CN108517090A - A method of preparing low temperature high rigidity polyvinyl chloride crust foaming plate material - Google Patents
A method of preparing low temperature high rigidity polyvinyl chloride crust foaming plate material Download PDFInfo
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- CN108517090A CN108517090A CN201810401822.9A CN201810401822A CN108517090A CN 108517090 A CN108517090 A CN 108517090A CN 201810401822 A CN201810401822 A CN 201810401822A CN 108517090 A CN108517090 A CN 108517090A
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Abstract
The invention discloses a kind of methods preparing low temperature high rigidity polyvinyl chloride crust foaming plate material, acrylic resin modified, Corvic, stabilizer are added in the mixed machine of heat, after being stirred 3 8min at 90 100 DEG C, lubricant and foaming agent is added, is stirred 3 5min, add plasticizer A and plasticizer B, 115 125 DEG C are warming up to after being stirred 5 10min, filler is added, after being stirred 10 15min, 30 40 DEG C are cooled to, melt is made；Using conical double screw extruder melt extrusion, then using shaper the melt of extrusion cool down, shape, draw, then cut to required size, obtained low temperature high rigidity polyvinyl chloride crust foaming plate material.Each raw material uniformly mixes in low temperature high rigidity polyvinyl chloride crust foaming plate material preparation process in the present invention, and foaming is abundant；The plank hardness of preparation is high, and uniformity is good, and glossiness is high, and resistance to low temperature is excellent, can adapt to temperature working environment jumpy；Mature preparation process, it is easily operated.
Description
Technical field
The invention belongs to polyvinyl-chloride plate material technical fields, and in particular to a kind of to prepare low temperature high rigidity polyvinyl chloride skinning
The method of foaming plate.
Background technology
Polyvinyl chloride be vinyl chloride monomer in initiators such as peroxide, azo compounds under light, heat effect by free radical
The polymer that polymerization reaction mechanism is polymerized has abundant raw material, manufacturing process are ripe, cheap, widely used etc. to dash forward
Go out feature, has become the second largest resins for universal use for being only second to polyethylene in the world, accounted for World Synthetic Resin aggregate consumption
29%.Polyvinyl chloride is easily worked, and can be processed by molding, laminated, injection molding, extrusion molding, calendering, the blowing modes such as hollow.It is poly-
Vinyl chloride can also produce plank, door and window, pipeline and valve mainly for the production of the plastics soft goods such as artificial leather, film, trunking
The plastics boardy products such as door.
Polyvinyl chloride foamed plate adds other auxiliary agents to enhance its heat resistance, toughness, extension using polyvinyl chloride as raw material
Property etc. performances, there are waterproof, fire-retardant, acid and alkali-resistance, mothproof, light, heat preservation, sound insulation, damping, convenient storage, the spies such as easy for construction
Point is widely used in the fields such as automobile, building, household, printing anti-corrosion, is the ideal substitute of timber, aluminium, composite board.
Polyvinyl chloride foamed plate can be divided into free foaming plank, crust foaming plate material, co-extrusion foaming plank according to its manufacture craft.From
It is general by foaming plate case hardness, it is widely used in the fields such as advertisement exhibition board, plate of mounting a picture, silk-screen, engraving；Crust foaming plate material
Case hardness is moderate, it is difficult to generate cut, be widely used in the fields such as cabinet, decoration；Co-extrusion foaming board case hardness is high, surface
It is smooth, there is certain mirror effect, is widely used in the fields such as building, automobile.
Polyvinyl chloride crust foaming plate material in process of production, once extruded by rapid forced to cool down, and makes by melt
Foam surface is cooled down strongly, and foaming can only carry out inside sandwich layer, and material section no longer increases, and surface is formed firmly
Skin, foaming carry out from outside to inside in material section.The prior art mainly adopts add Corvic and other auxiliary agents simultaneously
Enter the mixed machine of heat, be stirred, then through cold mixer cooling down, then by extrusion, cooling, sizing, cutting, prepares polyvinyl chloride
Crust foaming plate material.
