Method for preparing diphenyl sulfone by catalytic method
Diphenylsulfone was prepared by catalytic method, and the yield and purity were improved in the reflux reaction using Fe-type resin catalyst, which solved the problem of low purity of diphenylsulfone in the existing process, and achieved an efficient and environmentally friendly process flow, which was suitable for Solvent preparation of special engineering plastics.
Patent Information
- Application Number
- CN202310457077.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-04-25
- Publication Date
- 2024-12-13
- Estimated Expiration
- 2043-04-25
AI Technical Summary
In the existing diphenylsulfone preparation process, the solvent often contains toluene, diphenylsulfoxide, N,N-diphenylformamide, etc. during the preparation process of benzenesulfone, which leads to low purity of diphenylsulfone and complex process. More efficient preparation methods need to be explored.
By using the catalytic method, the reflux reaction of benzenesulfonyl chloride, benzene and catalyst at a predetermined temperature, the crude diphenylsulfone product was obtained, and the crystals were precipitated by decompression distillation, heat dissolution and cooling, and finally drying to obtain the pure diphenylsulfone. The Fe-type resin is used as a catalyst and is recycled to improve yield and purity.
The high yield and high purity preparation of diphenylsulfone is achieved, and it is suitable for solvents for special engineering plastics, simplifying the process flow, reducing production costs, and reducing the generation of wastewater and solid waste.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of diphenyl sulfone preparation methods, and specifically relates to a method for preparing diphenyl sulfone by catalysis. Background Art
[0002] Diphenyl sulfone and its derivatives are an important class of chemical products, which are widely used in the fields of medicine, pesticides, chemicals, papermaking, dyes, engineering materials, etc. For example, in medicine, they are used to prepare anti-epileptic drugs, phenylpropyl sulfone and other drugs; in the paper printing industry, they are used as plasticizers, thermal paper developers, and ink materials; in pesticides, they are used as ovicides and miticides; in special engineering plastics, they are used to prepare polyetheretherketone and high-temperature solvents for polyetherketone, which provides a broader prospect for the application of diphenyl sulfone.
[0003] In the prior art, the preparation process of diphenyl sulfone is as follows: For example, Chinese invention patent application No. 202010902259.0 discloses a process for extracting diphenyl sulfone from benzenesulfonyl chloride tailings. During the preparation process of benzenesulfonyl chloride, the reaction solvent often contains toluene, diphenyl sulfoxide, N,N-diphenylformamide, etc., and diphenyl sulfoxide is separated and collected from the benzenesulfonyl chloride tailings to finally prepare diphenyl sulfone. Although the proposed diphenyl sulfone has high purity, it is not prepared, but is obtained by extracting the solvent after diphenyl sulfoxide is added during the early preparation of benzenesulfonyl chloride. Therefore, it is necessary to explore a preparation process for diphenyl sulfone. Summary of the invention
[0004] In view of this, the present invention provides a new method for preparing diphenyl sulfone by catalysis.
[0005] A method for preparing diphenyl sulfone by catalysis comprises the following steps:
[0006] S1 crude diphenyl sulfone: benzenesulfonyl chloride, benzene and a catalyst are subjected to reflux reaction at a predetermined temperature. When the reaction reaches an end point, a solution containing a crude diphenyl sulfone is obtained. The crude diphenyl sulfone solution is post-treated to obtain a crude diphenyl sulfone;
[0007] S2 Purification of crude diphenyl sulfone: The crude diphenyl sulfone is subjected to reduced pressure distillation to collect the diphenyl sulfone fraction, and then the diphenyl sulfone is thermally dissolved, cooled to precipitate crystals, filtered to obtain diphenyl sulfone crystals, and then the diphenyl sulfone crystals are dried to obtain pure diphenyl sulfone.
