CN116554533B - Brominated butyl rubber/polyethylene heat-insulating buffer material and preparation process thereof - Google Patents
Brominated butyl rubber/polyethylene heat-insulating buffer material and preparation process thereof Download PDFInfo
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- CN116554533B CN116554533B CN202310738828.6A CN202310738828A CN116554533B CN 116554533 B CN116554533 B CN 116554533B CN 202310738828 A CN202310738828 A CN 202310738828A CN 116554533 B CN116554533 B CN 116554533B
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- 239000004698 Polyethylene Substances 0.000 title claims abstract description 67
- 229920000573 polyethylene Polymers 0.000 title claims abstract description 67
- 239000000463 material Substances 0.000 title claims abstract description 61
- 229920005557 bromobutyl Polymers 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 238000012360 testing method Methods 0.000 claims abstract description 77
- 238000005187 foaming Methods 0.000 claims abstract description 54
- 229920001971 elastomer Polymers 0.000 claims abstract description 47
- -1 polyethylene Polymers 0.000 claims abstract description 35
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 28
- 150000001875 compounds Chemical class 0.000 claims abstract description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 22
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000011787 zinc oxide Substances 0.000 claims abstract description 14
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 13
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 13
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008117 stearic acid Substances 0.000 claims abstract description 13
- 239000004964 aerogel Substances 0.000 claims abstract description 9
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 8
- 239000004014 plasticizer Substances 0.000 claims abstract description 7
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 6
- 230000002745 absorbent Effects 0.000 claims abstract description 5
- 239000002250 absorbent Substances 0.000 claims abstract description 5
- 238000003825 pressing Methods 0.000 claims description 31
- 238000009413 insulation Methods 0.000 claims description 21
- 238000004073 vulcanization Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000005520 cutting process Methods 0.000 claims description 10
- 238000007731 hot pressing Methods 0.000 claims description 4
- 239000004808 2-ethylhexylester Substances 0.000 claims description 2
- QZCLKYGREBVARF-UHFFFAOYSA-N Acetyl tributyl citrate Chemical compound CCCCOC(=O)CC(C(=O)OCCCC)(OC(C)=O)CC(=O)OCCCC QZCLKYGREBVARF-UHFFFAOYSA-N 0.000 claims description 2
- KRADHMIOFJQKEZ-UHFFFAOYSA-N Tri-2-ethylhexyl trimellitate Chemical compound CCCCC(CC)COC(=O)C1=CC=C(C(=O)OCC(CC)CCCC)C(C(=O)OCC(CC)CCCC)=C1 KRADHMIOFJQKEZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000000465 moulding Methods 0.000 claims description 2
- 239000001038 titanium pigment Substances 0.000 claims description 2
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 5
- BJAJDJDODCWPNS-UHFFFAOYSA-N dotp Chemical compound O=C1N2CCOC2=NC2=C1SC=C2 BJAJDJDODCWPNS-UHFFFAOYSA-N 0.000 claims 1
- 230000006835 compression Effects 0.000 abstract description 6
- 238000007906 compression Methods 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract 1
- 239000006261 foam material Substances 0.000 description 14
- OEIWPNWSDYFMIL-UHFFFAOYSA-N dioctyl benzene-1,4-dicarboxylate Chemical compound CCCCCCCCOC(=O)C1=CC=C(C(=O)OCCCCCCCC)C=C1 OEIWPNWSDYFMIL-UHFFFAOYSA-N 0.000 description 10
- 238000010586 diagram Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 239000006260 foam Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 239000004088 foaming agent Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229920005610 lignin Polymers 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 230000000087 stabilizing effect Effects 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- BSKJUAKMZZKMKC-UHFFFAOYSA-N 1,2-ditert-butyl-3,4-di(propan-2-yl)benzene Chemical compound CC(C)C1=CC=C(C(C)(C)C)C(C(C)(C)C)=C1C(C)C BSKJUAKMZZKMKC-UHFFFAOYSA-N 0.000 description 1
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 1
- 239000004156 Azodicarbonamide Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 description 1
- 235000019399 azodicarbonamide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 229920005549 butyl rubber Polymers 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000013012 foaming technology Methods 0.000 description 1
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 description 1
- 229920005555 halobutyl Polymers 0.000 description 1
- 238000007542 hardness measurement Methods 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000010128 melt processing Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/122—Hydrogen, oxygen, CO2, nitrogen or noble gases
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/06—CO2, N2 or noble gases
