Preparation method of diphenyl ethyoxyl phosphine and product thereof

Abstract

The invention provides a preparation method of diphenyl ethyoxyl phosphine and a product thereof. Taking diphenyl phosphonium chloride and absolute ethyl alcohol as raw materials, petroleum ether as a solvent and triethylamine as an acid-binding agent; the reaction process comprises the following steps: reacting diphenyl phosphine chloride with ethanol to generate diphenyl ethyoxyl phosphine and hydrogen chloride, and reacting hydrogen chloride with triethylamine to generate triethylamine hydrochloride. And after the reaction is finished, separating triethylamine hydrochloride separated by crystallization from the liquid organic phase through centrifugation, taking the obtained triethylamine hydrochloride as a co-product, carrying out desolvation treatment on the obtained liquid organic phase to obtain a diphenylethoxyphosphine crude product, and rectifying to obtain the high-quality diphenylethoxyphosphine. The preparation process provided by the invention is mild in reaction condition, simple and convenient to operate and low in requirements on equipment and energy consumption; the raw materials are wide in source and low in cost, and the solvent and the acid-binding agent can be recycled, so that the method has the advantage of environmental protection. The prepared diphenyl ethyoxyl phosphine is high in purity and good in yield, and has a wide industrial application prospect.

Description

Technical Field

[0001] The invention belongs to the technical field of diphenylethoxyphosphine processes, and particularly relates to a preparation method of diphenylethoxyphosphine and a product thereof. Background Art

[0002] Diphenylethoxyphosphine, molecular formula C 14 H 15 OP, with its chemical structure consisting of two phenyl groups and an ethoxy group attached to a phosphorus atom, possesses unique chemical properties. It typically appears as a colorless to pale yellow, transparent liquid and is relatively stable in air, but may undergo chemical reactions when exposed to strong oxidants, strong acids, or strong bases. In organic synthesis, diphenylethoxyphosphine is an indispensable intermediate. Due to the unique electronic structure and reactivity of the phosphorus atom, it can participate in a variety of organic reactions, such as phosphonation and nucleophilic substitution, and is used to construct various phosphorus-containing organic compounds. With its widespread application in pharmaceuticals, pesticides, materials science, and other fields, diphenylethoxyphosphine has become a crucial material foundation for technological development in multiple industries. The optimization and innovation of its preparation process has also been a research hotspot in chemical synthesis.

[0003] Currently, the preparation methods of diphenylethoxyphosphine mainly include Grignard reagent method, transesterification method and phase transfer catalysis method. Specifically:

[0004] (1) The Grignard reagent method involves first reacting magnesium chips with halogenated benzene in an organic solvent such as anhydrous ether or tetrahydrofuran to produce a Grignard reagent, then reacting the Grignard reagent with ethoxyphosphoryl chloride, and finally obtaining diphenylethoxyphosphine through steps such as hydrolysis and purification. However, the preparation of the Grignard reagent requires strict anhydrous and oxygen-free conditions, places high demands on the reaction equipment, and the operation process is complex and dangerous. Furthermore, halogenated benzene and ethoxyphosphoryl chloride are generally toxic and corrosive, posing certain hazards to the environment and operators. Furthermore, a large amount of by-products are produced during the reaction, resulting in a complex post-processing process and high costs.

[0005] (2) The transesterification method usually uses diphenylphosphonate and ethanol as raw materials, and carries out an ester exchange reaction in the presence of a catalyst to produce diphenylethoxyphosphine and the corresponding alcohol. However, this reaction relies on an efficient catalyst to promote the reaction, and the reaction is usually carried out at a relatively high temperature and pressure, which places high demands on the reaction equipment. At the same time, the transesterification reaction is also a reversible reaction with a limited reaction conversion rate. Effective separation measures need to be taken to separate the product from the reaction system in a timely manner to improve the reaction conversion rate and yield. In addition, the preparation of the raw material diphenylphosphonate is also relatively complicated, which increases the cost and difficulty of the entire production process.

