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Diethylaluminum chloride, molecular formula C4H10AlCl, CAS 96-10-6, appears as a colorless transparent liquid. This clear liquid state makes its operation in laboratories and industrial production relatively intuitive, but it also reminds us that although it may seem ordinary, it has extremely high chemical activity. It is easily soluble in organic solvents such as xylene and gasoline, and this good solubility provides convenience for its application in organic synthesis. However, this also means that once the material leaks, it may quickly mix with surrounding organic solvents, forming a more difficult to handle mixture, increasing the difficulty and danger of handling. As a highly active compound, it also exhibits some unique chemical properties. As an organic compound, it has a wide range of applications in the chemical field, especially as a catalyst in the polyolefin industry and as an intermediate in the manufacturing of organic compounds.
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C.F |
C4H10AlCl |
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E.M |
120 |
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M.W |
121 |
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m/z |
120 (100.0%), 122 (32.0%), 121 (4.3%), 123 (1.4%) |
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E.A |
C, 39.85; H, 8.36; Al, 22.38; Cl, 29.41 |
Diethyl aluminum cloride is an important organic reaction catalyst, for example, polybutadiene can be synthesized using the neodymium neodecanoate/n-butyl lithium/diethyl aluminum chlride catalytic system. The experimental investigation examined the effects of polymerization temperature, catalyst preparation of c (Li)/c (Nd) and c (Al)/c (Nd), and alkyl aluminum species on butadiene polymerization. The results showed that the catalyst had the highest catalytic activity when c (Li)/c (Nd) was around 12 and c (Al)/c (Nd) was around 15, and the polymer yield could reach 100%. Under the conditions of 0 ℃, c (Li)/c (Nd)=12, and c (Al)/c (Nd)=15, a polymer with a high cis-1,4- structure (molar content 97.6%) and a narrow molecular weight distribution (molecular weight distribution index 1.23) can be obtained. As the polymerization temperature increases, the activity of the catalytic system increases, and the relative molecular weight and cis-1,4-structural molar content of the resulting polymer decrease.
In addition, diethylaluminum chlride can also be used to synthesize a corrosion-resistant pipeline material for water supply equipment. The raw materials are as follows by weight: 3-10 parts of polyethylene resin, 5-10 parts of nanoparticles, 5-10 parts of carbon black, 2-7 parts of hydrogenated castor oil, 2-10 parts of sodium alkyl sulfonate, 2-7 parts of chlorofluoromethane, 3-11 parts of diethylaluminum chlride, 1-3 parts of acrylonitrile butadiene styrene copolymer, 3-9 parts of silane coupling agent, 2.5-4.5 parts of antioxidant, 0.5-6.5 parts of preservative, and 1.5-3.5 parts of lubricant. The pipe material prepared from polyethylene resin has good mechanical properties, impact resistance, corrosion resistance and aging resistance, excellent comprehensive performance and high application value.
Method 1:
The synthesis of Diethylaluminum Chloride is one of the common and important stps in organic synthesis, which is usually achieved by directly chlorinating diethyl aluminum chlride (C2H5) 2AlCl).
Reaction operation stps:
(a) Chlorination reaction process:
Prepare operating environment:
Ensure that the reactor and operating environment are protected by inert gases to prevent water and oxygen in the air from interfering with the reaction.
01
Adding reactants:
-Add liquid diethylaluminum (C2H5) 2Al) to the reactor.
-By controlling the flow rate and temperature, gradually introduce chlorine gas (Cl2) or hydrogen chlride (HCl) into the reactor as a chlorine source.
02
Reaction progress:
Observe the progress of the reaction under appropriate temperature and stirring conditions. Usually, the chlorination reaction is exothermic, and the reaction mixture may produce gas.
03
Reaction time control:
According to the experimental conditions, control the reaction time to ensure that the reaction reaches complete conversion or the required degree.
04
End of reaction:
When the reaction is complete, stop introducing chlorine gas or hydrogen chlride into the reactor.
05
Product processing and extraction:
Separation and extraction:
-Cool the reaction mixture and treat it in an appropriate environment.
-Separate the pure product of diethyl aluminum chlride (C2H5) 2AlCl2) through distillation or extraction methods.
01
Product collection:
Transfer the collected diethyl aluminum chlride to a suitable storage container for subsequent use or analysis.
02
Product collection:
Transfer the collected diethyl aluminum chlride to a suitable storage container for subsequent use or analysis.
03
3. Chemical equationAccording to the above operating steps, the synthesis reaction of diethyl aluminum chlorde can be expressed by a chemical equation as follows:
(C2H5) 2Al+Cl2 → (C2H5) 2AlCl2
Or when using hydrogen cloride as a chlorine source:
(C2H5) 2Al+HCl → (C2H5) 2AlCl2
These equations describe the process of diethyl aluminum reacting with chlorine gas or hydrogen chlorde to produce diethyl aluminum chlorde. In the reaction, chlorine gas or hydrogen chlorde provides chlorine atoms and reacts with diethyl aluminum to form the target product, diethyl aluminum chlorde.
Protective measures
Respiratory protection: Wear a gas mask when the concentration in the air is high. During emergency rescue or evacuation, it is necessary to wear a positive pressure respirator.
Eye protection: Wear chemical safety goggles.
Body protection: Wear protective clothing with adhesive tape.
Hand protection: Wear chemical resistant gloves.
Other: Minimize direct contact as much as possible.
Emergency measures
Skin contact: Remove contaminated clothing, wipe away toxins with gasoline or alcohol, do not rinse with water. Seek medical attention. Treat according to chemical burns.
