CN103342869A - Modified carbon black/PVA (polyvinyl alcohol) film and preparation method thereof - Google Patents

Modified carbon black/PVA (polyvinyl alcohol) film and preparation method thereof Download PDF

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CN103342869A
CN103342869A CN2013103183851A CN201310318385A CN103342869A CN 103342869 A CN103342869 A CN 103342869A CN 2013103183851 A CN2013103183851 A CN 2013103183851A CN 201310318385 A CN201310318385 A CN 201310318385A CN 103342869 A CN103342869 A CN 103342869A
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carbon black
modified carbon
pva
film
black
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王雁冰
魏冲
陈娜
彭睿
李文静
周晨光
程龙山
黄志雄
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Wuhan University of Technology WUT
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/07—Flat, e.g. panels
    • B29C48/08—Flat, e.g. panels flexible, e.g. films
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material

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Abstract

The invention relates to a modified carbon black/PVA (polyvinyl alcohol) film and a preparation method thereof. The preparation method comprises the following steps: dissolving m parts of modified carbon black and (100-m) parts of PVA in water at 90 DEG C, and carrying out cast molding, or carrying out extrusion molding at 225+/-10 DEG C, wherein 0<m<=10; the modified carbon black comprises oxidized black and polyetheramine-modified carbon black; the PVA comprises PVAs with different alcoholysis degrees and molecular weights; and the ionic bond formed by the reaction between the terminal amino group of the polyetheramine high polymer chain and the carboxyl group on the carbon black surface increases the interparticle repulsion, reduces the aggregation effect, and thus, is beneficial to the dispersion of the particles in the substrate. The ether oxygen bond and amino group in the polyetheramine molecular chain and the abundant hydroxyl groups in the PVA molecular chain can form hydrogen bonds, thereby enhancing the strength and modulus of the film; and the carbon black particles are used as a nucleating agent to promote the crystallization of the PVA. The preparation method provides an effective means for enhancing mechanical properties and crystallinity of the PVA film, and has favorable application prospects.

Description

A kind of modified carbon black/PVA film and preparation method thereof
Technical field
The invention belongs to the polymer matrix composite field of modified carbon black, relate to a kind of PVA film and preparation method thereof.
Background technology
Carbon black is a kind of common filler, is usually used in reinforcing rubber, pigment coloring or as electro-conductive material.But carbon black is little because of particle diameter, and specific surface energy is big, reunites easily, is difficult to disperse well in polymkeric substance, has influenced modified effect.In order to improve the dispersiveness of carbon black in polymkeric substance, investigation of materials person has proposed the method for modifying of a lot of carbon blacks, as pass through corona treatment, the plasma treatment carbon blacksurface obtains physical methods such as active group, introduce chemical processes such as active group with the coupling agent treatment carbon blacksurface, wherein introduce active group at carbon blacksurface, graft polymer chain is effect a kind of method preferably again.This method is introduced polymer chain on the carbon black particle surface, increased interparticle steric hindrance, and the ionic linkage that the carboxyl on the end amido of polyetheramine and carbon black particle surface forms increased interparticle repulsion, weakened the reunion effect, makes particle obtain good dispersiveness in polymkeric substance.
Polyvinyl alcohol (PVA) is a kind of Biodegradable polymer material, cheap, degree of crystallinity height, bonding force are by force, often prepare thin-film material by casting film-forming, pliable and tough level and smooth, the oil resistant of its goods, anti-solvent and gas barrier property are outstanding, have unique advantage aspect food, the drug packaging.But the PVA film strength, modulus is lower, and thermotolerance is relatively poor.
The present invention is by the strong acid oxidation, and the acid-base neutralisation method makes a kind of modified carbon black with good dispersion, and this modified carbon black is joined in the polyvinyl alcohol water solution through casting film-forming or extrusion moulding, has obtained a kind of modified carbon black/PVA film.The modified carbon black particle has played the effect of nucleator to PVA, has promoted the crystallization of PVA, has improved degree of crystallinity.Great amount of hydroxy group in ether-oxygen bond in the polyetheramine macromolecular chain, amido and the PVA molecular chain forms hydrogen bond, has improved melt temperature and the heat decomposition temperature of PVA.This method provides a kind of raising thin film mechanical performance and stable on heating effective means.