[0006] (3) Phase transfer catalysis is a method in which a phosphorus source (such as a phosphate ester) reacts with a halogenated benzene, ethanol, etc. in a two-phase system under the action of a phase transfer catalyst to produce diphenylethoxyphosphine. However, the price of a phase transfer catalyst is relatively high, which increases production costs. In addition, the reaction conditions, such as temperature and pH value, need to be strictly controlled during the reaction process, otherwise the activity of the catalyst and the selectivity of the reaction will be affected. In addition, the recovery and reuse of the catalyst after the reaction is relatively difficult. If handled improperly, it will not only cause a waste of resources but also may pollute the environment.

[0007] In summary, the existing preparation methods of diphenylethoxyphosphine all have problems such as high safety risks, severe environmental pollution, low product purity, and high production costs, which are difficult to meet the needs of industrial large-scale production. There is an urgent need to develop a safe, environmentally friendly, efficient and low-cost preparation method for diphenylethoxyphosphine. Summary of the Invention

[0008] The present invention aims to provide a method for preparing diphenylethoxyphosphine, which effectively solves the problems of high safety risk, severe environmental pollution, low product purity, high production cost, etc. in the existing diphenylethoxyphosphine production process. The obtained products are high-quality diphenylethoxyphosphine and co-produced triethylamine hydrochloride, and no waste liquid is generated throughout the process, thereby greatly improving the economic benefits of the enterprise and achieving the beneficial effect of reducing costs and increasing efficiency.

[0009] To achieve the above object, the present invention provides a method for preparing diphenylethoxyphosphine, which uses diphenylphosphine chloride and anhydrous ethanol as raw materials, petroleum ether as a solvent, and triethylamine as an acid-binding agent, and undergoes an ethoxylation-desolventization-reduced pressure distillation process to prepare a diphenylethoxyphosphine product and a triethylamine hydrochloride co-product.

[0010] In a preferred embodiment, the preparation method of the diphenylethoxyphosphine specifically comprises the following steps:

[0011] S1 Ethoxylation reaction: Mix anhydrous ethanol, triethylamine and petroleum ether and stir them evenly at room temperature; reduce the system temperature to -15 to -5°C, add diphenylphosphine chloride dropwise, keep warm and stir evenly to obtain an ethoxylation reaction solution;

[0012] S2 centrifugation: in a protective atmosphere, centrifuge the ethoxylation reaction liquid of step S1 to obtain a solid and a liquid organic phase;

[0013] S3 desolventizing: desolventizing the liquid organic phase under negative pressure until no obvious material flows out, condensing to obtain liquid and solid, wherein the liquid is recycled for S1 ethoxylation reaction, and the solid is crude diphenylethoxyphosphine;

[0014] S4 distillation: distill the crude diphenylethoxyphosphine under reduced pressure to obtain the diphenylethoxyphosphine product.

[0015] In a preferred embodiment, in step S1, the diphenylphosphine chloride decomposes upon contact with water, and the reaction environment needs to avoid the introduction of air and moisture. Therefore, the anhydrous ethanol reaction further includes a dehydration and drying step, for example, first passing the anhydrous ethanol through a dryer containing a molecular sieve, and then mixing with other raw materials for reaction.

[0016] In a preferred embodiment, in step S1, the mass ratio of anhydrous ethanol, triethylamine, petroleum ether and diphenylphosphine chloride is 1:(2-2.4):(4-5.5):(9-11); preferably, the mass ratio of anhydrous ethanol, triethylamine, petroleum ether and diphenylphosphine chloride is 1:(2-2.3):(4.4-4.9):(9.6-10.3); more preferably, the mass ratio of anhydrous ethanol, triethylamine, petroleum ether and diphenylphosphine chloride is 1:2.1:4.5:9.7.

