CN103865129A - Preparation method of high-performance antioxidant of butyronitrile rubber latex - Google Patents
Preparation method of high-performance antioxidant of butyronitrile rubber latex Download PDFInfo
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- CN103865129A CN103865129A CN201410127261.XA CN201410127261A CN103865129A CN 103865129 A CN103865129 A CN 103865129A CN 201410127261 A CN201410127261 A CN 201410127261A CN 103865129 A CN103865129 A CN 103865129A
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Abstract
The invention relates to the technical field of antioxidant preparation methods, and in particular relates to a preparation method of a high-performance antioxidant of butyronitrile rubber latex. The preparation method disclosed by the invention comprises the following steps: mixing an emulsion type primary antioxidant of 2,2'-methylene-bis-(4-methyl-6-tert-butylphenol), paracresol and dicyclopentadiene butylated products with a tri[2,4-di-tertiary butyl-phenyl] phosphite ester emulsion type auxiliary antioxidant according to a certain proportion, and uniformly dispersing by stirring mechanically, wherein the viscosity of the formed emulsion is 0.2-2 pa.s, and the average particle size is less than or equal to 2 mu m. Compared with the prior art, firstly, the antioxidant prepared by the preparation method disclosed by the invention has the advantages of being good in antioxidant effect, high in heat-resistant stability, environment-friendly, convenient for use and the like; simultaneously, by adopting tri[2,4-di-tertiary butyl-phenyl] phosphite ester, the butyronitrile rubber latex can be effectively prevented from becoming aged and yellow; the instability effect of the rubber latex does not exist.
Description
Technical field
The present invention relates to oxidation inhibitor preparation method technical field, be specifically related to a kind of nitrile rubber high-performance oxidation inhibitor preparation method.
Background technology
Nowadays, ABS, MBS, rubber, plastics, latex etc. are the important source material of daily life, its Application Areas is constantly widened, but no matter macromolecular material is natural or synthetic, all easily there is oxidizing reaction, make that material fades, yellowing, sclerosis, be full of cracks, and then cause the reduction of the physicalies such as resistance to impact shock, anti-flexing intensity, tensile strength and elongation, impact is used.Simple effective method so add oxidation inhibitor in these materials.Because single phenolic antioxidant antioxidant effect is more single, so use time taking phenolic antioxidant as primary antioxidant, select at least one method combining for auxiliary anti-oxidant in monothioester and phosphorous acid ester, produce synergistic effect, it is very important that object reaches nitrile rubber antioxidant effect.
Summary of the invention
The object of this invention is to provide and be a kind ofly mixed according to a certain percentage by different major-minor oxidation inhibitor emulsions, have that technique is simple, heat resistanceheat resistant stability is high, a nitrile rubber high-performance oxidation inhibitor preparation method of environmental protection, low power consumption and other advantages.
In order to solve the existing problem of background technology, the present invention is by the following technical solutions: a kind of nitrile rubber high-performance oxidation inhibitor preparation method, comprise that mass percent is 50～60% primary antioxidant emulsion, 40～50% auxiliary antioxidant emulsion, concrete steps are as follows.
(1), prepare primary antioxidant emulsion, be 20～50% by mass percent 2,2'-methylene-bis-(4-methyl-6-tert-butylphenol), p-cresol and dicyclopentadiene butylation product, in 6～12% sodium lauryl sulphate and polyoxyethylenated alcohol sodium sulfate at least one, and deionized water carries out mix and blend, thereby make primary antioxidant emulsion; Wherein, described 2,2'-methylene-bis-(4-methyl-6-tert-butylphenol), p-cresol and dicyclopentadiene butylation product, i.e. oxidation inhibitor KY-616(Wingstay L), antioxidant 2246.
(2), prepare auxiliary anti-oxidant emulsion, three [2.4-di-tert-butyl-phenyl] phosphorous acid ester that is 20～50% by quality percentage, in 6～12% sodium lauryl sulphate and polyoxyethylenated alcohol sodium sulfate at least one, and deionized water carries out mix and blend, thereby make auxiliary antioxidant emulsion; Wherein, described three [2.4-di-tert-butyl-phenyl] phosphorous acid ester, i.e. irgasfos 168.
(3), the above-mentioned primary antioxidant emulsion of making, auxiliary anti-oxidant emulsion are heated and mixed under mechanical stirring, be heated to 40～120 DEG C of temperature, under 220～400 revs/min of mechanical stirring, stir 20min～1h and reach even.
