CN114350007A - Preparation method of modified TPE composite material and modified TPE composite material - Google Patents
Preparation method of modified TPE composite material and modified TPE composite material Download PDFInfo
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- CN114350007A CN114350007A CN202210120898.0A CN202210120898A CN114350007A CN 114350007 A CN114350007 A CN 114350007A CN 202210120898 A CN202210120898 A CN 202210120898A CN 114350007 A CN114350007 A CN 114350007A
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- 239000002131 composite material Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000203 mixture Substances 0.000 claims abstract description 81
- 238000012545 processing Methods 0.000 claims abstract description 3
- 229920002725 thermoplastic elastomer Polymers 0.000 claims description 82
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 64
- 238000003756 stirring Methods 0.000 claims description 33
- 238000000034 method Methods 0.000 claims description 23
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 22
- 239000004327 boric acid Substances 0.000 claims description 22
- 235000011187 glycerol Nutrition 0.000 claims description 22
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 20
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 15
- 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 claims description 10
- 239000004156 Azodicarbonamide Substances 0.000 claims description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 10
- 235000021355 Stearic acid Nutrition 0.000 claims description 10
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 claims description 10
- 235000019399 azodicarbonamide Nutrition 0.000 claims description 10
- 229910052791 calcium Inorganic materials 0.000 claims description 10
- 239000011575 calcium Substances 0.000 claims description 10
- 238000005187 foaming Methods 0.000 claims description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 10
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 10
- 239000000843 powder Substances 0.000 claims description 10
- 229920002545 silicone oil Polymers 0.000 claims description 10
- 239000008117 stearic acid Substances 0.000 claims description 10
- 239000011787 zinc oxide Substances 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 9
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 8
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 5
- 239000000376 reactant Substances 0.000 claims description 5
- 238000010074 rubber mixing Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- 235000014692 zinc oxide Nutrition 0.000 claims description 5
- 229910000831 Steel Inorganic materials 0.000 description 6
- 239000010959 steel Substances 0.000 description 6
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
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Abstract
The invention relates to the technical field of composite materials, and provides a preparation method of a modified TPE composite material and the modified TPE composite material, which comprises the following steps: preparing a first mixture, namely modifying TPE to obtain a first mixture; preparing a TPE composite material, namely processing the first mixture and the first composition to obtain the TPE composite material; the TPE composite material obtained through the steps of preparing the first mixture and preparing the TPE composite material not only shows excellent flexibility, but also has excellent resilience.
Description
Technical Field
The invention relates to the technical field of composite materials, in particular to a preparation method of a modified TPE composite material and the modified TPE composite material.
Background
TPE is a thermoplastic elastomer with both plastic and rubber properties. TPE has the characteristics of high elasticity, high strength and high resilience of rubber at normal temperature, and can be plasticized and molded at high temperature. Meanwhile, the TPE also has the excellent characteristics of safety, environmental protection, weather resistance, temperature resistance and the like, so that the TPE is widely applied to the cushioning and shock absorption fields of yoga mats and the like.
As a protective material with excellent mechanical properties, the rebound resilience and flexibility of TPE still need to be further improved, and the goal is always the development direction of TPE materials. How to effectively solve the technical difficulties is a problem to be solved by the technical personnel in the field at present.
Disclosure of Invention
In order to solve the technical problems or at least partially solve the technical problems, the invention provides a preparation method of a modified TPE composite material and the modified TPE composite material.
The preparation method of the modified TPE composite material comprises the following steps:
preparing a first mixture, namely modifying TPE to obtain a first mixture;
and preparing the TPE composite material, namely processing the first mixture and the first composition to obtain the TPE composite material.
Further, in the step of preparing the first mixture, the material components for modifying the TPE include:
89-93 parts of hydroxyl silicone oil, 4-6 parts of boric acid and 3-11 parts of glycerol.