[0017] In a preferred embodiment, in step S1, the stirring time at room temperature is 5-15 minutes; preferably, the stirring time at room temperature is 10 minutes.

[0018] In a preferred embodiment, in step S1, the insulation and stirring temperature is -15 to -5°C, and the stirring time is 2-4 hours; preferably, the insulation and stirring temperature is -10°C, and the stirring time is 3 hours.

[0019] In a preferred embodiment, in step S2, the protective atmosphere is nitrogen.

[0020] In a preferred embodiment, in step S2, the temperature of the centrifugal separation is -15 to -5°C.

[0021] In a preferred embodiment, in step S2, the solid is triacetamine hydrochloride.

[0022] In a preferred embodiment, in step S3, the negative pressure desolvation conditions include: vacuum degree -0.10 to -0.06 MPa, and desolvation temperature 75 to 85°C; preferably, the desolvation conditions include: vacuum degree -0.08 MPa, and desolvation temperature 80°C.

[0023] In a preferred embodiment, in step S3, the condensation temperature is 5-9°C; preferably, the condensation temperature is 7°C.

[0024] In a preferred embodiment, in step S3, the liquid includes one or more of petroleum ether, unreacted ethanol and triethylamine, which can be recycled for the ethoxylation reaction in S1 without the need to treat the waste liquid.

[0025] In a preferred embodiment, in step S4, the reduced pressure distillation conditions include: vacuum degree -0.11 to -0.07 MPa, and distillation temperature 180-220°C; preferably, the reduced pressure distillation conditions include: vacuum degree -0.09 MPa, and distillation temperature 200°C.

[0026] In a preferred embodiment, in step S4, the purity of the prepared diphenylethoxyphosphine product can reach 99.5%, and the conversion rate of diphenylphosphine chloride can reach 99%.

[0027] In the present invention, high vacuum distillation is used to effectively improve the distillation efficiency and shorten the distillation time, and the distillation temperature is reduced by 10°C compared with the conventional distillation temperature, so that high boiling point substances are significantly reduced, thereby improving the product purity and yield.

[0028] Another object of the present invention is to provide diphenylethoxyphosphine prepared by any one of the above methods.

[0029] In the production technique of the present invention, diphenylphosphine chloride and absolute ethanol are used as raw materials, petroleum ether is used as solvent, and triethylamine is used as acid binding agent. The specific reaction process comprises: diphenylphosphine chloride and ethanol react to generate diphenylethoxyphosphine and hydrogen chloride, and hydrogen chloride and triethylamine react to generate triethylamine hydrochloride. Since triethylamine hydrochloride is insoluble in petroleum ether, the triethylamine hydrochloride generated in the reaction process can continuously crystallize out. After the ethoxylation reaction ends, the solid-state triethylamine hydrochloride separated out by crystallization can be separated from the liquid organic phase by centrifugation, and the gained triethylamine hydrochloride can be used as a co-product. The liquid organic phase is subjected to precipitation treatment, and petroleum ether and unreacted ethanol and triethylamine are condensed and recovered for S1 ethoxylation reaction, and the solid diphenylethoxyphosphine crude product is obtained by rectification to obtain high-quality diphenylethoxyphosphine.

[0030] Compared with the prior art, the technical solution of the present invention has the following advantages:

[0031] From the perspective of raw material selection, the present invention uses diphenylphosphine chloride and anhydrous ethanol as basic raw materials, both of which are widely available and relatively stable in price. Petroleum ether is used as a solvent, which has good solubility and can fully disperse the raw materials to ensure uniform reaction. Its low boiling point makes it easy to separate and recover in the subsequent decompression and desolventizing step, achieving the effect of recycling and further reducing production costs. Triethylamine is used as an acid binding agent, which has moderate alkalinity and can effectively neutralize the hydrogen chloride generated by the ethoxylation reaction, promoting the reaction to proceed in the forward direction, while not easily inducing side reactions of the raw materials or products, thereby ensuring reaction selectivity.

