CN109760257A - A kind of preparation method of long fiber reinforcement polyvinyl chloride microporous foam product - Google Patents
A kind of preparation method of long fiber reinforcement polyvinyl chloride microporous foam product Download PDFInfo
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- CN109760257A CN109760257A CN201811513326.9A CN201811513326A CN109760257A CN 109760257 A CN109760257 A CN 109760257A CN 201811513326 A CN201811513326 A CN 201811513326A CN 109760257 A CN109760257 A CN 109760257A
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Abstract
The invention belongs to foaming macromolecular product technique fields, more particularly to a kind of preparation method of long fiber reinforcement polyvinyl chloride microporous foam product, pass through mixing, it squeezes out, the processing steps such as injection molding carry out foaming product preparation, simultaneously, select specific raw material: Corvic, auxiliary agent, long fibre ensures the performance of product, and in extrusion process, long fibre and supercritical fluid substep are added, promote the abundant combination of long fibre and matrix resin, promote the performance of product, the present invention can reduce the degradation and long stapled fracture of polyvinyl chloride in process, improve long fibre dispersion effect, achieve the purpose that improve product properties on the basis of energy conservation and environmental protection, and this method is easy to be promoted in the industrial production, with wide prospects for commercial application.
Description
Technical field
The invention belongs to foaming macromolecular product technique fields, and in particular to a kind of long fiber reinforcement polyvinyl chloride micropore hair
The preparation method of brewage.
Background technique
Polyvinyl chloride microporous foam product refer to it is a kind of using polyvinyl chloride as substrate and there are the micro- of numerous bubbles inside it
Hole product.Polyvinyl chloride microporous foam product has many advantages, such as that light, specific strength is high, cushion performance is good, in daily necessities, traffic work
The fields such as tool, construction material are widely used.For example, polyvinyl chloride microporous foam system can be used for instrument in automotive field
Dash board epidermis, seat leather, article shading curtain etc. are the second largest plastics of automobile.
Currently, the conventional production process of production polyvinyl chloride microporous foam product is produced using chemical foaming agent,
Since the decomposition temperature of chemical foaming agent is generally at 200 DEG C or so, and polyvinyl chloride is easy degradation at this temperature, so
Need to add the heat stabilizer for reducing polyvinyl chloride degradation in production process, addition makes chemical foaming agent at a lower temperature again
That decomposes facilitates agent.This production method formula is complicated, and technical process is not easily controlled, and production efficiency is low.In addition, using chemistry
It is easy to appear when foaming in product there are foaming agent residue, chemical foaming agent pollution corrosion molding equipment and product is subsequent makes
The problems such as used time is limited by environmental requirement.Therefore, it is received increasingly using physical blowing method to prepare polymeric foamable material
More concerns and popularization.Wherein, supercritical carbon dioxide have when being used as physical blowing agent dissolubility is strong, diffusivity is good,
It is safe and non-toxic, environmentally protective, chemical stability is high, no solvent residue, it is easily controllable, reduce processing temperature the advantages that.In addition, super
The microporous foam product cell density with higher that critical carbon dioxide foaming is prepared, can get microstructure and macroscopic view
The microcellular plastics of function admirable.Therefore, it is used widely in polymer foaming field, becomes current research heat
Point.
As the patent of publication number 102321268A discloses a kind of use carbon dioxide foaming agent production polyvinyl chloride hard
The method of foamed plastics, this method squeeze out hair by tandem extruder and static mixer using carbon dioxide combined foaming agent
Bubble, is made polyvinyl chloride hard foamed plastics.
But due to having a large amount of abscesses inside microporous foam product, so that still there is intensity when it is used as structural fabrication
The inadequate defect with modulus.
Summary of the invention
In view of the above problems, the present invention provides a kind of length for making up the defects of foaming product intensity is low, modulus is few
The preparation method of fiber reinforcement polyvinyl chloride microporous foam product.
