CN112094295B - Synthesis process of diphenyl phosphorus oxide - Google Patents
Synthesis process of diphenyl phosphorus oxide Download PDFInfo
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- CN112094295B CN112094295B CN202011100996.5A CN202011100996A CN112094295B CN 112094295 B CN112094295 B CN 112094295B CN 202011100996 A CN202011100996 A CN 202011100996A CN 112094295 B CN112094295 B CN 112094295B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/28—Phosphorus compounds with one or more P—C bonds
- C07F9/50—Organo-phosphines
- C07F9/53—Organo-phosphine oxides; Organo-phosphine thioxides
- C07F9/5325—Aromatic phosphine oxides or thioxides (P-C aromatic linkage)
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Abstract
The invention provides a synthesis process of diphenyl phosphorus oxide, which comprises the following steps: step S1, adding diphenyl phosphorus chloride into distilled water, reacting at a first temperature, and carrying out solid-liquid separation to obtain a first solid phase; s2, adding dichloromethane into the first solid phase until the dichloromethane is completely dissolved to obtain a first mixed solution; s3, adding a mixed aqueous solution of sodium bicarbonate and sodium hydroxide into the first mixed solution, washing the mixed solution for a first time at a first rotating speed, and standing and separating the mixed solution to obtain a first organic phase; s4, distilling the first organic phase at a second temperature and under the pressure of 0.1-0.8 MP, and then cooling to a third temperature to obtain a first distilled organic phase; and S5, adding a crystallization solution into the first distillation organic phase, and crystallizing, separating and drying to obtain a target product. The invention solves the technical problem of low yield of the traditional diphenyl phosphorus oxide synthesis method by optimizing the synthesis process of the diphenyl phosphorus oxide.
Description
Technical Field
The invention relates to the field of chemical synthesis, in particular to a synthesis process of diphenyl phosphorus oxide.
Background
The common high polymer material has a low oxygen index and belongs to a flammable material, and the high polymer material cannot be separated in daily life of people, so that once a fire disaster happens, the high polymer material has a combustion-supporting risk and endangers the property and life safety of people. How to reduce the combustion performance of polymer materials has become an increasingly concerned technical and social problem. In recent years, fire caused by flammability of polymer materials frequently occurs, and great threat is brought to life and property safety of people. At present, all countries around the world put forward high standards for the requirements of high polymer materials on flame retardance, and also provide a wide market for the research and development of flame retardants.
The diphenyl phosphorus oxide is a novel organic phosphorus flame retardant product, and can be industrially used as a flame retardant for metal materials and other high-end materials. However, the synthesis method of diphenylphosphine oxide in the related art is only in the laboratory stage due to the harsh synthesis conditions and the unstable nature of diphenylphosphine oxide. The traditional laboratory synthesis method of diphenyl phosphorus oxide is to take diphenyl phosphorus chloride as a raw material, and obtain a product by hydrolyzing, extracting, separating and distilling an organic solvent, or crystallize the product through benzene/toluene.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a synthesis process of diphenyl phosphorus oxide, which aims to solve the technical problem of low yield of the traditional diphenyl phosphorus oxide synthesis method in the related art.
The invention provides a synthesis process of diphenyl phosphorus oxide, which comprises the following steps:
step S1, adding diphenyl phosphorus chloride into distilled water at a first flow rate according to the mass ratio of the distilled water to the diphenyl phosphorus chloride of 25-30;
s2, adding dichloromethane into the first solid phase until the dichloromethane is completely dissolved to obtain a first mixed solution; wherein the mass ratio of the dichloromethane to the diphenyl phosphorus chloride in the step S1 is 1-3:1;
s3, adding a mixed aqueous solution of sodium bicarbonate and sodium hydroxide into the first mixed solution, washing the mixed solution for a first time at a first rotating speed, standing and separating to obtain a second liquid phase and a first organic phase; wherein the mass ratio of the sodium bicarbonate and sodium hydroxide mixed aqueous solution to the diphenyl phosphorus chloride in the step S1 is 4-5.5;
s4, distilling the first organic phase at a second temperature under the environment of 0.1-0.8 MP, and then cooling to a third temperature to obtain a first distilled organic phase;
s5, adding a crystallization solution into the first distillation organic phase, and crystallizing, separating and drying to obtain a target product; wherein the mass ratio of the crystallization solution to the diphenyl phosphorus chloride in the step S1 is 18-25.
