CN110054843A - Nano-TiO2Modified epdm and preparation method thereof - Google Patents
Nano-TiO2Modified epdm and preparation method thereof Download PDFInfo
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- CN110054843A CN110054843A CN201910395081.2A CN201910395081A CN110054843A CN 110054843 A CN110054843 A CN 110054843A CN 201910395081 A CN201910395081 A CN 201910395081A CN 110054843 A CN110054843 A CN 110054843A
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- 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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/02—Organic and inorganic ingredients
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- 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
- C08K3/06—Sulfur
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- 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
- C08K2201/011—Nanostructured additives
Abstract
The present invention relates to a kind of nano-TiOs2Modified epdm and preparation method thereof belongs to nano-titanium dioxide modified field of rubber technology.The nano-titanium dioxide composite rubber material, by being made according to the following component of mass fraction meter: nano-TiO20 ~ 20 part, 350 ~ 450 parts of EPDM rubber, 5 ~ 25 parts of zinc oxide, 1-7 parts of stearic acid, 2-10 parts of sulphur, 2-10 parts of promotor.The improved production technology of the present invention improves the tearing strength and toughness of EPDM, reduce the production cost of rubber product, improve the mechanical property of EPDM, improve due to non-conjugated diene hydrocarbon comonomer can only provide a small amount of double bond crosslinking, the crosslinking of vulcanizate less, the poor disadvantage of the comprehensive performance of good tridimensional network and vulcanizate cannot be formed, be nano-TiO2The expansion of/EPDM composite material application provides more extensive approach.
Description
Technical field
The invention belongs to nano-TiOs2Modified rubber technical field, in particular to a kind of nano-TiO2Modified epdm and its system
Preparation Method.
Background technique
With the continuous development of society, scientific and technical to be constantly progressive, all trades and professions all start sane development.Changing
In work this kind industry, since rubber product has better heat-resistant antifriction and other more excellent property after vulcanization
Can, the favor of numerous researchers is obtained, this develops rubber industry gradually and is intended to maturation.Nowadays rubber has been
It is widely used among people's lives, is increasingly becoming the indispensable a part of people's life, it is small to life at one's side
Articles, food packaging and office equipment etc. arrive greatly the vehicles, medical equipment, electric machinery, building trade and military state
The various fields such as anti-, there is the one seat of rubber.Therefore, present Rubber Industry is faced with new challenge, single rubber system
The product obtained can not all compare favourably with mixed rubber product again in terms of performance and other physical and chemical performances, can no longer meet
Demand of the society to higher performance material, new material need studied exploitation.Therefore all kinds of single rubber are blended
It is modified to obtain the optimal high molecular material of performance, it has also become a key areas of scientific research personnel's research.
In numerous rubber clones, the use scope of ethylene propylene diene rubber (EPDM) is very extensive.EPDM
Raw rubber is a kind of solid that the color that the particle by particle size about 4mm is bonded together is partially white, it viscosity in rubber compared with
Commonly, it can generally be torn with hand.Because its relative density is low so that its elasticity is larger, in addition, its also have it is preferable resistance to smelly
Oxygen, heat-resisting, ageing-resistant performance and good water-resisting property, insulating properties, chemicals-resistant corrosivity.But its that there are plasticity is low, strong
Degree is smaller, may deform at a lower temperature, and mechanical strength is insufficient.
Currently, the use scope of EPDM is more and more extensive, yield increases year by year, occupies synthetic rubber at present and is number three.
According to the report of research and market (Research and Markets) company, 2017~2021 years whole world EPDM market values it is expected that with
7.36% Compound Annual Growth Rate increases, and such as on September 17th, 2018, wholly-owned subsidiary, Ente Nazionale Idrocarburi Versalis was announced, takes notice of
The big northern Ferrara city (Ferrara) of benefit has opened up an EPDM production plant, and general item investment is more than 2.5 hundred million Euros, construction
One is approved the newborn producing line for industrial use, and the EPDM aggregated capacity for making Versalis is improved about 50,000 t/, EPDM development
It is in the ascendant.Therefore EPDM is modified, to make up its defect in performance, to widen its use scope, it appears outstanding
It is important.
