperature to form a suspension, add 914 mg of triethylaluminum to the aluminum powder suspension, mix thoroughly after stirring, and seal the first reactor;

[0099] 2. Vacuumize the first reactor, then charge 8 MPa of hydrogen pressure to the first reactor, raise the temperature of the first reactor to 130°C and maintain for 4 hours;

[0100] 3. After the reaction is completed, reduce the temperature of the first reactor to room temperature, recover the remaining hydrogen gas in the reactor, and introduce the final product of the first reactor to the second reactor;

[0101] 4. Vacuumize the second reactor, then charge 0.5 MPa of ethylene to the reactor, raise the temperature to 80°C and maintain for 6 hours to obtain a liquid product;

[0102] 5. After the reaction is completed, reduce the temperature to room temperature, recover the remaining ethylene in the reactor, use 2 / 3 of the liquid product as the triethylaluminum seed for the next batch of reaction, and transport the remaining 1 / 3 of the liquid product to the third reactor to be decomposed.

[0103] 6. Add 10 mg of STAB to the third reactor containing the triethylaluminum to be decomposed, and charge 6 MPa of hydrogen pressure, then raise the temperature of the third reactor 3 to 150°C and maintain for 6 hours;

[0104] 7. After the reaction is completed, reduce to room temperature, and recover the gas in the reactor; filter the solid-liquid mixture after the reaction, collect the solid product, wash repeatedly with anhydrous ethanol for three times, and then place in a vacuum dryer at 50°C to obtain 59 mg of product aluminum hydride. Yield: 98%, purity: 96%. (The synthesized aluminum hydride contains a small amount of surfactant)

[0105] As shown in FIG. 3 to FIG. 5, the aluminum hydride prepared in Example 1 and Example 2 was subjected to X-ray diffraction phase analysis, and obvious aluminum hydride characteristic peaks were observed in the spectrum, proving the successful synthesis of aluminum hydride. Under transmission electron microscope observation, under the stabilizing action of the surfactant, the prepared aluminum hydride particles were nanoscale.

[0106] The above merely illustrates the specific embodiments of the present application, and some modifications or improvements can be made on the basis of the present application, which is obvious to those skilled in the art. Therefore, these modifications or improvements made on the basis of not deviating from the spirit of the present application, all belong to the scope of the present application. Embodiments of the present application

[0107] Enter the embodiment description paragraph of the present application here. Industrial applicability

[0108] The present application directly uses hydrogen as raw material, and completes the storage of hydrogen in carrier metal aluminum through a chemical process, is suitable for synthesizing aluminum hydride for the purpose of hydrogen carrier fuel, and can be used for the regeneration of aluminum powder left after the release of hydrogen from aluminum hydride; at the same time, compared with the prior art, the cost can be significantly reduced, and the safety is higher. In addition, according to the production process designed by the present method, most of the chemical raw materials can be recycled within the process, improving the raw material utilization efficiency and atomic economy, and reducing emissions; compared with the prior art, the aluminum hydride preparation method described in the present application has high safety performance, low production cost, very good input-output ratio, and high economic efficiency when used for large-scale industrial production. Free content of sequence listing

[0109] Enter the free content description paragraph of the sequence listing here.