Optionally, in step S1, the first flow rate is 2.5 to 5L/min.
Optionally, in step S1, the first temperature is 10 to 28 ℃.
Alternatively, in step S3, the mixed aqueous solution of sodium bicarbonate and sodium hydroxide is a mixed aqueous solution of sodium bicarbonate and sodium hydroxide having a concentration of 20%, and the mass ratio of sodium bicarbonate to sodium hydroxide is 0.4 to 2.5.
Optionally, in step S3, the first rotation speed is 85 to 300r/min; and/or the presence of a gas in the gas,
in step S3, the first time period is 30 to 120min.
Optionally, in step S4, the second temperature is 75 to 95 ℃; and/or the presence of a gas in the gas,
in step S4, the third temperature is 38 to 45 ℃.
Alternatively, in step S5, the crystallization solution comprises dichloromethane and n-heptane in a volume ratio of 5 to 25.
Optionally, in step S5, the specific step of crystallizing includes:
and (3) reducing the temperature from the third temperature to 10-15 ℃ in a stepped manner, wherein the time of temperature reduction is 3-6 hours, and then keeping stirring for 2-3 hours to obtain a crystallization mixture.
Optionally, in step S5, the specific steps of separating and drying to obtain the target product include:
filtering said crystallized mixture to obtain a crystalline solid;
and transferring the crystallized solid into a double-cone dryer, and drying for 3-5 hours at 35-50 ℃ under the pressure of 0.1-0.8 MP to obtain the target product.
Optionally, the synthesis process further includes, after step S5:
s6, collecting the first liquid phase and the second liquid phase into a reaction kettle, adding dichloromethane, stirring and extracting for 1-2 hours, standing and taking an organic phase to obtain a diphenyl phosphoric acid byproduct;
and S7, collecting hydrogen chloride gas generated in the reaction, and introducing the hydrogen chloride gas into a falling film absorption tower to obtain an industrial-grade hydrochloric acid byproduct.
Compared with the prior art, the invention has the following beneficial effects:
in the technology, the synthesis process of the diphenyl phosphorus oxide is optimized, so that the operation period is shortened, the yield of the product is greatly improved, and the quality of the product is guaranteed; meanwhile, the synthesis process of the diphenyl phosphorus oxide provided by the invention does not use benzene or toluene in the traditional synthesis process as an extracting agent, so that the toxicity of the product is greatly reduced, and the environmental pollution is reduced; the whole synthesis process is simple and safe to operate and easy to industrially popularize.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly apparent, the technical solutions of the present invention are further described below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention provides a synthesis process of diphenyl phosphorus oxide, which comprises the following steps:
step S1, adding diphenyl phosphorus chloride into distilled water at a first flow rate according to the mass ratio of the distilled water to the diphenyl phosphorus chloride of 25-30;
s2, adding dichloromethane into the first solid phase until the dichloromethane is completely dissolved to obtain a first mixed solution; wherein the mass ratio of the dichloromethane to the diphenyl phosphorus chloride in the step S1 is 1-3:1;
s3, adding a mixed aqueous solution of sodium bicarbonate and sodium hydroxide into the first mixed solution, washing the mixed solution for a first time at a first rotating speed, and standing and separating the mixed solution to obtain a second liquid phase and a first organic phase; wherein the mass ratio of the sodium bicarbonate and sodium hydroxide mixed aqueous solution to the diphenyl phosphorus chloride in the step S1 is 4-5.5;
s4, distilling the first organic phase at a second temperature under the environment of 0.1-0.8 MP, and then cooling to a third temperature to obtain a first distilled organic phase;
s5, adding a crystallization solution into the first distillation organic phase, and crystallizing, separating and drying to obtain a target product; wherein the mass ratio of the crystallization solution to the diphenyl phosphorus chloride in the step S1 is 18-25.