But the existing research that EPDM is modified using nano-titanium dioxide at present, it is primarily present following deficiency:
First, TiO2It is a kind of modified material emerging in recent years, particularly in when its dosage is in a certain range, can not only mentions
The tearing strength and toughness of high EPDM, reduces the production cost of rubber product, moreover it is possible to improve the mechanical property and thermostabilization of EPDM
Property, also imparts its uvioresistant and anti-aging performance, but it is studied at present it is less, using deficiency；In addition, for comprehensive benefit
With titanium resource, the new way of development and application greatly reduces aluminium manufacturer's titanium processing discharge red mud and pollutes to environment bring, fundamentally
Eliminate the conflict between environment and development for a long time.Second, nano-TiO2Surface treatment be improve reuniting effect,
The effective ways of performance are improved, but method of modifying is often cumbersome, causes production cost higher, therefore the present invention plans nanometer
TiO2Powder is added in rubber mass, by being improved to process recipe to improve the performance of rubber mass；Third, due to non-total
Yoke diolefin comonomers can only provide a small amount of double bond crosslinking, and the crosslinking of vulcanizate is few, cannot be formed three-dimensional netted well
The comprehensive performance of structure, vulcanizate is poor, therefore is nano-TiO2The approach that has provided of application.
Summary of the invention
A kind of nano-TiO is proposed the purpose of the present invention is overcome the deficiencies in the prior art2Modified epdm and its preparation side
Method, modified EPDM have good mechanical property.
Technical solution of the present invention:
Nano-TiO2Modified epdm, which is characterized in that including the following component according to mass fraction meter: nano-TiO20 ~ 20 part,
350 ~ 450 parts of EPDM, 5 ~ 25 parts of zinc oxide, 1-7 parts of stearic acid, 2-10 parts of sulphur, 2-10 parts of promotor.
Further, the nano-TiO2Partial size be 10-40nm.
Further, the promotor is at least one of Vulcanization accelerator TMTD and captax.
Further, the promotor is the mixture of Vulcanization accelerator TMTD and captax, Vulcanization accelerator TMTD and promotor
The mass ratio of M is 2:1.
Further, the nano-TiO2Modified epdm includes the following component according to mass fraction meter: nano-TiO20~
20 parts, EPDM350 ~ 450 part, 5 ~ 25 parts of zinc oxide, 1-7 parts of stearic acid, 2-10 parts of sulphur, 2-10 parts of promotor.
Further, the nano-TiO2The preparation method of modified epdm, includes the following steps:
Step 1: according to the quality proportioning, weighing each component, spare；
Step 2: by load weighted EPDM through multiple roll-in, turn refining, until starting out after forming smooth non-porous packet roller glue-line
Refining, sequentially adds zinc oxide, stearic acid, promotor, nano-TiO2And sulphur, regulating roller away from, continue to turn refining, to each component mix
Color uniform outer surface is smooth；
Step 3: adjustment roll spacing, one knife of flat mouth, sizing material roll-in discharging can remove, stand, obtain rubber compound；
Step 4: rubber compound being put into vulcameter and is vulcanized, and curing temperature is 150 ~ 160 DEG C.
Further, EPDM described in step 2 through 3 ~ 4 roll-ins, turn refining.
Further, roll spacing described in step 2 is 0.5 ~ 1.0mm, it is described when turning over experienced using triangle bag, the side of clot
Method carries out.
Further, time of repose described in step 3 is for 24 hours.
Its remarkable advantage is the present invention compared with prior art: the present invention utilizes nano-TiO2EPDM is modified, is led to
The tearing strength and toughness for improving formula and production technology to improve EPDM are crossed, production cost is reduced, has widened improvement EPDM power
Learn the approach of performance and the effect of application；It improves and is handed over since non-conjugated diene hydrocarbon comonomer can only provide a small amount of double bond
Connection, vulcanizate crosslinking less, the poor disadvantage of the comprehensive performance of good tridimensional network and vulcanizate cannot be formed,
For nano-TiO2The expansion of/EPDM composite material application provides more extensive approach.
Detailed description of the invention
Fig. 1 is the vulcanization time curve of EPDM；
Fig. 2 is 1 to 5 gained nano-TiO of embodiment2The firmness change curve of modified epdm；
Fig. 3 is 1 to 5 gained nano-TiO of embodiment2The variable density curve of modified epdm；
Fig. 4 is 1 to 5 gained nano-TiO of embodiment2The tearing strength change curve of modified epdm；
Fig. 5 is 1 to 5 gained nano-TiO of embodiment2The tensile strength change curve of modified epdm；
Fig. 6 is 1 to 5 gained nano-TiO of embodiment2The change curve of the elongation at break of modified epdm；
Fig. 7 is 1 to 5 gained nano-TiO of embodiment2The permanent deformation curve of modified epdm.