[0008] Preferably, in the S1 crude diphenyl sulfone step, the catalyst is an Fe-type resin, and the Fe-type resin is prepared by the following steps:
[0009] Pretreatment: washing the strongly acidic ion exchange resin with hydrochloric acid, deionized water, anhydrous ethanol and acetone respectively to obtain a wet H-type resin, and then drying the wet H-type resin until the weight no longer changes to obtain an H-type resin;
[0010] Fe-type resin: H-type resin is added to an acetone solution of ferric chloride and refluxed for a predetermined time to prepare a wet Fe-type resin, the wet Fe-type resin is cooled and filtered, and washed with anhydrous ethanol and acetone respectively, and then the wet Fe-type resin is dried until the weight no longer changes to obtain a Fe-type resin, so that the Fe content in the Fe-type resin is 10%-20%.
[0011] Preferably, in the Fe-type resin step: the predetermined time is 4h-10h.
[0012] Preferably, in the S1 crude diphenyl sulfone step, the post-treatment is specifically: filtering the crude diphenyl sulfone solution, cooling the filtrate to precipitate solids to obtain Fe-type resin, the Fe-type resin is recycled as a catalyst, and the filter residue is the crude diphenyl sulfone.
[0013] Preferably, in the S1 crude diphenyl sulfone step, the catalyst is ferric chloride.
[0014] Preferably, in the step of preparing crude diphenyl sulfone in step S1, the post-treatment is specifically as follows: adding sodium hydroxide solution to the crude diphenyl sulfone solution for azeotropy, and filtering to obtain the crude diphenyl sulfone.
[0015] Preferably, in the S1 crude diphenyl sulfone step, the molar ratio of the benzenesulfonyl chloride to the benzene is 1:2-5.
[0016] Preferably, in the S1 crude diphenyl sulfone step, the reaction reaches the endpoint specifically when the benzenesulfonyl chloride content is less than 1%.
[0017] Preferably, in the S1 crude diphenyl sulfone step, the predetermined temperature is 60°C-85°C.
[0018] Preferably, in the step of purifying the crude S2 diphenyl sulfone, the thermal dissolution is specifically performed by thermal dissolution in toluene.
[0019] Compared with the prior art, the present invention has the following beneficial effects:
[0020] The method for preparing diphenyl sulfone by catalysis of the present invention comprises the following steps: subjecting benzenesulfonyl chloride and benzene to a reflux reaction at a predetermined temperature under the catalysis of a catalyst, obtaining a solution containing a crude diphenyl sulfone when the reaction reaches an end point, and performing post-treatment on the crude diphenyl sulfone solution to obtain a crude diphenyl sulfone; performing reduced pressure distillation on the crude diphenyl sulfone to collect a diphenyl sulfone fraction, then performing thermal dissolution on the diphenyl sulfone, cooling to precipitate crystals, filtering to obtain diphenyl sulfone crystals, and then drying the diphenyl sulfone crystals to obtain pure diphenyl sulfone. Therefore, the diphenyl sulfone prepared by the method has high yield and high purity and can be used for preparing a solvent for special engineering plastics. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Figure 1 This is the gas chromatogram of experiment 10. DETAILED DESCRIPTION
[0022] The technical solutions and technical effects of the embodiments of the present invention are further described in detail below in conjunction with the accompanying drawings of the present invention.
[0023] A method for preparing diphenyl sulfone by catalysis comprises the following steps:
[0024] S1 crude diphenyl sulfone: benzenesulfonyl chloride, benzene and a catalyst are subjected to reflux reaction at a predetermined temperature. When the reaction reaches an end point, a solution containing a crude diphenyl sulfone is obtained. The crude diphenyl sulfone solution is post-treated to obtain a crude diphenyl sulfone;
[0025] S2 Purification of crude diphenyl sulfone: The crude diphenyl sulfone is subjected to reduced pressure distillation to collect the diphenyl sulfone fraction, and then the diphenyl sulfone is thermally dissolved, cooled to precipitate crystals, filtered to obtain diphenyl sulfone crystals, and then the diphenyl sulfone crystals are dried to obtain pure diphenyl sulfone.
