CN105218851A - A kind of method preparing polymkeric substance hole-opening foaming material - Google Patents
A kind of method preparing polymkeric substance hole-opening foaming material Download PDFInfo
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- CN105218851A CN105218851A CN201510565901.XA CN201510565901A CN105218851A CN 105218851 A CN105218851 A CN 105218851A CN 201510565901 A CN201510565901 A CN 201510565901A CN 105218851 A CN105218851 A CN 105218851A
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Abstract
The present invention relates to a kind of method preparing polymkeric substance hole-opening foaming material, the present invention utilizes supercutical fluid foaming technique, adopt moulded from foam mode, under the prerequisite not affecting other performance of polymkeric substance, with the addition of the nanoparticle with nucleator and pore-creating agent double effects, considerably improve nucleation density and the percentage of open area of polymkeric substance; In the present invention, perforate auxiliary agent adds the effect can playing heterogeneous nucleation agent on the one hand, promotion cell nucleation, increase cell density; On the other hand, perforate auxiliary agent is again a kind of good pore-creating agent, promotes that cell wall is broken, increases percentage of open area; Whole technological process environmental protection of the present invention, without chemical residual; And can by regulating the pressure and temperature of swelling treatment process, the hole-opening foaming material of obtained different abscess-size, makes polymkeric substance hole-opening foaming of the present invention have the Modulatory character of abscess-size in a large number.
Description
Technical field
The present invention relates to a kind of method preparing polymkeric substance hole-opening foaming material.
Background technology
Hole-opening foaming material refers to it is not closed between abscess, but is interconnected, and body material exists with the cell wall be interconnected.This special foam structure can make solid granule or liquid flow between abscess, imparts the function and application that it is new, as separation, sorbing material, support of the catalyst, Thermosensitive Material Used for Controlled Releasing of Medicine etc., can have huge application prospect.
The requirement of preparation to equipment and process of hole-opening foaming material is stricter, technical difficulty is larger, preparation method is divided into chemical foaming and physical blowing usually, and great majority research at present concentrates on chemical foaming aspect, but the residual of chemical foaming agent has a significant impact the properties of material.The preparation method of chemical foaming polymer beads is extruded disclosed in number of patent application CN200810120399.1, that injection port is set in the middle part of the machine barrel of screw extrusion press, polymer foaming material and auxiliary agent thereof are added in screw extrusion press, alkane whipping agent is injected machine barrel from injection port foam, in production process, fluid foaming agent is all injected in twin screw extruder and carries out mixing extrusion pelletizing, owing to being subject to humidity in mixing process, the impact of the uniformity coefficient of dispersing shear and the consistency of mixing, so high to forcing machine processing requirement, wayward, and make the content of the whipping agent in finished product bead uneven, cause product unstable.In addition, alkanes whipping agent is inflammable and explosive, very easily causes potential safety hazard.In addition, US Patent No. 7318713 discloses a kind of method utilizing overcritical injection molding technology to prepare polymer micro foam material, supercutical fluid is imported the barrel of injection moulding machine by the method, in barrel, form the homogeneous phase solution of polymkeric substance/supercutical fluid, homogeneous phase solution is being injected into the immediate effervescence of mould.The method is lower due to bubble nucleating speed, and the hole density obtained is less, can only realize the loss of weight that foaming product is less, and general injection moulding microporous foam goods loss of weight can not more than 30%, and therefore perforate effect is not remarkable.Patent publication No. CN101531770A discloses a kind of preparation method of open-cell foamed polyolefin.By polyolefine with mixed by identical olefines polyolefin pellets, nucleator, the nucleator masterbatch that helps foaming antishrinking agent, oxidation inhibitor to make after, drop into heating plasticizing melting in singe screw between length-to-diameter ratio 20-50 or twin screw extruder and inject high pressure gas, high pressure gas and the abundant melting mixing of polyolefine are extruded, when going out extruding dies, release of pressure is expanded foamed, makes the open-cell foamed products of different shape.But hole-opening foaming material has very large requirement to foaming machine and technique, select to be difficult to during extrusion foaming control the factor larger on foaming impact such as the injected gas scale of construction, screw-rod structure, Heating temperature.
