CN111763418B - High-elasticity nylon and preparation method thereof - Google Patents
High-elasticity nylon and preparation method thereof Download PDFInfo
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- 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
- C08J9/14—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 organic
- C08J9/141—Hydrocarbons
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/243—Two or more independent types of crosslinking for one or more polymers
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- C—CHEMISTRY; METALLURGY
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0014—Use of organic additives
- C08J9/0023—Use of organic additives containing oxygen
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- C—CHEMISTRY; METALLURGY
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- 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
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- C—CHEMISTRY; METALLURGY
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- 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
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
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- C—CHEMISTRY; METALLURGY
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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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- 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
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/14—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers in which at least two but not all the silicon atoms are connected by linkages other than oxygen atoms
Abstract
The embodiment of the invention provides a preparation method of high-elasticity nylon, which comprises the following steps: obtaining nylon, polyborosiloxane and polyethylene glycol, and drying the polyborosiloxane; putting nylon, polyborosiloxane and polyethylene glycol into preset equipment, heating and uniformly mixing to obtain a first mixed material; obtaining cyclopentane, and placing the cyclopentane and the mixed material in an internal mixer for heating and internal mixing to obtain a second mixed material; preparing the second mixed material into slices, and placing the slices into a granulator for granulation to obtain granular substances; foaming the granular substance to obtain the high-elasticity nylon. Compared with the existing nylon elastomer, the high-elasticity nylon prepared by the method provided by the embodiment of the invention greatly improves the permanent compression deformation rate.
Description
Technical Field
The invention relates to the technical field of nylon elastomer modification methods, in particular to high-elasticity nylon and a preparation method thereof.
Background
Nylon elastomer (PEBAX) is a block polyamide elastomer product, belonging to engineering polymer. The product has a rather wide hardness range and good rebound resilience, and the remarkable processability makes the product an ideal material for producing parts.
The nylon elastomer also has good chemical resistance, heat resistance and weather resistance, and is widely applied to the fields of sports equipment, impact-resistant parts, watch shells and the like. However, the conventional nylon elastomer has a poor compression set and is difficult to recover its original state after compression set.
Disclosure of Invention
Aiming at the technical problems that the compression set rate of the existing nylon elastomer is poor and the original state is difficult to recover after compression deformation in the prior art, the embodiment of the invention provides high-elasticity nylon and a preparation method thereof. The specific technical scheme is as follows:
in a first aspect, an embodiment of the present invention provides a method for preparing a high-elasticity nylon, including:
obtaining nylon, polyborosiloxane and polyethylene glycol, and drying the polyborosiloxane; wherein the mass ratio of the nylon to the polyborosiloxane is 10-100: 1; the mass of the polyethylene glycol is 10% of that of the polyborosiloxane;
placing the nylon, the polyborosiloxane and the polyethylene glycol in a preset device, heating and uniformly mixing to obtain a first mixed material; wherein the heating temperature is 150 ℃ and 180 ℃, and the heating time is 3-5 min;
obtaining cyclopentane, and placing the cyclopentane and the mixed material in an internal mixer for heating and internal mixing to obtain a second mixed material; wherein the mass of the cyclopentane is 5-10% of the mass of the first mixed material, the banburying temperature is 150-180 ℃, and the banburying time is 7-10 min;
preparing the second mixed material into a slice, and placing the slice into a granulator for granulation to obtain granular substances;
foaming the particle substances to obtain high-elasticity nylon; wherein the foaming temperature is 160-180 ℃, the foaming time is 5-7min, and the foaming pressure is 140-160kg/cm2。
Optionally, the thickness of the sheet is 10 mm.
Optionally, the predetermined device is an extruder.
Optionally, the extruder is a twin-screw extruder or a single-screw extruder.
In a second aspect, the embodiment of the invention provides a high-elasticity nylon prepared by the preparation method of the high-elasticity nylon.
