CN101462333B - Method for preparing polystyrol thick sheet material - Google Patents

Method for preparing polystyrol thick sheet material Download PDF

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Publication number
CN101462333B
CN101462333B CN200910076841XA CN200910076841A CN101462333B CN 101462333 B CN101462333 B CN 101462333B CN 200910076841X A CN200910076841X A CN 200910076841XA CN 200910076841 A CN200910076841 A CN 200910076841A CN 101462333 B CN101462333 B CN 101462333B
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plastic
sheet material
temperature
polystyrene
pressure
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CN101462333A (en
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温汉东
熊泽林
陈明炜
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Zhonghao Chenguang Research Institute of Chemical Industry Co Ltd
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Zhonghao Chenguang Research Institute of Chemical Industry Co Ltd
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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
    • B29C48/92—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
    • 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
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/397—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using a single screw
    • 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
    • B29C2948/92514—Pressure
    • 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
    • B29C2948/92895—Barrel or housing
    • 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
    • B29C2948/92904—Die; Nozzle zone

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)
  • Extrusion Moulding Of Plastics Or The Like (AREA)

Abstract

The invention provides a method for preparing a thick polystyrene board, which comprises the following steps: firstly extruding and plasticizing heat-resistant polystyrene resin by an extruder at a temperature of between 140 and 165 DEG C; then feeding the polystyrene resin into a die cavity of a die at the pressure of 6 to 12MPa; and finally pressing and forming the thick polystyrene board in the die cavity of the die. The method adopts processes of extruding, pressing and forming to form the thick polystyrene board, is favorable for discharge of volatile components in a plastic fused body, and avoids a molecular chain segment of a high polymer generating chain scission reaction because the plastic fused body is in a high temperature state for a long time to reduce product performance. The preparation method can produce an extra thick polystyrene plastic board of a large-sized medium lens material.