Further, in the step of preparing the first mixture, the modifying treatment of the TPE comprises:
a dissolving step of dissolving the boric acid in the glycerol to obtain a second mixture;
a first heating step, namely heating the second mixture for the first time to obtain a third mixture;
and a second heating step, namely heating the third mixture for the second time to obtain a first mixture.
Further, in the dissolving step, the process of dissolving boric acid and glycerin is;
adding glycerol and boric acid into a reaction container, starting stirring, setting the temperature of an electric furnace to be 80-84 ℃, continuing stirring for 27-33min when the temperature reaches the set temperature, wherein the stirring speed is 300 r/min until the reactant is colorless and transparent, and the boric acid is completely dissolved in the glycerol.
Further, in the first heating step, the first heating of the second mixture is performed by:
and adding hydroxyl silicone oil into the reaction container, starting stirring, setting the temperature of the electric furnace to be 140-148 ℃, continuing stirring and keeping for 4 hours when the temperature reaches the set temperature, then closing stirring, standing for 10min, and pouring out the upper layer liquid in the reaction container, wherein the upper layer liquid is the third mixture.
Further, in the second heating step, the second heating of the third mixture is performed by:
putting the third mixture into a vacuum drying box, extracting vacuum, keeping the temperature for 2 hours when the temperature reaches the set temperature of 160-163 ℃, and naturally cooling to obtain the first mixture;
wherein the pressure in the vacuumizing process is between-1 MPa and-4 MPa.
Further, in the step of preparing the TPE composite, the first composition component comprises:
62-66 parts of ethylene-vinyl acetate copolymer, 13-16 parts of TPE, 12-15 parts of calcium powder, 2-4 parts of azodicarbonamide, 1-2 parts of zinc oxide, 0.5-1 part of stearic acid and 0.6-1.1 part of dicumyl peroxide.
Further, in the step of preparing the TPE composite, the step of treating the first mixture with the first composition comprises:
heating a double-roller rubber mixing mill to 127-;
adding calcium powder, azodicarbonamide, zinc oxide, stearic acid and dicumyl peroxide into the fourth mixture, and banburying for the second time to obtain a fifth mixture;
and (3) placing the fifth mixture into a foaming machine, and foaming for 18-23min at the temperature of 148-156 ℃ to obtain the TPE composite material.
Further, slicing the TPE composite material to obtain a test sample.
The modified TPE composite material is prepared according to the preparation method.
In the present invention, the TPE composite obtained through the first mixture preparation step and the TPE composite preparation step exhibits not only excellent flexibility but also excellent resilience.
Drawings
Figure 1 is a tensile stress-strain graph of TPE bulk and TPE composite provided in this example.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, the present invention will be further described in detail with reference to the accompanying drawings and examples. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. The following examples are intended to illustrate the invention, but not to limit it. All other embodiments, which can be derived by a person skilled in the art from the described embodiments of the invention, are within the scope of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
It is noted that, in this document, relational terms such as "first" and "second," and the like, may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. The terms "connected" and "coupled" are used broadly and may include, for example, a fixed connection, a removable connection, or an integral part; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. The terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Example 1
Adding glycerol and boric acid into a reaction container, starting stirring, setting the temperature of an electric furnace to be 80 ℃, continuing stirring for 33min when the temperature reaches the set temperature, wherein the stirring speed is 300 r/min until the reactant is colorless and transparent, and the boric acid is completely dissolved in the glycerol.
After boric acid is completely dissolved in glycerol, adding hydroxyl silicone oil into the reaction vessel, simultaneously starting stirring, setting the temperature of the electric furnace to be 140 ℃, continuing stirring and keeping for 4 hours when the temperature reaches the set temperature, then closing stirring, standing for 10min, and pouring out the upper layer liquid in the reaction vessel, wherein the upper layer liquid is a third mixture.
93 parts of hydroxyl silicone oil, 4 parts of boric acid and 11 parts of glycerol.
