CN115453007A

CN115453007A - Process for quantitatively analyzing diphenyl carbonate by gas chromatography

Info

Publication number: CN115453007A
Application number: CN202211231165.0A
Authority: CN
Inventors: 唐旭; 陈建煌; 张菊; 成烽; 杨泽平
Original assignee: Hainan Huasheng New Material Technology Co ltd
Current assignee: Hainan Huasheng New Material Technology Co ltd
Priority date: 2022-10-09
Filing date: 2022-10-09
Publication date: 2022-12-09

Abstract

The invention discloses a method for quantitatively analyzing component change in a diphenyl carbonate process by a gas chromatography, which relates to the technical field of diphenyl carbonate processes, and comprises methanol, isopropanol, dimethyl carbonate, anisole, phenol, methyl benzoate, methyl phenyl carbonate, diphenyl carbonate and heavy components, wherein the content component determination method comprises the following steps: preparing chromatographic conditions, preparing a standard solution, and measuring the content by adopting a gas chromatography. The method comprises the steps of transferring 5g +/-0.5 g of sample into a 25mL volumetric flask, weighing the sample to the mass of 0.0001g, adding 0.5g +/-0.1 g of GC-grade diphenyl ether solution as an internal standard solution into the volumetric flask, weighing to the mass of 0.0001g, adding acetonitrile to the volumetric flask to the volume of 25mL, shaking uniformly, filtering the mixture through a 0.45-micron filter, adding about 1.5mL of the sample dissolving reagent into a gas chromatography vial, and using different reagents for originally dissolving different components to be detected to find a reagent capable of dissolving all DPC analysis project components and having good response with instruments, internal standards and detectors.

Description

Process for quantitatively analyzing diphenyl carbonate by gas chromatography

Technical Field

The invention relates to the technical field of diphenyl carbonate processes, in particular to a process for quantitatively analyzing diphenyl carbonate by a gas chromatography method.

Background

Diphenyl carbonate is mainly used as a raw material for synthesizing engineering plastics, such as polycarbonate, poly-p-hydroxybenzoate and the like, can also be used as a plasticizer and a solvent of cellulose nitrate, and is mainly used for synthesizing methyl isocyanate in pesticides so as to prepare carbamate pesticide carbofuran. In addition, it is mainly used in the plastics industry for the production of poly (aryl carbonate) and poly (p-hydroxybenzoic acid) polyesters, monoisocyanates, diisocyanates. Plastics plasticizers can also be prepared. The product is used as solvent and heat carrier in chemical production, and the impurities in the production process of diphenyl carbonate include acetone, o-cresol, methanol, dimethyl carbonate, anisole, phenol, methylphenyl carbonate, diphenyl carbonate, bisphenol A and other components. The components have complex reaction, more side reactions and more impurity components, more than 10 impurity components are monitored daily, and the synthesis of downstream engineering plastics, such as polycarbonate, poly-p-hydroxybenzoate and the like, can be influenced by excessive impurities. The component transformation range of the intermediate control process is wide, wherein dimethyl carbonate used as a raw material is from less than 100ppm to more than 99.95 percent in the production process, the concentration interval of the measured components is wide, the impurity types are various, and 12 impurity components can be monitored by gas chromatography. The following problems exist in the prior art:

at present, the diphenyl carbonate content determination method is more, gas chromatography, high performance liquid chromatography and the like are adopted, but no method can simultaneously analyze 12 impurities, the method comprises the steps of measuring by a plurality of instruments in a plurality of methods, and combining data to obtain a final result

Disclosure of Invention

The invention provides a process for quantitatively analyzing diphenyl carbonate by a gas chromatography, which solves the technical problems in the background technology.

In order to solve the technical problems, the technical scheme adopted by the invention is as follows:

a method for quantitatively analyzing component change in a diphenyl carbonate process by a gas chromatography method comprises the following steps of: s1, preparing chromatographic conditions, S2, preparing a standard solution, and S3, performing content measurement by adopting a gas chromatography.

