CN109294004B - Anti-ozone rubber and preparation method thereof - Google Patents
Anti-ozone rubber and preparation method thereof Download PDFInfo
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- CN109294004B CN109294004B CN201811148098.XA CN201811148098A CN109294004B CN 109294004 B CN109294004 B CN 109294004B CN 201811148098 A CN201811148098 A CN 201811148098A CN 109294004 B CN109294004 B CN 109294004B
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Abstract
The invention discloses an ozone-resistant rubber and a preparation method thereof, wherein the ozone-resistant rubber comprises the following components in parts by mass: 2 parts by mass of zinc oxide, 1 part by mass of stearic acid, 1.5 parts by mass of accelerator CZ, 0.5 part by mass of accelerator DM, 2 parts by mass of sulfur, 1-10 parts by mass of polyisobutylene and 100 parts by mass of unsaturated rubber. The preparation method of the ozone-resistant rubber comprises the following steps: weighing zinc oxide, stearic acid, an accelerator, sulfur, polyisobutylene and unsaturated rubber according to a formula; preheating and mixing the weighed unsaturated rubber and polyisobutylene, then adding the weighed zinc oxide, stearic acid, accelerator CZ and accelerator DM for mixing, discharging rubber, adding sulfur, tabletting, discharging, cooling and standing to obtain the ozone-resistant rubber. The ozone-resistant rubber prepared by the invention has the advantages of excellent oxidation resistance and ozone resistance, and simultaneously has the basic performances of good heat resistance, chemical resistance, weather resistance, ultraviolet resistance, acid resistance, alkali resistance and the like.
Description
Technical Field
The invention belongs to the field of rubber application, and particularly relates to an ozone-resistant rubber and a preparation method thereof.
Background
The rubber industry is one of the important basic industries of national economy. It not only provides daily and medical light industrial rubber products which are indispensable to daily life for people, but also provides various rubber production equipment or rubber parts for heavy industries such as mining, traffic, building, machinery, electronics and the like and emerging industries. It can be seen that the products in the rubber industry are of various types and have wide backward industry.
Rubbers are very diverse and Natural Rubber (NR), Styrene Butadiene Rubber (SBR), butyl rubber (IIR), hydrogenated nitrile rubber (HNBR), ethylene propylene rubber (EPDM), nitrile rubber (NBR), neoprene (CR) are commonly used. The environment of the rubber material at present is increasingly polluted, the most prominent is the influence of ozone, and particularly, the rubber varieties such as Natural Rubber (NR), Styrene Butadiene Rubber (SBR), Butadiene Rubber (BR), Isoprene Rubber (IR) and the like which are not resistant to ozone have unsaturated double bonds in the rubber, the double bonds are broken under the action of ozone, the performance of the rubber product is seriously damaged, and how to prolong the service life of the rubber product is increasingly important.
The research on the antiozonants at home and abroad is many, but the antiozonants serving as an auxiliary agent added into rubber inevitably change other properties of the rubber. Polyisobutylene (PIB) is a viscous or semisolid substance which is colorless, tasteless, five-toxin and nontoxic, has good heat resistance, chemical resistance, weather resistance, ultraviolet resistance, acid resistance and alkali resistance, and more importantly has oxygen resistance and ozone resistance.
Polyisobutylene (PIB) is divided into low molecular polyisobutylene with a relative molecular weight of 350 to 5000, medium molecular polyisobutylene with a relative molecular weight of 1 ten thousand to 10 ten thousand and high molecular polyisobutylene with a relative molecular weight of more than 10 ten thousand, and with the increase of the molecular weight, the content of alpha-double bond at the end of a molecular chain is increased, and the excellent performance and the price are increased with the increase. The rubber mixed with the polyisobutylene can be filled with more fillers during mixing, and can also improve the water resistance, the air permeability, the heat resistance, the ultraviolet resistance, the physical strength and the like.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention mainly aims to provide a preparation method of ozone-resistant rubber.
