CN106633467A - Method for preparing hard sandwich cross-linked PVC foam material - Google Patents
Method for preparing hard sandwich cross-linked PVC foam material Download PDFInfo
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- CN106633467A CN106633467A CN201510741657.8A CN201510741657A CN106633467A CN 106633467 A CN106633467 A CN 106633467A CN 201510741657 A CN201510741657 A CN 201510741657A CN 106633467 A CN106633467 A CN 106633467A
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- hard sandwich
- preparing hard
- expanded material
- crosslinked pvc
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- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000006261 foam material Substances 0.000 title abstract description 9
- 239000004088 foaming agent Substances 0.000 claims abstract description 26
- 239000002608 ionic liquid Substances 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 25
- -1 polyethylene, isocyanate Polymers 0.000 claims abstract description 22
- 239000003381 stabilizer Substances 0.000 claims abstract description 20
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims abstract description 16
- 150000008064 anhydrides Chemical class 0.000 claims abstract description 15
- 239000004094 surface-active agent Substances 0.000 claims abstract description 15
- 239000004709 Chlorinated polyethylene Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004132 cross linking Methods 0.000 claims abstract description 9
- 239000003999 initiator Substances 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims description 45
- 238000009835 boiling Methods 0.000 claims description 13
- 239000012948 isocyanate Substances 0.000 claims description 13
- 239000003795 chemical substances by application Substances 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 239000002131 composite material Substances 0.000 claims description 10
- 150000001875 compounds Chemical class 0.000 claims description 10
- 150000002513 isocyanates Chemical class 0.000 claims description 10
- 238000005187 foaming Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 239000004604 Blowing Agent Substances 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Natural products CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- MUTGBJKUEZFXGO-UHFFFAOYSA-N hexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21 MUTGBJKUEZFXGO-UHFFFAOYSA-N 0.000 claims description 6
- 238000000643 oven drying Methods 0.000 claims description 6
- 229920002732 Polyanhydride Polymers 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 4
- 230000002745 absorbent Effects 0.000 claims description 4
- 239000002250 absorbent Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 239000003063 flame retardant Substances 0.000 claims description 4
- 150000002333 glycines Chemical class 0.000 claims description 4
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 claims description 4
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 4
- 239000011976 maleic acid Substances 0.000 claims description 4
- 238000012856 packing Methods 0.000 claims description 4
- 239000000049 pigment Substances 0.000 claims description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 4
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 3
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 3
- XOZUGNYVDXMRKW-AATRIKPKSA-N azodicarbonamide Chemical compound NC(=O)\N=N\C(N)=O XOZUGNYVDXMRKW-AATRIKPKSA-N 0.000 claims description 3
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 3
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 3
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 3
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 2
- DGTNSSLYPYDJGL-UHFFFAOYSA-N phenyl isocyanate Chemical compound O=C=NC1=CC=CC=C1 DGTNSSLYPYDJGL-UHFFFAOYSA-N 0.000 claims description 2
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims 1
- 239000004643 cyanate ester Substances 0.000 claims 1
- 239000011347 resin Substances 0.000 abstract description 3
- 229920005989 resin Polymers 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 2
- 238000004898 kneading Methods 0.000 abstract 1
- 238000000465 moulding Methods 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 37
- 239000004800 polyvinyl chloride Substances 0.000 description 37
- 238000006243 chemical reaction Methods 0.000 description 11
- 239000006260 foam Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 230000005587 bubbling Effects 0.000 description 3
- 238000006735 epoxidation reaction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 235000014593 oils and fats Nutrition 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 description 2
- 238000005660 chlorination reaction Methods 0.000 description 2
- 235000019197 fats Nutrition 0.000 description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 239000004616 structural foam Substances 0.000 description 2
- OTEKOJQFKOIXMU-UHFFFAOYSA-N 1,4-bis(trichloromethyl)benzene Chemical compound ClC(Cl)(Cl)C1=CC=C(C(Cl)(Cl)Cl)C=C1 OTEKOJQFKOIXMU-UHFFFAOYSA-N 0.000 description 1
- OZAIFHULBGXAKX-VAWYXSNFSA-N AIBN Substances N#CC(C)(C)\N=N\C(C)(C)C#N OZAIFHULBGXAKX-VAWYXSNFSA-N 0.000 description 1
- 241000208340 Araliaceae Species 0.000 description 1
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- KXBFLNPZHXDQLV-UHFFFAOYSA-N [cyclohexyl(diisocyanato)methyl]cyclohexane Chemical compound C1CCCCC1C(N=C=O)(N=C=O)C1CCCCC1 KXBFLNPZHXDQLV-UHFFFAOYSA-N 0.000 description 1
- 206010000269 abscess Diseases 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000013012 foaming technology Methods 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000012745 toughening agent Substances 0.000 description 1
Abstract
The invention relates to a method for preparing a hard sandwich cross-linked PVC foam material. The method comprises the following steps: weighing PVC resins, chlorinated polyethylene, isocyanate, an ionic liquid surfactant, a foaming agent, anhydride and a stabilizer as raw materials, taking azodiisobutyronitrile as an initiator, and adding the components into a kneading machine for uniformly mixing; carrying plasticizing, molding, blank demolding, water vapor demolding and cross-linking, drying in a drying oven, and the like, thereby obtaining the hard sandwich cross-linked PVC foam material. Compared with the prior art, the PVC foam material disclosed by the invention has the advantage that the comprehensive performance is greatly improved.