And putting the third mixture into a vacuum drying box, vacuumizing, keeping the pressure at-1 MPa and the set temperature at 163 ℃ in the vacuumizing process for 2 hours when the temperature reaches the set temperature, and naturally cooling to obtain a first mixture, thereby finishing the modification of the TPE material.
And (3) heating the two-roll rubber mixing mill to 127 ℃, adding the ethylene-vinyl acetate copolymer, the TPE and the first mixture, and stirring for 2 hours to uniformly mix the mixture to obtain a fourth mixture.
And adding calcium powder, azodicarbonamide, zinc oxide, stearic acid and dicumyl peroxide into the fourth mixture, and banburying for the second time to obtain a fifth mixture.
The coating comprises, by weight, 66 parts of an ethylene-vinyl acetate copolymer, 13 parts of TPE, 15 parts of calcium powder, 2 parts of azodicarbonamide, 2 parts of zinc oxide, 0.5 part of stearic acid and 1.1 part of dicumyl peroxide.
And putting the fifth mixture into a foaming machine, and foaming at the temperature of 148 ℃ for 23min to obtain the TPE composite material.
And slicing the TPE composite material to obtain a test sample for testing the performance of the TPE composite material.
The modified TPE composite material is prepared according to the preparation method.
Example 2
Adding glycerol and boric acid into a reaction container, starting stirring, setting the temperature of an electric furnace to 82 ℃, continuing stirring for 30min when the temperature reaches the set temperature, wherein the stirring speed is 300 r/min until the reactant is colorless and transparent, and the boric acid is completely dissolved in the glycerol.
After boric acid is completely dissolved in glycerol, adding hydroxyl silicone oil into the reaction vessel, simultaneously starting stirring, setting the temperature of the electric furnace to 144 ℃, continuing stirring and keeping for 4 hours when the temperature reaches the set temperature, then closing stirring, standing for 10 minutes, and pouring out the upper layer liquid in the reaction vessel, wherein the upper layer liquid is a third mixture.
91 parts of hydroxyl silicone oil, 5 parts of boric acid and 7 parts of glycerol.
And putting the third mixture into a vacuum drying box, vacuumizing, keeping the pressure at-2 MPa and the set temperature at 162 ℃ in the vacuumizing process, keeping for 2 hours when the temperature reaches the set temperature, naturally cooling to obtain a first mixture, and finishing the modification of the TPE material.
And (3) heating the two-roll rubber mixing mill to 130 ℃, adding the ethylene-vinyl acetate copolymer, the TPE and the first mixture, and stirring for 2 hours to uniformly mix the mixture to obtain a fourth mixture.
And adding calcium powder, azodicarbonamide, zinc oxide, stearic acid and dicumyl peroxide into the fourth mixture, and banburying for the second time to obtain a fifth mixture.
Wherein, 64 parts of ethylene-vinyl acetate copolymer, 15 parts of TPE, 13 parts of calcium powder, 3 parts of azodicarbonamide, 1.5 parts of zinc oxide, 0.7 part of stearic acid and 0.8 part of dicumyl peroxide.
And (4) placing the fifth mixture into a foaming machine, and foaming for 21min at the temperature of 152 ℃ to obtain the TPE composite material.
And slicing the TPE composite material to obtain a test sample for testing the performance of the TPE composite material.
The modified TPE composite material is prepared according to the preparation method.
Example 3
Adding glycerol and boric acid into a reaction container, starting stirring, setting the temperature of an electric furnace to 84 ℃, continuing stirring for 27min when the temperature reaches the set temperature, wherein the stirring speed is 300 r/min until the reactant is colorless and transparent, and the boric acid is completely dissolved in the glycerol.
After boric acid is completely dissolved in glycerol, adding hydroxyl silicone oil into the reaction vessel, simultaneously starting stirring, setting the temperature of the electric furnace to be 148 ℃, continuing stirring and keeping for 4 hours when the temperature reaches the set temperature, then closing stirring, standing for 10 minutes, and pouring out the upper layer liquid in the reaction vessel, wherein the upper layer liquid is a third mixture.
