CN114225869A - Production device of transparent polyimide slurry - Google Patents

Production device of transparent polyimide slurry Download PDF

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Publication number
CN114225869A
CN114225869A CN202111542542.8A CN202111542542A CN114225869A CN 114225869 A CN114225869 A CN 114225869A CN 202111542542 A CN202111542542 A CN 202111542542A CN 114225869 A CN114225869 A CN 114225869A
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Prior art keywords
unit
premixing
transparent polyimide
temperature
nitrogen
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Inventor
詹世治
曾西平
靳世东
彭礼明
王海波
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Shenzhen Huake Tek Co Ltd
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Shenzhen Huake Tek Co Ltd
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Priority to CN202111542542.8A priority Critical patent/CN114225869A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D46/00—Filters or filtering processes specially modified for separating dispersed particles from gases or vapours
    • B01D46/0002—Casings; Housings; Frame constructions
    • B01D46/0012—In-line filters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006—Controlling or regulating processes
    • B01J19/0013—Controlling the temperature of the process
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/0066—Stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00—Feed or outlet devices; Feed or outlet control devices
    • B01J4/008—Feed or outlet control devices
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
    • C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
    • C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08G73/1003—Preparatory processes

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)

Abstract

The invention relates to a production device of transparent polyimide slurry. The system comprises a material storage unit, a premixing unit, a main reaction unit, a nitrogen filtering unit, an activation processing unit, a temperature control system and a main control unit; the storage unit consists of a plurality of constant temperature containers which are arranged in parallel, and each constant temperature container is provided with a feeding hole and a discharging hole; the input end of the premixing unit is connected with the discharge port of the constant-temperature container through a metering pump, and the output end of the premixing unit is connected with the main reaction unit; the input end of the activation processing unit is connected with the discharge hole of the constant-temperature container, and the output end of the activation processing unit is connected with the main reaction unit; part of the discharge hole of the constant temperature container and the temperature control system are connected with the main reaction unit; the input end of the nitrogen filtering unit is connected with the nitrogen storage unit, and the output end of the nitrogen filtering unit is connected with the main reaction unit. Compared with the prior art, the device promotes transparent polyimide thick liquids production order of magnitude, ensures the stability and the continuity of product in the production process.

Description

Production device of transparent polyimide slurry
Technical Field
The invention relates to the technical field of production equipment, in particular to a production device of transparent polyimide slurry.
Background
In recent years, along with the trend of light weight, miniaturization, ultra-thinning and flexibility of photoelectric devices, the CPI film (transparent polyimide film) has been widely applied to the manufacture of photoelectric devices such as touch screens, flexible printed circuit boards, flexible solar cells and flexible displays because of the good colorless transparency, heat resistance and insulation, and has great market potential.
In the traditional production, the process from the synthesis of the transparent polyimide to the finished slurry is manually operated, and the synthesis amount is small; and the quality stability of the slurry have great fluctuation, so that the comprehensive performance of the material after film formation is influenced.
In summary, it is needed to provide a novel apparatus for producing transparent polyimide paste, so as to improve the production level of the transparent polyimide paste.
Disclosure of Invention
Aiming at the defects, the invention provides the production device of the transparent polyimide slurry, which not only quantifies indexes in the production process of the transparent polyimide slurry and improves the production level of the transparent polyimide slurry, but also ensures the stability and continuity of products in the production process and improves the production efficiency.
The invention adopts the following technical scheme: a production device of transparent polyimide slurry comprises a material storage unit, a premixing unit, a main reaction unit, a nitrogen filtering unit, an activation processing unit, a temperature control system and a main control unit;
the storage unit consists of a plurality of constant temperature containers which are arranged in parallel, and each constant temperature container is provided with a feeding hole and a discharging hole;
the input end of the premixing unit is connected with the discharge hole of the constant-temperature container through a metering pump, and the output end of the premixing unit is connected with the main reaction unit;
the input end of the activation processing unit is connected with the discharge hole of the constant-temperature container, and the output end of the activation processing unit is connected with the main reaction unit;
part of the discharge hole of the constant temperature container and the temperature control system are connected with the main reaction unit;
the input end of the nitrogen filtering unit is connected with the nitrogen storage unit, and the output end of the nitrogen filtering unit is connected with the main reaction unit;
the storage unit, the premixing unit, the main reaction unit, the nitrogen filtering unit, the activation processing unit and the temperature control unit are respectively electrically connected with the main control unit.
