CN110028695A - A kind of polypropylene expanded high fondant-strength foaming concentrate and preparation method thereof - Google Patents
A kind of polypropylene expanded high fondant-strength foaming concentrate and preparation method thereof Download PDFInfo
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- CN110028695A CN110028695A CN201910349795.XA CN201910349795A CN110028695A CN 110028695 A CN110028695 A CN 110028695A CN 201910349795 A CN201910349795 A CN 201910349795A CN 110028695 A CN110028695 A CN 110028695A
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- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
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- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
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- C08J2203/02—CO2-releasing, e.g. NaHCO3 and citric acid
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- C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
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- C08J2403/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2403/12—Amylose; Amylopectin; Degradation products thereof
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- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
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Abstract
The present invention provides a kind of polypropylene expanded high fondant-strength foaming concentrates and preparation method thereof.Active inorganic fiber powder is obtained after inorfil powder with acicular texture is handled using surfactant, then with high amylopectin starch graft reaction, obtain needle-shaped type inorfil/high amylopectin starch composite material, finally high fondant-strength foaming concentrate is used to get polypropylene expanded with chemical foaming agent, nucleating agent, lubricant, dispersing agent, polypropylene mixing extruding pelletization.This method is by obtaining composite material in needle-shaped type inorfil surface grafting high amylopectin starch, and then masterbatch is mixed to prepare with foaming agent, after polypropene blended, the melt strength of expanded polypropylene can be effectively improved, improve foaming quality, and additive amount is small, can effectively realize lightening effect, at low cost, application prospect is good.
Description
Technical field
The present invention relates to polymeric material fields, and in particular to the preparation of polymer master batch, more particularly to one kind poly- third
Alkene foaming high fondant-strength foaming concentrate and preparation method thereof.
Background technique
Expanded polypropylene material, it is a kind of highly crystalline type polymer/gas recombination material of performance brilliance, with its uniqueness
And superior performance becomes fastest-rising environment-friendly novel resistance to compression at present and buffers heat-barrier material.Conventional method production polypropylene be
A kind of line style semicrystalline polymeric, the seldom branching of strand, molecular weight distribution relative narrower, this leads to its softening point and melts
Point very close to.Before temperature reaches fusing point, it is not flowed substantially, and after temperature is more than fusing point, melt strength sharply declines, this
Kind melt is difficult to encase gas;In addition, polypropylene, which is changed into crystalline state from molten state, can release a large amount of heat, by melt transform
It is longer the time required to for solid;In addition polypropylene air penetrability is high, and foamed gas is easily escaped.Therefore it is suitable for polypropylene expanded humidity province
Between it is narrow, foaming process is difficult to control, and easily causes in foaming process that steep that wall rupture, gas escape, abscess collapses and bubble merges.
Polyacrylic melt strength is low, significantly limits its range of work and application field, such as in thermo forming fields, by
Low in melt strength of polypropylene, container wall thickness is uneven when causing plastics sucking moulding or rupture;When extrusion coated, plain polypropylene
Apparent constriction and melt resonance are shown, thus phenomena such as edge curl, shrink occurs；When extrusion foaming, micro-pore wall is easily sent out
It is raw to rupture, expansion ratio is low etc..Therefore, to obtain the PP foam material of high quality, it is crucial for improving its melt strength.
Chinese invention patent application number 201510678792.2 discloses a kind of environment-protective water expanded polypropylene masterbatch, by with
The material of lower parts by weight is made: 5 ~ 10 parts of modifying agent, 5 ~ 10 parts of LDPE, micropore absorbs water 30 ~ 60 parts of inorganic foamed material, causes
0.01 ~ 0.2 part of agent, 1 ~ 3 part of surfactant, 0.1 ~ 0.5 part of plastic antioxidants, modifying agent is ethylene-vinyl acetate copolymer,
EP rubbers, ethylene-propylene diene copolymer, SBS, one or more of polybutene or POE.
It is female that Chinese invention patent application number 201710728117.5 discloses a kind of foaming for expandable polypropylene resin
Material and preparation method thereof, the present invention are used for the foaming concentrate of expandable polypropylene resin, the component comprising following parts by weight: polyethylene
40 parts of resin, 10 ~ 50 parts of sodium bicarbonate, 10 ~ 50 points of sodium citrate, 1 ~ 10 part of talcum powder, 1 ~ 5 part of stearic acid, 1 ~ 5 part of paraffin,
0.1 ~ 3 part of white oil, polyvinyl resin is the polyvinyl resin that its melt index is 40 ~ 50g/10min.The invention is used for polypropylene
The preparation method of resin expanded foaming concentrate passes through pelleter by being added to squeeze out in screw extruder by whole components again
Pelletizing is prepared.
Chinese invention patent application number 201210101328.3 discloses a kind of polypropylene expanded masterbatch and preparation method thereof,
It is to add azodicarbonamide, nano montmorillonite, glycerin monostearate, zinc stearate, poly- two using polyvinyl resin as matrix
Foaming concentrate is made in extruding pelletization after methylsiloxane, foam stabilizer mixing.
