CN112662095A - Ternary fluororubber nanocomposite with three-crosslinking-network structure and preparation method thereof - Google Patents
Ternary fluororubber nanocomposite with three-crosslinking-network structure and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of polymer material preparation, and particularly relates to a modified ternary fluororubber nanocomposite and a preparation method thereof. According to the invention, the untreated aminated multi-walled carbon nanotubes and graphene are directly added during open milling feeding, then open milling and vulcanization are carried out, the aminated multi-walled carbon nanotubes and graphene and the ternary fluororubber matrix respectively form a cross-linked structure, meanwhile, the aminated multi-walled carbon nanotubes and graphene also generate a cross-linked structure to form another-C-N-bond, and a tri-cross-linked network structure is formed in the obtained fluororubber nanocomposite, so that the ternary fluororubber has better strength and heat conductivity.
Description
Technical Field
The invention belongs to the technical field of polymer material preparation, and particularly relates to a modified ternary fluororubber nanocomposite and a preparation method thereof.
Background
The ternary fluorine rubber is a terpolymer containing a large number of C-F bonds, has excellent high-temperature resistance, medium resistance and physical and mechanical properties due to the special structure, shows better processing performance in aromatic hydrocarbon, ethanol, methanol, water, steam and acid, has similar or better fluid resistance, is mainly applied to aerospace, automobiles, petroleum and natural gas industries and other high-temperature environments at present, and is also applied to gaskets, sealing rings, rubber tubes, dipped products, protective articles and the like.
The requirement on the strength and the thermal stability of the ternary fluororubber under the high temperature condition is high, and how to improve the heat resistance and the stability of the ternary fluororubber material under the high temperature condition is a popular research direction at present. Patent CN109233157A discloses a heat-conducting fluororubber. Adding fluororubber, magnesium oxide, calcium hydroxide, microcrystalline wax, an accelerator, a vulcanizing agent and a modified heat-conducting filler into an open mill, stirring and mixing for 30-40 min at the temperature of 100-120 ℃ and the rotating speed of 300-400 r/min, and vulcanizing for 10-30 min at the temperature of 160-180 ℃ to obtain the heat-conducting fluororubber. The prepared rubber has excellent heat-conducting property, but the filler treatment process and the rubber refining process are too complicated and are not suitable for general application.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a modified ternary fluororubber nanocomposite and a preparation method thereof.
A preparation method of a ternary fluororubber nanocomposite with a three-crosslinking network structure comprises the following steps:
(1) the following raw materials were weighed:
(2) the ternary fluororubber, an acid-absorbing agent, an accelerator, a vulcanizing agent, an aminated multi-walled carbon nanotube and graphene are mixed in an open mill at the temperature of 48-52 ℃ and uniformly mixed to obtain a mixed rubber;
(3) vulcanizing the rubber compound refined in the step (2) in a flat vulcanizing machine and pressing the rubber compound into rubber sheets;
(4) and (3) putting the rubber sheet into an oven for second-stage vulcanization to prepare the fluororubber nanocomposite with the three-crosslinking network structure.
The ratio of the aminated multi-walled carbon nanotube to graphene is 1: 1.
The aminated multi-walled carbon nanotube accounts for 5 parts by mass.
Wherein, in the step (2), the open mill conditions comprise: the rotation speed is 25-30 rpm.
Wherein in the step (3), the processing temperature in the plate vulcanizing machine is 165-175 ℃, and the time is 7-11 min.
In the step (4), the secondary vulcanization is carried out in an oven, wherein the oven temperature is 230-240 ℃ and the time is 2-16 h.
The ternary fluororubber nanocomposite with the three-crosslinking network structure prepared by the preparation method of the ternary fluororubber nanocomposite with the three-crosslinking network structure.
