TGIC total chlorine distillation process control device

Abstract

The utility model relates to the technical field of TGIC (triglycidyl isocyanurate) production, in particular to a device for controlling total chlorine of TGIC in a distillation process. Comprising a primary distillation kettle, the gas phase end of the primary distillation kettle is communicated with a first vacuum receiving tank through a first secondary condenser, the liquid phase end of the primary distillation kettle is communicated with the liquid inlet end of a fine distillation kettle through a filter, and the gas phase end of the fine distillation kettle is communicated with a second vacuum receiving tank through a second secondary condenser; and the liquid phase end of the fine steaming kettle is communicated with the first crystallizing tank and the second crystallizing tank. The purity of the TGIC product can be directly improved after the TGIC product passes through the primary steaming kettle and the fine steaming kettle. The TGIC product is filtered by the filter when entering the fine steaming kettle, so that impurities in the TGIC product can be filtered out, and the purity of the TGIC product discharged from the liquid phase of the fine steaming kettle can be further improved.

Description

Technical Field

[0001] The utility model relates to the technical field of TGIC production, in particular to a control device for total chlorine in TGIC during the distillation process. Background Art

[0002] TGIC (triglycidyl isocyanurate, or: tris (2,3-epoxypropyl) isocyanurate) is a curing agent used in powder coatings. It is widely used because of its good thermal stability, weather resistance, excellent yellowing resistance and outstanding mechanical properties. With the upgrading of the industrial industry, the purity requirement for TGIC in its processing is getting higher and higher. The main process steps of TGIC processing include esterification, cyclization, pressure filtration, water washing, distillation, crystallization, centrifugation, drying and granulation. Changes in the parameters and conditions of each link will affect the purity of the TGIC finished product. In the existing process, the purity of the TGIC product is basically 92-95%, and the yield is (75-78%); for some industries with high purity requirements, the TGIC products obtained by the current process method can no longer meet their requirements. Therefore, it is necessary to adjust and improve the existing process to improve the purity of the TGIC product. TGIC for electronic packaging has higher requirements than general TGIC products, requiring higher purity and smaller particle size. Therefore, during the production process, better system stability is required. Deviations in the proportion of materials and processing environment in the production system may cause a decrease in the purity of the product.

[0003] In the existing TGIC production process, after the esterification, cyclization, pressure filtration and water washing processes are completed, a large amount of a mixture of ECH and water is recovered during the distillation reaction process. The mixture of ECH and water collected by distillation is subjected to static separation, and the crude TGIC obtained by distillation is directly sent to a crystallization kettle for crystallization, resulting in a relatively low purity of the TGIC product.

[0004] The patent document with the publication number CN216824868U discloses a TGIC processing system for electronic packaging, including a synthesis kettle, a cyclization kettle, a filtration device, a separator, a distillation kettle, etc. arranged in sequence. An ECH recovery pipe is provided on the distillation kettle for receiving impurity gases such as ECH and water vapor. The ECH recovery pipe is connected with a static separation tank, and a condenser is provided on the ECH recovery pipe. Through the condenser, the ECH vapor and water vapor and other gases are condensed and enter the static separation tank for static separation. After separation, the upper layer is an aqueous solution and the lower layer is an ECH solution. An outlet is provided at the bottom of the static separation tank, and a water outlet is provided on the side wall. To facilitate viewing the water level of the separation, a liquid level window is also provided on the static separation tank. The upper aqueous solution after static separation is discharged through the water outlet, and the ECH solution is discharged through the outlet at the bottom.

