Process for making flexible rubbers

专利摘要:
A process, and the product thereof, is provided for the production of improved silica filled rubbery vulcanizates which process comprises mixing a vulcanizable hydrocarbyl polymer containing epoxy groups and silica, shearing the mixture at an elevated temperature, incorporating vulcanization active compounds and vulcanizing. The vulcanizates may be used where reinforced vulcanizates are required.
公开号:SU1037843A3
申请号:SU782603200
申请日:1978-04-13
公开日:1983-08-23
发明作者:Камерон Эдвардс Дуглас；Сато Киосаку
申请人:Полисар Лимитед (Фирма)；
IPC主号:

专利说明:

SLE vj
00
WITH
The invention relates to the rubber industry, in particular, to a process for producing elastic rubber.
A known method for the preparation of elastic rubbers by mixing an epoxy-containing carbage, pnou rubber with silica and a vulcanizing agent, for example, amine f1J.
Rubber from a known mixture have poor physical and mechanical properties.
The purpose of the invention is to improve the physicochemical properties of rubber.
The goal is achieved by the fact that according to the method of producing elastic rubbers by mixing epoxy-containing carbon chain rubber with silicon dioxide, a vulcanizing agent, Kap6 chain rubber — glycidyl methacrylate copolymer — with butadiene and styrene or acrylonitrile is mixed with the 4–60 mm copolymer with butadiene and styrene or acrylonitrile when the content of the 4–60 mm is combined with butadiene and styrene or acrylonitrile, while the content of the first 4–60 mm is combined with butadiene and styrene or acrylonitrile when the content of the first 4–60 mm is mixed with the butadiene and styrene or acrylonitrile, while the content of the first 4–60 mm is combined with butadiene and styrene or acrylonitrile. weight.h. silicon dioxide and a vulcanizing agent at 150 ° C for 3 minutes under shear force, followed by vulcanization at 160-16b C for 15-30 minutes.
Example 1. Using a conventional polymerization method without an emulsion for polymerization, a series of polymers are prepared which contain from 0 to 2% by weight of glycidyl methacrylate, about 34% by weight, acrylonitrile and for equilibrium with butene diene.
Samples of these polymers are mixed in 50 weight.h. per 100 weight. including polymer containing silica with a fine particle size. Some of these compounds are heat treated on a roll for 3 minutes at. The other part of the compounds are not heat treated.
After cooling to ambient temperature, each compound is treated at. rollers operating at 40c, added dicumyl peroxide, and carefully dispersed. Then these compounds are vulcanized by heating for 30 minutes at 1 ° C.
In tab. Figure 1 shows the compounds that are heat treated, the amount of dicumyl peroxide added (in weight, parts per 100 weight, polymer h) and the properties of the vulcanized.
The results show that even with a bound glycidyl methacrylate level of 0.5 wt. % vulcanizer has improved properties when the compound has been heat treated. When the level of gliandylmeth krylate in the polymer is about 1 wt. %, a significant improvement is achieved in the properties of the vulcanite. Experiment 1 is a control and shows the state of the art in which a silica filler and a polymer that does not contain epoxy groups are used.
Example 2. A polymer of a composition similar to that of polymer from experiment 3 in example 1, i.e. containing 34 wt. % Acrylonitrile and 1 weight. % glycidyl methacrylate.
0 One part of the polymer is combined with 60 parts by weight. silica, heat treated by rolling for 3 minutes at 150 seconds, cooled, combined with 5 to 3.5 wt.% dicumyl peroxide and vulcanized by heating at 30 minutes.
The other part of the polymer is combined with 60 parts by weight, silica, 2 weight, h. zinc stearate and 12.5 wt.h dioctyl phthalate. Then this part of the polymer is heat treated by rolling at 150 ° C for 30 minutes, cooled, combined with 5 parts by weight of zinc oxide,. 5 1.5 weight.h, stearic acid and 3.5 weight% of dicumyl peroxide are vulcanized by heating for 15 minutes.
The third part of the polymer is combined with 60 weight, h, silica;
2 wt.h, zinc stearate and 12.5 wt .; dioctyl phthalate. Then the polymer is subjected to heat treatment, the roller for 3 minutes 5 After cooling, the polymer is combined with 5 parts by weight. oxide cynic, 1.5 weight.h. stearic acid, -1.5 weight.h. benzothiazyl disulfide, 0.5 weight.h. tetramethylthiuram disulfide and 1.75 weight, h, sulfur, and vulcanized by heating at 166 ° C for 15 minutes.
The composition of the mixture and the properties of the volcanicate are shown in Table. -2
The properties of the volcanizer for Experiment 6 are similar to those of Vulcanizate from Experiment 4B in Example 1, and it is indicated that, in the presence of other compounds during the heat treatment, it does not significantly affect the properties of the vulcanizate. Through the use of sulfur as a vulcanizing agent, a vulcanizate is obtained, having properties similar to those of the improved peroxide-derived vulcanizates.