Optionally, in step S1, the first flow rate is 2.5 to 5L/min.
Optionally, in step S1, the first temperature is 10 to 28 ℃.
Alternatively, in step S3, the mixed aqueous solution of sodium bicarbonate and sodium hydroxide is a mixed aqueous solution of sodium bicarbonate and sodium hydroxide having a concentration of 20%, and the mass ratio of sodium bicarbonate to sodium hydroxide is 0.4 to 2.5.
Optionally, in step S3, the first rotation speed is 85 to 300r/min; and/or the presence of a gas in the gas,
in step S3, the first time period is 30 to 120min.
Optionally, in step S4, the second temperature is 75 to 95 ℃; and/or the presence of a gas in the atmosphere,
in step S4, the third temperature is 38 to 45 ℃.
Alternatively, in step S5, the crystallization solution comprises dichloromethane and n-heptane in a volume ratio of 5 to 25.
Optionally, in step S5, the specific step of crystallizing includes:
and (3) reducing the temperature from the third temperature to 10-15 ℃ in a stepped manner, wherein the cooling time is 3-6 hours, and then keeping stirring for 2-3 hours to obtain a crystallization mixture.
Optionally, in step S5, the specific steps of separating and drying to obtain the target product include:
filtering said crystallized mixture to obtain a crystalline solid;
and transferring the crystallized solid into a double-cone dryer, and drying for 3-5 hours at 35-50 ℃ under the pressure of 0.1-0.8 MP to obtain the target product.
Optionally, the synthesis process further includes, after step S5:
s6, collecting the first liquid phase and the second liquid phase to a reaction kettle, adding dichloromethane, stirring and extracting for 1-2 hours, standing and taking an organic phase to obtain a diphenyl phosphoric acid byproduct;
and S7, collecting hydrogen chloride gas generated in the reaction, and introducing the hydrogen chloride gas into a falling film absorption tower to obtain an industrial-grade hydrochloric acid byproduct.
In the technology, the synthesis process of the diphenyl phosphorus oxide is optimized, so that the operation period is shortened, the yield of the product is greatly improved, and the quality of the product is guaranteed; meanwhile, the synthesis process of the diphenyl phosphorus oxide provided by the invention does not use benzene or toluene in the traditional synthesis process as an extracting agent, so that the toxicity of the product is greatly reduced, and the environmental pollution is reduced; the whole synthesis process is simple and safe to operate and easy to industrially popularize.
The invention also provides a synthesis system of diphenyl phosphorus oxide, which comprises the following components:
the dropping device is used for accommodating diphenyl phosphorus chloride;
the first reaction kettle is communicated with the dripping device and is used for containing distilled water;
a solid-liquid separation device for separating the first liquid phase and the first solid phase;
the second reaction kettle is used for reacting to obtain the first mixed liquid;
the third reaction kettle is used for reacting to obtain the second liquid phase and the first organic phase;
the fourth reaction kettle is used for reacting to obtain the first distillation organic phase;
a filtration device for filtering the first distilled organic phase;
the double-cone dryer is used for drying the first distillation organic phase to obtain a target product;
a fifth reaction kettle, which is used for recovering the first liquid phase and the second liquid phase and reacting to obtain the diphenyl phosphoric acid;
and the falling film absorption tower is used for recovering hydrogen chloride gas generated in the synthesis process and concentrating to obtain industrial-grade hydrochloric acid.
Optionally, the first reaction vessel is an enamel reaction vessel.
Optionally, the first reaction kettle, the second reaction kettle, the third reaction kettle and the fourth reaction kettle are the same reaction kettle.