Summary of the invention
Technical problem to be solved by this invention is the present situation for prior art, provides a kind of and prepares the high and method of abscess-size regulatable polymkeric substance hole-opening foaming material of percentage of open area.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of method preparing polymkeric substance hole-opening foaming material, is characterized in that comprising the following steps:
(1) polymer matrix material mixed with perforate auxiliary agent and add in forcing machine or injection moulding machine, by forcing machine or injection moulding machine, the mixing material of polymer matrix material and perforate auxiliary agent being prepared into the effigurate polymer composites of tool;
(2) step (1) resulting polymers matrix material is placed in Belt-type tools, moulding press matched moulds sealed mold; First purge Belt-type tools with supercutical fluid, the air displacement in mould is gone out, then continue to pour supercutical fluid in Belt-type tools, at 0 ~ 350 DEG C, swelling treatment 0.3 ~ 24h under 1 ~ 50MPa;
(3) quick pressure releasing is to normal pressure, is cooled to 0 ~ 50 DEG C, namely obtains described polymkeric substance hole-opening foaming material.
As preferably, described polymer matrix material is selected from one or more the blend in polystyrene, polycarbonate, acrylonitrile-butadiene-styrene copolymer, polyimide, polymeric amide, polyphenylene sulfide, polyethersulfone, polyvinyl chloride, natural rubber, silicon rubber, paracril, polypropylene, polyethylene, poly(lactic acid), polyethylene terephthalate.
Preferably, described perforate auxiliary agent is selected from polymkeric substance or nanoparticle.
Further preferably, described polymkeric substance is one or more in LLDPE, ultrahigh molecular weight polyethylene(UHMWPE), ultrahigh molecular weight polypropylene; Described nanoparticle is one or more in Graphene, polynite, carbon nanotube, talcum powder, nano-calcium carbonate.
As improvement, the weight of described perforate auxiliary agent is 0.1% ~ 10% of polymer composites gross weight.
Preferably, the flow velocity pouring supercutical fluid in step (2) in described Belt-type tools is 0.1MPa/s ~ 10MPa/s.
Preferably, the pressure release speed in step (3) is 0.1MPa/s ~ 100MPa/s.
Preferably, described supercutical fluid is the mixed gas of the one or both in carbonic acid gas, nitrogen.
Compared with prior art, the invention has the advantages that:
The present invention utilizes supercutical fluid foaming technique, adopts moulded from foam mode, under the prerequisite not affecting other performance of polymkeric substance, with the addition of the nanoparticle with nucleator and pore-creating agent double effects, considerably improve nucleation density and the percentage of open area of polymkeric substance;
The abscess of polymkeric substance hole-opening foaming material is formed and is generally divided into three phases, i.e. nucleation, the cell growth of abscess, cell wall is thinning breaks with cell wall, and in the present invention, perforate auxiliary agent adds the effect can playing heterogeneous nucleation agent on the one hand, promote cell nucleation, increase cell density; On the other hand, perforate auxiliary agent is again a kind of good pore-creating agent, promotes that cell wall is broken, increases percentage of open area;
Whole technological process environmental protection of the present invention, without chemical residual; And can by regulating the pressure and temperature of swelling treatment process, the hole-opening foaming material of obtained different abscess-size, makes polymkeric substance hole-opening foaming material of the present invention have the Modulatory character of abscess-size.
Accompanying drawing explanation
Fig. 1 is the SEM figure of polyethylene/ultrahigh molecular weight polyethylene(UHMWPE) prepared in the embodiment of the present invention 1;
Fig. 2 is polypropylene/talcous SEM figure prepared in the embodiment of the present invention 2;
Fig. 3 is the SEM figure of polyethylene/carbon nanotube prepared in the embodiment of the present invention 3.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in further detail.