Specific embodiment
The raw material that the present invention uses such as table 1.
The raw material that 1 present invention of table uses
The instrument and equipment that the present invention uses such as table 2.
The instrument and equipment that 2 present invention of table uses
Embodiment 1
Nano-TiO2Modified epdm, including the following component according to mass fraction meter: 400 parts of EPDM, 9 parts of zinc oxide, tristearin
Sour 4 parts, 6 parts of sulphur, 6 parts of promotor.
The nano-TiO2Modified epdm the preparation method is as follows:
Step 1: by quality weighing EPDM400 parts, 9 parts of zinc oxide, 4 parts of stearic acid, 6 parts of sulphur, 6 parts of promotor (in mass ratio
TMTD the and M mixture of 2:1 weighs), it is spare.
Step 2: by load weighted EPDM through 3 ~ 4 roll-ins (0.5 ~ 1.0mm of roll spacing), turn refining (using triangle bag, clot
Method carry out), until forming mill after smooth non-porous packet roller glue-line, sequentially add zinc oxide, stearic acid, promotor and sulphur
Sulphur, regulating roller is away from continuing to turn refining, it is smooth to mix and surface uniform to color to each component；
Step 3: adjustment roll spacing, one knife of flat mouth, sizing material roll-in discharging remove standing for 24 hours, obtain rubber compound；
Step 4: rubber compound is put into vulcameter and is vulcanized (temperature is 155 DEG C, time 9min36s).
Test piece machine, standard and right-angle type rubber batten cutter sample preparation are cut with universal material and obtains dumbbell and perpendicular type batten, respectively
3 are cut, through detection data and is averaged.
Embodiment 2
Nano-TiO2Modified epdm, including the following component according to mass fraction meter: nano-TiO2 1.25 parts, 400 parts of EPDM,
9 parts of zinc oxide, 4 parts of stearic acid, 6 parts of sulphur, 6 parts of promotor.
The nano-TiO2Modified epdm the preparation method is as follows:
Step 1: quality weighing nano-TiO is pressed2 1.25 parts (partial size 20nm), EPDM400 parts, 9 parts of zinc oxide, stearic acid 4
Part, 6 parts of sulphur, 6 parts of promotor (TMTD the and M mixture of 2:1 in mass ratio weighs), it is spare.
Step 2: by load weighted EPDM through 3 ~ 4 roll-ins (0.5 ~ 1.0mm of roll spacing), turn refining (using triangle bag, clot
Method carry out), until forming mill after smooth non-porous packet roller glue-line, sequentially add zinc oxide, stearic acid, promotor, nanometer
TiO2And sulphur, regulating roller is away from continuing to turn refining, it is smooth to mix and surface uniform to color to each component；
Step 3: adjustment roll spacing, one knife of flat mouth, sizing material roll-in discharging remove standing for 24 hours, obtain rubber compound；
Step 4: rubber compound is put into vulcameter and is vulcanized (temperature is 155 DEG C, time 9min36s).
Test piece machine, standard and right-angle type rubber batten cutter sample preparation are cut with universal material and obtains dumbbell and perpendicular type batten, respectively
3 are cut, through detection data and is averaged.
Embodiment 3
Nano-TiO2Modified epdm, including the following component according to mass fraction meter: nano-TiO20 ~ 20 part, EPDM 350 ~ 450
Part, 5 ~ 25 parts of zinc oxide, 1-7 parts of stearic acid, 2-10 parts of sulphur, 2-10 parts of promotor.
The nano-TiO2Modified epdm the preparation method is as follows:
Step 1: quality weighing nano-TiO is pressed22.5 parts (partial size 20nm), EPDM400 parts, 9 parts of zinc oxide, 4 parts of stearic acid,
6 parts of sulphur, 6 parts of promotor (TMTD the and M mixture of 2:1 in mass ratio weighs), it is spare.
