CN101649085A - Method for preparing polymer-matrix composite material by in-situ bubble stretching one-step defoaming method - Google Patents

Method for preparing polymer-matrix composite material by in-situ bubble stretching one-step defoaming method Download PDF

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CN101649085A
CN101649085A CN200910093282A CN200910093282A CN101649085A CN 101649085 A CN101649085 A CN 101649085A CN 200910093282 A CN200910093282 A CN 200910093282A CN 200910093282 A CN200910093282 A CN 200910093282A CN 101649085 A CN101649085 A CN 101649085A
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temperature
district
polypropylene
screw extruder
twin screw
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CN101649085B (en
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吴大鸣
刘颖
陈卫红
许红
赵利涛
林春平
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Beijing University of Chemical Technology
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Beijing University of Chemical Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
    • B29C48/918—Thermal treatment of the stream of extruded material, e.g. cooling characterized by differential heating or cooling
    • B29C48/9185—Thermal treatment of the stream of extruded material, e.g. cooling characterized by differential heating or cooling in the direction of the stream of the material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04—Particle-shaped
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • B29C2948/9259—Angular velocity
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92885—Screw or gear
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895—Barrel or housing

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention relates to a method for preparing a polymer-matrix composite material by an in-situ bubble stretching one-step defoaming method, belonging to the technical field of polymer-based composite material preparation. The method comprises the following steps: preparing a polypropylene and stuffing organic matter master batch: mixing polypropylene and stuffing, and then adding an antioxidant, a compatibilizer and a processing aid to the mixture of polypropylene and the stuffing; evenly mixing in a blender, and then melting and mixing through a double-screw extruder to prepare the polypropylene and stuffing organic matter master batch; evenly mixing the organic matter master batch, a foaming agent and the antioxidant in the blender, and then adding to a single-screw extruder to carryout foaming; directly entering the double-screw extruder without cooling after the material is extruded from a nose of the single-screw extruder, subsequently defoaming, and finally pelletizing through melting, mixing and extruding. The invention avoids the energy loss caused by cooling then melting and is convenient, simple and direct; moreover, the defoaming effect is more obvious. The inventioncan be widely used for producing polymer-based composite materials, and the prepared composite materials have good performance.

Description

The in-situ bubble stretching one-step defoaming legal system is equipped with the method for polymer matrix composite
Technical field
The invention belongs to the technical field of polymer matrix composite preparation, be specifically related to the technology and the preparation method of polymer matrix composite.The present invention can be widely used in the production polymer matrix composite, and the matrix material that uses this processing method to prepare has good performance.
Background technology
The the most basic of preparation polymer matrix composite also is that method is shearing dispersing and stretching dispersion method the most widely, its principle is shear field and the stretching field that utilizes mixing facilities such as forcing machine that external phase is produced, and realizes the distribution mixing and the dispersing and mixing of disperse phase.But because ordinary method is difficult to obtain very high stretching field, so main method adopts shearing method to carry out the preparation of polymer matrix composite on the present engineering.We know in polymkeric substance and to add some physical and chemical performances that fine particle can improve material, but forcing machine commonly used, and the shearing rate that can provide approximately has only 10 3～10 4s -1, this dispersion to fine particle is not enough.Beijing University of Chemical Technology has proposed in-situ bubble stretching method (ISBS) and has promptly utilized the high rate of extension of air bubble expansion generation that the particulate around the bubble is carried out the dispersive method.The in-situ bubble stretching method can be used for the dispersion of polymer melt solid particulate coacervate, because molecule and coacervate can play nucleogenesis in the polymkeric substance, bubble preferentially in molecule and generation of coacervate place and expansion, produces original position stretching and disperses.Because the speed of air bubble expansion is exceedingly fast, the polymkeric substance around the abscess can produce very big tensile stress, and this tensile stress affacts on the particulate, will force microparticulate.Theoretical Calculation shows, its polymer melt is on every side produced up to 10 6s -1Rate of extension, than the obtainable shearing of common mechanical dispersion method institute or high two orders of magnitude of rate of extension, thereby can obtain to be better than the dispersion effect of conventional dispersing and mixing equipment.