[0026] Specifically, the benzenesulfonyl chloride can be added dropwise.
[0027] Compared with the prior art, the present invention has the following beneficial effects:
[0028] The method for preparing diphenyl sulfone by catalysis of the present invention comprises the following steps: subjecting benzenesulfonyl chloride and benzene to a reflux reaction at a predetermined temperature under the catalysis of a catalyst, obtaining a solution containing a crude diphenyl sulfone when the reaction reaches an end point, and performing post-treatment on the crude diphenyl sulfone solution to obtain a crude diphenyl sulfone; performing reduced pressure distillation on the crude diphenyl sulfone to collect a diphenyl sulfone fraction, then performing thermal dissolution on the diphenyl sulfone, cooling to precipitate crystals, filtering to obtain diphenyl sulfone crystals, and then drying the diphenyl sulfone crystals to obtain pure diphenyl sulfone. Therefore, the diphenyl sulfone prepared by the method has high yield and high purity and can be used for preparing a solvent for special engineering plastics.
[0029] Furthermore, in the S1 crude diphenyl sulfone step, diphenyl sulfone is added to the raw material, and the amount of diphenyl sulfone added is 1% of the weight of the raw material.
[0030] Furthermore, in the step of preparing crude diphenyl sulfone, the catalyst is an Fe-type resin, and the Fe-type resin is prepared by the following steps:
[0031] Pretreatment: washing the strongly acidic ion exchange resin with hydrochloric acid, deionized water, anhydrous ethanol and acetone respectively to obtain a wet H-type resin, and then drying the wet H-type resin until the weight no longer changes to obtain an H-type resin;
[0032] Fe-type resin: H-type resin is added to an acetone solution of ferric chloride and refluxed for a predetermined time to prepare a wet Fe-type resin, the wet Fe-type resin is cooled and filtered, and washed with anhydrous ethanol and acetone respectively, and then the wet Fe-type resin is dried until the weight no longer changes to obtain a Fe-type resin, so that the Fe content in the Fe-type resin is 10%-20%.
[0033] Furthermore, in the Fe-type resin step: the predetermined time is 4h-10h.
[0034] Furthermore, in the S1 crude diphenyl sulfone step, the post-treatment is specifically as follows: filtering the crude diphenyl sulfone solution, cooling the filtrate to precipitate solids, obtaining an Fe-type resin, and recycling the Fe-type resin as a catalyst, and the filter residue is the crude diphenyl sulfone.
[0035] Furthermore, in the S1 crude diphenyl sulfone step, the catalyst is ferric chloride.
[0036] Furthermore, in the S1 crude diphenyl sulfone step, the post-treatment is specifically: adding sodium hydroxide solution to the crude diphenyl sulfone solution for azeotropy, and filtering to obtain the crude diphenyl sulfone.
[0037] Furthermore, in the S1 diphenyl sulfone crude product step, the molar ratio of the benzenesulfonyl chloride to the benzene is 1:2-5.
[0038] Furthermore, in the S1 crude diphenyl sulfone step, the reaction reaches the endpoint specifically when the benzenesulfonyl chloride content is less than 1%.
[0039] Furthermore, in the S1 crude diphenyl sulfone step, the predetermined temperature is 60°C-85°C.
[0040] Furthermore, in the S2 diphenyl sulfone crude product purification step, the thermal dissolution is specifically performed by thermal dissolution through toluene.
[0041] For ease of understanding, the present invention is further illustrated by the following examples:
[0042] Embodiment 1:
[0043] 1. Preparation of Fe-type resin catalyst:
[0044] Pretreatment: The strong acid ion exchange resin is: strong acid styrene cation exchange resin 732 (produced by Chengdu Kelong Chemical Co., Ltd.), with a proton exchange capacity of ≥4.2mmol / g; the strong acid styrene cation exchange resin 732 is washed with 1M-2M hydrochloric acid, deionized water, anhydrous ethanol, and acetone, respectively, and then dried under reduced pressure at 60°C for 12h to obtain an H-type resin.