The present invention has following beneficial effect: a kind of nitrile rubber high-performance oxidation inhibitor preparation method of the present invention, first by 2,2'-methylene-bis-(4-methyl-6-tert-butylphenol), emulsion-type primary antioxidant and three [2.4-di-tert-butyl-phenyl] the phosphorous acid ester emulsion-type auxiliary anti-oxidant of p-cresol and dicyclopentadiene butylation product mixes by a certain percentage, is uniformly dispersed by mechanical stirring; The emulsion-type viscosity forming is 0.2～2pa.s, median size≤2 μ m, compared with prior art, first the oxidation inhibitor that this invention is produced not only has that antioxidant effect is good, heat resistanceheat resistant stability is high, environmental protection and the advantage such as easy to use, adopt three [2.4-di-tert-butyl-phenyl] phosphorous acid ester can effectively prevent the aging xanthochromia of nitrile rubber simultaneously, to latex without unsettled effect; Secondly the oxidation inhibitor emulsion that prepared by this invention, particle diameter is less, need not filter, and can directly add in nitrile rubber emulsion, disperses quick, even.In addition, the preparation method of the described oxidation inhibitor that this invention provides compared with other oxidation inhibitor, has that technique is simple, an environmental protection, low power consumption and other advantages.
Embodiment
The present invention will be further described in detail below.
Embodiment mono-: a kind of nitrile rubber high-performance oxidation inhibitor preparation method, comprise that mass percent is 60% primary antioxidant emulsion, 40% auxiliary antioxidant emulsion, concrete steps are as follows.
(1), prepare primary antioxidant emulsion, be 90g by quality 2,2'-methylene-bis-(4-methyl-6-tert-butylphenol), p-cresol and dicyclopentadiene butylation product, in the sodium lauryl sulphate of 10.8g and polyoxyethylenated alcohol sodium sulfate at least one, and the deionized water of 79.2g carries out mix and blend, thereby make primary antioxidant emulsion.
(2), prepare auxiliary anti-oxidant emulsion, three [2.4-di-tert-butyl-phenyl] phosphorous acid ester that is 60g by quality, in the sodium lauryl sulphate of 7.2g and polyoxyethylenated alcohol sodium sulfate at least one, and the deionized water of 52.8g carries out mix and blend, thereby makes auxiliary antioxidant emulsion.
(3), in 500ml tetra-hole flasks, add the above-mentioned 180g primary antioxidant emulsion preparing, 120g auxiliary anti-oxidant emulsion is heated to 40 DEG C of temperature under mechanical stirring, stirs 20min and reach even under 220 revs/min of mechanical stirring.
Embodiment bis-: a kind of nitrile rubber high-performance oxidation inhibitor preparation method, comprise that mass percent is 50% primary antioxidant emulsion, 50% auxiliary antioxidant emulsion, concrete steps are as follows.
(1), prepare primary antioxidant emulsion, be 30g by quality 2,2'-methylene-bis-(4-methyl-6-tert-butylphenol), p-cresol and dicyclopentadiene butylation product, in the sodium lauryl sulphate of 18g and polyoxyethylenated alcohol sodium sulfate at least one, and 102g deionized water carries out mix and blend, thereby make primary antioxidant emulsion.
(2), prepare auxiliary anti-oxidant emulsion, three [2.4-di-tert-butyl-phenyl] phosphorous acid ester that is 30g by quality, in the sodium lauryl sulphate of 18g and polyoxyethylenated alcohol sodium sulfate at least one, and 102g deionized water carries out mix and blend, thereby makes auxiliary antioxidant emulsion.
(3), in 500ml tetra-hole flasks, add the above-mentioned 150g primary antioxidant emulsion preparing, 150g auxiliary anti-oxidant emulsion is heated to 60 DEG C under mechanical stirring, under 250 revs/min of rotating speeds, stir 30min reach evenly, be cooled to 40 DEG C of dischargings.
Embodiment tri-: a kind of nitrile rubber high-performance oxidation inhibitor preparation method, comprise that mass percent is 55% primary antioxidant emulsion, 45% auxiliary antioxidant emulsion, concrete steps are as follows.
(1), prepare primary antioxidant emulsion, be 49.5g by quality 2,2'-methylene-bis-(4-methyl-6-tert-butylphenol), p-cresol and dicyclopentadiene butylation product, in the sodium lauryl sulphate of 16.5g and polyoxyethylenated alcohol sodium sulfate at least one, and 99g deionized water carries out mix and blend, thereby make primary antioxidant emulsion.
(2), prepare auxiliary anti-oxidant emulsion, three [2.4-di-tert-butyl-phenyl] phosphorous acid ester that is 40.5g by quality, in the sodium lauryl sulphate of 13.5g and polyoxyethylenated alcohol sodium sulfate at least one, and 81g deionized water carries out mix and blend, thereby makes auxiliary antioxidant emulsion.
(3), in 500ml tetra-hole flasks, add the above-mentioned 165g primary antioxidant emulsion preparing, 135g auxiliary anti-oxidant emulsion is heated to 80 DEG C under mechanical stirring, under 340 revs/min of rotating speeds, stir 45min reach evenly, be cooled to 40 DEG C of dischargings.
Embodiment tetra-: a kind of nitrile rubber high-performance oxidation inhibitor preparation method, comprise that mass percent is 58% primary antioxidant emulsion, 42% auxiliary antioxidant emulsion, concrete steps are as follows.