As the requirement to properties of product in production and application is higher and higher, it is good that consumer wishes that foaming plate has
Hardness and weatherability can adapt to the lower use environment of temperature, and can adapt to the change dramatically of temperature.Application No. is
201410150082.8 entitled《A kind of Low-temperature antifreeze type polychloroethylene pipes and its production method》Chinese invention patent, it is open
A kind of polychloroethylene pipes of Low-temperature antifreeze function admirable are pressed using EPDM, haloflex is as impact modifier, system
Standby tubing has good lower temperature resistance and shock resistance.It is entitled that application No. is 201611237979.X《It is a kind of low temperature resistant
Polychloroethylene pipes formula》Chinese invention patent, with Corvic, plasticizer, glycerine, toner etc. be original
Material is prepared for a kind of low temperature resistant polychloroethylene pipes, and the tubing is at low ambient temperatures using can prevent PVC pipe from freezing
The case where splitting.Above-mentioned pvc material has good resistance to low temperature, but the product prepared has certain unevenness
Easily there is pit, pin hole and lamination in even property, product.
Invention content
In order to solve the deficiencies in the prior art, low temperature high rigidity polyvinyl chloride skinning is prepared the present invention provides a kind of
The method of foaming plate acrylic resin modified, Corvic, stabilizer is added in the mixed machine of heat, at 90-100 DEG C
After being stirred 3-8min, lubricant and foaming agent is added, is stirred 3-5min, adds plasticizer A and plasticizer B, stir
It is warming up to 115-125 DEG C after mixing mixing 5-10min, filler is added, after being stirred 10-15min, is cooled to 30-40 DEG C, system
Obtain melt；Using conical double screw extruder melt extrusion, then using shaper the melt of extrusion cool down, be shaped,
Traction, then cuts to required size, and low temperature high rigidity polyvinyl chloride crust foaming plate material is made.Low temperature is high hard in the present invention
Each raw material uniformly mixes in degree polyvinyl chloride crust foaming plate material preparation process, and foaming is abundant；The plank hardness of preparation is high, uniformly
Property it is good, glossiness is high, and resistance to low temperature is excellent, can adapt to temperature working environment jumpy；Preparation method is simple, is easy to
Operation.
Institute of the invention technique effect to be achieved is realized by following scheme：
The present invention provides a kind of methods preparing low temperature high rigidity polyvinyl chloride crust foaming plate material, include the following steps：
S01, the preparation of melt：It is respectively acrylic resin modified, 40%-50% the polychlorostyrene second of 15%-25% by mass percent
Olefine resin, 8%-15% stabilizer be added in the mixed machine of heat, after being stirred 3-8min at 90-100 DEG C, mass percent is added
The foaming agent that lubricant and mass percent for 5%-10% are 5%-10%, is stirred 3-5min, adds mass percent
The plasticizer B that plasticizer A and mass percent for 5%-15% are 0.5%-3%, 115- is warming up to after being stirred 5-10min
125 DEG C, the filler that mass percent is 10%-20% is added, after being stirred 10-15min, is cooled to 30-40 DEG C, is made molten
Body；
S02, the extrusion of melt：The melt conveying of gained in S01 to conical double screw extruder is squeezed out, screw speed is controlled
20-30r/min, processing temperature are 180-210 DEG C, melt extrusion；
S03, the preparation of low temperature high rigidity polyvinyl chloride crust foaming plate material：Using shaper to the melt that is squeezed out in S02 into
Row is cooling, sizing, draws, and then cuts to required size, low temperature high rigidity polyvinyl chloride crust foaming plate material is made；
It is described it is acrylic resin modified be thermosetting acrylic resin, preparation method is：It is respectively 50%- by mass percent
The curing agent mixing of 60% hard monomer, the epoxy resin of 20%-30%, the calcium carbonate of 5%-10%, the silica of 5%-10%, 5%-8%
It is squeezed out through conical double screw extruder after uniformly, controls screw speed 20-30r/min, processing temperature is 150-170 DEG C, is made
Thermosetting acrylic resin.