To achieve the goals above, the invention adopts the following technical scheme:
A kind of preparation method of long fiber reinforcement polyvinyl chloride microporous foam product, includes the following steps:
(1) mixing: Corvic, auxiliary agent are added in high-speed mixer and mix to obtain premix；
(2) it squeezes out: premix is added in extruder barrel by drawing-in device, it is first equal in barrel leading portion fusion plastification
It is even, then surface treated long fibre is fed in barrel middle section side feed mouth, blend melt is formed, high-pressure metering pump is then passed through
Supercritical fluid is injected in extruder gas injection port, last blend melt is depressured foaming after passing through extruder die head, obtains expanded particle；
(3) it is molded: expanded particle is added in injection molding machine, surpassed by high-pressure metering pump in the gas injection port injection of injection molding machine and faced
Boundary's fluid, uniformly injection mold is foamed, is cooled down melting mixing afterwards, obtains foaming product.
The present invention divides sequence to add supercritical fluid, in addition to having conventional physical step by step in the preparation process of foaming product
Outside the effect of pore-creating, it is often more important that, it is squeezed out during extruding pelletization using supercritical fluid auxiliary, processing temperature can be reduced
It spends to reduce the degradation of polyvinyl chloride in process, meanwhile, good long fibre point can be obtained at low shear rates
Effect is dissipated, so that foaming product is with longer fibre length (long fibre is avoided to be broken in process) and higher
Mechanical property.That is the effect of supercritical fluid has been no longer limited in physics pore-creating, is more as a kind of auxiliary material
Material helps stable resin matrix, keeps it not degradable, and fiber can be helped preferably to be combined with resin matrix.
Preferably, the product includes the component of following parts by weight: Corvic: 30-50 parts, auxiliary agent:
23.3-83 parts, long fibre: 10-45 parts.
Further preferably, the long fibre includes one of glass fibre, carbon fiber, aramid fiber or a variety of.
Further preferably, the long fibre is continuous fiber.
Further preferably, the long stapled length is more than 10mm.
Further preferably, the reagent that the long stapled surface treatment uses includes organosiloxane coupling agent, titanate esters
One of coupling agent, aluminate coupling agent are a variety of.
The present invention is special in Corvic to be added to continuous fiber, compared with general fibre, continuous fiber
It with continuity, is equivalent to and forms " reinforcing rib " in resin matrix, can more be obviously improved the mechanics of resin matrix
Performance, and then guarantee last product intensity with higher, expand application field.And use coupling agent in advance to long fibre into
Row surface treatment, can effectively promote dispersion effect of the long fibre in resin matrix.
Preferably, the auxiliary agent is made of the component of following parts by weight: plasticizer: 20-50 parts, antioxidant:
0.3-3 parts, fire retardant: 0.5-5 parts, heat-resisting stabilizing agent: 0.5-10 parts, filler: 2-15 parts, lubricant: 0.1-0.5 parts.
Further preferably, the plasticizer includes that diisooctyl phthalate, epoxidized soybean oil, tri trimellitate are pungent
One of ester, haloflex, HL-918 or a variety of.
Further preferably, the antioxidant includes one of main anti-oxidant 1010, auxiliary antioxidant 168 or two
Kind.
Further preferably, the fire retardant can be HT-103.
Further preferably, the heat-resisting stabilizing agent include one of calcium-zinc composite stabilizing agent, organic tin stabilizer or
Two kinds.
Further preferably, the organic tin stabilizer can be thiol methyl tin DX-181.
Further preferably, the filler include nano barium sulfate, nanometer calcium carbonate, clay, alkali alumina, magnesia,
One of carclazyte, white carbon black are a variety of.The heat resistance and mechanical performance of foaming product can be improved in filler of the invention, and
It can play the role of nucleating agent in foaming process, promote cell nucleation to obtain more uniform foam structure.
Further preferably, the lubricant can be stearic acid 1801.
Preferably, step (2) described extruder includes one of single screw extrusion machine, double screw extruder or two
Kind.
Preferably, step (2) extruder barrel is divided into 5 heated zones, the first section by extruder length
To be 120-140 DEG C close to the temperature of charging extreme direction, the first section, the temperature of remaining 4 sections is 120-180 DEG C.
Preferably, step (2) installs high-pressure solenoid valve and self-locking also between the outlet of high-pressure metering pump and extruder
Formula air injection uni-direction.It is mainly used for the on-off of control injection fluid, and can prevents plastic melt in extruder from flowing backwards entrance
In supercritical fluid transport device.
