CN105801928B - Using the rubber and preparation technology of graphene oxide - Google Patents
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The present invention relates to a kind of rubber and preparation technology using graphene oxide, it is characterized in that, comprise the following steps：（1）Natural rubber is crossed into roller on a mill, mill roll spacing be 1.3 ± 0.15mm, and roller temperature is maintained at 70 ± 5 DEG C, and the film obtained after mistake roller 5~15 times is cooled down in drier；（2）Film is crossed into roller 1~5 time on a mill, bag roller, roll spacing are not 0.1~0.5mm；（3）Roll spacing is adjusted to 0.5~1.5mm, makes film bag roller, then roll spacing is adjusted to 1.5~2mm, continued 3~5min of roller；（4）Graphene oxide is added, cutter is carried out, triangle bag was beaten after continuing 2~4min of roller；（5）Add zinc oxide, stearic acid, sulphur, accelerator and anti-scorching agent CTP, cross after roller continues 2~5min and carry out cutter, continued 2~4min of roller；（6）Sizing material is removed, roll spacing is adjusted to 0.5~2mm；Sizing material is crossed into roller 4~8 times again.The addition of graphene oxide is few in rubber of the present invention, can effective control cost, and time of scorch can be extended.
Description
Technical field
It is especially a kind of to use graphene oxide the present invention relates to a kind of rubber and preparation technology using graphene oxide
Rubber and preparation technology as auxiliary antiscorching agent.
Background technology
Sizing material is in the effect stored be heated during machine-shaping, generation prevulcanization (crosslinking) and the energy that loses flowability
With the ability of reprocessing, referred to as incipient scorch phenomenon.One of the problem of incipient scorch of sizing material is common during rubber processing.Rubber size
Certain stability and process safety are kept in process, in the technical process such as the mixing, calendering and extrusion of sizing material
It is a key issue.Reinforcing (quick banburying, quick extrusion and calendering, the high speed sulphur of production process are particularly directed in recent years
Change etc.) and use the material for easily causing incipient scorch, such as fine particle carbon black makes this problem more prominent.Utilize rubber anti-chark agent
It is a kind of easy-to-use method to improve the processing characteristics of rubber.At present, anti-scorching agent CTP is that tyre industry is most widely used
A kind of antiscorching agent.
Graphene is a kind of carbon material emerging in recent years, is widely used in the fields such as material modified, biological medicine.Its
Finder obtained Nobel Prize in physics in 2010.Graphene oxide is the presoma in graphene preparation process, and surface has
There is abundant oxygen-containing functional group.Such as carboxyl (- COOH-), carbonyl (- CO-), sulfonyl (O=S=O) etc..Lot of experiments
Confirm that the addition of graphene oxide is obviously improved effect to all kinds of high polymer material performances, and product price is significantly less than
Graphene.
Scattered in high score subclass material of graphene oxide composite material is significantly better than graphene, when particularly content is less
(being less than 3 ‰), pass through simple and mechanical mixing.The vulcanizating glue physical performance for adding graphene oxide is substantially better than reference group.
In rubber family macromolecule formula, in addition to investigating the physical property of sizing material, the exploitation of the investigation of scorch safety for formula
An and important indicator.
The content of the invention
The purpose of the present invention is to overcome the deficiencies in the prior art, there is provided a kind of rubber using graphene oxide and
Preparation technology, the addition of graphene oxide is few, can effective control cost, and time of scorch can be extended.
According to technical scheme provided by the invention, the rubber using graphene oxide, it is characterized in that, including with the following group
Part, component ratio by mass number meter：100 parts of natural rubbers, 0.2~1 part of stearic acid, 2~10 parts of zinc oxide, 0.1~1 part of rush
Enter agent, 0~0.3 part of anti-scorching agent CTP, 1~5 part of sulphur, 0.1~1 part of graphene oxide.
In a detailed embodiment, the accelerator is captax or accelerator NS.
In a detailed embodiment, when the accelerator uses captax, the parts by weight of anti-scorching agent CTP are 0.1
~0.3 part.
In a detailed embodiment, when the accelerator uses accelerator NS, the parts by weight of anti-scorching agent CTP are 0
~0.3 part.