[0005] The liquid outlet pipeline is connected with a pretreatment kettle for vacuum distillation and impurity removal of the incoming material. A transfer pump is arranged on the pipeline between the static settling tank and the pretreatment kettle, and the ECH solution in the static settling tank is pumped into the pretreatment kettle through the transfer pump. An outlet is arranged at the bottom of the pretreatment kettle, and valves are arranged at both the liquid inlet and the outlet of the pretreatment kettle. An exhaust pipe is arranged at the top of the pretreatment kettle, a condenser is arranged on the exhaust pipe, a storage tank is connected to the end of the exhaust pipe, and a vacuum extraction pipe is connected to the storage tank. A heating coil is arranged in the pretreatment kettle. After the ECH solution is pumped into the pretreatment kettle, the valves at the liquid inlet and the outlet are closed, and the vacuum extraction pipe is used for vacuum extraction to keep the pressure in the pretreatment kettle above -0.098 Mpa. At the same time, the heating coil works to heat the pretreatment kettle to keep the temperature in the pretreatment kettle between 35 and 55 °C. Through vacuum distillation, the residual water and impurities such as 1,2-dichloropropanol and 1,3-dichloropropanol in the ECH are discharged in the form of steam through the exhaust pipe, and are condensed into liquid under the action of the condenser on the exhaust pipe, enter the storage tank for storage and are discharged regularly.

[0006] The outlet is connected to a synthesis kettle to transport the ECH obtained after vacuum distillation to the synthesis kettle for synthesis reaction. This structure can improve the purity of the ECH entering the synthesis kettle, reduce the influence of water and impurities in the ECH on the synthesis reaction, and improve the stability and quality of the synthesis reaction.

[0007] This system improves the purity of the TGIC product by improving the purity of the ECH, rather than directly improving the purity of the TGIC product. Summary of the Invention

[0008] The technical problem to be solved by the present invention is a control device for the total chlorine of TGIC in the distillation process that can directly improve the purity of the TGIC product.

[0009] To achieve the above object, the technical solution provided by the present invention is:

[0010] A control device for the total chlorine of TGIC in the distillation process includes a primary distillation kettle. The gas phase end of the primary distillation kettle is communicated with a first vacuum receiving tank through a first two-stage condenser. The liquid phase end of the primary distillation kettle is communicated with the liquid inlet end of a fine distillation kettle through a filter. The gas phase end of the fine distillation kettle is communicated with a second vacuum receiving tank through a second two-stage condenser. The liquid phase end of the fine distillation kettle is communicated with a first crystallization tank and a second crystallization tank.

[0011] Specifically, the filter is a bag filter.

[0012] Specifically, a methanol pipeline is communicated with the first crystallization tank and the second crystallization tank.

[0013] Specifically, the methanol pipeline is communicated with the fine distillation kettle.

[0014] Compared with the prior art, the beneficial effects of the present utility model are as follows:

[0015] 1. After passing through the primary distillation kettle and the fine distillation kettle, the purity of the TGIC product can be directly improved.

[0016] 2. When the TGIC product enters the fine distillation kettle, it is filtered by a filter, and the impurities therein can be filtered out, which can further improve the purity of the TGIC product discharged from the liquid phase of the fine distillation kettle.

[0017] 3. During the crystallization or fine distillation process, methanol is added to the TGIC product through a methanol pipeline. After the methanol vaporizes, it carries the impurities in the TGIC product and is discharged, which can improve the purity of the TGIC product. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a schematic diagram of the first embodiment of this control device.

[0019] Figure 2 It is a schematic diagram of the second embodiment of this control device.

[0020] The names of the components in the drawings are: 1. Primary distillation kettle, 2. First and second-stage condenser, 3. First vacuum receiving tank, 4. Filter, 5. Fine distillation kettle, 6. Second and second-stage condenser, 7. Second vacuum receiving tank, 8. First crystallization tank, 9. Second crystallization tank, 10. Methanol pipeline. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0021] Next, the technical solutions in the embodiments of the present utility model will be clearly and completely described in conjunction with the drawings in the embodiments of the present utility model. Obviously, the described embodiments are only a part of the embodiments of the present utility model, rather than all the embodiments.

[0022] Embodiment 1: Refer to Figure 1 As shown, a control device for total chlorine in TGIC during distillation includes a primary distillation kettle 1. The gas phase end of the primary distillation kettle 1 is connected to a first vacuum receiving tank 3 through a first and second-stage condenser 2.

[0023] The liquid phase end of the primary distillation kettle 1 is connected to the liquid inlet end of a fine distillation kettle 5 through a filter 4. The filter 4 is a bag filter.

