CN116444933A - Thermoplastic elastomer with low compression set characteristic and preparation method thereof - Google Patents
Thermoplastic elastomer with low compression set characteristic and preparation method thereof Download PDFInfo
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- 229920002725 thermoplastic elastomer Polymers 0.000 title claims abstract description 45
- 238000007906 compression Methods 0.000 title claims abstract description 31
- 230000006835 compression Effects 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims description 27
- 229920006132 styrene block copolymer Polymers 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 19
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 19
- 239000003921 oil Substances 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 239000000945 filler Substances 0.000 claims abstract description 13
- 239000004793 Polystyrene Substances 0.000 claims abstract description 9
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 9
- 229920002223 polystyrene Polymers 0.000 claims abstract description 9
- 229920002545 silicone oil Polymers 0.000 claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 62
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical class [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 52
- 229920001661 Chitosan Polymers 0.000 claims description 51
- 238000003756 stirring Methods 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 31
- 239000000243 solution Substances 0.000 claims description 30
- 239000000440 bentonite Substances 0.000 claims description 27
- 229910000278 bentonite Inorganic materials 0.000 claims description 27
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 27
- 239000005543 nano-size silicon particle Substances 0.000 claims description 27
- 239000003607 modifier Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000007864 aqueous solution Substances 0.000 claims description 22
- 235000012239 silicon dioxide Nutrition 0.000 claims description 21
- 239000002253 acid Substances 0.000 claims description 18
- 238000000498 ball milling Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 18
- 238000005406 washing Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 17
- 150000001875 compounds Chemical class 0.000 claims description 16
- 235000019198 oils Nutrition 0.000 claims description 15
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000001125 extrusion Methods 0.000 claims description 12
- 235000010413 sodium alginate Nutrition 0.000 claims description 12
- 239000000661 sodium alginate Substances 0.000 claims description 12
- 229940005550 sodium alginate Drugs 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 8
- 239000007822 coupling agent Substances 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 7
- 230000004048 modification Effects 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical group C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 6
- GHKOFFNLGXMVNJ-UHFFFAOYSA-N Didodecyl thiobispropanoate Chemical compound CCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCC GHKOFFNLGXMVNJ-UHFFFAOYSA-N 0.000 claims description 6
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 6
- BXOUVIIITJXIKB-UHFFFAOYSA-N ethene;styrene Chemical group C=C.C=CC1=CC=CC=C1 BXOUVIIITJXIKB-UHFFFAOYSA-N 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 239000000155 melt Substances 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 6
- 239000003549 soybean oil Substances 0.000 claims description 6
- 235000012424 soybean oil Nutrition 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 230000008569 process Effects 0.000 claims description 4
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 229920000742 Cotton Polymers 0.000 claims description 3
- 235000019482 Palm oil Nutrition 0.000 claims description 3
- 239000003225 biodiesel Substances 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 239000004927 clay Substances 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 150000002430 hydrocarbons Chemical class 0.000 claims description 3
- 239000002540 palm oil Substances 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims 1
- 239000012752 auxiliary agent Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 3
- 239000000654 additive Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 238000005457 optimization Methods 0.000 description 6
- 238000005260 corrosion Methods 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 4
- 230000006872 improvement Effects 0.000 description 2
- YZCKVEUIGOORGS-OUBTZVSYSA-N Deuterium Chemical compound [2H] YZCKVEUIGOORGS-OUBTZVSYSA-N 0.000 description 1
- YZCKVEUIGOORGS-NJFSPNSNSA-N Tritium Chemical compound [3H] YZCKVEUIGOORGS-NJFSPNSNSA-N 0.000 description 1
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L53/00—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L53/02—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes
- C08L53/025—Compositions of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers of vinyl-aromatic monomers and conjugated dienes modified
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/04—Thermoplastic elastomer
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a thermoplastic elastomer with low compression set characteristics, which comprises the following raw materials in parts by weight: 45-55 parts of hydrogenated polystyrene-butadiene-styrene block copolymer, 25-30 parts of polystyrene, 2-6 parts of vulcanizing agent, 3-6 parts of hydroxyl silicone oil, 2-5 parts of auxiliary oil, 5-7 parts of filler and 1-2 parts of antioxidant. The thermoplastic elastomer of the invention uses hydrogenated polystyrene-butadiene-styrene block copolymer and polystyrene ratio as matrix material, and adds vulcanizing agent, hydroxy silicone oil, auxiliary agent and other additives to enhance the functional effect of the product and improve the low compression set property of the product.