The preparation technology of the rubber using graphene oxide, it is characterized in that, comprise the following steps, component ratio is by weight
Measure number meter：
(1) 100 parts of natural rubbers are crossed into roller on a mill, mill roll spacing is 1.3 ± 0.15mm, and roller temperature is maintained at 70
± 5 DEG C, cross after roller 5~15 times obtained film and cooled down in drier；
(2) film for obtaining step (1) crosses roller 1~5 time on a mill, and bag roller, roll spacing are not 0.1~0.5mm；
(3) roll spacing is adjusted to 0.5~1.5mm, makes film bag roller, then roll spacing is adjusted to 1.5~2mm, continued roller 3~
5min；
(4) 0.1~1 part of graphene oxide is added, cutter is carried out, triangle bag was beaten 3~5 times after continuing 2~4min of roller；
(5) 2~10 parts of zinc oxide, 0.2~1 part of stearic acid, 1~5 part of sulphur, 0.1~1 part of accelerator and 0~0.3 are added
Part anti-scorching agent CTP, cross after roller continues 2~5min and carry out cutter, continued 2~4min of roller；
(6) sizing material is removed, roll spacing is adjusted to 0.5~2mm；Sizing material is crossed into roller 4~8 times again.
In the step (2)~step (6), roller temperature is maintained at 70 ± 5 DEG C.
In the step (4), cutter carries out 3 3/4 cutteves from every side of mill.
In the step (5), cutter carries out 3 3/4 cutteves from every side of mill.
In a detailed embodiment, a diameter of 160mm of the mill mixer roller, roller width is 320mm, front and rear
Roller speed is than being 1:1~1:2, blanket roller speed is 10~15m/min.
In a detailed embodiment, a diameter of 160mm of the mill mixer roller, roller width is 320mm, front and rear
Roller speed is than being 1:1.4, blanket roller speed is 10.4m/min.
The present invention compared with prior art, has advantages below：
(1) addition is few：Graphene oxide addition is only 0.1 parts by weight or 0.3 parts by weight in the formula of the present invention, i.e.,
Time of scorch can be extended；
(2) calendering process is simple, without to graphene oxide specially treated, it is only necessary to directly mixed using mill or banbury
Refining；
(3) graphite alkenes carbon material price is less into downward trend year by year, particularly addition, and cost is gradually by each application
Field is received；
(4) numerous studies show the addition of graphene oxide for the effect of haveing a certain upgrade of the mechanical property of rubber, because
This has double effects after adding；
(5) rubber size should possess excellent mechanical property take into account again production scorch safe performance, graphene oxide
Material makes such material rooted out in the heavy industrialization of rubber materials to sizing material production Jiao as the application of auxiliary antiscorching agent
Burn the trouble and worry of security.
Embodiment
With reference to specific embodiment, the invention will be further described.
Graphene oxide product used in the embodiment of the present invention is by the hexa-atomic limited public affairs of cellulosic material science and technology share in Changzhou
Department provides.
For the present invention using graphene oxide as auxiliary incipient scorch agent, the exploitation for following graphene rubber-like materials plays one
Determine impetus, not only extended application of the graphene oxide composite material in elastomeric material but also be this developing material high-performance tire
Material provides the foundation.It is mainly that the suppression to disulfide group is realized that graphene oxide, which aids in the mechanism of anti-scorch effect, in addition, rubber
Various ingredients in glue, surface of graphene oxide acidic-group is set to may participate in all kinds of reactions, it is in rule to make anti-scorch effect during different amounts
The change of rule property.
Have a variety of acidic-groups, such as carboxyl (- COOH-), carbonyl (- CO-), sulfonyl in graphene oxide (GO) surface
(O=S=O) etc., these groups can hinder the formation of free radical in vulcanization reaction, and and can suppresses biradical sulphur in initial vulcanization step
Produce, therefore can postpone to vulcanize, there is the anti-incipient scorch effect of certain auxiliary.For the difference of accelerator in different formulations, stone is aoxidized
Black alkene, which plays, aids in the mechanism of anti-scorch effect different.Graphene oxide is mainly by controlling the generation of disulfide group to play anti-scorch effect
Fruit, during anti-scorching agent CTP dosage difference, the reaction that GO is participated in is different therefore also different to the influence degree of incipient scorch.