Preferably, melt pressure is 6-20MPa, die temperature 120-175 in the die head of step (2) described extruder
℃。
Further preferably, the diameter of the mouth mold is 0.5-1.5mm, opens 3-8 hole in mouth mold.
Preferably, the temperature of step (3) described injecting machine material tube is 120-200 DEG C, the injection pressure of injection molding machine is 60-
250MPa, injection speed 50-200mm/s.
Preferably, the time of step (3) described cooling is 10-50s.
Preferably, the injection rate of supercritical fluid is 0.3-5 parts in step (2), step (3).Supercritical fluid
Additional amount must be added in strict accordance with attribute (i.e. product material is different, and additional amount is also different) of product itself, work as fluid
When too high levels, it may result in the stomata to be formed and be adhered, and then the structural strength of product is caused to reduce, when content is too low,
The stomatal frequency of formation is insufficient, and structural strength is inadequate.
Further preferably, step (2) and supercritical fluid described in step (3) include supercritical carbon dioxide, it is overcritical
One or both of nitrogen.
Compared with prior art, the present invention has the advantage that
(1) present invention combines the two preferably, in energy conservation using supercritical fluid to the miscellaneous function of resin, fiber
It enhances product performance on the basis of environmental protection.
(2) of the invention preparation method is simple, is easy to be promoted in the industrial production, and there is wide industry to answer
Use prospect.
(3) long fibre that the present invention adds, compared with being not added with fiber or the common chopped strand of addition, long fiber reinforcement
The intensity and modulus of foaming product significantly improves.
(4) present invention uses supercritical fluid to prepare microporous foam product as foaming agent, safe and non-toxic, environmentally protective,
And be conducive to obtain the microporous foam product of high cell density.
Specific embodiment
The following is specific embodiments of the present invention, and technical scheme of the present invention will be further described, but the present invention is simultaneously
It is not limited to these embodiments.
Long fiber reinforcement polyvinyl chloride microporous foam product, the component including following parts by weight: Corvic:
30-50 parts, auxiliary agent: 23.3-83 parts, long fibre: 10-45 parts；
Its medium-length fibre includes one of glass fibre, carbon fiber, aramid fiber or a variety of, and long fibre is greater than for length
The continuous fiber of 10mm, and with one of organosiloxane coupling agent, titanate coupling agent, aluminate coupling agent or it is a variety of into
The surface treatment of row long fibre；
Wherein auxiliary agent is made of the component of following parts by weight: plasticizer: 20-50 parts, antioxidant: 0.3-3 parts, fire-retardant
Agent: 0.5-5 parts, heat-resisting stabilizing agent: 0.5-10 parts, filler: 2-15 parts, lubricant: 0.1-0.5 parts, plasticizer includes adjacent benzene two
One of formic acid diisodecyl ester, epoxidized soybean oil, trioctyl trimellitate (TOTM), haloflex, HL-918 or a variety of, it is anti-oxidant
Agent includes one or both of main anti-oxidant 1010, auxiliary antioxidant 168, and fire retardant can be HT-103, heat-resisting steady
Determining agent includes one or both of calcium-zinc composite stabilizing agent, organic tin stabilizer, and organic tin stabilizer can be mercaptan
Methyl tin DX-181, filler include nano barium sulfate, nanometer calcium carbonate, clay, alkali alumina, magnesia, carclazyte, white carbon black
One of or it is a variety of, lubricant can be stearic acid 1801.
