CN112851998B - High-rate nylon 6 foam material and preparation method thereof - Google Patents
High-rate nylon 6 foam material and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/122—Hydrogen, oxygen, CO2, nitrogen or noble gases
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- 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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- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/12—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08J2427/18—Homopolymers or copolymers of tetrafluoroethylene
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Abstract
The invention discloses a high-rate nylon 6 foam material and a preparation method thereof. The preparation method comprises the following steps: adding the chain extender and the additive into nylon 6 for melt blending to obtain modified nylon 6 with high melt strength; melting the modified nylon 6 with high melt strength, introducing a foaming agent to form a homogeneous system, and then preparing the high-magnification nylon 6 foaming material by adopting a high-temperature soaking low-temperature isothermal pressure-relief method. The preparation method is simple and convenient to operate and easy to manufacture, the foam material prepared from the modified nylon 6 obtained by simple melt blending not only reduces the foaming cost of the nylon 6, but also is easy to adjust the foaming performance of the nylon 6, and the foam material with excellent cell size is obtained by adjusting the process conditions. And the aim of regulating and controlling the foaming performance is achieved by adding the additive to regulate and control the crystallization behavior of the nylon 6.
Description
Technical Field
The invention relates to the technical field of engineering plastics, in particular to a high-rate nylon 6 foam material and a preparation method thereof.
Background
Nylon 6 is used as an engineering plastic and applied to various fields. It has the advantages of high use temperature, high rigidity, self-lubricating property, chemical corrosion resistance and the like. With the development of society, light weight of materials is concerned in all regions of the world, and foamed materials play an important role, and have many advantages such as sound insulation, heat insulation, light weight and the like. The high-rate nylon 6 foam makes a certain contribution to light weight.
The prior methods for preparing the foam material include an extrusion foaming method, a batch kettle foaming method and the like. Although the batch still foaming method cannot realize continuous production compared with the extrusion foaming method, the batch still foaming method has the advantages of being convenient for adjusting the process and being capable of producing products with complex shapes. It is also very important to select a green and efficient foaming agent at the same time, supercritical CO 2 The physical foaming agent has the outstanding advantages of high safety, environmental protection, low cost and the like, and accords with the development theme of green and recyclable society of the modern times. Microcellular foams are defined as having cell sizes of about 10 microns and cell densities>10 9 The micro-porous foam has excellent mechanical property, strong heat insulation and sound insulation performance and high multiplying power and can provide excellent heat insulation and sound insulation performanceThe comprehensive performance and the material consumption are reduced to achieve the purpose of reducing the cost.
However, the preparation of the high-magnification nylon 6 microcellular foaming material has great technical difficulty. Firstly, nylon 6 is easy to absorb water and degrade, and needs to be fully dried to remove water before processing; secondly, the nylon 6 is a linear molecular chain, and the foaming performance of the unmodified nylon 6 is limited due to low melt strength; thirdly, nylon 6 is a semi-crystalline polymer and has a high crystallization speed and a narrow foaming window, and the foaming behavior of the nylon is not easily regulated by crystallization. These technical difficulties make the preparation of nylon 6 high-rate microcellular foam difficult to some extent, and the preparation of nylon 6 high-rate microcellular foam material requires higher melt strength and more bubble nucleation points. Chinese patents CN 108546405A and CN 110256840A both successfully prepare nylon foam materials, but the prepared samples do not have the characteristics of small pores and high multiplying power. Multiple bubble nucleation sites can create more cells to provide cell density, and high melt strength can control the growth and solidification of bubbles to keep the cells small in size.
Nylon 6 foaming is very dependent on nylon 6 with high melt strength, but if the melt strength of nylon 6 is enhanced and more bubble nucleation points are added, a key problem to be solved in the process of preparing high-rate foam is needed.
Disclosure of Invention
In order to solve the above technical problems, the present invention aims to provide a high-ratio nylon 6 foam material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of a high-rate nylon 6 foaming material, which comprises the following steps:
adding a chain extender and an additive into nylon 6 for melt blending, wherein the additive is dispersed in a nylon 6 matrix while a chain extension reaction is carried out in the process so as to prepare modified nylon 6 with high melt strength;
and melting the modified nylon 6 with high melt strength, introducing a foaming agent to form a homogeneous system, and then preparing the high-magnification nylon 6 foaming material by adopting a high-temperature soaking low-temperature isothermal pressure-relief method.