Summary of the invention:
The purpose of this invention is to provide a kind of modified carbon black/PVA film and preparation method thereof, to improve intensity, modulus and the degree of crystallinity of PVA film.
To achieve these goals, technical scheme of the present invention is as follows:
Modified carbon black provided by the invention/PVA film, it dissolves back casting by quality m part modified carbon black and 100-m part PVA in water under 90 ℃, or in melt temperature (225 ± 10 ℃) following extrusion moulding, wherein 0＜m≤10; Described modified carbon black adopts oxygenated black, long-chain fat amine Soxylat A 25-7 modified carbon black, polyoxyethylene polyoxypropylene ether monoamine modified carbon black; Polyoxyethylene polyoxypropylene ether diamine modified carbon black.Described PVA adopts a kind of among PVA-1750, PVA-1778, PVA-1788, the PVA-1798.
Described long-chain fat amine Soxylat A 25-7 modified carbon black can adopt AC-1810 modified carbon black, AC-1830 modified carbon black or AC-1860 modified carbon black.
Described polyoxyethylene polyoxypropylene ether monoamine modified carbon black can adopt M-1000 modified carbon black, M-2005 modified carbon black M-2070 modified carbon black.
Described polyoxyethylene polyoxypropylene ether diamine modified carbon black can adopt ED-600 modified carbon black, ED-900 modified carbon black or ED-2003 modified carbon black.
The preparation method of first kind of modified carbon black provided by the invention/PVA film, be to adopt the casting forming method preparation, specifically: oxygenated black and the polyethex amine modification carbon black with the m mass parts joins in the distilled water respectively, through magnetic stirrer, adds 100-m mass parts PVA again, 0＜m≤10, dissolve fully through gradient increased temperature to polyvinyl alcohol then, stop heating, be cast on the sheet glass after the cooling, the demoulding behind steady placement 2～3d obtains modified carbon black/PVA film under the room temperature.
The preparation method of second kind of modified carbon black provided by the invention/PVA film, be to adopt the extruding forming method preparation, specifically: modified carbon black and the 100-m mass parts PVA of m mass parts are mixed, 0＜m≤10, through the forcing machine extruding pelletization, in extrusion moulding, extrusion temperature is 225 ± 10 ℃, 10～50 rev/mins of rotating speeds obtain modified carbon black/PVA film through calendering formation again.
Modified carbon black of the present invention can be made by following method, and its step comprises:
Step 1: the nitration mixture of the vitriol oil and concentrated nitric acid 3:1 preparation is by volume joined in the reactor that fills carbon black, in 70 ℃ ultrasonic down, stir 24h, be neutral through dialysing to dialyzate, take out and be placed in the baking oven 80 ℃ of oven dry, make the oxygenated black powder;
Step 2: press mass fraction, get the oxygenated black m in the step 1 1Part is scattered in 100-m 1In part distilled water, get m 2Part polyetheramine is dissolved in 100-m 2In part distilled water, 0＜m 1≤ 10,0＜m 2≤ 50, then the oxygenated black dispersant liquid drop is added in the polyether amine solution, under normal temperature, react 24h, obtain the aqueous dispersions of polyethex amine modification carbon black.
In the above-mentioned steps, described polyetheramine can adopt long-chain fat amine Soxylat A 25-7, polyoxyethylene polyoxypropylene ether monoamine, polyoxyethylene polyoxypropylene ether diamine.Described long-chain fat amine Soxylat A 25-7 can adopt AC-1810, AC-1830, and AC-1860, its molecular formula is (C 18H 37) N (CH 3CH 2OH) nH (CH 2CH 2O) mH, wherein AC-1810(m+n=10), AC-1830 (m+n=30), AC-1860(m+n=60).