89 parts of hydroxyl silicone oil, 6 parts of boric acid and 3 parts of glycerol.
And putting the third mixture into a vacuum drying box, vacuumizing, keeping the pressure at-4 MPa and the set temperature at 160 ℃ in the vacuumizing process for 2 hours when the temperature reaches the set temperature, and naturally cooling to obtain a first mixture, thereby finishing the modification of the TPE material.
And (3) heating the two-roll rubber mixing mill to 133 ℃, adding the ethylene-vinyl acetate copolymer, the TPE and the first mixture, and stirring for 2 hours to uniformly mix the mixture to obtain a fourth mixture.
And adding calcium powder, azodicarbonamide, zinc oxide, stearic acid and dicumyl peroxide into the fourth mixture, and banburying for the second time to obtain a fifth mixture.
The coating comprises, by weight, 62 parts of an ethylene-vinyl acetate copolymer, 16 parts of TPE, 12 parts of calcium powder, 4 parts of azodicarbonamide, 1 part of zinc oxide, 1 part of stearic acid and 0.6 part of dicumyl peroxide.
And (4) placing the fifth mixture into a foaming machine, and foaming for 18min at the temperature of 156 ℃ to obtain the TPE composite material.
And slicing the TPE composite material to obtain a test sample for testing the performance of the TPE composite material.
The modified TPE composite material is prepared according to the preparation method.
The TPE composites (15% of the first mixture) prepared by the methods of example 1, example 2 and example 3 were tested for their properties
Resilience performance
4g of steel ball is placed at the same height of 60cm, the steel ball freely falls down and then acts on the TPE material and the TPE composite material respectively, and the rebound resilience of the material is evaluated by measuring the rebound height of the steel ball.
Under the same falling height, the rebound height of the steel ball after acting on the TPE material is 17cm, and the rebound height of the steel ball acting on the TPE composite material is 28 cm. Therefore, compared with the TPE material, the rebound height of the steel ball impacting the TPE composite material is improved by 65%, which shows that the TPE composite material has better rebound resilience.
Tensile breaking Properties
And testing the tensile and tear resistance of the TPE material and the TPE composite material by using a universal material testing machine to obtain a load-deformation relation, and analyzing the breaking tension and the breaking elongation.
The tensile stress-strain curves of the TPE material and the TPE composite material are shown in FIG. 1, and the elongation at break of the TPE material and the TPE composite material is 188% and 221%, respectively. Thus, the elongation at break of the TPE composite increased by 17.5% relative to the TPE baseline, indicating that the TPE composite exhibited better toughness. Meanwhile, the elastic modulus (stress-strain curve elastic segment slope) of the TPE composite material is smaller than that of the TPE material, which shows that the TPE composite material has better flexibility.
The above description is not intended to limit the present invention, and it should be finally explained that: the above examples are only for illustrating the technical solutions of the present invention, and are not limited thereto. Although the present invention has been described in detail with reference to the foregoing embodiments. Those of ordinary skill in the art will understand that: it is to be understood that modifications may be made to the above-described arrangements in the embodiments or equivalents may be substituted for some of the features of the embodiments without departing from the spirit of the present invention.
Claims (10)
1. A preparation method of a modified TPE composite material is characterized by comprising the following steps:
preparing a first mixture, namely modifying TPE to obtain a first mixture;
and preparing the TPE composite material, namely processing the first mixture and the first composition to obtain the TPE composite material.
2. The method of claim 1, wherein in the step of preparing the first mixture, the material components for modifying the TPE comprise:
89-93 parts of hydroxyl silicone oil, 4-6 parts of boric acid and 3-11 parts of glycerol.
3. The method of claim 2, wherein in the step of preparing the first mixture, the modifying the TPE comprises:
a dissolving step of dissolving the boric acid in the glycerol to obtain a second mixture;
a first heating step, namely heating the second mixture for the first time to obtain a third mixture;
and a second heating step, namely heating the third mixture for the second time to obtain a first mixture.