According to the preparation method of the invention, preferably, the mass ratio of the chain extender to the nylon 6 is (10-15): 100. the chain extender has the function of enabling a linear molecular chain to become a branched molecular chain to improve the melt strength, but a cross-linked structure can be formed when the addition amount of the chain extender is too much, the cross-linked structure can increase the processing difficulty and influence the product waste recovery; too little addition of chain extender affects the degree of branching, thus making the foaming effect poor. More preferably, the mass ratio of the chain extender to the nylon 6 is 15:100.
according to the preparation method of the invention, the mass ratio of the additive to the nylon 6 is preferably (0.3-1.5): 100.
According to the preparation method of the present invention, preferably, the chain extender is at least one selected from the group consisting of an epoxy chain extender, an isocyanate chain extender and an acid anhydride chain extender.
According to the preparation method of the present invention, preferably, the additive is a nano additive selected from at least one of talc, montmorillonite, kaolin, silica, calcium carbonate, halloysite, nanocellulose and Polytetrafluoroethylene (PTFE).
The invention achieves the purpose of regulating and controlling the foaming performance by adding the additive to regulate and control the crystallization behavior of the nylon 6. The additive not only can be used as a bubble nucleation point to reduce the size of bubbles and increase the density of the bubbles, but also can enhance the strength of a melt and widen a nylon 6 foaming window.
According to the preparation method of the invention, preferably, the foaming agent is selected from butane, dimethyl ether and CO 2 And N 2 At least one of (a).
According to the preparation method of the present invention, preferably, the chain extender is an epoxy-based chain extender; the additive is polytetrafluoroethylene; the foaming agent is CO 2 。
According to the preparation method of the invention, preferably, the mass ratio of the epoxy chain extender to the nylon 6 is (10-15): 100; the mass ratio of the polytetrafluoroethylene to the nylon 6 is (0.3-1.5): 100.
According to the preparation method of the present invention, preferably, the mass ratio of the epoxy chain extender to the nylon 6 is 15:100, respectively; the mass ratio of the polytetrafluoroethylene to the nylon 6 is 0.9.
According to the preparation method of the invention, preferably, the high-temperature soaking low-temperature isothermal pressure-relief method comprises the following steps:
and (2) maintaining the modified nylon 6 with high melt strength at the saturation temperature of 230-235 ℃ and the saturation pressure of 15-20MPa, soaking in the foaming agent for 1-1.5h, then cooling to 210-225 ℃, maintaining for 10-30min, and then rapidly releasing pressure to normal temperature and normal pressure to obtain the high-magnification nylon 6 foaming material.
More preferably, the high-temperature soaking low-temperature isothermal pressure-relief method comprises the following steps:
and (2) maintaining the modified nylon 6 with high melt strength at a saturation temperature of 230 ℃ and a saturation pressure of 20MPa, soaking in the foaming agent for 1h, then cooling to 210-225 ℃, maintaining for 20min, and then rapidly releasing pressure to normal temperature and normal pressure to obtain the high-magnification nylon 6 foaming material.
According to the preparation method of the present invention, preferably, after obtaining the modified high melt strength nylon 6, the method further comprises the steps of using a hot plate press to prepare a sample to be foamed at a molding temperature for the modified high melt strength nylon 6; the sample to be foamed is then melted and a blowing agent is introduced.
According to the production method of the present invention, preferably, the molding temperature is 240 ℃.
According to the production method of the present invention, preferably, the temperature of the melt blending is 240 ℃.
The invention also provides a high-ratio nylon 6 foaming material prepared by the preparation method, wherein the foaming ratio is 9-18.
The beneficial effects of the invention include:
1) The preparation method of the high-magnification nylon 6 foam material is simple and convenient to operate and easy to manufacture, the foam material prepared from the modified nylon 6 obtained by simple melting and blending not only reduces the foaming cost of the nylon 6, but also is easy to adjust the foaming performance of the nylon 6, the aim of enhancing the melt strength and increasing the bubble nucleation points is achieved by adding the additive, the aim of adjusting the melt strength is achieved by adjusting different low-temperature foaming temperatures, the quantity of the bubble nucleation points and the regulation and control of the melt strength are achieved by changing the addition amount of the additive, and the optimal process conditions are obtained by combining the above steps, so that the nylon 6 foam material with high foaming magnification, large cell density and small cell size is obtained.
2) The additive provided by the invention not only can be used as a bubble nucleating point to reduce the size of a bubble and increase the density of the bubble, but also can enhance the strength of a melt and widen a nylon 6 foaming window.
3) The invention achieves the purpose of regulating and controlling the foaming performance by adding the additive to regulate and control the crystallization behavior of the nylon 6.
Drawings
Fig. 1 is a polarization microscope image of the nylon 6 blend of example 1 and comparative example 1.
Figure 2 is a plot of the complex viscosity of the nylon 6 blends of example 1, other examples, and comparative example 1.
