CN114351282B - Preparation method of heat-insulating smoke-suppressing polyphenylene sulfide composite material - Google Patents
Preparation method of heat-insulating smoke-suppressing polyphenylene sulfide composite material Download PDFInfo
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- 239000004734 Polyphenylene sulfide Substances 0.000 title claims abstract description 103
- 229920000069 polyphenylene sulfide Polymers 0.000 title claims abstract description 103
- 239000002131 composite material Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000835 fiber Substances 0.000 claims abstract description 42
- 238000002156 mixing Methods 0.000 claims abstract description 31
- 239000008187 granular material Substances 0.000 claims abstract description 25
- 150000002736 metal compounds Chemical class 0.000 claims abstract description 21
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 11
- 238000002074 melt spinning Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000001125 extrusion Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002425 crystallisation Methods 0.000 claims abstract description 5
- 230000008025 crystallization Effects 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 12
- 238000002036 drum drying Methods 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 4
- 230000003179 granulation Effects 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 claims description 2
- 239000000779 smoke Substances 0.000 abstract description 26
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 238000001746 injection moulding Methods 0.000 abstract description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 38
- 238000002485 combustion reaction Methods 0.000 description 23
- 239000000463 material Substances 0.000 description 12
- 239000000203 mixture Substances 0.000 description 11
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 238000004132 cross linking Methods 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
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- 239000003063 flame retardant Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
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- 239000011148 porous material Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910020599 Co 3 O 4 Inorganic materials 0.000 description 1
- 229910010707 LiFePO 4 Inorganic materials 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
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- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
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- 230000035515 penetration Effects 0.000 description 1
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Abstract
A preparation method of a heat-insulating smoke-suppressing polyphenylene sulfide composite material comprises the following steps: mixing PPS, a metal compound and a silane coupling agent, stirring, and granulating at 200-350 ℃ to obtain PPS composite master batch; extruding and granulating PPS at 200-350 ℃ to obtain pure PPS granules; mixing the PPS composite master batch with pure PPS granules, transferring to drying equipment for pre-crystallization and drying to obtain blending granules with the water content of less than 50 ppm; and (3) melt blending the blending granules at 200-350 ℃ and preparing the heat-insulating smoke-suppressing polyphenylene sulfide composite material through extrusion injection molding or melt spinning. The heat-insulating smoke-suppressing polyphenylene sulfide composite material provided by the invention has good heat-insulating smoke-suppressing performance, remarkably reduces heat release and smoke release, and has good spinnability and stable fiber formation.
Description
Technical Field
The invention relates to the technical field of composite material preparation, in particular to a preparation method of a heat-insulating smoke-suppressing polyphenylene sulfide composite material.
Background
Polyphenylene Sulfide (PPS) integrates the advantages of high mechanical strength, temperature resistance, flame retardance, chemical resistance and the like, and is widely applied as a high-performance material in various fields such as national defense and military industry, safety fire protection, human body safety protection, automobile interior trim and the like. The material can form a carbon layer structure through oxidative crosslinking in the combustion process, so that certain flame retardant performance is shown, the material has potential possibility of being developed into a heat protection material, but the combustion behavior of the material cannot meet the heat protection requirement. This is mainly because the polyphenylene sulfide combustion process is continuously affected by the excited oxygen and the pyrolyzed free matters, so that the formed carbon layer structure is loose, and the heat release and smoke release are high.
How to inhibit the combustion reaction, reduce the smoke release and the heat release is of great significance to the improvement of the performance of the polyphenylene sulfide product, and therefore, the improvement of the formulation and the preparation process of the prior polyphenylene sulfide product is necessary.
Disclosure of Invention
Based on the method, the invention provides a preparation method of a heat-insulating smoke-suppressing polyphenylene sulfide composite material, and aims to solve the technical problems that in the prior art, polyphenylene sulfide is continuously influenced by excited oxygen and pyrolysis free matters in the combustion process, so that a formed carbon layer structure is loose, and heat release and smoke release are high.