Another object of the present invention is to provide the above ozone resistant rubber.
The purpose of the invention is realized by the following technical scheme:
the ozone-resistant rubber comprises the following raw materials in parts by mass: 2 parts by mass of zinc oxide, 1 part by mass of stearic acid, 1.5 parts by mass of accelerator CZ, 0.5 part by mass of accelerator DM, 2 parts by mass of sulfur, 1-10 parts by mass of polyisobutylene and 100 parts by mass of unsaturated rubber.
The Polyisobutylene (PIB) is preferably liquid polyisobutylene with the molecular weight of 1 to 5 ten thousand, more preferably the molecular weight of the PIB is 15800, and the liquid polyisobutylene has good fluidity and can play a role of a solvent so as to fully and uniformly mix all components.
The Polyisobutylene (PIB) is preferably 5 to 10 parts by mass.
The Polyisobutylene (PIB) is preferably 5 parts by mass.
The unsaturated rubber is one or more of Natural Rubber (NR), Styrene Butadiene Rubber (SBR), Butadiene Rubber (BR) and Isoprene Rubber (IR).
The preparation method of the ozone-resistant rubber comprises the following steps:
(1) weighing the following components: weighing 2 parts by mass of zinc oxide (ZnO), 1 part by mass of Stearic Acid (SA), 1.5 parts by mass of accelerator CZ, 0.5 part by mass of accelerator DM, 2 parts by mass of sulfur, 1-10 parts by mass of Polyisobutylene (PIB) and 100 parts by mass of unsaturated rubber;
(2) mixing and molding: preheating and mixing the weighed unsaturated rubber and Polyisobutylene (PIB), adding the weighed zinc oxide, stearic acid, accelerator CZ and accelerator DM, mixing, discharging rubber, adding sulfur, tabletting, discharging, cooling, and standing to obtain the ozone-resistant rubber.
The mixing conditions in the step (2) are as follows: and controlling the mixing end point by using the rubber discharge temperature, wherein the rubber discharge temperature is 110-140 ℃, preferably 120 ℃, and the mixing period is 10-20 min, preferably 20 min.
The preheating temperature in the step (2) is 60 +/-5 ℃.
The mixing in the step (2) refers to mixing in an internal mixer.
The mixing in step (2) is preferably a conventional mixing method, i.e., one-stage mixing, but is not limited to the conventional mixing method, and other mixing methods are possible.
The chemical name of the accelerator CZ is N-cyclohexyl-2-benzothiazolyl sulfenamide; accelerator DM chemical name 2,2' -dithiodibenzothiazole.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the ozone-resistant rubber prepared by the invention can improve the basic performance of rubber products: heat resistance, chemical resistance, weather resistance, ultraviolet resistance, acid resistance and alkali resistance, and can effectively improve the oxidation resistance and the ozone resistance of the rubber product.
Drawings
FIG. 1 is a graph showing the effect of different amounts of PIB loading on the dynamic ozone resistance of rubber.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
The test method of the rubber product produced in the example of the invention was:
1. the ozone resistance of the rubber is measured according to GB/T7762--8g/L, the temperature is (40 +/-2) DEG C, the relative humidity is 60 +/-5%, and the longest time without crack is measured under 10% strain by adopting a method B in the standard;
2. the mechanical properties of the rubber material are measured according to GB/T528-1999;
3. the thermal aging resistance of the rubber material is performed according to the standard GB/T3512-2001, wherein the temperature is (100 +/-DEG C) and the time is 24 h.
The Natural Rubber (NR) used in the examples was vietnam 3L rubber; polyisobutylene (PIB) was produced by gold, plastic Limited, Dongguan.