[0045] Fe-type resin: Add 50g of H-type resin to 100ml of 40% ferric chloride acetone solution (w / v), heat and reflux for 6h to obtain a wet Fe-type resin; after cooling and filtering, wash the wet Fe-type resin with anhydrous ethanol and acetone respectively to remove the residual soluble iron in the resin, and then dry it at 80℃ for 12h to obtain a Fe-type resin.
[0046] 2. Preparation of diphenyl sulfone:
[0047] Test 1:
[0048] S1 Crude diphenyl sulfone: Add 8.0g Fe-type resin and 78.2g benzene (1.0mol) into a four-necked flask, install a reflux condenser and a tail gas absorber, heat the reaction solution to 70°C and stir, gradually add 44.2g benzenesulfonyl chloride (0.25mol) through a constant pressure dropping funnel for 15min; the hydrogen chloride gas produced by the reaction enters the tail gas absorber after cooling; then keep warm at 70°C for 4-6h, take samples to detect the progress of the reaction; when the benzenesulfonyl chloride content is <1%, stop keeping warm; filter while hot, recycle the Fe-type resin for the next preparation of diphenyl sulfone, and cool the hot filtrate to 10°C to precipitate a colorless to light yellow solid; filter to obtain crude diphenyl sulfone, and the reaction mother liquor is used for the preparation of the next batch of diphenyl sulfone.
[0049] Purification of crude diphenyl sulfone S2: The crude diphenyl sulfone was washed once with an equal volume of 2% NaOH hot aqueous solution, and residual water in the crude product was removed by pre-distillation; the temperature was increased for vacuum distillation, and the diphenyl sulfone fraction was collected; the obtained diphenyl sulfone was dissolved in toluene by heat, and then cooled to 5-8°C to precipitate crystals, and the obtained diphenyl sulfone crystals were filtered and dried at 90°C under reduced pressure to obtain 42.9g of white crystalline diphenyl sulfone with a yield of 78.6. The content of diphenyl sulfone and the content of chlorophenyl sulfone were 99.75% and 0.004% respectively by GC analysis.
[0050] Test 2:
[0051] S1 Crude diphenyl sulfone: 8.0 g Fe-type resin, 78.2 g benzene (1.0 mol), and 2.1 g diphenyl sulfone were added to a four-necked flask, and a reflux condenser and a tail gas absorber were installed. The temperature was raised to 70°C and stirred, and 44.2 g benzenesulfonyl chloride (0.25 mol) was gradually added dropwise through a constant pressure dropping funnel for 15 min. The hydrogen chloride gas produced by the reaction was cooled and then entered the tail gas absorber. The mixture was then kept warm at 70°C for 4-6 hours, and samples were taken to detect the progress of the reaction. When the content of benzenesulfonyl chloride was <1%, the heat preservation was stopped. The mixture was filtered while hot, and the Fe-type resin was recycled for the next preparation of diphenyl sulfone. The hot filtrate was cooled to 10°C to precipitate a colorless to light yellow solid. The crude diphenyl sulfone was obtained by filtration, and the mother liquor was used for the preparation of the next batch of diphenyl sulfone.
[0052] S2 Purification of crude diphenyl sulfone: The crude diphenyl sulfone is washed once with an equal volume of 2% NaOH hot water solution, and residual water in the crude product is removed by pre-distillation; the temperature is increased for vacuum distillation, and the diphenyl sulfone fraction is collected; the obtained diphenyl sulfone is dissolved in toluene by heat, and then cooled to 5-8°C to precipitate crystals, and the obtained diphenyl sulfone crystals are filtered. The recrystallization mother liquor can be reused, and dried at 90°C under reduced pressure to obtain 43.2g of white crystalline diphenyl sulfone, with a yield of 79.2%; and the content of diphenyl sulfone is 99.76%, and the content of chlorophenyl sulfone is 0.004%.