In order to achieve the above purpose, the invention provides a preparation method of a heat-insulating smoke-suppressing polyphenylene sulfide composite material, which comprises the following steps:
s1, taking PPS, a metal compound and a silane coupling agent, stirring and mixing according to the content of the metal compound of 1-5wt%, and blending and granulating at 200-350 ℃ to obtain PPS composite master batch;
s2, extruding and granulating PPS at 200-350 ℃ to obtain pure PPS master batches;
s3, mixing the PPS composite master batch and the pure PPS master batch according to the content of the metal compound accounting for 0.3-3.0wt% of the total amount after mixing;
s4, transferring the granules mixed in the step S3 into drying equipment for pre-crystallization and drying to obtain blended granules with the water content of less than 50 ppm;
s5, melt blending the blending granules at 200-350 ℃, and preparing the heat-insulating smoke-suppressing polyphenylene sulfide composite material with the metal compound content of 0.3-3.0wt% through extrusion injection molding or melt spinning.
As a further preferable technical scheme of the invention, in the step S1, the weight ratio of the silane coupling agent is 10-30wt% of the mass of the metal compound.
As a further preferable technical scheme of the invention, the weight of the silane coupling agent is 25wt% of the mass of the metal compound.
As a further preferable embodiment of the present invention, in step S1, the metal compound includes Fe 2 O 3 、Fe 3 O 4 、Co 3 O 4 、NiO、LiFePO 4 One or more of the following.
As a further preferable technical scheme of the invention, in the step S1, PPS, a metal compound and a silane coupling agent are taken and stirred and mixed according to the content of the metal compound of 2-3 wt%.
As a further preferable technical scheme of the invention, the blending granulation, extrusion granulation and melt blending all adopt double screw extrusion equipment.
As a further preferable embodiment of the present invention, the drying apparatus is a vacuum drum drying apparatus.
As a further preferable technical scheme of the invention, the technological conditions of the vacuum drum drying equipment for pre-crystallization and drying are as follows: respectively preserving heat at 95 ℃, 130 ℃ and 160 ℃ for 15 hours, 15 hours and 4 hours.
As a further preferable technical scheme of the invention, the heat-insulating smoke-suppressing polyphenylene sulfide composite material obtained in the step (5) is a composite fiber by adopting a melt spinning process.
The preparation method of the heat-insulating smoke-suppressing polyphenylene sulfide composite material can achieve the following beneficial effects by adopting the technical scheme:
(1) The method is simple, environment-friendly, strong in operability, high in yield and suitable for commercial production;
(2) In the melt spinning process, the heat-insulating smoke-suppressing polyphenylene sulfide composite material shows good spinnability, and the fiber is stable in fiber formation and good in performance;
(3) According to the method, through accurate proportion regulation and control, the metal compound is introduced to be compounded with the PPS, so that the combustion and carbonization performances of the PPS are obviously influenced, and compared with a pure PPS material, the combustion performance of the PPS material is improved as follows: peak heat release rate in combustion is from 100.41Kw/m 2 Reduced to 47.32Kw/m 2 Total heat release from 28.42MJ/m 2 Reduced to 15.73MJ/m 2 Peak smoke rate of 0.028m 3 Per second, total smoke yield of 2.61m 3 Reduced to 1.97m 3 。
Drawings
The invention will be described in further detail with reference to the drawings and the detailed description.
FIG. 1 is a SEM scan of the carbon burn-through of pure PPS fibers with the composite fibers of the various embodiments;
FIG. 2 is a graph of the heat release rate of pure PPS fiber (left) versus the composite fiber (right) of example 2;
FIG. 3 is a graph showing the total heat release profile of pure PPS fiber (left) and the composite fiber (right) of example 2;
FIG. 4 is a plot of smoke generation rate for pure PPS fiber (left) versus composite fiber (right) of example 2;
FIG. 5 is a plot of total smoke yield for pure PPS fiber (left) versus composite fiber (right) of example 2;
fig. 6 is a SEM scan of the burning char from the pure PPS fiber (left) and the composite fiber of example 2 (right).
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Description of the embodiments
The invention will be further described with reference to the drawings and detailed description. The terms such as "upper", "lower", "left", "right", "middle" and "a" in the preferred embodiments are merely descriptive, but are not intended to limit the scope of the invention, as the relative relationship changes or modifications may be otherwise deemed to be within the scope of the invention without substantial modification to the technical context.
