CN109021564A - A kind of acid anhydrides graft-polyamide enhancing conductive material and preparation method thereof - Google Patents

A kind of acid anhydrides graft-polyamide enhancing conductive material and preparation method thereof Download PDF

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CN109021564A
CN109021564A CN201810971790.6A CN201810971790A CN109021564A CN 109021564 A CN109021564 A CN 109021564A CN 201810971790 A CN201810971790 A CN 201810971790A CN 109021564 A CN109021564 A CN 109021564A
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added
polyamide
graft
taken
stirs evenly
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崔晓迪
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00Compositions of 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 C08L61/00 - C08L77/00
    • C08L79/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/04Antistatic

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Graft Or Block Polymers (AREA)
  • Conductive Materials (AREA)

Abstract

The invention discloses a kind of acid anhydrides graft-polyamides to enhance conductive material, it is composed of the following raw materials by weight: maleic anhydride 3-4, grafting auxiliary agent 1-2, pyrroles 140-160, ammonium persulfate 3-4, polyamide lotion 35-30, hexadecyltrimethylammonium chloride 1-2, the present invention uses maleic anhydride for raw material, using divinylbenzene as grafting agent, graft modification is carried out to polyamide, later using the graft emulsion as solvent, it polymerize by monomer of pyrroles, so as to improve dispersion compatibility of the polyamide between polypyrrole, the mechanical strength of finished-product material is improved.