The composition of the mixtures and the properties of rubber are given from them .; in tab. 2
Example 3: Comparison of a copolymer of butadiene and acrylonitrile, containing 34% by weight. The% acrylonitrile and having a Mooney viscosity of 50 is combined with carbon black and docculat peroxide and the properties of the volcanic edetate are determined.
The properties of the vulcanizer are compared 5 with the properties of the vulcanizates obtained according to the invention. It is noted that the invention eliminates known problems by using silica as a filler.
The composition and properties of rubber are given in table. 3 ..
Example 4. Polymer containing styrene (weight,%), butadiene and glycidyl methacrylate (v / 1 weight,% is pressed using the conventional method of radix polymerization without emulsion at 10 ° C. Part of the polymer is combined with 50 ve, including silica) 100 weight, h, polymer. Then this compound is heat treated on a roll for 3 min. After cooling, 0.67 weight, part of dicumyl peroxide (Di Cup 40C) per 100 weight, h, of polymer is added by kneading "Cah for rubber at. The resulting mixture is subjected to vulcanization by heating it for 30 minutes at
,
As a control, a sample (100 weight, h) of a copolymer containing styrene and butadiene, which contains 23 weight. % styrene and has a Mooney viscosity (ML 1 + 4 at 1.00 ° C) of about 51, mixed with 50 parts by weight, silica and 0.5 parts by weight. antioxidant, namely 2,6-two-butyl-α-methylphenol. Oles is subjected to heat treatment as indicated by BEL, then 2.0 wt. dicumyl peroxides and vulcanized by a similar method. As a benchmark example, a co-meter containing styrene
Associated CMA, weight,% Heat treated No compound
The amount of dicumyl peroxide, wt.% 1,5 1,5
Vulcanizate properties Tensile strength, kg / LM 318 298 332 680 660 560 Elongation,%
and butadiene, are treated in the manner described above, except for the heat treatment stage. four,
From tab. 4 shows a significant decrease in Young's modulus and a sufficient elongation for experiment A, which is in accordance with the invention,.
PRI me R 5. Apply a polymer composition similar to the composition of example 2, 100 weight, h. the polymer is mixed with 60 weight.h, silica, 12.5 weight.h. dioctyl phthalate and
 additives shown in the table. five.
With the exception of the control in Experiment 9, these compounds are then subjected to shear deformation when raised. temperature for 3 minutes at 150 ° C for rubber. After cooling, the mixture is mixed with active elements listed in Table. 5, and vulcanized by heating at for: 15 minutes Properties have been identified
5 vulcanizers, and it was shown that shear deformation at elevated temperature is necessary and that the presence of geekin or metal stearate, while shear deformation at elevated temperature, does not prevent the achievement of improved properties in vulcanizates; I -
As can be seen from the data presented. With respect to 1–1), the rubber from the proposed mixture is characterized by the best physical and mechanical properties; properties compared to known.
| TaOlica 1
0.7
1.0
2.0
1.5 1.5 1.5 1.5
40 DAG 278 281 341 263 279 400 630 450 310 250
Stress at elongation at 100% 5 kg / cm
25
Stress at elongation of 300%, kg / cm 58
Stress at elongation by 25%, kg / cm 12 11 13. eleven
Young's modulus, kg / cm
162 153 122
Residual elongation,% 25
Shore hardness, A2 78
Dicumyl peroxide
(Vulcanization time, min
Continued table.
40
27 43
26 40 50 75
80 152
199
90 210 239
11 10 12 15
151 59 89 72
94
15
15
85 75 85 77
85 79
78
3.5 15
15
1037843
.2
Continued tab
Heat treatment at 150 ° C for 3 minutes
Dicumyl peroxide, weight. h
Vulcanizate properties
tensile strength.
Table 4
Yes 2
No 2
Yes 0.67
- - No Yes Yes Yes,
- - -5- about

- - 1.5 g t, 5 1.5 1.5 1.5
Continued table. five
Yes
Yes
Yes

权利要求:
Claims (1)
[1]
METHOD FOR PRODUCING ELASTIC RUBBERS by mixing epoxy-containing carbochain rubber with silicon dioxide, a vulcanizing agent, characterized in that, in order to increase the physicomechanical properties of the rubbers, carbochain rubber - a glycidyl methacrylate copolymer - with butadiene and first styrene 60 mmol acrylate or 4 mm acrylate is mixed 100 g of a copolymer with 50-60 parts by weight silicon dioxide and a vulcanizing agent at 150 ° C for 3 min under shear, followed by vulcanization at 160-166 ° C for 15-30 min.
§ £ Λ in
GO with

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引用文献:

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法律状态:

优先权:

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申请号 | 申请日 | 专利标题

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CA276,158A|CA1094720A|1977-04-14|1977-04-14|Silica filled vulcanizates|

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