Adopt the in-situ bubble stretching method to disperse fine particle to be based on to the understanding of heterogeneous nucleation foaming process with to the stretching field that produces in the Bubble Growth Process, the research of oscillating field.According to the bubble nucleating theory of classics, outside the molten homogeneous system of degasification in the polymer melt, also there is solid dispersed phase, then bubble nucleating can preferentially produce both so-called heterogeneous nucleation on molten admittedly interface.People such as Colton and Suh is based on the bubble nucleating theory of classics, the heterogeneous nucleation theory of bubble in the polymer melt carried out perfect, proposed the heterogeneous nucleation theory at solid particulate wedge shaped cavities place.Result of study shows that with respect to the bubble homogeneous nucleation, the required Gibbs free energy that overcomes of heterogeneous nucleation reduces, so bubble nucleating will preferentially produce at these particle surfaces.When fine particle adds in the polymer melt as nucleator, because the high surface energy of himself, agglomeration can appear inevitably, and gas molecule can be mixed in wherein inevitably between the agglomerating particles, become the potential nucleation site, research according to Colton and Suh etc., gas molecule is assembled formed complex order of size should be about a hundreds of Ethylmercurichlorendimide, suitable with the size of nanoparticle, so the agglomerating particles surface of surface irregularity and the microcavities between the particle have just formed a large amount of potential nucleation sites.In addition, bubble is when expanding, and the melt around the bubble removes can produce 10 6s -1Even higher rate of extension, bubble can also can also produce frequency under certain condition up to 10 7The vibration of HZ, oscillation frequency are in hyperacoustic scope.The rapid expansion of abscess and HF oscillation can produce quick stretching action to polymer melt around it on the one hand, also may produce the ultrasonic cavitation effect on the other hand, the fragmentation of the powder that causes reuniting.
The advantage of ISBS is the rate of extension that can obtain than higher; simultaneously; because air bubble expansion mainly carries out around the nanoclusters aggressiveness; thereby has a higher dispersion efficiency; this method does not need special processing units; easy realization mass-producing, the polymer matrix composite after the ISBS method is disperseed can be carried out the also direct machine-shaping of froth breaking by expressing technique or by carrying out machine-shaping behind the mechanical high-speed pulverizing froth breaking, obtain goods at last.After but the filler that adds disperses through the ISBS method, the residual bubble of meeting in the matrix material, can influence the performance of material like this, therefore must carry out defoaming treatment, and in froth breaking and molding process, the chance that the fine particle in the compound system can occur being in contact with one another and collide mutually, in this case, fine particle is take place to reunite or separate, and being dominant by reunion effect in this process still is the separate effect decision that is dominant.
Summary of the invention
The invention provides a cover and directly eliminate the processing method of bubble, be used for eliminating the in-situ bubble stretching legal system and be equipped with the bubble that exists in the polymer matrix composite.And a so-called one-step defoaming method just is meant that directly entering twin screw extruder without cooling after polymer matrix composite is through the single screw extrusion machine foaming carries out froth breaking.So just avoided the first cooling energy waste that causes of fusion again, also avoided thermal history in the froth breaking process simultaneously the various Effect on Performance of matrix material.Be exactly to adopt this method more convenient simpler and more direct than other debubbling method in addition, defoaming effect is more obvious.By the processing parameter of adjusting two steps type forcing machine and the screw combinations of forcing machine, obtain best exhaust effect, finally reach the purpose of eliminating bubble, observe by the matrix material that field emission scanning electron microscope is prepared an one-step defoaming method, do not find exist (referring to the Figure of description 1) of obvious bubble, and the performance of material each side all is improved before eliminating bubble, makes material reach excellent performance.