Description
Technical Field
The invention relates to the technical field of thermoplastic elastomers, in particular to a thermoplastic elastomer with low compression set characteristics and a preparation method thereof.
Background
Thermoplastic elastomers are a class of elastomeric materials that have the elasticity of rubber at ordinary temperatures and are plasticized and shaped at high temperatures. The thermoplastic elastomer may be repeatedly processed and recycled using a process similar to that of a thermoplastic resin.
The prior thermoplastic elastomer has the advantages that the strength and the elongation at break performance are reduced in order to improve the low compression set performance, and the thermoplastic elastomer with the low compression set characteristic and the preparation method are improved by the coordination and improvement treatment of the prior thermoplastic elastomer.
Disclosure of Invention
In view of the drawbacks of the prior art, an object of the present invention is to provide a thermoplastic elastomer with low compression set characteristics and a method for preparing the same, so as to solve the problems set forth in the background art.
The invention solves the technical problems by adopting the following technical scheme:
the invention provides a thermoplastic elastomer with low compression set characteristics, which comprises the following raw materials in parts by weight:
45-55 parts of hydrogenated polystyrene-butadiene-styrene block copolymer, 25-30 parts of polystyrene, 2-6 parts of vulcanizing agent, 3-6 parts of hydroxyl silicone oil, 2-5 parts of auxiliary oil, 5-7 parts of filler and 1-2 parts of antioxidant.
Preferably, the hydrogenated polystyrene-butadiene-styrene block copolymer is a styrene-ethylene/propylene-styrene block copolymer.
Preferably, the thermoplastic elastomer is further added with 5-10 parts by weight of nano silicon dioxide modifier and 1-3 parts by weight of chitosan liquid modified calcium sulfate whisker complex.
Preferably, the preparation method of the nano silicon dioxide modifier comprises the following steps:
s01: firstly, 4-7 parts of nano silicon oxide is sent into 10-15 parts of sodium alginate aqueous solution for standing treatment for 15-25min, the standing temperature is 55-65 ℃, and after standing, water washing and drying are carried out;
s02: then heat treating at 210-220 deg.C for 10-20min, cooling to room temperature at 1-3 deg.C/min;
s03: finally, the mixture is sent into a ball mill for ball milling for 10-20min, the ball milling rotating speed is 1000-1500r/min, and the nano silicon dioxide modifier is obtained after the ball milling is finished.
Preferably, the mass fraction of the sodium alginate aqueous solution is 10-15%.
Preferably, the preparation method of the chitosan liquid modified calcium sulfate whisker complex comprises the following steps:
s101: delivering bentonite into deionized water with the power of 5-10 times of that of the bentonite, and fully dispersing the bentonite by ultrasonic with the ultrasonic power of 500-1000W for 5-10min to obtain dispersed bentonite;
s102: adding 5-10 parts of dispersed bentonite into 20-30 parts of chitosan aqueous solution, then adding 1-3 parts of sodium dodecyl sulfate and 2-4 parts of coupling agent KH560, and uniformly stirring to obtain chitosan compound solution;
s103: placing the calcium sulfate whisker into a mixed acid solution for pre-stirring modification, fully stirring, washing with water and drying;
s104: and adding the S103 product into the S102 product according to the weight ratio of 1:5, stirring fully, washing with water and drying to obtain the chitosan liquid modified calcium sulfate whisker complex.
Preferably, the mass fraction of the chitosan aqueous solution is 10-20%.
Preferably, the mixed acid solution is prepared by stirring and mixing a hydrogen peroxide solution with the mass fraction of 2-5% and a hydrochloric acid solution with the mass fraction of 1-3% according to the weight ratio of 1:3.
Preferably, the filler is one or more of talcum powder, calcium carbonate and clay, and the auxiliary oil is one or more of soybean oil, cotton oil, palm oil and hydrocarbon biodiesel; the antioxidant is antioxidant DLTP; the vulcanizing agent is dicumyl peroxide.
