CN106987227A - A kind of isocyanation esterification Carbon Black/polyurethane Conductive sealant and preparation method thereof - Google Patents
A kind of isocyanation esterification Carbon Black/polyurethane Conductive sealant and preparation method thereof Download PDFInfo
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- CN106987227A CN106987227A CN201710259533.5A CN201710259533A CN106987227A CN 106987227 A CN106987227 A CN 106987227A CN 201710259533 A CN201710259533 A CN 201710259533A CN 106987227 A CN106987227 A CN 106987227A
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- carbon black
- polyurethane
- isocyanation esterification
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- 239000006229 carbon black Substances 0.000 title claims abstract description 51
- 239000004814 polyurethane Substances 0.000 title claims abstract description 34
- 230000032050 esterification Effects 0.000 title claims abstract description 29
- 238000005886 esterification reaction Methods 0.000 title claims abstract description 29
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 28
- 239000000565 sealant Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000012948 isocyanate Substances 0.000 claims abstract description 20
- 238000010301 surface-oxidation reaction Methods 0.000 claims abstract description 13
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 11
- 229920000642 polymer Polymers 0.000 claims abstract description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229920005549 butyl rubber Polymers 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 7
- 230000005684 electric field Effects 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 229920001730 Moisture cure polyurethane Polymers 0.000 claims abstract description 6
- 230000000694 effects Effects 0.000 claims abstract description 5
- 239000005056 polyisocyanate Substances 0.000 claims abstract description 5
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 5
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 5
- 235000019241 carbon black Nutrition 0.000 claims description 45
- 238000006243 chemical reaction Methods 0.000 claims description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- 239000007800 oxidant agent Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical class CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical class CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 3
- 238000009835 boiling Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 229920001451 polypropylene glycol Polymers 0.000 claims description 3
- 238000010992 reflux Methods 0.000 claims description 3
- 238000002390 rotary evaporation Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical class CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 claims 1
- 238000007789 sealing Methods 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 125000002462 isocyano group Chemical group *[N+]#[C-] 0.000 abstract description 3
- 239000004588 polyurethane sealant Substances 0.000 abstract description 3
- 239000011231 conductive filler Substances 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- 239000000376 reactant Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000002322 conducting polymer Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- XLJMAIOERFSOGZ-UHFFFAOYSA-N cyanic acid Chemical compound OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- 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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
- C09J175/08—Polyurethanes from polyethers
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
- C08G18/6674—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203
- C08G18/6677—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/3203 having at least three hydroxy groups
-
- 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
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
-
- 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
- C08K3/04—Carbon
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- 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
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of isocyanation esterification Carbon Black/polyurethane Conductive sealant, carbon black is carried out surface oxidation treatment by its preparation first, toluene di-isocyanate(TDI) is reused by its isocyanate functional groupization, then the copolyreaction of polyalcohol and polyisocyanates is participated in, obtain isocyanation esterification Carbon Black/polyurethane performed polymer, Conductive sealant is mixed to prepare with liquid butyl rubber etc. afterwards, the effect with uniform electric field.Carbon blacksurface of the present invention is grafted with isocyano, participate in polyurethane prepolymer precursor reactant, improve compatibility of the conductive filler carbon black in polyurethane sealant, it is dispersed in Conductive sealant, the uneven of electric field in cable can effectively be reduced, other carbon black can be in filled polyurethane sealant layer space so that the adhesive property of Conductive sealant is enhanced.
Description
Technical field
The present invention relates to a kind of fluid sealant, and in particular to a kind of isocyanation esterification Carbon Black/polyurethane Conductive sealant and its
Preparation method.
Background technology
Conducting polymer materials are an important branch of functional material.With industries such as electronics industry and information technologies
Develop rapidly, the demand for the polymeric material with conducting function is more and more urgent.Because conducting polymer materials have
Light weight, easy processing into various complicated shapes, good stability of the dimension and resistivity interior adjustable in a big way the features such as, thus
It is widely used in the fields such as antistatic, conduction, electromagnetic shielding and electrochemistry.
Polyurethane（PU）Adhesive is the height for the unique energy that a class is produced by polyisocyanates and polyol reaction
Polymers, because with good lower temperature resistance, chemical resistance, rub resistance and the features such as pliability, therefore its application compared with
To be extensive.But, PU is a kind of insulating materials in itself, and its antistatic behaviour and electric conductivity are poor, so that its application field
Expansion is restricted.