Done in-situ bubble stretching (ISBS) one-step defoaming legal system as the checking of this invention and be equipped with the polymer matrix composite experiment, experiment may further comprise the steps:
1) preparation polypropylene/stuffing organic matter master batch
With polypropylene and filler by weight 3: 100-35: 100 mix, and add 0.1-1 part oxidation inhibitor again in per 100 parts of polypropylene/filler mixtures, 0.1-5 part expanding material also has other processing aids of 0.1-5 part.After stirrer for mixing is even, by the twin screw extruder melting mixing, make polypropylene/stuffing organic matter master batch, twin screw extruder is respectively distinguished temperature: district's temperature a: 170-190 ℃, two district's temperature: 180-220 ℃, three district's temperature: 190-230 ℃, four district's temperature: 180-230 ℃, five district's temperature: 190-240 ℃, six district's temperature: 190-240 ℃, the twin screw rotating speed is 30-1200r/min.
2) carry out froth breaking with list-twin screw extruder one one-step defoaming method
70-120 part, 0.01-3.5 part, 0.1-1 part add in the single screw extrusion machine and foam after stirrer for mixing is even by weight ratio with organic matter master batch, whipping agent, oxidation inhibitor.After extruding, material carries out froth breaking in the twin screw extruder without cooling off directly to enter from the single screw extrusion machine head, through the melting mixing extruding pelletization, and the polypropylene-base matrix material behind the bubble that is eliminated.Wherein, single-screw machine tube temperature: district's temperature a: 170-190 ℃, two district's temperature: 180-220 ℃, three district's temperature: 180-230 ℃, four district's temperature: 190-240 ℃, five district's temperature: 190-240 ℃, single-screw machine head temperature: 180-220 ℃, single screw speed is 30-1200r/min, and single-screw machine head pressure is reduced to 30-200bar; Twin screw extruder is respectively distinguished temperature: district's temperature a: 160-190 ℃, two district's temperature: 165-205 ℃, three district's temperature: 170-210 ℃, four district's temperature: 180-220 ℃, five district's temperature: 180-230 ℃, six district's temperature: 190-240 ℃, the twin screw rotating speed is 30-1200r/min.
Described filler is micro-calcium carbonate, nano-calcium carbonate (nano-CaCO 3), nano-sized magnesium hydroxide (nano-Mg (OH) 2) or nanometer butadiene-styrene-vinyl rubber (SBR) powder; Described oxidation inhibitor is phenols, phosphorous acid esters, contain one or more the mixture in thioesters class, the metal passivator; Described expanding material refers to hard ester acid, silane, organosilicon, titanium ester acids coupling agent, polymeric surface active agent etc.; Described other processing aids are one or more the mixture in fatty acid amide, fatty acid mixture, paraffin, white mineral oil, the alpha-methyl styrene.
Wherein, preferred atactic copolymerized polypropene PPR; Homo-polypropylene PP: preferred median size is the micro-calcium carbonate of 1-53 μ m; Preferred median size is the nano-calcium carbonate (nano-CaCO of 30-9Onm 3); Preferred median size is the nano-sized magnesium hydroxide (nano-Mg (OH) of 50-100nm 2); Preferred median size is the nanometer butadiene-styrene-vinyl rubber (SBR) of 60-110nm.
According to the similar compatibility principle polypropylene and filler and various auxiliary agent are carried out premix in the step 1) of the present invention, help the dispersion of filler in matrix resin, thereby improve the mechanical property of polymer matrix composite.
What utilize step 2 of the present invention) is " in-situ bubble stretching method " (ISBS) [Chinese plastics, 2004,18 (4) .59-63] polypropylene/filler for preparing in the step 1) is foamed, its objective is the homodisperse that helps filler in polypropylene/filler master batch.
