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Preparation method of carbon black dispersion liquid for black polyimide film

A technology of polyimide film and dispersion liquid, which is applied in the field of preparation of carbon black dispersion liquid for black polyimide film, can solve the problem of deterioration of dispersion condition, difficulty and large workload of dispersant selection, and selection range of dispersant. Narrowing etc.

Pending Publication Date: 2022-07-15
山东万达微电子材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem with this method is that the introduced hyperbranched dispersant has poor high temperature resistance and can only meet the preparation of polyimide films with an imidization temperature below 290°C. For those with a higher imidization temperature (usually 350 The preparation of polyimide film is not applicable; the second is that the selection criteria of the dispersant are not determined according to the different pH values ​​of graphene oxide, which leads to the difficulty and heavy workload of dispersant selection for different graphene oxide
However, there are many difficulties in realizing the stable dispersion of carbon black in the synthesis process of black polyimide.
The problems that usually occur include: when the well-dispersed carbon black dispersion is added to the diamine solution, poor dispersion such as flocculation occurs; the well-dispersed carbon black dispersion system in the diamine solution, in the process of adding dianhydride to prepare polyamic acid It is also prone to the phenomenon of worsening dispersion
The existence of the above-mentioned problems leads to the narrowing of the selection range of the dispersant and increasing the difficulty when preparing the carbon black dispersion

Method used

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  • Preparation method of carbon black dispersion liquid for black polyimide film
  • Preparation method of carbon black dispersion liquid for black polyimide film
  • Preparation method of carbon black dispersion liquid for black polyimide film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Experimental raw materials: N,N-dimethylacetamide (DMAc), pyromellitic dianhydride (PMDA), 4,4'-diaminodiphenyl ether (ODA), carbon black (brand: Orilon FW200; PH value 2.5);

[0053] Experimental equipment: double-layer glass reactor, circulating cooler, electric stirrer, sand mill;

[0054] Add 695g of DMAc to the double-layer glass reactor, add 60g of ODA, start the electric stirrer and stir at 150r / min for 30min, divide 45g of PMDA into two equal parts, slowly add the first part of dianhydride to the reactor, and stir for 15min. Then slowly add the second part of dianhydride into the reactor, stir for 30min, and control the polymerization temperature between 45±2°C during the reaction. After adding 200g of carbon black (brand: Orilong FW200, pH 2.5) and stirring evenly, the slurry was ground with a sand mill at 2800r / min for 10 hours.

[0055] The mass percentage of carbon black in the obtained dispersion was 20%, the molar ratio of PDMA to ODA was 0.7 (R=0.7), an...

Embodiment 2

[0058] This example is similar to the technical solution adopted in Example 1, except that the carbon black brand used is LampBLACK 101 (the pH value of the product is 7.5), and the quality of the PDMA used is 58.81 g (R=0.9 at this time). ).

[0059] After testing, the median particle size of carbon black in the prepared carbon black dispersion was 50 nm (D 50 = 50nm) for 90 days: no sedimentation.

Embodiment 3

[0060] Example 3: Preparation of carbon black dispersion for black polyimide film

[0061] This example is similar to the technical solution adopted in Example 1, except that the carbon black brand used is PRINTEX L6 (commodity pH value is 9.5), and the quality of the PDMA used is 64g (R is 0.98 at this time) .

[0062] After testing, the median particle size of carbon black in the prepared carbon black dispersion was 50 nm (D 50 =50nm), placed for 90 days without sedimentation.

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Abstract

The invention relates to a preparation method of a carbon black dispersion liquid for a black polyimide film, which is characterized by comprising the following steps of: dissolving a diamine monomer into a strong-polarity aprotic organic solvent, adding a dianhydride monomer in batches, controlling the molar ratio of the dianhydride monomer to the diamine monomer to be 0.7-0.98, controlling the reaction temperature to be 40-50 DEG C, and reacting for 40-60 minutes to obtain a carbon black dispersing agent of a polyamide acid system; the preparation method comprises the following steps: adding carbon black into a carbon black dispersant of a polyamide acid system, stirring, and grinding for 9-11 hours by using a grinding machine to obtain a carbon black dispersion liquid; the carbon black can realize high-stability dispersion in the aspect of preparing modified polyimide, and stable preparation of the high-performance carbon black-polyimide composite material is realized.

Description

technical field [0001] The present invention relates to a preparation method of carbon black dispersion liquid for black polyimide film. Background technique [0002] Polyimide (PI) is a general term for heterocyclic polymers containing imide groups in the main chain. It is one of the engineering plastics with the best heat resistance. With excellent mechanical strength and non-combustibility, it is widely used in films, coatings, advanced composite materials, fibers, engineering plastics and other fields. Polyimide can be divided into three categories: thermosetting polyimide, thermoplastic polyimide and modified polyimide, and it is developing rapidly. Among them, the composite modification of polyimide by filling to achieve the improvement of function and performance is the current research focus. [0003] The preparation of aromatic polyimide by polycondensation is the current mainstream process, which is prepared by the reaction of aromatic diamines with aromatic dian...

Claims

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Application Information

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IPC IPC(8): C08J3/09C08J5/18C08G73/10C08L79/08C08K3/04
CPCC08J3/096C08J5/18C08G73/1007C08G73/105C08G73/1071C08J2379/08C08K3/04C08K2201/011
Inventor 初明辉王会宾王聪聪朱星驰
Owner 山东万达微电子材料有限公司
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