[0032] From the perspective of the reaction process, the ethoxylation reaction provided by the present invention has mild reaction conditions and does not require high temperature, high pressure or harsh reaction environment, thereby reducing the requirements for reaction equipment, energy consumption and safety risks. The use of triethylamine to neutralize hydrogen chloride avoids the complex acid treatment process in traditional processes, simplifies the operation steps, and improves production efficiency. The reaction system is carried out in a petroleum ether solvent, which can effectively control the transfer of reaction heat, prevent local overheating, facilitate the smooth progress of the reaction, and improve the stability of product quality.

[0033] In terms of product quality, the diphenylethoxyphosphine prepared by the present invention has few side reactions and high purity. Furthermore, the subsequent separation and purification process is simple, reducing product loss and improving yield. The petroleum ether, ethanol, and triethylamine used in the reaction can all be recycled through vacuum desolventization and condensation recovery, significantly reducing organic solvent emissions and environmental pollution, in line with the concepts of green chemistry and sustainable development. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] These and / or other aspects and advantages of the present invention will become more apparent and more readily understood from the following detailed description of embodiments of the present invention in conjunction with the accompanying drawings, in which:

[0035] Figure 1 1 is a process flow chart of an embodiment of the present invention. DETAILED DESCRIPTION

[0036] In order to enable those skilled in the art to better understand the present invention, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments. However, it should be understood that the protection scope of the present invention is not limited to the specific embodiments.

[0037] The embodiments of the present invention provide a preparation method of diphenylethoxyphosphine and a product thereof, thereby effectively solving the problems of high safety risk, severe environmental pollution, low product purity, high production cost, etc. in the existing diphenylethoxyphosphine production process.

[0038] The present invention aims to solve the above problems. The specific solution is as follows: diphenylphosphine chloride and anhydrous ethanol are used as raw materials, petroleum ether is used as solvent, and triethylamine is used as acid binding agent. The ethoxylation-desolventization-reduced pressure distillation process is used to prepare diphenylphosphine ethoxy product and triethylamine hydrochloride co-product. The specific process flow is as follows: Figure 1 shown.

[0039] The ethoxylation reaction mechanism in this case involves the following: the phosphorus atom within the diphenylphosphine chloride molecule, linked to the electron-withdrawing chlorine atom and the phenyl group, possesses a strong electropositive property, making it an electrophilic center. The ethanol oxygen atom in the anhydrous ethanol molecule contains a lone pair of electrons, acting as a nucleophile. Based on a nucleophilic substitution reaction mechanism, the lone pair of electrons from the ethanol oxygen atom attacks the phosphorus atom of the diphenylphosphine chloride, forming a transition intermediate. Simultaneously, triethylamine, acting as an acid-binding agent, rapidly captures the generated hydrogen chloride via the lone pair of electrons on its nitrogen atom, forming a stable triethylamine hydrochloride. This process not only significantly reduces the hydrogen chloride concentration in the system, disrupting the reaction equilibrium and providing a continuous driving force for the forward reaction, but also prevents potential damage to the raw materials and products by hydrogen chloride, inhibiting side reactions. Petroleum ether, acting as a solvent, leverages its nonpolarity and low dielectric constant to reduce the ionization tendency of the reactants, minimizing ionic side reactions. Furthermore, through intermolecular forces, it disperses the reactant molecules, promoting effective molecular collisions and improving reaction rate and selectivity. The synergistic effect of these multiple factors ensures the high efficiency, stability, and purity of the product of the ethoxylation reaction.

[0040] The technical solution of this application is described in detail below through specific embodiments:

[0041] Unless otherwise specified, the technical means used in the present invention are conventional means well known to those skilled in the art. The various raw materials, reagents, instruments, and equipment used in the present invention can be purchased from the market or prepared by existing methods. Unless otherwise specified, the reagents used in the present invention are of analytical grade.