To further illustrate the effectiveness of the enhanced diphenylphosphine oxide synthesis process of the present invention, the following example sets are chosen for the detailed description. It should be understood that the following set of examples are only intended to illustrate the effect of the synthetic process of the present invention and do not limit the synthetic process of the present invention.
The experimental methods used in the following examples were all conventional methods unless otherwise specified. Materials, reagents, equipment and the like used in the following examples are commercially available unless otherwise specified.
EXAMPLE 1 Effect of different reaction temperatures (first temperature) on the yield of diphenylphosphine oxide
1. And (3) experimental operation:
step S1, 2500 liters of distilled water is put into an enamel reaction kettle with the volume of 5000 liters, and a cooling device is arranged outside the enamel reaction kettle so as to enable the distilled water to be at a first temperature, wherein the first temperature is shown in Table 1; taking 600 kg of diphenyl phosphorus chloride in a dripping device, and adding the diphenyl phosphorus chloride into distilled water at the flow rate of 3L/min until the reaction is completed; then carrying out solid-liquid separation by a solid-liquid separation device to obtain a first liquid phase and a first solid phase;
s2, adding 600 kilograms of dichloromethane into the first solid phase until the dichloromethane is completely dissolved to obtain a first mixed solution;
s3, adding a mixed aqueous solution of sodium bicarbonate and sodium hydroxide with the concentration of 20% into the first mixed solution, washing for 30min at the speed of 90r/min, standing and separating to obtain a second liquid phase and a first organic phase; wherein in the mixed aqueous solution of sodium bicarbonate and sodium hydroxide, the volume ratio of the sodium bicarbonate to the sodium hydroxide is 1:1;
s4, distilling the first organic phase at 90 ℃ under reduced pressure, wherein the pressure is 0.1-0.8 MP, and then cooling to 40 ℃ to obtain a first distilled organic phase;
s5, adding 2000 liters of crystallization solution prepared by 10 percent of dichloromethane and 90 percent of n-heptane into the first distillation organic phase, carrying out stepped cooling to 15 ℃, and keeping stirring for 2 hours to obtain a crystallization mixture; then, carrying out suction filtration on the crystallized mixture through a filtering device to obtain a crystallized solid; transferring the crystallized solid into a double-cone dryer, distilling at 40 ℃ under reduced pressure, drying for 3 hours to obtain a target product, wherein the pressure is 0.1-0.8 MP, and obtaining a synthetic result shown in Table 1; then, under the environment of nitrogen protection, the target product is filled into a paperboard barrel;
s6, collecting the first liquid phase and the second liquid phase into a reaction kettle, adding 200 kg of dichloromethane, stirring and extracting for 1 hour, standing for layering, taking an organic phase, concentrating and crystallizing to obtain a diphenyl phosphoric acid byproduct;
and S7, collecting hydrogen chloride gas generated in the reaction, and introducing the hydrogen chloride gas into a falling film absorption tower to obtain an industrial-grade hydrochloric acid byproduct with the concentration of 32%.
TABLE 1 productivity Table at different reaction temperatures
| Group of | First temperature/. Degree.C | Purity of the product/%) | Product yield/% | Yield of by-products/%) |
| Example 1 | 5 | 97 | 65 | 35 |
| Example 2 | 10 | 97 | 75 | 25 |
| Example 3 | 20 | 99 | 80 | 20 |
| Example 4 | 25 | 98 | 75 | 25 |
| Example 5 | 30 | 96 | 65 | 35 |
2. And (4) analyzing results: the reaction temperature has certain influence on the product yield and the byproduct yield, and the influence of the reaction temperature on the product purity is not obvious. At a certain reaction temperature, the product yield is improved along with the increase of the reaction temperature, and the byproduct yield is reduced along with the increase of the reaction temperature; after a certain reaction temperature is exceeded, the product yield decreases with increasing reaction temperature, and the by-product yield increases with increasing reaction temperature. Specifically, when the reaction temperature is in the range of 5-30 ℃, the influence on the product purity is not great, and the product purity is maintained to be more than 96%. When the reaction temperature is lower than 20 ℃, the product yield is increased along with the increase of the reaction temperature, when the reaction temperature is 20 ℃, the product yield is highest and can reach 80 percent, at the moment, the byproduct yield is lowest and is 20 percent, and the product purity reaches 99 percent; when the reaction temperature is higher than 20 ℃, the product yield decreases with the increase of the reaction temperature, and the byproduct yield increases with the increase of the reaction temperature.