Description

A kind of acid anhydrides graft-polyamide enhancing conductive material and preparation method thereof
Technical field
The invention belongs to field of lithium ion battery, and in particular to a kind of acid anhydrides graft-polyamide enhancing conductive material and its system Preparation Method.
Background technique
Lithium ion battery steps into people with the features such as higher energy density, good cycle performance, memory-less effect Sight, and become researchers' focus of attention in recent years.
Conductive additive is one of indispensable critical material of lithium ion battery, especially in power-type lithium ion battery High current charge-discharge during have a very important role.Different conductive agents have the characteristics that respective, and form is also respectively to have An eternal lasting;Present battery can be divided into the three categories such as conductive black, electrically conductive graphite and novel conductive agent using wide conductive agent, newly Type conductive agent refers mainly to carbon nanotube, graphene etc., and polypyrrole has good conductive stable as a kind of conducting polymer Property, however due to being still had several drawbacks in its mechanical property, it is also relatively low in the application of field of batteries.Therefore, originally The purpose of invention is to provide that a kind of novel electric conductivity is strong, and mechanical property is good, the high additives for battery of conductive stability.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of enhancings of acid anhydrides graft-polyamide to lead Electric material and preparation method thereof.
To achieve the above object, the invention adopts the following technical scheme:
A kind of acid anhydrides graft-polyamide enhancing conductive material, it is composed of the following raw materials by weight:
Maleic anhydride 3-4, grafting auxiliary agent 1-2, pyrroles 140-160, ammonium persulfate 3-4, polyamide lotion 35-30, cetyl Trimethyl ammonium chloride 1-2.
What the polyamide lotion was made of the raw material of following weight parts:
Acrylamide 40-50, ammonium persulfate 1-1.2, barium stearate 1-2, cyanethyl cellulose 2-3, polysorbate 0.7-1.
The preparation method of the polyamide lotion, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 30-40 times of its weight, stirs evenly;
(2) cyanethyl cellulose is taken, is added in the dimethylformamide of 5-7 times of its weight, stirs evenly, stearic acid is added Barium, increasing temperature is 50-55 DEG C, insulated and stirred 10-20 minutes, obtains fiber solution;
(3) acrylamide, polysorbate mixing are taken, is added in the deionized water of 13-20 times of mixture weight, stirs evenly, It is sent in reaction kettle, is passed through nitrogen, adjusting temperature of reaction kettle is 65-70 DEG C, and it is water-soluble that above-mentioned fiber solution, ammonium persulfate is added Liquid, insulated and stirred 4-5 hours, discharging was cooling to get the polyamide lotion.
The grafting auxiliary agent is divinylbenzene.
A kind of preparation method of acid anhydrides graft-polyamide enhancing conductive material, comprising the following steps:
(1) grafting auxiliary agent, hexadecyltrimethylammonium chloride mixing are taken, the deionized water of 13-20 times of mixture weight is added to In, it stirs evenly, obtains graft dispersion liquid;
(2) maleic anhydride is taken, is added in above-mentioned polyamide lotion, stirs evenly, increasing temperature is 70-75 DEG C, is added above-mentioned Graft dispersion liquid insulated and stirred 3-4 hours, obtains graft emulsion;
(3) ammonium persulfate is taken, is added in the deionized water of 5-8 times of its weight, stirs evenly, obtain initiator solution;
(4) pyrroles is taken, is added in above-mentioned graft emulsion, stirs evenly, be sent in reaction kettle, is passed through nitrogen, adjusts reaction Kettle temperature degree is 70-75 DEG C, and above-mentioned initiator solution is added, insulated and stirred 4-5 hours, discharges, filters, filter cake is washed, room temperature It is dry to enhance conductive material to get the acid anhydrides graft-polyamide.
Advantages of the present invention:
The present invention is first using acrylamide as monomer, using the amide solution of cyanethyl cellulose as reaction dissolvent, makees in initiator With lower polymerization, obtain polyamide solution, then use maleic anhydride for raw material, using divinylbenzene as grafting agent, to polyamide into Row graft modification polymerize later using the graft emulsion as solvent by monomer of pyrroles, so as to improve polyamide in poly- pyrrole Dispersion compatibility between coughing up improves the mechanical strength and stability of finished-product material, and then the use for improving lithium ion battery is strong Degree and safety in utilization.
Specific embodiment
Embodiment 1
A kind of acid anhydrides graft-polyamide enhancing conductive material, it is composed of the following raw materials by weight:
Maleic anhydride 3, grafting auxiliary agent 1, pyrroles 140, ammonium persulfate 3, polyamide lotion 35, hexadecyltrimethylammonium chloride 1.
What the polyamide lotion was made of the raw material of following weight parts:
Acrylamide 40, ammonium persulfate 1, barium stearate 1, cyanethyl cellulose 2, polysorbate 0.7.
The preparation method of the polyamide lotion, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 30 times of its weight, stirs evenly;
(2) cyanethyl cellulose is taken, is added in the dimethylformamide of 5 times of its weight, stirs evenly, barium stearate is added, Increasing temperature is 50 DEG C, insulated and stirred 10 minutes, obtains fiber solution;
(3) acrylamide, polysorbate mixing are taken, is added in 13 times of mixture weight of deionized water, stirs evenly, be sent into Into reaction kettle, it is passed through nitrogen, adjusting temperature of reaction kettle is 65 DEG C, and above-mentioned fiber solution, ammonium persulfate aqueous solution is added, and is kept the temperature Stirring 4 hours, discharging are cooling to get the polyamide lotion.
The grafting auxiliary agent is divinylbenzene.
A kind of preparation method of acid anhydrides graft-polyamide enhancing conductive material, comprising the following steps:
(1) grafting auxiliary agent, hexadecyltrimethylammonium chloride mixing are taken, is added in 13 times of mixture weight of deionized water, It stirs evenly, obtains graft dispersion liquid;
(2) maleic anhydride is taken, is added in above-mentioned polyamide lotion, stirs evenly, increasing temperature is 70 DEG C, and above-mentioned grafting is added Dispersion liquid insulated and stirred 3 hours, obtains graft emulsion;
(3) ammonium persulfate is taken, is added in the deionized water of 5 times of its weight, is stirred evenly, obtain initiator solution;
(4) pyrroles is taken, is added in above-mentioned graft emulsion, stirs evenly, be sent in reaction kettle, is passed through nitrogen, adjusts reaction Kettle temperature degree is 70 DEG C, and above-mentioned initiator solution is added, insulated and stirred 4-5 hours, discharges, filters, filter cake is washed, room temperature is dry It is dry to enhance conductive material to get the acid anhydrides graft-polyamide.
Embodiment 2
A kind of acid anhydrides graft-polyamide enhancing conductive material, it is composed of the following raw materials by weight:
Maleic anhydride 4, grafting auxiliary agent 2, pyrroles 160, ammonium persulfate 4, polyamide lotion 30, hexadecyltrimethylammonium chloride 2.
What the polyamide lotion was made of the raw material of following weight parts:
Acrylamide 50, ammonium persulfate 1.2, barium stearate 2, cyanethyl cellulose 3, polysorbate 1.
The preparation method of the polyamide lotion, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 40 times of its weight, stirs evenly;
(2) cyanethyl cellulose is taken, is added in the dimethylformamide of 7 times of its weight, stirs evenly, barium stearate is added, Increasing temperature is 55 DEG C, insulated and stirred 20 minutes, obtains fiber solution;
(3) acrylamide, polysorbate mixing are taken, is added in 20 times of mixture weight of deionized water, stirs evenly, be sent into Into reaction kettle, it is passed through nitrogen, adjusting temperature of reaction kettle is 70 DEG C, and above-mentioned fiber solution, ammonium persulfate aqueous solution is added, and is kept the temperature Stirring 5 hours, discharging are cooling to get the polyamide lotion.
The grafting auxiliary agent is divinylbenzene.
A kind of preparation method of acid anhydrides graft-polyamide enhancing conductive material, comprising the following steps:
(1) grafting auxiliary agent, hexadecyltrimethylammonium chloride mixing are taken, is added in 20 times of mixture weight of deionized water, It stirs evenly, obtains graft dispersion liquid;
(2) maleic anhydride is taken, is added in above-mentioned polyamide lotion, stirs evenly, increasing temperature is 75 DEG C, and above-mentioned grafting is added Dispersion liquid insulated and stirred 4 hours, obtains graft emulsion;
(3) ammonium persulfate is taken, is added in the deionized water of 8 times of its weight, is stirred evenly, obtain initiator solution;
(4) pyrroles is taken, is added in above-mentioned graft emulsion, stirs evenly, be sent in reaction kettle, is passed through nitrogen, adjusts reaction Kettle temperature degree is 75 DEG C, and above-mentioned initiator solution is added, insulated and stirred 5 hours, discharges, filters, filter cake is washed, air drying, Enhance conductive material up to the acid anhydrides graft-polyamide.
Performance test:
Acid anhydrides graft-polyamide enhancing conductive material of the invention is subjected to charge-discharge test, under the conditions of 0.2A/g charge and discharge Specific capacitance be 180.5-193.0F/g;Tensile strength is 150.5-161.2Mpa.

