3, 3, 3 apos; , 5, 5apos; high-conversion-rate preparation device of tetramethyl biphenol

Abstract

The utility model relates to the technical field of reaction devices, in particular to a high-conversion-rate preparation device for 3, 3 ', 5, 5'-tetramethyl biphenol. The preparation device comprises a reaction kettle, a 1 # filter, a first-stage purification kettle, a 2 # filter, a 3 # filter, a second-stage purification kettle and a 4 # filter which are sequentially connected, a discharge port of the reaction kettle is connected with a 1 # filter, a product outlet of the 1 # filter is connected with a primary purification kettle, the top of the primary purification kettle is connected with a purification reagent storage tank and an activated carbon tank, a bottom outlet is sequentially connected with a 2 # filter and a 3 # filter, a product outlet of the 3 # filter is connected with a secondary purification kettle, and the top of the secondary purification kettle is connected with the purification reagent storage tank; a bottom outlet is connected with a 4 # filter, and a product outlet of the 4 # filter is connected with a refined product collecting pipe. According to the device, TMBP is prepared through multi-step purification and separation, meanwhile, organic solid waste generated in the purification process is recycled, and the product purity and yield are high.

Description

Technical Field

[0001] The utility model relates to the technical field of reaction devices, in particular to a high conversion rate preparation device for 3,3',5,5'-tetramethylbiphenol. Background Art

[0002] 3,3′,5,5′-tetramethylbiphenol (TMBP) is an upstream raw material for epoxy resin used in the field of electronic packaging. Its metal ion content has a significant impact on the dielectric constant, curing strength and glass transition temperature of downstream epoxy resin products. At present, the process product yield of synthesizing 3,3′,5,5′-tetramethylbiphenol (TMBP) is between 60% and 80%, which will cause the waste of some raw materials, and the COD content in the generated wastewater and waste solid is high, which also increases the treatment cost of wastewater and waste solid, which invisibly increases the production cost of TMBP. Therefore, it is necessary to design a high conversion rate preparation device for 3,3′,5,5′-tetramethylbiphenol. Utility Model Content

[0003] The technical problem to be solved by the utility model is: to provide a high conversion rate preparation device for 3,3',5,5'-tetramethylbiphenol, wherein the purity of TMBP prepared by multi-step purification and separation is as high as over 99%, and the metal ion content is extremely low, and at the same time, the organic solid waste generated in the purification process is recycled to improve the TMBP conversion rate.

[0004] The high conversion rate preparation device of 3,3',5,5'-tetramethylbiphenol described in the utility model comprises a reaction kettle, a No. 1 filter, a primary purification kettle, a No. 2 filter, a No. 3 filter, a secondary purification kettle and a No. 4 filter which are connected in sequence; the discharge port of the reaction kettle is connected to the No. 1 filter; the product outlet of the No. 1 filter is connected to the primary purification kettle, and the filtrate outlet is connected to the extraction kettle; the top solvent inlet of the extraction kettle is connected to a toluene storage tank, the side solvent outlet is connected to a toluene distillation tower, and the bottom outlet of the toluene distillation tower is connected to the reaction kettle; the top of the primary purification kettle is connected to a purification reagent storage tank and an activated carbon tank, and the bottom outlet is connected to the No. 2 filter and the No. 3 filter in sequence; the product outlet of the No. 3 filter is connected to the secondary purification kettle, the filtrate outlet is connected to the purification reagent distillation tower, and the bottom outlet of the purification reagent distillation tower is connected to the reaction kettle; the top of the secondary purification kettle is connected to the purification reagent storage tank, and the bottom outlet is connected to the No. 4 filter; the product outlet of the No. 4 filter is connected to a refined product collection pipe, and the filtrate outlet is connected to the purification reagent distillation tower.

[0005] Preferably, the top of the reactor is connected to a hydrochloric acid delivery pipe, a feed pipe and an oxygen delivery pipe. The reaction raw materials are added into the reactor through the feed pipe, and oxygen is continuously introduced through the oxygen delivery pipe for reaction. After the reaction is completed, hydrochloric acid is added through the hydrochloric acid delivery pipe to adjust the pH value of the system to the required range.