Step 2: by load weighted EPDM through 3 ~ 4 roll-ins (0.5 ~ 1.0mm of roll spacing), turn refining (using triangle bag, clot
Method carry out), until forming mill after smooth non-porous packet roller glue-line, sequentially add zinc oxide, stearic acid, promotor, nanometer
TiO2And sulphur, regulating roller is away from continuing to turn refining, and surface uniform to each component blend color is smooth；
Step 3: adjustment roll spacing, one knife of flat mouth, sizing material roll-in discharging remove standing for 24 hours, obtain rubber compound；
Step 4: rubber compound is put into vulcameter and is vulcanized (temperature is 155 DEG C, time 9min36s).
Test piece machine, standard and right-angle type rubber batten cutter sample preparation are cut with universal material and obtains dumbbell and perpendicular type batten, respectively
3 are cut, through detection data and is averaged.
Embodiment 4
Nano-TiO2Modified epdm, including the following component according to mass fraction meter: nano-TiO23.75 parts, 400 parts of EPDM,
9 parts of zinc oxide, 4 parts of stearic acid, 6 parts of sulphur, 6 parts of promotor.
The nano-TiO2Modified epdm the preparation method is as follows:
Step 1: quality weighing nano-TiO is pressed2 3.75 parts (partial size 20nm), EPDM400 parts, 9 parts of zinc oxide, stearic acid 4
Part, 6 parts of sulphur, 6 parts of promotor (TMTD the and M mixture of 2:1 in mass ratio weighs), it is spare.
Step 2: by load weighted EPDM through 3 ~ 4 roll-ins (0.5 ~ 1.0mm of roll spacing), turn refining (using triangle bag, clot
Method carry out), until forming mill after smooth non-porous packet roller glue-line, sequentially add zinc oxide, stearic acid, promotor, nanometer
TiO2And sulphur, regulating roller is away from continuing to turn refining, it is smooth to mix and surface uniform to color to each component；
Step 3: adjustment roll spacing, one knife of flat mouth, sizing material roll-in discharging remove standing for 24 hours, obtain rubber compound；
Step 4: rubber compound is put into vulcameter and is vulcanized (temperature is 155 DEG C, time 9min36s).
Test piece machine, standard and right-angle type rubber batten cutter sample preparation are cut with universal material and obtains dumbbell and perpendicular type batten, respectively
3 are cut, through detection data and is averaged.
Embodiment 5
Nano-TiO2Modified epdm, including the following component according to mass fraction meter: nano-TiO25 parts, 400 parts of EPDM, oxygen
Change 9 parts of zinc, 4 parts of stearic acid, 6 parts of sulphur, 6 parts of promotor.
The nano-TiO2Modified epdm the preparation method is as follows:
Step 1: quality weighing nano-TiO is pressed2 5 parts (partial size 20nm), EPDM400 parts, 9 parts of zinc oxide, 4 parts of stearic acid,
6 parts of sulphur, 6 parts of promotor (TMTD the and M mixture of 2:1 in mass ratio weighs), it is spare.
Step 2: by load weighted EPDM through 3 ~ 4 roll-ins (0.5 ~ 1.0mm of roll spacing), turn refining (using triangle bag, clot
Method carry out), until forming mill after smooth non-porous packet roller glue-line, sequentially add zinc oxide, stearic acid, promotor, nanometer
TiO2And sulphur, regulating roller is away from continuing to turn refining, and surface uniform to each component blend color is smooth；
Step 3: adjustment roll spacing, one knife of flat mouth, sizing material roll-in discharging remove standing for 24 hours, obtain rubber compound；
Step 4: rubber compound is put into vulcameter and is vulcanized (temperature is 155 DEG C, time 9min36s).
Test piece machine, standard and right-angle type rubber batten cutter sample preparation are cut with universal material and obtains dumbbell and perpendicular type batten, respectively
3 are cut, through detection data and is averaged.
To nano-TiO produced by the present invention2Modified epdm is tested for the property:
Shao Er A type hardness tester is carried out by GB/T531-1999.
Tearing strength is carried out by GB/T529-1999.
Tensile strength, elongation at break and setafter break are carried out by GB528-1998 standard.
Density is carried out by 2005 standard of GBT/1463.
By the vulcanization time curve and relevant test data of Fig. 1 and EPDM of table 3 it is found that when 9min36s, torque capacity
(MH) almost no longer change, 9min36s is the optimum sulfurating time of EPDM.