EXAMPLE 2 Effect of different sodium bicarbonate and sodium hydroxide ratios on Diphenylphosphine oxide
1. Experimental operation:
step S1, 2500 liters of distilled water is taken to be put into an enamel reaction kettle with the volume of 5000 liters, and a cooling device is arranged outside the enamel reaction kettle so as to enable the distilled water to be at a temperature of below 25 ℃; taking 600 kg of diphenyl phosphorus chloride in a dripping device, and adding the diphenyl phosphorus chloride into distilled water at the flow rate of 3L/min until the reaction is completed; then carrying out solid-liquid separation through a solid-liquid separation device to obtain a first liquid phase and a first solid phase;
s2, adding 600 kilograms of dichloromethane into the first solid phase until the dichloromethane is completely dissolved to obtain a first mixed solution;
s3, adding a mixed aqueous solution of sodium bicarbonate and sodium hydroxide with the concentration of 20% into the first mixed solution, washing for 30min at the speed of 90r/min, standing and separating to obtain a second liquid phase and a first organic phase; wherein, in the mixed aqueous solution of sodium bicarbonate and sodium hydroxide, the volume ratio of sodium bicarbonate and sodium hydroxide is shown in table 2;
s4, distilling the first organic phase at 90 ℃ under reduced pressure, wherein the pressure is 0.1-0.8 MP, and then cooling to 40 ℃ to obtain a first distilled organic phase;
s5, adding 2000 liters of crystallization solution prepared by 10 percent of dichloromethane and 90 percent of n-heptane into the first distillation organic phase, carrying out stepped cooling to 15 ℃, and keeping stirring for 2 hours to obtain a crystallization mixture; then, carrying out suction filtration on the crystallized mixture through a filtering device to obtain a crystallized solid; transferring the crystallized solid into a double-cone dryer, distilling at 40 ℃ under reduced pressure, drying for 3 hours to obtain a target product, wherein the pressure is 0.1-0.8 MP, and obtaining a synthetic result shown in table 2; then, under the environment of nitrogen protection, the target product is filled into a paperboard barrel;
s6, collecting the first liquid phase and the second liquid phase into a reaction kettle, adding 200 kg of dichloromethane, stirring and extracting for 1 hour, standing for layering, taking an organic phase, and concentrating and crystallizing to obtain a diphenylphosphoric acid byproduct;
and S7, collecting hydrogen chloride gas generated in the reaction, and introducing the hydrogen chloride gas into a falling film absorption tower to obtain an industrial grade hydrochloric acid byproduct with the concentration of 32%.
TABLE 2 sodium bicarbonate and sodium hydroxide Mass ratio Table
2. And (4) analyzing results: the ratio of sodium bicarbonate to sodium hydroxide has certain influence on the product purity, the product yield and the byproduct yield. Within a certain ratio range of the sodium bicarbonate to the sodium hydroxide, the product purity and the product yield are increased along with the increase of the ratio of the sodium bicarbonate to the sodium hydroxide, and the byproduct yield is reduced along with the increase of the ratio of the sodium bicarbonate to the sodium hydroxide. When the ratio of the sodium bicarbonate to the sodium hydroxide is beyond a certain range, the product purity and the product yield are both reduced along with the increase of the ratio of the sodium bicarbonate to the sodium hydroxide, and the byproduct yield is increased along with the increase of the ratio of the sodium bicarbonate to the sodium hydroxide. Specifically, when the ratio of sodium bicarbonate to sodium hydroxide is 1, the maximum product purity is 99%, the maximum product yield is 80%, and the minimum byproduct yield is 20%.