Xi Xiangrong, Yu Chaosheng et al. are at it《The preparation of reduced nano graphite/conductive polyurethane glue and performance study》One text
In, three kinds of different base polyurethane prepolymer for use as of performance are produced under different reaction conditions using isocyanates and polyalcohol（PUⅠ、
PUⅡAnd PUⅢ）, three kinds of PU conducting resinls, its electric conductivity are then mixed with reduced nano graphite, trimethylolpropane respectively
It is significantly improved with mechanical property.But the direct filling of its graphite is added, with polyurethane matrix poor compatibility, easily occurs group
It is poly-, cause the inhomogeneities of electric field in cable.
The content of the invention
In view of the shortcomings of the prior art, the present invention provide a kind of isocyanation esterification Carbon Black/polyurethane Conductive sealant and its
Preparation method.
Carbon black is carried out surface oxidation treatment by a kind of isocyanation esterification Carbon Black/polyurethane Conductive sealant, its preparation first,
Toluene di-isocyanate(TDI) is reused by its isocyanate functional groupization, polyalcohol is then participated in and the copolymerization of polyisocyanates is anti-
Should, isocyanation esterification Carbon Black/polyurethane performed polymer is obtained, Conductive sealant is mixed to prepare with liquid butyl rubber etc. afterwards, had
There is the effect of uniform electric field.
Comprise the following steps that：
（1）The surface oxidation treatment of carbon black：
10-16 parts of carbon blacks and 55-70 parts of oxidants are added in three-necked flask, mechanical agitation, oil bath heating, at 75-85 DEG C
At a temperature of react 8-11 hour, reaction terminate after, be cooled to room temperature, filtering, deionized water cyclic washing is used, in filtrate is in
Property untill, finally by filter residue at 70-85 DEG C dry, produce Surface Oxidation Modification carbon black；
（2）The isocyanate functional groupization of carbon blacksurface：
Above-mentioned Surface Oxidation Modification carbon black, 35-40 parts of toluene di-isocyanate(TDI)s are added in three-necked flask, toluene is solvent, machine
Tool is stirred, and is added 2-6 parts of triethylamines and is made acid binding agent, ice bath reacts 25-35 minutes, 110-130 DEG C of continuation is heated slowly to afterwards
Reaction 20-30 minutes, reaction product removes unreacted isocyanates in 80 DEG C of rotary evaporations, produces isocyanation esterification carbon black；
（3）The preparation of isocyanation esterification Carbon Black/polyurethane performed polymer：
In the four-hole boiling flask equipped with electric mixer, reflux condensing tube and thermometer, 65-80 parts of polypropylene glycols 2000 are added,
Vacuumized in 80-100 DEG C and slough moisture, be cooled to 55-65 DEG C, 40-55 parts of toluene diisocyanates are then added under nitrogen protection
Acid esters and step（2）Isocyanation esterification carbon black, temperature control reacts 4-6 hours, and isocyanation esterification Carbon Black/polyurethane performed polymer is made；
（4）The preparation of isocyanation esterification Carbon Black/polyurethane Conductive sealant：
8-20 parts of liquid butyl rubbers are added in above-mentioned base polyurethane prepolymer for use as, control temperature adds 2-7 under the conditions of 45-55 DEG C
Part dibutyl tin laurate, 2-9 parts of trimethylolpropanes, are mixed 5-25 minutes after being well mixed on three-roll grinder, envelope
Dress storage.
Wherein, described oxidant is mixed by the concentrated sulfuric acid with hydrogen peroxide constitutes, and wherein the consumption of the concentrated sulfuric acid is 65-70%.
Wherein, described step（3）Middle controlling reaction temperature is at 60-70 DEG C.
Compared with prior art, the present invention has advantages below：
（1）Carbon black is carried out surface oxidation treatment by the present invention first by the concentrated sulfuric acid and hydrogen peroxide mixture as oxidant,
With the intensification of degree of oxidation, the oxy radical of carbon blacksurface is lifted, and is generated weakly acidic hydroxyl, can effectively be solved nanoparticle
The cluster states of son, afterwards using the hydroxyl of nanoparticle surface, react with the contraposition isocyano of toluene di-isocyanate(TDI),
Carbon blacksurface is grafted with isocyano, participate in polyurethane prepolymer precursor reactant, improve conductive filler carbon black in polyurethane seal
Compatibility in glue, is dispersed in Conductive sealant, can effectively reduce the uneven of electric field in cable.
（2）Contacted in fluid sealant of the present invention between conductive carbon black filler and overlap it is compact, and in Conductive sealant formed
Continuous conductive path, so that Conductive sealant is conductive, system is changed into conductor from insulator, and carbon blacksurface is different in addition
Key and effect occur for cyanate radical active group and polyurethane macromolecular, the space that carbon black can be in filled polyurethane sealant layer, from
And it is enhanced the adhesive property of Conductive sealant.