Example 1
(1) Weighing the following components: weighing 2 parts by mass of zinc oxide (ZnO), 1 part by mass of Stearic Acid (SA), 1.5 parts by mass of accelerator CZ, 0.5 part by mass of accelerator DM, 2 parts by mass of sulfur, 1 part by mass of liquid Polyisobutylene (PIB) with molecular weight of 15800 and 100 parts by mass of natural rubber;
(2) mixing and molding: preheating and mixing the weighed Natural Rubber (NR) and Polyisobutylene (PIB) at 60 ℃, adding the weighed zinc oxide, stearic acid, accelerator CZ and accelerator DM, mixing in an internal mixer for 20min, discharging rubber at 120 ℃, adding sulfur, tabletting, discharging, cooling and standing to obtain the ozone-resistant rubber.
Example 2
(1) Weighing the following components: weighing 2 parts by mass of zinc oxide (ZnO), 1 part by mass of Stearic Acid (SA), 1.5 parts by mass of accelerator CZ, 0.5 part by mass of accelerator DM, 2 parts by mass of sulfur, 5 parts by mass of liquid Polyisobutylene (PIB) with molecular weight of 15800 and 100 parts by mass of natural rubber;
(2) mixing and molding: preheating and mixing the weighed Natural Rubber (NR) and Polyisobutylene (PIB) at 60 ℃, adding the weighed zinc oxide, stearic acid, accelerator CZ and accelerator DM, mixing in an internal mixer for 20min, discharging rubber at 120 ℃, adding sulfur, tabletting, discharging, cooling and standing to obtain the ozone-resistant rubber.
Example 3
(1) Weighing the following components: weighing 2 parts by mass of zinc oxide (ZnO), 1 part by mass of Stearic Acid (SA), 1.5 parts by mass of accelerator CZ, 0.5 part by mass of accelerator DM, 2 parts by mass of sulfur, 10 parts by mass of liquid Polyisobutylene (PIB) with molecular weight of 15800 and 100 parts by mass of natural rubber;
(2) mixing and molding: preheating and mixing the weighed Natural Rubber (NR) and Polyisobutylene (PIB) at 60 ℃, adding the weighed zinc oxide, stearic acid, accelerator CZ and accelerator DM, mixing in an internal mixer for 20min, discharging rubber at 120 ℃, adding sulfur, tabletting, discharging, cooling and standing to obtain the ozone-resistant rubber.
Example 4
(1) Weighing the following components: weighing 2 parts by mass of zinc oxide (ZnO), 1 part by mass of Stearic Acid (SA), 1.5 parts by mass of accelerator CZ, 0.5 part by mass of accelerator DM, 2 parts by mass of sulfur, 5 parts by mass of liquid Polyisobutylene (PIB) with molecular weight of 10080 and 100 parts by mass of natural rubber;
(2) mixing and molding: preheating and mixing the weighed Natural Rubber (NR) and Polyisobutylene (PIB) at 60 ℃, adding the weighed zinc oxide, stearic acid, accelerator CZ and accelerator DM, mixing in an internal mixer for 20min, discharging rubber at 120 ℃, adding sulfur, tabletting, discharging, cooling and standing to obtain the ozone-resistant rubber.
Example 5
(1) Weighing the following components: weighing 2 parts by mass of zinc oxide (ZnO), 1 part by mass of Stearic Acid (SA), 1.5 parts by mass of accelerator CZ, 0.5 part by mass of accelerator DM, 2 parts by mass of sulfur, 5 parts by mass of liquid Polyisobutylene (PIB) with molecular weight of 49870 and 100 parts by mass of natural rubber;
(2) mixing and molding: preheating and mixing the weighed Natural Rubber (NR) and Polyisobutylene (PIB) at 60 ℃, adding the weighed zinc oxide, stearic acid, accelerator CZ and accelerator DM, mixing in an internal mixer for 20min, discharging rubber at 120 ℃, adding sulfur, tabletting, discharging, cooling and standing to obtain the ozone-resistant rubber.