Description

A kind of preparation method of polystyrol thick sheet material
Technical field
The present invention relates to a kind of preparation method of polystyrol thick sheet material, belong to the plastic shaping manufacture field.
Background technology
Polystyrene plastics is water white pearl or granular non-crystalline type thermoplastic resin, colourless, tasteless, odorless, relative density 1.05, use under 60～75 ℃ and underload, have higher rigidity, case hardness and glossiness, dimensional stability is good, coloring, decorative surface, radiation resistance are good, good electrical property, especially high-frequency insulation is functional, and arc resistance is good.The polystyrene processing and forming is good, can adopt processing method moulding such as injection, extrusion molding, blowing, foaming, thermoforming, bonding, coating, welding, machined, printing.Be widely used in electric, instrument, optical lens electricity electric insulating film frequently, high-frequency insulation material etc.
At present, polystyrene extensively adopts radical polymerization to produce.Its polymerization has: polymerisation in bulk, polymerisation in solution, suspension polymerisation and emulsion polymerisation.The polymerization methods difference, its material property and processing characteristics have very big-difference, and polymerisation in bulk is simple, and gained resin transparent and electrical property are good, but because exothermic reaction and product molecular weight distribution are very wide, cause difference in material properties bigger.In order to improve operation and heat transfer conditions, the normal tandem solution polymerization process that adopts is produced, but can causing the chain transmission, solution makes molecular weight and molecular weight, though most of problem has been avoided in suspension polymerisation, but also there is polymer suspension agent pollution problems, the component of emulsion polymerisation is many, and remaining in influences the transparency and electrical property in the resin, seldom adopts.
The structures shape performance, owing to contain tertiary carbon (asymmetric carbon) atom in the polystyrene strand, that the structure of polymer has is random, three kinds of isotactics, a rule, its performance has remarkable difference, and is as shown in table 1.
Table 1
Stereospecificity Polymerization catalyst or initator Solid structure T g，℃ T m，℃ Crystalline rate
Random polystyrene Organic peroxide or azo-compound, lithium alkylide Amorphous 100 -- --
Isotactic polyphenylacetylene ?TiCl 3/AIR 3 Crystallization shape 100 220 Slowly
Syndiotactic polytyrene Single Site catalyst Crystallization shape 100 260～270 Hurry up
Molecular weight and distribution thereof are the important parameters of polystyrene resin.Molecular weight is lower than 50,000, and the intensity of polystyrene is very low; Along with molecular weight is increased to 100,000, intensity improves very fast; Molecular weight is greater than after 100,000, and intensity increases slowly.
Residual monomer content is bigger to the softening temperature influence of polymer in the polystyrene, and content of monomer is increased at 5% o'clock from zero, and softening temperature can reduce by 30 ℃.Simultaneously, monomer can volatilize when converted products, and the gas that is produced can distort and make goods produce defective, as crazing, spot.Therefore should reduce styrene monomer content as possible in the mill, improve hear resistance.
The excellent optical performance of polystyrene has the high transmittance of visible light all wavelengths and its high index of refraction (1.592), makes it have extra high " brightness ".
The electrical property of polystyrene is fine.Frequency is from 60～106Hz, and is very little to the influence of dielectric constant and dielectric loss angle tangent, and its value is respectively 2.45～2.65 and 1 * 10 -4～2 * 10 -4
The hot property characteristics of polystyrene are low-down heat conductivity (being about 0.13W/ (mK)) and lower softening temperature.In addition, its specific heat capacity is lower, and heat energy required during heating and cooling is also lower.
As the polystyrene plastics of di-lens is that di-lens tightens the core devices in the development task, from what medium tightened field system related parameter and specification requirement is arranged, and other material still can't be made lens by the substituted polystyrene plastics at present.Its reason is that the polystyrene plastics electrical property is good, and lustrous surface is good.Machining and processability are good, and shrinkage factor is very low in the forming process, and there are the too small problem of dimensions equally in product size good stability, the substitute of other material.Simultaneously, if adopt bonding to reach the used thickness requirement of huge media lens material, will cause serviceability not reach re-set target, especially interlaminar bonding, because adhesive surface material homogeneity, the density variation that can't eliminate, will cause microwave by the time refraction and diffuse reflection, produce error.Therefore develop the special thick polystyrene plastics sheet material of huge media lens material, satisfy the demand of military project high-tech product, seem particularly necessary and urgent.It is for the modernization level and the scientific and technological content that promote military electronics, makes the high-new tip direction development of military electronics to " high-performance, multi-functional, miniaturization ", thereby adapts to the requirement of modern war, has far-reaching society and national defence meaning.