Description
Technical field
The present invention relates to a kind of preparation method of expanded material, more particularly, to one kind the crosslinking of hard sandwich is prepared
The method of PVC foam material.
Background technology
Hard PVC foaming product has lot of advantages, and its abscess fine and even, mechanical mechanics property is excellent.
Cross-linked rigid PVC foams, are widely used in the sandwiches such as wind energy, yacht, sports equipment, railway and space flight
In composite application.But, the technique for producing PVC foam material also there are problems that, such as because of life
The difference of production. art, PVC foam process may result in degraded, the foaming cured later time it is longer and
Color problem of PVC foam toughness of products deficiency and mechanical mechanics property difference and product etc..It is hard with regard to crosslinking
The stability problem of the course of processing of matter PVC foam material.Patent discloses report, adds in formula
The epoxy component of 3%-15% can alleviate the resolution problem in the PVC courses of processing as stabilizer and toughener,
But extend hardening time in post-production, additionally, also can further function as surely by addition Ca Zn composite agent
Determine the effect of PVC foam.
The other alkaline PVC and HHPA also having been reported that using K values for 70, energy improve production efficiency,
But because alkalescence PVC have impact on the acidity of reaction environment, technique controlling difficulty is increased, limit technique ginseng
Number.
The content of the invention
The purpose of the present invention is exactly the defect in order to overcome above-mentioned prior art to exist and provides a kind of comprehensive
The method for preparing hard sandwich crosslinked PVC expanded material that can be greatly improved.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of method for preparing hard sandwich crosslinked PVC expanded material, using following steps：
(1) get the raw materials ready：Weigh dilute Corvic, chlorinated polyethylene, isocyanates, ionic liquid surface
Activating agent, foaming agent, anhydride, stabilizer are raw material, and using azodiisobutyronitrile as initiator；
(2) pre- stirring and heating：To uniformly mix in each component input kneader in formula, control temperature
20-40 DEG C, mixing speed 500-1000r/min makes raw material mix homogeneously, while avoid foaming agent from decomposing,
Low boiling point solvent volatilizees or each component does not occur chemical reaction；
(3) plasticizing forming：The mixed material for obtaining is poured in mould, mould closure is pressurizeed and heated,
Heating-up temperature 100-110 DEG C, now compound generation polyreaction heat release, makes mold temperature be increased to 170-190
DEG C, mixed material plasticizing forming at such a temperature；To prevent intensification too high and reaction of decomposing, mould sets
Put cooling system.
(4) mold temperature is down to into 130-150 DEG C, then carries out the blank demoulding；
(5) vapor foaming and crosslinking：Prefoam blank after the demoulding is put into into temperature more than 95 DEG C
Decocting in water 4-6h in hot water, then in oven drying, that is, prepares hard sandwich crosslinked PVC expanded material.
Corvic, dilute chlorinated polyethylene, isocyanates, ionic liquid surface activity in step (1)
Agent, foaming agent, anhydride, the weight ratio of stabilizer are 100：1-10：30-120：0.05-2.5：3-12：
1-30：3.
Described isocyanates are the isocyanates chemical combination with two or more multiple isocyanate functional groups
Thing.
Preferably, isocyanates include but is not limited to 2,2 '-dimethyl -3, and 3 ', 5, the isocyanide of 5 '-triphenyl methane four
Acid esters, 2,4 toluene diisocyanate, 2,6- toluene di-isocyanate(TDI)s, hexamethylene diisocyanate, hexichol
Dicyclohexylmethane diisocyanate, 4,4' methylene bis (carbanil) or isophorone diisocyanate.