The technical scheme of the invention is further improved as follows: wherein the pretreatment steps of the diphenyl carbonate intermediate control process sample are as follows: transferring 5g +/-0.5 g of sample into a 25mL volumetric flask, weighing the sample to the accurate mass of 0.0001g, adding 0.5g +/-0.1 g of GC-grade diphenyl ether solution of an internal standard solution into the volumetric flask, and weighing to the accurate mass of 0.0001g. Acetonitrile was added to a volume of 25mL, shaken well, and the pretreated sample solution was filtered through a 0.45 μm filter and added to a gas chromatography vial in an amount of about 1.5 mL.

The technical scheme of the invention is further improved as follows: the S1 also comprises the following components in percentage by mass: 300 ℃, and (2) temperature programming: initial temperature 50 ℃ holding time 5min, heating up to 100 ℃ holding time 2min at a heating rate of 10 ℃/min, heating up to 250 ℃ holding time 20min, (3) FID detector: 300 ℃ (4), program upflow: keeping the flow rate at 4mL/min for 5min, increasing the flow rate at 2mL/min to 6mL/min, and dividing the flow rate by 10:1, (5) sample injection amount: 0.2 mu L, under the condition, all components can be completely separated, and the time of all components appearing is controlled within 30 minutes, so that the analysis accuracy requirement is met and the timeliness is achieved.

The technical scheme of the invention is further improved as follows: (1) The instrument comprises a Pananol A91PLUS gas chromatograph, a split/non-split sample inlet, an FID detector and a B76 double-tower sample injector; (2) a glass graduated volumetric flask (25 mL) with a plug; (3) a one-ten-thousandth analytical balance; (4) Methanol (HPLC), isopropanol (HPLC), dimethyl carbonate (GC grade, abbreviated as DMC in the following partial data sheet), anisole (GC grade, abbreviated as ANI in the following partial data sheet), phenol (GC grade, abbreviated as PHL in the following partial data sheet), methyl benzoate (GC grade, mcoline reagent), tolyl carbonate (purity 98%, abbreviated as PMC in the following partial data sheet), diphenyl carbonate (purity not less than 99%, alatin reagent (DPC in the following partial data sheet), phenyl 2-methoxybenzoate (purity 95%).

The technical scheme of the invention is further improved as follows: the S2 also comprises that commercial high-grade pure standard substances such as methanol, isopropanol, dimethyl carbonate, anisole, phenol, methyl benzoate, methyl phenyl carbonate, diphenyl carbonate and 2-methoxybenzoate (instead of heavy component substances in the process) are purchased outside the market, the components are added into a 25mL volumetric flask according to a preparation scheme of a standard curve, the actual mass of each component in the volumetric flask is weighed to be accurate to 0.0001g, the sum of the masses of the components is within the range of 5g +/-0.5 g, 0.5g +/-0.1 g of an internal standard solution GC-grade diphenyl ether solution is added into the volumetric flask, the weighing is accurate to 0.0001g, acetonitrile is added to be constant volume to 25mL, and the mixture is fully shaken up.

The technical scheme of the invention is further improved as follows: the method comprises the following steps: controlling the content of constant dimethyl carbonate, and adopting a universal measuring method, hereinafter referred to as M1; and the method 2: a method for measuring the content of the middle control constant isopropanol and phenol, which is hereinafter referred to as M2; the method 3 comprises the following steps: a method for measuring the content of the medium-control constant methanol and anisole, which is hereinafter referred to as M3; the method 4 comprises the following steps: a method for measuring a medium-control constant diphenyl carbonate, which is hereinafter referred to as M4; the method 5 comprises the following steps: a method for measuring the content of a central control trace component, which is hereinafter referred to as M5; the design method is experimentally verified: establishing M1, M2, M3 and M4 standard curves, respectively establishing standard curves of different concentration intervals of each component according to different components determined by each method, and preparing a simulation sample with the content close to the content of the component at an actual sampling point to verify the reliability of the standard curves.