Fe 2 O 3 As a metal oxide, the catalyst exhibits good performance in the fields of catalyzing the combustion of polymers to form carbon, inhibiting combustion reaction, reducing smoke release and heat release. And Fe (Fe) 2 O 3 Is a raw material with wide sources and mature process, and can achieve the high-efficiency effect under low load. According to the invention, the iron oxide is introduced into the polyphenylene sulfide matrix through a melt blending process, so that the performance of burning the polyphenylene sulfide into charcoal is obviously affected.
The present invention will be described in further detail by specific embodiments.
Example 1
(1) Taking PPS powder and Fe 2 O 3 And fully stirring and mixing the silane coupling agent, wherein the weight ratio of the silane coupling agent is Fe 2 O 3 25wt% of mass, fe 2 O 3 The weight ratio of the mixture is 3wt% of the whole mixture, and the mixture is blended and granulated at 295 ℃ by a double-screw extruder to obtain PPS/Fe 2 O 3 Compounding master batches;
(2) Granulating PPS powder at 295 ℃ by a double-screw extruder to prepare pure PPS granules;
(3) PPS/Fe 2 O 3 Composite master batch and pure PPS granules are prepared according to Fe 2 O 3 Mixing at a content of 0.3 wt%;
(4) Transferring the mixed granules into vacuum drum drying equipment, respectively preserving heat at 95 ℃, 130 ℃ and 160 ℃ for 15 hours, 15 hours and 4 hours, pre-crystallizing and drying to obtain blended granules with the water content of less than 50 ppm;
(5) Melt blending at 295 ℃ by a twin screw extruder, and then preparing the blended granules into composite fibers at 320 ℃ by adopting a melt spinning technology, wherein Fe 2 O 3 The content of (C) was 0.3wt%.
Example 2
(1) Taking PPS powder and Fe 2 O 3 And fully stirring and mixing the silane coupling agent, wherein the weight ratio of the silane coupling agent is Fe 2 O 3 25wt% of mass, fe 2 O 3 The weight ratio of the mixture is 3wt% of the whole mixture, and the mixture is blended and granulated at 295 ℃ by a double-screw extruder to obtain PPS/Fe 2 O 3 Compounding master batches;
(2) Granulating PPS powder at 295 ℃ by a double-screw extruder to prepare pure PPS granules;
(3) PPS/Fe 2 O 3 Composite master batch and pure PPS granules are prepared according to Fe 2 O 3 Mixing at a content of 1.0 wt%;
(4) Transferring the mixed granules into vacuum drum drying equipment, respectively preserving heat at 95 ℃, 130 ℃ and 160 ℃ for 15 hours, 15 hours and 4 hours, pre-crystallizing and drying to obtain blended granules with the water content of less than 50 ppm;
(5) Melt blending at 295 ℃ by a twin screw extruder, and then preparing the blended granules into composite fibers at 320 ℃ by adopting a melt spinning technology, wherein Fe 2 O 3 The content of (C) was 1.0wt%.
Example 3
(1) Taking PPS powder and Fe 2 O 3 And fully stirring and mixing the silane coupling agent, wherein the weight ratio of the silane coupling agent is Fe 2 O 3 10-30wt% of Fe 2 O 3 The weight ratio of the mixture is 3wt% of the whole mixture, and the mixture is blended and granulated at 295 ℃ by a double-screw extruder to obtain PPS/Fe 2 O 3 Compounding master batches;
(2) Granulating PPS powder at 295 ℃ by a double-screw extruder to prepare pure PPS granules;
(3) PPS/Fe 2 O 3 Composite master batch and pure PPS granules are prepared according to Fe 2 O 3 Mixing at a content of 1.5 wt%;
(4) Transferring the mixed granules into vacuum drum drying equipment, respectively preserving heat at 95 ℃, 130 ℃ and 160 ℃ for 15 hours, 15 hours and 4 hours, pre-crystallizing and drying to obtain blended granules with the water content of less than 50 ppm;
(5) By passing throughMelt blending at 295 ℃ by a double screw extruder, and preparing the blended granules into composite fibers at 320 ℃ by adopting a melt spinning technology, wherein Fe 2 O 3 The content of (2) was 1.5% by weight.