[0053] By comparing Experiment 1 with Experiment 2, it can be seen that adding a little diphenyl sulfone to the raw materials can increase the initial reaction rate and shorten the total reaction time. Therefore, adding an appropriate amount of diphenyl sulfone in the early stage of the reaction is beneficial to accelerate the reaction.
[0054] Experiment 3: Preparation of diphenyl sulfone by repeated use of catalyst
[0055] S1 Crude diphenyl sulfone: Add the Fe-type resin recovered in Experiment 2, the reaction mother liquor after removing diphenyl sulfone from Experiment 2 (mainly containing benzene, and the rest including diphenyl sulfone and residual benzenesulfonyl chloride), and 43g benzene (0.55mol) into a four-necked flask, install a reflux condenser and a tail gas absorption device, heat the reaction liquid to 70°C and stir, gradually add 44.5g benzenesulfonyl chloride through a constant pressure dropping funnel, and it takes 15min; the hydrogen chloride gas produced by the reaction enters the tail gas absorption device after cooling; then keep warm at 70°C for 4h, take samples to detect the progress of the reaction; stop keeping warm when the content of benzenesulfonyl chloride is less than 1%; filter while hot, recycle the Fe-type resin, and cool the hot filtrate to 10°C to precipitate solids; filter to obtain crude diphenyl sulfone, and the reaction mother liquor is directly used for the preparation of the next group of diphenyl sulfone.
[0056] S2 Purification of crude diphenyl sulfone: The purification of crude diphenyl sulfone was the same as that of S2 in Experiment 2, and diphenyl sulfone crystals were obtained, 52.6 g, with a yield of 96.5%; diphenyl sulfone content 99.95% (GC), chlorophenyl sulfone 0.005%; the recrystallization mother liquor can be reused for the recrystallization of the next batch of crude product.
[0057] Experiment 4-9: Preparation of diphenyl sulfone by continuous reuse of catalyst
[0058] S1 crude diphenyl sulfone: using the reaction mother liquor of the previous batch and the catalyst Fe-type resin obtained by filtration, after supplementing benzene (0.55 mol), a quantitative amount of benzenesulfonyl chloride (0.25 mol) was added dropwise; according to the preparation process of crude S1 diphenyl sulfone of experiment 3, the time taken for the reaction conversion rate to reach 99% was recorded; crude diphenyl sulfone was obtained, and the recycled catalyst and reaction mother liquor were used for the preparation of the next batch of diphenyl sulfone.
[0059] S2 Purification of crude diphenyl sulfone: The purification of crude diphenyl sulfone was the same as step S2 in Experiment 3.
[0060] The above method was repeated 6 times to prepare diphenyl sulfone using the recovered Fe-type resin catalyst; the diphenyl sulfone yield, content and chlorophenyl sulfone content of each group of experiments are shown in Table 1.
[0061] Table 1
[0062]
[0063] It can be seen from experiments 3-9 that the present invention solidifies the catalyst so that when benzenesulfonyl chloride reacts with benzene, the catalyst can be reused without waste, thereby reducing production costs and greatly reducing the generation of wastewater and solid waste. When the catalyst is solidified to catalyze the reaction of benzenesulfonyl chloride with benzene, the yield of diphenyl sulfone reaches more than 95%, and the content of thionyl chloride in diphenyl sulfone is low. In experiments 5, 6, 7, and 8, the content of thionyl chloride in diphenyl sulfone is below 0.005%, which can meet the requirements for the synthesis of engineering plastic polyetheretherketone.
[0064] During the reaction, when the insulation time required for the conversion rate to reach 99% exceeds 360 minutes, the Fe-type resin needs to be reactivated through the step of 1. preparing the Fe-type resin catalyst.
[0065] Test 10:
[0066] Based on the above tests, a pilot experiment was carried out.