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/08—Supercritical fluid
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention relates to the technical field of heat-insulating buffer materials, in particular to a brominated butyl rubber/polyethylene heat-insulating buffer material and a preparation process thereof. The preparation process comprises the following steps: s1, mixing brominated butyl rubber, polyethylene, zinc oxide, stearic acid, a plasticizer, titanium dioxide, an ultraviolet absorbent, an anti-aging agent and aerogel to obtain primary mixed rubber; uniformly mixing the primary mixed rubber and a vulcanizing agent to obtain secondary mixed rubber; s2, placing the rubber compound into an open mill to obtain a pressed test piece; s3, presulfiding the pressed test piece to obtain a presulfided test piece; s4, performing supercritical nitrogen foaming on the pre-vulcanized test piece to obtain a foamed sample; and S5, vulcanizing the foaming sample to obtain the brominated butyl rubber/polyethylene heat-insulating buffer material. The brominated butyl rubber/polyethylene heat-insulating buffer material obtained by the invention has good rebound resilience, small compression set, good heat-insulating performance, green and pollution-free, and meets the new requirements of the environmental protection field.
Description
Technical Field
The invention relates to the technical field of heat-insulating buffer materials, in particular to a brominated butyl rubber/polyethylene heat-insulating buffer material and a preparation process thereof.
Background
Polyethylene (PE) has excellent physical and chemical characteristics, has the advantages of high productivity, low price, easy acquisition and the like, and the foaming material has the advantages of low density, light weight, special porous structure, good buffering performance, flexibility, toughness and heat insulation performance, is one of the foaming materials used in the earliest industrialization, and is widely applied to various fields such as packaging, chemical industry, building and the like. However, the mere polyethylene foam materials have the defects of poor flame retardant effect, poor aging resistance and compression performance and unsatisfactory bonding and printing effects on the surfaces of products, and the performance of the foam materials is often required to be improved by a certain method. The brominated butyl rubber (BIIR) is one of halogenated butyl rubber, has the advantages of high vulcanization rate, good compatibility with other rubber types and more excellent heat resistance of vulcanized products on the basis of preserving the good corrosion resistance of common butyl rubber, and meanwhile, the rubber foaming material generally has good flexibility and elongation at break, and can play a role in efficient heat preservation, heat insulation and energy conservation. Two or more polymer materials are usually blended to form a new polymer material after melt processing, so that the performance of the material is improved, and the application of the product is enlarged.
Patent CN108752770a provides a modified polyethylene foam thermal insulation material, through utilizing the reinforcement function and flame retardant function of modified shell powder, there is high porosity in the inside simultaneously, optimizes polyethylene foam thermal insulation material raw material ratio, has both strengthened the intensity of polyethylene foam, has improved its thermal-insulated fire-retardant efficiency again, has improved the comprehensive properties of heat preservation.
The patent CN105860201A provides a modified composite foam material and a preparation method thereof, wherein the composite foam material comprises the following raw material components in parts by weight of 100 parts of low-density polyethylene, 5-10 parts of enzymolysis lignin, 4 parts of glycidyl methacrylate, 5 parts of azodicarbonamide, 0.6 part of zinc oxide and 1.2 parts of dicumyl peroxide. The composite foam material is prepared by a preparation method of pretreatment lignin, melting plasticating mixture and mould pressing foaming. The composite foam material realizes higher specific strength, thermal stability and excellent foaming performance through the lignin modified polyethylene foam plastic substrate.
At present, the new requirements of the market on the polyethylene foam materials are met by using a filler and a blending method, and chemical foaming and physical foaming methods of alkane gas are adopted, wherein a chemical foaming agent has a certain residue in the foaming materials, the foaming process is difficult to control, so that products are tasty and have color deviation, and the physical foaming agent of alkane gas has the danger of inflammability and explosiveness, so that the wide application of the physical foaming agent in the field of high-precision markets is limited.
