专利摘要:
1448328 Modified bromobutyl rubber POLYSAR Ltd 5 Nov 1974 [8 Nov 1973] 47856/74 Heading C3P Bromobutyl rubber is modified by reaction with any of a number of types of tertiary amines, defined by general formulµ, in an amount of 1/100th to 1/8th chemical equivalent of amine per chemical equivalent of bromine. The product has improved green strength, and may be blended with other rubbers and with conventional compounding ingredients. In examples, the amines used are N,N,N<SP>1</SP>,N<SP>11</SP>,N<SP>111</SP>,N<SP>111</SP>-hexamethyltriethylene tetramine, triethylene diamine, N,N-dimethyl benzylamine, N-methylpiperidine, N,N,N<SP>1</SP>,N<SP>1</SP> - tetramethylhexamethylene diamine, N,N-dimethyldodecylamine, N,N - dimethyloctadecylamine and N,N-dimethylhexylamine.
公开号:SU764612A3
申请号:SU742073496
申请日:1974-11-06
公开日:1980-09-15
发明作者:Джек Баклер Эрнест;Фениак Джордж
申请人:Полисар Лимитед (Фирма);
IPC主号:
专利说明:

one
The invention relates to the rubber industry, in particular, to the development of a method for the modification of bromobutyl rubber.
A known method of modifying bromobutyl rubber by mixing with an organic amine, for example, phenylamine; with subsequent aging at 160 ° C. fi.
Rubber obtained on the basis of known rubber, have insufficient strength properties.
The purpose of the invention is to improve the strength properties of rubbers based on modified bromobutyl rubber.
The goal is achieved by the method of modifying a bromobutyl rubber by mixing with an organic amine followed by an extract using an organic amine selected from the group: methyl (ethyl) piperidine, methyl (ethyl) piperazine, triethylenediamine, action
four,
fh
formulas
/
Kg
where R, Rg is ethyl, methyl
X is C5-C o-alkyl, benzyl,
,, d-alkylene, including as a substitute
N-x
X
ten
And exposure is carried out at 25-150 ° C for 1-48 hours.
Example 1. The bromobutyl rubber used has a Myi. Number of 45 and contains
IS 2.0 wt.% Bromine.
 Bromobutyl rubber (IBD) samples are reacted with various amounts of a number of amines. Reaction
2 & between the rubber and the amine is carried out at the intermixing of the rubber in the mill at about the addition of the necessary amount of amine. The polymer is then rolled into a sheet.
25 and heated in an air circulating dryer for 16 hours in order to ensure that the reaction of the amine with the polymer is complete. A composition is prepared from the obtained polymer according to the following formulation, parts by weight.
Polymer100
Soot62,5
Mineral oil 14.0
2.2-Dithiobisbenzothiazole (accelerator
vulcanization) 1.25
Resinous adhesive
vetzhestvo4,0
Stearic acid 1.0
zinc oxide 5.0
Sulfur0.5
The strength of this composition is then determined in its unvulcanised state.
Table 1 shows the names of the amines used, their amount and the results of measuring the strength of the composition in the unvulcanized state at room temperature. The results clearly show the increased strength of the unvulcanized polymer composition.
In addition, samples of these compositions are ground at approximately and extruded at. and a screw rotation speed of 70 rpm. It was found that, basically, the characteristics of the composition during grinding and extrusion do not differ significantly from similar characteristics of the composition before grinding.
Example 2. The bromobutyl polymer samples described in Example 1 are then treated with various amounts of monoamines, such as: N, N-dimethyldodecylamine, N, N-dimethyloctadecylamine and M, M-dimethylhexylgly The treatment is carried out in a mill, as in Example 1 and then perform the same heat treatment. From the obtained treated samples of bromobutyl polymer, the compositions are prepared according to the formulation described in Example IFa and then they are tested.
The results are presented in table 2.
Grinding and extrusion is carried out on samples treated with M, N-dimethyldodecylamine in the amount of 0.45 weight.h, per 100 weight.h. bromobutyl rubber.
The solvent in cyclohexane of the starting bromobutyl is 96.4%; the solubility of the polymer, processed; N, M-dimethyloctadecyl-AU is 91.3%, i.e. no significant change in solubility.
Example 3 A portion of the samples (described in example 1, processed and mixed into a composition as described) are tested to determine the time for premature vulcanization. and then answer. The resulting curing agents are stretched.
The results are presented in table 3. From these results, it can be seen that no significant effect on the properties of the vulcanizates is found.
Example 4. Samples of bromobutyl rubber from example 1 are treated with N, N-dimethyloctadecylamine (0.4 weight.h.
at 1.00 weight.h. bromobutyl rubber)
As described in Example 1, it is heat-treated and blended into a composition for making tire liners. The strength of the composition in an unvulcanized state is determined.
and also tests are performed to determine the time of premature vulcanization, then the compositions are cured and the vulcanizates are tested to determine tensile properties.