[0067] Benzenesulfonyl chloride and benzene are mixed in a ratio of 1:4 (equivalent ratio), and diphenyl sulfone is added, wherein the amount of diphenyl sulfone added is 1% of the weight of the raw materials, and Fe-type resin is used as filler to fill a tubular reactor, and the reaction solution is transferred into the tubular reactor (preheated to 78° C.) by a peristaltic pump, and the raw materials enter the collecting bottle after reacting in the reactor, and the hydrogen chloride gas generated by the reaction enters the absorption device; the raw material consumption and product conditions are detected, and the raw material addition rate is controlled to make the benzenesulfonyl chloride react basically completely (less than 1%); after the reaction solution is collected, most of the benzene is removed by distillation, and the crude diphenyl sulfone is precipitated by cooling and crystallization; the filtrate is filtered and re-entered into the reactor for the next batch of reaction, and the obtained crude diphenyl sulfone is treated with alkaline water, pre-distilled and vacuum distilled to obtain the fine diphenyl sulfone, and recrystallized to obtain a white crystalline solid, and the preparation using a tubular reactor can make the conversion rate reach 99%, the required insulation time is about 15 minutes, the purity of diphenyl sulfone is ≥99.95%, and the content of chlorophenyl sulfone is less than 0.006%, see Figure 1 .
[0068] Pilot tests have shown that the immobilized Fe-type resin prepared by the present invention can be used as a catalyst in industrial production, and the diphenyl sulfone prepared has a short time, high yield and high purity.
[0069] Embodiment 2
[0070] S1 Crude diphenyl sulfone: Add 3.2g ferric chloride and 78.2g benzene (1.0mol) into a four-necked flask, install a reflux condenser and a tail gas absorber, heat the reaction solution to 80°C and stir, gradually add 44.2g benzenesulfonyl chloride (0.25mol) through a constant pressure dropping funnel, and it takes 15min; the hydrogen chloride gas produced by the reaction enters the tail gas absorber after cooling; then keep warm for 6h, take samples to detect the progress of the reaction; when the content of benzenesulfonyl chloride is less than 1%, stop keeping warm; gradually add the reaction solution into a 5% sodium hydroxide hot water solution, use azeotropic distillation to remove the benzene that does not participate in the reaction, and filter to obtain a yellow crude diphenyl sulfone (mainly diphenyl sulfone and ferric hydroxide);
[0071] S2 Purification of crude diphenyl sulfone: pre-distill the crude diphenyl sulfone to remove residual water in the crude product; heat up and perform vacuum distillation to collect the diphenyl sulfone fraction. The iron hydroxide in the crude diphenyl sulfone remains as residue at the bottom of the reactor during the vacuum distillation and is treated as solid waste; the obtained diphenyl sulfone is dissolved in toluene by heat, and then cooled to 5-8°C to precipitate crystals. The obtained diphenyl sulfone crystals are filtered and dried at 90°C under reduced pressure to obtain 51.5g of white crystalline diphenyl sulfone, with a yield of 94.5%, and the content of diphenyl sulfone is 99.91% (GC detection), 0.006% of chlorophenyl sulfone, and the required insulation time for the conversion rate to reach 99% is 300min.
[0072] By comparing Experiments 3-10 with Example 2, it can be seen that (1) by curing the catalyst into an Fe-type resin, the catalyst can be easily and effectively separated from other components in the solution after the S1 diphenyl sulfone crude product is prepared, making the purification of the diphenyl sulfone crude product simpler and more convenient; (2) and the Fe-type resin is cured, so that in the reaction, the catalyst loss is reduced, the catalyst can be recycled, the post-treatment wastewater is reduced, and the catalyst solid waste in conventional production is eliminated, which meets the requirements of green production; (3) the Fe-type resin is cured in the preparation of diphenyl sulfone, and the continuous flow technology (experiment 10) is used, so that the heating area of the reaction system is small, the reaction conditions are controllable, and the reaction time is short, so that various factors affecting the organic reaction such as excessive reaction speed or excessive temperature can be avoided; at the same time, the formation of by-products is reduced, the tail gas is controllable, and the reaction can be carried out continuously, and the manual error is relatively greatly reduced; (4) and the Fe-type resin is compared with the ferric chloride catalyst, and the catalytic activity of the Fe-type resin catalyst is higher than that of the ferric chloride catalyst, so the reaction time is greatly reduced.