[0006] Preferably, the bottom of the extraction kettle is connected to a wastewater delivery pipe, through which the wastewater in the extraction kettle is delivered to a wastewater treatment system.

[0007] Preferably, the top outlet of the toluene distillation tower is connected to a toluene storage tank after passing through a toluene condenser, a buffer tank, and a vacuum pump. The extract enters the toluene distillation tower, and toluene evaporates from the top of the tower. After condensation by the toluene condenser, it is buffered by the buffer tank and transported to the toluene storage tank by the vacuum pump for repeated use.

[0008] Preferably, the top outlet of the purification reagent distillation tower is connected to the purification reagent storage tank after passing through the purification reagent condenser. The filtrate of the 3# filter and the 4# filter enters the purification reagent distillation tower, and the purification reagent is evaporated from the top of the tower, condensed by the purification reagent condenser, and then transported to the purification reagent storage tank for repeated use.

[0009] Preferably, the 1# filter, 3# filter and 4# filter are cold filters, in which cooling crystallization and filtration of the product are simultaneously achieved; and the 2# filter is a hot filter, which only achieves the filtering function.

[0010] The working process of the high conversion rate preparation device of 3,3′,5,5′-tetramethylbiphenol is as follows:

[0011] The reaction raw materials are added to the reactor through the feed pipe, and oxygen is continuously introduced through the oxygen delivery pipe for reaction. After the reaction is completed, hydrochloric acid is added through the hydrochloric acid delivery pipe to adjust the pH value of the system to the required range, and the mixture is cooled and crystallized. The mixture is cooled, crystallized and filtered through the 1# filter. The crystals enter the first-level purification kettle through the product outlet. Purification reagents are added to the first-level purification kettle for stirring and dissolving, and activated carbon is added to adsorb the residual catalyst. The mixture is then sent to the 2# filter and the 3# filter for filtration in sequence, wherein the 2# filter is hot filtration, mainly to filter out the activated carbon, and the 3# filter is cold filtration. The product is cooled and crystallized in the 3# filter. The crystals enter the second-level purification kettle through the product outlet. Purification reagents are added to the second-level purification kettle for stirring and dissolving, and then sent to the 4# filter for cooling, crystallization and filtration. The crystals are collected through the product outlet.

[0012] In the above production process, the filtrate of the 1# filter enters the extraction kettle, toluene is added to extract the unreacted raw materials and residual products, the extract enters the toluene distillation tower, the toluene is distilled out and condensed for reuse, and the bottom liquid returns to the reactor to continue to participate in the reaction, so as to improve the utilization rate of raw materials. The filtrate of the 3# filter and the 4# filter enters the purification reagent distillation tower, the purification reagent is distilled out and condensed for reuse, and the bottom liquid returns to the reactor to continue to participate in the reaction.

[0013] Compared with the prior art, the utility model has the following beneficial effects:

[0014] The utility model discloses a high conversion rate preparation device for 3,3',5,5'-tetramethylbiphenol, which has a simple structure and is easy to operate. The utility model realizes the separation of the residual catalyst and the unreacted 2,6-dimethylphenol in the crude product of 3,3',5,5'-tetramethylbiphenol through multi-stage purification and treatment of the purified filtrate. The purity of TMBP prepared through multi-step purification and separation is as high as more than 99%, and the metal ion content is extremely low. At the same time, the purified filtrate is reused, thereby improving the conversion rate and yield of 3,3',5,5'-tetramethylbiphenol. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 This is a schematic structural diagram of a reaction device of a high conversion rate preparation device for 3,3′,5,5′-tetramethylbiphenol of the utility model;

[0016] In the figure: 1. hydrochloric acid delivery pipe; 2. feed pipe; 3. oxygen delivery pipe; 4. reactor; 5. 1# filter; 6. extraction reactor; 7. wastewater delivery pipe; 8. toluene storage tank; 9. toluene distillation tower; 10. purification reagent storage tank; 11. activated carbon tank; 12. primary purification reactor; 13. toluene condenser; 14. buffer tank; 15. vacuum pump; 16. 2# filter; 17. 3# filter; 18. secondary purification reactor; 19. 4# filter; 20. refined product collection pipe; 21. purification reagent condenser; 22. purification reagent distillation tower. DETAILED DESCRIPTION

