CN109054724A - A kind of synthetic method of PTC function polyimides adhesive - Google Patents

A kind of synthetic method of PTC function polyimides adhesive Download PDF

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Publication number
CN109054724A
CN109054724A CN201810722208.2A CN201810722208A CN109054724A CN 109054724 A CN109054724 A CN 109054724A CN 201810722208 A CN201810722208 A CN 201810722208A CN 109054724 A CN109054724 A CN 109054724A
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CN
China
Prior art keywords
synthetic method
degrees celsius
polyimides adhesive
ptc function
coupling agent
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201810722208.2A
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Chinese (zh)
Inventor
汪元元
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New Mstar Technology Ltd In Hefei
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New Mstar Technology Ltd In Hefei
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Priority to CN201810722208.2A priority Critical patent/CN109054724A/en
Publication of CN109054724A publication Critical patent/CN109054724A/en
Withdrawn legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J179/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen, with or without oxygen, or carbon only, not provided for in groups C09J161/00 - C09J177/00
    • C09J179/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C09J179/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • 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
    • C08G73/1075—Partially aromatic polyimides
    • C08G73/1078—Partially aromatic polyimides wholly aromatic in the diamino moiety
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/0806—Silver

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The present invention proposes a kind of synthetic method of PTC function polyimides adhesive, which comprises the steps of: (1) under nitrogen protection, aromatic diamines are dissolved in polar solvent；(2) dianhydride compound is dissolved in same polar solvent, electrolytic silver powder and coupling agent is added, is uniformly dispersed；(3) under lower than -15 degrees Celsius salt water condition of ice bath, two parts of polar solvents is mixed according to aromatic diamines and dianhydride compound molar ratio 1: 1, is stirred to react to obtain amide acid solution, is put into -15 degrees Celsius of refrigerators below and saves；(4) solution is taken out when using, catalyst is added, and is heated to 60-80 degrees Celsius of solidification bonding.Polyimides adhesive is greatly reduced compared to traditional circuit plate plating process for filling hole cost as two-sided or multilayer epoxy glass wiring board, ceramic circuit-board plate through-hole conductive filler, saves wiring board area.

