Reinforced reaction system for preparing epoxy resin

Abstract

The utility model relates to the technical field of epoxy resin preparation, and provides an enhanced reaction system for preparing epoxy resin, the enhanced reaction system comprises a feeding unit, a reaction unit and a circulating unit, the reaction unit comprises a reaction kettle, a micro-interface generator is arranged in the reaction kettle, the micro-interface generator is connected with the feeding unit, and the circulating unit is connected with the feeding unit; the circulating unit comprises a circulating pipeline and a circulating pump, the feeding end of the circulating pipeline is connected with the bottom end of the reaction kettle, the discharging end of the circulating pipeline is connected with the micro-interface generator, and the circulating pump is arranged on the circulating pipeline. The system realizes full solid-liquid and liquid-liquid contact and continuous material treatment, and has the advantages of cost saving, continuous production and safer production process. Meanwhile, compared with a traditional reactor, the system has the advantages that the phase boundary area in the system is increased by more than 50 times, and the production efficiency is improved by more than 20%.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of epoxy resin preparation, and more particularly relates to a reinforced reaction system for preparing epoxy resin. BACKGROUND

[0002] Epoxy resin is a kind of organic polymer with two or more epoxy groups in the molecular structure, which has a wide range of applications in adhesives, coatings, casting materials, molding materials, adhesives, laminates and other fields. At present, low molecular weight liquid epoxy resin and medium molecular weight solid epoxy resin generally adopt one-step process; high molecular weight epoxy resin adopts two-step process. Epoxy resin can be synthesized by two-step process (etherification reaction and polycondensation reaction) in industry. Two-step process is that organic raw materials and epichlorohydrin are reacted under the action of a catalyst (such as quaternary ammonium salt) to generate a diphenylpropane chlorohydrin ether intermediate in the first step, and then a ring-closing polycondensation reaction is carried out under the action of NaOH (sodium hydroxide solution) to generate epoxy resin in the second step.

[0003] However, most of the current epoxy resin preparation processes are non-continuous processes, which have high time cost and complex operation difficulty. Compared with non-continuous process, the advantage of continuous production is that the process is highly automated, the production efficiency is often higher than that of non-continuous production, and it is suitable for large-scale and standardized production environment, which can greatly save time, material and operation cost.

[0004] The epoxy resin preparation process is relatively traditional, and a traditional stirred tank reactor is used, which has the problems of uneven mixing, low intrinsic safety of the device, poor oil-water mass transfer efficiency, long reaction time, etc. Therefore, new process intensification technology equipment is needed to realize the transformation and upgrading of the epoxy resin production process. SUMMARY

[0005] In view of the above-mentioned deficiencies of the existing transmission stirred tank reactor, the purpose of the embodiments of the present application is to provide a reinforced reaction system for preparing epoxy resin, which has the advantages of continuous production and improved production efficiency.

[0006] To achieve the above-mentioned purpose, the technical scheme adopted by the present application is to provide a reinforced reaction system for preparing epoxy resin, comprising: a feeding unit, a reaction unit and a circulating unit, the reaction unit comprises a reaction kettle, a micro-interface generator is arranged in the reaction kettle, the micro-interface generator is connected with the feeding unit, the circulating unit comprises a circulating pipeline and a circulating pump, the feeding end of the circulating pipeline is connected with the bottom end of the reaction kettle, the discharging end of the circulating pipeline is connected with the micro-interface generator, and the circulating pump is arranged on the circulating pipeline.

[0007] In an embodiment, the micro-interface generator is a pneumatic micro-interface generator, a hydraulic micro-interface generator, and / or a pneumatic-hydraulic micro-interface generator.

[0008] In an embodiment, the micro-interface generator generates micro-droplets with a diameter of greater than or equal to 1 pm and less than 1 mm.

[0009] In an embodiment, the micro-droplets have a diameter of 200-400 pm.

[0010] In an embodiment, a circulation heater is provided on the circulation pipeline.

[0011] In an embodiment, a branch pipeline is provided on the circulation pipeline, one end of the branch pipeline is connected to the middle part of the reaction kettle, and the other end of the branch pipeline is connected to the circulation pipeline.

[0012] In an embodiment, the top of the reaction kettle is connected to a cooler through a separation pipeline, the cooler is connected to an oil-water separator, and the oil-water separator is connected to the micro-interface generator through a reflux pipeline.

[0013] In an embodiment, the feeding unit includes a raw material storage tank and a NaOH storage tank, and the raw material storage tank and the NaOH storage tank are respectively connected to the reaction kettle through a raw material feeding pipeline, and an alkali feeding pump is provided on the raw material feeding pipeline connected to the NaOH storage tank.

[0014] In an embodiment, a temperature sensor is provided on the reaction kettle.