Compared with prior art, the present invention has following beneficial effect:
An one-step defoaming method provided by the present invention goes a step further than former debubbling method is more preceding, method in the past is after the material cooling is waited in the foaming back on the forcing machine, then with carrying out froth breaking after the crusher in crushing again, need two steps to finish, and an one-step defoaming method is can reach the purpose of eliminating bubble once going on foot.Adopt present method to prepare polymer matrix composite and shortened the thermal history among the preparation technology, saved preparation cost, and the performance of composites of preparing is more excellent, can be widely used in making in the production of polymer matrix composite.
Description of drawings
Fig. 1, in-situ bubble stretching one-step defoaming legal system of the present invention are equipped with the electromicroscopic photograph figure before and after the polymer matrix composite froth breaking.(a)-(e) is the preceding electromicroscopic photograph of sample froth breaking that makes with in-situ bubble stretching (ISBS) method among Fig. 1, and (f)-(j) is through the method for an one-step defoaming and through the injection molding sample electromicroscopic photograph of injection moulding machine among Fig. 1.
Fig. 2, in-situ bubble stretching one-step defoaming legal system of the present invention are equipped with the preparation flow figure of polymer matrix composite.
Fig. 3, in-situ bubble stretching one-step defoaming legal system of the present invention are equipped with the equipment flowsheet of polymer matrix composite.Shown in the numbering indication thes contents are as follows among the figure: 1: resin, powder, whipping agent etc.; 2: controlled ISBS foaming; 3: single screw extrusion machine; The 4:ISBS foam; 5: enter the direct froth breaking of twin screw extruder; 6: twin screw extruder (froth breaking); 7: the extrusion moulding unit; 8: extruded product
The invention will be further described below in conjunction with accompanying drawing and specific implementation method.
Embodiment
Embodiment 1
1) preparation polypropylene/stuffing organic matter master batch
Polypropylene and nano-sized magnesium hydroxide were mixed in 70: 3 by weight percentage, in per 100 parts of polypropylene/nano-sized magnesium hydroxide mixture, add 0.1 part of antioxidant 1010 again, 3 parts of titanic acid ester, 0.1 part white mineral oil, after stirrer for mixing is even, by the twin screw extruder melting mixing, make polypropylene/nano-sized magnesium hydroxide organic matter master batch, twin screw extruder is respectively distinguished temperature: district's temperature: 170 ℃, two district's temperature: 180 ℃, three district's temperature: 190 ℃, four district's temperature: 180 ℃, five district's temperature: 190 ℃, six district's temperature: 190 ℃, the twin screw rotating speed is 30r/min.
2) carry out froth breaking with list-twin screw extruder one one-step defoaming method
With 100 parts by weight ratio, 0.01 part, 0.1 part of organic matter master batch, AC whipping agent, antioxidant 1010 stirrer for mixing evenly after, add in the single screw extrusion machine and foam.After extruding, material carries out froth breaking in the twin screw extruder without cooling off directly to enter from the single screw extrusion machine head, through the melting mixing extruding pelletization, and the polypropylene-base matrix material behind the bubble that is eliminated.Wherein, single-screw machine tube temperature: district's temperature: 170 ℃, two district's temperature: 180 ℃, three district's temperature: 180 ℃, four district's temperature: 190 ℃, five district's temperature: 190 ℃, single-screw machine head temperature: 190 ℃, single screw speed is 30r/min, and single-screw machine head pressure is reduced to 30bar; Twin screw extruder is respectively distinguished temperature: district's temperature: 160 ℃, two district's temperature: 165 ℃, three district's temperature: 170 ℃, four district's temperature: 180 ℃, five district's temperature: 180 ℃, six district's temperature: 190 ℃, the twin screw rotating speed is 30r/min.
