CN101033306A - Process for preparing expanded product of thermoplastic resin - Google Patents
Process for preparing expanded product of thermoplastic resin Download PDFInfo
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- CN101033306A CN101033306A CN 200610056813 CN200610056813A CN101033306A CN 101033306 A CN101033306 A CN 101033306A CN 200610056813 CN200610056813 CN 200610056813 CN 200610056813 A CN200610056813 A CN 200610056813A CN 101033306 A CN101033306 A CN 101033306A
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Abstract
The invention discloses a method for preparing a kind of thermoplastic resin foam by using ultrasonic technology. The method includes following steps: 1) it put the thermoplastic resin samples into the autoclave, then it access to the high-pressure fluid for constant temperature and pressure. 2) it release the high-pressure fluid and take out the samples form the autoclave, then it puts the samples in the liquid medium of ultrasonic environment for foaming. After that it rapidly quenches the foam samples to form the cell structure of stereotypes to achieve the products. In the invention, the method improves the nuclear density of the thermoplastic resin foam and promotes the process of nucleation and gas nuclear growth.
Description
Technical field
The present invention relates to a kind of method for preparing expanded product of thermoplastic resin, particularly relate to a kind of method of utilizing ultrasonic wave to prepare expanded product of thermoplastic resin.
Background technology
Expanded product of thermoplastic resin is a basal component with the resin, contains a large amount of abscesses.Compare with virgin resin, it has the performance of a lot of excellences, as light weight, specific tenacity height, to have the ability that absorbs shock load, heat insulation and sound-proofing properties good etc.Therefore, be used widely in fields such as packing, daily necessities, building, automobile, bio-medical, space flight and aviation.For example the flex foam of good springiness now is used in aspects such as various cushions, liner, pillow, clothes in a large number; The heat-insulating property of foaming product is good, can be used as various insulations, heat insulation liner; The foaming product lightweight has the ability that absorbs shock load again, therefore, is the surface modifying material and the biomedical articles that can be used to make packaging material for food, high-strength light sound damping aircraft and trolley part, low friction.
The method for preparing expanded product of thermoplastic resin comprises physical blowing method and chemical blowing process.Traditional method commonly used to deleterious chloro fluorocarbon compound of ozonosphere and inflammable hydrocarbon polymer etc. as pneumatogen.Along with the raising of people's environmental consciousness, adopt clean, cheap, eco-friendly CO
2And N
2As pneumatogen, paid close attention to widely.But the affinity of these rare gas elementes and thermoplastic resin is poor, solubleness is low in resin, and their velocity of diffusion in polymkeric substance are fast, this makes foaming product have big abscess-size and uneven distribution of sizes and low abscess quantity, causes aspect variation such as outward appearance, mechanical property, barrier property, expansion ratio.
Summary of the invention
The purpose of this invention is to provide a kind of method of utilizing ultrasonic wave to prepare expanded product of thermoplastic resin.
The present invention utilizes ultrasonic wave to prepare the method for thermoplastic expanded goods, can adopt following dual mode:
First kind of mode comprises the steps:
1) the thermoplastic resin sample is placed autoclave, feed high pressure fluid, constant temperature and pressure is penetrated in the sample high pressure fluid;
2) high pressure fluid is discharged, take out sample, put into the liquid medium that is in ultrasonic environment and foam; With the sample quenching after the foaming, make the foam structure typing, obtain foaming product.
The second way comprises the steps:
1) the thermoplastic resin sample is placed autoclave, feed high pressure fluid, constant temperature and pressure is penetrated in the sample high pressure fluid;
2) in ultrasonic environment with the high pressure fluid snap-out release, make the abscess nucleation, sample is incubated in autoclave abscess is increased, and obtains foaming product.
In two kinds of preparation methods, selected high pressure fluid can be a high pressure CO usually
2And/or high pressure N
2The temperature of high pressure fluid is that 20～80 ℃, pressure are that 1～20MPa, saturation time are 0.5～10h.Apply hyperacoustic mode and can adopt oil bath or water-bath etc., hyperacoustic power is 50～300W, and frequency is 15～30kHz; Blowing temperature is that 40～120 ℃, foamed time are 5～300s.
