Refining and purifying system for polyimide monomer

Abstract

The utility model discloses a refining and purifying system for a polyimide monomer. The refining and purifying system comprises an auxiliary metering tank, a decolorizing kettle, a plate filter, a micro-filter and a three-in-one filter, the three-in-one filter is provided with a three-in-one filter feed port, a three-in-one filter solid discharge port, a three-in-one filter mother liquor discharge port, a three-in-one filter cleaning port, a three-in-one filter nitrogen inlet, a three-in-one filter exhaust port, a three-in-one filter medium inlet, a three-in-one filter medium outlet, a stirring device and a filtering device. According to the refining and purifying system of the polyimide monomer, through the multifunctional decoloring kettle and the three-in-one filter, the refining and purifying effect is effectively improved, the exposure time of a product in air in the production process is shortened, oxidation and hydrolysis of the product are avoided, the quality of the product is improved, and the competitiveness of the product is enhanced; the product quality and the production efficiency are improved, and good popularization and application prospects are achieved.

Description

TECHNICAL FIELD

[0001] The utility model relates to a kind of refining purification systems of polyimide monomer. BACKGROUND

[0002] Polyimide is widely used in aerospace, microelectronics, nanometer, liquid crystal, separation membrane, laser and other fields as a kind of special engineering material.

[0003] With the preparation technology innovation of microelectronic, nanometer material and separation membrane material, industry puts forward higher and higher requirements to the quality of polyimide monomer, not only requires product to have higher purity, also puts forward higher requirements to chroma, metal ion content, halogen content, specific organic impurity content, ash, drying weight loss, moisture, particle size and solubility etc., plus the deteriorating characteristics of polyimide monomer, it is particularly urgent to study the refining purification technology of polyimide monomer.

[0004] There are hundreds of polyimide monomers, and there are two types of commonly used polyimide monomers, one is diamine, and the other is dianhydride. Diamine monomer is easy to oxidize and increase the content of impurities, and dianhydride is easy to hydrolyze to form the corresponding acid and lose reactivity, which puts higher requirements on the refining purification system and packaging and storage of polyimide monomer.

[0005] The existing polyimide monomer refining purification process is generally as follows: monomer, solvent, decolorizing agent and other additives are added to the decolorizing kettle for decolorization, and the decolorized material is filtered into the crystallization kettle, cooled and crystallized, filtered and dried to obtain polyimide monomer. The refining purification process product is exposed to air for a long time, which is easy to absorb moisture and hydrolyze or oxidize, and it is difficult to obtain high-quality products. UTILITY MODEL CONTENTS

[0006] The utility model aims at solving the above problems, and provides a kind of refining purification system of polyimide monomer.

[0007] The technical scheme for achieving the purpose of the polyimide monomer refining and purifying system is: a polyimide monomer refining and purifying system, comprising an additive metering tank, a decoloring kettle, a plate filter, a microfilter and a three-in-one filter; the additive metering tank is provided with a metering tank feed inlet, a metering tank discharge outlet, a metering tank nitrogen inlet and a metering tank exhaust port; the decoloring kettle is provided with a decoloring kettle liquid feed inlet, a decoloring kettle discharge outlet, a decoloring kettle nitrogen inlet, a decoloring kettle exhaust port, a decoloring kettle solid feed inlet and a decoloring kettle stirrer; the decoloring kettle liquid feed inlet is connected with the metering tank discharge outlet; the plate filter is provided with a plate filter feed inlet, a plate filter discharge outlet, a plate filter exhaust port and a filter plate; the plate filter feed inlet is connected with the decoloring kettle discharge outlet; the three-in-one filter is provided with a three-in-one filter feed inlet, a three-in-one filter solid discharge outlet, a three-in-one filter mother liquor discharge outlet, a three-in-one filter cleaning port, a three-in-one filter nitrogen inlet, a three-in-one filter exhaust port, a three-in-one filter medium inlet, a three-in-one filter medium outlet, a stirring device and a filtering device; the three-in-one filter feed inlet is connected with the plate filter discharge outlet through the microfilter.

[0008] Further, the stirring device comprises a stirrer and a stirrer hydraulic lifting system; the stirrer is composed of a stirring rod and stirring blades; the stirring blades are designed to be curved in the rotation direction.