At present, both at home and abroad mostly manufacturer is the polystyrene plastics sheet material of some stock sizes, performance, does not also see the relevant report of big molded dimension product, and polystyrene plastics sheet material mostly is extrusion board, and its sheet metal thickness is all less than 20mm.
Production method for plastic plate generally has extrusion molding, laminating and direct shaping method to suppress.Extrusion molding is the continuous production processes method, and it is to utilize plastic extruder plasticizing feed, the moulding of sheet material head, three-roller calendar press polish typing and form sheet material through the traction cutting again; Characteristics such as it is simple to have equipment, and cost of investment is low, and production operation is easy to control; But, since the processing technology of extrusion molding own, the difficult thicker sheet material of thickness of producing, and general thickness all below 20mm, can not satisfy the thickness requirement of p-poly-phenyl ethylene plate.Same laminating is to utilize the plastic sheet of rolling process or extrusion molding production through being layering, outside having, do not heat extrusion forming under the situation of frame mould, be suitable for minimum material of processing temperature state current downflow or thickness materials with smaller, such as: polyvinyl-chloride plate material, epoxy glass fabric sheet material etc., for polystyrene plates, just can't finalize the design at all.
Directly shaping method to suppress is with plastic grain or utilizes extrusion molding and sheet material that rolling process is produced directly adds in the mould; heating pressurization cooling and shaping forms then; because sheet metal thickness is up to 200mm, the thermal conductivity factor of plastic material is extremely low again, and (thermal conductivity factor of polystyrene is 0.101～0.156Wm -1K -1), only for steel 2～3.3% (thermal conductivity factor of steel is 46.7Wm -1K -1), compare with steel, be exactly heat-insulating material simply, make mold heat pass to plastics inner, and reach process stipulation temperature required time by the die cavity wall, and again from high temperature drop to can the demoulding the required time of temperature, with regard to length very, plastics are under the high temperature for a long time, and chain-breaking reaction will take place strand, molecular weight sharply descends, and causes material property to descend; Simultaneously, because heat is inwardly to pass to plastics inner by mold cavity wall, so, the plastics that link to each other with mold cavity wall will at first obtain heat and reach the process stipulation temperature, become melt state, with be mixed between tablet and plastic material in volatile ingredient be enclosed in material internal, produce bubble, cause fault in material, can't obtain instructions for use.
Mould of plastics is the required instrument of product of the various materials of moulding, difformity and size when producing, mould for plastics is because moulding material, article construction, output, forming method is different with use equipment and different, after plastics variety and contour machining equipment thereof are determined, the quality of plastic products quality and the height of production efficiency, the mould factor accounts for 80%.Therefore, the quality of die quality also will directly have influence on the quality of board quality, and for mould, influence factor mainly contains two aspects: the one, and the structure of mould, the 2nd, the temperature control and the control accuracy thereof of mould.
According to above-mentioned analysis, above contour machining procedure is difficult to reach the specification requirement of huge media lens material p-poly-phenyl ethylene plate, we just must seek a kind of board contour machining procedure, could satisfy the specification requirement of huge media lens material p-poly-phenyl ethylene plate.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of polystyrol thick sheet material, this process using is extruded compression moulding technology, can guarantee plastic plate size and internal performance, guarantee the inner pore-free of plastic plate, the plate face is smooth and material performance uniformity everywhere, can the special thick polystyrene plastics sheet material of production huge media lens material.
In order to realize the object of the invention, the preparation method of a kind of polystyrol thick sheet material of the present invention, it comprises the steps:
Earlier with heat-resisting polystyrene resin under 140～165 ℃ through the extruder extrusion plasticizing, the pressure with 6～12MPa enters mold cavity then, is pressed in mold cavity at last.
--extrusion plasticizing--charge into die cavity--pressurization cooling--post processing that concrete process route of the present invention is: raw material.
It is raw material that the present invention selects heat-resisting polystyrene resin for use, is random polystyrene, and MFR is 2～3g/10min, and its heat distortion temperature is greater than 84 ℃, and softening point is greater than 100 ℃, and hot strength is greater than 50MPa.