When compared with a control sample based on the known bromobutyl, it was found that the properties of the vulcanizates of the compositions according to the invention did not change significantly. Improved
the strength of the compositions in the unvulcanized state appears when they are mixed with the second rubber.
; Table 4 presents the formulations of the preparation of the compositions and the results of tests of vulcanizates.
Example 5. Samples of bromobutyl rubber from example 1 is treated
dodecylamine or octadecylamine, as described in example 1, and heat-treated for 16 hours at / 90 ° in an oven. Processed samples of bromobutyl rubber are tested for strength
compositions in an unvulcanized state as previously described.
The results are presented in table.5. As follows from the table.1-5, the proposed method of modifying BBK has
mainly before the well-known for its durable properties and the possibility of recycling at elevated temperatures of 1X.
 9S
a s t; with
nS f
 Table
Properties of compositions based on modified bromobutyl rubber from viya organic amine
N, M-, y1 methyldocylamine, wt. per 100 weight parts rubber
N, N-Dimethyloctadecylamine, parts by weight per 100 weight parts
H, N-Dimethylhexylamine, parts by weight per 100 weight parts rubber
Elongation at the peak,%
Maximum tensile strength at break, kgf / s
Module at 100% elongation, kg / cm
Module at 200% elongation, kg / cm
dM,%
   T a b l and c a 3
Properties of compositions based on modified in accordance with example 1 bromobutyl rubber
The time of premature zulcanization t ,, m
Strength at break, kgf / cm
Elongation,%
Module at 300% elongation, kGS / cm
0.45
0.47
0.30
1000
90
15
14 3.2.
5.0 4.8
4.2
3.2
5.7 5.2
4.6
2.8 14 8.3 8.7 -12.5
15
12
99
100 680 600
47
43 Composition of rubber compounds and properties of rubber from them
- -t- - - - - .TBLii :, - - --- -.
The known method - 75 - 100
Processed bromobutyl rubber 75 - 100
Natural rubber corrugated smoked-sheets
Soot
Stearic acid
Resinous adhesive
Mineral Oil Zinc Oxide
1.25 1.25 1.25 1.25
 .
 0.20
- - 0.5 0.5 8 min
40 s
% 940 900 900 940, 90 900
6,42,69,4. 3,52,6-4,1
. 3.8 2.3 4.5
n
. 107 111 101
655 580 765
1012 10
, T a b l and c a 4
8 min 8 min 8 min 11 s 17 s 6s
1000
90
2.8 2.8
2.5
102
765
-liU:
Properties of compositions based on modified: cyaned bromobutyl rubber
Dodedylamine, wt.h. per 100 weight parts bromobutyl rubber
Octadecylamine, wt.h. on. 100 weight.h. bromobutyl rubber
Elongation at break,%
Maximum tensile strength
A method of modifying brOMBUTILKauch by mixing with an organic amine followed by support, with the aim of improving the strength properties of rubbers based on this rubber, to use an organic amine selected from the group: methyl i (ethyl) piperidine , methyl (ethyl) piperazi triethylenediamine, am n of formula
-.
Kg
Table 5
0.3 350
where R.R is ethyl, methyl,
X - Su-C d-alkyl, benzyl,
Cd-CjQ-alkylene, including as a substituent
N-x
and the suspension is carried out at 25-150 ° C for 1-48 hours.
Sources of information taken into account in the examination
1. Vulcanization of elastomers. M., Himi, 1967, p. 271-273 (prototype) ..
权利要求:
Claims (1)
[1]
Claim
A method of modifying bromobutyl rubber by mixing with an organic amine followed by aging, which is used: In order to improve the strength properties of rubbers based on this rubber, organic amine selected from the group of methyl ί (ethyl) piperidine, methyl (ethyl) piperazine triethylenediamine, amine of formula
thirty
Ν-Χ
where K4 is ethyl, methyl,
x ~ C 5 - C ao- alkyl, benzyl,
Cd-C £ O- alkylene, including as a substitute
Ν-Χ
35
Ig
40
and holding is carried out at 25-150 C for 1-48 hours.
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同族专利:
公开号 | 公开日
DE2452915A1|1975-05-15|
AU7501174A|1976-05-06|
CA1030699A|1978-05-02|
IN142949B|1977-09-10|
BR7409212A|1976-05-11|
DE2452915C2|1984-08-16|
GB1448328A|1976-09-02|
BE821862A|1975-05-05|
JPS5714681B2|1982-03-26|
FR2250799A1|1975-06-06|
AR202732A1|1975-07-15|
NL172328C|1983-08-16|
ZA747152B|1976-05-26|
US4256857A|1981-03-17|
JPS5089449A|1975-07-17|
NL172328B|1983-03-16|
ES431649A1|1976-11-01|
FR2250799B1|1980-03-28|
NL7414516A|1975-05-12|
IT1024751B|1978-07-20|
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法律状态:
优先权:
申请号 | 申请日 | 专利标题
CA185,311A|CA1030699A|1973-11-08|1973-11-08|Halobutyl of improved green strength|
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