Method and equipment for preparing and purifying p-hydroxyphenyl ether

Abstract

The invention provides a method and equipment for preparing and purifying p-hydroxyphenyl ether, and the method comprises the following steps: reacting a phenyl ether raw material with an oxidant in the presence of a catalyst to generate a reaction product material; carrying out azeotropic distillation operation on the reaction product material; and carrying out vacuum rectification on the product flow obtained in the previous step. According to the method and the equipment disclosed by the invention, the product with high purity and excellent quality is prepared with high yield under the conditions that the energy consumption and the production cost are obviously reduced and the process is greatly simplified.

Description

Technical Field

[0001] The present application relates to the field of fine chemicals, and more specifically to a method for preparing and purifying p - hydroxy phenyl ether, and an apparatus specifically for this method. Background Art

[0002] p - Hydroxyanisole (also known as p - methoxyphenol, hydroquinone monomethyl ether, p - benzenediol monomethyl ether) and its various derivatives are widely used as efficient polymerization inhibitors in the production, storage, and transportation of chemical monomers such as acrylic acid / ester, methacrylic acid / ester, etc. In addition, such compounds are also commonly used as important raw materials or reagents for fine chemical products such as pharmaceuticals, fragrances, and pesticides. There has always been a high demand for such p - hydroxyanisole compounds in the market, and with the development of related industries, the market demand has been continuously increasing.

[0003] In contrast to the above - mentioned extremely high market demand, the methods for synthesizing p - hydroxyanisole in the prior art have always been unsatisfactory. For example, the main synthesis processes used in the prior art are the dimethyl sulfate method and the methanol method for preparing the target product through esterification reaction with hydroquinone as the raw material, and the p - aminophenetole method with p - aminophenetole as the raw material. However, the process using dimethyl sulfate as the methylating agent has the disadvantages that dimethyl sulfate is a highly toxic substance, the reaction conditions are harsh, the reaction selectivity is poor, and tar is easily generated. Although the process using methanol as the methylating agent avoids the toxicity defect of dimethyl sulfate, its disadvantages are that after the reaction, complex post - treatment processes such as extraction, neutralization, water washing, rectification, and recrystallization are required to obtain qualified products. In addition, the above - mentioned prior - art processes also have problems such as low reaction efficiency and product yield, complex reaction steps, complex catalyst regeneration, difficult product purification, complex steps, and large amounts of three wastes. In response to the above problems, researchers have invested a large amount of manpower and scientific research funds and tried to optimize and improve various reaction processes, but no significant success has been achieved. Therefore, there is an urgent need in this field to develop a new technology that can solve the above problems. Summary of the Invention

[0004] In view of the current situation in this field, the inventors have developed a novel method and apparatus through in - depth research, successfully solving the problems that have long existed in the prior art. Specifically, the first aspect of the present application provides a method for preparing and purifying p - hydroxy phenyl ether of formula A, the method comprising:

[0005] Step 1: Reacting a phenyl ether raw material of formula 1 with an oxidant in the presence of a catalyst to generate a reaction product material;

[0006]

[0007] In Formula A and Formula 1, R1, R2 and R3 are each independently selected from H, C1-C6 alkyl, C3-C6 cycloalkyl, C6-C12 aryl, halogen, halo-C1-C6 alkyl, halo-C3-C6 cycloalkyl, halo-C6-C12 aryl;

[0008] Step 2: Perform azeotropic distillation on the reaction product material;

[0009] Step 3: Perform vacuum distillation on the product stream obtained in Step 2.

[0010] According to one embodiment of the first aspect of the present application, in Step 1, R1 is selected from: methyl, ethyl, propyl or butyl. According to another embodiment of the first aspect of the present application, in Step 1, R2 and R3 are each independently selected from: hydrogen, methyl, chlorine, chloromethyl.

[0011] According to another embodiment of the first aspect of the present application, in Step 1, the oxidant is selected from one or more of the following: hydrogen peroxide, tert-butyl hydroperoxide, ozone.