Described ionic liquid surfactant is following molecular structure：
Wherein, R1、R2、R3、R4For H, OH, SH or Me,
X=I, Br, Cl, PF6, BF4, SbF6,
The ionic liquid surfactant for using is a kind of ionic liquid of long chain, and two ends have hydrophilic simultaneously
With the compound of oleophylic, by premixing stirring come the excellent hard crosslinked PVC structural foam of processability.
Hydrophilic segment can effectively increase the toughness of microvesicle, meanwhile, having the part of ionic liquid concurrently can more effectively dissolve
Low-boiling foaming agent, improves nucleation efficiencies.
In addition, by adding the dilute toughness to increase PVC foam of chlorinated polyethylene.
Described foaming agent is low boiling physical blowing agent or CBA.
Preferably, low boiling physical blowing agent be hexamethylene, CBA is 2,2 '-azobis isobutyronitrile or
One or two in azodicarboamide.
Anhydride described in described anhydride be maleic acid bar, poly sebacic polyanhydride, the one kind in HHPA.
Described stabilizer is epoxidation oils and fatss such as Oleum Glycines, oleum lini, magnesium oxide, the metal such as Ca Zn composite agent
One kind in stabilizer.
Also add in raw material one kind in pigment, UV absorbent, packing material or phosphorous flame-retardant material or
It is several.
The weight of Corvic accounts for the 40-60% of gross weight in raw material.
Compared with prior art, the ionic liquid surfactant that the present invention is adopted is for regulation system porous
Structure, shearing traction, the foamable polymer for improving mechanical performance has a direct impact.
Improve the toughness of microvesicle, frothing percentage, mechanical strength, by adding by adding ionic liquid surfactant
Plus chlorination PVC is improving the mechanical property of PVC composites, due to the ionic liquid being dispersed on polyvinyl chloride resin
Body surface activity, the bubbling efficiency of foaming agent is greatly improved, so as to PVC composite foams show it is excellent
Mechanical strength, i.e., using a small amount of foaming agent, can still be readily available higher bubbling efficiency.By drawing
Enter the dilute high tenacity having of chlorinated polyethylene in itself and excellent mechanical property, finally cause PVC foam material
Combination property is greatly improved.
The present invention is except using crosslinked foaming technology, most distinct characteristic is the use of ionic liquid formula, no
Only help to improve cell density, while the effect with stable bubble hole.
Specific embodiment
With reference to specific embodiment, the present invention is described in detail.
A kind of method for preparing hard sandwich crosslinked PVC expanded material, using following steps：
(1) get the raw materials ready：Weigh dilute Corvic, chlorinated polyethylene, isocyanates, ionic liquid surface
Activating agent, foaming agent, anhydride, stabilizer are raw material, and it is 100 that its weight ratio is weight ratio：1-10：30-120：
0.05-2.5：3-12：1-30：3, and using azodiisobutyronitrile as initiator, wherein, isocyanates
It is the isocyanate compound with two or more multiple isocyanate functional groups, it is for instance possible to use 2,2 '-
Dimethyl -3,3 ', 5,5 '-triphenyl methane tetraisocyanate, 2,4 toluene diisocyanate, 2,6- toluene diisocyanates
Acid esters, hexamethylene diisocyanate, methyl diphenylene diisocyanate, 4,4' methylene bis (Carbimide. benzene
Ester) or isophorone diisocyanate.
Ionic liquid surfactant is following molecular structure：
Wherein, R1、R2、R3、R4For H, OH, SH or Me,
X=I, Br, Cl, PF6, BF4, SbF6,
The ionic liquid surfactant for using is a kind of ionic liquid of long chain, and this is that the present invention has wound
One place of the property made, two ends have the compound of hydrophilic and oleophylic simultaneously, are prepared by premixing stirring
The hard crosslinked PVC structural foam of excellent performance.Hydrophilic segment can effectively increase the toughness of microvesicle, meanwhile,
Having the part of ionic liquid concurrently can more effectively dissolve low-boiling foaming agent, improve nucleation efficiencies.