The technical scheme of the invention is further improved as follows: the S3 also comprises: chromatographic condition preparation, (1) injection port temperature: 300 ℃, and (2) temperature programming: initial temperature 50 ℃ holding time 5min, heating up to 100 ℃ holding time 2min at a heating rate of 10 ℃/min, heating up to 250 ℃ holding time 20min, (3) FID detector: 300 ℃, and (4) ascending procedure: keeping the flow rate at 4mL/min for 5min, increasing the flow rate at 2mL/min to 6mL/min, and dividing the flow rate by 10:1, (5) sample injection amount: 0.2. Mu.L, the chromatographic conditions are those of the apparatus commonly used for M1, M2, M3 and M4. .

The technical scheme of the invention is further improved as follows: the S3 also comprises: the M1, M2, M3 and M4 standard solutions are prepared by purchasing commercial superior pure standard substances of methanol, isopropanol, dimethyl carbonate, anisole, phenol, methyl benzoate, methylphenyl carbonate, diphenyl carbonate and 2-methoxybenzoate (replacing heavy component substances in the process) outside the market, adding the components into a 25mL volumetric flask according to a preparation scheme of a standard curve, weighing the actual mass of each component in the volumetric flask to be accurate to 0.0001g, adding 0.5g +/-0.1 g of GC-grade diphenyl ether solution as an internal standard solution into the volumetric flask, and weighing to be accurate to 0.0001g, wherein the mass sum of the components is within a range of 5g +/-0.5 g. Adding acetonitrile to a constant volume of 25mL, fully shaking up, and referring to an M1-M4 standard solution preparation information table in figure 2.

The technical scheme of the invention is further improved as follows: the S3 also comprises: verifying standard curves of M1, M2, M3 and M4, verifying the reliability of the standard curves by preparing a simulation sample with the content close to that of the standard curves and returning the standard solutions to the standard curves, preparing the standard solutions of M1, M2, M3 and M4, respectively adding the components into 25mL volumetric flasks according to the preparation scheme of the simulation sample by using superior pure standard substances of methanol, isopropanol, dimethyl carbonate, anisole, phenol, methyl benzoate, methyl phenyl carbonate, diphenyl carbonate and phenyl 2-methoxybenzoate (replacing heavy component substances in the process), weighing the actual mass of each component in the volumetric flasks to be 0.0001g, adding 0.5g +/-0.1 g of GC-grade diphenyl ether solution of an internal standard solution into the volumetric flasks, weighing the total mass of the components to be 0.0001g. Acetonitrile is added to the solution until the volume is 25mL, and the solution is fully shaken up.

Due to the adoption of the technical scheme, compared with the prior art, the invention has the technical progress that:

1. the invention provides a method for quantitatively analyzing component change in a diphenyl carbonate process by a gas chromatography, which comprises the steps of transferring 5g +/-0.5 g of sample into a 25mL volumetric flask, weighing the sample to the mass of 0.0001g, adding 0.5g +/-0.1 g of GC-grade diphenyl ether solution as an internal standard solution into the volumetric flask, weighing to the mass of 0.0001g. Adding acetonitrile to a constant volume of 25mL, fully shaking up, filtering the pretreated sample solution through a 0.45-micron filter, adding about 1.5mL of the sample solution into a gas chromatography vial to create a sample dissolving reagent, and using different reagents for originally dissolving different components to be detected to find a reagent which can dissolve all DPC analysis project components and has good response with instruments, internal standards and detectors.

2. The invention provides a method for quantitatively analyzing component change in a diphenyl carbonate process by a gas chromatography, which comprises the following steps: 300 ℃, temperature programming: initial temperature 50 ℃ holding time 5min, heating speed 10 ℃/min to 100 ℃ holding time 2min, heating speed 30 ℃/min to 250 ℃ holding time 20min, FID detector: 300 ℃, program upflow: keeping the flow rate at 4mL/min for 5min, increasing the flow rate at 2mL/min to 6mL/min, and dividing the flow rate by 10:1, sample size: 0.2 mu L, under the condition, each component can be completely separated, chromatographic separation conditions are innovated, an analysis condition is obtained through experiments, the solvent, the component to be detected and the internal standard substance which are found by people can be completely separated, and a detector can form linear response to each component.