Description

A kind of synthetic method of PTC function polyimides adhesive
Technical field
The invention belongs to electronic materials and adhesive to synthesize field, be related to a kind of conjunction of PTC function polyimides adhesive At method.
Background technique
Polymer-based positive temperature coefficient (PPTC) material is widely used on all kinds of electronic circuit protection components.PPTC material Material has lower room temperature resistivity, and resistivity increases with the raising of temperature, sharply increases in some temperature spot resistance, big Resistance, which sharply increases, under current heating state realizes circuit shutdown, and can voluntarily restore low resistive state after troubleshooting.Currently, It is to develop more mature application mode in the market that the resistance of PPTC function, which is made into SMD surface mount elements, and technique is more mature, busy line Road plate space is smaller, but the factors such as its welding, route design as discrete component also will increase the manufacturing cost of integral device.
For two-sided, multilayer circuit board, connection of the route on different panels is realized often through conductive through hole.Traditional electricity Plating plug-hole technique is also the difficult point that technique is made in wiring board, it is contemplated that PPTC device is all to connect to play protection work in circuit With, using the medium of PTC current-limiting protection function as the hole-blocking agent of conductive through hole, can effectively save wiring board area, reduce Manufacturing cost.
Summary of the invention
For prior art defect, the purpose of the present invention is to provide a kind of synthesis of PTC function polyimides adhesive Method, which comprises the steps of:
(1) under nitrogen protection, aromatic diamines are dissolved in polar solvent；
(2) dianhydride compound is dissolved in same polar solvent, electrolytic silver powder and coupling agent is added, is uniformly dispersed；
(3) lower than under -15 degrees Celsius of salt water condition of ice bath, according to aromatic diamines and dianhydride compound molar ratio 1: 1 by two Part polar solvent mixing, is stirred to react to obtain amide acid solution, is put into -15 degrees Celsius of refrigerators below and saves；
(4) solution is taken out when using, catalyst is added, and is heated to 60-80 degrees Celsius of solidification bonding.
The aromatic diamines include one of p-phenylenediamine, m-phenylene diamine (MPD), Isosorbide-5-Nitrae-naphthylenediamine, 1,5- naphthylenediamine, described Dianhydride compound includes 1,2,3,4- cyclobutane dianhydrides, one of 1,2,3,4- pentamethylene dianhydride.
The electrolytic silver powder grain diameter is between 0.05 micron to 5 microns, and for partial size draw ratio less than 50, additional amount is most Final curing binder volume fraction 30%-50%, the coupling agent are chelating titanate coupling agent, the coupling of corrdination type titanate esters One of agent or combinations thereof.
The polar solvent includes one of n,N-Dimethylformamide, -2 pyrrolidones of 1- methyl.
The catalyst is one of pyridine, 3- picoline, and additional amount is step (2) amic acid mole 1-1.5 Times.
The PTC function polyimides adhesive application method of preparation is for two-sided or multilayer epoxy glass wiring board, pottery The conductive fill of porcelain wiring board plate through-hole plays the role of that wiring board upper layer and lower layer route is connected, when electric current is excessive or overheat When, resistance, which sharply increases, at plug-hole realizes circuit shutdown, can be self-healing conducting after troubleshooting.
The present invention is using the medium of PTC current-limiting protection function as two-sided or multilayer epoxy glass wiring board, ceramic circuit-board The conductive filler of plate through-hole is greatly reduced compared to traditional circuit plate plating process for filling hole cost, while making PTC function embedding Enter in wiring board, save wiring board area, promotes device circuit reliability.In addition, after original through-hole is for solidification on wiring board PTC functional unit naturally occur frame mould, can play and prevent water oxygen intrusion, promote the military service that repeatedly acts of overcurrent protection Performance.
The contents of the present invention and feature have revealed that as above, however the present invention that describes of front only briefly or pertains only to this The specific part of invention, feature of the invention may be more than what content disclosed herein was related to.Therefore, protection model of the invention The revealed content of embodiment should be not limited to by enclosing, and should include the combination of all the elements embodied in different piece, with And it is various without departing substantially from replacement and modification of the invention, and covered by claims of the present invention.
Specific embodiment
Embodiment 1:
(1) under nitrogen protection, 10mmol p-phenylenediamine is dissolved in 50mL n,N-Dimethylformamide；
(2) 1,2,3,4- cyclobutane dianhydride of 10mmol is dissolved in 50mL n,N-Dimethylformamide, 120g electricity is added Silver powder and 0.5g chelating titanate coupling agent are solved, is uniformly dispersed；
(3) mixed solution under lower than -15 degrees Celsius salt water condition of ice bath, is stirred to react to obtain amide acid solution, is put into -15 It is saved in degree Celsius refrigerator below；
(4) solution is taken out when using, 15mmol pyridine is added, and is heated to 60 degrees Celsius of solidification bondings, shear strength: 12MPa；Conductivity: 23Scm-1；PTC intensity: 2.5.
Embodiment 2:
(1) under nitrogen protection, 10mmol m-phenylene diamine (MPD) is dissolved in -2 pyrrolidones of 50mL 1- methyl；
(2) 1,2,3,4- cyclobutane dianhydride of 10mmol is dissolved in -2 pyrrolidones of 50mL 1- methyl, 180g electricity is added Silver powder and 0.5g chelating titanate coupling agent are solved, is uniformly dispersed；
(3) mixed solution under lower than -15 degrees Celsius salt water condition of ice bath, is stirred to react to obtain amide acid solution, is put into -15 It is saved in degree Celsius refrigerator below；
(4) solution is taken out when using, 10mmol pyridine is added, and is heated to 80 degrees Celsius of solidification bondings, shear strength: 9.6MPa；Conductivity: 34Scm-1；PTC intensity: 2.8.
Embodiment 3:
(1) under nitrogen protection, Isosorbide-5-Nitrae-naphthylenediamine of 10mmol is dissolved in 50mLN, in dinethylformamide；
(2) 1,2,3,4- pentamethylene dianhydride of 10mmol is dissolved in 50mL n,N-Dimethylformamide, 150g electricity is added Silver powder and 0.5g corrdination type titanate coupling agent are solved, is uniformly dispersed；
(3) mixed solution under lower than -15 degrees Celsius salt water condition of ice bath, is stirred to react to obtain amide acid solution, is put into -15 It is saved in degree Celsius refrigerator below；
(4) solution is taken out when using, the 3- picoline of 15mmol is added, is heated to 70 degrees Celsius of solidification bondings, shearing Intensity: 10MPa；Conductivity: 27Scm-1；PTC intensity: 2.4.
Embodiment 4:
(1) under nitrogen protection, 1, the 5- naphthylenediamine of 10mmol is dissolved in -2 pyrrolidones of 50mL 1- methyl；
(2) 1,2,3,4- cyclobutane dianhydride of 10mmol is dissolved in -2 pyrrolidones of 50mL 1- methyl, 180g electricity is added Silver powder and 0.5g chelating titanate coupling agent are solved, is uniformly dispersed；
(3) mixed solution under lower than -15 degrees Celsius salt water condition of ice bath, is stirred to react to obtain amide acid solution, is put into -15 It is saved in degree Celsius refrigerator below；
(4) solution is taken out when using, 10mmol pyridine is added, and is heated to 70 degrees Celsius of solidification bondings, shear strength: 8.8MPa；Conductivity: 30Scm-1；PTC intensity: 2.5.
Embodiment 5:
(1) under nitrogen protection, 10mmol p-phenylenediamine is dissolved in 50mL n,N-Dimethylformamide；
(2) 1,2,3,4- pentamethylene dianhydride of 10mmol is dissolved in 50mL n,N-Dimethylformamide, 160g electricity is added Silver powder and 0.5g corrdination type titanate coupling agent are solved, is uniformly dispersed；
(3) mixed solution under lower than -15 degrees Celsius salt water condition of ice bath, is stirred to react to obtain amide acid solution, is put into -15 It is saved in degree Celsius refrigerator below；
(4) solution is taken out when using, the 3- picoline of 12mmol is added, is heated to 70 degrees Celsius of solidification bondings, shearing Intensity: 9.1MPa；Conductivity: 31Scm-1；PTC intensity: 2.6.