The dilute toughness that can increase PVC foam of chlorinated polyethylene of addition, chlorination PVC is compound to improve PVC
The mechanical property of material, due to the ionic liquid surface activity being dispersed on polyvinyl chloride resin, the foaming of foaming agent
Efficiency is greatly improved, so as to PVC composite foams show excellent mechanical strength, i.e., using a small amount of
Foaming agent, can still be readily available higher bubbling efficiency, in addition, the dilute high-ductility having of chlorinated polyethylene in itself
Property and excellent mechanical property, final that the combination property of PVC foam material is greatly improved, this is
Second innovative point of the present invention.
Foaming agent is low boiling physical blowing agent or CBA.Such as low boiling physical blowing agent is hexamethylene
Alkane, CBA is 2, one or two in 2 '-azobis isobutyronitrile or azodicarboamide.
Anhydride be maleic acid bar, poly sebacic polyanhydride, the one kind in HHPA.Stabilizer is epoxidation oils and fatss
Such as the one kind in the metallic stabilizers such as Oleum Glycines, oleum lini, magnesium oxide, Ca Zn composite agent.
In addition, pigment, UV absorbent, packing material or phosphorous flame-retardant can also be added in raw material
One or more in material, the weight of Corvic accounts for the 40-60% of gross weight in above-mentioned raw materials；
(2) pre- stirring and heating：To uniformly mix in each component input kneader in formula, control temperature
20-40 DEG C, mixing speed 500-1000r/min makes raw material mix homogeneously, while avoid foaming agent from decomposing,
Low boiling point solvent volatilizees or each component does not occur chemical reaction；
(3) plasticizing forming：The mixed material for obtaining is poured in mould, mould closure is pressurizeed and heated,
Heating-up temperature 100-110 DEG C, now compound generation polyreaction heat release, makes mold temperature be increased to 170-190
DEG C, mixed material plasticizing forming at such a temperature；To prevent intensification too high and reaction of decomposing, mould sets
Put cooling system.
(4) mold temperature is down to into 130-150 DEG C, then carries out the blank demoulding；
(5) vapor foaming and crosslinking：Prefoam blank after the demoulding is put into into temperature more than 95 DEG C
Decocting in water 4-6h in hot water, then in oven drying, that is, prepares hard sandwich crosslinked PVC expanded material.
Embodiment 1
A kind of method for preparing hard sandwich crosslinked PVC expanded material, using following steps：
(1) raw material is weighed by weight：100 parts of Corvic, chlorinated polyethylene is dilute 5 parts, isocyanide
80 parts of acid esters (MDI), 2 parts of this ionic liquid surfactant, 10 parts of foaming agent, 10 parts of anhydride,
3 parts of stabilizer, and using AIBN as initiator, wherein, the isocyanates for using are 2,2 '-dimethyl
- 3,3 ', 5,5 '-triphenyl methane tetraisocyanate, ionic liquid surfactant is following molecular structure：
Wherein, R1、R2、R3、R4Respectively H, OH, SH, Me, X is Br, and foaming agent is hexamethylene
Alkane, anhydride is maleic acid bar, and poly sebacic polyanhydride, one kind in HHPA is used in the present embodiment
Maleic anhydride.Stabilizer is epoxidation oils and fatss such as Oleum Glycines, oleum lini, magnesium oxide, the metal such as Ca Zn composite agent
One kind in stabilizer, uses oleum lini in the present embodiment.
(2) pre- stirring and heating：Each component is put in kneader and is uniformly mixed, control 20 DEG C, stirring
Speed 1000r/min, mix homogeneously, while avoiding foaming agent from decomposing, low boiling point solvent volatilization or each component are not
Generation chemical reaction.
(3) plasticizing forming：Compound is poured in mould, and mould closure is pressurizeed and heated, heating-up temperature 100
DEG C, now there is polyreaction heat release in compound, make mold temperature be increased to 180 DEG C or so, mixed material
Plasticizing forming at this temperature.To prevent intensification too high and reaction of decomposing, mould arranges cooling system.
(4) mold temperature control is at 130 DEG C, the blank demoulding.
(5) vapor foaming and crosslinking.Prefoam blank after the demoulding is put into into temperature more than 95 DEG C
In hot water, decocting in water 4 hours.
(6) oven drying, is processed into product, and product mechanical property sees attached list.