In the present invention, one or more in the optional self-polystyrene of thermoplastic resin, polymethylmethacrylate, polyvinyl chloride, polycarbonate, poly-terephthalic acid second diester, poly(lactic acid), polycaprolactone, nylon and the polyolefine.Used thermoplastic resin can also be the matrix material of above-mentioned resin and filler, and wherein nano-sized filler comprises nanometer illiteracy holder soil, nano-attapulgite, carbon nanotube, carbon nanofiber, nano silicon, nano titanium oxide, nano whisker, nano-apatite etc.; The micron order filler comprises carbon black, granulated glass sphere, mica, wood chip etc.Can choose in these fillers one or more and join in the thermoplastic resin, filler can directly add or add after surface modification.
The present invention utilizes ultrasonic technology to assist solid-state foaming, the method of the solid-state foaming of a kind of ultrasonic technology auxiliary polyalcohol is provided, improve the nucleation density of abscess in the expanded product of thermoplastic resin, promote the gentle nuclear of nucleation in the polymer foaming process to increase, compare with not applying ultrasonic wave, can make things convenient for, prepare effectively the expanded product of thermoplastic resin of the excellent performance that cell diameter is little, expansion ratio is high.The inventive method has that technology is simple, pollution-free, the more effective characteristics of method, and the foam material of preparation has better physical and mechanical property.
Description of drawings
Figure 1A is not for adding the electromicroscopic photograph of hyperacoustic PMMA goods section;
Figure 1B is the electromicroscopic photograph that applies hyperacoustic PMMA goods section;
Fig. 2 A is not for adding the electromicroscopic photograph of hyperacoustic PS goods section;
Fig. 2 B is the electromicroscopic photograph that applies hyperacoustic PS goods section;
Fig. 3 A is not for adding the electromicroscopic photograph of hyperacoustic PC goods section;
Fig. 3 B is the electromicroscopic photograph that applies hyperacoustic PC goods section;
Fig. 4 A is not for adding the electromicroscopic photograph of hyperacoustic PS/PMMA goods section;
Fig. 4 B is the electromicroscopic photograph that applies hyperacoustic PS/PMMA goods section;
Fig. 5 A is not for adding the electromicroscopic photograph of hyperacoustic PS/CNT goods section;
Fig. 5 B is the electromicroscopic photograph that applies hyperacoustic PS/CNT goods section;
Fig. 6 A is not for adding hyperacoustic PC/SiO
2The electromicroscopic photograph of goods section;
Fig. 6 B is for applying hyperacoustic PC/SiO
2The electromicroscopic photograph of goods section;
Fig. 7 A is not for adding the electromicroscopic photograph of hyperacoustic PS goods section;
Fig. 7 B is the electromicroscopic photograph that applies hyperacoustic PS goods section.
Embodiment
The preparation of embodiment 1, PMMA foaming product
At 200 ℃ of fusion compressing tablets, the cold water quenching prepares the thick sample of 1mm with the polymethylmethacrylate after the vacuum-drying (PMMA).
Above-mentioned PMMA sample is inserted in the autoclave, feed the CO of 20 ℃/12MPa
2, behind the constant temperature and pressure 6h sample is taken out from autoclave, foaming (ultrasonic power is that 100W, ultrasonic frequency are 20kHz) in water-bath and in applying hyperacoustic water-bath respectively, blowing temperature is 80 ℃, foamed time is 20s.