Furthermore, the premixing unit comprises a premixing reaction tank, and a gravity sensor, a premixing stirring mechanism, a nitrogen protection mechanism and a pressure relief mechanism which are arranged in the premixing reaction tank.
Furthermore, the gravity sensor is electrically connected with the main control unit and is used for measuring weight data of the material and transmitting the weight data to the main control unit.
Further, the main reaction unit comprises a reaction kettle body, and a dispersing mechanism, a vibration viscometer and a temperature sensor which are arranged in the reactor kettle; the vibration viscometer and the temperature sensor are respectively arranged on the inner wall of the reactor body, and an air pressure protection mechanism and a small molecule reactant collection mechanism are externally connected to the reactor body.
Further, dispersion mechanism including fixed mounting drive motor on the reation kettle body and with the enamel agitator that the drive motor transmission is connected, the enamel agitator comprises double-deck stirring rake, and is double-deck the stirring rake is arranged from top to bottom, and all is (35 ~ 45) inclination setting with vertical direction.
Further, the reactor comprises an reactor body and an autoclave cover arranged above the reactor body; the reaction kettle body is of a hollow structure with an opening at the top and is provided with an inner wall and an outer wall, the inner wall is made of enamel materials, the outer wall is made of stainless steel materials, and the outer wall is connected with the temperature control system.
Further, the nitrogen filtering unit consists of two multi-stage filtering towers.
Further, the temperature control system is a LAUDA constant temperature system.
Furthermore, the discharge hole of the constant temperature container is connected with the input end of the activation processing unit through a metering pump.
Compared with the prior art, the invention has the beneficial effects that:
the production device of the transparent polyimide slurry comprises a material storage unit and a constant temperature container; a pre-mixing unit; the coordination operation of the main reaction unit, the nitrogen filtering unit, the activation processing unit, the temperature control system and the main control unit provides a full-automatic production line for the production of the transparent polyimide slurry, so that the indexes in the production process of the transparent polyimide slurry are quantized, the production magnitude of the transparent polyimide slurry is improved, meanwhile, the stability and the continuity of the product in the production process are ensured, and the production efficiency is improved; in addition, the device is provided with a main control unit, and the unit can monitor the physical and chemical parameters of the product in real time, so that the stability of the product is further ensured.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic view showing the overall configuration of an embodiment of a production apparatus for a transparent polyimide paste according to the present invention;
FIG. 2 is a schematic structural view of the main reaction unit in FIG. 1;
FIG. 3 is a TGA curve analysis of thermal performance analysis of a CPI film;
FIG. 4 is a TMA curve analysis of a thermal performance analysis of a CPI film;
FIG. 5 is a DSC curve analysis of thermal performance analysis of a CPI film;
wherein: the device comprises a material storage unit 1 and a constant temperature container 10; a premixing unit 2 and a premixing reaction tank 20; a main reaction unit 3, a reactor 30, a dispersing mechanism 31, an enamel stirrer 311, a vibration viscometer 32, a temperature sensor 33, an air pressure protection mechanism 34 and a small molecule reactant collecting mechanism 35; a nitrogen filtering unit 4; an activation processing unit 5; a temperature control system 6; a metering pump 7.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention is discussed in detail below with reference to figures 1 to 5 and specific embodiments:
as shown in fig. 1-2, a device for producing transparent polyimide slurry includes a storage unit 1, a premixing unit 2, a main reaction unit 3, a nitrogen filtering unit 4, an activation processing unit 5, a temperature control system 6, and a main control unit.
The material storage unit 1 is used for storing materials and comprises a plurality of constant temperature containers 10 which are arranged in parallel, the constant temperature containers 10 are mutually independent, and each constant temperature container 10 is provided with an independent feeding hole and an independent discharging hole; the feed inlet is used for the input of material, and the discharge gate is used for the output of material. Correspondingly, in this embodiment, the material stored in the storage unit 1 includes a solvent: such as NMP (N-methylpyrrolidone), DMAC (dimethylacetamide), GBL (γ -butyrolactone), etc., monomers: such as 6FDA (hexafluorodianhydride), ODA (diaminodiphenyl ether), CPODA (octahedral-3H, 3H '-spiro [ [4,7] methoxyisobenzofuran-5, 1' -cyclopentane-3 ', 5 "- [4,7] methoxyisobenzofuran ] -1, 1", 2', 3,3 "(4H, 4" H) -pentanone), TFMB (4,4 '-diamino-2, 2' -bistrifluoromethylbiphenyl), and other dianhydrides or diamines, and the like, catalysts: such as pyridine, isoquinoline, and the like; each solvent, monomer, or catalyst is stored separately in a separate thermostatic vessel 10 for use. The thermostatic vessel 10 of the present invention is a vessel capable of maintaining a constant temperature in the vessel, and the specific structural design thereof is not limited, and the vessel may be a product sold on the market or designed by a person skilled in the art.