3. The invention provides a method for quantitatively analyzing component change in a diphenyl carbonate process by a gas chromatography, which comprises the steps of establishing M1, M2, M3 and M4 standard curves, respectively establishing standard curves of different concentration intervals of each component according to different components determined by each method, preparing a simulation sample with the content close to the content of the component at an actual sampling point, verifying the reliability of the standard curves, innovating a data processing mode, changing an analysis item corresponding to an original concentration curve into a concentration curve corresponding to an analysis item, and reducing data processing steps.

Drawings

FIG. 1 is a schematic flow chart of the present invention

FIG. 2 is a schematic diagram of information for preparing M1-M4 standard solutions according to the present invention;

FIG. 3 is a schematic diagram of the M1 standard solution data of the present invention;

FIG. 4 is a schematic diagram of the verification data of the M1 simulation of the present invention;

FIG. 5 is a schematic diagram of the verification data of the M2 simulation of the present invention;

FIG. 6 is a schematic diagram of verification data of an M3 simulation of the present invention.

Detailed Description

The present invention will be described in further detail with reference to the following examples:

example 1

As shown in fig. 1 to 5, the present invention provides a method for quantitatively analyzing component changes in a diphenyl carbonate process by a gas chromatography, wherein each component includes methanol, isopropanol, dimethyl carbonate, anisole, phenol, methyl benzoate, methylphenyl carbonate, diphenyl carbonate and heavy components, and the method for measuring the content component includes the following steps: s1, preparing chromatographic conditions, S2, preparing a standard solution, and S3, measuring the content by adopting a gas chromatography, wherein the pretreatment step of the diphenyl carbonate intermediate control process sample comprises the following steps: transferring 5g +/-0.5 g of sample into a 25mL volumetric flask, weighing the mass of the sample to be accurate to 0.0001g, adding 0.5g +/-0.1 g of GC-grade diphenyl ether solution as an internal standard solution into the volumetric flask, and weighing to be accurate to 0.0001g. Adding acetonitrile to a constant volume of 25mL, fully shaking up, filtering the pretreated sample solution through a 0.45-micron filter, taking about 1.5mL, adding the sample solution into a gas chromatography vial, and finding a reagent which can dissolve all DPC analysis project components and has good response with instruments, internal standards and detectors.

Example 2

As shown in fig. 1 to 5, on the basis of embodiment 1, the present invention provides a technical solution: preferred (1), injection port temperature: 300 ℃, and (2) raising the temperature by program: initial temperature 50 ℃ holding time 5min, heating up to 100 ℃ holding time 2min at a heating rate of 10 ℃/min, heating up to 250 ℃ holding time 20min, (3) FID detector: 300 ℃ (4), program upflow: keeping the flow rate at 4mL/min for 5min, increasing the flow rate at 2mL/min to 6mL/min, and dividing the flow rate by 10:1, (5) sample injection amount: 0.2 mu L, under the condition, all components can be completely separated, the time of all components appearing is controlled within 30 minutes, the requirement of analysis accuracy is met, and meanwhile, the timeliness is achieved, and instruments and reagents related in the embodiment comprise: the device comprises a Pananol A91PLUS gas chromatograph, a shunting/non-shunting sample inlet, an FID detector, a B76 double-tower sample injector, a volumetric flask (25 mL) with a plug glass scale, (3) a ten thousand analytical balance, (4) methanol (HPLC), isopropanol (HPLC), dimethyl carbonate (GC grade, DMC in the following data table), anisole (GC grade, ANI in the following data table), phenol (GC grade, PHL in the following data table), methyl benzoate (GC grade, michelin reagent), tolyl carbonate (purity 98%, PMC in the following data table), diphenyl carbonate (purity is not less than 99%, arlatin reagent (DPC in the following data table), and 2-methoxybenzoic acid phenyl ester (purity 95%), innovative chromatographic separation conditions are obtained through experiments, an analytical condition can be obtained, a found solvent, a detected component and an internal standard substance are completely separated, and the detector can form a linear response to each component.