Figure 1A is not for adding the electromicroscopic photograph of hyperacoustic PMMA goods section, Figure 1B is the electromicroscopic photograph that applies hyperacoustic PMMA goods section, the result shows: after ripple applies ultrasonic wave, the expansion ratio of the PMMA of foaming never adds hyperacoustic 2.3 and is increased to 4.6, cell diameter is reduced to 4.2 μ m from 14.0 μ m, and cell density is by 3.8 * 10
8Cells/cm
3Bring up to 2.5 * 10
10Cells/cm
3
The preparation of embodiment 2, PS foaming product
Polystyrene after the vacuum-drying (PS) is heated to 200 ℃, kept 3 minutes, the cold water quenching prepares the thick sample of 1mm.
Above-mentioned PS sample is inserted in the autoclave, feed the CO of 40 ℃/8MPa
2, behind the constant temperature and pressure 6h sample is taken out from autoclave, respectively in water-bath with apply in hyperacoustic water-bath foaming (ultrasonic power is that 200W, ultrasonic frequency are 20kHz), blowing temperature is 80 ℃, foamed time is 20s.
Fig. 2 A is not for adding the electromicroscopic photograph of hyperacoustic PS goods section, Fig. 2 B is the electromicroscopic photograph that applies hyperacoustic PS goods section, the result shows: after applying ultrasonic wave, the expansion ratio of the PS of foaming never adds hyperacoustic 1.3 and is increased to 2.4, and cell density is by 7.5 * 10
10Cells/cm
3Bring up to 2.3 * 10
11Cells/cm
3, abscess-size does not become 1.6 μ m, but cell size distribution becomes more even.
The preparation of embodiment 3, PC foaming product
At 260 ℃ of fusion compressing tablets, the cold water quenching prepares the thick sample of 1mm with the polycarbonate after the vacuum-drying (PC).
Above-mentioned PC sample is inserted in the autoclave, feed the CO of 20 ℃/20MPa
2, behind the constant temperature and pressure 10h sample is taken out from autoclave, foam (ultrasonic power is that 100W, ultrasonic frequency are 20kHz) with applying in hyperacoustic glycerol bath at glycerol bath respectively, blowing temperature is 100 ℃, foamed time is 30s.
Fig. 3 A is not for adding the electromicroscopic photograph of hyperacoustic PC goods section, Fig. 3 B is the electromicroscopic photograph that applies hyperacoustic PC goods section, the result shows: after applying ultrasonic wave, the expansion ratio of the PC of foaming never adds hyperacoustic 1.1 and is increased to 1.7, cell diameter is reduced to 2.1 μ m from 2.4 μ m, and cell density is by 1.2 * 10
10Cells/cm
3Bring up to 5.5 * 10
10Cells/cm
3
The preparation of embodiment 4, PLA foaming product
At 190 ℃ of fusion compressing tablets, the cold water quenching prepares the thick sample of 0.5mm with the poly(lactic acid) after the vacuum-drying (PLA).
Above-mentioned PLA sample is inserted in the autoclave, feed the CO of 35 ℃/1MPa
2, behind the constant temperature and pressure 5h sample is taken out from autoclave, respectively in water-bath with apply in hyperacoustic water-bath foaming (ultrasonic power is that 100W, ultrasonic frequency are 20kHz), blowing temperature is 40 ℃, foamed time is 300s.
The result shows: apply ultrasonic after, the expansion ratio of the PLA of foaming never adds hyperacoustic 1.2 and is increased to 1.9.
The preparation of embodiment 5, PS/PMMA foaming product
With Banbury mixer after with vacuum-drying PS and PMMA in 200 ℃ of melt blendings.PS and PMMA mass ratio are 85/15.Sample after the blend is at 200 ℃ of fusion compressing tablets, and the cold water quenching prepares the thick sample of 1mm.
Above-mentioned sample is inserted in the autoclave, feed the CO of 40 ℃/8MPa
2, behind the constant temperature and pressure 6h sample is taken out from autoclave, respectively in water-bath with apply in hyperacoustic water-bath foaming (ultrasonic power is that 100W, ultrasonic frequency are 20kHz), blowing temperature is 80 ℃, foamed time is 30s.