Stabilizer can prevent from deviating from hydrogen chloride in Corvic strand, or prevent this reaction, terminate and divide
Solution acts on, and improves the decomposition temperature of Corvic, between raw material phase mutual friction mix, be warming up to 90-100 DEG C, be conducive to
The moisture and volatile matter carried secretly in acrylic resin modified and Corvic is discharged, adds lubricant and foaming agent allows tree
Fat fully absorbs, and lubricant can promote the plasticizing of modified polyurethane and Corvic, reduces melt viscosity, improves its stream
Dynamic property, moreover it is possible to which the intensity for improving melt prevents the merging of bubble, obtains the product of even foaming, while also ensuring that melt has
There is good mobility, to obtain the good product of appearance.
Plasticizer is the important recipe ingredient of polrvinyl chloride product, is influenced on polrvinyl chloride product very big.Increase in the present invention
Modeling agent is cold resistant plasticizer, and plasticizing efficiency is high, can assign plank excellent resistance to low temperature.Filler is generally heat resistance
Excellent high melting solid substance can improve the density, hardness, elasticity modulus of crust foaming plate material, improve the mechanics of plank
Performance and impact strength add after being warming up to 115-125 DEG C, are conducive to the activity for improving filler, while the temperature is less than
The decomposition temperature of Corvic can keep the stabilization of Corvic chemical property.
After the completion of each raw material mixing, it is cooled to 30-40 DEG C, melt keeps certain viscosity and mobility, and the temperature model
It encloses interior melt property to stablize, convenient for storage and transport, facilitates taking for supplied materials in extrusion.
Conical double screw extruder has good charging performance, mixing plasticizing capacity, exhaust performance, extrusion stability etc.
Feature selects double screw extruder to be capable of the extrusion of the above-mentioned melt of completion of efficient quality guaranteeing guarantor amount, according to the viscosity of melt
The screw speed for selecting 20-30r/min, selects processing temperature for 180-210 DEG C according to the composition of melt.Temperature is too low, melt
Due to mixing unevenness, it is nucleated less and disperses uneven and form air pocket；When the temperature is excessively high, material viscosity reduces, melt strength
Become larger, abscess, which can be combined with each other, to become larger, and gas is to external diffusion into the surface, causing foaming excessive, abscess is uneven, has broken in melt
Hole；180-210 DEG C of moderate temperature, material are uniformly mixed, and plasticizing is good, and gas solubility in melt increases and nucleation quantity increases
It is more, it foams fine and smooth uniform.
Thermosetting acrylic resin is added in melt preparation process, the hardness of plank, the thermosetting can be further enhanced
Property acrylic resin and Corvic have good compatibility in the molten state, can be uniformly distributed in melt.It is described
In thermosetting acrylic resin preparation process, after mixing by raw material, squeezed out up to required by conical double screw extruder
Thermosetting acrylic resin, reaction efficiency is high, and raw material availability is high.
Further, the degree of polymerization of Corvic described in S01 is 700-900.The degree of polymerization increase, resin it is basic
Performance improves, but fusion time extends therewith, and fusion factor becomes larger, poor processability, and the degree of polymerization is that 700-900 is common
Corvic, basic performance is excellent, and processing performance is good.
Further, mixing speed is 900-1000r/min in the mixed machine of heat described in S01.It is high-speed stirred in the mixed machine of heat,
Be conducive to being sufficiently mixed for raw material.
Further, stabilizer described in S01 is Ca Zn composite object, carboxylic acid organotin, one kind in barium stearate or several
Kind.
Further, lubricant described in S01 be calcium stearate, oxidized polyethylene wax, stearic acid, tristerin,
One or more of paraffin.
Further, foaming agent described in S01 is carbon dioxide, butane, azodicarbonamide, azodiisobutyronitrile, carbon
One or more of sour hydrogen sodium, ammonium hydrogen carbonate, azido compound.
Further, plasticizer A described in S01 be adipic acid dibutyl ester, diisodecyl adipate (DIDA), dioctyl azelate,
One or more of dioctyl sebacate；Plasticizer B described in S01 is hexamethylphosphoramide.Plasticizer A makes excellent resistance to
Cold plasticizer makes plank obtained that there is excellent resistance to low temperature, plasticizer B can be effectively reduced the solidification of plasticizer
Point strengthens the effect that resists cold.
Further, filler described in S01 is one or more of calcium carbonate, talcum powder, kaolin.