The premixing unit 2 is used for premixing partial key materials, the input end of the premixing unit 2 is connected with the discharge hole of the constant temperature container 10 through a metering pump 7, and the output end of the premixing unit 2 is connected with the main reaction unit 3. Specifically, according to actual requirements, the discharge port of a part of the thermostatic container 10 is connected with the main reaction unit 3 through the metering pump 7 and the premixing unit 2, and materials to be premixed are premixed by the premixing unit 2 and then input into the main reaction unit 3.
The activation processing unit 5 is used for activating a material to be activated, the input end of the activation processing unit 5 is connected with the discharge hole of the constant-temperature container 10, and the output end of the activation processing unit 5 is connected with the main reaction unit 3, so that the activation processing operation of the material to be activated is realized. Specifically, a metering pump 7 may be provided between the discharge port of the thermostatic vessel 10 and the activation processing unit 5, and the input amount of the material is metered by the metering pump 7.
Part of discharge ports of the constant temperature container 10 can be directly connected with the main reaction unit 3, and materials which do not need premixing and activation treatment are directly input into the main reaction unit 3 for reaction; the main reaction unit 3 is a production site of transparent polyimide. Meanwhile, the temperature control system 6 is also connected with the main reaction unit 3 to realize the temperature control of the main reaction unit 3. Specifically, the specific structure of the temperature control system 6 is not limited in the present invention, and a temperature control system product sold in the existing market can be adopted, for example, the temperature control system 6 is a german LAUDA constant temperature system in this embodiment. The temperature control system 6 is simple to operate, rapid in temperature change and wide in temperature range, and meets the temperature control requirement of the temperature change range from-150 ℃ to 550 ℃.
The nitrogen filtering unit 4 is mainly used for filtering nitrogen input into the main reaction unit 3 and removing impurities in the nitrogen, such as filtering water molecules in the nitrogen; the input end of the nitrogen filtering unit 4 is connected with the nitrogen storage unit, and the output end of the nitrogen filtering unit 4 is connected with the main reaction unit 3, so that the nitrogen is filtered. The specific structure of the nitrogen filtering unit 4 is not limited in the invention, as long as the nitrogen filtering operation can be realized, and the finished product of the filtering device sold in the existing market can be adopted, for example, in the embodiment, the nitrogen filtering unit 4 consists of two multi-stage filtering towers, and is multi-stage filtering and good in filtering effect.
Meanwhile, in the production device of the transparent polyimide slurry, the storage unit 1, the premixing unit 2, the main reaction unit 3, the nitrogen filtering unit 4, the activation processing unit 5 and the temperature control unit 6 are respectively and electrically connected with the main control unit, and the control of other units is realized through the active unit 7. In this embodiment, the main control unit is a computer main control unit, and program control of other units is realized. Through the control of main control unit, not only can improve the precision of control, the index in the transparent polyimide thick liquids production process still can quantify promotes transparent polyimide thick liquids production order of magnitude, guarantees the stability and the continuity of product in the production process.
The production device of the transparent polyimide slurry comprises a material storage unit 1 and a constant temperature container 10; a pre-mixing unit 2; the coordination operation of the main reaction unit 3, the nitrogen filtering unit 4, the activation processing unit 5, the temperature control system 6 and the main control unit provides a full-automatic production line for the production of the transparent polyimide slurry, so that the indexes in the production process of the transparent polyimide slurry are quantized, the production magnitude of the transparent polyimide slurry is improved, meanwhile, the stability and the continuity of products in the production process are ensured, and the production efficiency is improved; in addition, the device is provided with a main control unit, and the unit can monitor the physical and chemical parameters of the product in real time, so that the stability of the product is further ensured.
Further, in some specific embodiments, the premixing unit 2 is optimally designed, and the specific design scheme is as follows: the premixing unit 2 comprises a premixing reaction tank 20, and a gravity sensor, a premixing stirring mechanism, a nitrogen protection mechanism and a pressure relief mechanism which are arranged in the premixing reaction tank 20.