Comparative example 1
(1) Weighing the following components: weighing 2 parts by mass of zinc oxide (ZnO), 1 part by mass of Stearic Acid (SA), 1.5 parts by mass of accelerator CZ, 0.5 part by mass of accelerator DM, 2 parts by mass of sulfur, 5 parts by mass of liquid Polyisobutylene (PIB) with molecular weight of 3580 and 100 parts by mass of natural rubber;
(2) mixing and molding: preheating and mixing the weighed Natural Rubber (NR) and Polyisobutylene (PIB) at 60 ℃, adding the weighed zinc oxide, stearic acid, accelerator CZ and accelerator DM, mixing in an internal mixer for 20min, discharging rubber at 120 ℃, adding sulfur, tabletting, discharging, cooling and standing to obtain the ozone-resistant rubber 2-1.
Comparative example 2
(1) Weighing the following components: weighing 2 parts by mass of zinc oxide (ZnO), 1 part by mass of Stearic Acid (SA), 1.5 parts by mass of accelerator CZ, 0.5 part by mass of accelerator DM, 2 parts by mass of sulfur, 5 parts by mass of solid Polyisobutylene (PIB) with the molecular weight of 76500 and 100 parts by mass of natural rubber;
(2) mixing and molding: preheating and mixing the weighed Natural Rubber (NR) and Polyisobutylene (PIB) at 60 ℃, adding the weighed zinc oxide, stearic acid, accelerator CZ and accelerator DM, mixing in an internal mixer for 20min, discharging rubber at 120 ℃, adding sulfur, tabletting, discharging, cooling and standing to obtain the ozone-resistant rubber 2-2.
Comparative example 3
(1) Weighing the following components: weighing 2 parts by mass of zinc oxide (ZnO), 1 part by mass of Stearic Acid (SA), 1.5 parts by mass of accelerator CZ, 0.5 part by mass of accelerator DM, 2 parts by mass of sulfur, 20 parts by mass of liquid Polyisobutylene (PIB) with molecular weight of 15800 and 100 parts by mass of natural rubber;
(2) mixing and molding: preheating and mixing the weighed Natural Rubber (NR) and Polyisobutylene (PIB) at 60 ℃, adding the weighed zinc oxide, stearic acid, accelerator CZ and accelerator DM, mixing in an internal mixer for 20min, discharging rubber at 120 ℃, adding sulfur, tabletting, discharging, cooling and standing to obtain the ozone-resistant rubber 2-3.
FIG. 1 is a graph showing the effect of different amounts of PIB added on the dynamic ozone resistance of rubber, wherein 0 represents a comparative sample in which liquid Polyisobutylene (PIB) is not added, and the amounts of PIB added are 1 part by mass, 5 parts by mass and 10 parts by mass, respectively, corresponding to rubber samples prepared in examples 1, 2 and 3. The results show that the addition of liquid Polyisobutylene (PIB) obviously improves the ozone resistance of the rubber, but the improvement of the ozone resistance of the rubber is not linearly increased but is slowed down after 5 parts by mass (100 parts by mass of natural rubber) along with the increase of the adding amount.
TABLE 1 influence of different molecular weights and different amounts of PIB on the aging resistance of rubber
Table 1 shows the effect of different molecular weights and different amounts of PIB on the aging behavior of the rubber, 0 representing a comparative sample without liquid polyisobutene PIB. After the liquid PIB with the molecular weight of 15800 is doped, the tensile strength of the rubber before aging is basically not changed greatly and is slightly improved; the rubber aging performance is greatly improved, the aged tensile strength of the liquid polyisobutylene added with 1 part by mass (compared with 100 parts by mass of natural rubber) is improved by 10.14 percent, the aged tensile strength is improved by 36.58 percent after 5 parts by mass is added, the PIB mass (10 parts by mass and 20 parts by mass) is continuously increased, the improvement effect of the tensile strength is not linearly increased but is slowed down, and the cost is increased.