Embodiment 1
(1) mixing: weighing raw material by the component of said products, by 50 parts of Corvics, 20 parts of phthalic acids two
Isodecyl ester, 5 parts of HL-918 are added in high-speed mixer and mix 2min, and 10 parts of haloflexes, 5 parts of calcium carbonate, 5 parts are then added
Carclazyte, 5 parts of barium sulfate, 0.5 part of antioxidant 1010,0.3 part of auxiliary antioxidant, 168,1.7 parts of calcium zinc stabilizers, 0.1 part of tristearin
Acid 1801 mixes 3 minutes, obtains premix；
(2) it squeezes out: premix being added in twin-screw extruder barrel by drawing-in device, screw speed 80rpm is fed
Doses is 3Kg/h, and the temperature that extruder barrel is arranged is 5 sections, is followed successively by 120 DEG C -130 DEG C -150 DEG C -150 DEG C -150
DEG C, it is first uniform in barrel the first section fusion plastification, then by the 15 parts of roving glass fibers crossed through organosiloxane coupling agent treatment in material
Cylinder third section side feed mouth feeding, forms blend melt, then injects 5 parts in extruder gas injection port by high-pressure metering pump and super faces
Boundary's carbon dioxide, last blend melt are 150 DEG C by temperature, after pressure is the extruder die head of 12MPa, diameter 1mm, are opened
Hole count is that 5 die temperatures are 135 DEG C, and decompression foaming obtains expanded particle；
(3) it is molded: expanded particle is added in injection molding machine, the temperature that injecting machine material tube is arranged is 5 sections, is followed successively by
130 DEG C -150 DEG C -150 DEG C -150 DEG C -150 DEG C, injection molding machine injection pressure is 150MPa, and injection speed 120mm/s passes through height
Press metering pump injection molding machine gas injection port inject 5 parts of supercritical carbon dioxides, melting mixing uniformly afterwards injection mold foamed,
Cooling 15s, obtains foaming product.
Embodiment 2
(1) mixing: weighing raw material by the component of said products, by 50 parts of Corvics, 22.5 parts of phthalic acids
Diisodecyl ester, 3.5 parts of epoxidized soybean oils are added in high-speed mixer and mix 2min, and 10 parts of haloflexes, 5 parts of carbon are then added
Sour calcium, 2.5 parts of magnesia, 1.5 parts of alkali aluminas, 0.5 part of antioxidant 1010,0.2 part of auxiliary antioxidant, 168,1 parts of mercaptan
Methyl tin DX-181,0.1 part of stearic acid 1801 mix 3 minutes, obtain premix；
(2) it squeezes out: premix being added in single screw extrusion machine barrel by drawing-in device, screw speed 70rpm is fed
Doses is 2.5Kg/h, and the temperature that extruder barrel is arranged is 5 sections, is followed successively by 120 DEG C -140 DEG C -160 DEG C -160 DEG C -160
DEG C, it is first uniform in barrel the first section fusion plastification, then by the 10 parts of roving glass fibers crossed through organosiloxane coupling agent treatment in material
Cylinder third section side feed mouth feeding, forms blend melt, then injects 4 parts in extruder gas injection port by high-pressure metering pump and super faces
Boundary's carbon dioxide, last blend melt are 150 DEG C by temperature, after pressure is the extruder die head of 15MPa, diameter 1mm, are opened
Hole count is that 8 die temperatures are 140 DEG C, and decompression foaming obtains expanded particle；
(3) it is molded: expanded particle is added in injection molding machine, the temperature that injecting machine material tube is arranged is 5 sections, is followed successively by
130 DEG C -150 DEG C -160 DEG C -160 DEG C -160 DEG C, injection molding machine injection pressure is 170MPa, and injection speed 120mm/s passes through height
Press metering pump injection molding machine gas injection port inject 5 parts of supercritical carbon dioxides, melting mixing uniformly afterwards injection mold foamed,
Cooling 15s, obtains foaming product.
Embodiment 3
(1) mixing: weighing raw material by the component of said products, by 50 parts of Corvics, 25 parts of phthalic acids two
Isodecyl ester be added high-speed mixer in mix 2min, then be added 10 parts of haloflexes, 3 parts of calcium carbonate, 1.5 parts of magnesia,
1.5 parts of alkali aluminas, 2.5 parts of carclazytes, 0.5 part of antioxidant 1010,0.2 part of auxiliary antioxidant, 168,1 parts of thiol methyl tins
DX-181,0.1 part of stearic acid 1801 mix 3 minutes, obtain premix；
(2) it squeezes out: premix being added in twin-screw extruder barrel by drawing-in device, screw speed 100rpm,
Feeding capacity is 4Kg/h, and the temperature that extruder barrel is arranged is 5 sections, is followed successively by 120 DEG C -150 DEG C -160 DEG C -160 DEG C -160
DEG C, it is first uniform in barrel the first section fusion plastification, then by the 20 parts of roving glass fibers crossed through organosiloxane coupling agent treatment in material
Cylinder third section side feed mouth feeding, forms blend melt, then injects 3 parts in extruder gas injection port by high-pressure metering pump and super faces
Boundary's carbon dioxide, last blend melt are 140 DEG C by temperature, after pressure is the extruder die head of 10MPa, diameter 1mm, are opened
Hole count is that 8 die temperatures are 140 DEG C, and decompression foaming obtains expanded particle；
(3) it is molded: expanded particle is added in injection molding machine, the temperature that injecting machine material tube is arranged is 5 sections, is followed successively by
130 DEG C -160 DEG C -165 DEG C -165 DEG C -165 DEG C, injection molding machine injection pressure is 200MPa, and injection speed 150mm/s passes through height
Press metering pump injection molding machine gas injection port inject 3 parts of supercritical carbon dioxides, melting mixing uniformly afterwards injection mold foamed,
Cooling 20s, obtains foaming product.