[0015] The preparation of the reinforced reaction system for epoxy resin provided by the present application has the following advantages:

[0016] 1. By providing a micro-interface generator connected to the feeding unit inside the reaction kettle, the phase interface mass transfer area between epichlorohydrin and organic raw materials during etherification reaction is increased by more than 50 times;

[0017] 2. The advantage of continuous production is that the process is highly automated, the production efficiency is improved by about 20%, and it is suitable for large-scale and standardized production environment, which can greatly save time, materials and operation cost;

[0018] 3. The circulation pump is arranged outside the reaction kettle, which isolates certain safety risks, makes the two-phase mixing more sufficient, improves the safety of the system and can appropriately improve the mass transfer performance in the reaction kettle, and provides reliable experience for continuous production of epoxy resin. BRIEF DESCRIPTION OF DRAWINGS

[0019] In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the embodiments or prior art description will be briefly introduced. Obviously, the drawings in the following description only constitute some embodiments of the present application, and other drawings can be obtained by those skilled in the art without any creative effort.

[0020] Figure 1 A simplified structure schematic diagram of a reinforced reaction system for preparing epoxy resin provided by the embodiments of the present application.

[0021] In the drawings, various reference signs:

[0022] 1, raw material storage tank; 2, NaOH storage tank; 3, raw material feeding pipeline; 4, lye feeding pump; 5, reaction kettle; 6, micro-interface generator; 7, circulating pump; 8, circulating heater; 9, cooler; 10, oil-water separator. DETAILED DESCRIPTION

[0023] In order to make the technical problems, technical solutions and beneficial effects of the present application more clearly understood, the present application will be further described in detail below with reference to the drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present application and not intended to limit the present application.

[0024] It should be noted that when an element is referred to as being "fixed to" or "disposed on" another element, it can be directly on the other element or indirectly on the other element. When an element is referred to as being "connected to" another element, it can be directly connected to the other element or indirectly connected to the other element.

[0025] It should be understood that the terms "length", "width", "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only used to facilitate the description of the present application and simplify the description, and therefore cannot be understood as indicating or implying that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the present application.

[0026] In addition, the terms "first", "second", "third", etc. are only used for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Therefore, the features defined with "first", "second", etc. can explicitly or implicitly include one or more of the features. In the description of the present application, the meaning of "multiple" is two or more, unless otherwise specifically limited.

[0027] As Figure 1As shown, the present application provides a kind of preparation of epoxy resin enhanced reaction system. The preparation of epoxy resin enhanced reaction system is prepared by etherification polycondensation reaction of organic raw materials and epichlorohydrin epoxy resin, wherein the organic raw material can be diphenyl A, bisphenol F, bisphenol S and other diphenyl compounds, hydrogenated bisphenol type compound. Specifically, the preparation of epoxy resin enhanced reaction system, including: feed unit, reaction unit and circulating unit. Feed unit includes raw material storage tank 1 and NaOH storage tank 2, raw material storage tank 1 is used to store and transport organic raw materials and epichlorohydrin; NaOH storage tank 2 is used to store and transport NaOH solution; wherein, raw material storage tank 1 and NaOH storage tank 2 are connected by a raw material feeding pipe 3 and reaction kettle 5 respectively, and the raw material feeding pipe 3 connected with NaOH storage tank 2 is provided with lye feeding pump 4.

[0028] Wherein, reaction unit includes reaction kettle 5, reaction kettle 5 as organic raw materials and epichlorohydrin etherification reaction, diphenyl propane chlorohydrin ether intermediate and NaOH polycondensation reaction place; reaction kettle 5 is equipped with micro-interface generator 6, micro-interface generator 6 is connected with feed unit, for accepting reaction raw materials, and before reaction, epichlorohydrin / NaOH is broken into micron level microdroplets, the phase interface mass transfer area between epichlorohydrin and organic raw materials, diphenyl propane chlorohydrin ether intermediate and NaOH in etherification polycondensation reaction process is increased by 50-100 times, and the etherification and polycondensation reaction efficiency is improved by 20%.

[0029] Wherein, circulating unit includes circulating pipe and circulating pump 7, the inlet end of circulating pipe is connected with the bottom end of reaction kettle 5, the outlet end of circulating pipe is connected with micro-interface generator 6, and circulating pump 7 is arranged on circulating pipe; circulating pump 7 is used for circulating reaction liquid, and the mixture is continuously extracted and circulated back to reaction kettle 5. Branch pipe is arranged on circulating pipe, one end of branch pipe is connected with the middle part of reaction kettle 5, and the other end of branch pipe is connected with circulating pipe, so as to realize the circulation of reaction liquid at different positions; circulating pipe is provided with circulating heater 8, which is used for temperature control of reaction circulating liquid.