Disclosure of Invention
In order to solve the technical problems, the invention improves various properties of the polyethylene foam material by blending the polyethylene and the brominated butyl rubber, and simultaneously adopts a physical foaming method of supercritical nitrogen foaming, thereby being environment-friendly, pollution-free and residue-free in the product and promoting further application of the polyethylene foam material.
The invention provides a preparation process of a brominated butyl rubber/polyethylene heat-insulating buffer material, which comprises the following steps:
step S1, secondary banburying: adding brominated butyl rubber and polyethylene into an internal mixer for banburying, sequentially adding zinc oxide, stearic acid, a plasticizer, titanium pigment, an ultraviolet absorbent, an anti-aging agent and aerogel after torque is stable, uniformly mixing, and taking out to obtain primary mixed rubber; adding the primary mixed rubber and the vulcanizing agent into an internal mixer, and uniformly mixing to obtain secondary mixed rubber;
step S2, open mill pressing test pieces: putting the rubber compound obtained in the step S1 into an open mill, pressing into a sheet through the open mill, and cutting to obtain a pressed test piece;
step S3, pre-vulcanizing a test piece: putting the pressed test piece obtained in the step S2 into a die, and pressing by using a flat vulcanizing machine to obtain a pre-vulcanized test piece;
step S4, supercritical foaming: putting the pre-vulcanized test piece obtained in the step S3 into a supercritical reaction kettle for supercritical nitrogen foaming to obtain a foaming sample;
step S5, vulcanization: and (3) putting the foaming sample obtained in the step (S4) into an oven, and performing secondary high-temperature vulcanization to obtain the brominated butyl rubber/polyethylene heat-insulating buffer material.
Preferably, in the step S1, 20-80 parts by mass of brominated butyl rubber, 20-80 parts by mass of polyethylene, 3-8 parts by mass of zinc oxide, 1-5 parts by mass of stearic acid, 0.5-2 parts by mass of vulcanizing agent, 5-40 parts by mass of plasticizer, 0-20 parts by mass of titanium dioxide, 0-2 parts by mass of ultraviolet absorber, 0.5-2 parts by mass of antioxidant and 0-10 parts by mass of aerogel.
Preferably, the plasticizer in step S1 comprises one or more of DOTP, TOTM, ATBC, DPHP; the ultraviolet absorbent comprises one or more of GW-540, UV-O, UV-531, 744; the anti-aging agent comprises one or more of 4010NA, 4020 and D; the vulcanizing agent comprises one or more of bis 2,4, BIPB and BPO.
Preferably, in the step S1, the temperature of the primary banburying is 110-140 ℃, and the temperature of the secondary banburying is 70-110 ℃.
Preferably, the molding pressure in the step S3 is 10MPa, the hot pressing temperature is 130-160 ℃, and the hot pressing time is 4-20min.
Preferably, the supercritical reaction kettle in the step S4 has the temperature of 80-130 ℃, the saturation pressure of 16-35MPa and the saturation time of 2-6h.
Preferably, the oven temperature in step S5 is 140-180deg.C, and the vulcanization time is 6-20min.
The invention provides a brominated butyl rubber/polyethylene heat-insulating buffer material, which is prepared according to the preparation process of the brominated butyl rubber/polyethylene heat-insulating buffer material.
Compared with the prior art, the invention has the following beneficial technical effects:
the addition of the brominated butyl rubber improves the rebound resilience of the polyethylene heat-insulating buffer material, reduces compression set, and can also reduce the gas permeability of the foaming material, thereby reducing the conduction of gas in the material, reducing the heat conductivity coefficient and improving the heat-insulating property of the material; meanwhile, the supercritical fluid foaming technology uses environment-friendly inert nitrogen as a foaming agent, is environment-friendly and pollution-free, and meets the new requirements of the environment-friendly field. The density of the brominated butyl rubber/polyethylene foam material in the invention can reach 0.05-0.09g/cm 3 The heat conductivity coefficient is 0.035-0.052W/mK. The density of the foam material can be reduced by adding aerogel, and the heat conductivity coefficient of the material can be reduced; the titanium dioxide can play roles in preventing aging and filling materials, improving the light resistance and weather resistance of the materials, and can play a role in nucleation points in the foaming process.