Embodiment 4
Difference with embodiment 1 is only that the material pvc weight resin number of 4 product of embodiment is 25 parts.
Embodiment 5
Difference with embodiment 1 is only that the oxide spinel calcium parts by weight of 5 product of embodiment are 15 parts.
Embodiment 6
Difference with embodiment 1 is only that the raw material long fibre parts by weight of 6 product of embodiment are 46 parts.
Embodiment 7
Difference with embodiment 1 is only that the raw material long fibre parts by weight of 7 product of embodiment are 9 parts.
Embodiment 8
Difference with embodiment 1 is only that the raw material long fiber length of 8 product of embodiment is 3mm.
Embodiment 9
Difference with embodiment 1 is only that 9 the first zone temperatures of extruder barrel of embodiment are 150 DEG C.
Embodiment 10
Difference with embodiment 1 is only that melt pressure is 5MPa in the die head of 10 extruder of embodiment.
Embodiment 11
Difference with embodiment 1 is only that the parts by weight of the injection rate of the supercritical fluid of 11 injection molding machine of embodiment are 0.1
Part.
Embodiment 12
Difference with embodiment 1 is only that the die temperature of 12 extruder of embodiment is 110 DEG C.
Embodiment 13
Difference with embodiment 1 is only that the die temperature of 13 extruder of embodiment is 180 DEG C.
Embodiment 14
Difference with embodiment 1 is only that the parts by weight of the injection rate of 14 supercritical fluid of embodiment are 0.1 part.
Embodiment 15
Difference with embodiment 1 is only that the parts by weight of the injection rate of 15 supercritical fluid of embodiment are 6 parts.
Embodiment 16
Difference with embodiment 1 is only that the diameter of 16 mouth mold of embodiment is 0.1mm.
Embodiment 17
Difference with embodiment 1 is only that the diameter of 17 mouth mold of embodiment is 2mm.
Comparative example 1
Difference with embodiment 1 is only that, long fibre is free of in 1 product raw material of comparative example.
Comparative example 2
Difference with embodiment 1 is only that, does not add supercritical carbon dioxide in 2 extrusion process of comparative example.
Comparative example 3
Difference with embodiment 1 is only that, does not add long fibre and overcritical titanium dioxide in 3 extrusion process of comparative example simultaneously
Carbon.
The foaming product of embodiment 1-17 and comparative example 1-3 are tested, test its loss of weight amount, abscess average diameter,
Tensile strength, the results are shown in Table 1:
Table 1: the performance of product in embodiment 1-17 and comparative example 1-3
As can be seen from the table, embodiment 9,12 can not be successfully extrusion because of the limit temperature of machine, product preparation
Failure, and embodiment 15 is because supercritical fluid is excessive, and cause unstable, desirable influence can not be formed to product, it is real
Applying example 16 cannot be kept the safety in production due to pressure limit, and embodiment 17 is insufficient due to squeezing out staged pressure, and is unable to reach super face
Boundary's state causes supercritical fluid auxiliaring effect to fail.
It is skilled to this field although present invention has been described in detail and some specific embodiments have been cited
For technical staff, as long as it is obvious for can making various changes or correct without departing from the spirit and scope of the present invention.