The gravity sensor is electrically connected or in communication connection with the main control unit, and is used for measuring weight data of materials, transmitting the weight data to the main control unit and storing the weight data; the weight sensor can realize secondary verification of the weight of the materials input into the premixing unit 2, improves the accuracy of the input quantity of the materials and realizes accurate verification of the proportioning of the premixed materials. Correspondingly, a metering pump 7 between the thermostatic container 10 and the premixing unit 2 is electrically or communicatively connected with the main control unit, and the metering pump 7 is used for measuring flow data or volume data of materials and transmitting the flow data or volume data to the main control unit.
The main control unit compares the flow data or the volume data measured by the metering pump 7 with the weight data measured by the gravity sensor for analysis, and if the deviation between the flow data and the volume data meets the preset deviation requirement, the materials input into the premixing unit 2 are premixed; and if the deviation between the two is not satisfied with the preset deviation requirement, calculating the weight of the premixed material based on the weight data measured by the gravity sensor. The predetermined deviation requirement is set by one skilled in the art based on experience.
This mix in advance rabbling mechanism, nitrogen protection mechanism and pressure release mechanism can adopt the finished product of selling on the existing market to with the installation that above-mentioned mechanism corresponds on mixing retort 20 in advance, realize function such as stirring in advance and protection pressure release to mixing in advance the material.
Further, in some embodiments, the main reaction unit 3 is designed in detail, and the specific design scheme is as follows: the main reaction unit 3 comprises a reactor body 30, and a dispersing mechanism 31, a vibration viscometer 32 and a temperature sensor 33 which are arranged in the reactor body 30; the vibratile viscometer 32 and the temperature sensor 33 are respectively arranged on the inner wall of the reactor body 30, and an air pressure protection mechanism 34 and a small molecule reactant collecting mechanism 35 are externally connected to the reactor body 30.
The reactor 30 comprises a reactor body and a reactor cover arranged above the reactor body, and the reactor body 30 is designed in a split manner, so that later maintenance, repair and the like are facilitated. The reaction kettle body is of a hollow structure with an opening at the top, and is provided with an inner wall and an outer wall, wherein the inner wall is made of enamel materials, the outer wall is made of stainless steel materials, and the outer wall is connected with the temperature control system 6, so that the temperature control operation of the reaction kettle body 30 is realized. The inner wall of the reactor 30 is made of enamel material, so that the reactor is strong in corrosion resistance, has good non-adhesiveness, is not easy to bond materials, and is beneficial to the mixing reaction of the materials in the reactor 30. Meanwhile, the outer wall of the reactor 30 is made of stainless steel material, and has the characteristics of rapid heating, good high temperature resistance, strong corrosion resistance and the like. In addition, a plurality of feed inlets are arranged at the top of the reactor 30, and comprise a solid feed inlet, a liquid feed inlet, a gas feed inlet and the like, and are correspondingly connected with the discharge outlet of the thermostatic vessel 10, the premixing reaction tank 20, the activation treatment unit 5, the nitrogen filtering unit 4 and the like, so that the materials are conveyed into the reactor 30; the bottom of the reaction kettle 30 is provided with a discharge port for discharging the reacted materials, so that the reacted materials can be discharged uniformly.
This dispersion mechanism 31 is used for realizing the stirring of material in reactor 30 and mixes, and it includes fixed mounting drive motor on reactor 30 and with enamel agitator 311 that drive motor transmission is connected, through drive motor, drives this enamel agitator 311 and rotates, realizes the function of mixing the stirring to the material. This enamel stirrer 311 comprises double-deck stirring rake, and is double-deck the stirring rake is arranged from top to bottom, and all is (35 ~ 45) inclination setting with vertical direction to set up round annular square structure in the outside of double-deck stirring rake, make this dispersion mechanism 31 existing even stirring of being favorable to, be favorable to the mass transfer again. Through repeated tests, the stirring paddle with the inclined angle can perform effective mass transfer effect on high-viscosity materials, and the mass transfer effect is optimal when the inclined angle is (35-45 degrees). In the invention, the concrete structure of the stirring paddle is not limited, the stirring paddle structure in the prior art can be adopted, and the stirring paddle can be designed by a person skilled in the art according to the actual situation.