For ease of illustration, fe in the composite fibers prepared according to examples 1-3 2 O 3 The content of (C) is different, and the composite fiber is expressed as PPS/Fe according to the components 2 O 3 -x, wherein x represents Fe 2 O 3 Is contained in the composition.
The composite fibers prepared in examples 1-3 were used as test groups, respectively, and commercially available pure PPS fibers (designated PPS) were used as control groups, and the heat release and smoke release parameters during combustion were summarized in table 1 by cone calorimetric characterization of the heat release and smoke release of the control group and the test group, respectively, and the obtained Heat Release Rate (HRR), total Heat Release (THR), smoke Production Rate (SPR), total Smoke Production (TSP).
TABLE 1 PPS and PPS/Fe 2 O 3 PHRR, THR, PSPR and TSP parameters of (C)
| Sample | PHRR(Kw/m 2 ) | THR（MJ/m 2 ） | PSPR（m 3 /s） | TSP（m 3 ） |
| PPS | 100.41 | 28.42 | 0.028 | 2.61 |
| PPS/Fe 2 O 3 -0.3 | 73.82 | 16.10 | 0.026 | 2.52 |
| PPS/Fe 2 O 3 -1.0 | 55.62 | 19.00 | 0.011 | 2.00 |
| PPS/Fe 2 O 3 -1.5 | 47.32 | 15.73 | 0.015 | 1.97 |
Note that: PPS/Fe 2 O 3 -x represents Fe 2 O 3 The content of (2) is x
Analysis of the above table shows that the peak heat release rate in combustion was 100.41Kw/m in the experimental group compared to the control group 2 Reduced to 47.32Kw/m 2 Total heat release from 28.42MJ/m 2 Reduced to 15.73MJ/m 2 Peak smoke rate of 0.028m 3 Per second, total smoke yield of 2.61m 3 Reduced to 1.97m 3 The metal compound and PPS are introduced to be compounded, so that the combustion char formation performance of PPS is obviously influenced, the heat release rate, the total heat release amount, the total smoke release rate and the total smoke release amount in combustion are obviously reduced, the combustion reaction inhibition effect is obvious, the flame retardant performance is strong, the combustion behavior is weak, and the flame retardant material can be widely applied to heat protection materials. At the same time, by the method for Fe 2 O 3 The content of the fiber is precisely regulated and controlled in proportion, and the regulation and control of the heat release rate, the total heat release amount, the smoke release rate and the total smoke release amount of the composite fiber can be achieved, so that different use requirements can be met.
The composite fibers prepared in examples 1-3 are respectively used as test groups, and pure PPS fibers (marked as PPS) on the market are additionally used as control groups, as shown in four groups of SEM images of FIG. 1, the pure PPS fibers, the composite fibers of example 1, the composite fibers of example 2 and the composite fibers of example 3 are sequentially arranged from left to right in the drawing, and all the composite fibers show good morphological characteristics under a high-power scanning electron microscope, so that the composite fiber has stable spinning process and good fiber formability, and can be used for manufacturing fabrics such as fire resistance and flame retardance.
To further investigate the properties of the composite fibers prepared according to the present invention, the following analyses were performed, respectively, with reference to fig. 2 to 6, in combination with pure PPS fibers of the control group, taking the preparation product of example 2 as an example.
FIG. 2 shows a HRR curve, which shows that the pure PPS fiber shows higher peak value with PHRR as high as 100.41Kw/m 2 And the continuous high-speed heat release is kept for a long time, so that flame diffusion and heat injury are easily caused in practical application. The HRR curve of the PPS material doped with the Fe2O3 metal nano material is obviously moved downwards, the PHRR value is effectively reduced, the high-speed heat release time is shortened, and better heat insulation performance is shown.
Fig. 3 is a THR curve, and analysis shows the total heat release during combustion of the reaction material. The total heat release of combustion of the pure PPS fiber is increased with time, and the final heat release value is as high as 28.42MJ/m 2 Indicating that the heat quantity is large in penetration and the generated heat damage is high. After the Fe2O3 is introduced, the total heat release is always lower than that of pure PPS fiber, and the final heat release value is greatly reduced.