Embodiment 2
A kind of method for preparing hard sandwich crosslinked PVC expanded material, using following steps：
(1) get the raw materials ready：By weight it is 100：1：30：0.05：3：1：3 weigh Corvic,
Chlorinated polyethylene is dilute, isocyanates, ionic liquid surfactant, foaming agent, anhydride, stabilizer are raw material,
And using azodiisobutyronitrile as initiator, wherein, the isocyanates for using are 2,4- toluene diisocynates
Ester, ionic liquid surfactant is following molecular structure：
Wherein, R1、R2、R3、R4H is, X is I, and foaming agent is 2,2 '-azobis isobutyronitrile, acid
Acid anhydride is poly sebacic polyanhydride, and stabilizer is magnesium oxide；
(2) pre- stirring and heating：To uniformly mix in each component input kneader in formula, control temperature
30 DEG C, mixing speed 800r/min makes raw material mix homogeneously, while avoiding foaming agent from decomposing, low boiling is molten
There is no chemical reaction in agent volatilization or each component；
(3) plasticizing forming：The mixed material for obtaining is poured in mould, mould closure is pressurizeed and heated,
100 DEG C of heating-up temperature, now compound generation polyreaction heat release, makes mold temperature be increased to 170 DEG C,
Mixed material plasticizing forming at such a temperature；To prevent intensification too high and reaction of decomposing, mould arranges cold
But system.
(4) mold temperature is down to into 130 DEG C, then carries out the blank demoulding；
(5) vapor foaming and crosslinking：Prefoam blank after the demoulding is put into into temperature more than 95 DEG C
Decocting in water 4h in hot water, then in oven drying, that is, prepares hard sandwich crosslinked PVC expanded material,
Product mechanical property sees attached list.
Embodiment 3
A kind of method for preparing hard sandwich crosslinked PVC expanded material, using following steps：
(1) get the raw materials ready：By weight it is 100：10：120：2.5：12：30：3 weigh polrvinyl chloride tree
Fat, chlorinated polyethylene are dilute, isocyanates, ionic liquid surfactant, foaming agent, anhydride, stabilizer are
Raw material, and using azodiisobutyronitrile as initiator, wherein, the isocyanates for using are 4,4'- methylene
Double (carbanils), ionic liquid surfactant is following molecular structure：
Wherein, R1、R2、R3、R4H is, X is PF6, foaming agent is 2,2 '-azobis isobutyronitrile,
Anhydride is HHPA, and stabilizer is Ca Zn composite agent；
(2) pre- stirring and heating：To uniformly mix in each component input kneader in formula, control temperature
40 DEG C, mixing speed 500r/min makes raw material mix homogeneously, while avoiding foaming agent from decomposing, low boiling is molten
There is no chemical reaction in agent volatilization or each component；
(3) plasticizing forming：The mixed material for obtaining is poured in mould, mould closure is pressurizeed and heated,
110 DEG C of heating-up temperature, now compound generation polyreaction heat release, makes mold temperature be increased to 190 DEG C,
Mixed material plasticizing forming at such a temperature；To prevent intensification too high and reaction of decomposing, mould arranges cold
But system.
(4) mold temperature is down to into 150 DEG C, then carries out the blank demoulding；
(5) vapor foaming and crosslinking：Prefoam blank after the demoulding is put into into temperature more than 95 DEG C
Decocting in water 6h in hot water, then in oven drying, that is, prepares hard sandwich crosslinked PVC expanded material.
Embodiment 4
A kind of method for preparing hard sandwich crosslinked PVC expanded material, it is substantially the same manner as Example 1, it is different
Part is also to include pigment, UV absorbent in the present embodiment in raw material, Corvic
Weight accounts for the 40% of gross weight.
Embodiment 5
A kind of method for preparing hard sandwich crosslinked PVC expanded material, it is substantially the same manner as Example 1, it is different
Part is also to include packing material, phosphorous flame-retardant material, polrvinyl chloride tree in the present embodiment in raw material
The weight of fat accounts for the 60% of gross weight.
Table 1：Two kinds of different densities products (60,80kg/m3) mechanical property parameters
Claims (10)
1. a kind of method for preparing hard sandwich crosslinked PVC expanded material, it is characterised in that the method is adopted
Use following steps：
(1) get the raw materials ready：Weigh dilute Corvic, chlorinated polyethylene, isocyanates, ionic liquid surface
Activating agent, foaming agent, anhydride, stabilizer are raw material, and using azodiisobutyronitrile as initiator；
(2) pre- stirring and heating：To uniformly mix in each component input kneader in formula, control temperature
20-40 DEG C, mixing speed 500-1000r/min makes raw material mix homogeneously；
(3) plasticizing forming：The mixed material for obtaining is poured in mould, mould closure is pressurizeed and heated,
Heating-up temperature 100-110 DEG C, now compound generation polyreaction heat release, makes mold temperature be increased to 170-190
DEG C, mixed material plasticizing forming at such a temperature；
(4) mold temperature is down to into 130-150 DEG C, then carries out the blank demoulding；
(5) vapor foaming and crosslinking：Prefoam blank after the demoulding is put into into temperature more than 95 DEG C
Decocting in water 4-6h in hot water, then in oven drying, that is, prepares hard sandwich crosslinked PVC expanded material.