Fig. 4 A is not for adding the electromicroscopic photograph of hyperacoustic PS/PMMA goods section, Fig. 4 B is the electromicroscopic photograph that applies hyperacoustic PS/PMMA goods section, the result shows: apply ultrasonic after, the expansion ratio of foaming sample never adds hyperacoustic 1.1 and is increased to 2.1, cell diameter is reduced to 3.0 μ m by 2.3 μ m, and cell density is from 1.2 * 10
10Cells/cm
3Bring up to 3.5 * 10
10Cells/cm
3
The preparation of embodiment 6, PS/CNT foaming product
Prepare PS and multi-walled carbon nano-tubes (CNT) matrix material with Banbury mixer at 200 ℃.The mass ratio of PS and CNT is 99/1.Sample after the blend is at 200 ℃ of fusion compressing tablets, and the cold water quenching prepares the thick sample of 1mm.
Above-mentioned sample is inserted in the autoclave, feed the CO of 40 ℃/8MPa
2, behind the constant temperature and pressure 6h sample is taken out from autoclave, respectively in water-bath with apply in hyperacoustic water-bath foaming (ultrasonic power is that 100W, ultrasonic frequency are 20kHz), blowing temperature is 80 ℃, foamed time is 20s.
Fig. 5 A is not for adding the electromicroscopic photograph of hyperacoustic PS/CNT goods section, Fig. 5 B is the electromicroscopic photograph that applies hyperacoustic PS/CNT goods section, the result shows: apply ultrasonic after, the expansion ratio of foaming sample never adds hyperacoustic 1.1 and is increased to 1.4, cell diameter is reduced to 0.6 μ m by 1.0 μ m, and cell density is by 4.2 * 10
10Cells/cm
3Bring up to 7.5 * 10
11Cells/cm
3
Embodiment 7, PC/SiO
2The preparation of foaming product
With PC and the nanometer SiO of twin screw extruder after with vacuum-drying
2Melt extrude in 260 ℃.PC and SiO
2Mass ratio be 99/1.Sample after the blend is at 260 ℃ of fusion compressing tablets, and the cold water quenching prepares the thick sample of 1mm.
Above-mentioned sample is inserted in the autoclave, feed the CO of 20 ℃/20MPa
2, behind the constant temperature and pressure 10h sample is taken out from autoclave, foam (ultrasonic power is that 50W, ultrasonic frequency are 30kHz) with applying in hyperacoustic glycerol bath at glycerol bath respectively, blowing temperature is 100 ℃, foamed time is 30s.
Fig. 6 A is not for adding hyperacoustic PC/SiO
2The electromicroscopic photograph of goods section, Fig. 6 B is for applying hyperacoustic PC/SiO
2The electromicroscopic photograph of goods section, the result shows: after applying ultrasonic wave, the expansion ratio of foaming sample never adds hyperacoustic 1.1 and is increased to 1.5, and sample exists from the abscess that foams a large amount of hardly.
The preparation of embodiment 8, PS foaming product
At 200 ℃ of fusion compressing tablets, the cold water quenching prepares the thick sample of 1mm with the PS after the vacuum-drying.
Above-mentioned PS sample is inserted in the autoclave, feed the CO of 60 ℃/12MPa
2, behind the constant temperature and pressure 6h, respectively in water-bath with add to unload rapidly in hyperacoustic water-bath (ultrasonic power is that 300W, ultrasonic frequency are 15kHz) and be depressed into normal atmosphere, insulation 30min.
Fig. 7 A is not for adding the electromicroscopic photograph of hyperacoustic PS goods section, Fig. 7 B is the electromicroscopic photograph that applies hyperacoustic PS goods section, the result shows: with do not add ultrasonic wave and compare, after applying ultrasonic wave, the expansion ratio of the PS sample of foaming is increased to 1.7 from 1.2, cell diameter is reduced to 7.9 μ m by 23.5 μ m, and cell density is by 2.9 * 10
7Cells/cm
3Bring up to 1.2 * 10
9Cells/cm
3
Claims (11)
1, a kind of method for preparing expanded product of thermoplastic resin comprises the steps:
1) the thermoplastic resin sample is placed autoclave, feed high pressure fluid, constant temperature and pressure is penetrated in the sample high pressure fluid;
2) high pressure fluid is discharged, take out sample, put into the liquid medium that is in ultrasonic environment and foam; With the sample quenching after the foaming, make the foam structure typing, obtain foaming product.