Claims (15)
1. a kind of preparation method of long fiber reinforcement polyvinyl chloride microporous foam product, which is characterized in that the method includes such as
Lower step:
(1) mixing: Corvic, auxiliary agent are added in high-speed mixer and mix to obtain premix；
(2) it squeezes out: premix is added in extruder barrel by drawing-in device, it is first uniform in barrel leading portion fusion plastification, then
Surface treated long fibre is fed in barrel middle section side feed mouth, forms blend melt, is then being squeezed by high-pressure metering pump
Machine gas injection port injects supercritical fluid out, and last blend melt is depressured foaming after passing through extruder die head, obtains expanded particle；
(3) it is molded: expanded particle is added in injection molding machine, the gas injection port by high-pressure metering pump in injection molding machine injects shooting flow
Body, uniformly injection mold is foamed, is cooled down melting mixing afterwards, obtains foaming product.
2. the preparation method of long fiber reinforcement polyvinyl chloride microporous foam product according to claim 1, which is characterized in that
The product includes the component of following parts by weight: Corvic: 30-50 parts, auxiliary agent: 23.3-83 parts, long fibre: 10-
45 parts.
3. the preparation method of long fiber reinforcement polyvinyl chloride microporous foam product according to claim 2, which is characterized in that
The long fibre includes one of glass fibre, carbon fiber, aramid fiber or a variety of.
4. the preparation method of long fiber reinforcement polyvinyl chloride microporous foam product according to claim 2 or 3, feature exist
In the long fibre is continuous fiber.
5. special according to the preparation method of any long fiber reinforcement polyvinyl chloride microporous foam product of claim 2-4
Sign is that the long stapled length is more than 10mm.
6. the preparation method of long fiber reinforcement polyvinyl chloride microporous foam product according to claim 2, which is characterized in that
The auxiliary agent is made of the component of following parts by weight: plasticizer: 20-50 parts, antioxidant: 0.3-3 parts, fire retardant: 0.5-5
Part, heat-resisting stabilizing agent: 0.5-10 parts, filler: 2-15 parts, lubricant: 0.1-0.5 parts.
7. the preparation method of long fiber reinforcement polyvinyl chloride microporous foam product according to claim 6, which is characterized in that
The plasticizer includes diisooctyl phthalate, epoxidized soybean oil, trioctyl trimellitate (TOTM), haloflex, HL-918
One of or it is a variety of.
8. the preparation method of long fiber reinforcement polyvinyl chloride microporous foam product according to claim 6, which is characterized in that
The filler includes one of nano barium sulfate, nanometer calcium carbonate, clay, alkali alumina, magnesia, carclazyte, white carbon black
Or it is a variety of.
9. the preparation method of long fiber reinforcement polyvinyl chloride microporous foam product according to claim 1, which is characterized in that
Step (2) extruder barrel is divided into 5 heated zones by extruder length, and the first section is close charging extreme direction,
The temperature of first section is 120-140 DEG C, and the temperature of remaining 4 sections is 120-180 DEG C.
10. the preparation method of long fiber reinforcement polyvinyl chloride microporous foam product according to claim 1, feature exist
In step (2) installs high-pressure solenoid valve and self-locking air injection uni-direction also between the outlet of high-pressure metering pump and extruder.
11. the preparation method of long fiber reinforcement polyvinyl chloride microporous foam product according to claim 1, feature exist
In melt pressure is 6-20MPa in the die head of step (2) described extruder, and die temperature is 120-175 DEG C.
12. the preparation method of long fiber reinforcement polyvinyl chloride microporous foam product according to claim 11, feature exist
In the diameter of the mouth mold is 0.5-1.5mm, opens 3-8 hole in mouth mold.
13. the preparation method of long fiber reinforcement polyvinyl chloride microporous foam product according to claim 1, feature exist
In the temperature of step (3) described injecting machine material tube is 120-200 DEG C, and the injection pressure of injection molding machine is 60-250MPa, injection speed
Degree is 50-200mm/s.
14. the preparation method of long fiber reinforcement polyvinyl chloride microporous foam product according to claim 1, feature exist
In the time of step (3) described cooling is 10-50s.
15. the preparation method of long fiber reinforcement polyvinyl chloride microporous foam product according to claim 1, feature exist
In the parts by weight of the injection rate of supercritical fluid are 0.3-5 parts in step (2), step (3).
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Application publication date: 20190517 |
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