Described polyoxyethylene polyoxypropylene ether monoamine can adopt M-1000(x:y=3:19), M-2005(x:y=29:6), M-2070(x:y=10:31), its structural formula formula is:
Figure BDA00003573146000021
Described polyoxyethylene polyoxypropylene ether diamine can adopt ED-600(y=～3.6, x+z=～9.0), ED-900(y=～12.5, x+z=～6.0) or ED-2003(y=～39, x+z=～6.0).Its molecular structural formula is:
Polyethex amine modification carbon black of the present invention can adopt the polyethex amine modification carbon black of the different percentage of grafting that control oxygenated black and the mass ratio of polyetheramine obtain.
The carbon black that the present invention adopts, its model can comprise the carbon black of different-grain diameter size, in order to can be applicable to that with different purposes, the carbon black of different-grain diameter carries out modification, can be applied to different production fields.As graphitized carbon black XC72R(30～1000nm), colour carbon black M880(35～1000nm), printing ink carbon black R660(40～1000nm), hard(carbon)black N330(26～1000nm).
The present invention has following advantage compared with the prior art:
1. carbon blacksurface is carried out oxide treatment, generated in a large number-COOH at carbon blacksurface, be beneficial to and the reaction of polyetheramine generation acid-base neutralisation, polyetheramine has improved 20%～90% at the percentage of grafting of carbon blacksurface.
2. dispersion technology such as ultra-sonic dispersion, magnetic agitation have been used, effectively improved carbon black particle, the polyetheramine dispersion state in water, for-COOH and polyetheramine surface group provide good reaction environment, further improved the percentage of grafting of polyetheramine at carbon blacksurface.
3. select for use polyetheramine as graft polymer chain, the ether-oxygen bond in the polyetheramine molecular chain and end amido can with the PVA molecular chain in great amount of hydroxy group form hydrogen bond, increased the consistency of carbon black particle and PVA matrix.
4. after adding certain density modified carbon black, the melt temperature of PVA film has improved 1～10 ℃, and the intensity maximum is brought up to 95MPa, and purer PVA improves 1.32 times; The modulus maximum is brought up to 4GPa, and purer PVA has improved 1.48 times.Degree of crystallinity has improved 30%～40%.
Description of drawings
Fig. 1 is AC-1830 modified carbon black TEM image, and by image as can be known, the carbon black particle surface has coated the shell that the one layer of polymeric chain is formed, and has increased the steric hindrance between carbon black particle, has weakened the reunion effect of particle.
Fig. 2 is the PVA scanning electron microscope image, in contrast group.
Fig. 3 is 2%wt oxygenated black/PVA film SEM image, can observe the oxygenated black particle by image and be scattered in equably in the PVA matrix.
Fig. 4 is 5%wt polyetheramine AC-1830 modified carbon black/PVA film SEM image, can observe AC-1830 modified carbon black particle by image and be scattered in equably in the PVA matrix.
Embodiment
In order to understand the present invention better, introduce the concrete case study on implementation of the present invention below, but content of the present invention is not limited only to following case study on implementation.
Embodiment 1: modified carbon black/PVA film
This film dissolves back casting by quality m part modified carbon black and 100-m part PVA in water under 90 ℃, or in melt temperature (225 ± 10 ℃) following extrusion moulding, wherein 0＜m≤10; Described modified carbon black adopts oxygenated black, long-chain fat amine Soxylat A 25-7 modified carbon black, polyoxyethylene polyoxypropylene ether monoamine modified carbon black, polyoxyethylene polyoxypropylene ether diamine modified carbon black; Described PVA adopts a kind of among PVA-1750, PVA-1778, PVA-1788, the PVA-1798.
Described long-chain fat amine Soxylat A 25-7 modified carbon black can adopt AC-1810 modified carbon black, AC-1830 modified carbon black or AC-1860 modified carbon black.
