CN107337825B - A kind of preparation method of yielding rubber - Google Patents
A kind of preparation method of yielding rubber Download PDFInfo
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- CN107337825B CN107337825B CN201710641922.4A CN201710641922A CN107337825B CN 107337825 B CN107337825 B CN 107337825B CN 201710641922 A CN201710641922 A CN 201710641922A CN 107337825 B CN107337825 B CN 107337825B
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 66
- 239000005060 rubber Substances 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000003365 glass fiber Substances 0.000 claims abstract description 58
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 27
- 239000004014 plasticizer Substances 0.000 claims abstract description 22
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920000459 Nitrile rubber Polymers 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000004202 carbamide Substances 0.000 claims abstract description 16
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000005864 Sulphur Substances 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 11
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 11
- 229960003638 dopamine Drugs 0.000 claims abstract description 9
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 9
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 10
- YXIWHUQXZSMYRE-UHFFFAOYSA-N 1,3-benzothiazole-2-thiol Chemical compound C1=CC=C2SC(S)=NC2=C1 YXIWHUQXZSMYRE-UHFFFAOYSA-N 0.000 claims description 7
- 239000003963 antioxidant agent Substances 0.000 claims description 7
- 230000003078 antioxidant effect Effects 0.000 claims description 7
- ZZMVLMVFYMGSMY-UHFFFAOYSA-N 4-n-(4-methylpentan-2-yl)-1-n-phenylbenzene-1,4-diamine Chemical compound C1=CC(NC(C)CC(C)C)=CC=C1NC1=CC=CC=C1 ZZMVLMVFYMGSMY-UHFFFAOYSA-N 0.000 claims description 6
- 238000004073 vulcanization Methods 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 3
- ZFMQKOWCDKKBIF-UHFFFAOYSA-N bis(3,5-difluorophenyl)phosphane Chemical compound FC1=CC(F)=CC(PC=2C=C(F)C=C(F)C=2)=C1 ZFMQKOWCDKKBIF-UHFFFAOYSA-N 0.000 claims description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 2
- FIBARIGPBPUBHC-UHFFFAOYSA-N octyl 8-(3-octyloxiran-2-yl)octanoate Chemical compound CCCCCCCCOC(=O)CCCCCCCC1OC1CCCCCCCC FIBARIGPBPUBHC-UHFFFAOYSA-N 0.000 claims description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims 2
- 235000005128 Sapium sebiferum Nutrition 0.000 claims 1
- 244000057114 Sapium sebiferum Species 0.000 claims 1
- 239000006185 dispersion Substances 0.000 claims 1
- 238000007654 immersion Methods 0.000 claims 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims 1
- 238000001914 filtration Methods 0.000 abstract description 9
- 238000005406 washing Methods 0.000 abstract description 5
- 239000004926 polymethyl methacrylate Substances 0.000 abstract description 4
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 2
- 239000002861 polymer material Substances 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract description 2
- 230000032683 aging Effects 0.000 description 17
- 239000000463 material Substances 0.000 description 14
- 239000000047 product Substances 0.000 description 14
- 238000013016 damping Methods 0.000 description 10
- 238000007599 discharging Methods 0.000 description 9
- 238000012360 testing method Methods 0.000 description 6
- 239000011152 fibreglass Substances 0.000 description 5
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000012065 filter cake Substances 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 244000043261 Hevea brasiliensis Species 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 3
- 229920003052 natural elastomer Polymers 0.000 description 3
- 229920001194 natural rubber Polymers 0.000 description 3
- 230000035939 shock Effects 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 230000001133 acceleration Effects 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical class [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 150000004702 methyl esters Chemical class 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- -1 poly-methyl methacrylates Chemical class 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- IMYZYCNQZDBZBQ-UHFFFAOYSA-N (+-)-8-(cis-3-octyl-oxiranyl)-octanoic acid Natural products CCCCCCCCC1OC1CCCCCCCC(O)=O IMYZYCNQZDBZBQ-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- GJCOSYZMQJWQCA-UHFFFAOYSA-N 9H-xanthene Chemical compound C1=CC=C2CC3=CC=CC=C3OC2=C1 GJCOSYZMQJWQCA-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 1
- 230000003679 aging effect Effects 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 description 1