Because the selected heat-resisting polystyrene resin of the present invention has molecular weight preferably, it is minimum to contain additive, does not contain mineral oil or other flow promortor; Heat stable resin generally only contains releasing agent or extrusion aid such as zinc stearate or stearic acid.Simultaneously, this resin also has less melt index (MI), and heat distortion temperature is higher, and physical property is better, is more suitable for the compression moulding of sheet material.
The process conditions of polystyrene resin extrusion plasticizing of the present invention are: adopt the gradation type single screw extrusion machine, extrusion temperature is 140～165 ℃, extrusion pressure 6～12MPa.
Polystyrol thick sheet material compression moulding process of the present invention is divided into three phases such as the preparation, compression forming (melt mold filling, compacting, the demoulding), plastic post processing of melt material, in the compression moulding process, mold temperature is controlled at 90～110 ℃, just near the softening point of polystyrene resin, avoid resin to be in high temperature for a long time and cause degraded, have deformability again, help cooling and shrink feed supplement, molding pressure control 7～11MPa guarantees that material does not contract and plate surface is smooth; The single-piece clamp time was controlled at 80～100 minutes, did not deform after the depanning of assurance sheet material and was advisable.
Molding temperature is 90～110 ℃ during compression moulding of the present invention.Under 6～12MPa pressure, charge into mold cavity through the melt material that plastifies by extruder, by entering the lower mold cavity of temperature in the high temperature extruder, contact with die surface with regard to beginning cooling and form surperficial duricrust, inside is solidified after a while, is shunk, bears tension because of limited by shell.There is residual compressive stress on plastic top layer after the curing, and there is residual tension inside, and the existence of these residual stress warpage, cracking and intensity decline occur after making plastic parts moulding.Each plastics all has its molding temperature scope that is fit to, especially for the special thick plastic plate of thickness up to 200mm.Molding temperature is too high, can cause degrading with the material of mold cavity contact portion, and products surface quality is descended, and causes material surface and inherent quality to differ; Molding temperature is low excessively, the too early surperficial duricrust that forms, can stop the volatile ingredient of melt inside to discharge, cause bubble, swelling, warpage, cracking occurring after the plastic demoulding, therefore, material temperature difference in the die cavity should be reduced guaranteeing that fused materials can fully be full of under the prerequisite of mold cavity as far as possible, high-quality plastic product could be obtained.
Molding pressure is 7～11MPa during compression moulding, when being meant compression forming on direction of exerting pressure upper cavity unit are suffered pressure.Its effect is to make the pressure that the low molecular weight volatile thing is produced in plastics density, promotion Flow of Goods and Materials, the balance die cavity.High molding pressure increases plastic density, and molding shrinkage reduces, and increases Flow of Goods and Materials, overcomes swelling, prevents to produce bubble; But also can increase the plastic internal residual stress.So should select suitable molding pressure according to material property, cooperation molding temperature, just can obtain the plastic product of high-quality.
Clamp time is 80～100 minutes during compression moulding, and it is meant the fully closed back of mould between the mold open, and material is heated in mould time of cooling curing.Its effect is abundant cooling curing typing of time, reaches the material mechanical performance of expection or specific using property data.The shape of clamp time and plastic type and composition, plastic is relevant with multiple factors such as thickness, mould structure, molding temperature and molding pressures.Improve mold temperature, clamp time extends thereupon, and plastic thickness is big, needs clamp time longer.When molding temperature and molding pressure one timing, clamp time just becomes the key factor of decision plastic part quality.Clamp time is short, and plastic is inner not to be solidified fully, is prone to warpage, swelling, shrinkage cavity and bad mechanical property; Clamp time is long, can increase the residual stress of plastic inside and cracks.Suitable clamp time helps improving every performance, especially hear resistance, electrical insulating property and the intensity of plastic.
Adopt the key technical indexes of polystyrol thick sheet material of technology of the present invention preparation as follows:
Hot strength 〉=46Mpa;
Dielectric constant (1MHz)＜2.6;
95～100 ℃ of softening points (dimension card);
Outward appearance: plasticizing is even, and surfacing is smooth, water white transparency, flawless and impurity;
Blank dimension: tentative for ≠ 200 * 800 (more than) * 800 (more than).