The invention has the following beneficial effects: according to the invention, the untreated aminated multi-walled carbon nanotubes and graphene are directly added during open milling feeding, then open milling and vulcanization are carried out, the aminated multi-walled carbon nanotubes and graphene and the ternary fluororubber matrix respectively form a cross-linked structure, meanwhile, the aminated multi-walled carbon nanotubes and graphene also generate a cross-linked structure to form another-C-N-bond, and a tri-cross-linked network structure is formed in the obtained fluororubber nanocomposite, so that the fluororubber has better strength and heat conductivity.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is within the scope of the present invention for those skilled in the art to obtain other drawings based on the drawings without inventive exercise.
FIG. 1 is a test chart of the tensile strength of a composite material;
FIG. 2 is a test chart of elongation at break of the composite material;
FIG. 3 is a test chart of 100% stress at definite elongation of the composite material;
FIG. 4 is a test chart of the hardness of the composite material;
FIG. 5 is a test chart of thermal conductivity of a composite material;
FIG. 6 is a graph of Thermogravimetry (TG) of a composite;
FIG. 7 is a test chart of thermogravimetric analysis (DTG) of the composite material;
FIG. 8 is a test chart of the char yield of a composite material;
fig. 9 is a Scanning Electron Microscope (SEM) test image of the composite material, (a) S9; (b) s10; (c) s11; (d) s12; (e) MWCNT-A; (f) graphene;
FIG. 10 is a graph of Fourier Infrared Spectroscopy (FTIR) measurements of a composite material.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings.
In the following examples and comparative examples, the following starting materials were used:
ternary fluororubber (GF-600S), DuPont, USA; aminated multiwall carbon nanotube (MWCNT-A, purity)>95 percent, the amino content is 0.7mmol/g), Shenzhen Zijing graphene science and technology Limited; graphene, henna taiji chemical products limited; 2, 5-dimethyl-2, 5-bis (t-butylperoxy) hexane (
101-50D), Yuyao Mingri chemical Co., Ltd, used as a vulcanizing agent; triallyl isocyanurate (TAIC), rhine chemical (Qingdao) ltd, used as an accelerator; zinc oxide (ZnO), yangzhou zigzagzn limited, is used as an acid acceptor.
The preparation method comprises the following steps:
(1) the weighed ternary fluororubber, the acid absorbent, the accelerator, the vulcanizing agent and the carbon material are milled in an open mill, and the feeding sequence is as follows: and (3) refining the ternary fluororubber to have rubber viscosity, and adding an acid absorbing agent, an accelerator, a vulcanizing agent, an aminated multi-wall carbon nano tube and graphene in batches.
The open mixing temperature is 48-52 ℃, the optimal temperature is 50 ℃, and the mixture is uniformly mixed to obtain the rubber compound.
(2) The refined rubber compound is pressed into rubber sheets in a flat vulcanizing press.
(3) And (3) putting the rubber sheet into an oven for second-stage vulcanization to prepare the fluororubber nanocomposite with the three-crosslinking network structure.
(4) Carrying out performance test on the prepared nano composite material, wherein the tensile property is tested according to the method in GB/T528-2009; the Shore hardness is tested according to the method in GB/T6031-2017; the thermal conductivity was tested according to the method in GB/T11205-2009.
Example 1:
100 parts of ternary fluororubber, 3 parts of zinc oxide, 3 parts of TAIC,
101-50D 5 parts, 5 parts of aminated multi-walled carbon nanotube and 5 parts of graphene. The feeding sequence is as follows: the ternary fluororubber is refined to have the glue viscosity, the zinc oxide and the TAIC are added after being uniformly mixed for 8-10 times,
adding the mixture for 2-4 times in 101-50D, and adding the mixture for 10 times after uniformly mixing the aminated multi-walled carbon nanotube and the graphene. Taking out after the open milling is finished, standing for 24h, and then back millingVulcanizing on a flat vulcanizing machine, preparing a sample, and testing the rubber performance. The resulting composite is designated S12.