Example 3

As shown in fig. 1 to 5, on the basis of embodiment 1, the present invention provides a technical solution: preferably, by purchasing commercially superior pure standard substances of methanol, isopropanol, dimethyl carbonate, anisole, phenol, methyl benzoate, methylphenyl carbonate, diphenyl carbonate and 2-methoxybenzoic acid phenyl ester outside the market (replacing heavy component substances in the process), adding the components into a 25mL volumetric flask according to a preparation scheme of a standard curve, weighing the actual mass of each component in the volumetric flask to be accurate to 0.0001g, adding 0.5g +/-0.1 g of GC-grade diphenyl ether solution as an internal standard solution into the volumetric flask, weighing to be accurate to 0.0001g, adding acetonitrile to be constant volume to 25mL, and fully shaking.

Example 4

As shown in fig. 1 to 5, on the basis of embodiment 1, the present invention provides a technical solution: preferably, method 1: the general determination method for controlling the content of the constant dimethyl carbonate is called M1 for short, and the method 2 comprises the following steps: the method for measuring the content of the medium-control constant isopropanol and phenol is called M2 for short, and the method 3 comprises the following steps: the method for measuring the content of the medium-control constant methanol and anisole is called M3 for short, and the method 4 comprises the following steps: a method for measuring a medium-control constant diphenyl carbonate, which is hereinafter referred to as M4, and a method 5: the method for measuring the content of the central control trace component is hereinafter referred to as M5, and the design method is verified through experiments: establishing M1, M2, M3 and M4 standard curves, respectively establishing standard curves of different concentration intervals of each component according to different weight determination components of each method, preparing a simulation sample with the content close to that of the component at an actual sampling point to verify the reliability of the standard curves, verifying the M1, M2, M3 and M4 standard curves, verifying the reliability of the standard curves by preparing the simulation sample with the content close to that of the standard curves and returning the standard solution to the standard mode, preparing the M1, M2, M3 and M4 standard solutions, weighing the actual mass of each component in the volumetric flask to be accurate to 0.0001g, wherein the sum of the masses of the components is within the range of 5g +/-0.5 g, adding an internal standard solution GC 0.5g to 0.1g, and weighing the volumetric flask to be accurate to 0.0001g. Acetonitrile is added to the solution with constant volume of 25mL, the solution is fully shaken up, a data processing mode is innovated, an analysis item corresponding to an original concentration curve is changed into a concentration curve corresponding to an analysis item, and data processing steps are reduced.

The working principle of the method for quantitatively analyzing component change in the diphenyl carbonate process by using the gas chromatography is described in detail below.