The present invention utilize plastic extruder directly to mold cavity provide temperature evenly, the plastic melt of flow and pressure stability, constantly be full of mold cavity, because after plastic melt enters mold cavity, pressure is vanishing almost, help monomer component and volatile ingredient discharge in the plastic melt, avoid bubble occurring in the plate forming process; On the other hand,, come from the extrusion pressure of extruder along with melt constantly is full of mold cavity, continuous compacting plastic melt, and set up cavity pressure, this extrusion pressure can reach more than the 10MPa.Then, cools down curing molding under the pressure of press.
The present invention adopts and extrudes press technology for shaping moulding polystyrol thick sheet material, help the discharge of volatile ingredient in the plastic melt, avoid plastic melt to be in the condition of high temperature for a long time and cause high-polymer molecular chain segment generation chain-breaking reaction, reduce properties of product.But the special thick polystyrene plastics sheet material of preparation technology's production huge media lens material of the present invention.
Description of drawings
Fig. 1 is preparation technology's flow chart of polystyrol thick sheet material of the present invention.
The specific embodiment
Following examples are used to illustrate the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
As shown in Figure 1, the polystyrol thick sheet material preparation technology of present embodiment is as follows:
Selecting heat-resisting polystyrene resin for use is raw material (MFR is 2.2g/10min, and its heat distortion temperature reaches 86 ℃, and softening point reaches 104 ℃, and hot strength reaches 54MPa), be dried earlier stand-by, 80 ℃ of temperature, the time was greater than 6 hours.
Then resin is added the gradation type single screw extrusion machine, each section of extruder temperature is controlled at 140,165,155 ℃ respectively, extrusion pressure 7 ± 1MPa, with 60 rev/mins of feed in mould of screw speed, 100 ± 10 ℃ of mold system temperature treat that material is full of in the mould, and extruder stops, disconnect between extruder and the mold system, and the closed mould charging aperture.
Press is exerted pressure to sheet material, and under 10MPa pressure, the segmentation thermoisopleth descends and carries out cooling and shaping.Be incubated 15 minutes respectively at 80 ℃ and 60 ℃, pressurize is 90 minutes altogether.In order to control temperature better, around framed, increased the temperature control system that is used alternatingly by steam and cooling water.
After arriving cool time, the sheet material depanning, and sheet material is put into by steam-heated water carried out post processing rapidly, water temperature is controlled at 95 ± 2 ℃, and the processing time was greater than 12 hours.
Embodiment 2
As shown in Figure 1, the polystyrol thick sheet material preparation technology of present embodiment is as follows:
Selecting heat-resisting polystyrene resin for use is raw material (model: GP-303, MFR are 2.1g/10min, and its heat distortion temperature reaches 88 ℃, and softening point reaches 105 ℃, and hot strength reaches 53MPa), be dried earlier stand-by, 80 ℃ of temperature, the time was greater than 6 hours.
Then resin is added the gradation type single screw extrusion machine, each section of extruder temperature is controlled at 145,160,150 ℃ respectively, extrusion pressure 10 ± 1MPa, with 80 rev/mins of feed in mould of screw speed, 95 ± 10 ℃ of mold system temperature treat that material is full of in the mould, and extruder stops, disconnect between extruder and the mold system, and the closed mould charging aperture.
Press is exerted pressure to sheet material, and under 8MPa pressure, the segmentation thermoisopleth descends and carries out cooling and shaping.Be incubated 15 minutes respectively at 85 ℃ and 60 ℃, pressurize is 100 minutes altogether.In order to control temperature better, around framed, increased the temperature control system that is used alternatingly by steam and cooling water.
After arriving cool time, the sheet material depanning, and sheet material is put into by steam-heated water carried out post processing rapidly, water temperature is controlled at 95 ± 2 ℃, and the processing time was greater than 12 hours.
Though above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.

Claims (2)

1. the preparation method of a polystyrol thick sheet material is characterized in that, it comprises the steps:
Be 2～3g/10min with MFR earlier, heat distortion temperature is greater than 84 ℃, softening point is greater than 100 ℃, and hot strength is greater than the heat-resisting random polystyrene resin of 50Mpa, under 140～165 ℃ through the extruder extrusion plasticizing, pressure with 6～12MPa enters mold cavity then, be pressed in mold cavity at last, during described compression moulding, mold temperature is controlled at 90～110 ℃, molding pressure is controlled at 7～11Mpa, and clamp time was controlled at 80～100 minutes.
2. the preparation method of polystyrol thick sheet material according to claim 1 is characterized in that, the process conditions of described extrusion plasticizing are: adopt the gradation type single screw extrusion machine, extrusion pressure 6～12MPa.
CN200910076841XA 2009-01-22 2009-01-22 Method for preparing polystyrol thick sheet material Active CN101462333B (en)

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