Further, shaper described in S03 is vacuum water-cooled shaping mold；Cooling velocity described in S03 is 40-50
DEG C/min, temperature is 20-30 DEG C after cooling.Vacuum water-cooled shaping mould shape is efficient, and cooling velocity is fast, and cooling temperature is steady
Fixed, melt is forced to cool down once extruded by rapid, and surface forms sclerderm, and crust foaming plate material hardness obtained is high.
Further, in the preparation method of the thermosetting acrylic resin, the hard monomer is methyl acrylate, methyl
One or more of methyl acrylate, acrylonitrile, acrylamide；The curing agent is ethylenediamine, aminoethyl piperazine, diamino
One or more of hexamethylene, m-phenylene diamine (MPD), m-xylene diamine.
The present invention has the following advantages：
1. raw material uniformly mixes in low temperature high rigidity polyvinyl chloride crust foaming plate material preparation process in the present invention, foaming is abundant.
2. low temperature high rigidity polyvinyl chloride crust foaming plate material hardness is high in the present invention, resistance to low temperature is good, adapts to temperature
Spend use environment jumpy.
3. low temperature high rigidity polyvinyl chloride crust foaming plate material uniformity is good in the present invention, glossiness is high.
4. low temperature high rigidity polyvinyl chloride crust foaming plate material preparation process is simply ripe in the present invention, easily operated.
Specific implementation mode
With reference to embodiment, the present invention will be described in detail.
Embodiment 1
S01, the preparation of melt：It is respectively 15% thermosetting acrylic resin, 41.5% polyvinyl chloride tree by mass percent
Fat（PVC resin polymerization degree is 800）, 8% barium stearate be added in the mixed machine of heat, controlling mixing speed in the mixed machine of heat is
After being stirred 4min at 95 DEG C, the paraffin that mass percent is 5% and the carbon that mass percent is 5% is added in 1000r/min
Sour hydrogen sodium, is stirred 3min, adds the adipic acid dibutyl ester that mass percent is 15% and mass percent is 0.5% six
Methyl phosphoric triamide is warming up to 120 DEG C after being stirred 5min, and the talcum powder that mass percent is 10% is added, is stirred
After 10min, 30 DEG C are cooled to, melt is made；
S02, the extrusion of melt：The melt conveying of gained in S01 to conical double screw extruder is squeezed out, screw speed is controlled
25r/min, processing temperature are 180 DEG C, melt extrusion；
S03, the preparation of low temperature high rigidity polyvinyl chloride crust foaming plate material：Using vacuum water-cooled shaping mold to being squeezed out in S02
Melt cool down, shape, draw, cooling velocity is 40 DEG C/min, it is cooling after temperature be 25 DEG C, then cut to required
Low temperature high rigidity polyvinyl chloride crust foaming plate material is made in size；
The preparation method of the thermosetting acrylic resin is：By mass percent be respectively 50% methyl acrylate, 25%
Epoxy resin, 10% calcium carbonate, 7% silica, 8% ethylenediamine be uniformly mixed after squeezed out through conical double screw extruder, control
Screw speed 20r/min processed, processing temperature are 160 DEG C, and thermosetting acrylic resin is made.
Embodiment 2
S01, the preparation of melt：It is respectively 15% thermosetting acrylic resin, 43.5% polyvinyl chloride tree by mass percent
Fat（PVC resin polymerization degree is 800）, 8% barium stearate be added in the mixed machine of heat, controlling mixing speed in the mixed machine of heat is
After being stirred 4min at 95 DEG C, the paraffin that mass percent is 5% and the carbon that mass percent is 5% is added in 1000r/min
Sour hydrogen sodium, is stirred 3min, adds the adipic acid dibutyl ester that mass percent is 13% and mass percent is 0.5% six
Methyl phosphoric triamide is warming up to 120 DEG C after being stirred 5min, and the talcum powder that mass percent is 10% is added, is stirred
After 10min, 30 DEG C are cooled to, melt is made；
S02, the extrusion of melt：The melt conveying of gained in S01 to conical double screw extruder is squeezed out, screw speed is controlled
25r/min, processing temperature are 180 DEG C, melt extrusion；
S03, the preparation of low temperature high rigidity polyvinyl chloride crust foaming plate material：Using vacuum water-cooled shaping mold to being squeezed out in S02
Melt cool down, shape, draw, cooling velocity is 40 DEG C/min, it is cooling after temperature be 25 DEG C, then cut to required
Low temperature high rigidity polyvinyl chloride crust foaming plate material is made in size；
The preparation method of the thermosetting acrylic resin is：By mass percent be respectively 50% methyl acrylate, 25%
Epoxy resin, 10% calcium carbonate, 7% silica, 8% ethylenediamine be uniformly mixed after squeezed out through conical double screw extruder, control
Screw speed 20r/min processed, processing temperature are 160 DEG C, and thermosetting acrylic resin is made.