[0012] According to another embodiment of the first aspect of the present application, in Step 1, the catalyst is selected from one or more of the following: titanium silicalite molecular sieve, ZSM-5 molecular sieve, γ molecular sieve, β molecular sieve.

[0013] According to another embodiment of the first aspect of the present application, before Step 2 and after Step 1, the reaction product material is filtered using a filter to remove the solid catalyst from the reaction product material. According to another embodiment of the first aspect of the present application, the filter is selected from: candle filter, precision filter, plate and frame filter.

[0014] According to another embodiment of the first aspect of the present application, in Step 2, the reaction product material is subjected to azeotropic distillation in a first distillation column to obtain a first overhead component and a first bottom component.

[0015] According to another embodiment of the first aspect of the present application, in Step 2, the first overhead component contains water and the unreacted phenyl ether raw material of Formula 1.

[0016] According to another embodiment of the first aspect of the present application, in Step 2, the first bottom component contains p-hydroxyphenyl ether of Formula A and by-products.

[0017] According to another embodiment of the first aspect of the present application, in Step 3, the first bottom component is subjected to vacuum distillation in a second distillation column to obtain a second overhead component and a second bottom component.

[0018] According to another embodiment of the first aspect of the present application, in the step three, the second overhead component contains by-products.

[0019] According to another embodiment of the first aspect of the present application, in the step three, the second bottom component contains p-hydroxyphenyl ether of formula A.

[0020] According to another embodiment of the first aspect of the present application, the method further includes separating the first overhead component in a separator to obtain separated water and unreacted phenyl ether raw material of formula 1, and recycling at least a part of the unreacted phenyl ether raw material of formula 1 back to the first rectification column to repeat the azeotropic rectification operation of the step two.

[0021] The second aspect of the present application provides a reaction-purification device for implementing the method according to any of the embodiments of the above first aspect. The device includes: a reactor R101, a filter F101, a first rectification column T101, a second rectification column T102, and a separator D102.

[0022] According to an embodiment of the second aspect of the present application, the outlet of the reactor R101 is communicated with the inlet of the filter F101; the filter F101 has an upper outlet and a bottom outlet, and its upper outlet is communicated with the inlet of the first rectification column T101; the outlet at the top of the first rectification column T101 is communicated with the inlet of the separator D102, and the outlet at the bottom of the first rectification column T101 is communicated with the inlet of the second rectification column T102.

[0023] In the following detailed implementation part, the method and polymer products of the present application are further introduced in conjunction with the drawings. Description of the Drawings

[0024] Figure 1 Shows the anisole hydroxylation reaction according to an embodiment of the present application;

[0025] Figure 2 Shows a schematic flow chart of the method according to another embodiment of the present application;

[0026] Figure 3 Shows the liquid chromatogram of p-methoxyphenol prepared according to an example of the present application.

[0027] In Figure 2 The meanings of the reference numerals appearing are as follows:

[0028] Reactor R101, filter F101, first rectification column T101, second rectification column T102, separator D102;

[0029] Anisole 1, hydrogen peroxide 2, solid catalyst 3, reaction product material 4, liquid material 5, solid material 6, first tower top component 7, recycled anisole 8, recovered anisole 9, water 10, first tower bottom component 11, second tower top component 12, second tower bottom component 13. Detailed implementation mode

[0030] The "ranges" disclosed herein are in the form of lower and upper limits. There can be one or more lower limits, and one or more upper limits respectively. A given range is defined by selecting a lower limit and an upper limit. The selected lower limit and upper limit define the boundaries of a particular range. All ranges that can be defined in this way are inclusive and combinable, that is, any lower limit can be combined with any upper limit to form a range. For example, ranges of 60 - 120 and 80 - 110 are listed for a specific parameter, and ranges of 60 - 110 and 80 - 120 are understood to be contemplated. In addition, if the minimum range values 1 and 2 are listed, and if the maximum range values 3, 4, and 5 are listed, then the following ranges are all contemplated: 1 - 3, 1 - 4, 1 - 5, 2 - 3, 2 - 4, and 2 - 5.