1~embodiment of embodiment 9：A kind of preparation technology of rubber using graphene oxide, comprises the following steps：
(1) natural rubber is crossed into roller on a mill, mill roll spacing is 1.3mm, and roller temperature is maintained at 70 DEG C, crosses roller 10 times
The film obtained afterwards is cooled down in drier；A diameter of 160mm of the mill mixer roller, roller width is 320mm, preceding
Roller speed is than being 1 afterwards:1.4, blanket roller speed is 10.4m/min；
(2) film for obtaining step (1) crosses roller 2 times on a mill, not bag roller, roll spacing 0.2mm；
(3) roll spacing is adjusted to 1.4mm, makes film bag roller, then roll spacing is adjusted to 1.8mm, continue roller 4min；
(4) graphene oxide (GO) is added, carries out cutter, cutter carries out 3 3/4 cutteves from every side of mill, held
Triangle bag was beaten after continuing 2~4min of roller 3 times；
(5) zinc oxide, stearic acid, sulphur, captax and anti-scorching agent CTP are added, crosses after roller continues 4min and carries out cutter,
Cutter carries out 3 3/4 cutteves from every side of mill, continues roller 3min；
(6) sizing material is removed, roll spacing is adjusted to 0.8mm；Sizing material is crossed into roller 6 times again；
In above-mentioned steps (2)~step (6), roller temperature is maintained at 70 DEG C.
The dosage of each component is as shown in table 1 in 1~embodiment of embodiment 9.
Table 1
10~embodiment of embodiment 18：A kind of preparation technology of rubber using graphene oxide, comprises the following steps, group
Part ratio by mass number meter：
(1) natural rubber is crossed into roller on a mill, mill roll spacing is 1.45mm, and roller temperature is maintained at 75 DEG C, crosses roller 15
The film obtained after secondary is cooled down in drier；A diameter of 160mm of the mill mixer roller, roller width are 320mm,
Front and rear roller speed is than being 1:1.4, blanket roller speed is 10.4m/min；
(2) film for obtaining step (1) crosses roller 5 times on a mill, not bag roller, roll spacing 0.5mm；
(3) roll spacing is adjusted to 1.5mm, makes film bag roller, then roll spacing is adjusted to 2mm, continue roller 5min；
(4) graphene oxide is added, carries out cutter, cutter carries out 3 3/4 cutteves from every side of mill, continued
Triangle bag is beaten after roller 4min 5 times；
(5) zinc oxide, stearic acid, sulphur, accelerator NS and anti-scorching agent CTP are added, crosses after roller continues 5min and carries out cutter,
Cutter carries out 3 3/4 cutteves from every side of mill, continues roller 4min；
(6) sizing material is removed, roll spacing is adjusted to 2mm；Sizing material is crossed into roller 8 times again；
In above-mentioned steps (2)~step (6), roller temperature is maintained at 75 DEG C.
The dosage of each component is as shown in table 2 in 10~embodiment of embodiment 18.
Table 2
The sample sizing material obtained to 1~embodiment of above-described embodiment 18 tests 127 DEG C of time of scorch (min), as a result such as table
3rd, shown in table 4.As a result show, time of scorch can be extended by adding the different formulations of captax and NS, ensure sizing material process
Security.
Table 3
Table 4
As shown in table 3, using M as accelerator, after adding CTP, anti-scorch lifting effect declines with the raising of CTP contents.
Respectively lifting 7.9% (CTP 0.3phr, GO 0.1phr) is down to by lifting 11.1% (CTP 0.1phr, GO 0.1phr)；By
13.3% (CTP 0.1phr, GO 0.3phr) of lifting is down to lifting 11.2% (CTP 0.3phr, GO 0.3phr).Such as the institute of table 4
Show, using NS as accelerator, remove 0.3 parts by weight of CTP additions and cause anti-scorch effect decline outer, also show similar rule.Point
Lifting 13.2% (CTP 0.1phr, GO 0.1phr) is not down to by lifting 14.3% (CTP 0phr, GO 0.1phr)；By being lifted
19.6% (CTP 0phr, GO 0.3phr) is down to lifting 19.2% (CTP 0.1phr, GO 0.3phr).