2. a kind of method for preparing hard sandwich crosslinked PVC expanded material according to claim 1,
Characterized in that, Corvic, dilute chlorinated polyethylene, isocyanates, ionic liquid in step (1)
Surfactant, foaming agent, anhydride, the weight ratio of stabilizer are 100：1-10：30-120：0.05-2.5：
3-12：1-30：3.
3. a kind of side for preparing hard sandwich crosslinked PVC expanded material according to claim 1 and 2
Method, it is characterised in that described isocyanates are with the different of two or more multiple isocyanate functional groups
Cyanate esters, including but not limited to 2,2 '-dimethyl -3,3 ', 5,5 '-triphenyl methane tetraisocyanate,
2,4 toluene diisocyanate, 2,6- toluene di-isocyanate(TDI)s, hexamethylene diisocyanate, diphenyl methane
Diisocyanate, 4,4' methylene bis (carbanil) or isophorone diisocyanate.
4. a kind of side for preparing hard sandwich crosslinked PVC expanded material according to claim 1 and 2
Method, it is characterised in that described ionic liquid surfactant is following molecular structure：
Wherein, R1、R2、R3、R4For H, OH, SH or Me,
5. a kind of side for preparing hard sandwich crosslinked PVC expanded material according to claim 1 and 2
Method, it is characterised in that described foaming agent is low boiling physical blowing agent or CBA.
6. a kind of method for preparing hard sandwich crosslinked PVC expanded material according to claim 5,
Characterized in that, described low boiling physical blowing agent is hexamethylene, described CBA is 2,2 '-
One or two in azobis isobutyronitrile or azodicarboamide.
7. a kind of side for preparing hard sandwich crosslinked PVC expanded material according to claim 1 and 2
Method, it is characterised in that described anhydride is the one kind in maleic acid bar, poly sebacic polyanhydride or HHPA,
Described stabilizer is the one kind in Oleum Glycines, oleum lini, magnesium oxide or Ca Zn composite metallic stabilizer.
8. a kind of method for preparing hard sandwich crosslinked PVC expanded material according to claim 1,
Characterized in that, also adding in raw material in pigment, UV absorbent, packing material or phosphorous flame-retardant material
One or more.
9. a kind of side for preparing hard sandwich crosslinked PVC expanded material according to claim 1 or 8
Method, it is characterised in that the weight of Corvic accounts for the 40-60% of gross weight in raw material.
10. a kind of method for preparing hard sandwich crosslinked PVC expanded material according to claim 1,
Characterized in that, cooling system is additionally provided with outside mould in step (3).
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432813A (en) * | 2011-03-21 | 2012-05-02 | 常州凯诺深冷科技工程有限公司 | Method for preparing PIR (polyisocyanurate) material with ionic liquid catalyst |
| CN103509273A (en) * | 2012-06-29 | 2014-01-15 | 威海维赛新材料科技有限公司 | Modified rigid cross-linked polyvinyl chloride foam and preparation method thereof |
| CN104672706A (en) * | 2015-02-13 | 2015-06-03 | 中国科学院长春应用化学研究所 | Suspension PVC (Polyvinyl Chloride) resin-based foaming material and preparation method thereof |
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2015
- 2015-11-04 CN CN201510741657.8A patent/CN106633467B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102432813A (en) * | 2011-03-21 | 2012-05-02 | 常州凯诺深冷科技工程有限公司 | Method for preparing PIR (polyisocyanurate) material with ionic liquid catalyst |
| CN103509273A (en) * | 2012-06-29 | 2014-01-15 | 威海维赛新材料科技有限公司 | Modified rigid cross-linked polyvinyl chloride foam and preparation method thereof |
| CN104672706A (en) * | 2015-02-13 | 2015-06-03 | 中国科学院长春应用化学研究所 | Suspension PVC (Polyvinyl Chloride) resin-based foaming material and preparation method thereof |
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