The invention also provides a preparation method of the thermoplastic elastomer with low compression set characteristics, which comprises the following steps: sequentially stirring and uniformly mixing the raw materials, then sending the raw materials into an extruder, and obtaining a thermoplastic elastomer material through melting, extrusion and granulation of the extruder; wherein the length-diameter ratio of the double-screw extruder is more than 56, the melt blending extrusion temperature is 210-220 ℃, and the rotating speed of the extruder is 350r/min.
Compared with the prior art, the invention has the following beneficial effects:
according to the thermoplastic elastomer disclosed by the invention, the hydrogenated polystyrene-butadiene-styrene block copolymer and the polystyrene ratio are used as matrix materials, the vulcanizing agent, the hydroxyl silicone oil, the auxiliary agents such as auxiliary agents and the like are added to enhance the functional effect of the product, the low compression set characteristic performance of the product is improved, the nano silicon dioxide modifier and the chitosan liquid modified calcium sulfate whisker complex are added in a coordinated manner, the calcium sulfate whisker is distributed into the matrix as a whisker-like structure, the low compression set performance can be optimized through optimization modification and matched with the nano silicon dioxide modifier in a coordinated manner, meanwhile, the strength and elongation at break performance of the product are improved, and in addition, the product still has excellent performance stability under the acid corrosion condition.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The thermoplastic elastomer with low compression set characteristics in the embodiment comprises the following raw materials in parts by weight:
45-55 parts of hydrogenated polystyrene-butadiene-styrene block copolymer, 25-30 parts of polystyrene, 2-6 parts of vulcanizing agent, 3-6 parts of hydroxyl silicone oil, 2-5 parts of auxiliary oil, 5-7 parts of filler and 1-2 parts of antioxidant.
The hydrogenated polystyrene-butadiene-styrene block copolymer of this example is a styrene-ethylene/propylene-styrene block copolymer.
The thermoplastic elastomer of the embodiment is also added with 5-10 parts by weight of nano silicon dioxide modifier and 1-3 parts by weight of chitosan liquid modified calcium sulfate whisker complex.
The preparation method of the nano silicon dioxide modifier in the embodiment comprises the following steps:
s01: firstly, 4-7 parts of nano silicon oxide is sent into 10-15 parts of sodium alginate aqueous solution for standing treatment for 15-25min, the standing temperature is 55-65 ℃, and after standing, water washing and drying are carried out;
s02: then heat treating at 210-220 deg.C for 10-20min, cooling to room temperature at 1-3 deg.C/min;
s03: finally, the mixture is sent into a ball mill for ball milling for 10-20min, the ball milling rotating speed is 1000-1500r/min, and the nano silicon dioxide modifier is obtained after the ball milling is finished.
The mass fraction of the sodium alginate aqueous solution of the embodiment is 10-15%.
The preparation method of the chitosan liquid modified calcium sulfate whisker complex of the embodiment comprises the following steps:
s101: delivering bentonite into deionized water with the power of 5-10 times of that of the bentonite, and fully dispersing the bentonite by ultrasonic with the ultrasonic power of 500-1000W for 5-10min to obtain dispersed bentonite;
s102: adding 5-10 parts of dispersed bentonite into 20-30 parts of chitosan aqueous solution, then adding 1-3 parts of sodium dodecyl sulfate and 2-4 parts of coupling agent KH560, and uniformly stirring to obtain chitosan compound solution;
s103: placing the calcium sulfate whisker into a mixed acid solution for pre-stirring modification, fully stirring, washing with water and drying;
s104: and adding the S103 product into the S102 product according to the weight ratio of 1:5, stirring fully, washing with water and drying to obtain the chitosan liquid modified calcium sulfate whisker complex.
The mass fraction of the chitosan aqueous solution of the embodiment is 10-20%.
The mixed acid solution of the embodiment is prepared by stirring and mixing a hydrogen peroxide solution with the mass fraction of 2-5% and a hydrochloric acid solution with the mass fraction of 1-3% according to the weight ratio of 1:3.
The filler of the embodiment is one or more of talcum powder, calcium carbonate and clay, and the auxiliary oil is one or more of soybean oil, cotton oil, palm oil and hydrocarbon biodiesel; the antioxidant is antioxidant DLTP; the vulcanizing agent is dicumyl peroxide.