Drawings
FIG. 1 is a cell structure diagram of the insulation buffer material of comparative example 1;
FIG. 2 is a cell structure diagram of the insulation buffer material of comparative example 2;
FIG. 3 is a diagram showing the structure of cells of the brominated butyl rubber/polyethylene thermal insulation buffer material of example 1;
FIG. 4 is a diagram showing the structure of cells of the brominated butyl rubber/polyethylene thermal insulation buffer material of example 2;
FIG. 5 is a diagram of the cell structure of the brominated butyl rubber/polyethylene thermal insulation buffer material of example 3;
FIG. 6 is a diagram of the cell structure of the brominated butyl rubber/polyethylene thermal insulation buffer material of example 4;
FIG. 7 is a diagram of the cell structure of the brominated butyl rubber/polyethylene thermal insulation buffer material of example 5;
FIG. 8 is a cell structure diagram of the brominated butyl rubber/polyethylene thermal insulation buffer material of example 6.
Detailed Description
In order that the above-recited objects, features and advantages of the invention will be more clearly understood, a more particular description of the invention will be rendered by reference to specific embodiments thereof. It should be noted that, in the case of no conflict, the embodiments of the present application and the features in the embodiments may be combined with each other.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced in other ways than those described herein, and therefore the scope of the present invention is not limited to the specific embodiments disclosed below.
Example 1
The preparation method of the brominated butyl rubber/polyethylene heat-insulating buffer material comprises the following steps:
step S1, secondary banburying: setting the temperature of an internal mixer to 130 ℃, after stabilizing the temperature, sequentially adding 20 parts by mass of brominated butyl rubber, 80 parts by mass of polyethylene, 5 parts by mass of zinc oxide, 1.5 parts by mass of stearic acid and 10 parts by mass of dioctyl terephthalate (DOTP), uniformly mixing, and taking out to obtain primary rubber compound; the temperature of an internal mixer is reduced to 90 ℃, and primary rubber compound, 1 part by mass of bis (tert-butyl) diisopropylbenzene peroxide (BIPB) and 1 part by mass of bis (2, 4) -dichlorobenzoyl peroxide (bis (2, 4)) are added, and are uniformly mixed to obtain secondary rubber compound;
step S2, open mill pressing test pieces: putting the rubber compound obtained in the step S1 into an open mill, pressing into a sheet through the open mill, and cutting to obtain a pressed test piece;
step S3, pre-vulcanizing a test piece: putting the pressed test piece obtained in the step S2 into a die, and pressing for 8min by a flat vulcanizing machine under the conditions of 160 ℃ and 10MPa of pressure to obtain a pre-vulcanized test piece;
step S4, supercritical foaming: placing the pre-vulcanized test piece obtained in the step S3 into a supercritical reaction kettle, and performing supercritical nitrogen foaming for 4 hours under the conditions of the temperature of 120 ℃ and the pressure of 20MPa to obtain a foaming test piece;
step S5, vulcanization: and (3) putting the foaming sample obtained in the step (S4) into an oven, and vulcanizing at 160 ℃ for 10min at a high temperature to obtain the brominated butyl rubber/polyethylene heat-insulating buffer material.