Example group 3 Effect of different dichloromethane and n-heptane ratios on crystallization Effect
1. And (3) experimental operation:
s1, placing 2500 liters of distilled water into an enamel reaction kettle with the volume of 5000 liters, wherein a cooling device is arranged outside the enamel reaction kettle to ensure that the distilled water is at a temperature of 25 ℃; taking 600 kg of diphenyl phosphorus chloride in a dropping device, and adding the diphenyl phosphorus chloride into distilled water at the flow rate of 3L/min until the reaction is completed; then carrying out solid-liquid separation by a solid-liquid separation device to obtain a first liquid phase and a first solid phase;
s2, adding 600 kg of dichloromethane into the first solid phase until the dichloromethane is completely dissolved to obtain a first mixed solution;
s3, adding a mixed aqueous solution of sodium bicarbonate and sodium hydroxide with the concentration of 20% into the first mixed solution, washing for 30min at the speed of 90r/min, standing and separating to obtain a second liquid phase and a first organic phase; wherein in the mixed aqueous solution of sodium bicarbonate and sodium hydroxide, the volume ratio of the sodium bicarbonate to the sodium hydroxide is 1:1;
s4, distilling the first organic phase at 90 ℃ under reduced pressure, wherein the pressure is 0.1-0.8 MP, and then cooling to 40 ℃ to obtain a first distilled organic phase;
step S5, adding 2000 liters of crystallization solution prepared by dichloromethane and n-heptane according to the mixture ratio shown in the table 3 into the first distillation organic phase, carrying out step cooling to 15 ℃, and keeping stirring for 2 hours to obtain a crystallization mixture; then, carrying out suction filtration on the crystallized mixture through a filtering device to obtain a crystallized solid; transferring the crystallized solid into a double-cone dryer, distilling at 40 ℃ under reduced pressure, drying for 3 hours to obtain a target product, wherein the pressure is 0.1-0.8 MP, and obtaining a synthetic result shown in table 3; then, under the environment of nitrogen protection, the target product is filled into a paperboard barrel;
s6, collecting the first liquid phase and the second liquid phase into a reaction kettle, adding 200 kg of dichloromethane, stirring and extracting for 1 hour, standing for layering, taking an organic phase, concentrating and crystallizing to obtain a diphenyl phosphoric acid byproduct;
and S7, collecting hydrogen chloride gas generated in the reaction, and introducing the hydrogen chloride gas into a falling film absorption tower to obtain an industrial-grade hydrochloric acid byproduct with the concentration of 32%.