The preparation method of the thermoplastic elastomer with low compression set characteristic in the embodiment comprises the following steps: sequentially stirring and uniformly mixing the raw materials, then sending the raw materials into an extruder, and obtaining a thermoplastic elastomer material through melting, extrusion and granulation of the extruder; wherein the length-diameter ratio of the double-screw extruder is more than 56, the melt blending extrusion temperature is 210-220 ℃, and the rotating speed of the extruder is 350r/min.
Example 1
The thermoplastic elastomer with low compression set characteristics in the embodiment comprises the following raw materials in parts by weight:
45 parts of hydrogenated polystyrene-butadiene-styrene block copolymer, 25 parts of polystyrene, 2 parts of vulcanizing agent, 3 parts of hydroxyl silicone oil, 2 parts of auxiliary oil, 5 parts of filler and 1 part of antioxidant.
The hydrogenated polystyrene-butadiene-styrene block copolymer of this example is a styrene-ethylene/propylene-styrene block copolymer.
The thermoplastic elastomer of the embodiment is also added with 5 parts by weight of nano silicon dioxide modifier and 1 part by weight of chitosan liquid modified calcium sulfate whisker complex.
The preparation method of the nano silicon dioxide modifier in the embodiment comprises the following steps:
s01: firstly, 4 parts of nano silicon oxide is sent into 10 sodium alginate aqueous solution for standing treatment for 15min, the standing temperature is 55 ℃, and after standing, water washing and drying are carried out;
s02: then heat-treating at 210 ℃ for 10min, and cooling to room temperature at a speed of 1 ℃/min after the treatment is finished;
s03: finally, the mixture is sent into a ball mill for ball milling for 10min, the ball milling rotating speed is 1000r/min, and the nano silicon dioxide modifier is obtained after the ball milling is finished.
The mass fraction of the sodium alginate aqueous solution of this example was 10%.
The preparation method of the chitosan liquid modified calcium sulfate whisker complex of the embodiment comprises the following steps:
s101: delivering bentonite into deionized water with the power of 5 times, and fully dispersing the bentonite by ultrasonic, wherein the ultrasonic power is 500W, and the ultrasonic time is 5min, so as to obtain dispersed bentonite;
s102: adding 5 parts of dispersed bentonite into 20 parts of chitosan aqueous solution, then adding 1 part of sodium dodecyl sulfate and 2 parts of coupling agent KH560, and uniformly stirring to obtain chitosan compound solution;
s103: placing the calcium sulfate whisker into a mixed acid solution for pre-stirring modification, fully stirring, washing with water and drying;
s104: and adding the S103 product into the S102 product according to the weight ratio of 1:5, stirring fully, washing with water and drying to obtain the chitosan liquid modified calcium sulfate whisker complex.
The mass fraction of the chitosan aqueous solution of this example was 10%.
The mixed acid solution in the embodiment is prepared by stirring and mixing a hydrogen peroxide solution with the mass fraction of 2% and a hydrochloric acid solution with the mass fraction of 1% according to the weight ratio of 1:3.
The filler in the embodiment is talcum powder, and the auxiliary agent oil is soybean oil; the antioxidant is antioxidant DLTP; the vulcanizing agent is dicumyl peroxide.
The preparation method of the thermoplastic elastomer with low compression set characteristic in the embodiment comprises the following steps: sequentially stirring and uniformly mixing the raw materials, then sending the raw materials into an extruder, and obtaining a thermoplastic elastomer material through melting, extrusion and granulation of the extruder; wherein the length-diameter ratio of the double-screw extruder is more than 56, the melt blending extrusion temperature is 210 ℃, and the rotating speed of the extruder is 350r/min.
Example 2
The thermoplastic elastomer with low compression set characteristics in the embodiment comprises the following raw materials in parts by weight:
55 parts of hydrogenated polystyrene-butadiene-styrene block copolymer, 30 parts of polystyrene, 6 parts of vulcanizing agent, 6 parts of hydroxyl silicone oil, 5 parts of auxiliary oil, 7 parts of filler and 2 parts of antioxidant.