Claims (6)

1. a kind of synthetic method of PTC function polyimides adhesive, which comprises the steps of:
(1) under nitrogen protection, aromatic diamines are dissolved in polar solvent；
(2) dianhydride compound is dissolved in same polar solvent, electrolytic silver powder and coupling agent is added, is uniformly dispersed；
(3) lower than under -15 degrees Celsius of salt water condition of ice bath, according to aromatic diamines and dianhydride compound molar ratio 1: 1 by two parts of poles Property solution mixing, be stirred to react to obtain amide acid solution, be put into -15 degrees Celsius of refrigerators below and save；
(4) solution is taken out when using, catalyst is added, and is heated to 60-80 degrees Celsius of solidification bonding.
2. a kind of synthetic method of PTC function polyimides adhesive according to claim 1, which is characterized in that the virtue Fragrant diamines includes one of p-phenylenediamine, m-phenylene diamine (MPD), Isosorbide-5-Nitrae-naphthylenediamine, 1,5- naphthylenediamine, and the dianhydride compound includes 1,2,3,4- cyclobutane dianhydride, one of 1,2,3,4- pentamethylene dianhydride.
3. a kind of synthetic method of PTC function polyimides adhesive according to claim 1, which is characterized in that the electricity Silver powder particles partial size is solved between 0.05 micron to 5 microns, for partial size draw ratio less than 50, additional amount is final solidification binder body Fraction 30%-50%, the coupling agent be one of chelating titanate coupling agent, corrdination type titanate coupling agent or its Combination.
4. a kind of synthetic method of PTC function polyimides adhesive according to claim 1, which is characterized in that the pole Property solvent includes one of n,N-Dimethylformamide, -2 pyrrolidones of 1- methyl.
5. a kind of synthetic method of PTC function polyimides adhesive according to claim 1, which is characterized in that described to urge Agent is one of pyridine, 3- picoline, and additional amount is 1-1.5 times of amic acid mole of step (2).
6. prepared by a kind of synthetic method of PTC function polyimides adhesive as claimed in any one of claims 1 to 5, wherein PTC function polyimides adhesive, application method are for two-sided or multilayer epoxy glass wiring board, ceramic circuit-board plate through-hole Conductive fill, play the role of that wiring board upper layer and lower layer route is connected, when electric current is excessive or overheat, resistance is anxious at plug-hole Increase severely plus realize circuit shutdown, can be self-healing conducting after troubleshooting.
CN201810722208.2A 2018-06-26 2018-06-26 A kind of synthetic method of PTC function polyimides adhesive Withdrawn CN109054724A (en)

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Application Number Priority Date Filing Date Title
CN201810722208.2A CN109054724A (en) 2018-06-26 2018-06-26 A kind of synthetic method of PTC function polyimides adhesive

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Application Number Priority Date Filing Date Title
CN201810722208.2A CN109054724A (en) 2018-06-26 2018-06-26 A kind of synthetic method of PTC function polyimides adhesive

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CN109054724A true CN109054724A (en) 2018-12-21

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1786096A (en) * 2004-12-08 2006-06-14 Lg电线株式会社 Anisotropic conductive adhesive having PTC characteristics
CN101560371A (en) * 2008-04-18 2009-10-21 中国科学院化学研究所 High temperature resistant thermosetting polyimide adhesive and preparation method thereof
CN103865471A (en) * 2012-12-18 2014-06-18 上海市合成树脂研究所 Polyimide adhesive and preparation method thereof
CN106478950A (en) * 2016-09-26 2017-03-08 安徽国风塑业股份有限公司 A kind of preparation method of high-adhesion Kapton

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1786096A (en) * 2004-12-08 2006-06-14 Lg电线株式会社 Anisotropic conductive adhesive having PTC characteristics
CN101560371A (en) * 2008-04-18 2009-10-21 中国科学院化学研究所 High temperature resistant thermosetting polyimide adhesive and preparation method thereof
CN103865471A (en) * 2012-12-18 2014-06-18 上海市合成树脂研究所 Polyimide adhesive and preparation method thereof
CN106478950A (en) * 2016-09-26 2017-03-08 安徽国风塑业股份有限公司 A kind of preparation method of high-adhesion Kapton

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Application publication date: 20181221

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