Eye contact: Lift the eyelids and rinse with flowing water for 15 minutes. Seek medical attention.
Inhalation: Quickly leave the scene and move to a place with fresh air. Administer oxygen when experiencing difficulty breathing. When breathing stops, immediately perform artificial respiration. Seek medical attention.
Ingestion: If ingested by mistake, rinse mouth with water, drink milk or egg whites, and seek medical attention immediately.
Comprehensive analysis of the coupling efficiency between aluminum nuclear spin (I=5/2) and microwave pulses in Diethylaluminum Chloride
In quantum information processing and nuclear magnetic resonance (NMR) technology, the coupling efficiency between nuclear spin and microwave pulses is the core parameter that determines system performance. For aluminum (Al), its natural isotope ² ⁷ Al has a nuclear spin quantum number I=5/2, which gives it both the resonance response capability of magnetic atomic nuclei and the unique relaxation mechanism induced by electric quadrupole (Q). Diethylaluminum chloride (DEAC) is an aluminum containing organic metal compound, in which the aluminum atom in its molecular structure is in a dual coordination environment of organic ligand (ethyl) and inorganic ligand (chlorine). This chemical environment significantly affects the local electric field gradient (EFG) of the aluminum core, thereby regulating its coupling efficiency with microwave pulses.
Quantum properties and relaxation mechanism of aluminum nuclear spin (I=5/2)
Correlation between Nuclear Spin Quantum Number and Magnetic Moment
According to quantum mechanics, the spin quantum number I of an atomic nucleus determines the quantized state of its magnetic moment. For an aluminum core with I=5/2, its magnetic quantum number m can be taken as -5/2, -3/2, -1/2,+1/2,+3/2,+5/2, a total of 6 energy levels. Under the action of a static magnetic field B ₀, these energy levels undergo Zeeman splitting, and the energy difference between adjacent energy levels is Δ E=γ ħ B ₀, where γ is the magnetic spin ratio of the aluminum nucleus (γ of ² ⁷ Al=6.976 × 10 ⁷ rad · s ⁻¹ · T ⁻¹). Microwave pulses induce transitions between energy levels and manipulate nuclear spin states by applying a radio frequency field (B ₁) that matches Δ E.
Regulation of relaxation time by electric quadrupole moment
Half of the atomic nuclei have non-zero electric quadrupole moments (Q=eQR ², where Q is the quadrupole constant and R is the nuclear radius), resulting in significant energy level splitting influenced by local electric field gradients (EFG). In DEAC molecules, aluminum atoms are in a tetrahedral coordination environment (two ethyl and two chlorine atoms), and the symmetry of EFG is low, causing the following effects: the interaction between electric quadrupole and EFG leads to inelastic scattering between energy levels, accelerating the decay of transverse magnetization. According to the formula for natural spectral line width Δ ν=1/(π T ₂), the shortening of T ₂ leads to an increase in spectral line width.
The competitive relationship between chemical shift and quadrupole coupling
The resonance frequency of aluminum nuclei is not only affected by the magnetic spin ratio (γ) and static magnetic field (B ₀), but also related to the chemical displacement (δ) and quadrupole coupling constant (C_Q). In DEAC, the electron donating effect of ethyl and the electron withdrawing effect of chlorine work together to cause a change in the electron cloud density of the aluminum core, resulting in fluctuations in δ within the range of 0-500 ppm. C_Q=e²Qq/ħ, Where q is the maximum component of EFG. In DEAC, the typical value of C_Q is 1-10 MHz, which is much larger than the frequency shift caused by chemical shift (δ ·ν₀, where ν₀ is the Larmor frequency). Therefore, quadrupole interaction dominates the spectral line characteristics.
Optimization of Microwave Pulse Parameters on Coupling Efficiency
Pulse shape and bandwidth matching
The bandwidth of microwave pulses (Δ v _p) needs to be matched with the spectral line width of aluminum nuclei (Δ v) to achieve efficient excitation. For ² ⁷ Al in DEAC:
Hard pulse: If Δ ν _p ≫ Δ ν, the pulse can excite all energy level transitions, but may trigger nonlinear responses (such as Bloch Siegert shift).
Soft pulse: If Δ ν _p ≈ Δ ν, the pulse selectively excites specific energy level transitions, reducing unnecessary energy dissipation. For example, using Gaussian shaped soft pulses (duration τ=10-100 μ s) can reduce spectral line distortion while maintaining excitation efficiency.
Pulse power and flip angle control
The power (P) of microwave pulses determines the flip angle (θ) of nuclear spin, which is related to θ=γ B ₁τ. In Diethylaluminum chloride:
Low power pulse: When θ<π/2, the nuclear spin is not completely flipped, and the signal strength is proportional to θ ², but it can avoid power broadening effects.
High power pulse: When θ=π, complete flipping is achieved, but it may cause dynamic nuclear polarization (DNP) or spin locking effects, which need to be optimized based on specific experimental conditions.
Pulse sequence design
To overcome the limitation of T ₂ shortening, special pulse sequences (such as CPMG sequences) need to be used to improve signal fidelity:
CPMG sequence: By applying multiple 180 ° pulses (τ -180 ° - τ - echo), the transverse magnetization is reunited to prolong the effective T ₂. In the NMR experiment of DEAC, the CPMG sequence can prolong the signal attenuation time by 3-5 times.
Adiabatic pulse: By slowly changing the pulse parameters (such as frequency or amplitude), adiabatic transitions between energy levels are achieved, reducing non adiabatic losses.
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