Described polyoxyethylene polyoxypropylene ether monoamine modified carbon black can adopt M-1000 modified carbon black, M-2005 modified carbon black, M-2070 modified carbon black.
Described polyoxyethylene polyoxypropylene ether diamine modified carbon black can adopt ED-600 modified carbon black, ED-900 modified carbon black, ED-2003 modified carbon black.
Embodiment 2: the preparation of modified carbon black/PVA film
Get 0.5～10 part of oxygenated black powder, add the oxygenated black aqueous dispersions that distilled water is mixed with 1%wt, through magnetic stirrer 30min, add 90～99.5 parts of PVA, adding distilled water to PVA mass concentration is 5%～10%.Begin to heat up by 10 ℃/0.5h from 40 ℃, to 90 ℃ of insulation 2h, stop heating, behind the normal temperature cooling 20min, mixed solution is cast on the sheet glass of smooth cleaning film forming thickness 0.06～0.1mm.The demoulding after steadily leaving standstill 2d under the room temperature obtains oxygenated black/PVA film,
Embodiment 3: the preparation of modified carbon black/PVA film
Get 0.5 part of AC-1830 modified carbon black (oxygenated black and polyetheramine mass ratio 1:m, 0＜m≤10), add the modified carbon black aqueous dispersions that distilled water is mixed with 1%wt, through magnetic stirrer 30min, add 99.5 parts of PVA, adding distilled water to PVA mass concentration is 5%～10%.Begin to heat up by 10 ℃/0.5h from 40 ℃, to 90 ℃ of insulation 2h, stop heating, behind the normal temperature cooling 20min, mixed solution is cast on the sheet glass of smooth cleaning film forming thickness 0.06～0.1mm, the demoulding after steadily leaving standstill 2d under the room temperature obtains AC-1830 modified carbon black (1:m)/PVA film.
Embodiment 4: the preparation of modified carbon black/PVA film
(oxygenated black and polyetheramine mass ratio are 1:m to get 10 parts of M-1000 modified carbon blacks, 0＜m≤10), add the modified carbon black aqueous dispersions that distilled water is mixed with 1%wt, through magnetic stirrer 30min, add 90 parts of PVA, adding distilled water to PVA mass concentration is 5%～10%.Begin to heat up by 10 ℃/0.5h from 40 ℃, to 90 ℃ of insulation 2h, stop heating, behind the normal temperature cooling 20min, mixed solution is cast on the sheet glass of smooth cleaning film forming thickness 0.06～0.1mm, the demoulding after steadily leaving standstill 2d under the room temperature obtains M-1000 modified carbon black (1:m)/PVA film.
Embodiment 5: the preparation of modified carbon black/PVA film
(oxygenated black and polyetheramine mass ratio are 1:m to get 20 parts of M-2070 modified carbon blacks, 0＜m≤10), add the modified carbon black aqueous dispersions that distilled water is mixed with 1%wt, through magnetic stirrer 30min, add 80 parts of PVA, adding distilled water to PVA mass concentration is 5%～10%.Begin to heat up by 10 ℃/0.5h from 40 ℃, to 90 ℃ of insulation 2h, stop heating, behind the normal temperature cooling 20min, mixed solution is cast on the sheet glass of smooth cleaning film forming thickness 0.06～0.1mm, the demoulding after steadily leaving standstill 2d under the room temperature obtains M-2070 modified carbon black (1:m)/PVA film.
Embodiment 6: the preparation of modified carbon black/PVA film
(oxygenated black and polyetheramine mass ratio are 1:m to get 0.5～20 part of ED-600 modified carbon black, 0＜m≤10), add the modified carbon black aqueous dispersions that distilled water is mixed with 1%wt, through magnetic stirrer 30min, add 99.5～80 parts of PVA, adding distilled water to PVA mass concentration is 5%～10%.Begin to heat up by 10 ℃/0.5h from 40 ℃, to 90 ℃ of insulation 2h, stop heating, behind the normal temperature cooling 20min, mixed solution is cast on the sheet glass of smooth cleaning film forming thickness 0.06～0.1mm, the demoulding after steadily leaving standstill 2d under the room temperature obtains E-600 modified carbon black (1:m)/PVA film.