Embodiment 2
1) preparation polypropylene/nano-calcium carbonate organic matter master batch
Polypropylene and nano-calcium carbonate were mixed in 100: 10 by weight percentage, in per 100 parts of polypropylene/nano-calcium carbonate calcium compounds, add 1 part of antioxidant 1076 again, 0.1 part aluminic acid ester, 2.5 part whiteruss, after stirrer for mixing is even, by the twin screw extruder melting mixing, make polypropylene/nano-calcium carbonate organic matter master batch, the temperature of respectively distinguishing of twin screw extruder is: district's temperature: 180 ℃, two district's temperature: 190 ℃, three district's temperature: 195 ℃, four district's temperature: 205 ℃, five district's temperature: 215 ℃, six district's temperature: 220 ℃, the twin screw rotating speed is 260r/min.
2) carry out froth breaking with list-twin screw extruder one one-step defoaming method
With 100 parts by weight ratio, 1.5 parts, 1 part of organic matter master batch, AC whipping agent, antioxidant 1076 stirrer for mixing evenly after, add in the single screw extrusion machine and foam.After extruding, material carries out froth breaking in the twin screw extruder without cooling off directly to enter from the single screw extrusion machine head, through the melting mixing extruding pelletization, and the polypropylene-base matrix material behind the bubble that is eliminated.Wherein, single-screw machine tube temperature: district's temperature: 175 ℃, two district's temperature: 190 ℃, three district's temperature: 205 ℃, four district's temperature: 215 ℃, five district's temperature: 205 ℃, single-screw machine head temperature: 195 ℃, single screw speed is 200r/min, and single-screw machine head pressure is reduced to 80bar; Twin screw extruder is respectively distinguished temperature: district's temperature: 170 ℃, two district's temperature: 175 ℃, three district's temperature: 190 ℃, four district's temperature: 200 ℃, five district's temperature: 210 ℃, six district's temperature: 205 ℃, the twin screw rotating speed is 400r/min.
Embodiment 3
1) preparation polypropylene/stuffing organic matter master batch
Polypropylene and micro-calcium carbonate were mixed in 100: 15 by weight percentage, in per 100 parts of polypropylene/micro-calcium carbonate mixture, add 0.5 part of antioxidant 300 again, 3 parts of stearic acid, 5 parts of amine hydroxybenzenes, after stirrer for mixing is even, by the twin screw extruder melting mixing, make polypropylene/micro-calcium carbonate organic matter master batch, twin screw extruder is respectively distinguished temperature: district's temperature: 190 ℃, two district's temperature: 220 ℃, three district's temperature: 230 ℃, four district's temperature: 230 ℃, five district's temperature: 235 ℃, six district's temperature: 230 ℃, the twin screw rotating speed is 600r/min.
2) carry out froth breaking with list-twin screw extruder one one-step defoaming method
With 100 parts by weight ratio, 2 parts, 0.5 part of organic matter master batch, AC whipping agent, antioxidant 300 stirrer for mixing evenly after, add in the single screw extrusion machine and foam.After extruding, material carries out froth breaking in the twin screw extruder without cooling off directly to enter from the single screw extrusion machine head, through the melting mixing extruding pelletization, and the polypropylene-base matrix material behind the bubble that is eliminated.Wherein, single-screw machine tube temperature: district's temperature: 190 ℃, two district's temperature: 200 ℃, three district's temperature: 220 ℃, four district's temperature: 240 ℃, five district's temperature: 240 ℃, single-screw machine head temperature: 220 ℃, single screw speed is 650r/min, and single-screw machine head pressure is reduced to 130bar; Twin screw extruder is respectively distinguished temperature: district's temperature: 190 ℃, two district's temperature: 200 ℃, three district's temperature: 210 ℃, four district's temperature: 220 ℃, five district's temperature: 230 ℃, six district's temperature: 220 ℃, the twin screw rotating speed is 1000r/min.