[0031] In this application, unless otherwise specified, the numerical range "a - b" represents an abbreviated representation of any real number combination between a and b, where a and b are both real numbers. For example, the numerical range "0 - 5" means that all real numbers between "0 - 5" have been fully listed herein, and "0 - 5" is only an abbreviated representation of these numerical combinations.

[0032] In this application, if there is no special instruction, all the implementation modes and preferred implementation modes mentioned herein can be combined with each other to form a new technical solution.

[0033] In this application, if there is no special instruction, all the technical features and preferred features mentioned herein can be combined with each other to form a new technical solution.

[0034] In this application, if there is no special instruction, the "including" mentioned herein means open-ended or can also be closed-ended. For example, the "including" can mean that other components not listed can also be included, or it can only include the listed components.

[0035] The method of the present invention first performs the first step: in the presence of a catalyst, reacting the phenyl ether raw material of formula 1 with an oxidant to generate a reaction product material.

[0036]

[0037] According to one embodiment of the present application, in Formula A and Formula 1, R1, R2, and R3 are each independently selected from H, C1-C6 alkyl, C3-C6 cycloalkyl, C6-C12 aryl, halogen, halo-C1-C6 alkyl, halo-C3-C6 cycloalkyl, halo-C6-C12 aryl; for example, R1 is selected from methyl, ethyl, propyl, or butyl, and R2 and R3 are each independently selected from hydrogen, methyl, chlorine, and chloromethyl. According to a specific embodiment, in the compound of Formula A, R1 is methyl, ethyl, or propyl, and both R2 and R3 are hydrogen atoms.

[0038] According to one embodiment of the present application, the catalyst used in the reaction of Step 1 can be one or more of the following: titanium silicalite molecular sieve, ZSM-5 molecular sieve, γ molecular sieve, β molecular sieve; preferably titanium silicalite molecular sieve. The titanium silicalite molecular sieve, ZSM-5 molecular sieve, γ molecular sieve, and β molecular sieve can be synthesized by processes known in the art or commercially purchased from suppliers. For example, the above various molecular sieve catalysts can be synthesized by mixing various raw materials (such as titanium source (such as organic carbonate), silicon source (such as organic silicate), pH regulator, template agent), etc., through self-assembly reaction under hydrothermal conditions at high pressure or under heating conditions at normal pressure. According to an exemplary embodiment of the present application, the titanium silicalite molecular sieve catalyst can be TS-1 titanium silicalite molecular sieve synthesized according to the method disclosed in US Patent US4410501.

[0039] According to one embodiment of the present application, the oxidant used in the reaction of Step 1 can be one or more of the following: hydrogen peroxide, tert-butyl hydroperoxide, ozone; the preferred oxidant is hydrogen peroxide, for example, hydrogen peroxide aqueous solution (hydrogen peroxide), and its concentration can be 5-50% by weight, preferably 10-40% by weight, more preferably 20-30% by weight.

[0040] According to one embodiment of the present application, the reaction temperature of Step 1 can be 60-90 °C. According to another embodiment of the present application, the reaction of Step 1 can be carried out under normal pressure conditions. According to another embodiment of the present application, the reaction of Step 1 can use a reaction kettle made of stainless steel or glass-lined steel, and this reaction kettle can be equipped with a gas outlet and a condensation device.

[0041] According to one aspect of the present application, in the reaction of Step 1, the weight ratio of the raw material of Formula 1 to the oxidant (such as 30% by weight hydrogen peroxide) is 10:1 to 1:2, preferably 5:1 to 1:1.

[0042] According to another aspect of the present application, in the reaction of Step 1, the weight ratio of the raw material of Formula 1 to the catalyst (such as) is 30:1 to 5:1, preferably 15:1 to 8:1, more preferably about 12:1 to 10:1.

[0043] In Figure 1 In the exemplary embodiment shown, anisole is used as a raw material and reacted with an oxidizing agent in the presence of a catalyst to produce the target product p - hydroxyanisole and by - products (o - hydroxyanisole).