Claims

1. A process for the preparation of an aluminum hydride, characterized in that, The preparation of triethylaluminum includes the preparation of diethylaluminum hydride and the preparation of newly synthesized triethylaluminum: in a first reaction kettle, hydrogen and triethylaluminum as seeds are added to an aluminum suspension to generate diethylaluminum hydride; the generated diethylaluminum hydride is added to a second reaction kettle, raw material ethylene is introduced into the second reaction kettle, and heating generates newly synthesized triethylaluminum; the newly synthesized triethylaluminum contains triethylaluminum equivalent to the seeds and triethylaluminum for aluminum hydride synthesis; The preparation of aluminum hydride: in a third reaction kettle, triethylaluminum for aluminum hydride synthesis is thermally decomposed under the action of a surfactant to obtain aluminum hydride and newly generated ethylene; The newly synthesized triethylaluminum equivalent to the seeds is used as a new seed for the preparation of new triethylaluminum; the newly generated ethylene is equivalent in amount to the raw material ethylene, and the newly generated ethylene is recycled and purified for the preparation of triethylaluminum; The surfactant is a long-chain surfactant; the surfactant concentration is 0.3 mM to 6 mM; the gas in the third reaction kettle is hydrogen, the hydrogen pressure in the third reaction kettle is 3-6 MPa, the reaction temperature is 150-180℃, and the reaction time is 6-10 h. The reaction conditions in the first reaction kettle are as follows: the gas in the first reaction kettle is hydrogen, the hydrogen pressure in the first reaction kettle is 6 MPa to 10 MPa after sealing, the reaction temperature is 100℃ to 150℃, and the reaction time is 2 h to 6 h.

2. The method for preparing aluminum alkylene according to claim 1, characterized in that, The reaction conditions in the second reaction kettle are as follows: the gas in the second reaction kettle is ethylene, the ethylene pressure in the second reaction kettle is 0.4 MPa to 1 MPa after sealing, the reaction temperature is 60℃ to 100℃, and the reaction time is 5 h to 8 h.

3. The method for preparing aluminum alkylene according to claim 1, characterized in that, The preparation of triethylaluminum includes the preparation of diethylaluminum hydride and the preparation of newly synthesized triethylaluminum: in a first reaction kettle, hydrogen and triethylaluminum as seeds are added to an aluminum suspension to generate diethylaluminum hydride; the generated diethylaluminum hydride is added to a second reaction kettle, raw material ethylene is introduced into the second reaction kettle, and heating generates newly synthesized triethylaluminum; the newly synthesized triethylaluminum contains triethylaluminum equivalent to the seeds and triethylaluminum for aluminum hydride synthesis; 4. An aluminum alkane production system using the production method according to any one of claims 1 to 3, characterized by, The preparation of aluminum hydride: in a third reaction kettle, triethylaluminum for aluminum hydride synthesis is thermally decomposed under the action of a surfactant to obtain aluminum hydride and newly generated ethylene; The newly synthesized triethylaluminum equivalent to the seeds is used as a new seed for the preparation of new triethylaluminum; the newly generated ethylene is equivalent in amount to the raw material ethylene, and the newly generated ethylene is recycled and purified for the preparation of triethylaluminum; The surfactant is a long-chain surfactant; the surfactant concentration is 0.3 mM to 6 mM; the gas in the third reaction kettle is hydrogen, the hydrogen pressure in the third reaction kettle is 3-6 MPa, the reaction temperature is 150-180℃, and the reaction time is 6-10 h. The reaction conditions in the first reaction kettle are as follows: the gas in the first reaction kettle is hydrogen, the hydrogen pressure in the first reaction kettle is 6 MPa to 10 MPa after sealing, the reaction temperature is 100℃ to 150℃, and the reaction time is 2 h to 6 h.