The hydrogenated polystyrene-butadiene-styrene block copolymer of this example is a styrene-ethylene/propylene-styrene block copolymer.
The thermoplastic elastomer of the embodiment is also added with 10 parts by weight of nano silicon dioxide modifier and 3 parts by weight of chitosan liquid modified calcium sulfate whisker complex.
The preparation method of the nano silicon dioxide modifier in the embodiment comprises the following steps:
s01: firstly, 7 parts of nano silicon oxide is sent into 15 sodium alginate aqueous solution for standing treatment for 25min, the standing temperature is 65 ℃, and after standing, water washing and drying are carried out;
s02: then heat-treating at 220 ℃ for 20min, and cooling to room temperature at a speed of 3 ℃/min after the treatment is finished;
s03: finally, the mixture is sent into a ball mill for ball milling for 20min, the ball milling rotating speed is 1500r/min, and the nano silicon dioxide modifier is obtained after the ball milling is finished.
The mass fraction of the sodium alginate aqueous solution of this example was 15%.
The preparation method of the chitosan liquid modified calcium sulfate whisker complex of the embodiment comprises the following steps:
s101: delivering bentonite into 10 times deionized water for full ultrasonic dispersion, wherein the ultrasonic power is 1000W, and the ultrasonic time is 5-10min, so as to obtain dispersed bentonite;
s102: adding 10 parts of dispersed bentonite into 30 parts of chitosan aqueous solution, then adding 3 parts of sodium dodecyl sulfate and 4 parts of coupling agent KH560, and uniformly stirring to obtain chitosan compound solution;
s103: placing the calcium sulfate whisker into a mixed acid solution for pre-stirring modification, fully stirring, washing with water and drying;
s104: and adding the S103 product into the S102 product according to the weight ratio of 1:5, stirring fully, washing with water and drying to obtain the chitosan liquid modified calcium sulfate whisker complex.
The mass fraction of the chitosan aqueous solution of this example was 20%.
The mixed acid solution in the embodiment is prepared by stirring and mixing 5% of hydrogen peroxide solution and 3% of hydrochloric acid solution according to a weight ratio of 1:3.
The filler in the embodiment is talcum powder, and the auxiliary agent oil is soybean oil; the antioxidant is antioxidant DLTP; the vulcanizing agent is dicumyl peroxide.
The preparation method of the thermoplastic elastomer with low compression set characteristic in the embodiment comprises the following steps: sequentially stirring and uniformly mixing the raw materials, then sending the raw materials into an extruder, and obtaining a thermoplastic elastomer material through melting, extrusion and granulation of the extruder; wherein the length-diameter ratio of the double-screw extruder is more than 56, the melt blending extrusion temperature is 220 ℃, and the rotating speed of the extruder is 350r/min.
Example 3
The thermoplastic elastomer with low compression set characteristics in the embodiment comprises the following raw materials in parts by weight:
50 parts of hydrogenated polystyrene-butadiene-styrene block copolymer, 27 parts of polystyrene, 4 parts of vulcanizing agent, 4.5 parts of hydroxyl silicone oil, 3.5 parts of auxiliary oil, 6 parts of filler and 1.5 parts of antioxidant.
The hydrogenated polystyrene-butadiene-styrene block copolymer of this example is a styrene-ethylene/propylene-styrene block copolymer.
The thermoplastic elastomer of the embodiment is also added with 7.5 parts by weight of nano silicon dioxide modifier and 1-3 parts by weight of chitosan liquid modified calcium sulfate whisker complex.
The preparation method of the nano silicon dioxide modifier in the embodiment comprises the following steps:
s01: firstly, 5 parts of nano silicon oxide is sent into 12 sodium alginate aqueous solution for standing treatment for 20min, the standing temperature is 60 ℃, and after standing, water washing and drying are carried out;
s02: then heat-treating at 215 ℃ for 15min, and cooling to room temperature at a rate of 2 ℃/min after the treatment is finished;
s03: finally, the mixture is sent into a ball mill for ball milling for 15min, the ball milling rotating speed is 1250r/min, and the nano silicon dioxide modifier is obtained after the ball milling is finished.
The mass fraction of the sodium alginate aqueous solution of this example was 12%.