Chinese invention patent application number 201210086754.4 discloses a kind of microporous foam polypropylene material, material master
If being made by containing the following parts by weight: 80 ~ 95 parts of acrylic resin, 1 ~ 10 part of high bath strength acrylic resin,
1 ~ 20 part of masterbatch, 0.5 ~ 8 part of crosslinking agent, 0.8 ~ 10 part of assistant crosslinking agent, 0.1 ~ 1 part of foaming agent, 0.1 ~ 5 part of antioxidant of nucleation.
The present invention also discloses the preparation methods of above-mentioned microporous foam polypropylene material.
According to above-mentioned, in existing scheme for polypropylene expanded plastics because material self reason and processing technology not at
It is ripe, there are solution intensity is low, the undesirable defect of foaming effect.
Summary of the invention
The defects of there are solution intensity is low, and foaming quality is poor for the wider polypropylene expanded plastics of current application, this hair
It is bright to propose a kind of polypropylene expanded high fondant-strength foaming concentrate and preparation method thereof, so as in a small amount of addition preparation foaming
Polypropylene effectively improves polyacrylic solution intensity, and foaming quality is high, and lightening effect is good.
Specific technical solution of the present invention is as follows:
A kind of polypropylene expanded preparation method with high fondant-strength foaming concentrate, comprising the following steps:
(1) the inorfil powder with acicular texture is added in solvent, is uniformly dispersed and suspension is made, is subsequently added into surface
Activating agent carries out microwave treatment, and 3 ~ 8h is then freeze-dried at -10 ~ -30 DEG C, and the active inorganic fiber powder of acicular texture is made
Body；
(2) high amylopectin starch, ammonium persulfate/urea are caused system to be scattered in supercritical fluid, is sufficiently swollen, and carried and draw
Hair agent fully penetrates into inside starch granules, is subsequently added into active inorganic fiber powder made from step (1), carries out heating and adds
Pressure reaction, so that introducing large number of grafted chain on needle-shaped type inorfil surface, is filtered, washed after reaction, dries,
Needle-shaped type inorfil/high amylopectin starch composite material is made；
(3) by needle-shaped type inorfil/high amylopectin starch composite material made from step (2) and chemical foaming agent, nucleating agent, profit
Lubrication prescription, dispersing agent, polypropylene are added in high-speed mixer and are uniformly mixed, and are then transferred in Dual inoculation squeeze out and make
Grain, extrusion temperature are 80 ~ 100 DEG C and use high fondant-strength foaming concentrate to get polypropylene expanded.
The present invention is by the way that under the swelling action of supercritical fluid, high amylopectin starch successfully grafts on needle-shaped type inorfil
Surface introduces large number of grafted chain, by the masterbatch with it is polypropene blended, utilize numerous the connecing on needle-shaped type inorfil surface
Branch chain and polypropylene macromolecular chain carry out abundant physical entanglement, improve polyacrylic melt strength, greatly improvement foaming quality.
Preferably, step (1) the inorfil powder with acicular texture is calcium carbonate crystal whisker, wollastonite, Hai Pao
At least one of stone, shepardite, glass fibre, pyrophillite, nepheline.
Preferably, step (1) solvent is one of deionized water, dehydrated alcohol.
Preferably, step (1) surfactant is cetyl trimethylammonium bromide.
Preferably, the microwave power of step (1) described microwave treatment is 680 ~ 720W, and treatment temperature is 60 ~ 80 DEG C, processing
5 ~ 6min of time.
Preferably, in step (1), 20 ~ 40 parts by weight of inorfil powder, 56 ~ 78 weight of solvent with acicular texture
Part, 2 ~ 4 parts by weight of surfactant.
Preferably, step (2) supercritical fluid is supercritical water, supercritical carbon dioxide, supercritical nitrogen, surpasses and face
One of boundary's ethyl alcohol.
Preferably, step (2) it is described heating compressive reaction temperature be 60 ~ 70 DEG C, pressure be 20 ~ 25MPa, the time be 3 ~
5h。
Preferably, in step (2), 14 ~ 18 parts by weight of high amylopectin starch, 2 ~ 4 parts by weight of ammonium persulfate, 2 ~ 4 weight of urea
Part, 44 ~ 57 parts by weight of supercritical fluid, 25 ~ 30 parts by weight of active inorganic fiber powder.
Preferably, step (3) chemical foaming agent is sodium bicarbonate, ammonium hydrogen carbonate, 2,2'- azodiisobutyronitrile, idol
One of nitrogen dioctyl phthalate diisopropyl ester.
Preferably, step (3) nucleating agent be talcum powder, calcium carbonate, silica, calcium oxide, magnesia, carbon black,
At least one of mica.
Preferably, step (3) lubricant is stearic acid, in butyl stearate, oleamide, ethylene bis stearamide
It is at least one.
Preferably, step (3) dispersing agent is barium stearate, zinc stearate, calcium stearate, cadmium stearate, stearic acid
At least one of magnesium, copper stearate.
Preferably, in step (3), needle-shaped type inorfil/61 ~ 73 parts by weight of high amylopectin starch composite material, chemistry hair
15 ~ 20 parts by weight of infusion, 5 ~ 8 parts by weight of nucleating agent, 4 ~ 6 parts by weight of lubricant, 3 ~ 5 parts by weight of dispersing agent, polypropylene 10-20 weight
Measure part.