Embodiment 3
S01, the preparation of melt：It is respectively 16% thermosetting acrylic resin, 42% Corvic by mass percent
（PVC resin polymerization degree is 800）, 9% barium stearate be added in the mixed machine of heat, controlling mixing speed in the mixed machine of heat is
After being stirred 4min at 95 DEG C, the paraffin that mass percent is 7% and the carbon that mass percent is 7% is added in 1000r/min
Sour hydrogen sodium, is stirred 3min, adds the adipic acid dibutyl ester that mass percent is 6% and the pregnancy that mass percent is 1%
Base phosphoric triamide is warming up to 120 DEG C after being stirred 5min, and the talcum powder that mass percent is 12% is added, is stirred
After 10min, 30 DEG C are cooled to, melt is made；
S02, the extrusion of melt：The melt conveying of gained in S01 to conical double screw extruder is squeezed out, screw speed is controlled
25r/min, processing temperature are 180 DEG C, melt extrusion；
S03, the preparation of low temperature high rigidity polyvinyl chloride crust foaming plate material：Using vacuum water-cooled shaping mold to being squeezed out in S02
Melt cool down, shape, draw, cooling velocity is 40 DEG C/min, it is cooling after temperature be 25 DEG C, then cut to required
Low temperature high rigidity polyvinyl chloride crust foaming plate material is made in size；
The preparation method of the thermosetting acrylic resin is：By mass percent be respectively 50% methyl acrylate, 25%
Epoxy resin, 10% calcium carbonate, 7% silica, 8% ethylenediamine be uniformly mixed after squeezed out through conical double screw extruder, control
Screw speed 20r/min processed, processing temperature are 160 DEG C, and thermosetting acrylic resin is made.
Embodiment 4-10
Compared with Example 1, embodiment 4-10 the difference is that, in melt preparation process, the mass percent of raw material is not
Together.Other preparation methods, parameter are same as Example 1.
Thermosetting acrylic resin in embodiment 1-10, Corvic, barium stearate, paraffin, sodium bicarbonate, oneself two
Sour dibutyl ester, hexamethylphosphoramide, the mass percent of talcum powder such as following table：
To the polyvinyl chloride crust foaming plate material that is prepared in embodiment carry out appearance detection, surface gloss detection, hardness determination,
Cryogenic property is tested.Wherein appearance uses visual inspection；Surface gloss is measured with vancometer；Hardness uses D type Shore durometers
It measures；Cryogenic property carries out -30 DEG C using clod wash case and deflects test, according to《GB/T 12706.1-2008 rated voltages
1kV(U m=1.2kV) to 35kV (U m=40.5kV) extrusion insulating power cable and attachment》It is tested.Testing result such as following table：
It can be seen from the test results that the crust foaming plate material uniformity prepared in embodiment is good, surface without pit, pin-free,
Surface gloss is high, and hardness is high, and resistance to low temperature is excellent.
Finally, it should be noted that above example be only to illustrate the embodiment of the present invention technical solution rather than to its into
Row limitation, although the embodiment of the present invention is described in detail with reference to preferred embodiment, those skilled in the art
It should be understood that the technical solution of the embodiment of the present invention can be still modified or replaced equivalently, and these are changed or wait
The range of modified technical solution disengaging technical solution of the embodiment of the present invention cannot also be made with replacement.