As shown in fig. 1-5, first: s1, preparing chromatographic conditions, S2, preparing a standard solution, and S3, measuring the content of the diphenyl carbonate solution by adopting a gas chromatography, wherein the pretreatment step of the intermediate control process sample of the diphenyl carbonate comprises the following steps: transferring 5g +/-0.5 g of sample into a 25mL volumetric flask, weighing the sample to the accurate mass of 0.0001g, adding 0.5g +/-0.1 g of GC-grade diphenyl ether solution of an internal standard solution into the volumetric flask, and weighing to the accurate mass of 0.0001g. Adding acetonitrile to a constant volume of 25mL, fully shaking up, filtering the pretreated sample solution through a 0.45-micron filter, adding about 1.5mL of the sample solution into a gas chromatography vial, (1), the injection port temperature: 300 ℃, and (2) raising the temperature by program: initial temperature 50 ℃ holding time 5min, heating up to 100 ℃ holding time 2min at a heating rate of 10 ℃/min, heating up to 250 ℃ holding time 20min, (3) FID detector: 300 deg.C, (4), procedure upflow: keeping the flow rate at 4mL/min for 5min, increasing the flow rate at 2mL/min to 6mL/min, and dividing the flow rate by 10:1, (5) sample injection amount: 0.2 mu L, under the condition, all components can be completely separated, the peak emergence time of all components is controlled within 30 minutes, the components are added into a 25mL volumetric flask according to a preparation scheme of a standard curve, the actual mass of each component in the volumetric flask is weighed to be accurate to 0.0001g, the sum of the masses of the components is within the range of 5g +/-0.5 g, 0.5g +/-0.1 g of GC-grade diphenyl ether solution as an internal standard solution is added into the volumetric flask, the weighing is carried out to be accurate to 0.0001g, acetonitrile is added to be constant volume to 25mL, and the components are fully shaken up, wherein the method 1: the general method for measuring the content of the medium-controlled constant dimethyl carbonate is called M1 for short, and the method 2 comprises the following steps: the method for measuring the content of the medium-control constant isopropanol and phenol is called M2 for short, and the method 3 comprises the following steps: the method for measuring the content of the medium-control constant methanol and anisole is called M3 for short, and the method 4 comprises the following steps: a method for measuring a medium-control constant amount of diphenyl carbonate, which is hereinafter referred to as M4, and a method 5: the method for measuring the content of the central control trace component is hereinafter referred to as M5, and the design method is verified through experiments: establishing M1, M2, M3 and M4 standard curves, respectively establishing standard curves of different concentration intervals of each component according to different components determined by each method, preparing a simulated sample with the component content close to that of an actual sampling point, and verifying the reliability of the standard curves and preparing chromatographic conditions, (1) sampling port temperature: 300 ℃, and (2) temperature programming: initial temperature 50 ℃ holding time 5min, heating up to 100 ℃ holding time 2min at a heating rate of 10 ℃/min, heating up to 250 ℃ holding time 20min, (3) FID detector: 300 ℃, and (4) ascending the program: keeping the flow rate at 4mL/min for 5min, increasing the flow rate at 2mL/min to 6mL/min, and dividing the flow rate by 10:1, (5) sample injection amount: 0.2 mu L, wherein the chromatographic conditions are the general instrument conditions of M1, M2, M3 and M4, and the preparation of the standard solution of M1, M2, M3 and M4 is realized by purchasing commercially superior pure standard substances of methanol, isopropanol, dimethyl carbonate, anisole, phenol, methyl benzoate, methyl phenyl carbonate, diphenyl carbonate and 2-methoxybenzoate (replacing heavy component substances in the process) outside the market, adding the components into a 25mL volumetric flask according to the preparation scheme of a standard curve, weighing the actual mass of each component in the volumetric flask to the nearest 0.0001g, wherein the sum of the masses of the components is within the range of 5g +/-0.5 g, adding 0.5g +/-0.1 g of an internal standard solution GC grade diphenyl ether solution into the volumetric flask, weighing the mixture to the nearest 0.0001g. Adding acetonitrile to a constant volume of 25mL, fully shaking up, referring to an M1-M4 standard solution preparation information table in a figure 2, verifying M1, M2, M3 and M4 standard curves, verifying the reliability of the standard curves by preparing a simulation sample with the content close to that of the standard curves and returning the standard solutions to the standards, preparing the M1, M2, M3 and M4 standard solutions, respectively adding the above components into a 25mL volumetric flask according to the preparation scheme of the simulation sample by using superior pure standards of methanol, isopropanol, dimethyl carbonate, anisole, phenol, methyl benzoate, methyl phenyl carbonate, diphenyl carbonate and phenyl 2-methoxybenzoate (replacing heavy component substances in the process), weighing the actual mass of each component in the volumetric flask to be 0.0001g, weighing the sum of the masses of the components to be within the range of 5g +/-0.5 g, adding 0.5g +/-0.1 g of an internal standard solution GC grade diphenyl ether solution into the volumetric flask, and weighing the volumetric flask to be accurate to be 0.0001g. Adding acetonitrile to a constant volume of 25mL, fully shaking up, creating a data processing mode, changing an analysis item corresponding to an original concentration curve into an analysis item corresponding to a concentration curve, and reducing data processing steps.

The present invention has been described in general terms in the foregoing, but it will be apparent to those skilled in the art that modifications and improvements can be made thereto based on the present invention. Therefore, modifications or improvements are within the scope of the invention without departing from the spirit of the inventive concept.