Embodiment 4
1) preparation polypropylene/stuffing organic matter master batch
Polypropylene and nano-calcium carbonate were mixed in 100: 18 by weight percentage, in per 100 parts of polypropylene/nano-calcium carbonate calcium compounds, add 0.6 part of oxidation inhibitor 268 again, 3 parts of silane, 2.5 part erucicamide, after stirrer for mixing is even, by the twin screw extruder melting mixing, make polypropylene/nano-calcium carbonate organic matter master batch, twin screw extruder is respectively distinguished temperature: district's temperature: 190 ℃, two district's temperature: 210 ℃, three district's temperature: 215 ℃, four district's temperature: 220 ℃, five district's temperature: 230 ℃, six district's temperature: 220 ℃, the twin screw rotating speed is 750r/min.
2) carry out froth breaking with list-twin screw extruder one one-step defoaming method
With 100 parts by weight ratio, 3.5 parts, 0.6 part in organic matter master batch, AC whipping agent, oxidation inhibitor 268 stirrer for mixing evenly after, add in the single screw extrusion machine and foam.After extruding, material carries out froth breaking in the twin screw extruder without cooling off directly to enter from the single screw extrusion machine head, through the melting mixing extruding pelletization, and the polypropylene-base matrix material behind the bubble that is eliminated.Wherein, single-screw machine tube temperature: district's temperature: 190 ℃, two district's temperature: 220 ℃, three district's temperature: 230 ℃, four district's temperature: 230 ℃, five district's temperature: 225 ℃, single-screw machine head temperature: 215 ℃, single screw speed is 1200r/min, and single-screw machine head pressure is reduced to 200bar; Twin screw extruder is respectively distinguished temperature: district's temperature: 190 ℃, two district's temperature: 195 ℃, three district's temperature: 205 ℃, four district's temperature: 210 ℃, five district's temperature: 220 ℃, six district's temperature: 230 ℃, the twin screw rotating speed is 1200r/min.
Embodiment 5
1) preparation polypropylene/stuffing organic matter master batch
Polypropylene and nano-sized magnesium hydroxide were mixed in 100: 20 by weight percentage, in per 100 parts of polypropylene/nano-sized magnesium hydroxide mixture, add 0.4 part of antioxidant 1010 again, 2.5 part stearic acid, 1 part of alpha-methyl styrene, after stirrer for mixing is even, by melting mixing in the twin screw extruder, make polypropylene/nano-sized magnesium hydroxide organic matter master batch, twin screw extruder is respectively distinguished temperature: district's temperature: 185 ℃, two district's temperature: 195 ℃, three district's temperature: 220 ℃, four district's temperature: 225 ℃, five district's temperature: 240 ℃, six district's temperature: 235 ℃, the twin screw rotating speed is 700r/min.
2) carry out froth breaking with list-twin screw extruder one one-step defoaming method
With 100 parts by weight ratio, 1 part, 0.5 part of organic matter master batch, AC whipping agent, antioxidant 1010 stirrer for mixing evenly after, add in the single screw extrusion machine and foam.After extruding, material carries out froth breaking in the twin screw extruder without cooling off directly to enter from the single screw extrusion machine head, through the melting mixing extruding pelletization, and the polypropylene-base matrix material behind the bubble that is eliminated.Wherein, single-screw machine tube temperature: district's temperature: 185 ℃, two district's temperature: 190 ℃, three district's temperature: 220 ℃, four district's temperature: 225 ℃, five district's temperature: 210 ℃, single-screw machine head temperature: 205 ℃, single screw speed is 900r/min, and single-screw machine head pressure is reduced to 65bar; Twin screw extruder is respectively distinguished temperature: district's temperature: 170 ℃, two district's temperature: 185 ℃, three district's temperature: 195 ℃, four district's temperature: 205 ℃, five district's temperature: 210 ℃, six district's temperature: 205 ℃, the twin screw rotating speed is 1200r/min.