The vibratile viscometer 32 is used for monitoring the viscosity of reaction materials in real time, is arranged on the inner wall of the reaction kettle body 30 and is electrically or communicatively connected with the main control unit, the viscosity of the reaction materials is fed back to the main control unit in real time, and the main control unit comprehensively analyzes and coordinately controls the action of the whole production device to realize optimized production. In the present invention, since the reaction mixture is contained in the closed reactor 30, a vibration viscometer 32 is required to monitor the viscosity change of the reaction mixture in real time.
The temperature sensor 33 is used for monitoring the temperature in the reactor 30 in real time, is arranged on the inner wall of the reactor 30, is electrically or communicatively connected with the main control unit, and feeds back the temperature in the reactor 30 to the main control unit in real time, so as to avoid the influence of over-high or over-low temperature in the reactor 30 on the reaction of the reaction materials.
The air pressure protection mechanism 34 is used for protecting the air pressure balance in the reaction kettle body 30 and avoiding the danger caused by the overlarge air pressure in the reaction kettle body 30. The specific structure of the pneumatic protection mechanism 34 is not limited in the present invention, and the pneumatic protection mechanism of the prior art may be adopted.
The small molecule reactant collecting mechanism 35 is used for collecting small molecule products generated in the reaction process, and the reaction end point is judged by combining the dynamic viscosity of materials.
The production device of the transparent polyimide paste of the invention has the following general working processes:
the first stage is as follows: the nitrogen gas filtered by nitrogen gas filtering unit 4 was introduced into the reactor 30 of main reaction unit 3, and then introduced with nitrogen gas for 1 hour. The main control unit instructs one or more aprotic polar solvents, monomers and the like with high boiling points stored in a constant temperature container 10 in the storage unit 1 to be conveyed into a premixing reaction tank 20 of the premixing unit 2 through a metering pump 7, and part of raw materials are premixed in the premixing unit 2 in proportion.
After the premixing, the obtained product is injected into the reactor 30 of the main reaction unit 3; the main control unit instructs the enamel stirrer 311 in the main reaction unit 3 to stir, and instructs the temperature control system 6 to heat to 100 ℃ and keep the constant temperature for 0.5 h; then cooling to 80 ℃, and keeping the constant temperature for 0.5 h; finally, the temperature is raised to 100 ℃ again, and the constant temperature is kept for 0.5 h.
And a second stage: the main control unit instructs solid materials which do not need activation treatment or premixing treatment in the material storage unit 1 to be injected into the main reaction unit 3, and the solid materials are stirred for 1 hour at constant temperature; the main control unit instructs the temperature control system 6 to heat to 210 ℃ and keep constant temperature (1.5-2 h); then cooling to 200 ℃, and keeping the temperature constant (1.5 h-2 h); then heating to 210 ℃, keeping the temperature constant (1.5-2 h), and continuing the whole heating, cooling and heating process for 5-6 h. Then, the auxiliary agents (such as catalyst and the like) in the main control unit instruction storage unit 1 are conveyed to the activation processing unit 5 through the metering pump 7, and are conveyed to the main reaction unit 3 after being activated, and are stirred and reacted at constant temperature.
And a third stage: the main control unit monitors the viscosity of the material and the generation amount of the small molecular reactant in real time, and the reaction is terminated when the viscosity of the material and the generation amount of the small molecular reactant reach the standard. In the present invention, the standards of the viscosity of the material and the amount of the small molecule reactant are not particularly limited, and may be selected by those skilled in the art according to the actual reaction material and the reaction synthesis product.
A fourth stage: the main control unit instructs the temperature control system 6 to cool, the cooling rate is 50 ℃/h to the normal temperature (the normal temperature is about 25 ℃ generally), and then the materials can be discharged.
Two comparative examples are given in the invention, one is to adopt the above-mentioned transparent polyimide thick liquids' production facility through the above-mentioned reaction method, produce transparent polyimide thick liquids after forming the volume production; and the other method is to produce the transparent polyimide slurry through a small experiment and by adopting the reaction method, so that the transparent polyimide slurry before mass production is formed.