Claims (10)
1. a kind of method preparing low temperature high rigidity polyvinyl chloride crust foaming plate material, it is characterised in that：Include the following steps：
S01, the preparation of melt：It is respectively acrylic resin modified, 40%-50% the polychlorostyrene second of 15%-25% by mass percent
Olefine resin, 8%-15% stabilizer be added in the mixed machine of heat, after being stirred 3-8min at 90-100 DEG C, mass percent is added
The foaming agent that lubricant and mass percent for 5%-10% are 5%-10%, is stirred 3-5min, adds mass percent
The plasticizer B that plasticizer A and mass percent for 5%-15% are 0.5%-3%, 115- is warming up to after being stirred 5-10min
125 DEG C, the filler that mass percent is 10%-20% is added, after being stirred 10-15min, is cooled to 30-40 DEG C, is made molten
Body；
S02, the extrusion of melt：The melt conveying of gained in S01 to conical double screw extruder is squeezed out, screw speed is controlled
20-30r/min, processing temperature are 180-210 DEG C, melt extrusion；
S03, the preparation of low temperature high rigidity polyvinyl chloride crust foaming plate material：Using shaper to the melt that is squeezed out in S02 into
Row is cooling, sizing, draws, and then cuts to required size, low temperature high rigidity polyvinyl chloride crust foaming plate material is made；
It is described it is acrylic resin modified be thermosetting acrylic resin, preparation method is：It is respectively 50%- by mass percent
The curing agent mixing of 60% hard monomer, the epoxy resin of 20%-30%, the calcium carbonate of 5%-10%, the silica of 5%-10%, 5%-8%
It is squeezed out through conical double screw extruder after uniformly, controls screw speed 20-30r/min, processing temperature is 150-170 DEG C, is made
Thermosetting acrylic resin.
2. the method for preparing low temperature high rigidity polyvinyl chloride crust foaming plate material as described in claim 1, it is characterised in that：S01
Described in Corvic the degree of polymerization be 700-900.
3. the method for preparing low temperature high rigidity polyvinyl chloride crust foaming plate material as described in claim 1, it is characterised in that：S01
Described in the mixed machine of heat mixing speed be 900-1000r/min.
4. the method for preparing low temperature high rigidity polyvinyl chloride crust foaming plate material as described in claim 1, it is characterised in that：S01
Described in stabilizer be Ca Zn composite object, carboxylic acid organotin, one or more of barium stearate.
5. the method for preparing low temperature high rigidity polyvinyl chloride crust foaming plate material as described in claim 1, it is characterised in that：S01
Described in lubricant be calcium stearate, oxidized polyethylene wax, stearic acid, tristerin, one or more of paraffin.
6. the method for preparing low temperature high rigidity polyvinyl chloride crust foaming plate material as described in claim 1, it is characterised in that：S01
Described in foaming agent be carbon dioxide, butane, azodicarbonamide, azodiisobutyronitrile, sodium bicarbonate, ammonium hydrogen carbonate, nitrine
One or more of compound.
7. the method for preparing low temperature high rigidity polyvinyl chloride crust foaming plate material as described in claim 1, it is characterised in that：S01
Described in plasticizer A be adipic acid dibutyl ester, diisodecyl adipate (DIDA), dioctyl azelate, one kind in dioctyl sebacate
Or it is several；Plasticizer B described in S01 is hexamethylphosphoramide.
8. the method for preparing low temperature high rigidity polyvinyl chloride crust foaming plate material as described in claim 1, it is characterised in that：S01
Described in filler be calcium carbonate, talcum powder, one or more of kaolin.
9. the method for preparing low temperature high rigidity polyvinyl chloride crust foaming plate material as described in claim 1, it is characterised in that：S03
Described in shaper be vacuum water-cooled shaping mold；Cooling velocity described in S03 is 40-50 DEG C/min, and temperature is after cooling
20-30℃。
10. the method for preparing low temperature high rigidity polyvinyl chloride crust foaming plate material as described in claim 1, it is characterised in that：Institute
In the preparation method for stating thermosetting acrylic resin, the hard monomer be methyl acrylate, methyl methacrylate, acrylonitrile,
One or more of acrylamide；The curing agent be ethylenediamine, aminoethyl piperazine, diaminocyclohexane, m-phenylene diamine (MPD),
One or more of benzene dimethylamine.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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