[0073] What is disclosed above is only a preferred embodiment of the present invention, which certainly cannot be used to limit the scope of rights of the present invention. A person skilled in the art can understand that all or part of the processes of the above embodiments and equivalent changes made according to the claims of the present invention still fall within the scope of the invention.
Claims
1. A method for preparing diphenyl sulfone by catalysis, characterized in that: The following steps are included: S1 crude diphenyl sulfone: benzenesulfonyl chloride, benzene and a catalyst are subjected to reflux reaction at a predetermined temperature. When the reaction reaches an end point, a solution containing a crude diphenyl sulfone is obtained. The crude diphenyl sulfone solution is post-treated to obtain a crude diphenyl sulfone; In the S1 diphenyl sulfone crude product step, the catalyst is an Fe-type resin, and the Fe-type resin is prepared by the following steps: Pretreatment: washing the strongly acidic ion exchange resin with hydrochloric acid, deionized water, anhydrous ethanol and acetone respectively to obtain a wet H-type resin, and then drying the wet H-type resin until the weight no longer changes to obtain an H-type resin; Fe-type resin: adding H-type resin to an acetone solution of ferric chloride and refluxing for a predetermined time to prepare a wet Fe-type resin, cooling and filtering the wet Fe-type resin, and washing with anhydrous ethanol and acetone respectively, and then drying the wet Fe-type resin until the weight no longer changes to obtain the Fe-type resin, so that the Fe content in the Fe-type resin is 10%-20%; S2 Purification of crude diphenyl sulfone: The crude diphenyl sulfone is subjected to reduced pressure distillation to collect the diphenyl sulfone fraction, and then the diphenyl sulfone is thermally dissolved, cooled to precipitate crystals, filtered to obtain diphenyl sulfone crystals, and then the diphenyl sulfone crystals are dried to obtain pure diphenyl sulfone.
2. The method for preparing diphenyl sulfone by catalysis as claimed in claim 1, characterized in that: In the Fe-type resin step: the predetermined time is 4h-10h.
3. The method for preparing diphenyl sulfone by catalysis as claimed in claim 1, characterized in that: In the step of preparing crude diphenyl sulfone in step S1, the post-treatment is as follows: filtering the crude diphenyl sulfone solution, cooling the filtrate to precipitate solids, and obtaining Fe-type resin, which is recycled as a catalyst, and the filter residue is the crude diphenyl sulfone.
4. The method for preparing diphenyl sulfone by catalysis as claimed in claim 1, characterized in that: In the S1 diphenyl sulfone crude product step, the catalyst is ferric chloride.
5. The method for preparing diphenyl sulfone by catalysis as claimed in claim 4, characterized in that: In the step S1 of preparing crude diphenyl sulfone, the post-treatment is specifically as follows: adding sodium hydroxide solution to the crude diphenyl sulfone solution for azeotropy, and filtering to obtain the crude diphenyl sulfone.
6. The method for preparing diphenyl sulfone by catalysis as claimed in claim 1, characterized in that: In the S1 crude diphenyl sulfone step, the molar ratio of the benzenesulfonyl chloride to the benzene is 1:2-5.
7. The method for preparing diphenyl sulfone by catalysis as claimed in claim 1, characterized in that: In the S1 crude diphenyl sulfone step, the reaction reaches the endpoint specifically when the benzenesulfonyl chloride content is less than 1%.
8. The method for preparing diphenyl sulfone by catalysis as claimed in claim 1, characterized in that: In the S1 crude diphenyl sulfone step, the predetermined temperature is 60°C-85°C.
9. The method for preparing diphenyl sulfone by catalysis as claimed in claim 2, characterized in that: In the S2 diphenyl sulfone crude product purification step, the thermal dissolution is specifically performed by thermal dissolution through toluene.