Embodiment 7: the preparation of modified carbon black/PVA film
(oxygenated black and polyetheramine mass ratio are 1:m to get 0.5 part of ED-900 modified carbon black, 0＜m≤10), add the modified carbon black aqueous dispersions that distilled water is mixed with 1%wt, through magnetic stirrer 30min, add 99.5 parts of PVA, adding distilled water to PVA mass concentration is 5%～10%.Begin to heat up by 10 ℃/0.5h from 40 ℃, to 90 ℃ of insulation 2h, stop heating, behind the normal temperature cooling 20min, mixed solution is cast on the sheet glass of smooth cleaning film forming thickness 0.06～0.1mm, the demoulding after steadily leaving standstill 2d under the room temperature obtains ED-900 modified carbon black (1:m)/PVA film.
Embodiment 8: the preparation of modified carbon black/PVA film
(oxygenated black and polyetheramine mass ratio are 1:m to get 10 parts of ED-2003 modified carbon blacks, 0＜m≤10), add the modified carbon black aqueous dispersions that distilled water is mixed with 1%wt, through magnetic stirrer 30min, add 90 parts of PVA, adding distilled water to PVA mass concentration is 5%～10%.Begin to heat up by 10 ℃/0.5h from 40 ℃, to 90 ℃ of insulation 2h, stop heating, behind the normal temperature cooling 20min, mixed solution is cast on the sheet glass of smooth cleaning film forming thickness 0.06～0.1mm, the demoulding after steadily leaving standstill 2d under the room temperature obtains ED-2003(1:m) modified carbon black/PVA film.
Embodiment 9: the preparation of modified carbon black/PVA film
Get 0.5～10 part of oxygenated black and 90～99.5 parts of PVA mix, in forcing machine, melt extrude granulation then.Extrusion temperature: 225 ± 10 ℃, 10～50 rev/mins of rotating speeds.Calendering formation on rolling press at last, rolling temperature is 225 ± 10 ℃, film forming thickness 0.06～0.1mm can obtain oxygenated black/PVA film.
Embodiment 10: the preparation of modified carbon black/PVA film
Get 20 parts of AC-1830 modified carbon blacks (oxygenated black and polyetheramine mass ratio 1:m, 0＜m≤10) and mix with 80 parts of PVA, in forcing machine, melt extrude granulation then.Extrusion temperature: 225 ± 10 ℃, 10～50 rev/mins of rotating speeds.Calendering formation on rolling press at last, temperature is 225 ± 10 ℃, film forming thickness 0.06～0.1mm can obtain AC-1830 modified carbon black (1:m)/PVA film.
Embodiment 11: the preparation of modified carbon black/PVA film
Get 0.5～20 part of M-1000 modified carbon black (oxygenated black and polyetheramine mass ratio 1:m, 0＜m≤10) and mix with 80～99.5 parts of PVA, in forcing machine, melt extrude granulation then.Extrusion temperature: 225 ± 10 ℃, 10～50 rev/mins of rotating speeds.Calendering formation on rolling press at last, temperature is 225 ± 10 ℃, film forming thickness 0.06～0.1mm can obtain M-1000 modified carbon black (1:m)/PVA film.
Embodiment 12: the preparation of modified carbon black/PVA film
Get 0.5 part of M-2070 modified carbon black (oxygenated black and polyetheramine mass ratio 1:m, 0＜m≤10) and mix with 99.5 parts of PVA, in forcing machine, melt extrude granulation then.Extrusion temperature: 225 ± 10 ℃, 10～50 rev/mins of rotating speeds.Calendering formation on rolling press at last, temperature is 225 ± 10 ℃, film forming thickness 0.06～0.1mm can obtain M-2070 modified carbon black (1:m)/PVA film.