Embodiment
Carbon black is carried out surface oxidation treatment by a kind of isocyanation esterification Carbon Black/polyurethane Conductive sealant, its preparation first,
Toluene di-isocyanate(TDI) is reused by its isocyanate functional groupization, polyalcohol is then participated in and the copolymerization of polyisocyanates is anti-
Should, isocyanation esterification Carbon Black/polyurethane performed polymer is obtained, Conductive sealant is mixed to prepare with liquid butyl rubber etc. afterwards, had
There is the effect of uniform electric field.
Comprise the following steps that：
（1）The surface oxidation treatment of carbon black：
15 parts of carbon blacks and 60 parts of oxidants are added in three-necked flask, mechanical agitation, oil bath heating, reacted at a temperature of 80 DEG C
10 hours, after reaction terminates, room temperature is cooled to, filters, uses deionized water cyclic washing, untill filtrate is in neutrality, finally
By filter residue in being dried at 80 DEG C, Surface Oxidation Modification carbon black is produced；
（2）The isocyanate functional groupization of carbon blacksurface：
Above-mentioned Surface Oxidation Modification carbon black, 35 parts of toluene di-isocyanate(TDI)s are added in three-necked flask, toluene is solvent, and machinery is stirred
Mix, add 3 parts of triethylamines and make acid binding agent, ice bath reacts 30 minutes, 120 DEG C are heated slowly to afterwards and continues reaction 25 minutes, instead
Answer product to remove unreacted isocyanates in 80 DEG C of rotary evaporations, produce isocyanation esterification carbon black；
（3）The preparation of isocyanation esterification Carbon Black/polyurethane performed polymer：
In the four-hole boiling flask equipped with electric mixer, reflux condensing tube and thermometer, 75 parts of polypropylene glycols 2000 are added, in 90
DEG C vacuumize and to slough moisture, be cooled to 60 DEG C, 46 parts of toluene di-isocyanate(TDI)s and step are then added under nitrogen protection（2）It is different
Cyanic acid is esterified carbon black, and temperature control reacts 5 hours, and isocyanation esterification Carbon Black/polyurethane performed polymer is made；
（4）The preparation of isocyanation esterification Carbon Black/polyurethane Conductive sealant：
12 parts of liquid butyl rubbers are added in above-mentioned base polyurethane prepolymer for use as, control temperature adds 4 parts of February under the conditions of 50 DEG C
Dilaurylate, 6 parts of trimethylolpropanes, are mixed 15 minutes after being well mixed on three-roll grinder, encapsulation storage.
Wherein, described oxidant is mixed by the concentrated sulfuric acid with hydrogen peroxide constitutes, and wherein the consumption of the concentrated sulfuric acid is 65-70%.
Wherein, described step（3）Middle controlling reaction temperature is at 60-70 DEG C.
Claims (4)
1. a kind of isocyanation esterification Carbon Black/polyurethane Conductive sealant, it is characterised in that carbon black is carried out surface by its preparation first
Oxidation processes, reuse toluene di-isocyanate(TDI) by its isocyanate functional groupization, then participate in polyalcohol and polyisocyanates
Copolyreaction, obtain isocyanation esterification Carbon Black/polyurethane performed polymer, be mixed to prepare afterwards with liquid butyl rubber etc. conductive close
Sealing, the effect with uniform electric field.
2. a kind of preparation method of isocyanation esterification Carbon Black/polyurethane Conductive sealant according to claims 1, it is special
Levy and be, comprise the following steps that：
（1）The surface oxidation treatment of carbon black：
10-16 parts of carbon blacks and 55-70 parts of oxidants are added in three-necked flask, mechanical agitation, oil bath heating, at 75-85 DEG C
At a temperature of react 8-11 hour, reaction terminate after, be cooled to room temperature, filtering, deionized water cyclic washing is used, in filtrate is in
Property untill, finally by filter residue at 70-85 DEG C dry, produce Surface Oxidation Modification carbon black；
（2）The isocyanate functional groupization of carbon blacksurface：
Above-mentioned Surface Oxidation Modification carbon black, 35-40 parts of toluene di-isocyanate(TDI)s are added in three-necked flask, toluene is solvent, machine
Tool is stirred, and is added 2-6 parts of triethylamines and is made acid binding agent, ice bath reacts 25-35 minutes, 110-130 DEG C of continuation is heated slowly to afterwards
Reaction 20-30 minutes, reaction product removes unreacted isocyanates in 80 DEG C of rotary evaporations, produces isocyanation esterification carbon black；
（3）The preparation of isocyanation esterification Carbon Black/polyurethane performed polymer：
In the four-hole boiling flask equipped with electric mixer, reflux condensing tube and thermometer, 65-80 parts of polypropylene glycols 2000 are added,
Vacuumized in 80-100 DEG C and slough moisture, be cooled to 55-65 DEG C, 40-55 parts of toluene diisocyanates are then added under nitrogen protection
Acid esters and step（2）Isocyanation esterification carbon black, temperature control reacts 4-6 hours, and isocyanation esterification Carbon Black/polyurethane performed polymer is made；
（4）The preparation of isocyanation esterification Carbon Black/polyurethane Conductive sealant：
8-20 parts of liquid butyl rubbers are added in above-mentioned base polyurethane prepolymer for use as, control temperature adds 2-7 under the conditions of 45-55 DEG C
Part dibutyl tin laurate, 2-9 parts of trimethylolpropanes, are mixed 5-25 minutes after being well mixed on three-roll grinder, envelope
Dress storage.