TABLE 3 volume ratio of dichloromethane to n-heptane
2. And (4) analyzing results: the ratio of dichloromethane to n-heptane has a certain influence on the crystallization time, product purity, product yield and byproduct yield. In a certain dichloromethane-n-heptane ratio range, the crystallization time is shortened along with the increase of the dichloromethane-n-heptane ratio, the product purity and the product yield are increased along with the increase of the dichloromethane-n-heptane ratio, and the byproduct yield is reduced along with the increase of the dichloromethane-n-heptane ratio; beyond a certain range of the ratio of dichloromethane to n-heptane, the crystallization time is prolonged with the increase of the ratio of dichloromethane to n-heptane, the product purity is not influenced by the ratio of dichloromethane to n-heptane, the product yield is reduced with the increase of the ratio of dichloromethane to n-heptane, and the byproduct yield is increased with the increase of the ratio of sodium bicarbonate to sodium hydroxide. Specifically, when the ratio of dichloromethane to n-heptane is 10:90 hours, the shortest crystallization time is 3 hours, the maximum product purity is 99 percent, the maximum product yield is 80 percent, and the minimum byproduct yield is 20 percent.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (7)
1. A synthesis process of diphenyl phosphorus oxide is characterized by comprising the following steps:
step S1, putting distilled water into a first reaction kettle, putting diphenyl phosphorus chloride into a dripping device, adding diphenyl phosphorus chloride into the distilled water at a first flow rate according to the mass ratio of the distilled water to the diphenyl phosphorus chloride of 25-30-6, reacting at a first temperature, and carrying out solid-liquid separation through a solid-liquid separation device to obtain a first liquid phase and a first solid phase;
s2, adding dichloromethane into the first solid phase until the dichloromethane is completely dissolved to obtain a first mixed solution; wherein the mass ratio of the dichloromethane to the diphenyl phosphorus chloride in the step S1 is 1-3:1;
s3, adding a mixed aqueous solution of sodium bicarbonate and sodium hydroxide into the first mixed solution, washing the mixed solution for a first time at a first rotating speed, and standing and separating the mixed solution to obtain a second liquid phase and a first organic phase; wherein the mass ratio of the sodium bicarbonate and sodium hydroxide mixed aqueous solution to the diphenyl phosphorus chloride in the step S1 is 4-5.5;
s4, distilling the first organic phase at a second temperature and under the pressure of 0.1-0.8 MP, and then cooling to a third temperature to obtain a first distilled organic phase;
s5, adding a crystallization solution into the first distillation organic phase, and crystallizing, separating and drying to obtain a target product; wherein the mass ratio of the crystallization solution to the diphenyl phosphorus chloride in the step S1 is 18-25,
in step S3, the mixed aqueous solution of sodium bicarbonate and sodium hydroxide is a mixed aqueous solution of sodium bicarbonate and sodium hydroxide with a concentration of 20%, and the mass ratio of sodium bicarbonate to sodium hydroxide is 1:1;
in the step S5, the crystallization solution is dichloromethane and n-heptane with the volume ratio of 5-25;
in step S1, the first temperature is 10 to 28 ℃.
2. The process for synthesizing diphenylphosphine oxide according to claim 1, wherein in step S1, the first flow rate is 2.5 to 5L/min.
3. The process for synthesizing diphenylphosphine oxide as claimed in claim 1, wherein in step S3, the first rotation speed is 85 to 300r/min; and/or the presence of a gas in the atmosphere,
in step S3, the first time period is 30 to 120min.
4. The process for synthesizing diphenylphosphine oxide as claimed in claim 1, wherein, in step S4, the second temperature is 75-95 ℃; and/or the presence of a gas in the gas,
in step S4, the third temperature is 38 to 45 ℃.
5. The process for the synthesis of diphenylphosphine oxide as claimed in any one of claims 1 to 4, wherein, in step S5, the crystallization step comprises:
and (3) reducing the temperature from the third temperature to 10-15 ℃ in a stepped manner, wherein the time of temperature reduction is 3-6 hours, and then keeping stirring for 2-3 hours to obtain a crystallization mixture.
6. The process for synthesizing diphenylphosphine oxide as claimed in claim 1, wherein in step S5, the specific steps of separating and drying to obtain the desired product include:
filtering said crystallized mixture to obtain a crystalline solid;
and transferring the crystallized solid into a double-cone dryer, and drying for 3-5 hours at 35-50 ℃ under the pressure of 0.1-0.8 MP to obtain the target product.
7. The process for synthesizing diphenylphosphine oxide according to any one of claims 1 to 4, further comprising, after step S5:
s6, collecting the first liquid phase and the second liquid phase into a reaction kettle, adding dichloromethane, stirring and extracting for 1-2 hours, standing and taking an organic phase to obtain a diphenyl phosphoric acid byproduct;
and S7, collecting hydrogen chloride gas generated in the reaction, and introducing the hydrogen chloride gas into a falling film absorption tower to obtain an industrial-grade hydrochloric acid byproduct.
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