The preparation method of the chitosan liquid modified calcium sulfate whisker complex of the embodiment comprises the following steps:
s101: the bentonite is sent into deionized water with the power of 7.5 times to be fully dispersed, the ultrasonic power is 750W, and the ultrasonic time is 7.5min, so as to obtain the dispersed bentonite;
s102:7.5 parts of dispersed bentonite is added into 25 parts of chitosan aqueous solution, then 2 parts of sodium dodecyl sulfate and 3 parts of coupling agent KH560 are added, and the mixture is stirred uniformly to obtain chitosan compound solution;
s103: placing the calcium sulfate whisker into a mixed acid solution for pre-stirring modification, fully stirring, washing with water and drying;
s104: and adding the S103 product into the S102 product according to the weight ratio of 1:5, stirring fully, washing with water and drying to obtain the chitosan liquid modified calcium sulfate whisker complex.
The mass fraction of the chitosan aqueous solution of this example was 15%.
The mixed acid solution of the embodiment is prepared by stirring and mixing 3.5% of hydrogen peroxide solution and 2% of hydrochloric acid solution according to a weight ratio of 1:3.
The filler in the embodiment is talcum powder, and the auxiliary agent oil is soybean oil; the antioxidant is antioxidant DLTP; the vulcanizing agent is dicumyl peroxide.
The preparation method of the thermoplastic elastomer with low compression set characteristic in the embodiment comprises the following steps: sequentially stirring and uniformly mixing the raw materials, then sending the raw materials into an extruder, and obtaining a thermoplastic elastomer material through melting, extrusion and granulation of the extruder; wherein the length-diameter ratio of the double-screw extruder is more than 56, the melt blending extrusion temperature is 215 ℃, and the rotating speed of the extruder is 350r/min.
Comparative example 1.
The difference from optimization example 3 is that no nano silica modifier was added.
Comparative example 2.
The difference from optimization example 3 is that the nano-silica modifier is replaced by nano-silica.
Comparative example 3.
The difference from the optimized example 3 is that the preparation method of the nano silicon dioxide modifier is different; the step S02 processing is not adopted.
Comparative example 4.
The difference from the optimized example 3 is that the calcium sulfate whisker complex modified by the chitosan solution is not added.
Comparative example 5.
The difference from the optimization example 3 is that no dispersed bentonite is added in the preparation of the chitosan liquid modified calcium sulfate whisker complex.
Comparative example 6.
The difference from the optimization example 3 is that the calcium sulfate whisker is replaced by aluminum borate whisker in the preparation of the chitosan liquid modified calcium sulfate whisker compound.
Comparative example 7.
The difference from the optimization example 3 is that the chitosan compound liquid is not added in the preparation of the chitosan liquid modified calcium sulfate whisker complex.
Comparative example 8.
The difference from the optimized example 3 is that no coupling agent KH560 is added into the chitosan complex solution.
Comparative example 9.
The difference from the optimized example 3 is that the calcium sulfate whisker is not treated with the mixed acid solution.
The results of the performance measurements of examples 1-3 and comparative examples 1-9 are as follows
The tensile strength and the elongation at break of the product have a coordinated improvement effect, and meanwhile, the product has excellent performance under the compression set of 70 ℃ and 22 hours, and in addition, the performance stability of the product is obvious under the acid corrosion condition;
the product performance is obviously deteriorated without adding one of the nano silicon dioxide modifier and the chitosan liquid modified calcium sulfate whisker compound, and the product performance is enhanced by adopting the cooperation of the nano silicon dioxide modifier and the chitosan liquid modified calcium sulfate whisker compound, and the stability of the product under the acid corrosion condition is optimized;
the preparation of the chitosan liquid modified calcium sulfate whisker compound is not added with dispersed bentonite, chitosan compound liquid and composition of the chitosan compound liquid are different, meanwhile, the calcium sulfate whisker is not treated by adopting mixed acid solution, the performance of the product is prone to be deteriorated, and only the chitosan liquid modified calcium sulfate whisker compound prepared by adopting the method has the most remarkable performance effect;
meanwhile, the calcium sulfate whisker adopted in the preparation of the chitosan liquid modified calcium sulfate whisker compound is replaced by other whiskers, and the data show that the product has more remarkable performance degradation under the acid corrosion condition, so that the raw materials adopted in the preparation of the chitosan liquid modified calcium sulfate whisker compound have the specificity, and meanwhile, the proportion and the process of the product have the specificity, and only the product prepared by adopting the process of the invention has the most remarkable performance effect.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (10)
1. The thermoplastic elastomer with low compression set characteristics is characterized by comprising the following raw materials in parts by weight:
45-55 parts of hydrogenated polystyrene-butadiene-styrene block copolymer, 25-30 parts of polystyrene, 2-6 parts of vulcanizing agent, 3-6 parts of hydroxyl silicone oil, 2-5 parts of auxiliary oil, 5-7 parts of filler and 1-2 parts of antioxidant.