3. a kind of preparation method of isocyanation esterification Carbon Black/polyurethane Conductive sealant according to claims 1,2, its
It is characterised by, described oxidant is mixed by the concentrated sulfuric acid with hydrogen peroxide to be constituted, wherein the consumption of the concentrated sulfuric acid is 65-70%.
4. a kind of preparation method of isocyanation esterification Carbon Black/polyurethane Conductive sealant according to claims 2, it is special
Levy and be, described step（3）Middle controlling reaction temperature is at 60-70 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710259533.5A CN106987227A (en) | 2017-04-20 | 2017-04-20 | A kind of isocyanation esterification Carbon Black/polyurethane Conductive sealant and preparation method thereof |
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| CN201710259533.5A CN106987227A (en) | 2017-04-20 | 2017-04-20 | A kind of isocyanation esterification Carbon Black/polyurethane Conductive sealant and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108192230A (en) * | 2018-02-05 | 2018-06-22 | 罗宇强 | The infrared reinforced plastics of television set |
| CN115181435A (en) * | 2022-06-28 | 2022-10-14 | 江南大学 | Surface modification method of carbon black flame-retardant pigment for in-situ polymerization polyester chip |
| CN115262272A (en) * | 2022-07-26 | 2022-11-01 | 中南大学 | Preparation method of impregnating resin material for densifying carbon fiber paper |
| CN115926665A (en) * | 2022-12-30 | 2023-04-07 | 郑州郑大可飞科技有限公司 | Elastic self-adhesive conductive sealing gasket with composite structure and preparation method thereof |
| CN117487279A (en) * | 2023-11-02 | 2024-02-02 | 迁安益昌电子材料有限公司 | Rubber composition and preparation method thereof and electromagnetic shielding sealing material |
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| CN105566699A (en) * | 2016-03-10 | 2016-05-11 | 安徽海源特种电缆有限公司 | High-strength and oil-resistant electric power cable |
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| CN104817995A (en) * | 2015-05-20 | 2015-08-05 | 叶芳 | Novel polyurethane conductive adhesive and preparation method thereof |
| CN105566699A (en) * | 2016-03-10 | 2016-05-11 | 安徽海源特种电缆有限公司 | High-strength and oil-resistant electric power cable |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108192230A (en) * | 2018-02-05 | 2018-06-22 | 罗宇强 | The infrared reinforced plastics of television set |
| CN115181435A (en) * | 2022-06-28 | 2022-10-14 | 江南大学 | Surface modification method of carbon black flame-retardant pigment for in-situ polymerization polyester chip |
| CN115181435B (en) * | 2022-06-28 | 2024-03-01 | 江南大学 | Surface modification method of carbon black flame-retardant pigment for in-situ polymerization polyester chip |
| CN115262272A (en) * | 2022-07-26 | 2022-11-01 | 中南大学 | Preparation method of impregnating resin material for densifying carbon fiber paper |
| CN115926665A (en) * | 2022-12-30 | 2023-04-07 | 郑州郑大可飞科技有限公司 | Elastic self-adhesive conductive sealing gasket with composite structure and preparation method thereof |
| CN115926665B (en) * | 2022-12-30 | 2024-05-10 | 郑州郑大可飞科技有限公司 | Elastic self-adhesive conductive sealing gasket with composite structure and preparation method thereof |
| CN117487279A (en) * | 2023-11-02 | 2024-02-02 | 迁安益昌电子材料有限公司 | Rubber composition and preparation method thereof and electromagnetic shielding sealing material |
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