[0042] Example 1

[0043] A method for preparing diphenylethoxyphosphine comprises the following steps:

[0044] (1) Ingredients: Prepare 10.32 g of anhydrous ethanol, 22 g of triethylamine, 44.4 g of petroleum ether, and 45 g of diphenylphosphine chloride.

[0045] (2) Ethoxylation process: Before production, check the condition of each equipment and valves and make preparations for feeding. The raw material anhydrous ethanol is pumped from the tank area into the workshop ethanol intermediate tank through a delivery pump, and then it is dried (molecular sieve dehydration) and dehydrated into the ethanol metering tank, and then the measured anhydrous ethanol is placed in the synthesis kettle; triethylamine is pumped from the tank area into the workshop metering tank through a pump, and then the discharge valve of the metering tank is opened to place the measured triethylamine in the synthesis kettle. Petroleum ether is pumped from the tank area into the workshop metering tank through a pump, and then the discharge valve of the metering tank is opened to place the measured petroleum ether in the synthesis kettle; the barreled diphenylphosphine chloride is taken out from the warehouse and pumped into the diphenylphosphine chloride high-level metering tank with a vacuum pump for standby use.

[0046] When the addition of anhydrous ethanol, triethylamine, and petroleum ether is completed, close the feeding valve and start stirring the synthesis kettle. Stir at room temperature for 10 minutes to fully mix the materials. Open the synthesis kettle jacket with chilled brine (-15°C) to start cooling. When the temperature of the materials in the synthesis kettle is cooled to -10°C, start adding diphenylphosphine chloride dropwise. Control the addition rate to maintain the reaction temperature at -10°C ± 2°C. When the temperature exceeds the set value, automatically adjust the diphenylphosphine chloride rate and open the chilled brine inlet valve. If stirring stops unexpectedly, interlock and stop the addition of diphenylphosphine chloride. After the addition is completed, continue to keep the temperature at -10°C and continue stirring for 3 hours.

[0047] During the ethoxylation reaction, petroleum ether is used as a solvent, diphenylphosphine chloride reacts with ethanol to produce diphenylphosphine ethoxylate and hydrogen chloride, and hydrogen chloride reacts with triethylamine to produce triethylamine hydrochloride. The reaction routes involved include:

[0048] (C6H5)2PCl+CH3CH2OH→(C6H5)2POCH2CH3+HCl+367.8kJ / mol

[0049] Diphenylphosphine chloride + anhydrous ethanol → diphenylethoxyphosphine + hydrogen chloride (exothermic reaction)

[0050] (CH3CH2)3N+HCl→(CH3CH2)3NHCl

[0051] Triethylamine + hydrogen chloride → triethylamine hydrochloride (exothermic reaction)

[0052] Because the ethoxylation reaction is exothermic, the reaction process is temperature-controlled using a chilled water jacket. The raw material, diphenylphosphine chloride, decomposes in contact with water. To prevent the ingress of air and moisture, the reaction environment is steam-dried and nitrogen-purged in the synthesis reactor and diphenylphosphine chloride header tank during initial startup or after a prolonged shutdown. Triethylamine acts as an acid-binding agent in the reaction. The hydrogen chloride generated by the ethoxylation reaction immediately reacts with triethylamine. The resulting triethylamine hydrochloride is insoluble in petroleum ether, resulting in continuous crystallization of triethylamine hydrochloride during the reaction.

[0053] (3) Centrifugation

[0054] Under nitrogen protection, the ethoxylation reaction liquid is placed in a sealed automatic unloading centrifuge. The crystallized solid triethylamine hydrochloride is separated from the liquid organic phase by centrifugation. The separated liquid is collected in a centrifuge mother liquor tank. The crystallized material is placed in ton bags, packaged, and transported to the warehouse. The centrifuge is sealed during the centrifugation process, and the temperature of the feed liquid is around -10°C.