Comparative example 1:
100 parts of ternary fluororubber, 3 parts of zinc oxide, 3 parts of TAIC,
101-50D 5 parts, and 0 part of aminated multi-walled carbon nanotube and 0 part of graphene. The feeding sequence is as follows: the ternary fluororubber is refined to have the glue viscosity, the zinc oxide and the TAIC are added after being uniformly mixed for 8-10 times,
adding the 101-50D into the mixture for 2-4 times. And taking out the rubber after the open milling is finished, standing the rubber for 24 hours, then carrying out the back milling, vulcanizing the rubber on a flat vulcanizing machine, preparing a sample, and testing the performance of the rubber. The resulting composite is designated S9.
Comparative example 2:
100 parts of ternary fluororubber, 3 parts of zinc oxide, 3 parts of TAIC,
101-50D 5 parts, 5 parts of aminated multi-walled carbon nanotube and 0 part of graphene. The feeding sequence is as follows: the ternary fluororubber is refined to have the glue viscosity, the zinc oxide and the TAIC are added after being uniformly mixed for 8-10 times,
adding the mixture for 2-4 times in 101-50D, and adding the aminated multi-walled carbon nanotube for 5 times. And taking out the rubber after the open milling is finished, standing the rubber for 24 hours, then carrying out the back milling, vulcanizing the rubber on a flat vulcanizing machine, preparing a sample, and testing the performance of the rubber. The resulting composite is designated S10.
The aminated multi-walled carbon nanotubes were reduced to 1 part and 3 parts, and the composites prepared were designated as S1 and S2, respectively, and the rubber properties were tested.
TABLE 1 Effect of the amount of aminated multiwall carbon nanotubes used on the Properties of the composite
In table 1, S9, S1, S2, and S10 are samples prepared by using 0 part, 1 part, 3 parts, and 5 parts of aminated multi-walled carbon nanotubes, respectively, and it can be seen from table 1 that when the amount of aminated multi-walled carbon nanotubes is 5 parts, the tensile strength, 100% stress at definite elongation, hardness, and thermal conductivity of the composite material are the highest, and the performance is the best.
The composite materials prepared by specifically adopting aminated multi-wall carbon nano-tubes with the tube lengths of 5-15 microns, 10-30 microns and 20-50 microns are respectively marked as S3, S4 and S5.
TABLE 2 Effect of tube length of aminated multiwall carbon nanotubes on various properties of composites
As can be seen from table 2, the carbon material with a long tube length performed better in various properties.
Comparative example 3:
100 parts of ternary fluororubber, 3 parts of zinc oxide, 3 parts of TAIC,
101-50D 5 parts, 0 part of aminated multi-walled carbon nanotube and 5 parts of graphene. The feeding sequence is as follows: the ternary fluororubber is refined to have the glue viscosity, the zinc oxide and the TAIC are added after being uniformly mixed for 8-10 times,
adding 101-50D for 2-4 times, and adding graphene for 5 times. And taking out the rubber after the open milling is finished, standing the rubber for 24 hours, then carrying out the back milling, vulcanizing the rubber on a flat vulcanizing machine, preparing a sample, and testing the performance of the rubber. The resulting composite is designated S11.
As shown in FIG. 1, in the composite material, the tensile strengths of S9, S10, S11 and S12 were 11.9MPa, 17.4MPa, 11.6MPa and 19.7MPa, respectively. Compared with S9, the tensile strength of S10 is improved by 46.2 percent, which shows that the tensile strength of the modified fluororubber is effectively improved due to the double-crosslinked network structure formed by MWCNT-A and the rubber matrix; the tensile strengths of S9 and S11 were comparable, indicating that graphene does not contribute much to improving tensile strength; and when the MWCNT-A and the graphene are added for synergistic modification, the tensile strength of S12 is respectively improved by 65.5% and 13.2% compared with that of S9 and S10, which shows that in addition to a double-crosslinking network structure, another crosslinking structure can also appear in the rubber, namely, a new crosslinking point is generated between the graphene and the MWCNT-A to form another-C-N-bond, and the three-crosslinking network structure enables the fluororubber to be broken under a larger force action, so that the S12 shows higher tensile strength.