[0024] The gas phase end of the fine distillation kettle 5 is connected to a second vacuum receiving tank 7 through a second and second-stage condenser 6. The liquid phase end of the fine distillation kettle 5 is connected to a first crystallization tank 8 and a second crystallization tank 9.

[0025] The methanol pipeline 10 is connected to the first crystallization tank 8 and the second crystallization tank 9.

[0026] During the production process of TGIC, the crude TGIC product obtained after the esterification, cyclization, pressure filtration, and water washing processes enters the primary evaporation kettle 1 through the liquid inlet end of the primary evaporation kettle 1. The crude TGIC product entering the primary evaporation kettle 1 undergoes primary evaporation in the primary evaporation kettle 1. The water and epichlorohydrin discharged from the gas phase end of the primary evaporation kettle 1 are condensed by the first and second condensers 2 and then enter the first vacuum receiving tank 3. The water and epichlorohydrin in the first vacuum receiving tank 3 are stratified.

[0027] The TGIC product discharged from the liquid phase end of the primary evaporation kettle 1 is filtered by the filter 4 and then impurities can be further removed.

[0028] The TGIC product passing through the filter 4 enters the fine evaporation kettle 5. The TGIC product entering the fine evaporation kettle 5 undergoes fine evaporation in the fine evaporation kettle 5. The water and epichlorohydrin discharged from the gas phase end of the fine evaporation kettle 5 are condensed by the second and second condensers 6 and then enter the second vacuum receiving tank 7. The water and epichlorohydrin in the second vacuum receiving tank 7 are stratified. The purity of the TGIC product can be improved after fine evaporation.

[0029] The TGIC product discharged from the liquid phase end of the fine evaporation kettle 5 enters the first crystallization tank 8 and the second crystallization tank 9 for crystallization.

[0030] When the TGIC product crystallizes, methanol is added to the first crystallization tank 8 and the second crystallization tank 9 through the methanol pipeline 10. When the methanol vaporizes during the crystallization of the TGIC product, it carries the impurities in the TGIC product and discharges from the first crystallization tank 8 and the second crystallization tank 9, which can further improve the purity of the TGIC product.

[0031] In this embodiment, the gas phase ends of the first crystallization tank 8 and the second crystallization tank 9 need to be connected to the methanol recovery equipment for recovering methanol.

[0032] Embodiment 2: This embodiment is the same as other features of Embodiment 1, except that, as shown in reference to Figure 2 The methanol pipeline 10 is communicated with the fine evaporation kettle 5.

[0033] In this embodiment, when the TGIC product is finely evaporated in the fine evaporation kettle 5, methanol is added to the fine evaporation kettle 5. After the methanol vaporizes, it can be condensed by the second and second condensers 6. The methanol can enter the second vacuum receiving tank 7 and mix with the water in the second vacuum receiving tank 7, thereby realizing the recovery of methanol.

[0034] The above are only the preferred embodiments of the present utility model and are not intended to limit the present utility model. Any modifications, equivalent replacements, and improvements made within the spirit and principle of the present utility model shall be included within the protection scope of the present utility model.

Claims

1. A total chlorine control device for TGIC during the distillation process, comprising a primary distillation kettle (1), the gas phase end of the primary distillation kettle (1) is communicated with a first vacuum receiving tank (3) through a first secondary condenser (2), and is characterized in that, The liquid phase end of the primary evaporation still (1) is connected to the liquid inlet end of the fine evaporation still (5) through a filter (4). The gas phase end of the fine evaporation still (5) is connected to the second vacuum receiving tank (7) through a second secondary condenser (6). The liquid phase end of the fine evaporation still (5) is connected to the first crystallization tank (8) and the second crystallization tank (9).

2. The total chlorine in TGIC distillation process control device according to claim 1, characterized in that, The filter (4) is a bag filter (4).

3. The total chlorine in TGIC distillation process control device according to claim 1, characterized in that, The methanol pipeline (10) is connected to the first crystallization tank (8) and the second crystallization tank (9).

4. The TGIC total chlorine distillation process control device according to claim 1, characterized in that, The methanol pipeline (10) is connected to the fine evaporation still (5).

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