(1), prepare primary antioxidant emulsion, be 69.6g by quality 2,2'-methylene-bis-(4-methyl-6-tert-butylphenol), p-cresol and dicyclopentadiene butylation product, in the sodium lauryl sulphate of 20.88g and polyoxyethylenated alcohol sodium sulfate at least one, and 83.52g deionized water carries out mix and blend, thereby make primary antioxidant emulsion.
(2), prepare auxiliary anti-oxidant emulsion, three [2.4-di-tert-butyl-phenyl] phosphorous acid ester that is 50.4g by quality, in the sodium lauryl sulphate of 15.12g and polyoxyethylenated alcohol sodium sulfate at least one, and 60.48g deionized water carries out mix and blend, thereby make auxiliary antioxidant emulsion.
(3), in 500ml tetra-hole flasks, add 174g primary antioxidant emulsion, 126g auxiliary anti-oxidant emulsion is heated to 120 DEG C under mechanical stirring, under 400 revs/min of rotating speeds, stir 1h reach evenly, be cooled to 40 DEG C of dischargings.
Performance Detection: the oxidation inhibitor of preparing with embodiment of the present invention 1-4 add in butyronitrile emulsion and blank sample to being compared to test specimens product, oxidation inhibitor volume is butyronitrile emulsion mass ratio 1%, get a certain amount of product and be placed in beaker, in 115 DEG C of electric drying chambers, dry 2 hours; The nitrile rubber that adds embodiment 1-4 oxidation inhibitor does not almost have xanthochromia, and blank nitrile rubber xanthochromia is serious.
Finally explanation is, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, other amendments that those of ordinary skill in the art make technical scheme of the present invention or be equal to replacement, only otherwise depart from the spirit and scope of technical solution of the present invention, all should be encompassed in the middle of claim scope of the present invention.
Claims (1)
1. a nitrile rubber high-performance oxidation inhibitor preparation method, comprises that mass percent is 50～60% primary antioxidant emulsion, and 40～50% auxiliary antioxidant emulsion, is characterized in that, concrete steps are as follows:
(1), prepare described primary antioxidant emulsion, be 20～50% by mass percent 2,2'-methylene-bis-(4-methyl-6-tert-butylphenol), p-cresol and dicyclopentadiene butylation product, in 6～12% sodium lauryl sulphate and polyoxyethylenated alcohol sodium sulfate at least one, and deionized water carries out mix and blend, thereby make primary antioxidant emulsion;
(2), prepare described auxiliary antioxidant emulsion, three [2.4-di-tert-butyl-phenyl] phosphorous acid ester that is 20～50% by quality percentage, in 6～12% sodium lauryl sulphate and polyoxyethylenated alcohol sodium sulfate at least one, and deionized water carries out mix and blend, thereby make auxiliary antioxidant emulsion;
(3), the above-mentioned described primary antioxidant emulsion of making, auxiliary anti-oxidant emulsion are heated and mixed under mechanical stirring, be heated to 40～120 DEG C of temperature, under 220～400 revs/min of mechanical stirring, stir 20min～1h and reach even.
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| CN201410127261.XA CN103865129A (en) | 2014-04-01 | 2014-04-01 | Preparation method of high-performance antioxidant of butyronitrile rubber latex |
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| CN201410127261.XA CN103865129A (en) | 2014-04-01 | 2014-04-01 | Preparation method of high-performance antioxidant of butyronitrile rubber latex |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016150141A1 (en) * | 2015-03-25 | 2016-09-29 | 江苏飞亚化学工业有限责任公司 | Butadiene rubber compound |
| CN111423617A (en) * | 2019-01-10 | 2020-07-17 | 中国石油天然气股份有限公司 | Preparation method of antioxidant for nitrile rubber |
| CN112778589A (en) * | 2020-12-29 | 2021-05-11 | 金发科技股份有限公司 | Anti-aging butyronitrile material and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4604417A (en) * | 1984-12-10 | 1986-08-05 | The Goodyear Tire & Rubber Company | Polymerizable thioester synergists |
| CN102181072A (en) * | 2011-02-24 | 2011-09-14 | 常州大学 | Preparation method of emulsion antioxidant |
-
2014
- 2014-04-01 CN CN201410127261.XA patent/CN103865129A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4604417A (en) * | 1984-12-10 | 1986-08-05 | The Goodyear Tire & Rubber Company | Polymerizable thioester synergists |
| CN102181072A (en) * | 2011-02-24 | 2011-09-14 | 常州大学 | Preparation method of emulsion antioxidant |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016150141A1 (en) * | 2015-03-25 | 2016-09-29 | 江苏飞亚化学工业有限责任公司 | Butadiene rubber compound |
| CN111423617A (en) * | 2019-01-10 | 2020-07-17 | 中国石油天然气股份有限公司 | Preparation method of antioxidant for nitrile rubber |
| CN111423617B (en) * | 2019-01-10 | 2022-02-01 | 中国石油天然气股份有限公司 | Preparation method of antioxidant for nitrile rubber |
| CN112778589A (en) * | 2020-12-29 | 2021-05-11 | 金发科技股份有限公司 | Anti-aging butyronitrile material and application thereof |
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Application publication date: 20140618 |