[0009] The filtering device comprises a filtering device hydraulic lifting system, a filtering device support, a detachable filter plate, a filtering liquid cavity and a heating cavity.

[0010] The polyimide monomer refining and purifying system has the following advantages:

[0011] (1) The polyimide monomer refining and purifying system of the utility model through the multifunctional decoloring kettle and the three-in-one filter, effectively improves the refining and purifying effect, reduces the exposure time of the product in the air in the production process, avoids the oxidation and hydrolysis of the product, improves the quality of the product, enhances the competitiveness of the product, improves the product quality and production efficiency, and has good popularization and application prospect.

[0012] (2) The three-in-one filter of the utility model adopts the stirring blades of the paddle stirrer, and is designed to be curved in the rotation direction; through the switching of the rotation direction, the full mixing of the materials during drying and the smooth discharge of the materials during discharging can be realized.

[0013] (3) The three-in-one filter of the utility model is provided with an auxiliary heating system on the stirring blades and a heating cavity in the filtering device, which not only effectively improves the drying efficiency, but also is beneficial to the uniform heating of the product and avoids local overheating, thereby affecting the product quality.

[0014] (4) The filter device in the three-in-one filter adopts detachable filter plates, and is provided with a support at the same time, so that the entire filter device can be cleaned thoroughly, cross contamination of products is effectively avoided, product switching is facilitated, and the use efficiency of the equipment is improved. BRIEF DESCRIPTION OF DRAWINGS

[0015] Figure 1 It is a structure schematic view of the polyimide monomer refining and purifying system.

[0016] Figure 2 It is an external structure schematic view of the three-in-one filter.

[0017] Figures 3-1 to 3-3 It is a structure schematic view of the stirrer in the three-in-one filter; wherein Figure 3-1 it is a front view, Figure 3-2 it is Figure 3-1 a top view, Figure 3-3 it is Figure 3-1 a left view. DETAILED DESCRIPTION

[0018] (Example 1)

[0019] Referring to Figure 1 , the polyimide monomer refining and purifying system of the embodiment comprises an additive metering tank 100, a decoloring kettle 200, a plate filter 300, a microfilter 400 and a three-in-one filter 500.

[0020] The additive metering tank 100 is provided with a metering tank feed inlet 101, a metering tank discharge outlet 102, a metering tank nitrogen inlet 103 and a metering tank exhaust outlet 104.

[0021] The decoloring kettle 200 is provided with a decoloring kettle liquid feed inlet 201, a decoloring kettle discharge outlet 202, a decoloring kettle nitrogen inlet 203, a decoloring kettle exhaust outlet 204, a decoloring kettle solid feed inlet 205 and a decoloring kettle stirrer 206; the decoloring kettle liquid feed inlet 201 is connected with the metering tank discharge outlet 102. The decoloring kettle stirrer 206 of the embodiment is a conventional frame stirrer.

[0022] The plate filter 300 is provided with a plate filter feed inlet 301, a plate filter discharge outlet 302, a plate filter exhaust outlet 303 and a filter plate 304; the plate filter feed inlet 301 is connected with the decoloring kettle discharge outlet 202.

[0023] Referring to Figure 1~Figure 3, the three-in-one filter 500 is provided with a three-in-one filter feed port 501, a three-in-one filter solid discharge port 502, a three-in-one filter mother liquor discharge port 503, a three-in-one filter cleaning port 504, a three-in-one filter nitrogen inlet 505, a three-in-one filter exhaust port 506, a three-in-one filter medium inlet 507-1, a three-in-one filter medium outlet 507-2, a stirring device 508, and a filtering device 509; the three-in-one filter feed port 501 is connected with the plate filter discharge port 302 through the microfilter 400.

[0024] The stirring device 508 comprises a stirrer and a stirrer hydraulic lifting system 508-1; the stirrer is composed of a stirring rod 508-2 and stirring blades 508-3; the stirring blades 508-3 are paddle stirrers and are designed in a curved shape in the rotation direction, and through switching of the rotation direction, the full mixing of the materials during drying and the smooth discharge of the materials during discharge can be realized.

[0025] In order to further improve the drying effect, the stirrer of the embodiment is additionally provided with an auxiliary heating system

not shown in the figure

[0026] The filtering device 509 comprises a filtering device hydraulic lifting system 509-1, a filtering device support 509-2, a detachable filter plate 509-3, a filter liquid cavity 509-4, and a heating cavity 509-5.