[0055] (4) Desolventizing process

[0056] Transfer the centrifuge mother liquor from the centrifuge mother liquor tank to the desolventizing kettle using a pump, and close the feed valve. Start negative pressure desolventizing in the desolventizing kettle. Turn on the vacuum system and adjust the vacuum to approximately -0.08 MPa. Start the steam in the desolventizing kettle jacket and slowly increase the temperature to 80°C. When no material is visible in the sight glass at the bottom of the condenser, stop heating and use "primary water cooling (7°C)" to condense and recover the petroleum ether, unreacted ethanol, and triethylamine. The recovered petroleum ether, ethanol, and triethylamine are all reused in the ethoxylation process. Transfer the crude diphenylethoxyphosphine to the rectification kettle.

[0057] (5) Distillation process

[0058] The bottom valve of the desolventizing kettle is opened to transfer the crude diphenylethoxyphosphine into the distillation kettle. After the transfer is completed, the feed valve and the bottom valve of the desolventizing kettle are closed, the vacuum system is opened to adjust the vacuum degree to -0.09 MPa, the heat transfer oil valve is fine-tuned to perform reduced pressure distillation, and the temperature is slowly raised to 120° C., the heating is reduced to maintain the temperature. The front fraction is a mixture of ethanol, petroleum ether, and triethylamine. The distilled low fraction is received in the front fraction receiving kettle to be applied to the next batch of ethoxylation process; after the vacuum degree and the material liquid level in the kettle are stable, the receiving pipeline valve is switched to the finished product kettle, and then the oil inlet of the heat transfer oil valve is slowly increased. The temperature is gradually raised to about 200° C. When the vacuum degree is -0.09 MPa, the finished diphenylethoxyphosphine is distilled out and received in the finished product kettle. When the distillation system has no reflux, it indicates that the distillation is complete, and then the heat transfer oil valve is closed. Transport the packaging barrel to the packaging area, open the packaging barrel cover for inspection, purge with nitrogen for 1 minute, and pack the finished product into the warehouse; then open the bottom valve of the distillation kettle for packaging. After the weight is qualified, close the bottom valve, seal the packaging barrel, and transport it to the designated place to continue packaging the products of the distillation kettle.

[0059] Example 2

[0060] Compared with Example 1, the only difference is that in step (1), 9.85 g of anhydrous ethanol, 22 g of triethylamine, 44.4 g of petroleum ether, and 45 g of diphenylphosphine chloride are prepared respectively. The other steps are exactly the same as those in Example 1.

[0061] Example 3

[0062] Compared with Example 1, the only difference is that in step (1), 10.32 g of anhydrous ethanol, 22 g of triethylamine, 40 g of petroleum ether, and 45 g of diphenylphosphine chloride are prepared respectively. The other steps are exactly the same as those in Example 1.

[0063] Example 4

[0064] Compared with Example 1, the only difference is step (2) of the ethoxylation process: after the addition of diphenylphosphine chloride is completed, the temperature is kept at -15°C and stirring is continued for 2 hours. The other steps are exactly the same as those in Example 1.

[0065] Comparative Example 1

[0066] Compared with Example 1, the only difference is that in step (1), the acid binding agent is not triethylamine but sodium carbonate of the same mass. The other method steps are exactly the same as those in Example 1.

[0067] Comparative Example 2

[0068] Compared with Example 1, the only difference is that in step (2), the temperature during the dropwise addition of diphenylphosphine chloride and the insulation is 0° C. The other steps are exactly the same as those in Example 1.

[0069] The products of Examples 1-4 and Comparative Examples 1-2 were tested, and the results are shown in Table 1.