Claims

1. The method for quantitatively analyzing the component change in the diphenyl carbonate process by using the gas chromatography is characterized by comprising the following steps of: the components comprise methanol, isopropanol, dimethyl carbonate, anisole, phenol, methyl benzoate, methylphenyl carbonate, diphenyl carbonate and heavy components, and the content component determination method comprises the following steps:

s1, preparing chromatographic conditions;

s2, preparing a standard solution;

and S3, performing content measurement by adopting a gas chromatography.

2. The method for quantitatively analyzing the component change in the diphenyl carbonate process by using the gas chromatography method according to claim 1, wherein the method comprises the following steps: wherein the pretreatment steps of the diphenyl carbonate intermediate control process sample are as follows: transferring 5g +/-0.5 g of sample into a 25mL volumetric flask, weighing the mass of the sample to be accurate to 0.0001g, adding 0.5g +/-0.1 g of GC-grade diphenyl ether solution as an internal standard solution into the volumetric flask, and weighing to be accurate to 0.0001g. Acetonitrile was added to a volume of 25mL, shaken well, and the pretreated sample solution was filtered through a 0.45 μm filter and added to a gas chromatography vial in an amount of about 1.5 mL.

3. The method for quantitatively analyzing the component change in the dpc process according to claim 1, wherein the method comprises the steps of: the S1 also comprises the following components in percentage by weight: 300 ℃, and (2) temperature programming: initial temperature 50 ℃ holding time 5min, heating up to 100 ℃ holding time 2min at a heating rate of 10 ℃/min, heating up to 250 ℃ holding time 20min, (3) FID detector: 300 deg.C, (4), procedure upflow: keeping the flow rate at 4mL/min for 5min, increasing the flow rate at 2mL/min to 6mL/min, and dividing the flow rate by 10:1, (5) sample injection amount: 0.2 mu L, under the condition, all components can be completely separated, and the time of all components appearing is controlled within 30 minutes, so that the analysis accuracy requirement is met and the timeliness is achieved.

4. The method for quantitatively analyzing the component change in the diphenyl carbonate process by using the gas chromatography method according to claim 3, wherein the method comprises the following steps: the apparatus and reagents referred to in claim 3 comprise: (1) The instrument comprises a Pananol A91PLUS gas chromatograph, a split/non-split sample inlet, an FID detector and a B76 double-tower sample injector; (2) a glass graduated volumetric flask (25 mL) with a plug; (3) a ten-thousandth analytical balance; (4) Methanol (HPLC), isopropanol (HPLC), dimethyl carbonate (GC grade, abbreviated as DMC in the following partial data sheet), anisole (GC grade, abbreviated as ANI in the following partial data sheet), phenol (GC grade, abbreviated as PHL in the following partial data sheet), methyl benzoate (GC grade, mcoline reagent), tolyl carbonate (purity 98%, abbreviated as PMC in the following partial data sheet), diphenyl carbonate (purity not less than 99%, alatin reagent (DPC in the following partial data sheet), phenyl 2-methoxybenzoate (purity 95%).

5. The method for quantitatively analyzing the component change in the diphenyl carbonate process by using the gas chromatography method according to claim 1, wherein the method comprises the following steps: the S2 also comprises that commercial high-grade pure standard substances such as methanol, isopropanol, dimethyl carbonate, anisole, phenol, methyl benzoate, methyl phenyl carbonate, diphenyl carbonate and 2-methoxybenzoate (instead of heavy component substances in the process) are purchased outside the market, the components are added into a 25mL volumetric flask according to a preparation scheme of a standard curve, the actual mass of each component in the volumetric flask is weighed to be accurate to 0.0001g, the sum of the masses of the components is within the range of 5g +/-0.5 g, 0.5g +/-0.1 g of an internal standard solution GC-grade diphenyl ether solution is added into the volumetric flask, the weighing is accurate to 0.0001g, acetonitrile is added to be constant volume to 25mL, and the mixture is fully shaken up.