Embodiment 6
1) preparation polypropylene/stuffing organic matter master batch
With polypropylene and nano-calcium carbonate percentage composition mixing in 120: 35 by weight, in per 100 parts of polypropylene/nano-calcium carbonate calcium compounds, add 0.1 part of antioxidant 2246 again, 1 part of aluminic acid ester, 2.5 part whiteruss, after stirrer for mixing is even, by the twin screw extruder melting mixing, make polypropylene/nano-calcium carbonate organic matter master batch, twin screw extruder is respectively distinguished temperature: district's temperature: 180 ℃, two district's temperature: 200 ℃, three district's temperature: 210 ℃, four district's temperature: 230 ℃, five district's temperature: 230 ℃, six district's temperature: 240 ℃, the twin screw rotating speed is 1200r/min.；
2) carry out froth breaking with list-twin screw extruder one one-step defoaming method
With 100 parts by weight ratio, 2.5 parts, 0.1 part of organic matter master batch, AC whipping agent, antioxidant 2246 stirrer for mixing evenly after, add in the single screw extrusion machine and foam.After extruding, material carries out froth breaking in the twin screw extruder without cooling off directly to enter from the single screw extrusion machine head, through the melting mixing extruding pelletization, and the polypropylene-base matrix material behind the bubble that is eliminated.Wherein, single-screw machine tube temperature: district's temperature: 190 ℃, two district's temperature: 215 ℃, three district's temperature: 220 ℃, four district's temperature: 240 ℃, five district's temperature: 220 ℃, single-screw machine head temperature: 210 ℃, single screw speed is 800r/min, and single-screw machine head pressure is reduced to 150bar; Twin screw extruder is respectively distinguished temperature: district's temperature: 190 ℃, two district's temperature: 200 ℃, three district's temperature: 210 ℃, four district's temperature: 220 ℃, five district's temperature: 230 ℃, six district's temperature: 240 ℃, the twin screw rotating speed is 1000r/min.
7) preparation polypropylene/stuffing organic matter master batch
Homo-polypropylene and nanometer butadiene-styrene-vinyl rubber powder were mixed in 100: 8 by weight percentage, in per 100 parts of polypropylene/nano-sized magnesium hydroxide mixture, add 0.1 part of antioxidant 1010 again, 3 parts of aluminic acid esters, 2.5 part white mineral oil, after stirrer for mixing is even, by the twin screw extruder melting mixing, make polypropylene/nanometer butadiene-styrene-vinyl rubber organic matter master batch, twin screw extruder is respectively distinguished temperature: district's temperature: 170 ℃, two district's temperature: 180 ℃, three district's temperature: 190 ℃, four district's temperature: 195 ℃, five district's temperature: 205 ℃, six district's temperature: 210 ℃, the twin screw rotating speed is 100r/min.
2) carry out froth breaking with list-twin screw extruder one one-step defoaming method
With 100 parts by weight ratio, 0.3 part, 0.1 part of organic matter master batch, AC whipping agent, antioxidant 1010 stirrer for mixing evenly after, add in the single screw extrusion machine and foam.After extruding, material carries out froth breaking in the twin screw extruder without cooling off directly to enter from the single screw extrusion machine head, through the melting mixing extruding pelletization, and the polypropylene-base matrix material behind the bubble that is eliminated.Wherein, single-screw machine tube temperature: district's temperature: 175 ℃, two district's temperature: 180 ℃, three district's temperature: 190 ℃, four district's temperature: 195 ℃, five district's temperature: 185 ℃, single-screw machine head temperature: 185 ℃, single screw speed is 200r/min, and single-screw machine head pressure is reduced to 70bar; Twin screw extruder is respectively distinguished temperature: district's temperature: 170 ℃, two district's temperature: 175 ℃, three district's temperature: 180 ℃, four district's temperature: 195 ℃, five district's temperature: 210 ℃, six district's temperature: 220 ℃, the twin screw rotating speed is 500r/min.