[0017] The specific implementation methods of the present invention will be described in detail below. In order to avoid too many unnecessary details, the well-known structures or functions will not be described in detail in the following embodiments. Unless otherwise defined, the technical and scientific terms used in the following embodiments have the same meanings as those generally understood by those skilled in the art to which the present invention belongs.

[0018] Example 1

[0019] like Figure 1As shown, the high conversion rate preparation device of 3,3′,5,5′-tetramethylbiphenol of the utility model comprises a reaction kettle 4, a 1# filter 5, a primary purification kettle 12, a 2# filter 16, a 3# filter 17, a secondary purification kettle 18 and a 4# filter 19 connected in sequence; the discharge port of the reaction kettle 4 is connected to the 1# filter 5; the product outlet of the 1# filter 5 is connected to the primary purification kettle 12, and the filtrate outlet is connected to the extraction kettle 6; the top solvent inlet of the extraction kettle 6 is connected to a toluene storage tank 8, the side solvent outlet is connected to a toluene distillation tower 9, and the bottom outlet of the toluene distillation tower 9 is connected to the reaction kettle 4; The top of the first-level purification kettle 12 is connected to the purification reagent storage tank 10 and the activated carbon tank 11, and the bottom outlet is connected to the 2# filter 16 and the 3# filter 17 in sequence; the product outlet of the 3# filter 17 is connected to the secondary purification kettle 18, and the filtrate outlet is connected to the purification reagent distillation tower 22, and the bottom outlet of the purification reagent distillation tower 22 is connected to the reaction kettle 4; the top of the secondary purification kettle 18 is connected to the purification reagent storage tank 10, and the bottom outlet is connected to the 4# filter 19; the product outlet of the 4# filter 19 is connected to the refined product collection pipe 20, and the filtrate outlet is connected to the purification reagent distillation tower 22.

[0020] The top of the reactor 4 is connected to a hydrochloric acid delivery pipe 1 , a feed pipe 2 and an oxygen delivery pipe 3 .

[0021] The bottom of the extraction kettle 6 is connected to a wastewater conveying pipe 7 .

[0022] The top outlet of the toluene distillation tower 9 is connected to the toluene storage tank 8 after passing through a toluene condenser 13 , a buffer tank 14 , and a vacuum pump 15 .

[0023] The top outlet of the purification reagent distillation tower 22 is connected to the purification reagent storage tank 10 after passing through the purification reagent condenser 21 .

[0024] The 1# filter 5, 3# filter 17 and 4# filter 19 are cold filters, in which cooling crystallization and filtration of the product are simultaneously realized; the 2# filter 16 is a hot filter, which only realizes the filtering function.

[0025] The working process of the high conversion rate preparation device of 3,3′,5,5′-tetramethylbiphenol is as follows:

[0026] The reaction raw materials are added to the reactor 4 through the feed pipe 2, and oxygen is continuously introduced through the oxygen delivery pipe 3 for reaction. After the reaction is completed, hydrochloric acid is added through the hydrochloric acid delivery pipe 1 to adjust the pH value of the system to the required range, and the mixture is cooled and crystallized. The mixture is cooled, crystallized and filtered through the 1# filter 5, and the crystals enter the primary purification kettle 12 through the product outlet. A purification reagent is added to the primary purification kettle 12 for stirring and dissolving, and activated carbon is added to adsorb the residual catalyst, and then the mixture is sent to the 2# filter 16 and the 3# filter 17 for filtration in sequence, wherein the 2# filter 16 is a hot filtration, mainly to filter out the activated carbon, and the 3# filter 17 is a cold filtration, and the product is cooled and crystallized in the 3# filter 17, and the crystals enter the secondary purification kettle 18 through the product outlet, and a purification reagent is added to the secondary purification kettle 18 for stirring and dissolving, and then the mixture is sent to the 4# filter 19 for cooling, crystallization and filtration, and the crystals are collected through the product outlet.