[0044] According to a preferred embodiment of the present application, the method of the present invention can be carried out in a continuous manner. For example, the raw material of formula A, the oxidizing agent and the catalyst can be continuously input into the reactor in the form of a continuous stream, and the reaction product stream can be continuously withdrawn from the reactor, and subsequent steps can be continuously carried out.

[0045] According to another embodiment of the present application, the catalyst can be mixed with a small amount of water to form a suspension, and then the suspension is added to the reactor, for example, in a continuous manner. For example, in Figure 2 In the flow chart shown, the raw material anisole 1, the oxidizing agent hydrogen peroxide 2 and the catalyst 3 (such as titanium silicalite molecular sieve) can be input into the reactor R101, preferably in a continuous - flow manner. In this embodiment, a small amount of water is mixed with the catalyst to prepare a suspension (where the catalyst concentration can be 30 - 90 wt%, for example, 50 - 80 wt%, or 60 - 70 wt%), and then the suspension is added to the reaction kettle. The reaction product stream 4 generated after the reaction flows out of the reactor R101, preferably continuously.

[0046] According to an embodiment of the present application, the reaction product material mainly contains the target product (p - hydroxyanisole shown in formula A), the unreacted anisole raw material shown in formula 1, water, the solid catalyst, by - products (mainly o - hydroxyanisole) and a small amount of other impurities.

[0047] According to another embodiment of the present application, after step one, a filter is used to filter the reaction product material obtained in step one to remove the solid catalyst from the reaction product material, and then the reaction product material (liquid material, which contains the target product (p - hydroxyanisole shown in formula A), the unreacted anisole raw material shown in formula 1, water, by - products (mainly o - hydroxyanisole) and a small amount of other impurities) after removing the solid catalyst is sent to the first rectification column for azeotropic rectification.

[0048] According to an embodiment of the present application, the filter can be selected from: candle filter, precision filter, plate - and - frame filter. Preferably, the filter is a candle filter. The candle filter has a fully enclosed filtration system, which consists of a vertical container and vertically installed filter elements. With the filter element as the skeleton and the filter cloth as the filtration medium, solid - liquid separation is achieved by pressurization, and the maximum operating pressure can reach 0.6 MPa.

[0049] According to an exemplary embodiment of the present application, as Figure 2 shown, the reaction product material 4 flowing out of the reactor R101 is transported to the filter F101, where solid-liquid separation is carried out. The solid material 6 (catalyst) is output from the bottom of the filter F101, while the liquid material 5 is output from the upper or middle outlet of the filter F101. The liquid material 5 mainly contains the target product (such as p-methoxyphenol), unreacted raw materials (such as anisole), water, by-products (o-methoxyphenol), and a small amount of other impurities.

[0050] Next, step two is carried out: the liquid material is transported to the first distillation column for azeotropic distillation therein.

[0051] According to an embodiment of the present application, the bottom temperature of the first distillation column is 50 - 100 °C, the pressure is 2 - 20 kPa, the number of trays therein is 8 - 15, and the liquid material enters the first distillation column at the 6th tray.

[0052] The first overhead component is taken from the top of the first distillation column, which contains water and the unreacted phenyl ether raw material of formula 1; the first bottom component is taken from the bottom, which contains the p-methoxyphenol target product of formula A and by-products (mainly o-methoxyphenol).

[0053] For example, according to an exemplary embodiment of the present application, as Figure 2 shown, the liquid material 5 is input into the first distillation column T101 for azeotropic distillation operation therein. Thus, the first overhead component 7 is taken from the top of the first distillation column T101, which contains water and unreacted raw materials (such as anisole); the first bottom component 11 is taken from the bottom, which contains the target product (such as p-methoxyphenol) and by-products (mainly o-methoxyphenol). According to an embodiment of the present application, the "azeotropic distillation operation" described herein means that anisole slightly soluble in water can form an azeotropic mixture with water under the temperature and pressure conditions in the first distillation column, and these two components are separated from other components [target product (such as p-methoxyphenol) and by-products (mainly o-methoxyphenol)] and removed as the overhead fraction of the distillation column.