2, method according to claim 1 is characterized in that: described high pressure fluid is a high pressure CO
2And/or high pressure N
2
3, method according to claim 2 is characterized in that: the temperature of described high pressure fluid is that 20～80 ℃, pressure are that 1～20MPa, saturation time are 0.5～10h.
4, method according to claim 1 is characterized in that: hyperacoustic power is 50～300W, and frequency is 15～30kHz; Blowing temperature is that 40～120 ℃, foamed time are 5～300s.
5, according to the arbitrary described method of claim 1-4, it is characterized in that: described thermoplastic resin is selected from one or more in polystyrene, polymethylmethacrylate, polyvinyl chloride, polycarbonate, poly-terephthalic acid second diester, poly(lactic acid), polycaprolactone, nylon and the polyolefine.
6, method according to claim 5, it is characterized in that: described thermoplastic resin can also contain one or more fillers, and described filler is selected from nanometer and covers holder soil, nano-attapulgite, carbon nanotube, carbon nanofiber, nano silicon, nano titanium oxide, nano whisker, nano-apatite, carbon black, granulated glass sphere, mica and wood chip.
7, a kind of method for preparing expanded product of thermoplastic resin comprises the steps:
1) the thermoplastic resin sample is placed autoclave, feed high pressure fluid, constant temperature and pressure is penetrated in the sample high pressure fluid;
2) in ultrasonic environment with the high pressure fluid snap-out release, make the abscess nucleation, sample is incubated in autoclave abscess is increased, and obtains foaming product.
8, method according to claim 7 is characterized in that: described high pressure fluid is a high pressure CO
2And/or high pressure N
2The temperature of high pressure fluid is that 20～80 ℃, pressure are that 1～20MPa, saturation time are 0.5～10h.
9, method according to claim 7 is characterized in that: hyperacoustic power is 50～300W, and frequency is 15～30kHz; Blowing temperature is that 40～120 ℃, foamed time are 5～300s.
10, according to the arbitrary described method of claim 7-9, it is characterized in that: described thermoplastic resin is selected from one or more in polystyrene, polymethylmethacrylate, polyvinyl chloride, polycarbonate, poly-terephthalic acid second diester, poly(lactic acid), polycaprolactone, nylon and the polyolefine.
11, method according to claim 10, it is characterized in that: described thermoplastic resin can also contain one or more fillers, and described filler is selected from nanometer and covers holder soil, nano-attapulgite, carbon nanotube, carbon nanofiber, nano silicon, nano titanium oxide, nano whisker, nano-apatite, carbon black, granulated glass sphere, mica and wood chip.
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|---|---|---|---|
| CNB2006100568138A CN100549073C (en) | 2006-03-07 | 2006-03-07 | A kind of method for preparing expanded product of thermoplastic resin |
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|---|---|---|---|
| CNB2006100568138A CN100549073C (en) | 2006-03-07 | 2006-03-07 | A kind of method for preparing expanded product of thermoplastic resin |
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| CN100549073C CN100549073C (en) | 2009-10-14 |
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| CN113444278A (en) * | 2021-06-30 | 2021-09-28 | 四川大学 | Method for preparing polymer foam material by utilizing ultrasonic-assisted high-pressure fluid |
| CN115850879A (en) * | 2022-11-26 | 2023-03-28 | 四川大学 | Method for preparing high-foaming-ratio foaming material by using ultrasonic and water-assisted high-pressure fluid |
| CN115850879B (en) * | 2022-11-26 | 2024-04-12 | 四川大学 | Method for preparing high-foaming-rate foaming material by ultrasonic and water-assisted high-pressure fluid |
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