Embodiment 1:
The method preparing polymkeric substance hole-opening foaming material of the present embodiment comprises the following steps:
(1) be 40,000 by number-average molecular weight, fusing point is that the polyethylene particle of 125 DEG C and ultrahigh molecular weight polyethylene(UHMWPE) mix and add in forcing machine or injection moulding machine, by forcing machine or injection moulding machine, the mixing material of polymer matrix material and perforate auxiliary agent is prepared into the polymer composites of sheet; Wherein, the processing temperature of forcing machine is 160 DEG C, and screw speed is 25 turns/min, or the processing temperature of injection moulding machine is 160 DEG C; The weight of ultra-high molecular weight base ethene is 3% of polymer composites gross weight;
(2) step (1) resulting polymers matrix material is placed in Belt-type tools, moulding press matched moulds sealed mold; First purge Belt-type tools with carbon dioxide, the air displacement in mould gone out, then continue to pour carbon dioxide in Belt-type tools, the flow velocity that pours of this carbonic acid gas is 0.1MPa/s, at 136 DEG C, swelling treatment 80min under 20MPa;
(3) with speed be 96MPa/s pressure release to normal pressure, be cooled to 50 DEG C, namely obtain polyethylene/ultra-high molecular weight base ethene hole-opening foaming material.
Through liquid nitrogen brittle failure, scanning electron microscope analysis is carried out to the tangent plane of polyethylene/ultra-high molecular weight base ethene hole-opening foaming material, as shown in Figure 1.The mean pore size of polyethylene/ultra-high molecular weight base ethene hole-opening foaming material is about 11.9 μm, and hole density is 5.4 × 10
9individual/cm
3, foam material comparatively raw material volume expands about 3.2 times.
Embodiment 2:
The method preparing polymkeric substance hole-opening foaming material of the present embodiment comprises the following steps:
(1) be 80,000 by number-average molecular weight, fusing point is that the polypropylene GRANULES of 158 DEG C and talcum powder mix and add in forcing machine or injection moulding machine, by forcing machine or injection moulding machine, the mixing material of polymer matrix material and perforate auxiliary agent is prepared into the polymer composites of sheet; Wherein, the processing temperature of forcing machine is 190 DEG C, and screw speed is 25 turns/min, or the processing temperature of injection moulding machine is 190 DEG C; Talcous weight is 5% of polymer composites gross weight;
(2) step (1) resulting polymers matrix material is placed in Belt-type tools, moulding press matched moulds sealed mold; First purge Belt-type tools with carbon dioxide, the air displacement in mould gone out, then continue to pour carbon dioxide in Belt-type tools, the flow velocity that pours of this carbonic acid gas is 10MPa/s, at 170 DEG C, swelling treatment 24h under 28MPa;
(3) with speed be 0.1MPa/s pressure release to normal pressure, be cooled to 10 DEG C, namely obtain polypropylene/talcum powder hole-opening foaming material.
Through liquid nitrogen brittle failure, scanning electron microscope analysis is carried out to the tangent plane of polypropylene/talcum powder hole-opening foaming material, as shown in Figure 2.The mean pore size of polypropylene/talcum powder hole-opening foaming material is about 12.6 μm, and hole density is 1.3 × 10
9individual/cm
3, foam material comparatively raw material volume expands about 5.1 times.
Embodiment 3:
The method preparing polymkeric substance hole-opening foaming material of the present embodiment comprises the following steps:
(1) be 60,000 by number-average molecular weight, fusing point is that the polyethylene particle of 125 DEG C and carbon nanotube mix and add in forcing machine or injection moulding machine, by forcing machine or injection moulding machine, the mixing material of polymer matrix material and perforate auxiliary agent is prepared into the polymer composites of sheet; Wherein, the processing temperature of forcing machine is 140 DEG C, and screw speed is 25 turns/min, or the processing temperature of injection moulding machine is 140 DEG C; The weight of carbon nanotube is 1% of polymer composites gross weight;
(2) step (1) resulting polymers matrix material is placed in Belt-type tools, moulding press matched moulds sealed mold; First use nitrogen purging Belt-type tools, the air displacement in mould gone out, then continue to pour nitrogen in Belt-type tools, this nitrogen to pour flow velocity be 1.7MPa/s at 140 DEG C, swelling treatment 80min under 30MPa;
(3) with speed be 100MPa/s pressure release to normal pressure, be cooled to 25 DEG C, namely obtain polyethylene/carbon nanotube hole-opening foaming material.