The testing result of 3 EPDM curing curve of table
(EPDM:ZnO:SA:S:TMTD:M=400:9:4:6:4:2 by mass)
By the nano-TiO of Fig. 22The firmness change curve of modified epdm is it is found that addition nano-TiO2EPDM composite material afterwards
Hardness obviously increases, and mechanical property improves.
By the nano-TiO of Fig. 32The variable density curve of modified epdm is it is found that nano-TiO2Addition have the density of EPDM
It is obviously improved.
By the nano-TiO of Fig. 42The tearing strength change curve of modified epdm is it is found that being added nano-TiO2Afterwards, tearing is strong
The extreme value of degree reaches 7.8MPa, nano-TiO2Content be more than after 3.75%, tearing strength reduces rapidly.
By the nano-TiO of Fig. 52The tensile strength change curve of modified epdm is it is found that with nano-TiO2Content increase,
The tensile strength of EPDM composite material is generally increasing always.Nano-TiO2There is preferable enhancing to make the tensile strength of EPDM
With, can be used as enhancing EPDM filler.
By the nano-TiO of Fig. 62The change curve of the elongation at break of modified epdm it is found that EPDM composite material fracture
The variation of elongation has the tendency that first reducing to increase afterwards.Work as nano-TiO2When content increases to 3.75%, the elongation of EPDM is slow
Slow rise, nano-TiO2When to 5%, elongation is still rising, this shows nano-TiO2The flexibility of/EPDM composite material improves.
By the nano-TiO of Fig. 72The setafter break curve of modified epdm is it is found that nano-TiO2Permanent change to EPDM
Shape has the effect of reduction.But reducing effect and nano-TiO2Content it is unrelated, remain that definite value no longer changes.
Embodiment described above is only to absolutely prove preferred embodiment that is of the invention and being lifted, and protection scope is unlimited
In this.Those skilled in the art's made equivalent substitute or transformation on the basis of the present invention, in protection of the invention
Within the scope of, protection scope of the present invention is subject to claims.
Claims (9)
1. nano-TiO2Modified epdm, which is characterized in that including the following component according to mass fraction meter: nano-TiO20 ~ 20 part,
EPDM350 ~ 450 part, 5 ~ 25 parts of zinc oxide, 1-7 parts of stearic acid, 2-10 parts of sulphur, 2-10 parts of promotor.
2. nano-TiO according to claim 12Modified epdm, which is characterized in that the nano-TiO2Partial size be 10-
40nm。
3. nano-TiO according to claim 12Modified epdm, which is characterized in that the promotor be Vulcanization accelerator TMTD and
At least one of captax.
4. nano-TiO according to claim 32Modified epdm, which is characterized in that the promotor be Vulcanization accelerator TMTD and
The mass ratio of the mixture of captax, Vulcanization accelerator TMTD and captax is 2:1.
5. nano-TiO according to claim 12Modified epdm, which is characterized in that including according to the as follows of mass fraction meter
Component: nano-TiO2 27 parts, 400 parts of ethylene propylene diene rubber, 13 parts of zinc oxide, 4 parts of stearic acid, 6 parts of sulphur, 6 parts of promotor.
6. nano-TiO described in claim 12The preparation method of modified epdm, which comprises the steps of:
Step 1: according to the quality proportioning, weighing each component, spare；
Step 2: by load weighted EPDM through multiple roll-in, turn refining, until starting out after forming smooth non-porous packet roller glue-line
Refining, sequentially adds zinc oxide, stearic acid, promotor, nano-TiO2And sulphur, regulating roller away from, continue to turn refining, to each component mix
It is smooth to color uniform outer surface；
Step 3: adjustment roll spacing, one knife of flat mouth, sizing material roll-in discharging can remove, stand, obtain rubber compound；
Step 4: rubber compound being put into vulcameter and is vulcanized, and curing temperature is 150 ~ 160 DEG C.
7. nano-TiO according to claim 62The preparation method of modified epdm, which is characterized in that described in step 2
EPDM through 3 ~ 4 roll-ins, turn refining.
8. nano-TiO according to claim 62The preparation method of modified epdm, which is characterized in that roller described in step 2
It is described to be carried out using triangle bag, the method for clot when turning over experienced away from for 0.5 ~ 1.0mm.
9. nano-TiO according to claim 62The preparation method of modified epdm, which is characterized in that quiet described in step 3
Setting the time is for 24 hours.
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