[0054] Next, step three is carried out: the first bottom component is transported to the second distillation column for vacuum distillation therein.

[0055] According to an embodiment of the present application, the bottom temperature of the second distillation column is 140 - 170 °C, the pressure is 2 - 20 kPa, the number of trays therein is 25 - 45, and the first bottom component enters the second distillation column at the 11th tray. The second overhead component is taken from the top of the second distillation column, which contains by-products (mainly o-methoxyphenol); the second bottom component is taken from the bottom, which contains the p-methoxyphenol target product of formula A.

[0056] For example, according to an exemplary embodiment of the present application, as Figure 2 shown, the first bottom component 11 is input into the second rectification column T102, where a vacuum rectification operation is performed. As a result, the first top component 12 containing by-products (such as o-methoxyphenol) is taken out from the top of the second rectification column T102; the first bottom component 13 containing the target product (such as p-methoxyphenol) is taken out from the bottom.

[0057] According to an embodiment of the present application, the method further includes performing a separation operation on the first top component in a separator to obtain separated water and the unreacted phenyl ether raw material of Formula 1, and recycling at least a part of the unreacted phenyl ether raw material of Formula 1 back to the first rectification column to repeat the azeotropic rectification operation of Step 2. According to another embodiment of the present application, part or all of the unreacted phenyl ether raw material of Formula 1 can also be recycled back to the reactor R101 as needed for the reaction in Step 1.

[0058] According to an embodiment of the present application, the separator is a baffle separator, a rotary separator, a gravity separator, a spiral channel separator, a louver separator, a film separator, a liquid distributor, etc.

[0059] For example, according to an exemplary embodiment of the present application, as Figure 2 shown, the first top component flowing out from the top 7 of the first rectification column T101 flows into the separator D102, where separation is performed. After the unreacted raw materials (such as anisole) 8 and 9 and the separated water 10 flow out from the separator D102, a part of the unreacted raw materials (such as anisole) 8 is recycled back to the first rectification column T101 for azeotropic rectification again (to remove water in the target product as completely as possible), while the unreacted raw materials (such as anisole) 9 and the separated water 10 can be collected and processed. For example, the unreacted raw materials (such as anisole) 9 can be recycled to the reactor R101 as needed for the reaction.

[0060] According to another embodiment of the present application, the present application further provides a reaction-purification device specifically designed to implement the method of the present invention described above. The device includes: a reactor R101, a filter F101, a first distillation column T101, a second distillation column T102, and a separator D102. According to an embodiment of the present application, the outlet of the reactor R101 is communicated with the inlet of the filter F101; the filter F101 has an upper outlet and a bottom outlet, and its upper outlet is communicated with the inlet of the first distillation column T101; the outlet at the top of the first distillation column T101 is communicated with the inlet of the separator D102, and the outlet at the bottom of the first distillation column T101 is communicated with the inlet of the second distillation column T102; one outlet of the separator 102 is communicated with one inlet of the first distillation column T101. According to another embodiment of the present application, the other outlet of the separator 102 may also be communicated with the reactor R101.

[0061] In the present application, when it is described that device A is "communicated" with device B, it means that a fluid (such as a liquid, a gas, a suspension, a slurry, etc.) can flow between device A and device B, but switches, pumps, flow meters, temperature regulating devices, pressure regulating devices, temperature sensors, pressure sensors, etc. may be additionally provided between device A and device B as needed.

[0062] Without wishing to be bound by any particular theory, the method of the present invention can achieve one or more of the following advantages: The method of the present invention simplifies the production-purification process flow through special design, and designs and selects the technologies and process parameters of each step in the separation section according to the properties and contents of each component, generally achieving simplified process steps, reduced equipment investment and energy consumption, and realizing high yield, high purity and excellent product quality of the target product with simple, easily obtainable and low-toxic raw materials.