Get the polymer matrix composite of final preparation among the embodiment 1-7 and the pure resin matrix of experiment usefulness and make tensile bars and impact batten on injection moulding machine, press GB/T 1040-92 standard testing tensile strength, specimen size is 150 * 10 * 4; Press ISO 179 standard testing shock strengths, specimen size is 80 * 10 * 4, notch depth 2mm;
The rerum natura numerical tabular of the polymer based nanocomposites for preparing among table 1 resin matrix and the routine 1-6
Figure G2009100932823D00091
The rerum natura numerical tabular of the polymer based nanocomposites of preparation in table 2 resin matrix and the example 7
Figure G2009100932823D00092

Claims (1)

1. the in-situ bubble stretching one-step defoaming legal system is equipped with the method for polymer matrix composite, it is characterized in that, may further comprise the steps:
1) preparation polypropylene and stuffing organic matter master batch
With polypropylene and filler by weight 3: 100-35: 100 mix, and add 0.1-1 part oxidation inhibitor again in per 100 parts of polypropylene and filler mixture, 0.1-5 part expanding material also has 0.1-5 part processing aid; After stirrer for mixing is even, by the twin screw extruder melting mixing, make polypropylene and stuffing organic matter master batch, twin screw extruder is respectively distinguished temperature: district's temperature a: 170-190 ℃, two district's temperature: 180-220 ℃, three district's temperature: 190-230 ℃, four district's temperature: 180-230 ℃, five district's temperature: 190-240 ℃, six district's temperature: 190-240 ℃, the twin screw rotating speed is 30-1200r/min;
2) carry out froth breaking with list-twin screw extruder one one-step defoaming method
70-120 part, 0.01-3.5 part, 0.1-1 part add in the single screw extrusion machine and foam after stirrer for mixing is even by weight ratio with organic matter master batch, whipping agent, oxidation inhibitor; After extruding, material carries out froth breaking in the twin screw extruder without cooling off directly to enter from the single screw extrusion machine head, through the melting mixing extruding pelletization, and the polypropylene-base matrix material behind the bubble that is eliminated; Wherein, single-screw machine tube temperature: district's temperature a: 170-190 ℃, two district's temperature: 180-220 ℃, three district's temperature: 180-230 ℃, four district's temperature: 190-240 ℃, five district's temperature: 190-240 ℃, single-screw machine head temperature: 180-220 ℃, single screw speed is 30-1200r/min, and single-screw machine head pressure is reduced to 30-200bar; Twin screw extruder is respectively distinguished temperature: district's temperature a: 160-190 ℃, two district's temperature: 165-205 ℃, three district's temperature: 170-210 ℃, four district's temperature: 180-220 ℃, five district's temperature: 180-230 ℃, six district's temperature: 190-240 ℃, the twin screw rotating speed is 30-1200r/min.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103454297B (en) * 2013-09-02 2016-03-30 武汉钢铁(集团)公司 Identify that masking liquid bubble causes the method for steel plate coating defect
CN112876842A (en) * 2021-01-15 2021-06-01 宿迁联盛科技股份有限公司 Preparation method of anti-aging polymer composite material with enhanced core-shell structure
CN113150360A (en) * 2021-05-18 2021-07-23 四川大学 Method for promoting dispersion of nano filler by utilizing stretching effect of pore wall of polymer foam material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4045403A (en) * 1972-07-19 1977-08-30 General Electric Company Method of compounding thermo-plastic polymeric materials and fillers
CN100346951C (en) * 2002-09-27 2007-11-07 北京化工大学 Disperseing process of abio-particle in polymers
CN100396727C (en) * 2005-09-06 2008-06-25 北京化工大学 Method for promoting property of nano calcium carbonate and polypropylene composite material

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103454297B (en) * 2013-09-02 2016-03-30 武汉钢铁(集团)公司 Identify that masking liquid bubble causes the method for steel plate coating defect
CN112876842A (en) * 2021-01-15 2021-06-01 宿迁联盛科技股份有限公司 Preparation method of anti-aging polymer composite material with enhanced core-shell structure
CN113150360A (en) * 2021-05-18 2021-07-23 四川大学 Method for promoting dispersion of nano filler by utilizing stretching effect of pore wall of polymer foam material

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