Example 2
The preparation method of the brominated butyl rubber/polyethylene heat-insulating buffer material comprises the following steps:
step S1, secondary banburying: setting the temperature of an internal mixer to 130 ℃, after the temperature is stable, sequentially adding 30 parts by mass of brominated butyl rubber, 70 parts by mass of polyethylene, 5 parts by mass of zinc oxide, 1.5 parts by mass of stearic acid and 10 parts by mass of dioctyl terephthalate, uniformly mixing, and taking out to obtain primary mixed rubber; the temperature of an internal mixer is reduced to 90 ℃, and primary rubber compound, 1 part by mass of di-tert-butyl diisopropyl peroxide and 1 part by mass of bis-2, 4-dichlorobenzoyl peroxide are added, and the secondary rubber compound is obtained after uniform mixing;
step S2, open mill pressing test pieces: putting the rubber compound obtained in the step S1 into an open mill, pressing into a sheet through the open mill, and cutting to obtain a pressed test piece;
step S3, pre-vulcanizing a test piece: putting the pressed test piece obtained in the step S2 into a die, and pressing for 8min by a flat vulcanizing machine under the conditions of 160 ℃ and 10MPa of pressure to obtain a pre-vulcanized test piece;
step S4, supercritical foaming: placing the pre-vulcanized test piece obtained in the step S3 into a supercritical reaction kettle, and performing supercritical nitrogen foaming for 4 hours under the conditions of the temperature of 120 ℃ and the pressure of 20MPa to obtain a foaming test piece;
step S5, vulcanization: and (3) putting the foaming sample obtained in the step (S4) into an oven, and vulcanizing at 160 ℃ for 10min at a high temperature to obtain the brominated butyl rubber/polyethylene heat-insulating buffer material.
Example 3
The preparation method of the brominated butyl rubber/polyethylene heat-insulating buffer material comprises the following steps:
step S1, secondary banburying: setting the temperature of an internal mixer to 130 ℃, after stabilizing the temperature, sequentially adding 30 parts by mass of brominated butyl rubber, 70 parts by mass of polyethylene, 6 parts by mass of zinc oxide, 2 parts by mass of stearic acid, 10 parts by mass of dioctyl terephthalate, 1 part by mass of GW-540,5 parts by mass of aerogel and 0.5 part by mass of 4010NA, uniformly mixing, and taking out to obtain primary mixed rubber; the temperature of an internal mixer is reduced to 90 ℃, primary rubber compound and 1.2 parts by mass of di-tert-butyl diisopropyl peroxide are added, and secondary rubber compound is obtained after uniform mixing;
step S2, open mill pressing test pieces: putting the rubber compound obtained in the step S1 into an open mill, pressing into a sheet through the open mill, and cutting to obtain a pressed test piece;
step S3, pre-vulcanizing a test piece: placing the pressed test piece obtained in the step S2 into a die, and pressing for 10min by a flat vulcanizing instrument under the conditions of the temperature of 150 ℃ and the pressure of 10MPa to obtain a pre-vulcanized test piece;
step S4, supercritical foaming: placing the pre-vulcanized test piece obtained in the step S3 into a supercritical reaction kettle, and performing supercritical nitrogen foaming for 4 hours under the conditions of the temperature of 120 ℃ and the pressure of 35MPa to obtain a foaming test piece;
step S5, vulcanization: and (3) putting the foaming sample obtained in the step (S4) into an oven, and vulcanizing at 160 ℃ for 15min at a high temperature to obtain the brominated butyl rubber/polyethylene heat-insulating buffer material.
Example 4
The preparation method of the brominated butyl rubber/polyethylene heat-insulating buffer material comprises the following steps:
step S1, secondary banburying: setting the temperature of an internal mixer to 130 ℃, after the temperature is stable, sequentially adding 40 parts by mass of brominated butyl rubber, 60 parts by mass of polyethylene, 6 parts by mass of zinc oxide, 5 parts by mass of stearic acid, 15 parts by mass of dioctyl terephthalate, 8 parts by mass of titanium dioxide, 0.5 part by mass of GW-540 and 5 parts by mass of aerogel, uniformly mixing, and taking out to obtain primary mixed rubber; the temperature of an internal mixer is reduced to 90 ℃, and primary rubber compound, 1.0 mass part of di-tert-butyl diisopropyl peroxide and 0.5 mass part of bis-2, 4-dichlorobenzoyl peroxide are added, and are uniformly mixed to obtain secondary rubber compound;
step S2, open mill pressing test pieces: putting the rubber compound obtained in the step S1 into an open mill, pressing into a sheet through the open mill, and cutting to obtain a pressed test piece;
step S3, pre-vulcanizing a test piece: putting the pressed test piece obtained in the step S2 into a die, and pressing for 6min by a flat vulcanizing instrument under the conditions of 160 ℃ and 10MPa of pressure to obtain a pre-vulcanized test piece;
step S4, supercritical foaming: placing the pre-vulcanized test piece obtained in the step S3 into a supercritical reaction kettle, and performing supercritical nitrogen foaming for 4 hours under the conditions of the temperature of 120 ℃ and the pressure of 30MPa to obtain a foaming test piece;
step S5, vulcanization: and (3) putting the foaming sample obtained in the step (S4) into an oven, and vulcanizing at 160 ℃ for 15min at a high temperature to obtain the brominated butyl rubber/polyethylene heat-insulating buffer material.