[0063] In the following embodiments, specific examples are used to specifically illustrate the method of the present application, aiming to better understand the content of the present application. It should be understood that these embodiments are merely illustrative and not restrictive. The reagents used in the embodiments are all conventionally purchased from the market unless otherwise specified. The methods and conditions used in the embodiments are conventional methods and conditions unless otherwise specified.

[0064] Embodiment

[0065] The catalyst used in the following examples is TS-1 titanium silicalite molecular sieve synthesized by the method disclosed in Example 1 of US Patent US4410501. The particle size of this TS-1 is about 250 nanometers; other reagents are all analytically pure reagents purchased commercially, and the water used is deionized water. In the following examples, the contents of each component in the logistics are characterized by liquid chromatography analysis technology. The liquid chromatography used is Shimadzu LC-20AD liquid chromatograph, the chromatographic column is octadecylsilane-bonded chromatographic column, and the mobile phase is methanol-aqueous solution.

[0066] Unless otherwise specified, the percentages in the examples are all weight percentages.

[0067] This example is in accordance with Figure 2 the shown reaction-purification equipment is constructed.

[0068] The solid catalyst is pre-mixed with water to form a suspension with a catalyst content of 70% by weight. A stainless steel reactor with a volume of 50 liters is used. The reactor is equipped with a stirring device, an exhaust port, a condensation device and a temperature control device. Under the conditions of 75 °C and normal pressure, anisole 1 with a mass flow rate of 20.8 kg / h, the catalyst suspension with a mass flow rate of 2.08 kg / h, and hydrogen peroxide 2 (concentration of 30%) with a mass flow rate of 14.45 kg / h are added to the reactor for reaction. After the reaction, the reaction product stream 4 flows out of the reactor. It is measured by liquid chromatography analysis technology that the reaction product stream 4 contains 27.81% of p-hydroxyanisole, 9.89% of o-hydroxyanisole, 26.75% of anisole and 35.55% of water. In addition, the reaction product stream also contains the solid catalyst titanium silicalite molecular sieve suspended therein.

[0069] The reaction product stream 4 is transported to the filter F101 (candle filter) for filtration operation at a temperature of 35 °C and a pressure of 0.2 MPa. The solid catalyst material 6 is discharged from the bottom outlet of the filter, while the liquid material 5 is discharged from the upper outlet of the filter and transported to the downstream first distillation column T101 for azeotropic distillation operation.

[0070] The number of trays of the first distillation column T101 is 10, and the liquid material 5 is input into the first distillation column T101 at the 6th tray. The bottom temperature in the first distillation column T101 is 75 °C and the pressure is 5 kPa.

[0071] The first overhead component 7 with a flow rate of 21.74 kg / h is withdrawn from the top of the first distillation column T101. It is measured by liquid chromatography analysis technology that it contains anisole and water.

[0072] The first top component 7 is fed into the separator D102. The separator D102 is a horizontal elliptical container with internal partitions, having a volume of 5 L. Phase separation operation is carried out under the conditions of a temperature of 40 °C and a pressure of 10 kPa. Two liquid streams are withdrawn from the outlet of the separator D102. The first liquid stream is anisole, which is further divided into two liquid streams 8 and 9. The anisole in liquid stream 8 is recycled into the rectification column T101 at a mass flow rate of 4.23 kg / h for azeotropic rectification dehydration. The anisole in liquid stream 9 is recovered at a mass flow rate of 5.11 kg / h. The second liquid stream 10 is water, which is treated as wastewater with a mass flow rate of 12.41 kg / h.

[0073] The first bottom component 11 is rich in p-hydroxyanisole and o-hydroxyanisole, with a mass flow rate of 13.16 kg / h. The number of trays in the second rectification column T102 is 33. The first bottom component 11 is fed into the second rectification column T102 at the 11th tray for vacuum rectification operation. The temperature in the second rectification column T102 is 155 °C and the pressure is 10 kPa.