In addition, incipient scorch lifting effect improves with the increase of graphene oxide content during using M as accelerator.Same such as table
Shown in 4, using NS as in the formula of accelerator, when graphene oxide addition is 0.1 part or 0.3 part, time of scorch is respectively increased
14.3%, 19.6% (0 part of CTP).CTP dosages are 0.1 part, when graphene oxide addition is 0.1 part or 0.3 part, incipient scorch
Time has been respectively increased 13.2%, 19.2%.Two kinds of accelerator show similar rule, i.e., with the increasing of graphene oxide dosage
Add, anti-scorch effect improves.With the increase of CTP dosages, anti-scorch effect reduces.
It is worth noting that when M is accelerator, without using CTP, for graphene oxide without anti-scorch effect, NS is accelerator
When, embody certain anti-scorch effect without using CTP.This may be relevant from the different reaction mechanisms of two kinds of accelerator, phase
Closing discussion will be described in following mechanism part.
CTP anti-scorch mechanism mainly carries out fast reaction generation accessory substance with captax, reduces M amount to slow down sulphur
Change reaction speed, play anti-incipient scorch effect, as shown in Equation 1：
Surface of graphene oxide acidic-group mainly may participate in two reactions, first, participating in chemical equilibrium reaction, promote to put down
Weighing apparatus is carried out to the right, and this process does not play directly anti-incipient scorch effect, but consumes partially acidic group.Second, participate in suppression
The effect of system reaction generation cystine linkage, the process directly plays anti-scorch effect, is core process.
When NS is as antiscorching agent, a large amount of acidic-groups that surface of graphene oxide contains can break NS accelerator decomposable processes
Normal reaction balance (reaction 1：),
A large amount of NS are made to be converted into M.But for second step reaction M generation DM process (reactions 2：
), acidic groups
The presence of group is played a part of suppressing disulfide group generation.For NS accelerator, exist even without CTP, add graphene oxide
Still there is certain anti-scorch effect.After adding a small amount of CTP, a large amount of product M generate accessory substance with CTP rapidly.Acidic-group is deposited
Promoting chemical balance (reaction 1) to carry out to the right, therefore generating more M, it means that CTP can consume more M,
Equivalent to the dosage for more reducing accelerator.But total M of consumption amount is certain, both depends on CTP dosages.It is more
Remaining M still may proceed to generate DM.Now, even if CTP loses anti-scorch effect after being exhausted, but remaining graphene oxide
Surface acidic groups can still suppress the formation (reaction 2) of disulfide group, and anti-scorch effect is relatively used alone CTP and increased.This
When, the anti-scorch effect of auxiliary of acidic-group is mainly reflected in facilitation and second step to first step reaction balance (reaction 1)
(reaction 2) suppresses the aspect of inhibitory action two of disulfide group generation.When CTP usage amounts increase to 0.3phr, due to CTP usage amounts compared with
Greatly, first step reaction balance is constantly carried out to the right, is continuously generated M, is consumed a large amount of acidic-groups.When whole acidic functionalities disappear
After consumption (the reaction balance for being primarily involved in the first step), second step can not be reacted and suppressed.That is CTP dosages carry
Height causes acidic-group to be exhausted earlier than CTP, can not participate in suppressing the reaction of disulfide group, therefore with the anti-scorch effects of CTP are used alone
It is identical.
It is further to note that GO dosages are identical, after CTP dosages rise to 0.1phr by 0phr, due to part GO tables
Face acidic-group more take part in the balanced reaction of reaction (1), and the acidic-group for participating in suppressing reaction (2) is reduced, therefore right
Reduced in the increase rate of incipient scorch effect and (be down to 13.2% by 14.3%, 19.2%) 19.6% is down to.
M is the mechanism of action of accelerator：Sulfenamide type accelerators NS decomposition reaction (reaction 1) is not present in M accelerator, directly
Disulfide group (reaction 2) can be generated by connecing.It is also to suppress M generation disulfide group processes that now graphene oxide, which aids in anti-scorch mechanism,.Do not add
During anti-scorching agent CTP, due to being not engaged in NS decomposition reactions, acidic-group is not consumed.Therefore part-COOH- may participate in aoxidizing
Series reaction (the reaction 6 of zinc：
Reaction 7：)。
M accelerator can directly generate zinc salt, the zinc salt co-ordination complex complicated with carboxyl generation with zinc oxide.The activity of co-ordination complex
Much higher compared with accelerator, the solubility in sizing material also greatly increases.Therefore, in the case of no addition CTP, oxidation is added
Graphene can promote incipient scorch.