The transparent polyimide slurry for production before and after mass production is coated on a glass plate by a 150-micron wire bar, and is dried in an oven at 80 ℃ for 30min, 120 ℃ for 30min, 150 ℃ for 30min, 180 ℃ for 30min and 210 ℃ for 60 min. And (3) after the glass plate is cooled, putting the glass plate into a hot water tank, peeling the CPI film, putting the glass plate on dust-free paper, and putting the glass plate into a 120 ℃ oven to be dried for 30 min. And comparing the CPI film material prepared from the slurry before and after mass production, wherein the comparison result is as follows:
1) the optical parameters of the CPI film were measured using a BYK haze transmission apparatus and an Achromatograph i7800, as shown in Table 1:
TABLE 1 optical parameters of CPI film measured by haze transmission and color difference instrument
Parameter(s) T H L* a* b*
Before delivery 90.8 0.59 95.45 -0.60 1.34
After the measurement 92.6 0.30 95.42 -0.85 1.02
Rate of increase +2％ +49％ -- -- 24％
Wherein T is Transmittance light Transmittance, H is Haze value, and both are values measured by BYK Haze transmission instrument; l is*、a*、b*A color gamut parameter value measured for an Alice colorimeter, L*Is lightness, a*Is a red/green value, b*Is the blue/yellow value.
From table 1, it can be seen that the light transmittance of the CPI film material is increased and the haze value is decreased after mass production, which indicates that the quality of the CPI film material is improved after mass production; at the same time, b*The larger the value is, the more yellow the chroma of the CPI film is, and the color gamut parameter value b of the CPI film is after mass production*The numerical value is obviously reduced, and the quality improvement of the CPI film material after the production is further explained.
2) The molecular weight distribution of the material was determined by Gel Permeation Chromatography (GPC) on a Waterse2695 instrument (Waters, MA, USA) by dissolving the CPI film pre-and post-dose in THF at a concentration of 5mg/mL, eluting with THF at a flow rate of 1mL/min at 40 deg.C, and comparing the results shown in Table 2 below:
TABLE 2 molecular weight distribution of materials by Gel Permeation Chromatography (GPC)
Name of distribution Mn Mw MP Polydispersity
Before delivery 46685 188115 136321 4.029431
After the measurement 128541 253215 216278 1.969918
Rate of increase +175％ +35％ +59％ +104％
Wherein Mn is a number average molecular weight, Mw is a weight average molecular weight, and Mp is an integral molecular weight.
From table 2, it can be seen that the number average molecular weight, the weight average molecular weight, and the integral molecular weight of the CPI film material after mass production are relatively increased, which proves that the stability of the material after mass production is improved; the polydispersity is an index for measuring the width of molecular weight distribution, and the smaller the value, the more concentrated the synthesized product, and the better the performance.
3) Respectively testing the CPI film before and after mass production on TGA, TMA and DSC instruments produced by TA instruments of America, and analyzing the thermal property of the CPI film, wherein the specific analysis results are shown in figures 3, 4 and 5; wherein curve 1 is a CPI film material before mass production; curve 2 is the CPI film after mass production.
The thermal properties of the CPI film were evaluated by TGA, TMA and DSC, among others. Analyzing the thermal decomposition process of the CPI film by using TGA, such as the TGA curve shown in figure 3, wherein the thermal decomposition curves of the CPI film before and after mass production are basically overlapped, and the Td5 percent is about 524 ℃, and the change is not large; however, the thermal dimensional stability of the CPI film was measured by TMA and expressed by the Coefficient of Thermal Expansion (CTE), and the CTE (50-250 ℃ C.) of the CPI film after mass production was 29.4ppm/k, and the film material before mass production was broken at 155 ℃. The glass transition temperature (Tg) of the CPI film was measured by DSC, and the glass transition temperature Tg before mass production was about 150 ℃ and the glass transition temperature Tg after mass production was 272.85 ℃ in combination with TMA, and generally, the larger this value, the better the stability of the polymer. Therefore, the slurry produced by the production device for the transparent polyimide slurry has stable product quality and good continuity.
The present invention has been further described with reference to specific embodiments, but it should be understood that the detailed description should not be construed as limiting the spirit and scope of the present invention, and various modifications made to the above-described embodiments by those of ordinary skill in the art after reading this specification are within the scope of the present invention.

Claims (9)

1. The utility model provides a production device of transparent polyimide thick liquids which characterized in that: the system comprises a storage unit, a premixing unit, a main reaction unit, a nitrogen filtering unit, an activation processing unit, a temperature control system and a main control unit;
the storage unit consists of a plurality of constant temperature containers which are arranged in parallel, and each constant temperature container is provided with a feeding hole and a discharging hole;
the input end of the premixing unit is connected with the discharge hole of the constant-temperature container through a metering pump, and the output end of the premixing unit is connected with the main reaction unit;
the input end of the activation processing unit is connected with the discharge hole of the constant-temperature container, and the output end of the activation processing unit is connected with the main reaction unit;
part of the discharge hole of the constant temperature container and the temperature control system are connected with the main reaction unit;
the input end of the nitrogen filtering unit is connected with the nitrogen storage unit, and the output end of the nitrogen filtering unit is connected with the main reaction unit;
the storage unit, the premixing unit, the main reaction unit, the nitrogen filtering unit, the activation processing unit and the temperature control unit are respectively electrically connected with the main control unit.