- 235000014413 iron hydroxide Nutrition 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000615 nonconductor Substances 0.000 description 1
- 239000008601 oleoresin Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920001596 poly (chlorostyrenes) Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 239000012763 reinforcing filler Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 229920001285 xanthan gum Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L15/00—Compositions of rubber derivatives
- C08L15/005—Hydrogenated nitrile rubber
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Reinforced Plastic Materials (AREA)
Abstract
The invention discloses a kind of preparation methods of yielding rubber, belong to technical field of polymer materials.The present invention first impregnates glass fibre with dopamine solution, pretreated glass fiber is made, glass fibre is uniformly mixed with ferric chloride solution again, and precipitating reagent urea liquid is added dropwise, after reaction, it is aged, filtering, washing and dry modified glass-fiber, then hydrogenated nitrile-butadiene rubber is plasticated, sequentially add polymethyl methacrylate, Corvic, Petropols, modified glass-fiber, sulphur, promotor, anti-aging agent and plasticizer, it is kneaded, and apply external magnetic field in mixing process, rubber compound is obtained after stewing process, finally rubber compound is heated and is vulcanized, up to yielding rubber.Gained yielding rubber of the invention has both excellent stability and mechanical property, and service life is long compared with conventional base rubber, and mechanical property keeps good.
Description
Technical field
The invention discloses a kind of preparation methods of yielding rubber, belong to technical field of polymer materials.
Background technique
Damping mechanical equipment, railroad track, ship, bridge, in terms of have important use.Especially in recent years
Come, earthquake frequently occurs, directly or indirectly to society and damage naturally so that damping is particularly important.In damping
In material, rubber is played an increasingly important role, and is the direction of vibration-absorptive material development.The characteristics of rubber is existing high-elastic
Property, and have high viscosity, and there are also its distinctive comprehensive mechanical property, i.e., low adjustable modulus and higher intrinsic resistances
Buddhist nun keeps its effect in terms of buffering, damping and dynamic sealing unrivaled.The shock absorption principle of rubber product utilizes rubber
High viscosity absorbs vibrational energy, and the mechanical energy of absorption or sound can be partially converted into thermal energy and dissipated, and subtracts to play
Less or reduce amplitude effect.
The morphosis because being known as rubber material, the blend rubber system each component of rubber damping damping performance are influenced at present
Compatibility, cross-linking system, use temperature and vibration frequency, polymer blending ratio, reinforcing filler and other auxiliary agents etc..
Natural rubber (NR) is the product of biosynthesis, and main component is rubber hydrocarbon, also containing a small amount of protein, fatty acid etc..Its
Processing method is a variety of, and the component content of obtained various NR is different, and mechanical property, damping performance etc. are also variant, in relation to this
The research of aspect is very few.
It is set as the heavy constructions such as damper element, especially senior constructure, bridge, internal combustion engine, train head or machinery
Standby foundation shock absorption element, relatively difficult due to installing and replacing, costly, product, which generally requires to have, longer uses the longevity
Life, to reduce maintenance and renewal cost.In the various factors for influencing shock absorbing rubber product service life, thermo-oxidative ageing is most heavy
One of factor wanted.This is because rubber itself is the non-conductor of heat, the mechanical energy that damping is absorbed is after being converted into thermal energy
It cannot be dissipated in time, therefore rubber will heat up, and the raising of temperature is in addition to declining the performance of rubber product, it is more main
What is wanted is the thermo-oxidative ageing process that will greatly accelerate rubber product, so as to shorten its service life.Therefore, as can inhibiting rubber
Thermo-oxidative ageing process, can improve the heat aging property of rubber product, to extend the service life of product.