[0070] Table 1

[0071]

[0072] As can be seen from Table 1, Comparative Example 1 changes the acid binding agent composition, while Comparative Example 2 increases the temperature for adding diphenylphosphine chloride and the temperature for insulation, both of which have an adverse effect on the purity and conversion rate of the diphenylphosphine chloride product. In contrast, Examples 1-4 of the present invention all achieve diphenylphosphine chloride product purities exceeding 98.5% and conversion rates exceeding 94%, without generating any waste liquid throughout the entire process. The resulting triethylamine hydrochloride can also be sold as a co-product, significantly improving the economic benefits of the enterprise and reducing its waste liquid treatment costs, thereby offering environmental benefits and broad application prospects.

[0073] The foregoing descriptions of specific exemplary embodiments of the present invention are for purposes of illustration and description. These descriptions are not intended to limit the invention to the precise forms disclosed, and it is apparent that many variations and modifications are possible in light of the foregoing teachings. The exemplary embodiments have been selected and described for the purpose of explaining the specific principles of the invention and their practical application, thereby enabling those skilled in the art to realize and utilize a variety of exemplary embodiments of the invention and various options and modifications. The scope of the invention is intended to be defined by the claims and their equivalents.

Claims

1. A method for preparing diphenylethoxyphosphine, characterized in that: The preparation method uses diphenylphosphine chloride and anhydrous ethanol as raw materials, petroleum ether as solvent, and triethylamine as acid-binding agent, and undergoes an ethoxylation-desolventization-reduced pressure distillation process to prepare a diphenylethoxyphosphine product and a triethylamine hydrochloride co-product.

2. The preparation method of diphenyl ethoxy phosphine as claimed in claim 1, wherein The specific steps include: S1 Ethoxylation reaction: Mix anhydrous ethanol, triethylamine and petroleum ether and stir them evenly at room temperature; reduce the system temperature to -15 to -5°C, add diphenylphosphine chloride dropwise, keep warm and stir evenly to obtain an ethoxylation reaction solution; S2 centrifugation: in a protective atmosphere, centrifuge the ethoxylation reaction liquid of step S1 to obtain a solid and a liquid organic phase; S3 desolventizing: desolventizing the liquid organic phase under negative pressure until no obvious material flows out, condensing to obtain liquid and solid, wherein the liquid is recycled for S1 ethoxylation reaction, and the solid is crude diphenylethoxyphosphine; S4 distillation: distill the crude diphenylethoxyphosphine under reduced pressure to obtain the diphenylethoxyphosphine product.

3. The preparation method of diphenyl ethoxy phosphine as claimed in claim 2, wherein In step S1, the mass ratio of anhydrous ethanol, triethylamine, petroleum ether and diphenylphosphine chloride is 1:(2-2.4):(4-5.5):(9-11).

4. The preparation method of diphenyl ethoxy phosphine as claimed in claim 2, wherein In step S1, the heat preservation and stirring temperature is -15 to -5°C, and the stirring time is 2 to 4 hours.

5. The preparation method of diphenyl ethoxy phosphine as claimed in claim 2, wherein In step S2, the solid is triacetamine hydrochloride.

6. The preparation method of diphenyl ethoxy phosphine as claimed in claim 2, wherein In step S3, the negative pressure desolvation conditions include: vacuum degree -0.10 to -0.06 MPa, and desolvation temperature 75 to 85°C.

7. The preparation method of diphenyl ethoxy phosphine as claimed in claim 2, wherein In step S3, the condensation temperature is 5-9°C.

8. The preparation method of diphenyl ethoxy phosphine as claimed in claim 2, wherein In step S4, the reduced pressure distillation conditions include: vacuum degree -0.11 to -0.07 MPa, and distillation temperature 180-220°C.

9. The method for preparing diphenyl ethoxy phosphine as claimed in claim 2, wherein In step S4, the purity of the prepared diphenylethoxyphosphine product can reach 99.5%, and the conversion rate of diphenylphosphine chloride can reach 99%.

10. The diphenylethoxyphosphine prepared by the method according to any one of claims 1 to 9.

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