The embodiment of the invention provides a preparation method of high-elasticity nylon, which comprises the following steps: obtaining nylon, polyborosiloxane and polyethylene glycol, and drying the polyborosiloxane; putting nylon, polyborosiloxane and polyethylene glycol into preset equipment, heating and uniformly mixing to obtain a first mixed material; obtaining cyclopentane, and placing the cyclopentane and the mixed material in an internal mixer for heating and internal mixing to obtain a second mixed material; preparing the second mixed material into slices, and placing the slices into a granulator for granulation to obtain granular substances; foaming the granular substance to obtain the high-elasticity nylon. According to the high-elasticity nylon prepared by the method provided by the embodiment of the invention, boron in the polyborosiloxane can form physical crosslinking and chemical crosslinking through strong interaction with oxygen, and compared with the existing nylon elastomer, the permanent compression deformation rate is greatly improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a flow chart of a method for preparing a high-elasticity nylon according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be described below with reference to the drawings in the embodiments of the present invention.
Example 1
Referring to fig. 1, in a first aspect, an embodiment of the present invention provides a method for preparing a high-elasticity nylon, including:
obtaining nylon, polyborosiloxane and polyethylene glycol, and drying the polyborosiloxane; wherein the mass ratio of the nylon to the polyborosiloxane is 10-100: 1; the mass of the polyethylene glycol is 10% of that of the polyborosiloxane;
the nylon, the polyborosiloxane and the polyethylene glycol can be obtained by direct purchase, the purity and the content of each component are not particularly limited in the embodiment of the invention, and the effective content of each component meets the requirement that the mass ratio of the nylon to the polyborosiloxane is 10-100: 1; the mass of the polyethylene glycol is 10% of that of the polyborosiloxane.
Placing the nylon, the polyborosiloxane and the polyethylene glycol in a preset device, heating and uniformly mixing to obtain a first mixed material; wherein the heating temperature is 150 ℃ and 180 ℃, and the heating time is 3-5 min;
it should be noted that the predetermined device may be any device that can be heated and can last for a predetermined time, or may be a heating device, and the user records the heating time by himself, and after the heating is completed, the preparation of the next process can be directly performed without cooling, and of course, the preparation of the next process can be performed after the preparation of the next process is self-cooled.
Obtaining cyclopentane, and placing the cyclopentane and the mixed material in an internal mixer for heating and internal mixing to obtain a second mixed material; wherein the mass of the cyclopentane is 5-10% of the mass of the first mixed material, the banburying temperature is 150-180 ℃, and the banburying time is 7-10 min;
it should be noted that when the internal mixer is in operation, the two rotors rotate relatively to each other, so that the material from the feed inlet is clamped and carried into the roll gap to be extruded and sheared by the rotors, passes through the roll gap and then touches the sharp edge of the lower top bolt to be divided into two parts, and then returns to the upper part of the roll gap along the gap between the front and rear chamber walls and the rotors. In one circle of the revolving flow, the materials are subjected to shearing and friction effects everywhere, so that the temperature of the rubber material is increased rapidly, the viscosity is reduced, the wettability of the rubber on the surface of the compounding agent is increased, and the rubber is in full contact with the surface of the compounding agent. The compounding agent lumps pass through the gaps between the rotor and the rotor, between the rotor and the upper and lower top bolts and between the rotor and the inner wall of the mixing chamber together with the rubber material, are sheared and crushed, are surrounded by the rubber which is stretched and deformed, and are stabilized in a crushed state. Meanwhile, the convex edges on the rotor enable the rubber to move along the axial direction of the rotor, so that the stirring and mixing effects are achieved, and the compounding agents are uniformly mixed in the rubber. The compounding agent is sheared and crushed repeatedly, the rubber material deforms and recovers to deform repeatedly, and the rotor ribs are stirred continuously, so that the compounding agent is uniformly dispersed in the rubber material and reaches a certain dispersion degree. Because the shearing action of the rubber material is much larger than that of an open mill during the mixing of the internal mixer, the rubber mixing temperature is high, and the rubber mixing efficiency of the internal mixer is greatly higher than that of the open mill. Specifically, in this example, cyclopentane and the first mixture were added to the feed port of an internal mixer, and the internal mixer was processed as described above to obtain the second mixture.
Forming the second mixed material into a flake, and placing the flake in a granulator for granulation to obtain a granular substance.