Summary of the invention
The present invention solves the technical problem of: in use for conventional base rubber material, damping is inhaled
The mechanical energy of receipts cannot be dissipated in time after being converted into thermal energy, accelerate the thermo-oxidative ageing of rubber, lead to product service life
Shorter problem provides a kind of preparation method of yielding rubber.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
(1) glass fibre is mixed for 1:50~1:80 in mass ratio with dopamine solution and impregnates 45~60min, using
Filter, obtains pretreated glass fiber;
It (2) is in mass ratio that 1:30~1:40 mixes addition reactor with ferric chloride solution by pretreated glass fiber, point
After dissipating uniformly, then 2~3 times of ferric chloride solution volume of urea liquid is added dropwise into reactor, wait be added dropwise, the reaction was continued 3
~5h, then it is aged, be filtered, washed and dried to obtain modified glass-fiber;
(3) according to parts by weight, 100~120 parts of hydrogenated nitrile-butadiene rubbers, 10~15 parts of poly-methyl methacrylates are successively taken
Ester, 8~10 parts of Corvics, 8~10 parts of Petropols, 10~20 parts of modified glass-fibers, 3~5 parts of sulphur, 1~3 part
Hydrogenated nitrile-butadiene rubber is first plasticated after 10~15min, is sequentially added poly- by promotor, 2~4 parts of anti-aging agents, 1~4 part of plasticizer
Methyl methacrylate, Corvic, Petropols, modified glass-fiber, sulphur, promotor, anti-aging agent and plasticizer,
After being kneaded 10~20min, and apply external magnetic field in mixing process, end to be mixed stands 6~8h, obtains rubber compound;
(4) mixing glue is heated into 45~60min of vulcanization, discharged to get yielding rubber.
Step (1) glass fibre is any one in alkali-free glass fibre or medium-alkali glass fibre.
Step (3) Petropols are any one in C5 Petropols or C9 Petropols.
Step (3) promotor is any one in Vulcanization accelerator TMTD, captax or promotor ZDMC.
Step (3) described anti-aging agent is mixed in mass ratio for 1:1:1 by antioxidant 4020, anti-aging agent RD and antioxidant NBC
It closes.
Step (3) the plasticizer is in dibutyl phthalate, octyl epoxy stearate or dioctyl adipate
Any one.
The beneficial effects of the present invention are: (1) technical solution of the present invention carries out glass fibre first with dopamine solution
It impregnates and is modified, improve the absorption property of glass fibre, then modified glass fibre is mixed with ferric chloride solution, be with urea
Precipitating reagent, make hydrolysis of urea generate hydroxide ion with iron ion in conjunction with, generation iron hydroxide nucleus, nucleus once being formed,
It is adsorbed by the dopamine of fiberglass surfacing, in subsequent processes, iron hydroxide dehydration generates iron oxide, and aoxidizes
Iron uniform adsorption improves the roughness of fiberglass surfacing in fiberglass surfacing, is conducive in subsequent processes linear
Rubber molecule, which is affiliated to, is wound in coarse fiberglass surfacing, in by vibration deformation process, can effectively improve rubber molecular chain
The resistance of motion steeply rises system internal friction, converts the mechanical energy that vibration generates to thermal energy and dissipate, at the same by
During power, glass fibre can share jointly external force with rubber molecular chain, disperse stress, play reinforcing effect, avoid system
Stress is concentrated and causes structure and elastic change dramatically, effectively limits the large scale deformation of product under external force, makes product
Mechanical property is further promoted, in addition, after iron oxide is adsorbed on fiberglass surfacing, it can be in process with externally-applied magnetic field side
To the enhancing network structure for making glass fibre form oriented alignment in rubber matrix, to effectively improve the thermal conductivity of system
Can, the thermal energy fast dissipation that conversion is formed avoids thermal energy buildup from causing rubber thermo-oxidative ageing inside system;(2) of the invention
Technical solution can increase rubber by adding polymethyl methacrylate, Corvic and Petropols in rubbery system
The polarity of xanthan molecule improves cohesive strength and surface energy, in addition, the addition of Petropols, can effectively improve system to glass fibers
The wettability of dimension effectively improves product mechanical performance to improve the binding force between system and glass fibre;
(3) technical solution of the present invention, can after nitrile rubber hydrogenation treatment using hydrogenated nitrile-butadiene rubber as base rubber material
The unstable double bond in rubber molecule is effectively reduced, so that effectively reduce rubber molecule occurs deterioration by oxidation under heating condition
Problem.