[0030] Wherein, the top of reaction kettle 5 is connected with cooler 9 through separation pipe, cooler 9 is connected with oil-water separator 10, oil-water separator 10 is connected with micro-interface generator 6 through reflux pipe, which is used for purifying product. Wherein, cooler 9 is used for cooling azeotrope, and then azeotrope is separated by oil-water separator 10, oil phase epichlorohydrin returns to reaction kettle 5 through reflux pipe, and water phase enters waste water system for treatment.

[0031] Wherein, temperature monitoring unit is further connected with reaction kettle 5, and temperature monitoring unit includes temperature sensor, which is used for detecting temperature change in reaction kettle 5.

[0032] In the present embodiment, the micro-interface generator 6 is divided into a pneumatic micro-interface generator, a hydraulic micro-interface generator and a gas-liquid linkage micro-interface generator according to the energy input mode or the gas-liquid ratio. Among them, the pneumatic micro-interface generator 6 adopts gas driving, and the input gas amount is much larger than the liquid amount; the hydraulic micro-interface generator 6 adopts liquid driving, and the input gas amount is generally less than the liquid amount; the gas-liquid linkage micro-interface generator 6 adopts gas-liquid simultaneous driving, and the input gas amount is close to the liquid amount. In the present embodiment, the micro-interface generator 6 can be one or several of the pneumatic micro-interface generator, the hydraulic micro-interface generator and the gas-liquid linkage micro-interface generator.

[0033] In the present embodiment, the micro-interface generator 6 converts the pressure energy of the gas and / or the kinetic energy of the liquid into the surface energy of the droplets and transmits it to the epoxy chloropropane / NaOH droplets, so that the epoxy chloropropane / NaOH is broken into micron-sized microdroplets with a diameter greater than or equal to 1 μm and less than 1 mm. Preferably, the size of the microdroplets is concentrated in 200 μm - 400 μm.

[0034] Embodiment 1:

[0035] The catalyst is filled into the reaction kettle 5, the organic raw material and the epoxy chloropropane are filled into the raw material storage tank 1, the NaOH solution is filled into the NaOH storage tank 2, the raw material feeding pipeline 3 is connected with the raw material storage tank 1 and the NaOH storage tank 2, and the system is started. The system temperature is set to 50°C, the organic raw material and the epoxy chloropropane are transported into the reaction kettle 5, at the same time, the epoxy chloropropane is transported into the micro-interface generator 6 through the raw material feeding pipeline 3. The epoxy chloropropane in the reaction kettle 5 is etherified with the organic raw material under the action of the catalyst to generate diphenyl propane chlorohydrin ether, at the same time, the micro-interface generator 6 breaks the epoxy chloropropane into micron-sized microdroplets, the particle size of the microdroplets is concentrated in about 300 μm, and the microdroplets are released into the reaction kettle 5, so that the epoxy chloropropane is in the state of microdroplets and fully contacts with the organic raw material to carry out the etherification reaction. The azeotrope of the etherification reaction is transported into the cooler 9 for cooling treatment, after the cooling is completed, it is transported into the oil-water separator 10 for phase separation treatment of the water and the epoxy chloropropane transported from the cooler 9, the oil phase epoxy chloropropane after the phase separation is recycled to the reaction kettle 5 for the etherification reaction in the reaction kettle 5 again, and the water phase is transported to the wastewater treatment system.

[0036] After the etherification reaction is completed, NaOH is filled into the reaction kettle 5 through the lye feeding pump 4, broken into micron-sized microdroplets by the micro-interface generator 6, the microdroplet particle size is concentrated at about 300 μm, and the microdroplets are released into the reaction kettle 5 to increase the phase interface mass transfer area between the diphenyl propane chlorohydrin ether and NaOH in the polycondensation reaction process, so that the NaOH is in the state of microdroplets and fully contacts with the diphenyl propane chlorohydrin ether, and the polycondensation reaction is carried out. During the polycondensation reaction, the circulating pump 7 connected with the reaction kettle 5 is used to circulate the reaction liquid, and the polycondensation reaction mixture is continuously extracted and circulated back to the reaction kettle 5.

[0037] Then the crude resin in the reaction kettle 5 is introduced into the subsequent purification process for purification treatment (the subsequent purification process is used to treat the crude resin formed in the reaction kettle 5, such as solvent recovery, refining extraction, etc., to purify the target product), and finally the high-purity epoxy resin product is obtained, and the epoxy resin is collected. The whole production efficiency is improved by about 22%.

[0038] Example 2

[0039] Compared with Example 1, other conditions remain unchanged, the system temperature is set to 52℃, and the microdroplet particle size is concentrated at about 280 μm. The production efficiency is improved by about 25%.

[0040] Example 3

[0041] Compared with Example 1, other conditions remain unchanged, the system temperature is set to 48℃. The microdroplet particle size is concentrated at about 350 μm. The production efficiency is improved by about 21%.