Through liquid nitrogen brittle failure, scanning electron microscope analysis is carried out to the tangent plane of polyethylene/carbon nanotube hole-opening foaming material, as shown in Figure 3.The mean pore size of polyethylene/carbon nanotube hole-opening foaming material is about 2.5 μm, and hole density is 1.8 × 10
10individual/cm
3, foam material comparatively raw material volume expands about 2.7 times.
In the various embodiments described above, foam material mean pore size and cell density can be analyzed by SEM photo.SEM photo adopts scanning electronic microscope (SEM) shooting, and analytical instrument is Japanese JEOL company JSM-6360LV type scanning electron microscope.From SEM photo, add up micropore number n (>100), determine photo area A (cm
2) and magnification M.Its mesopore density adopts document V.Kumar, the disclosed KUMAR method estimation of N.P.Suh.AprocessforMakingMicrocellularThermoplasticParts, Polymer.Eng.Sci.30,1323-1329 (1990):
Area density is:
Because particle is approximately ball-type, therefore can suppose abscess isotropic growth, then unit volume hole density is:
Claims (8)
1. prepare a method for polymkeric substance hole-opening foaming material, it is characterized in that comprising the following steps:
(1) polymer matrix material mixed with perforate auxiliary agent and add in forcing machine or injection moulding machine, by forcing machine or injection moulding machine, the mixing material of polymer matrix material and perforate auxiliary agent being prepared into the effigurate polymer composites of tool;
(2) step (1) resulting polymers matrix material is placed in Belt-type tools, moulding press matched moulds sealed mold; First purge Belt-type tools with supercutical fluid, the air displacement in mould is gone out, then continue to pour supercutical fluid in Belt-type tools, at 0 ~ 350 DEG C, swelling treatment 0.3 ~ 24h under 1 ~ 50MPa;
(3) quick pressure releasing is to normal pressure, is cooled to 0 ~ 50 DEG C, namely obtains described polymkeric substance hole-opening foaming material.
2. the method preparing polymkeric substance hole-opening foaming material according to claim 1, is characterized in that: described polymer matrix material is selected from one or more the blend in polystyrene, polycarbonate, acrylonitrile-butadiene-styrene copolymer, polyimide, polymeric amide, polyphenylene sulfide, polyethersulfone, polyvinyl chloride, natural rubber, silicon rubber, paracril, polypropylene, polyethylene, poly(lactic acid), polyethylene terephthalate.
3. the method preparing polymkeric substance hole-opening foaming material according to claim 1, is characterized in that: described perforate auxiliary agent is selected from polymkeric substance or nanoparticle.
4. the method preparing polymkeric substance hole-opening foaming material according to claim 3, is characterized in that: described polymkeric substance is one or more in LLDPE, ultrahigh molecular weight polyethylene(UHMWPE), ultrahigh molecular weight polypropylene; Described nanoparticle is one or more in Graphene, polynite, carbon nanotube, talcum powder, nano-calcium carbonate.
5. the method preparing polymkeric substance hole-opening foaming material according to claim 1, is characterized in that: the weight of described perforate auxiliary agent is 0.1% ~ 10% of polymer composites gross weight.
6. the method preparing polymkeric substance hole-opening foaming material according to claim 1, is characterized in that: the flow velocity pouring supercutical fluid in step (2) in described Belt-type tools is 0.1MPa/s ~ 10MPa/s.
7. the method preparing polymkeric substance hole-opening foaming material according to claim 1, is characterized in that: the pressure release speed in step (3) is 0.1MPa/s ~ 100MPa/s.
8. the method preparing polymkeric substance hole-opening foaming material according to claim 1, is characterized in that: described supercutical fluid is the mixed gas of the one or both in carbonic acid gas, nitrogen.
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| CN105778257A (en) * | 2016-03-17 | 2016-07-20 | 宁波大学 | Linear low-density polyethylene/carbon nanotube open-cell foam material and method for preparing same |
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| CN114714556A (en) * | 2022-04-01 | 2022-07-08 | 启东纽昇塑胶科技有限公司 | Preparation method for producing open-cell polyethylene foam material |
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