Example 5
The preparation method of the brominated butyl rubber/polyethylene heat-insulating buffer material comprises the following steps:
step S1, secondary banburying: setting the temperature of an internal mixer to 130 ℃, after the temperature is stable, sequentially adding 70 parts by mass of brominated butyl rubber, 30 parts by mass of polyethylene, 8 parts by mass of zinc oxide, 2 parts by mass of stearic acid, 15 parts by mass of dioctyl terephthalate, 5 parts by mass of titanium dioxide, 0.5 part by mass of GW-540 and 0.5 part by mass of 4010NA, uniformly mixing, and taking out to obtain primary mixed rubber; the temperature of an internal mixer is reduced to 90 ℃, primary rubber compound and 1.5 parts by mass of di-tert-butyl diisopropyl peroxide are added, and secondary rubber compound is obtained after uniform mixing;
step S2, open mill pressing test pieces: putting the rubber compound obtained in the step S1 into an open mill, pressing into a sheet through the open mill, and cutting to obtain a pressed test piece;
step S3, pre-vulcanizing a test piece: placing the pressed test piece obtained in the step S2 into a die, and pressing for 5min by a flat vulcanizing machine under the conditions of 140 ℃ and 10MPa to obtain a pre-vulcanized test piece;
step S4, supercritical foaming: placing the pre-vulcanized test piece obtained in the step S3 into a supercritical reaction kettle, and performing supercritical nitrogen foaming for 4 hours under the conditions of the temperature of 120 ℃ and the pressure of 30MPa to obtain a foaming test piece;
step S5, vulcanization: and (3) putting the foaming sample obtained in the step (S4) into an oven, and vulcanizing at 160 ℃ for 15min at a high temperature to obtain the brominated butyl rubber/polyethylene heat-insulating buffer material.
Example 6
The preparation method of the brominated butyl rubber/polyethylene heat-insulating buffer material comprises the following steps:
step S1, secondary banburying: setting the temperature of an internal mixer to 130 ℃, after stabilizing the temperature, sequentially adding 60 parts by mass of brominated butyl rubber, 40 parts by mass of polyethylene, 5 parts by mass of zinc oxide, 2 parts by mass of stearic acid, 20 parts by mass of dioctyl terephthalate, 10 parts by mass of titanium dioxide, 0.5 part by mass of GW-540, 8 parts by mass of aerogel and 0.5 part by mass of 4010NA, uniformly mixing, and taking out to obtain primary mixed rubber; the temperature of an internal mixer is reduced to 90 ℃, primary rubber compound and 1.2 parts by mass of di-tert-butyl diisopropyl peroxide are added, and secondary rubber compound is obtained after uniform mixing;
step S2, open mill pressing test pieces: putting the rubber compound obtained in the step S1 into an open mill, pressing into a sheet through the open mill, and cutting to obtain a pressed test piece;
step S3, pre-vulcanizing a test piece: putting the pressed test piece obtained in the step S2 into a die, and pressing for 5min by a flat vulcanizing machine under the conditions of the temperature of 150 ℃ and the pressure of 10MPa to obtain a pre-vulcanized test piece;
step S4, supercritical foaming: placing the pre-vulcanized test piece obtained in the step S3 into a supercritical reaction kettle, and performing supercritical nitrogen foaming for 4 hours under the conditions of the temperature of 120 ℃ and the pressure of 30MPa to obtain a foaming test piece;
step S5, vulcanization: and (3) putting the foaming sample obtained in the step (S4) into an oven, and vulcanizing at 160 ℃ for 15min at a high temperature to obtain the brominated butyl rubber/polyethylene heat-insulating buffer material.