As shown in fig. 2, the elongation at break at S9, S10, S11, and S12 were 402%, 203%, 322%, and 182%, respectively. As can be seen from the figure, the elongation at break of the modified fluororubber is reduced to different degrees after the carbon material is added, and the result of the carbon nano tube and the natural fiber reinforced rubber also shows that the reduction shows that the interaction force between the carbon material and the rubber is increased, the movement of rubber molecular chains is prevented, and the three-crosslinking network structure further limits the movement of the fluororubber molecular chains, so that the elongation at break of the modified fluororubber is reduced.
As is clear from fig. 3 and 4, the same results as the tensile strength were also shown in the 100% stress at definite elongation. The appearance of the three-crosslinking network structure leads the deformation of the sample to require larger stress, so that the 100 percent stress at definite elongation of the modified fluororubber is obviously improved, and the hardness is also obviously improved. The hardnesses of S9, S10, S11 and S12 were 53.9, 69.8, 60.3 and 72.5, respectively, and the hardnesses of S10, S11 and S12 were increased by 29.5%, 11.9% and 34.5%, respectively, compared with S9, indicating that both MWCNT-A and graphene can increase the hardness of fluororubber.
As can be seen from FIG. 5, the thermal conductivities of S9, S10, S11 and S12 were 0.1943W/(m.K), 0.2488W/(m.K), 0.1968W/(m.K) and 0.2476W/(m.K), respectively. After the MWCNT-A with the concentration of 5% is adopted for modification, compared with S9, the heat conductivity coefficient of S10 is improved by 28.0%; after 5% of graphene is adopted for modification, the difference between the heat conductivity coefficient and S9 is not great; compared with S9, the modified fluororubber S12 synergistically enhanced by MWCNT-A and graphene has the advantage that the thermal conductivity is improved by 27.8%. It can be seen that the network formed by MWCNT-A provides a good thermal conduction path, showing a significant increase in thermal conductivity in S10. The network formed by the graphene not only provides a heat conduction channel, but also generates a layered barrier effect, and the two functions are mutually counteracted, so that the heat conduction performances of S10 and S12 are not greatly different.
FIG. 6 is a Thermogravimetric (TG) curve of the modified fluororubber, and Table 3 shows the weight loss ratio and corresponding temperature of the modified fluororubber. As can be seen, the initial decomposition temperature of S9 was reduced after MWCNT-A was used; after the graphene and MWCNT-A are adopted for modification, the temperature of 5% and 10% of weight loss of S11 and S12 is improved, and the initial decomposition temperature of S11 is reduced to a small mutextent.
TABLE 3 weight loss ratio and corresponding temperature of the composite
As can be seen from fig. 7, there are two decomposition processes for the composite material: the first peak is that the rubber is partially decomposed firstly and then is subjected to dehydrogenation reaction; the second peak is the onset of rapid rubber decomposition. As can be seen from the figure, the first endothermic decomposition peak of S12 is delayed after the modified fluororubber is synergistically reinforced by MWCNT-A and graphene. The first exothermic peaks of S10 and S11 slightly advanced, probably due to the dehydrofluorination reaction during the temperature rise to generate HF which reacts with the amino groups on the MWCNT surface. And compared with GO, graphene in S12 has a more complete structure and is not easy to generate dehydrofluorination reaction with HF, so that the absorption peak is shifted backwards.
As can be seen from fig. 8, the carbon residue ratio of fluororubber modified with the carbon material was increased from 6.6% in S9 to 15.2% and 15.7% in S11 and S12, and the carbon residue ratios were increased by 130.3% and 137.9%, respectively.