5. The aluminum alkane production system of claim 4, wherein, The reaction conditions in the second reaction kettle are as follows: the gas in the second reaction kettle is ethylene, the ethylene pressure in the second reaction kettle is 0.4 MPa to 1 MPa after sealing, the reaction temperature is 60℃ to 100℃, and the reaction time is 5 h to 8 h. The preparation of triethylaluminum includes the preparation of diethylaluminum hydride and the preparation of newly synthesized triethylaluminum: in a first reaction kettle, hydrogen and triethylaluminum as seeds are added to an aluminum suspension to generate diethylaluminum hydride; the generated diethylaluminum hydride is added to a second reaction kettle, raw material ethylene is introduced into the second reaction kettle, and heating generates newly synthesized triethylaluminum; the newly synthesized triethylaluminum contains triethylaluminum equivalent to the seeds and triethylaluminum for aluminum hydride synthesis; The preparation of aluminum hydride: in a third reaction kettle, triethylaluminum for aluminum hydride synthesis is thermally decomposed under the action of a surfactant to obtain aluminum hydride and newly generated ethylene; The newly synthesized triethylaluminum equivalent to the seeds is used as a new seed for the preparation of new triethylaluminum; the newly generated ethylene is equivalent in amount to the raw material ethylene, and the newly generated ethylene is recycled and purified for the preparation of triethylaluminum; 6. The aluminum alkane production system of claim 5, wherein, The surfactant is a long-chain surfactant; the surfactant concentration is 0.3 mM to 6 mM; the gas in the third reaction kettle is hydrogen, the hydrogen pressure in the third reaction kettle is 3-6 MPa, the reaction temperature is 150-180℃, and the reaction time is 6-10 h. The reaction conditions in the first reaction kettle are as follows: the gas in the first reaction kettle is hydrogen, the hydrogen pressure in the first reaction kettle is 6 MPa to 10 MPa after sealing, the reaction temperature is 100℃ to 150℃, and the reaction time is 2 h to 6 h. The reaction conditions in the second reaction kettle are as follows: the gas in the second reaction kettle is ethylene, the ethylene pressure in the second reaction kettle is 0.4 MPa to 1 MPa after sealing, the reaction temperature is 60℃ to 100℃, and the reaction time is 5 h to 8 h. The preparation of triethylaluminum includes the preparation of diethylaluminum hydride and the preparation of newly synthesized triethylaluminum: in a first reaction kettle, hydrogen and triethylaluminum as seeds are added to an aluminum suspension to generate diethylaluminum hydride; the generated diethylaluminum hydride is added to a second reaction kettle, raw material ethylene is introduced into the second reaction kettle, and heating generates newly synthesized triethylaluminum; the newly synthesized triethylaluminum contains triethylaluminum equivalent to the seeds and triethylaluminum for aluminum hydride synthesis; The preparation of aluminum hydride: in a third reaction kettle, triethylaluminum for aluminum hydride synthesis is thermally decomposed under the action of a surfactant to obtain aluminum hydride and newly generated ethylene; The newly synthesized triethylaluminum equivalent to the seeds is used as a new seed for the preparation of new triethylaluminum; the newly generated ethylene is equivalent in amount to the raw material ethylene, and the newly generated ethylene is recycled and purified for the preparation of triethylaluminum; The surfactant is a long-chain surfactant; the surfactant concentration is 0.3 mM to 6 mM; the gas in the third reaction kettle is hydrogen, the hydrogen pressure in the third reaction kettle is 3-6 MPa, the reaction temperature is 150-180℃, and the reaction time is 6-10 h. The reaction conditions in the first reaction kettle are as follows: the gas in the first reaction kettle is hydrogen, the hydrogen pressure in the first reaction kettle is 6 MPa to 10 MPa after sealing, the reaction temperature is 100℃ to 150℃, and the reaction time is 2 h to 6 h. The reaction conditions in the second reaction kettle are as follows: the gas in the second reaction kettle is ethylene, the ethylene pressure in the second reaction kettle is 0.4 MPa to 1 MPa after sealing, the reaction temperature is 60℃ to 100℃, and the reaction time is 5 h to 8 h. A plurality of first booster pumps are correspondingly arranged at the first output end, and the first booster pumps increase the hydrogen pressure delivered to the first reactor and the third reactor to a preset value; An ethylene purification circulation system is used for purifying ethylene, and includes a plurality of second input ends and a second output end; the second input ends are respectively connected with the ethylene output end of the second reactor and the ethylene output end of the gas separation device; and the second output end is connected with the ethylene input end of the second reactor; A second booster pump is correspondingly arranged at the second output end, and the second booster pump increases the ethylene pressure delivered to the second reactor to a preset value; After the first reactor, the second reactor and the third reactor are reacted, the residual hydrogen and ethylene are correspondingly delivered to the hydrogen purification circulation system and the ethylene purification circulation system for purification and recycling.

Images