4. The method of claim 3, wherein in the dissolving step, the process of dissolving boric acid and glycerin is;
adding glycerol and boric acid into a reaction container, starting stirring, setting the temperature of an electric furnace to be 80-84 ℃, continuing stirring for 27-33min when the temperature reaches the set temperature, wherein the stirring speed is 300 r/min until the reactant is colorless and transparent, and the boric acid is completely dissolved in the glycerol.
5. The method of claim 3, wherein the first heating of the second mixture in the first heating step comprises:
and adding hydroxyl silicone oil into the reaction container, starting stirring, setting the temperature of the electric furnace to be 140-148 ℃, continuing stirring and keeping for 4 hours when the temperature reaches the set temperature, then closing stirring, standing for 10min, and pouring out the upper layer liquid in the reaction container, wherein the upper layer liquid is the third mixture.
6. The method of claim 3, wherein the second heating step is performed by subjecting the third mixture to:
putting the third mixture into a vacuum drying box, extracting vacuum, keeping the temperature for 2 hours when the temperature reaches the set temperature of 160-163 ℃, and naturally cooling to obtain the first mixture;
wherein the pressure in the vacuumizing process is between-1 MPa and-4 MPa.
7. The process of claim 1, wherein in the step of preparing a TPE composite, the first composition component comprises:
62-66 parts of ethylene-vinyl acetate copolymer, 13-16 parts of TPE, 12-15 parts of calcium powder, 2-4 parts of azodicarbonamide, 1-2 parts of zinc oxide, 0.5-1 part of stearic acid and 0.6-1.1 part of dicumyl peroxide.
8. The process of claim 7, wherein the step of preparing the TPE composite comprises the steps of treating the first mixture with a first composition by:
heating a double-roller rubber mixing mill to 127-;
adding calcium powder, azodicarbonamide, zinc oxide, stearic acid and dicumyl peroxide into the fourth mixture, and banburying for the second time to obtain a fifth mixture;
and (3) placing the fifth mixture into a foaming machine, and foaming for 18-23min at the temperature of 148-156 ℃ to obtain the TPE composite material.
9. The method of claim 8, wherein the TPE composite is sliced to obtain test samples.
10. A modified TPE composite prepared according to the method of any one of claims 1-9.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818075A (en) * | 2014-02-28 | 2014-05-28 | 浙江润阳新材料科技有限公司 | Foaming composite material with high thermal conductivity |
| EP3075528A1 (en) * | 2015-04-01 | 2016-10-05 | Lee, Yung-Teng | Multi-layered thermoplastic elastomer foam and process for manufacturing the same |
| CN107189188A (en) * | 2017-07-07 | 2017-09-22 | 三斯达（江苏）环保科技有限公司 | A kind of vibration-damping foamed materials of new TPE and its preparation |
| CN112625333A (en) * | 2020-12-18 | 2021-04-09 | 衡阳丰泰鞋业有限公司 | High-wear-resistance and high-damping sneaker sole material and preparation method thereof |
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- 2022-02-09 CN CN202210120898.0A patent/CN114350007A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103818075A (en) * | 2014-02-28 | 2014-05-28 | 浙江润阳新材料科技有限公司 | Foaming composite material with high thermal conductivity |
| EP3075528A1 (en) * | 2015-04-01 | 2016-10-05 | Lee, Yung-Teng | Multi-layered thermoplastic elastomer foam and process for manufacturing the same |
| CN107189188A (en) * | 2017-07-07 | 2017-09-22 | 三斯达（江苏）环保科技有限公司 | A kind of vibration-damping foamed materials of new TPE and its preparation |
| CN112625333A (en) * | 2020-12-18 | 2021-04-09 | 衡阳丰泰鞋业有限公司 | High-wear-resistance and high-damping sneaker sole material and preparation method thereof |
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