Specific embodiment
It is in mass ratio 1:50~1:80 by glass fibre and mass concentration is that 2g/L dopamine solution mixes and pours into beaker
In, and beaker immigration digital display constant temperature is tested the speed magnetic stirring apparatus, it is 55~65 DEG C in temperature, revolving speed is 300~500r/min item
Under part, constant temperature is stirred 45~60min, and filtering obtains filter cake, as pretreated glass fiber;Gained pretreated glass is fine
Dimension with mass fraction be 8~10% ferric chloride solutions be in mass ratio 1:30~1:40 be added reaction kettle in, in temperature be 45~55
DEG C, revolving speed be 400~600r/min under the conditions of, after constant temperature is dispersed with stirring 45~60min, then into reaction kettle be added dropwise iron chloride it is molten
The mass fraction of 2~3 times of liquid product is 10~15% urea liquids, and control urea liquid drop rate is 8~10mL/min, to
Urea liquid is added dropwise, and continues constant temperature and is stirred to react 3~5h, to the end of reacting, material in reaction kettle is transferred to ageing tank, in
Still aging 8~12h under room temperature, filtering, obtains filter residue, and be washed with deionized filter residue 3~5 times, then will be after washing
Filter residue is transferred in baking oven, is dried under the conditions of being 105~110 DEG C in temperature to constant weight, is obtained modified glass-fiber;In parts by weight
Meter, successively takes 100~120 parts of hydrogenated nitrile-butadiene rubbers, 10~15 parts of polymethyl methacrylates, 8~10 parts of Corvics,
8~10 parts of Petropols, 10~20 parts of modified glass-fibers, 3~5 parts of sulphur, 1~3 part of promotor, 2~4 parts of anti-aging agents, 1~
Hydrogenated nitrile-butadiene rubber, is first placed in open mill by 4 parts of plasticizer, and under the conditions of temperature is 40~80 DEG C, plasticate 10~15min,
It sequentially adds polymethyl methacrylate, Corvic, Petropols, modified glass-fiber, sulphur, promotor, prevent
Old agent and plasticizer are kneaded 5~15min under the conditions of being 130~160 DEG C in temperature, in mixing process, to material in open mill
Applying the external magnetic field that intensity is 40~50T, end to be mixed, discharging obtains rubber compound then at 6~8h is stood under room temperature, and
Gained rubber compound is transferred in vulcanizing press, is 180~200 DEG C in temperature, under the conditions of pressure is 20~30MPa, vulcanizes 45
~60min, discharging, is cooled to room temperature to get yielding rubber.The glass fibre is alkali-free glass fibre or middle alkali glass fiber
Any one in dimension.The Petropols are any one in C5 Petropols or C9 Petropols.The promotor is
Any one in Vulcanization accelerator TMTD, captax or promotor ZDMC.The anti-aging agent is by antioxidant 4020, anti-aging agent RD
It is mixed in mass ratio for 1:1:1 with antioxidant NBC.The plasticizer is dibutyl phthalate, epoxystearic acid is pungent
Any one in ester or dioctyl adipate.