Similarly, the blending amount is 5 parts by mass, and the mechanical properties of the rubber before and after aging are reduced by blending the high molecular weight (76500) PIB, because the high molecular weight PIB is mostly in an inert solid state and is not easy to mix and masticate; after the small molecular weight PIB (3580) is doped, the mechanical properties before and after the rubber is aged are respectively better than those before and after the rubber with the middle molecular weight (15800) is aged, but on one hand, the rubber cost is obviously increased due to the fact that the small molecular weight PIB is doped, on the other hand, the small molecular weight PIB has additional reaction due to too many double bonds during mixing, and in addition, residual double bonds are left in the prepared rubber material, so that the ozone resistance of the rubber material is seriously reduced (the longest time for a sample to have no cracks is 52h, and the ozone resistance is obviously reduced compared with that of the middle molecular weight which is more than 100 h).
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (9)
1. The ozone-resistant rubber is characterized by comprising the following raw materials in parts by mass: 2 parts by mass of zinc oxide, 1 part by mass of stearic acid, 1.5 parts by mass of accelerator CZ, 0.5 part by mass of accelerator DM, 2 parts by mass of sulfur, 1-10 parts by mass of polyisobutylene and 100 parts by mass of unsaturated rubber;
the polyisobutylene is liquid polyisobutylene with molecular weight of 1 to 5 ten thousand;
the unsaturated rubber is one or more of natural rubber, styrene butadiene rubber, butadiene rubber and isoprene rubber.
2. The ozone-resistant rubber according to claim 1, wherein the molecular weight of the polyisobutylene is 15800.
3. The ozone-resistant rubber according to claim 1 or 2, wherein the polyisobutylene is 5 to 10 parts by mass.
4. The ozone-resistant rubber according to claim 3, wherein the polyisobutylene is 5 parts by mass.
5. The method for preparing the ozone-resistant rubber according to any one of claims 1 to 4, comprising the steps of:
(1) weighing the following components: weighing 2 parts by mass of zinc oxide, 1 part by mass of stearic acid, 1.5 parts by mass of accelerator CZ, 0.5 part by mass of accelerator DM, 2 parts by mass of sulfur, 1-10 parts by mass of polyisobutylene and 100 parts by mass of unsaturated rubber;
(2) mixing and molding: preheating and mixing the weighed unsaturated rubber and polyisobutylene, then adding the weighed zinc oxide, stearic acid, accelerator CZ and accelerator DM for mixing, discharging rubber, adding sulfur, tabletting, discharging, cooling and standing to obtain the ozone-resistant rubber.
6. The method for preparing an ozone-resistant rubber according to claim 5, wherein the mixing conditions in the step (2) are as follows: the rubber discharging temperature is 110-140 ℃, and the mixing period is 10-20 min.
7. The method for preparing the ozone-resistant rubber according to claim 6, wherein the mixing conditions in the step (2) are as follows: the rubber discharging temperature is 120 ℃, and the mixing period is 20 min.
8. The method for preparing ozone resistant rubber according to claim 5 or 6, wherein the temperature of the preheating in the step (2) is 60 ± 5 ℃.
9. The method for preparing the ozone-resistant rubber according to claim 5 or 6, wherein the mixing in the step (2) is internal mixer mixing.
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| WO2009158604A2 (en) * | 2008-06-26 | 2009-12-30 | Bridgestone Corporation | Rubber compositions including metal-functionalized polyisobutylene derivatives and methods for preparing such compositions |
| CN103756037B (en) * | 2013-12-30 | 2016-03-09 | 宁国市正道橡塑零部件有限公司 | A kind of workability, ozone proof elastomeric material and preparation method thereof |
| CN104987547B (en) * | 2015-07-17 | 2017-07-21 | 安徽中鼎密封件股份有限公司 | A kind of bushing of resistance to ozone stable and preparation method thereof |
| CN105585748A (en) * | 2016-03-16 | 2016-05-18 | 长春实发汽车零部件有限公司 | Ozone aging resistance rubber and preparation method thereof |
| CN106084327A (en) * | 2016-07-04 | 2016-11-09 | 华南协同创新研究院 | Adhesion tire rubber prepared by a kind of epoxy natural rubber and preparation method thereof |
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