[0042] Comparative Example 1

[0043] The process method of Example 1 is adopted, except that the micro-interface generator 6 and the circulating pump 7 are removed, and the existing mechanical stirring type reaction kettle is used, and the mechanical stirring is used instead of the function of the circulating pump 7.

[0044] Analysis of the results under the conditions of this comparative example: the droplet particle size is concentrated at about 2 mm. The production efficiency is not improved.

[0045] Comparative Example 2

[0046] The process method of Example 1 is adopted, except that the micro-interface generator 6 is retained, and only the circulating pump 7 is removed, and the mechanical stirring is used instead of the circulating pump.

[0047] Analysis of the results under the conditions of this comparative example: the droplet particle size is concentrated at about 320 μm. The production efficiency is improved by about 10%.

[0048] Comparative Example 3

[0049] The process of Example 1 is adopted, except that the circulating pump 7 is retained and only the micro-interface generator 6 is removed.

[0050] Analysis of the results under the conditions of the comparative example: the droplet size is concentrated at about 2 mm. The production efficiency is not improved.

[0051] The microdroplet size, temperature of the reaction kettle and production efficiency improvement data of Examples 1-3 and Comparative Examples 1-3 are collated as follows:

[0052]

[0053] Comparing Examples 1-3, it can be seen that under the condition of having both a micro-interface generator and a circulating pump, the higher the temperature, the smaller the microdroplet size formed, and the higher the production efficiency improvement.

[0054] Comparing Example 1 with Comparative Example 1, it can be seen that the provision of a micro-interface generator and a circulating pump has a significant effect on the improvement of production efficiency.

[0055] Comparing Example 1 with Comparative Example 2, it can be seen that stirring using a circulating pump has a certain effect on the improvement of production efficiency compared with conventional mechanical stirring.

[0056] Comparing Example 1 with Comparative Examples 1 and 3, it can be seen that simply replacing conventional mechanical stirring with a circulating pump does not produce small-sized microdroplets and does not improve production efficiency, i.e. the size of the microdroplets affects production efficiency.

[0057] In summary, the use of both a micro-interface generator 6 and a circulating pump 7 in the present embodiment improves production efficiency.

[0058] The above only describes the preferred embodiments of the present application and is not intended to limit the present application. Any modifications, equivalent replacements and improvements made within the spirit and principle of the present application should be included in the protection scope of the present application.

Claims

1. A reinforcing reaction system for preparing epoxy resin, characterized in that, include: The unit comprises a feeding unit, a reaction unit, and a circulation unit. The reaction unit includes a reactor (5), which is equipped with a micro-interface generator (6). The micro-interface generator (6) is connected to the feeding unit. The circulation unit includes a circulation pipe and a circulation pump (7). The feed end of the circulation pipe is connected to the bottom end of the reactor (5), and the discharge end of the circulation pipe is connected to the micro-interface generator (6). The circulation pump (7) is installed on the circulation pipe.

2. The epoxy resin strengthening reaction system as described in claim 1, characterized in that: The micro-interface generator (6) is a pneumatic micro-interface generator, a hydraulic micro-interface generator, and / or a pneumatic-hydraulic linkage micro-interface generator.

3. The epoxy resin strengthening reaction system as described in claim 2, characterized in that: The microdroplets generated by the micro-interface generator (6) have a diameter greater than or equal to 1 μm and less than 1 mm.

4. The epoxy resin strengthening reaction system as described in claim 3, characterized in that: The diameter of the microdroplets is 200-400 μm.

5. The epoxy resin strengthening reaction system as described in claim 4, characterized in that: A circulating heater (8) is provided on the circulating pipeline.

6. The epoxy resin strengthening reaction system as described in claim 5, characterized in that: The circulation pipeline is provided with a branch pipe, one end of which is connected to the middle of the reactor (5), and the other end of which is connected to the circulation pipeline.

7. The epoxy resin strengthening reaction system according to any one of claims 1-6, characterized in that: The top of the reactor (5) is connected to a cooler (9) via a separation pipe. The cooler (9) is connected to an oil-water separator (10), which is connected to the micro-interface generator (6) via a reflux pipe.

8. The epoxy resin strengthening reaction system as described in claim 7, characterized in that: The feeding unit includes a raw material storage tank (1) and a NaOH storage tank (2). The raw material storage tank (1) and the NaOH storage tank (2) are respectively connected to the reactor (5) through a raw material feeding pipe (3). An alkaline feed pump (4) is provided on the raw material feeding pipe (3) connected to the NaOH storage tank (2).

9. The epoxy resin strengthening reaction system as described in claim 8, characterized in that: The reactor (5) is equipped with a temperature sensor.

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