The second mixed material can be made into slices by a hydraulic press, or by rolling with a rolling column, or by other equipment or methods which can roll objects into slices; the granulator is a forming machine which can manufacture materials into specific shapes. The special screw design and different configurations are adopted, and the reduction gearbox adopts the high-torque design, so that the performances of noiseless operation stability and the like are realized. The screw and the charging barrel are subjected to special hardening treatment, so that the screw and the charging barrel have the characteristics of wear resistance, good mixing performance and high yield, and the design of a vacuum exhaust or a common exhaust port can discharge moisture and waste gas in the production process, so that the discharging is more stable, the colloidal particles are firmer, and the excellent quality of the product is ensured. The physical properties of the plastic are changed by adopting the processes of high-temperature melting, plasticizing and extruding, so as to achieve the plasticizing and molding of the plastic.
Foaming the granular substance to obtain high-elasticity nylon; wherein the foaming temperature is 160-180 ℃, the foaming time is 5-7min, and the foaming pressure is 140-160kg/cm2。
The apparatus used for the foaming is a molding machine or a steam cylinder, and the basic steps of the foaming molding are the formation of cell nuclei, the growth or enlargement of cell nuclei, and the stabilization of cell nuclei. At a given temperature and pressure, the solubility of the gas decreases so that saturation is reached, allowing excess gas to escape and form bubbles, thereby effecting nucleation. Specifically, in the present application, the foaming temperature is 160-2。
Further, the thickness of the sheet is 10 mm.
Further, the predetermined apparatus is an extruder.
Further, the extruder is a double-screw extruder or a single-screw extruder.
The screw extruder depends on the pressure and shearing force generated by the rotation of the screw, so that the materials can be fully plasticized and uniformly mixed and are molded through a die. Specifically, nylon, polyborosiloxane and polyethylene glycol in a predetermined ratio are placed at a feeding port of an extruder, and a uniform mixed material with the three materials is processed by the extruder, namely a first mixed material.
In a second aspect, the embodiment of the invention provides a high-elasticity nylon prepared by the preparation method of the high-elasticity nylon.
The embodiment of the invention provides a preparation method of high-elasticity nylon, which comprises the following steps: obtaining nylon, polyborosiloxane and polyethylene glycol, and drying the polyborosiloxane; putting nylon, polyborosiloxane and polyethylene glycol into preset equipment, heating and uniformly mixing to obtain a first mixed material; obtaining cyclopentane, and placing the cyclopentane and the mixed material in an internal mixer for heating and internal mixing to obtain a second mixed material; preparing the second mixed material into slices, and placing the slices into a granulator for granulation to obtain granular substances; foaming the granular substance to obtain the high-elasticity nylon. Compared with the existing nylon elastomer, the high-elasticity nylon prepared by the method provided by the embodiment of the invention greatly improves the permanent compression deformation rate.
Example 2
On the basis of the above embodiment 1, the present invention will be further described with specific examples.
Step 1, drying nylon and Polyborosiloxane (PBDMS) according to the weight ratio of 10: 1, adding the mixture into an extruder, adding 10% of polyethylene glycol-400 by mass into the extruder, opening a heating module of the extruder to heat the mixture at 150 ℃ for 5min, and uniformly mixing the materials;
step 2, mixing the material obtained in the step 1 and a foaming agent cyclopentane according to the ratio of 100: 5, putting the mixture into an internal mixer for heating and internal mixing at the heating temperature of 150 ℃ for 10 min;
step 3, beating the material obtained in the step 2 into a 10mm slice;
step 4, feeding the membrane obtained in the step 3 into a granulator for granulation;
and 5, foaming the material obtained in the step 4 at the foaming temperature of 160 ℃, for 5min and under the pressure of 160kg/cm2 to obtain the high-elasticity nylon.