Example 1
It is in mass ratio 1:60 by alkali-free glass fibre and mass concentration is that 2g/L dopamine solution is mixed and poured into beaker,
And beaker immigration digital display constant temperature is tested the speed magnetic stirring apparatus, in temperature be 60 DEG C, under the conditions of revolving speed is 400r/min, constant temperature stirring
60min is mixed, filtering obtains filter cake, as pretreated glass fiber;It is 10% by gained pretreated glass fiber and mass fraction
Ferric chloride solution is that 1:40 is added in reaction kettle in mass ratio, is 50 DEG C in temperature, under the conditions of revolving speed is 400r/min, constant temperature is stirred
It mixes after dispersing 60min, then 2 times of ferric chloride solution volume of mass fraction is added dropwise as 10% urea liquid into reaction kettle, control is urinated
Plain solution drop rate is 10mL/min, is added dropwise to urea liquid, continues constant temperature and is stirred to react 3h, will to the end of reacting
Material is transferred to ageing tank in reaction kettle, and in still aging 8h under room temperature, filtering obtains filter residue, and filter is washed with deionized
Slag 3 times, then the filter residue after washing is transferred in baking oven, it dries under the conditions of being 100 DEG C in temperature to constant weight, obtains modified glass fibre
Dimension;According to parts by weight, 100 parts of hydrogenated nitrile-butadiene rubbers, 10 parts of polymethyl methacrylates, 10 parts of polyvinyl chloride trees are successively taken
Rouge, 10 parts of C5 Petropols, 10 parts of modified glass-fibers, 3 parts of sulphur, 3 parts of captaxes, 3 parts of anti-aging agents, 2 parts of plasticizer, first
Hydrogenated nitrile-butadiene rubber is placed in open mill, under the conditions of temperature is 40 DEG C, plasticate 10min, sequentially adds polymethyl
Sour methyl esters, Corvic, C5 Petropols, modified glass-fiber, sulphur, captax, anti-aging agent and plasticizer, Yu Wen
Degree is kneaded 10min under the conditions of being 150 DEG C, in mixing process, applies the external magnetic field that intensity is 50T to material in open mill, to
Mixing terminates, and discharging then at 8h is stood under room temperature, obtains rubber compound, and gained rubber compound is transferred in vulcanizing press, in
Temperature is 200 DEG C, under the conditions of pressure is 30MPa, vulcanizes 60min, discharging is cooled to room temperature to get yielding rubber.It is described anti-
Old agent is mixed in mass ratio for 1:1:1 by antioxidant 4020, anti-aging agent RD and antioxidant NBC.The plasticizer is neighbour
Dibatyl phithalate.
Example 2
According to parts by weight, 100 parts of hydrogenated nitrile-butadiene rubbers, 10 parts of polymethyl methacrylates, 10 parts of polychlorostyrene second are successively taken
Olefine resin, 10 parts of C5 Petropols, 10 parts of glass fibres, 3 parts of sulphur, 3 parts of captaxes, 3 parts of anti-aging agents, 2 parts of plasticizer, first
Hydrogenated nitrile-butadiene rubber is placed in open mill, under the conditions of temperature is 40 DEG C, plasticate 10min, sequentially adds polymethyl
Sour methyl esters, Corvic, C5 Petropols, glass fibre, sulphur, captax, anti-aging agent and plasticizer are in temperature
It is kneaded 10min under the conditions of 150 DEG C, in mixing process, the external magnetic field that intensity is 50T is applied to material in open mill, it is to be mixed
Terminate, discharging then at 8h is stood under room temperature, obtains rubber compound, and gained rubber compound is transferred in vulcanizing press, in temperature
It is 200 DEG C, under the conditions of pressure is 30MPa, vulcanizes 60min, discharging is cooled to room temperature to get yielding rubber.The anti-aging agent
It is to be mixed in mass ratio for 1:1:1 by antioxidant 4020, anti-aging agent RD and antioxidant NBC.The plasticizer is adjacent benzene two
Formic acid dibutyl ester.