Comparative example 1
The comparative example prepared a polyethylene thermal insulation buffer material, comprising the following steps:
step S1, secondary banburying: setting the temperature of an internal mixer to 130 ℃, after the temperature is stable, sequentially adding 100 parts by mass of polyethylene, 5 parts by mass of zinc oxide, 1.5 parts by mass of stearic acid and 10 parts by mass of dioctyl terephthalate, uniformly mixing, and taking out to obtain primary mixed rubber; the temperature of an internal mixer is reduced to 110 ℃, and primary rubber compound, 1 part by mass of di-tert-butyl diisopropyl peroxide and 1 part by mass of bis-2, 4-dichlorobenzoyl peroxide are added, and the secondary rubber compound is obtained after uniform mixing;
step S2, open mill pressing test pieces: putting the rubber compound obtained in the step S1 into an open mill, pressing into a sheet through the open mill, and cutting to obtain a pressed test piece;
step S3, vulcanizing a test piece: putting the pressed test piece obtained in the step S2 into a die, and pressing for 8min by a flat vulcanizing machine under the conditions of 160 ℃ and 10MPa of pressure to obtain the test piece;
step S4, supercritical foaming: and (3) placing the vulcanized test piece obtained in the step (S3) into a supercritical reaction kettle, and performing supercritical nitrogen foaming for 4 hours under the conditions of the temperature of 120 ℃ and the pressure of 20MPa to obtain the polyethylene heat-insulation buffer material.
Comparative example 2
The preparation method of the brominated butyl rubber heat-insulating buffer material comprises the following steps:
step S1, secondary banburying: setting the temperature of an internal mixer to 130 ℃, after the temperature is stable, sequentially adding 100 parts by mass of brominated butyl rubber, 5 parts by mass of zinc oxide, 1 part by mass of stearic acid, 2 parts by mass of titanium dioxide and 15 parts by mass of dioctyl terephthalate, uniformly mixing, and taking out to obtain primary mixed rubber; the temperature of an internal mixer is reduced to 90 ℃, primary rubber compound and 0.5 part by mass of di-tert-butyl diisopropyl peroxide are added, and secondary rubber compound is obtained after uniform mixing;
step S2, open mill pressing test pieces: putting the rubber compound obtained in the step S1 into an open mill, pressing into a sheet through the open mill, and cutting to obtain a pressed test piece;
step S3, pre-vulcanizing a test piece: putting the pressed test piece obtained in the step S2 into a die, and pressing for 8min by a flat vulcanizing machine under the conditions of 160 ℃ and 10MPa of pressure to obtain a pre-vulcanized test piece;
step S4, supercritical foaming: placing the pre-vulcanized test piece obtained in the step S3 into a supercritical reaction kettle, and performing supercritical nitrogen foaming for 4 hours under the conditions of the temperature of 120 ℃ and the pressure of 30MPa to obtain a foaming test piece;
step S5, vulcanization: and (3) putting the foaming sample obtained in the step (S4) into an oven, and vulcanizing at 160 ℃ for 10min at a high temperature to obtain the brominated butyl rubber heat-insulation buffer material.
Performance testing
Density testing: the density of the foamed sample was measured by GB/T6343-1995.
Hardness testing: the hardness of the foam sample was measured by the collapse method of GB/T10807-2006.
Rebound resilience performance test: the ball drop method of GB/T6670-2008 is adopted for measurement, and the rebound performance of the foaming sample is tested.
Compression set properties: the test was performed according to GB/T6669-2008. The test piece was compressed by 50%, placed in an environment of 70℃for 22 hours, and the compression set property was measured.
Scanning electron microscope test: cell morphology was determined using a JSM-7500 model scanning electron microscope.
Thermal conductivity testing: the thermal conductivity of the foamed samples was measured according to GB/T32064-2015.