Example 3
Step 1, drying nylon and Polyborosiloxane (PBDMS) according to the weight ratio of 10: 1, adding the mixture into an extruder, adding 10% of polyethylene glycol-400 by mass into the extruder, opening a heating module of the extruder to heat the mixture at 180 ℃ for 3min, and uniformly mixing the materials;
step 2, mixing the material obtained in the step 1 and a foaming agent cyclopentane according to the ratio of 100: 10, putting the mixture into an internal mixer for heating and internal mixing, wherein the heating temperature is 180 ℃, and the internal mixing time is 7 min;
step 3, beating the material obtained in the step 2 into a 10mm slice;
step 4, feeding the membrane obtained in the step 3 into a granulator for granulation;
and 5, foaming the material obtained in the step 4 at the foaming temperature of 180 ℃ for 7min under the pressure of 140kg/cm2 to obtain the high-elasticity nylon.
Example 4
Step 1, drying nylon and Polyborosiloxane (PBDMS) according to the weight ratio of 10: 1, adding the mixture into an extruder, adding 10% of polyethylene glycol-400 by mass into the extruder, opening a heating module of the extruder to heat the mixture at 150 ℃ for 5min, and uniformly mixing the materials;
step 2, mixing the material obtained in the step 1 and a foaming agent cyclopentane according to the ratio of 100: 5, putting the mixture into an internal mixer for heating and internal mixing at 180 ℃ for 7 min;
step 3, beating the material obtained in the step 2 into a 10mm slice;
step 4, feeding the membrane obtained in the step 3 into a granulator for granulation;
and 5, foaming the material obtained in the step 4 at the foaming temperature of 170 ℃, for 7min and under the pressure of 140kg/cm2 to obtain the high-elasticity nylon.
Example 5
Step 1, drying nylon and Polyborosiloxane (PBDMS) according to the weight ratio of 10: 1, adding the mixture into an extruder, adding 10% of polyethylene glycol-400 by mass into the extruder, opening a heating module of the extruder to heat the mixture at 180 ℃ for 3min, and uniformly mixing the materials;
step 2, mixing the material obtained in the step 1 and a foaming agent cyclopentane according to the ratio of 100: 10, putting the mixture into an internal mixer for heating and internal mixing, wherein the heating temperature is 170 ℃, and the internal mixing time is 8 min;
step 3, beating the material obtained in the step 2 into a sheet with the thickness of 10 mm;
step 4, feeding the membrane obtained in the step 3 into a granulator for granulation;
and 5, foaming the material obtained in the step 4 at the foaming temperature of 180 ℃ for 6min under the pressure of 140kg/cm2 to obtain the high-elasticity nylon.
Example 6
Step 1, drying nylon and Polyborosiloxane (PBDMS) according to the weight ratio of 10: 1, adding the mixture into an extruder, adding 10% of polyethylene glycol-400 by mass into the extruder, opening a heating module of the extruder to heat the mixture at 150 ℃ for 5min, and uniformly mixing the materials;
step 2, mixing the material obtained in the step 1 and a foaming agent cyclopentane according to the ratio of 100: 5, putting the mixture into an internal mixer for heating and internal mixing at 180 ℃ for 7 min;
step 3, beating the material obtained in the step 2 into a 10mm slice;
step 4, feeding the membrane obtained in the step 3 into a granulator for granulation;
and 5, foaming the material obtained in the step 4 at the foaming temperature of 170 ℃, for 6min and under the pressure of 150kg/cm2 to obtain the high-elasticity nylon.
Example 7
Step 1, drying nylon and Polyborosiloxane (PBDMS) according to the weight ratio of 10: 1, adding the mixture into an extruder, adding 10% of polyethylene glycol-400 by mass into the extruder, opening a heating module of the extruder to heat the mixture at 150 ℃ for 5min, and uniformly mixing the materials;
step 2, mixing the material obtained in the step 1 and a foaming agent cyclopentane according to the ratio of 100: 5, putting the mixture into an internal mixer for heating and internal mixing at 180 ℃ for 7 min;
step 3, beating the material obtained in the step 2 into a 10mm slice;
step 4, feeding the membrane obtained in the step 3 into a granulator for granulation;
and 5, foaming the material obtained in the step 4 at the foaming temperature of 180 ℃ for 5min under the pressure of 150kg/cm 2.