[0074] At the top of the second rectification column T102, the second top component 12 is withdrawn, with a mass flow rate of 3.45 kg / h. It is measured by liquid chromatography analysis technology and is o-hydroxyanisole. At the bottom of the second rectification column T102, the second bottom component 13 is withdrawn, with a mass flow rate of 9.71 kg / h. It is detected by liquid chromatography analysis technology as Figure 3 shown. The result shows that it is the target product p-hydroxyanisole with a purity of 99.5%, meeting the requirements of industrial superior grade products.

[0075] As described above, compared with the dimethyl sulfate method, dimethyl carbonate method and methanol method, which have various defects in the prior art, the present invention uses hydrogen peroxide as the oxidant, and the by-product is only water, truly realizing the green production of p-hydroxyanisole. And the reaction directly synthesizes p-hydroxyanisole from inexpensive anisole and hydrogen peroxide in one step, with simple reaction steps and low production costs. In addition, the present invention also has the advantages of high conversion rate, high yield of the target product, excellent product purity and quality.

Claims

1. A method for preparing and purifying p - hydroxy phenyl ether of formula A, the method comprising: Step 1: Reacting a phenyl ether raw material of formula 1 with an oxidant in the presence of a catalyst to produce a reaction product material; In formula A and formula 1, R1, R2 and R3 are each independently selected from H, C1 - C6 alkyl, C3 - C6 cycloalkyl, C6 - C12 aryl, halogen, halo - C1 - C6 alkyl, halo - C3 - C6 cycloalkyl, halo - C6 - C12 aryl; Step 2: Performing azeotropic distillation on the reaction product material; Step 3: Performing vacuum distillation on the product stream obtained in Step 2.

2. The method according to claim 1, characterized in that In Step 1, R1 is selected from: methyl, ethyl, propyl or butyl; R2 and R3 are each independently selected from: hydrogen, methyl, chlorine, chloromethyl.

3. The method according to claim 1, wherein In Step 1, the oxidant is selected from one or more of the following: hydrogen peroxide, tert - butyl hydroperoxide, ozone; The catalyst is selected from one or more of the following: titanium - silicon molecular sieve, ZSM - 5 molecular sieve, γ - molecular sieve, β - molecular sieve.

4. The method according to claim 1, characterized in that, After Step 1 and before Step 2, filtering the reaction product material using a filter to remove the solid catalyst from the reaction product material; The filter is selected from: candle - type filter, precision filter, plate - and - frame filter.

5. The method according to claim 1, characterized in that In Step 2, performing azeotropic distillation on the reaction product material in a first distillation column to obtain a first overhead component and a first bottom component; The first overhead component contains water and unreacted phenyl ether raw material of formula 1; The first bottom component contains p - hydroxy phenyl ether of formula A and by - products.

6. The method according to claim 5, characterized in that In Step 2, the bottom temperature in the first distillation column is 50 - 100 °C and the pressure is 2 - 20 kPa.

7. The method according to claim 5, wherein In Step 3, performing vacuum distillation on the first bottom component in a second distillation column to obtain a second overhead component and a second bottom component; The second overhead component contains by - products; The second bottom component contains p - hydroxy phenyl ether of formula A.

8. The method according to claim 7, characterized in that, In Step 3, the bottom temperature in the second distillation column is 140 - 170 °C and the pressure is 2 - 20 kPa.

9. The method according to claim 5, wherein The method further comprises separating the first overhead component in a separator to obtain separated water and unreacted phenyl ether raw material of formula 1, and recycling at least a part of the unreacted phenyl ether raw material of formula 1 back to the first distillation column to repeat the azeotropic distillation operation in Step 2.

10. A reaction-purification device for implementing the method according to any one of claims 1-9, the device comprising: Reactor (R101), filter (F101), first distillation column (T101), second distillation column (T102) and separator (D102); The outlet of the reactor (R101) is communicated with the inlet of the filter (F101); the filter (F101) has an upper outlet and a bottom outlet, and its upper outlet is communicated with the inlet of the first distillation column (T101); the outlet at the top of the first distillation column (T101) is communicated with the inlet of the separator (D102), and the outlet at the bottom of the first distillation column (T101) is communicated with the inlet of the second distillation column (T102).

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