[0027] In the above production process, the filtrate of the 1# filter 5 enters the extraction kettle 6, toluene is added to extract the unreacted raw materials and residual products, the extract enters the toluene distillation tower 9, toluene is distilled out and condensed for reuse, and the bottom liquid returns to the reactor 4 to continue to participate in the reaction to improve the utilization rate of raw materials. The filtrate of the 3# filter 17 and the 4# filter 19 enters the purification reagent distillation tower 22, the purification reagent is distilled out and condensed for reuse, and the bottom liquid returns to the reactor 4 to continue to participate in the reaction.

[0028] The above description is only a preferred embodiment of the utility model and is not intended to limit the utility model. Although the utility model is described in detail with reference to the above embodiments, those skilled in the art can still modify the technical solutions recorded in the above embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the utility model shall be included in the protection scope of the utility model.

Claims

1. A high conversion rate preparation device for 3,3',5,5'-tetramethylbiphenol, characterized in that: The invention comprises a reaction kettle (4), a No. 1 filter (5), a primary purification kettle (12), a No. 2 filter (16), a No. 3 filter (17), a secondary purification kettle (18) and a No. 4 filter (19) which are connected in sequence; the discharge port of the reaction kettle (4) is connected to the No. 1 filter (5); the product outlet of the No. 1 filter (5) is connected to the primary purification kettle (12), and the filtrate outlet is connected to the extraction kettle (6); the top solvent inlet of the extraction kettle (6) is connected to a toluene storage tank (8), and the side solvent outlet is connected to a toluene distillation tower (9); the bottom outlet of the toluene distillation tower (9) is connected to the reaction kettle (4); the top of the primary purification kettle (12) is connected to the toluene storage tank (8); the side solvent outlet is connected to a toluene distillation tower (9); the bottom outlet of the toluene distillation tower (9) is connected to the reaction kettle (4); the top of the primary purification kettle (12) is connected to the toluene storage tank (8); the bottom outlet of the toluene distillation tower (9) is connected to the reaction kettle (4); the top of the primary purification kettle (12) is connected to the toluene storage tank (8); the side solvent outlet is connected to the ... The top of the secondary purification kettle (18) is connected to the purification reagent storage tank (10) and the activated carbon tank (11), and the bottom outlet is connected to the 2# filter (16) and the 3# filter (17) in sequence; the product outlet of the 3# filter (17) is connected to the secondary purification kettle (18), and the filtrate outlet is connected to the purification reagent distillation tower (22), and the bottom outlet of the purification reagent distillation tower (22) is connected to the reaction kettle (4); the top of the secondary purification kettle (18) is connected to the purification reagent storage tank (10), and the bottom outlet is connected to the 4# filter (19); the product outlet of the 4# filter (19) is connected to the refined product collection pipe (20), and the filtrate outlet is connected to the purification reagent distillation tower (22).

2. The high conversion rate preparation device for 3,3',5,5'-tetramethylbiphenol according to claim 1, characterized in that: The top of the reaction kettle (4) is connected to a hydrochloric acid delivery pipe (1), a feed pipe (2) and an oxygen delivery pipe (3).

3. The high conversion rate preparation device for 3,3',5,5'-tetramethylbiphenol according to claim 1, characterized in that: The bottom of the extraction kettle (6) is connected to a wastewater delivery pipe (7).

4. The high conversion rate preparation device for 3,3',5,5'-tetramethylbiphenol according to claim 1, characterized in that: The top outlet of the toluene distillation tower (9) is connected to a toluene storage tank (8) via a toluene condenser (13), a buffer tank (14), and a vacuum pump (15).

5. The high conversion rate preparation device of 3,3',5,5'-tetramethylbiphenol according to claim 1, characterized in that: The top outlet of the purification reagent distillation tower (22) is connected to the purification reagent storage tank (10) after passing through the purification reagent condenser (21).

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