Embodiment 13: the preparation of modified carbon black/PVA film
Get 10 parts of E-600 modified carbon blacks (oxygenated black and polyetheramine mass ratio 1:m, 0＜m≤10) and mix with 90 parts of PVA, in forcing machine, melt extrude granulation then.Extrusion temperature: 225 ± 10 ℃, 10～50 rev/mins of rotating speeds.Calendering formation on rolling press at last, temperature is 225 ± 10 ℃, film forming thickness 0.06～0.1mm can obtain E-600 modified carbon black (1:m)/PVA film.
Embodiment 14: the preparation of modified carbon black/PVA film
Get 20 parts of ED-2003 modified carbon blacks (oxygenated black and polyetheramine mass ratio 1:m, 0＜m≤10) and mix with 80 parts of PVA, in forcing machine, melt extrude granulation then.Extrusion temperature: 225 ± 10 ℃, 10～50 rev/mins of rotating speeds.Calendering formation on rolling press at last, temperature is 225 ± 10 ℃, film forming thickness 0.06～0.1mm can obtain ED-2003 modified carbon black (1:m)/PVA film.
Referring to Fig. 1, prepared modified carbon black/PVA film in above-described embodiment, its carbon black particle surface has coated the shell that the one layer of polymeric chain is formed, and has increased the steric hindrance between carbon black particle, has weakened the reunion effect of particle.
Referring to Fig. 2-Fig. 4, prepared modified carbon black/PVA film in above-described embodiment, its modified carbon black particle is scattered in the PVA equably.

Claims (8)

1. modified carbon black/PVA film is characterized in that: this film be by quality m part modified carbon black and 100-m part PVA under 90 ℃ in water dissolving back casting, or in 225 ± 10 ℃ of following extrusion mouldings, wherein 0＜m≤10; Described modified carbon black adopts oxygenated black, long-chain fat amine Soxylat A 25-7 modified carbon black, polyoxyethylene polyoxypropylene ether monoamine modified carbon black, polyoxyethylene polyoxypropylene ether diamine modified carbon black.Described PVA adopts a kind of among PVA-1750, PVA-1778, PVA-1788, the PVA-1798.
2. modified carbon black according to claim 1/PVA film is characterized in that: described long-chain fat amine Soxylat A 25-7 modified carbon black employing AC-1810 modified carbon black, AC-1830 modified carbon black or AC-1860 modified carbon black.
3. modified carbon black according to claim 1/PVA film is characterized in that: described polyoxyethylene polyoxypropylene ether monoamine modified carbon black employing M-1000 modified carbon black, M-2005 modified carbon black, M-2070 modified carbon black.
4. modified carbon black according to claim 1/PVA film is characterized in that: described polyoxyethylene polyoxypropylene ether diamine modified carbon black employing ED-600 modified carbon black, ED-900 modified carbon black or ED-2003 modified carbon black.
5. modified carbon black according to claim 1/PVA film is characterized in that described polyethex amine modification carbon black adopts the polyethex amine modification carbon black of different percentage of grafting.
6. the preparation method of modified carbon black/PVA film, it is characterized in that adopting the casting forming method preparation, specifically: oxygenated black and the polyethex amine modification carbon black with the m mass parts joins in the distilled water respectively, through magnetic stirrer, adds 100-m mass parts PVA again, 0＜m≤10, dissolve fully through gradient increased temperature to polyvinyl alcohol then, stop heating, be cast on the sheet glass after the cooling, the demoulding behind steady placement 2～3d obtains modified carbon black/PVA film under the room temperature.
7. the preparation method of modified carbon black/PVA film, it is characterized in that adopting the extruding forming method preparation, specifically: modified carbon black and the 100-m mass parts PVA of m mass parts are mixed, 0＜m≤10, through the forcing machine extruding pelletization, in extrusion moulding, extrusion temperature is 225 ± 10 ℃, 10～50 rev/mins of rotating speeds obtain modified carbon black/PVA film through calendering formation again.