Example 3
In mass ratio to be 1:60 by glass fibre and mass concentration be, and 2g/L dopamine solution is mixed and is poured into beaker, and will
Beaker moves into digital display constant temperature and tests the speed magnetic stirring apparatus, is 60 DEG C in temperature, under the conditions of revolving speed is 400r/min, constant temperature is stirred
60min, filtering, obtains filter cake, as pretreated glass fiber;It is 10% chlorination by gained pretreated glass fiber and mass fraction
Ferrous solution is that 1:40 is added in reaction kettle in mass ratio, is 50 DEG C in temperature, under the conditions of revolving speed is 400r/min, constant temperature stirring divides
Dissipate 60min after, then into reaction kettle be added dropwise 2 times of ferric chloride solution volume mass fraction be 10% urea liquid, control urea it is molten
Drop rate of acceleration is 10mL/min, is added dropwise to urea liquid, continues constant temperature and is stirred to react 3h, to the end of reacting, will react
Material is transferred to ageing tank in kettle, and in still aging 8h under room temperature, filtering obtains filter residue, and filter residue 3 is washed with deionized
It is secondary, then the filter residue after washing is transferred in baking oven, it dries under the conditions of being 100 DEG C in temperature to constant weight, obtains modified glass-fiber;It presses
Parts by weight meter successively takes 100 parts of hydrogenated nitrile-butadiene rubbers, and 10 parts of modified glass-fibers, 3 parts of sulphur, 3 parts of captaxes, 3 parts anti-
Hydrogenated nitrile-butadiene rubber, is first placed in open mill by old agent, 2 parts of plasticizer, and under the conditions of temperature is 40 DEG C, plasticate 10min, then according to
Secondary addition modified glass-fiber, sulphur, captax, anti-aging agent and plasticizer are kneaded 10min under the conditions of being 150 DEG C in temperature,
In mixing process, the external magnetic field that intensity is 50T, end to be mixed, discharging, then at room temperature condition are applied to material in open mill
Lower standing 8h obtains rubber compound, and gained rubber compound is transferred in vulcanizing press, is 200 DEG C in temperature, pressure is 30MPa item
Under part, vulcanize 60min, discharging is cooled to room temperature to get yielding rubber.The anti-aging agent is by antioxidant 4020, anti-aging agent
RD and antioxidant NBC mix in mass ratio for 1:1:1.The plasticizer is dibutyl phthalate.
Example 4
In mass ratio to be 1:60 by glass fibre and mass concentration be, and 2g/L dopamine solution is mixed and is poured into beaker, and will
Beaker moves into digital display constant temperature and tests the speed magnetic stirring apparatus, is 60 DEG C in temperature, under the conditions of revolving speed is 400r/min, constant temperature is stirred
60min, filtering, obtains filter cake, as pretreated glass fiber;It is 10% chlorination by gained pretreated glass fiber and mass fraction
Ferrous solution is that 1:40 is added in reaction kettle in mass ratio, is 50 DEG C in temperature, under the conditions of revolving speed is 400r/min, constant temperature stirring divides
Dissipate 60min after, then into reaction kettle be added dropwise 2 times of ferric chloride solution volume mass fraction be 10% urea liquid, control urea it is molten
Drop rate of acceleration is 10mL/min, is added dropwise to urea liquid, continues constant temperature and is stirred to react 3h, to the end of reacting, will react
Material is transferred to ageing tank in kettle, and in still aging 8h under room temperature, filtering obtains filter residue, and filter residue 3 is washed with deionized
It is secondary, then the filter residue after washing is transferred in baking oven, it dries under the conditions of being 100 DEG C in temperature to constant weight, obtains modified glass-fiber;It presses
Parts by weight meter successively takes 100 parts of nitrile rubbers, 10 parts of polymethyl methacrylates, 10 parts of Corvics, 10 parts of C5 stones
Oleoresin, 10 parts of modified glass-fibers, 3 parts of sulphur, 3 parts of captaxes, 3 parts of anti-aging agents, 2 parts of plasticizer first set nitrile rubber
In open mill, under the conditions of temperature is 40 DEG C, plasticate 10min, sequentially adds polymethyl methacrylate, polyvinyl chloride tree
Rouge, C5 Petropols, modified glass-fiber, sulphur, captax, anti-aging agent and plasticizer mix under the conditions of being 150 DEG C in temperature
10min to be refined, in mixing process, the external magnetic field that intensity is 50T is applied to material in open mill, end to be mixed discharges, then at
8h is stood under room temperature, obtains rubber compound, and gained rubber compound is transferred in vulcanizing press, is 200 DEG C in temperature, pressure is
Under the conditions of 30MPa, vulcanize 60min, discharging is cooled to room temperature to get yielding rubber.The anti-aging agent is by anti-aging agent
4020, anti-aging agent RD and antioxidant NBC mix in mass ratio for 1:1:1.The plasticizer is dibutyl phthalate.