6. The method for quantitatively analyzing the component change in the diphenyl carbonate process by using the gas chromatography method according to claim 1, wherein the method comprises the following steps: the S3 also comprises: the method comprises the following steps: controlling the content of constant dimethyl carbonate, and adopting a universal measuring method, hereinafter referred to as M1; and the method 2: a method for measuring the content of the middle control constant isopropanol and phenol, which is hereinafter referred to as M2; the method 3 comprises the following steps: a method for measuring the content of the medium-control constant methanol and anisole, which is hereinafter referred to as M3; the method 4 comprises the following steps: a method for measuring a medium-control constant diphenyl carbonate, which is hereinafter referred to as M4; the method 5 comprises the following steps: a method for measuring the content of a central control trace component, which is hereinafter referred to as M5; the design method is experimentally verified: establishing M1, M2, M3 and M4 standard curves, respectively establishing standard curves of different concentration intervals of each component according to different components determined by each method, and preparing a simulation sample with the content close to the content of the component at an actual sampling point to verify the reliability of the standard curves.

7. The method for quantitatively analyzing the component change in the diphenyl carbonate process by using the gas chromatography method according to claim 6, wherein the method comprises the following steps: the S3 also comprises: chromatographic condition preparation, (1) injection port temperature: 300 ℃, and (2) temperature programming: initial temperature 50 ℃ holding time 5min, heating up to 100 ℃ holding time 2min at a heating rate of 10 ℃/min, heating up to 250 ℃ holding time 20min, (3) FID detector: 300 ℃, and (4) ascending the program: keeping the flow rate at 4mL/min for 5min, increasing the flow rate at 2mL/min to 6mL/min, and dividing the flow rate by 10:1, (5) sample injection amount: 0.2. Mu.L, the chromatographic conditions are those of the apparatus commonly used for M1, M2, M3 and M4.

8. The method for quantitatively analyzing the component change in the diphenyl carbonate process by using the gas chromatography method according to claim 7, wherein the method comprises the following steps: the S3 also comprises: the M1, M2, M3 and M4 standard solutions are prepared by purchasing commercial superior pure standard substances of methanol, isopropanol, dimethyl carbonate, anisole, phenol, methyl benzoate, methylphenyl carbonate, diphenyl carbonate and 2-methoxybenzoate (replacing heavy component substances in the process) outside the market, adding the components into a 25mL volumetric flask according to a preparation scheme of a standard curve, weighing the actual mass of each component in the volumetric flask to be accurate to 0.0001g, adding 0.5g +/-0.1 g of GC-grade diphenyl ether solution as an internal standard solution into the volumetric flask, and weighing to be accurate to 0.0001g, wherein the mass sum of the components is within a range of 5g +/-0.5 g. Acetonitrile is added to the solution to a constant volume of 25mL, and the solution is fully shaken up and is referred to an M1-M4 standard solution preparation information table in figure 2.

9. The method for quantitatively analyzing the component change in the diphenyl carbonate process by using the gas chromatography method according to claim 8, wherein the method comprises the following steps: the S3 also comprises: verifying standard curves of M1, M2, M3 and M4, verifying the reliability of the standard curves by preparing a simulation sample with the content close to that of the standard curves and a standard solution returning standard mode, preparing the standard solutions of M1, M2, M3 and M4, respectively adding high-grade pure standard substances of methanol, isopropanol, dimethyl carbonate, anisole, phenol, methyl benzoate, methyl phenyl carbonate, diphenyl carbonate and phenyl 2-methoxybenzoate (replacing heavy component substances in the process) into 25mL volumetric flasks according to a preparation scheme of the simulation samples, weighing the actual mass of each component in the volumetric flasks to be 0.0001g, adding 0.5g +/-0.1 g of an internal standard solution GC-grade diphenyl ether solution into the volumetric flasks, weighing the total mass of the components to be within the range of 5g +/-0.5 g, and weighing the total mass to be 0.0001g. Acetonitrile is added to the solution until the volume is 25mL, and the solution is fully shaken up.