As can be seen from FIG. 9, the S9 section where MWCNT-A and graphene were not added was slightly uneven; the surface of S10 with only MWCNT-A added is relatively flat, and part of MWCNT-A is mut mutextracted from the fluororubber; only part of graphene is exposed on the cross section of S11 added with graphene; s12 section of MWCNT-A and graphene synergistically modified has obvious wrinkled structure. FIG. 9(e) is an SEM photograph of MWCNT-A, which shows a higher tensile strength in the modified fluororubber due to a larger length-diameter ratio of MWCNT-A and acts as stress transfer and reinforcement to the fluororubber during stretching, and also shows a lower elongation at break and a flatter cross section due to the rigidity of MWCNT-A itself and a smaller elongation at break of S10. Since graphene has a sheet structure, as shown in fig. 9(f), the chain slip performance during stretching is improved, and the elongation at break of S11 is increased compared to S10. When the MWCNT-A and the graphene are cooperatively used for reinforcing the fluororubber, a three-crosslinking network structure is formed, so that the strength of S12 is improved, the movement of rubber molecular chains is hindered, a wrinkle-like structure is formed on a tensile section, and the elongation at break is reduced.
As can be seen from FIG. 10, 1000 to 700cm-1The C-H out-of-plane bending vibration of the olefin is 1400-730 cm-1Is the stretching vibration of C-F, 897cm-1，1398cm-1Has a peak of CH2＝CF2Characteristic absorption peak of (1), 1184cm-1The extremely strong peak is the characteristic absorption peak of C-F, 1694cm-1The peak is the characteristic absorption peak of amide, 2850cm-1And 2920cm-1Has a peak of-CF2Characteristic absorption peak of (E). The baseline was inclined to various degrees depending on the amount of the carbon material added. The characteristic absorption peaks of the four composite materials after the carbon material is added are basically consistent, which indicates that the chemical bonds are basically the same, no new functional groups appear, and the chemical reaction is probably generated, but the newly formed chemical bonds are the same as the previous chemical bonds in type.
The above disclosure is only for the purpose of illustrating the preferred embodiments of the present invention, and it is therefore to be understood that the invention is not limited by the scope of the appended claims.
Claims (7)
1. A preparation method of ternary fluororubber nanocomposite with a three-crosslinking network structure is characterized by comprising the following steps:
(1) the following raw materials were weighed:
100 parts of ternary fluororubber;
1-5 parts by mass of an acid acceptor;
1-5 parts of an accelerator;
1-5 parts by mass of a vulcanizing agent;
1-10 parts by mass of aminated multi-walled carbon nanotubes;
1-10 parts by mass of graphene;
(2) the ternary fluororubber, an acid-absorbing agent, an accelerator, a vulcanizing agent, an aminated multi-walled carbon nanotube and graphene are mixed in an open mill at the temperature of 48-52 ℃ and uniformly mixed to obtain a mixed rubber;
(3) vulcanizing the rubber compound refined in the step (2) in a flat vulcanizing machine and pressing the rubber compound into rubber sheets;
(4) and (3) putting the rubber sheet into an oven for second-stage vulcanization to prepare the fluororubber nanocomposite with the three-crosslinking network structure.
2. The method for preparing a ternary fluororubber nanocomposite material with a triple crosslinked network structure according to claim 1, characterized in that: the ratio of the aminated multi-walled carbon nanotube to graphene is 1: 1.
3. The method for preparing a ternary fluororubber nanocomposite material with a triple crosslinked network structure according to claim 1, characterized in that: the aminated multi-walled carbon nanotube accounts for 5 parts by mass.
4. The method for preparing a ternary fluororubber nanocomposite material with a triple crosslinked network structure according to claim 1, characterized in that: wherein, in the step (2), the open mill conditions comprise: the rotation speed is 25-30 rpm.
5. The method for preparing a ternary fluororubber nanocomposite material with a triple crosslinked network structure according to claim 1, characterized in that: wherein in the step (3), the processing temperature in the plate vulcanizing machine is 165-175 ℃, and the time is 7-11 min.
6. The method for preparing a ternary fluororubber nanocomposite material with a triple crosslinked network structure according to claim 1, characterized in that: in the step (4), the secondary vulcanization is carried out in an oven, wherein the oven temperature is 230-240 ℃ and the time is 2-16 h.
7. The ternary fluororubber nanocomposite of a triple crosslinked network structure produced by the process for producing a ternary fluororubber nanocomposite of a triple crosslinked network structure according to any one of claims 1 to 6.
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