FIG. 4 shows SPR curves, and analysis shows that the smoke release rate of the reaction material in the combustion process is low, the cyclized crosslinking efficiency of the pure PPS fiber is low due to the oxygen, a large amount of free radicals and low molecules are rapidly released from the matrix under the impact of heat in the combustion process, and the smoke generation rate is high, so that the pure PPS fiber is easy to produce harm in practical application. Fe (Fe) 2 O 3 The introduction of the polymer promotes the cyclization and crosslinking process, promotes the carbonization reaction, slows down the release of low molecules and free radicals, so that the SPR curve is obviously easy to lower, and the SPR peak value is obviously reduced.
FIG. 5 is a graph of TSP, analyzed to determine the total smoke production during combustion of the reactive material. As described above, PPS has low crosslinking carbonization efficiency under the action of hot oxygen to release a large amount of free radicals and low molecular fragments, so that a high smoke release amount is formed, and the total smoke yield is up to 2.61m 3 And at Fe 2 O 3 Under the promotion of the pressure, the overflow of low molecules and free radicals is effectively inhibited, so that the total smoke yield is also correspondingly and greatly reduced.
The appearance and the structure of the combustion carbon residue are correspondingly characterized after the combustion performance is characterized. FIG. 6 shows PPS and PPS/Fe 2 O 3 SEM image of burning carbon residue, the carbon residue structure of pure PPS shows larger pore structure, is loose, fe 2 O 3 The introduction of (2) makes the carbon residue structure develop to densification, just because of Fe 2 O 3 The pores in the carbon layer structure are reduced and the densification is grown, so that the heat transfer is inhibited, the substance precipitation is reduced, and the heat release and smoke release are reduced.
While particular embodiments of the present invention have been described above, it will be appreciated by those skilled in the art that these are merely illustrative, and that many variations or modifications may be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined only by the appended claims.
Claims (7)
1. The preparation method of the heat-insulating smoke-suppressing polyphenylene sulfide composite material is characterized by comprising the following steps of:
s1, taking PPS, a metal compound and a silane coupling agent, stirring and mixing according to the content of the metal compound of 1-5wt%, and blending and granulating at 200-350 ℃ to obtain PPS composite master batch, wherein the metal compound is Fe 2 O 3 A metal nanomaterial;
s2, extruding and granulating PPS at 200-350 ℃ to obtain pure PPS master batches;
s3, mixing the PPS composite master batch and the pure PPS master batch according to the content of the metal compound accounting for 0.3-3.0wt% of the total amount after mixing;
s4, transferring the granules mixed in the step S3 into drying equipment for pre-crystallization and drying to obtain blended granules with the water content of less than 50 ppm;
s5, melt blending the blending granules at 200-350 ℃, and preparing the heat-insulating smoke-suppressing polyphenylene sulfide composite material with the metal compound content of 0.3-3.0wt% by melt spinning, wherein the heat-insulating smoke-suppressing polyphenylene sulfide composite material is a composite fiber.
2. The preparation method of the heat-insulating smoke-suppressing polyphenylene sulfide composite material according to claim 1, wherein in the step S1, the weight ratio of the silane coupling agent is 10-30wt% of the mass of the metal compound.
3. The preparation method of the heat-insulating smoke-suppressing polyphenylene sulfide composite material according to claim 2, wherein the weight ratio of the silane coupling agent is 25wt% of the mass of the metal compound.
4. The method for preparing the heat-insulating smoke-suppressing polyphenylene sulfide composite material according to claim 1, wherein in the step S1, PPS, a metal compound and a silane coupling agent are mixed with stirring according to the content of the metal compound of 2-3 wt%.
5. The method for preparing the heat-insulating smoke-suppressing polyphenylene sulfide composite material according to claim 1, wherein the blending granulation, extrusion granulation and melt blending all adopt twin-screw extrusion equipment.
6. The method for preparing a heat-insulating smoke-suppressing polyphenylene sulfide composite material according to claim 1, wherein the drying equipment is a vacuum drum drying equipment.
7. The method for preparing the heat-insulating smoke-suppressing polyphenylene sulfide composite material according to claim 6, wherein the vacuum drum drying equipment performs the process conditions of pre-crystallization and drying: respectively preserving heat at 95 ℃, 130 ℃ and 160 ℃ for 15 hours, 15 hours and 4 hours.
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