2. A thermoplastic elastomer with low compression set properties according to claim 1 wherein the hydrogenated polystyrene-butadiene-styrene block copolymer is a styrene-ethylene/propylene-styrene block copolymer.
3. The thermoplastic elastomer with low compression set characteristics according to claim 1, wherein the thermoplastic elastomer is further added with 5-10 parts by weight of nano silica modifier and 1-3 parts by weight of chitosan liquid modified calcium sulfate whisker complex.
4. A thermoplastic elastomer with low compression set characteristics according to claim 3, wherein said nano silica modifier is prepared by the following steps:
s01: firstly, 4-7 parts of nano silicon oxide is sent into 10-15 parts of sodium alginate aqueous solution for standing treatment for 15-25min, the standing temperature is 55-65 ℃, and after standing, water washing and drying are carried out;
s02: then heat treating at 210-220 deg.C for 10-20min, cooling to room temperature at 1-3 deg.C/min;
s03: finally, the mixture is sent into a ball mill for ball milling for 10-20min, the ball milling rotating speed is 1000-1500r/min, and the nano silicon dioxide modifier is obtained after the ball milling is finished.
5. The thermoplastic elastomer with low compression set characteristics according to claim 4, wherein the mass fraction of the aqueous sodium alginate solution is 10-15%.
6. A thermoplastic elastomer with low compression set characteristics according to claim 3, wherein said chitosan liquid modified calcium sulfate whisker composite is prepared by the following steps:
s101: delivering bentonite into deionized water with the power of 5-10 times of that of the bentonite, and fully dispersing the bentonite by ultrasonic with the ultrasonic power of 500-1000W for 5-10min to obtain dispersed bentonite;
s102: adding 5-10 parts of dispersed bentonite into 20-30 parts of chitosan aqueous solution, then adding 1-3 parts of sodium dodecyl sulfate and 2-4 parts of coupling agent KH560, and uniformly stirring to obtain chitosan compound solution;
s103: placing the calcium sulfate whisker into a mixed acid solution for pre-stirring modification, fully stirring, washing with water and drying;
s104: and adding the S103 product into the S102 product according to the weight ratio of 1:5, stirring fully, washing with water and drying to obtain the chitosan liquid modified calcium sulfate whisker complex.
7. The thermoplastic elastomer with low compression set according to claim 6, wherein the mass fraction of the aqueous chitosan solution is 10-20%.
8. The thermoplastic elastomer with low compression set characteristics according to claim 6, wherein the mixed acid solution is a hydrogen peroxide solution with the mass fraction of 2-5% and a hydrochloric acid solution with the mass fraction of 1-3% which are mixed according to the weight ratio of 1:3.
9. The thermoplastic elastomer with low compression set characteristics according to claim 1, wherein the filler is one or more of talcum powder, calcium carbonate and clay, and the auxiliary oil is one or more of soybean oil, cotton oil, palm oil and hydrocarbon biodiesel; the antioxidant is antioxidant DLTP; the vulcanizing agent is dicumyl peroxide.
10. A process for the preparation of a thermoplastic elastomer having low compression set characteristics comprising the steps of: sequentially stirring and uniformly mixing the raw materials, then sending the raw materials into an extruder, and obtaining a thermoplastic elastomer material through melting, extrusion and granulation of the extruder; wherein the length-diameter ratio of the double-screw extruder is more than 56, the melt blending extrusion temperature is 210-220 ℃, and the rotating speed of the extruder is 350r/min.
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