Fig. 3 is a graph of the storage modulus of nylon 6 blends of example 1, other examples, and comparative example 1.
FIG. 4 is a graph of loss tangent values for nylon 6 blends of example 1, other examples, and comparative example 1.
Fig. 5 is a scanning electron micrograph of the foamed samples of example 1, other examples, and comparative example 1.
Detailed Description
In order to more clearly illustrate the present invention, the present invention is further described below in conjunction with preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and is not to be taken as limiting the scope of the invention.
All numerical designations herein (e.g., temperature, time, concentration, and weight, etc., including ranges for each) may generally be approximated as varied (+) or (-) in increments of 0.1 or 1.0, as appropriate. All numerical designations should be understood as preceded by the term "about".
The following parameter determination process in the embodiment of the invention comprises the following steps:
cell size: SEM cell morphology photographs were analyzed by graphic analysis software (Image-Pro Plus 6.0) and statistical calculations were performed.
Density: the test was carried out according to ASTM D792-2000 (i.e., drainage method), and at least 6 samples were selected under the same conditions and then averaged.
Foaming ratio: the ratio of the average density of the unfoamed sample to the density of the foamed article.
Example 1
The present embodiment prepares a high-rate nylon 6 foam material, and raw materials thereof include the following components by mass:
50g of nylon 6 resin;
7.5g of epoxy chain extender;
0.15g of polytetrafluoroethylene additive;
the preparation process comprises the following steps:
s1, drying the components, putting the components into a torque rheometer for melt blending, wherein the melt temperature is 240 ℃, the rotation speed is 100rads/min, and the nylon 6 blend with high melt strength is formed after blending for 10 min.
S2, cooling the blend obtained in the step S1, and performing die pressing for 10min at a die pressing temperature of 240 ℃ by using a hot plate pressing machine to obtain a sample to be foamed of 10mm multiplied by 1 mm.
S3, placing the sample to be foamed into a high-pressure kettle, soaking at high temperature and injecting 20MPa of CO by using a low-temperature isothermal pressure relief method 2 Keeping the stable soaking temperature in the kettle at 230 ℃ for 1h to completely melt the crystals in the nylon 6, then reducing the temperature in the kettle to 210 ℃ for 20min, and finally quickly relieving the pressure to normal temperature and high pressure, and taking out the foamed product.
Other embodiments
The remaining examples were carried out as in example 1, but with differences in the quality composition and the process conditions, as shown in Table 1 below.
TABLE 1
Comparative example 1
The comparative example prepared a nylon 6 foam material whose raw materials included the following components by mass:
50g of nylon 6 resin;
7.5g of epoxy chain extender;
the preparation process comprises the following steps:
s1, drying the components, putting the components into a torque rheometer for melt blending, wherein the melt temperature is 240 ℃, the rotating speed is 100rads/min, and the blend is blended for 10min to form a nylon 6 blend with high melt strength;
s2, cooling the blend obtained in the step S1, and performing mould pressing for 10min at a mould pressing temperature of 240 ℃ by using a hot plate pressing machine to prepare a sample to be foamed, wherein the sample is 10mm multiplied by 1 mm;
s3, placing the sample to be foamed into a high-pressure kettle, soaking at high temperature and injecting 20MPa of CO by using a low-temperature isothermal pressure relief method 2 Keeping the stable soaking temperature in the kettle at 230 ℃ for 1h to completely melt the crystals in the nylon 6, then reducing the temperature in the kettle to 210 ℃ for 20min, and finally quickly relieving the pressure to normal temperature and high pressure, and taking out the foamed product.
For the following description and analysis to be clearer and quicker, the examples and comparative examples are named in short in the following table 2.
TABLE 2
FIG. 1 is a polarization microscope image of the nylon 6 blend of example 1 and comparative example 1, wherein (a) in FIG. 1 is a crystal morphology image of comparative example 1, from which the crystal dispersion formation in comparative example 1 can be seen, and (b) - (c) in FIG. 1 are POM morphology images of example 1 in a molten state, at the beginning of crystallization for 2 seconds and at the beginning of crystallization for 20 seconds, and since it can be seen that the effect of polytetrafluoroethylene as a heterogeneous nucleating agent is very obvious, the nylon 6 can be clearly seen to crystallize along the polytetrafluoroethylene fiber.