The properties of the thermal insulation buffer materials obtained in examples 1 to 6 and comparative examples 1 to 2 were examined, and the results of the examination are shown in Table 1,
table 1 performance test data
As can be seen by combining the data in Table 1 and the electron microscope photographs in the accompanying drawings 1-8, the brominated butyl rubber is added into the polyethylene foam material as a rubber material, so that the high strength of the polyethylene is weakened, the defects of poor rebound resilience and large compression set of the polyethylene foam material are improved, the cell density is increased, the radiation heat conductivity is reduced, the heat conductivity of the foam material is further reduced, and the heat preservation performance of the material is improved.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the scope of the present invention.
Claims (7)
1. The preparation process of the brominated butyl rubber/polyethylene heat-insulating buffer material is characterized by comprising the following steps of:
step S1, secondary banburying: adding brominated butyl rubber and polyethylene into an internal mixer for banburying, sequentially adding zinc oxide, stearic acid, a plasticizer, titanium pigment, an ultraviolet absorbent, an anti-aging agent and aerogel after torque is stable, uniformly mixing, and taking out to obtain primary mixed rubber; adding the primary mixed rubber and the vulcanizing agent into an internal mixer, and uniformly mixing to obtain secondary mixed rubber; wherein, 20-80 parts by weight of brominated butyl rubber, 20-80 parts by weight of polyethylene, 3-8 parts by weight of zinc oxide, 1-5 parts by weight of stearic acid, 0.5-2 parts by weight of vulcanizing agent, 5-40 parts by weight of plasticizer, 0-20 parts by weight of titanium dioxide, 0-2 parts by weight of ultraviolet absorber, 0.5-2 parts by weight of anti-aging agent and 0-10 parts by weight of aerogel;
step S2, open mill pressing test pieces: putting the rubber compound obtained in the step S1 into an open mill, pressing into a sheet through the open mill, and cutting to obtain a pressed test piece;
step S3, pre-vulcanizing a test piece: putting the pressed test piece obtained in the step S2 into a die, and pressing by using a flat vulcanizing machine to obtain a pre-vulcanized test piece;
step S4, supercritical foaming: putting the pre-vulcanized test piece obtained in the step S3 into a supercritical reaction kettle for supercritical nitrogen foaming to obtain a foaming sample;
step S5, vulcanization: and (3) putting the foaming sample obtained in the step (S4) into an oven, and performing secondary high-temperature vulcanization to obtain the brominated butyl rubber/polyethylene heat-insulating buffer material.
2. The process for preparing a brominated butyl rubber/polyethylene thermal insulation buffer material of claim 1, wherein the plasticizer in step S1 comprises one or more of DOTP, TOTM, ATBC, DPHP; the ultraviolet absorbent comprises one or more of GW-540, UV-O, UV-531, 744; the anti-aging agent comprises one or more of 4010NA, 4020 and D; the vulcanizing agent comprises one or more of bis 2,4, BIPB and BPO.
3. The process for preparing a brominated butyl rubber/polyethylene thermal insulation buffer material according to claim 1, wherein in step S1, the temperature of the primary banburying is 110-140 ℃, and the temperature of the secondary banburying is 70-110 ℃.
4. The process for preparing the brominated butyl rubber/polyethylene thermal insulation buffer material according to claim 1, wherein the molding pressure in the step S3 is 10MPa, the hot pressing temperature is 130-160 ℃, and the hot pressing time is 4-20min.
5. The process for preparing the brominated butyl rubber/polyethylene thermal insulation buffer material according to claim 1, wherein the temperature of the supercritical reaction kettle in the step S4 is 80-130 ℃, the saturation pressure is 16-35MPa, and the saturation time is 2-6h.
6. The process for preparing a brominated butyl rubber/polyethylene thermal insulation buffer material according to claim 1, wherein the oven temperature in step S5 is 140-180 ℃ and the vulcanization time is 6-20min.
7. A brominated butyl rubber/polyethylene thermal insulation buffer material, characterized in that the material is prepared by a preparation process of the brominated butyl rubber/polyethylene thermal insulation buffer material according to any one of claims 1-6.
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