[0027] The three-in-one filter 500 is also provided with a control system 511 and an online sampling device 512.

[0028] The process of the polyimide monomer refining and purification system of the embodiment is as follows:

[0029] ①The refining and purification system is fully replaced with nitrogen, then under the protection of nitrogen, the auxiliary agent is added to the auxiliary agent metering tank 100 through the metering tank feed port 101

the auxiliary agent is used for refining, for dianhydride, the auxiliary agent is acetic anhydride, etc.; for diamines, the auxiliary agent is a reducing auxiliary agent, so that decolorization and refining and purification can be carried out simultaneously, and the multifunctionalization of the decolorization kettle 200 can be realized

[0030] ②The decolored material is added to the plate filter 300 through the plate filter feed port 301 from the decolorization kettle discharge port 202, filtered through the plate filter 300 first, and then filtered through the microfilter 400 to the three-in-one filter 500.

[0031] ③In the three-in-one filter 500, the refrigerant is first introduced through the medium inlet and outlet 507-1, 507-2, cooled and crystallized, filtered, and the filtrate is discharged from the mother liquor outlet 503.

[0032] Then the height of the stirrer is lowered by the stirrer hydraulic lifting system 508-1 to fully contact the material, and the material is washed by adding cleaning liquid through the cleaning port 504, filtered again, and the filtrate is discharged from the mother liquor outlet 503.

[0033] Next, the heating medium is introduced through the medium inlet and outlet 507-1, 507-2, and at the same time, the stirrer is adjusted to the specified height by the stirrer hydraulic lifting system 508-1, and the auxiliary heating system on the stirring blade 508-3 and the heating cavity 509-5 in the filter device are started, the three-in-one filter is vacuumized, the material is vacuum dried, and the material moisture is sampled and detected by the online sampling device 512 until it is qualified.

[0034] Finally, under the protection of nitrogen, the solid outlet 502 is opened, the rotation direction of the stirring blade 508-3 is adjusted, and the material is discharged.

[0035] The temperature, pressure, stirring device, and lifting of the filter device in the three-in-one filter 500 are displayed and controlled by the control system 511, and the related operations are interlocked to reduce the misoperation and improve the automation level of the equipment, ensuring the efficient and orderly production.

Claims

1. A purification system for polyimide monomers, characterized in that... Includes an auxiliary agent metering tank (100), a decolorizing kettle (200), a plate filter (300), a microfilter (400), and a three-in-one filter (500); The additive metering tank (100) is provided with a metering tank inlet (101), a metering tank outlet (102), a metering tank nitrogen inlet (103), and a metering tank exhaust port (104). The decolorizing kettle (200) is provided with a liquid inlet (201), a discharge outlet (202), a nitrogen inlet (203), an exhaust outlet (204), a solid inlet (205), and a stirrer (206); the liquid inlet (201) is connected to the discharge outlet (102) of the metering tank. The plate filter (300) is provided with a plate filter inlet (301), a plate filter outlet (302), a plate filter exhaust port (303), and a filter plate (304); the plate filter inlet (301) is connected to the decolorization kettle outlet (202); The three-in-one filter (500) is provided with a three-in-one filter inlet (501), a three-in-one filter solid outlet (502), a three-in-one filter mother liquor outlet (503), a three-in-one filter cleaning port (504), a three-in-one filter nitrogen inlet (505), a three-in-one filter exhaust port (506), a three-in-one filter media inlet (507-1), a three-in-one filter media outlet (507-2), a stirring device (508), and a filtering device (509); the three-in-one filter inlet (501) and the plate filter outlet (302) are connected through a microfilter (400).

2. The purification system for polyimide monomers according to claim 1, characterized in that: The stirring device (508) includes a stirrer and a stirrer hydraulic lifting system (508-1); the stirrer consists of a stirring rod (508-2) and a stirring blade (508-3); the stirring blade (508-3) is curved in the direction of rotation.

3. The purification system for polyimide monomers according to claim 1, characterized in that: The filter device (509) includes a hydraulic lifting system (509-1), a support (509-2), a detachable filter plate (509-3), a filtrate chamber (509-4), and a heating chamber (509-5).

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