FIG. 2 is a plot of the complex viscosity of the nylon 6 blends of example 1, other examples, and comparative example 1, the presence of polytetrafluoroethylene enhancing the complex viscosity of nylon 6, and the melt strength of the nylon 6 blends with polytetrafluoroethylene added is further improved compared to CEPA 6. The melting point of polytetrafluoroethylene is about 325 ℃, so that nylon 6 melts at a temperature of 240 ℃ and polytetrafluoroethylene remains in the melt of PA 6. The complex viscosity of nylon 6 blends begins to decrease at relatively high polytetrafluoroethylene loadings and when the amount of polytetrafluoroethylene exceeds 0.45g, the polytetrafluoroethylene particles coalesce together. The melt of the nylon 6 blend shows non-Newtonian plateau and shear thinning at low frequency, and the investigation of complex viscosity can prove that the melt strength of nylon 6 is obviously improved by the polytetrafluoroethylene and the addition amount of the polytetrafluoroethylene has an optimal value.
The storage modulus curves for the CEPA6 and nylon 6 blend samples are shown in FIG. 3. The storage modulus still shows the trend of decreasing with the increase of the addition amount of the polytetrafluoroethylene, the increase of the storage modulus also indicates that the addition of the polytetrafluoroethylene increases the melt strength of the nylon 6, and the addition amount of the polytetrafluoroethylene has an optimal value.
FIG. 4 is a graph of loss tangent values for the nylon 6 blends of example 1, other examples, and comparative example 1, which can be used to better understand the relaxation change, with a decrease in loss tangent value for the nylon 6 blend demonstrating an improvement in viscoelasticity which is indicative of a further increase in the foaming properties of the nylon 6 blend.
Figure 5 shows SEM photographs of CEPA6 and nylon 6 blend foam samples at different foaming temperatures and different polytetrafluoroethylene addition conditions. The addition of polytetrafluoroethylene reduced the cell size of PA6 at the same foaming temperature. When the foaming temperature is 225 ℃, collapse of cells occurs due to a decrease in melt strength caused by a high foaming temperature. The cell morphology improved significantly upon addition of the polytetrafluoroethylene, a phenomenon that confirms the effect of the polytetrafluoroethylene additive on improving cell morphology and enhancing melt strength.
The foam properties of the foamed samples of example 1, other examples and comparative example 1 are shown in table 3.
TABLE 3 foam Properties in examples and comparative examples
As can be seen from table 3, the addition of ptfe significantly reduces the cell size and significantly increases the cell density without significantly affecting the expansion ratio. In experiments, a preferable interval and an optimal formula exist between the cooling foaming temperature and the addition amount of the polytetrafluoroethylene. Wherein the addition of the polytetrafluoroethylene is 0.15-0.75g as a preferred interval, the cooling foaming temperature is 210-225 ℃ as a preferred interval, the optimum formula is that the addition of the polytetrafluoroethylene is 0.45g, and the cooling foaming temperature is 215 ℃ and 220 ℃.
It should be understood that the above-mentioned embodiments of the present invention are only examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention, and it will be obvious to those skilled in the art that other variations or modifications may be made on the basis of the above description, and all embodiments may not be exhaustive, and all obvious variations or modifications may be included within the scope of the present invention.
Claims (3)
1. A preparation method of a high-magnification nylon 6 foaming material is characterized by comprising the following steps:
adding a chain extender and an additive into nylon 6, and carrying out melt blending at 240 ℃ to obtain modified nylon 6 with high melt strength;
preparing the modified nylon 6 with high melt strength into a sample to be foamed at the mould pressing temperature of 240 ℃ by using a hot plate press; melting the sample to be foamed, introducing a foaming agent to form a homogeneous system, and then preparing the high-rate nylon 6 foaming material by adopting a high-temperature soaking low-temperature isothermal pressure-release method, wherein the foaming rate is 15.9, the cell size is 14.5 mu m, and the cell density is 39x 10 8 Per cm 3 ；
The chain extender is an epoxy chain extender; the additive is polytetrafluoroethylene; the hairFoaming agent CO 2 ；
The mass ratio of the epoxy chain extender to the nylon 6 is 15:100, respectively; the mass ratio of the polytetrafluoroethylene to the nylon 6 is 0.9.
2. The method according to claim 1, wherein the high-temperature soaking low-temperature isothermal pressure-relief method comprises:
and (2) maintaining the modified nylon 6 with high melt strength at a saturation temperature of 230 ℃ and a saturation pressure of 20MPa, soaking in the foaming agent for 1h, then cooling to 215 ℃ for 20min, and then relieving pressure to normal temperature and normal pressure to obtain the high-magnification nylon 6 foaming material.
3. A high-rate nylon 6 foam obtained by the preparation method of claim 1 or 2.
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| CN115124834B (en) * | 2022-07-13 | 2023-03-17 | 北京化工大学 | Thermoplastic polyamide elastomer blending foaming material and preparation method thereof |
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