2. The apparatus for producing transparent polyimide paste according to claim 1, wherein:
the premixing unit comprises a premixing reaction tank, and a gravity sensor, a premixing stirring mechanism, a nitrogen protection mechanism and a pressure relief mechanism which are arranged in the premixing reaction tank.
3. The apparatus for producing transparent polyimide paste according to claim 2, wherein:
the gravity sensor is electrically connected with the main control unit and used for measuring weight data of materials and transmitting the weight data to the main control unit.
4. The apparatus for producing transparent polyimide paste according to claim 1, wherein:
the main reaction unit comprises a reaction kettle body, and a dispersing mechanism, a vibration viscometer and a temperature sensor which are arranged in the reaction kettle body; the vibration viscometer and the temperature sensor are respectively arranged on the inner wall of the reactor body, and an air pressure protection mechanism and a small molecule reactant collection mechanism are externally connected to the reactor body.
5. The apparatus for producing transparent polyimide paste according to claim 4, wherein:
the dispersion mechanism comprises a driving motor fixedly mounted on the reaction kettle body and an enamel stirrer in transmission connection with the driving motor, wherein the enamel stirrer is composed of double-layer stirring paddles, and the double-layer stirring paddles are vertically arranged and are all arranged at an inclination angle of (35-45 degrees) with the vertical direction.
6. The apparatus for producing transparent polyimide paste according to claim 4, wherein:
the reactor body comprises a reactor body and a reactor cover arranged above the reactor body; the reaction kettle body is of a hollow structure with an opening at the top and is provided with an inner wall and an outer wall, the inner wall is made of enamel materials, the outer wall is made of stainless steel materials, and the outer wall is connected with the temperature control system.
7. The apparatus for producing transparent polyimide paste according to claim 1, wherein:
the nitrogen filtering unit consists of two multi-stage filtering towers.
8. The apparatus for producing transparent polyimide paste according to claim 1, wherein:
the temperature control system is a LAUDA constant temperature system.
9. The apparatus for producing transparent polyimide paste according to claim 1, wherein:
and the discharge port of the constant-temperature container is connected with the input end of the activation processing unit through a metering pump.
CN202111542542.8A 2021-12-16 2021-12-16 Production device of transparent polyimide slurry Pending CN114225869A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050054116A1 (en) * 2003-09-05 2005-03-10 Potyrailo Radislav A. Method of manufacturing and evaluating sensor coatings and the sensors derived therefrom
CN205007944U (en) * 2015-09-25 2016-02-03 南通凯英薄膜技术有限公司 A automatic material conveying equipment for preparing polyimide resin
CN207614830U (en) * 2017-11-14 2018-07-17 江苏常青树新材料科技有限公司 A kind of highly effective reaction device for one isooctyl of phosphorous acid hexichol
CN208082339U (en) * 2018-02-09 2018-11-13 广东润洁日化有限公司 A kind of not viscous wall Bidirectional stirrer
CN212017781U (en) * 2020-01-06 2020-11-27 深圳市华科创智技术有限公司 Automatic production device for water-based nano silver wire conductive ink

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050054116A1 (en) * 2003-09-05 2005-03-10 Potyrailo Radislav A. Method of manufacturing and evaluating sensor coatings and the sensors derived therefrom
CN205007944U (en) * 2015-09-25 2016-02-03 南通凯英薄膜技术有限公司 A automatic material conveying equipment for preparing polyimide resin
CN207614830U (en) * 2017-11-14 2018-07-17 江苏常青树新材料科技有限公司 A kind of highly effective reaction device for one isooctyl of phosphorous acid hexichol
CN208082339U (en) * 2018-02-09 2018-11-13 广东润洁日化有限公司 A kind of not viscous wall Bidirectional stirrer
CN212017781U (en) * 2020-01-06 2020-11-27 深圳市华科创智技术有限公司 Automatic production device for water-based nano silver wire conductive ink

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