Comparative example: the damping rubber block of Hebei product of rubber and plastic Co., Ltd production
1 to 4 gained yielding rubber of example and comparative example product are subjected to performance detection, the specific detection method is as follows:
1. Mechanics Performance Testing: using XL-250A type tensile testing machine (four factory of Shanghai chemical machinery), by GB/T528-
2009 execute;
2. senile experiment: using DHX-9143 type electric heating constant temperature air blast ageing oven (the limited public affairs of Shanghai good fortune Ma experimental facilities
Department), experiment condition: aging temperature: 100 DEG C, the time: 48 hours.
The specific testing result of performance is as shown in table 1 before thermo-oxidative ageing:
Table 1
The specific testing result of performance is as shown in table 2 after thermo-oxidative ageing:
Table 2
By Tables 1 and 2 testing result it is found that yielding rubber obtained by technical solution of the present invention has both excellent stability and power
Performance is learned, service life is long compared with conventional base rubber, and mechanical property keeps good.
Claims (6)
1. a kind of preparation method of yielding rubber, it is characterised in that specific preparation step are as follows:
(1) glass fibre is mixed to 45~60min of immersion with dopamine solution for 1:50~1:80 in mass ratio, using filter,
Obtain pretreated glass fiber;
It (2) is in mass ratio that 1:30~1:40 mixes addition reactor with ferric chloride solution by pretreated glass fiber, dispersion is equal
After even, then 2~3 times of ferric chloride solution volume of urea liquid is added dropwise into reactor, wait be added dropwise, the reaction was continued 3~5h,
It is aged again, be filtered, washed and dried to obtain modified glass-fiber;
(3) according to parts by weight, 100~120 parts of hydrogenated nitrile-butadiene rubbers are successively taken, 10~15 parts of polymethyl methacrylates, 8~
10 parts of Corvics, 8~10 parts of Petropols, 10~20 parts of modified glass-fibers, 3~5 parts of sulphur, 1~3 part of promotion
Hydrogenated nitrile-butadiene rubber is first plasticated after 10~15min, sequentially adds poly- methyl by agent, 2~4 parts of anti-aging agents, 1~4 part of plasticizer
Methyl acrylate, Corvic, Petropols, modified glass-fiber, sulphur, promotor, anti-aging agent and plasticizer are kneaded
After 10~20min, and apply external magnetic field in mixing process, end to be mixed stands 6~8h, obtains rubber compound;
(4) mixing glue is heated into 45~60min of vulcanization, discharged to get yielding rubber.
2. a kind of preparation method of yielding rubber according to claim 1, it is characterised in that: step (1) described glass fibers
Dimension is any one in alkali-free glass fibre or medium-alkali glass fibre.
3. a kind of preparation method of yielding rubber according to claim 1, it is characterised in that: step (3) the petroleum tree
Rouge is any one in C5 Petropols or C9 Petropols.
4. a kind of preparation method of yielding rubber according to claim 1, it is characterised in that: step (3) described promotor
For any one in Vulcanization accelerator TMTD, captax or promotor ZDMC.
5. a kind of preparation method of yielding rubber according to claim 1, it is characterised in that: step (3) described anti-aging agent
It is to be mixed in mass ratio for 1:1:1 by antioxidant 4020, anti-aging agent RD and antioxidant NBC.
6. a kind of preparation method of yielding rubber according to claim 1, it is characterised in that: step (3) the plasticizer
For any one in dibutyl phthalate, octyl epoxy stearate or dioctyl adipate.
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CN103846075A (en) * | 2013-12-22 | 2014-06-11 | 北京工业大学 | Preparation method for alpha-Fe2O3 nano wire chemically-modified kieselguhr adsorbent |
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