After 0.1phr CTP are added, CTP can generate accessory substance directly with M booster responses.Meanwhile M gives birth to zinc oxide
Reaction into zinc salt is also affected and suppressed, and also inhibits the reaction that carboxyl participates in generation complex compound.When CTP is exhausted
Afterwards, surface of graphene oxide acidic-group can suppress remaining M generations disulfide group again.Therefore it is burnt to embody auxiliary for graphene oxide
Burn performance.Even if CTP dosages are improved to 0.3phr, due to consuming acidic-group (reaction not in such as NS decomposition reaction
1), after CTP has been gradually used up, graphene oxide can still generate the progress of disulfide group suppression vulcanization reaction by suppressing M.
Therefore still there is the anti-scorch effect of auxiliary.
In addition, GO dosages are identical, it is finally remaining by the reacted M of CTP after CTP dosages rise to 0.3phr by 0.1phr
Generation complex compound can be reacted with zinc salt and promote incipient scorch for 0.1phr, remaining acidic-group-COOH- by measuring, therefore with CTP dosages
Increase, the increase rate of the GO incipient scorch effects of same amount reduces (is down to 7.9%, 11.2%) 13.3% is down to by 11.1%.
Claims (2)
1. a kind of preparation technology of rubber using graphene oxide, it is characterized in that, comprise the following steps, component ratio by mass
Number meter：
（1）100 parts of natural rubbers are crossed into roller on a mill, mill roll spacing is 1.3mm, and roller temperature is maintained at 70 DEG C, crosses roller 10
The film obtained after secondary is cooled down in drier；A diameter of 160mm of the mill mixer roller, roller width are 320mm,
Front and rear roller speed is than being 1:1.4, blanket roller speed is 10.4m/min；
（2）By step（1）Obtained film crosses roller 2 times on a mill, not bag roller, roll spacing 0.2mm；
（3）Roll spacing is adjusted to 1.4mm, makes film bag roller, then roll spacing is adjusted to 1.8mm, continued roller 4min；
（4）Add 0.1 part of graphene oxide（GO）, cutter is carried out, cutter carries out 3 3/4 cutteves from every side of mill, held
Triangle bag was beaten after continuing 2~4min of roller 3 times；
（5）6 parts of zinc oxide, 0.5 part of stearic acid, 3.5 parts of sulphur, 0.5 part of captax and 0.1 part of anti-scorching agent CTP are added, crosses roller
Cutter is carried out after continuing 4min, cutter carries out 3 3/4 cutteves from every side of mill, continued roller 3min；
（6）Sizing material is removed, roll spacing is adjusted to 0.8mm；Sizing material is crossed into roller 6 times again；
Above-mentioned steps（2）~step（6）In, roller temperature is maintained at 70 DEG C.
2. a kind of preparation technology of rubber using graphene oxide, it is characterized in that, comprise the following steps, component ratio by mass
Number meter：
（1）100 parts of natural rubbers are crossed into roller on a mill, mill roll spacing is 1.3mm, and roller temperature is maintained at 70 DEG C, crosses roller 10
The film obtained after secondary is cooled down in drier；A diameter of 160mm of the mill mixer roller, roller width are 320mm,
Front and rear roller speed is than being 1:1.4, blanket roller speed is 10.4m/min；
（2）By step（1）Obtained film crosses roller 2 times on a mill, not bag roller, roll spacing 0.2mm；
（3）Roll spacing is adjusted to 1.4mm, makes film bag roller, then roll spacing is adjusted to 1.8mm, continued roller 4min；
（4）Add 0.1 part of graphene oxide（GO）, cutter is carried out, cutter carries out 3 3/4 cutteves from every side of mill, held
Triangle bag was beaten after continuing 2~4min of roller 3 times；
（5）6 parts of zinc oxide, 0.5 part of stearic acid, 3.5 parts of sulphur, 0.5 part of captax and 0.3 part of anti-scorching agent CTP are added, crosses roller
Cutter is carried out after continuing 4min, cutter carries out 3 3/4 cutteves from every side of mill, continued roller 3min；
（6）Sizing material is removed, roll spacing is adjusted to 0.8mm；Sizing material is crossed into roller 6 times again；
Above-mentioned steps（2）~step（6）In, roller temperature is maintained at 70 DEG C.
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