Claims (4)

1. a kind of acid anhydrides graft-polyamide enhances conductive material, it is composed of the following raw materials by weight:
Maleic anhydride 3-4, grafting auxiliary agent 1-2, pyrroles 140-160, ammonium persulfate 3-4, polyamide lotion 35-30, cetyl Trimethyl ammonium chloride 1-2;It is characterized in that, the grafting auxiliary agent is divinylbenzene.
2. a kind of acid anhydrides graft-polyamide according to claim 1 enhances conductive material, which is characterized in that the polyamides Amine lotion is made of the raw material of following weight parts:
Acrylamide 40-50, ammonium persulfate 1-1.2, barium stearate 1-2, cyanethyl cellulose 2-3, polysorbate 0.7-1.
3. a kind of acid anhydrides graft-polyamide according to claim 2 enhances conductive material, which is characterized in that the polyamides The preparation method of amine lotion, comprising the following steps:
(1) ammonium persulfate is taken, is added in the deionized water of 30-40 times of its weight, stirs evenly;
(2) cyanethyl cellulose is taken, is added in the dimethylformamide of 5-7 times of its weight, stirs evenly, stearic acid is added Barium, increasing temperature is 50-55 DEG C, insulated and stirred 10-20 minutes, obtains fiber solution;
(3) acrylamide, polysorbate mixing are taken, is added in the deionized water of 13-20 times of mixture weight, stirs evenly, It is sent in reaction kettle, is passed through nitrogen, adjusting temperature of reaction kettle is 65-70 DEG C, and it is water-soluble that above-mentioned fiber solution, ammonium persulfate is added Liquid, insulated and stirred 4-5 hours, discharging was cooling to get the polyamide lotion.
4. a kind of preparation method of acid anhydrides graft-polyamide enhancing conductive material as described in claim 1, which is characterized in that packet Include following steps:
(1) grafting auxiliary agent, hexadecyltrimethylammonium chloride mixing are taken, the deionized water of 13-20 times of mixture weight is added to In, it stirs evenly, obtains graft dispersion liquid;
(2) maleic anhydride is taken, is added in above-mentioned polyamide lotion, stirs evenly, increasing temperature is 70-75 DEG C, is added above-mentioned Graft dispersion liquid insulated and stirred 3-4 hours, obtains graft emulsion;
(3) ammonium persulfate is taken, is added in the deionized water of 5-8 times of its weight, stirs evenly, obtain initiator solution;
(4) pyrroles is taken, is added in above-mentioned graft emulsion, stirs evenly, be sent in reaction kettle, is passed through nitrogen, adjusts reaction Kettle temperature degree is 70-75 DEG C, and above-mentioned initiator solution is added, insulated and stirred 4-5 hours, discharges, filters, filter cake is washed, room temperature It is dry to enhance conductive material to get the acid anhydrides graft-polyamide.
CN201810971790.6A 2018-08-24 2018-08-24 A kind of acid anhydrides graft-polyamide enhancing conductive material and preparation method thereof Pending CN109021564A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113667257A (en) * 2021-05-14 2021-11-19 赛轮集团股份有限公司 Modified nano-cellulose/polypyrrole composite material and preparation method thereof, antistatic rubber composition and preparation method thereof

Citations (3)

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Publication number Priority date Publication date Assignee Title
IE36142L (en) * 1971-03-30 1972-09-30 Buckman Labor Inc Graft polymers
CN105001420A (en) * 2015-07-24 2015-10-28 佛山市维晨科技有限公司 Preparing method for polypyrrole nanofiber conductive electrode material
CN105778089A (en) * 2016-03-18 2016-07-20 赵守彬 Inorganic particle modified magnetic composite material and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
IE36142L (en) * 1971-03-30 1972-09-30 Buckman Labor Inc Graft polymers
CN105001420A (en) * 2015-07-24 2015-10-28 佛山市维晨科技有限公司 Preparing method for polypyrrole nanofiber conductive electrode material
CN105778089A (en) * 2016-03-18 2016-07-20 赵守彬 Inorganic particle modified magnetic composite material and preparation method thereof

Non-Patent Citations (1)

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Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113667257A (en) * 2021-05-14 2021-11-19 赛轮集团股份有限公司 Modified nano-cellulose/polypyrrole composite material and preparation method thereof, antistatic rubber composition and preparation method thereof
CN113667257B (en) * 2021-05-14 2023-09-29 赛轮集团股份有限公司 Modified nanocellulose/polypyrrole composite material and preparation method thereof, antistatic rubber composition and preparation method thereof

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