Test examples
The compression set test of the examples 2 and 3 and the comparative example is carried out, the test method is that the compression set is 10 percent in the environment with the temperature of 70 ℃, after the treatment for 24 hours, the compression set ratio CS is calculated, and the calculation method of CS is as follows:
CS＝(h0-h2)/(h0-h1)
in the formula, h 0: height of sample/mm before compression; h 1: height of compression set/mm; h 2: height/mm after sample recovery.
The preparation method of the comparative example is as follows:
step 1, mixing nylon, polyethylene glycol-400 and cyclopentane according to the weight ratio of 100: 10: 5, putting the mixture into an internal mixer for heating and internal mixing at the heating temperature of 150 ℃ for 10 min;
step 2, beating the material obtained in the step 1 into a 10mm slice;
step 3, feeding the film obtained in the step 2 into a granulator for granulation;
and 4, foaming the material obtained in the step 3, wherein the foaming temperature is 160 ℃, the foaming time is 5min, and the pressure is 160kg/cm 2.
The test results were as follows:
| example 2 | Example 3 | Comparative example | |
| Compression set CS | 66.7 | 60 | 80 |
From the test results, it can be found that the compression set CS of the comparative examples is increased by 16.7% and 25% respectively in example 2 and example 3, which indicates that the method of the present invention can significantly improve the permanent compression set of the nylon elastomer.
It is noted that, herein, 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. Also, 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 an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
All the embodiments in the present specification are described in a related manner, and the same and similar parts among the embodiments may be referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (5)
1. A preparation method of high-elasticity nylon is characterized by comprising the following steps:
obtaining nylon, polyborosiloxane and polyethylene glycol, and drying the polyborosiloxane; wherein the mass ratio of the nylon to the polyborosiloxane is 10-100: 1; the mass of the polyethylene glycol is 10% of that of the polyborosiloxane;
placing the nylon, the polyborosiloxane and the polyethylene glycol in a preset device, heating and uniformly mixing to obtain a first mixed material; wherein the heating temperature is 150 ℃ and 180 ℃, and the heating time is 3-5 min;
obtaining cyclopentane, and placing the cyclopentane and the mixed material in an internal mixer for heating and internal mixing to obtain a second mixed material; wherein the mass of the cyclopentane is 5-10% of the mass of the first mixed material, the banburying temperature is 150-180 ℃, and the banburying time is 7-10 min;
preparing the second mixed material into a slice, and placing the slice into a granulator for granulation to obtain granular substances;
foaming the granular substance to obtain high-elasticity nylon; wherein the foaming temperature is 160-180 ℃, the foaming time is 5-7min, and the foaming pressure is 140-160kg/cm2。
2. The method of claim 1, wherein the sheet has a thickness of 10 mm.
3. The method of producing highly elastic nylon according to claim 1, wherein the predetermined equipment is an extruder.
4. The method for preparing the high-elasticity nylon of claim 3, wherein the extruder is a twin-screw extruder or a single-screw extruder.
5. A highly elastic nylon produced by the process for producing a highly elastic nylon according to any one of claims 1 to 4.
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| PCT/CN2021/097722 WO2022001557A1 (en) | 2020-07-02 | 2021-06-01 | High elastic nylon and preparation method therefor |
| JP2022581719A JP7422252B2 (en) | 2020-07-02 | 2021-06-01 | High elasticity nylon and its manufacturing method |
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| CN110903627A (en) * | 2019-10-30 | 2020-03-24 | 晋江兴迅新材料科技有限公司 | Thermoplastic elastomer blend supercritical foaming material and preparation method thereof |
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| GB0130834D0 (en) | 2001-12-22 | 2002-02-06 | Design Blue Ltd | Energy absorbing material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110903627A (en) * | 2019-10-30 | 2020-03-24 | 晋江兴迅新材料科技有限公司 | Thermoplastic elastomer blend supercritical foaming material and preparation method thereof |
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| JP2023533933A (en) | 2023-08-07 |
| JP7422252B2 (en) | 2024-01-25 |
| WO2022001557A1 (en) | 2022-01-06 |
| CN111763418A (en) | 2020-10-13 |
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