8. according to the preparation method of claim 6 or 7 described modified carbon black/PVA films, it is characterized in that described modified carbon black made by following method, its step comprises:
Step 1: the nitration mixture of the vitriol oil and concentrated nitric acid 3:1 preparation is by volume joined in the reactor that fills carbon black, in 70 ℃ ultrasonic down, stir 24h, be neutral through dialysing to dialyzate, take out and be placed in the baking oven 80 ℃ of oven dry, make the oxygenated black powder;
Step 2: press mass fraction, get the oxygenated black m in the step 1 1Part is scattered in 100-m 1In part distilled water, get m 2Part polyetheramine is dissolved in 100-m 2In part distilled water, 0＜m 1≤ 10,0＜m 2≤ 50, then the oxygenated black dispersant liquid drop is added in the polyether amine solution, under normal temperature, react 24h, obtain the aqueous dispersions of polyethex amine modification carbon black.
CN2013103183851A 2013-07-26 2013-07-26 Modified carbon black/PVA (polyvinyl alcohol) film and preparation method thereof Pending CN103342869A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103897331A (en) * 2014-04-21 2014-07-02 四川大学 Heat-conducting polyformaldehyde composite material and preparation method thereof
CN109738364A (en) * 2018-12-25 2019-05-10 山东东宏管业股份有限公司 A method of detection carbon black dispersion
CN113292796A (en) * 2021-05-25 2021-08-24 天津蔚领新材料有限公司 Preparation method of high-heat-conductivity ultrahigh molecular weight polyethylene composite material
CN113993637A (en) * 2019-06-11 2022-01-28 日涂表面处理化工有限公司 Hydrophilizing agent and method for forming hydrophilic coating film
CN114213833A (en) * 2021-12-27 2022-03-22 中国科学院兰州化学物理研究所 Preparation method of amine modified carbon black reinforced polyurea composite material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1551906A (en) * 2001-07-27 2004-12-01 莱克斯马克国际公司 Surface modified carbon black
CN101516992A (en) * 2006-08-09 2009-08-26 胡茨曼石油化学公司 Comb-like polyether alkanolamine in ink and paint

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1551906A (en) * 2001-07-27 2004-12-01 莱克斯马克国际公司 Surface modified carbon black
CN101516992A (en) * 2006-08-09 2009-08-26 胡茨曼石油化学公司 Comb-like polyether alkanolamine in ink and paint

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
薛鹏飞: "改性炭黑-聚合物高折射复合材料的制备与性能研究", 《中国博士学位论文全文数据库 工程科技I辑》 *

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103897331A (en) * 2014-04-21 2014-07-02 四川大学 Heat-conducting polyformaldehyde composite material and preparation method thereof
CN103897331B (en) * 2014-04-21 2016-08-17 四川大学 A kind of Heat-conduction polyformaldehyde composite material and preparation method thereof
CN109738364A (en) * 2018-12-25 2019-05-10 山东东宏管业股份有限公司 A method of detection carbon black dispersion
CN113993637A (en) * 2019-06-11 2022-01-28 日涂表面处理化工有限公司 Hydrophilizing agent and method for forming hydrophilic coating film
CN113993637B (en) * 2019-06-11 2023-04-18 日涂表面处理化工有限公司 Hydrophilizing agent and method for forming hydrophilic coating film
CN113292796A (en) * 2021-05-25 2021-08-24 天津蔚领新材料有限公司 Preparation method of high-heat-conductivity ultrahigh molecular weight polyethylene composite material
CN113292796B (en) * 2021-05-25 2022-08-23 深圳市鹏塑科技发展有限公司 Preparation method of high-heat-conductivity ultrahigh molecular weight polyethylene composite material
CN114213833A (en) * 2021-12-27 2022-03-22 中国科学院兰州化学物理研究所 Preparation method of amine modified carbon black reinforced polyurea composite material

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