The present invention also provides the polypropylene expanded use high fondant-strength foaming concentrates that a kind of above-mentioned preparation method is prepared.
The inorfil powder with acicular texture is selected, is dispersed in solvent and suspension is made, surfactant 16 is added
Alkyl trimethyl ammonium bromide carries out microwave treatment, and the active inorganic fiber powder of acicular texture is obtained after freeze-drying；Height is propped up
Chain starch, ammonium persulfate/urea initiation system are dispersed in supercritical fluid and are sufficiently swollen, and carries initiator and fully permeate
Into inside starch granules, gained active inorganic fiber powder is added, heat up compressive reaction, draws on needle-shaped type inorfil surface
Enter large number of grafted chain, obtains needle-shaped type inorfil/high amylopectin starch composite material；By needle-shaped type inorfil/height
Amylopectin composite material mixes in a high speed mixer with auxiliary agents such as chemical foaming agent, nucleating agent, lubricant, dispersing agents
It is even, it is then added to extruding pelletization in Dual inoculation, obtains product.
The present invention provides a kind of polypropylene expanded high fondant-strength foaming concentrates and preparation method thereof, with the prior art
It compares, the feature and excellent effect protruded is:
1, propose to be grafted with high amylopectin starch needle-shaped type inorfil prepare it is polypropylene expanded with high fondant-strength foaming concentrate
Method.
2, it by obtaining composite material in needle-shaped type inorfil surface grafting high amylopectin starch, and then is mixed with foaming agent
Masterbatch is made, after polypropene blended, the melt strength of expanded polypropylene can be effectively improved, improve foaming quality.
3, the additive amount of foaming concentrate produced by the present invention is small, and modified effect is good, can effectively realize lightening effect, cost
Low, application prospect is good.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
Preparation process are as follows:
(1) the inorfil powder with acicular texture is added in solvent, is uniformly dispersed and suspension is made, is subsequently added into surface
Activating agent carries out microwave treatment, is then freeze-dried 5h at -20 DEG C, and the active inorganic fiber powder of acicular texture is made；Tool
The inorfil powder for having acicular texture is calcium carbonate crystal whisker；Solvent is deionized water；Surfactant is cetyl front three
Base ammonium bromide；The microwave power of microwave treatment is 690W, and treatment temperature is 68 DEG C, handles time 6min；Wherein, there is needle-shaped knot
28 parts by weight of inorfil powder, 69 parts by weight of solvent, 3 parts by weight of surfactant of structure；
(2) high amylopectin starch, ammonium persulfate/urea are caused system to be scattered in supercritical fluid, is sufficiently swollen, and carried and draw
Hair agent fully penetrates into inside starch granules, is subsequently added into active inorganic fiber powder made from step (1), carries out heating and adds
Pressure reaction, is filtered, washed after reaction, dries, needle-shaped type inorfil/high amylopectin starch composite material is made；It is overcritical
Fluid is supercritical water；The temperature of heating compressive reaction is 66 DEG C, pressure 23MPa, time 4h；Wherein, high amylopectin starch
15 parts by weight, 3 parts by weight of ammonium persulfate, 3 parts by weight of urea, 52 parts by weight of supercritical fluid, 27 weight of active inorganic fiber powder
Measure part；
(3) by needle-shaped type inorfil/high amylopectin starch composite material made from step (2) and chemical foaming agent, nucleating agent, profit
Lubrication prescription, dispersing agent, polypropylene are added in high-speed mixer and are uniformly mixed, and are then transferred in Dual inoculation squeeze out and make
Grain, extrusion temperature are 80 DEG C and use high fondant-strength foaming concentrate to get polypropylene expanded；Chemical foaming agent is sodium bicarbonate；At
Core agent is talcum powder；Lubricant is stearic acid；Dispersing agent is barium stearate；Wherein, needle-shaped type inorfil/high amylopectin starch is multiple
67 parts by weight of condensation material, 17 parts by weight of chemical foaming agent, 7 parts by weight of nucleating agent, 5 parts by weight of lubricant, 4 parts by weight of dispersing agent,
10 parts by weight of polypropylene.
Test method are as follows:
Expanded polypropylene melt strength: being added polypropylene matrix according to mass ratio 10% for foaming concentrate made from embodiment 1,
Mixing, which squeezes out, is made expanded polypropylene sample, measures foaming poly- third using German Rheotens71.97 type solution strength tester
The melt strength of alkene sample；
Expanded polypropylene density: polypropylene matrix, mixing is added according to mass ratio 10% in foaming concentrate made from embodiment 1
It squeezes out and expanded polypropylene sample is made, the density of expanded polypropylene sample is measured using density tester.
The melt strength of expanded polypropylene made from the foaming concentrate addition of the embodiment 1 measured as the above method and close
Degree is as shown in table 1.
Embodiment 2
Preparation process are as follows:
(1) the inorfil powder with acicular texture is added in solvent, is uniformly dispersed and suspension is made, is subsequently added into surface
Activating agent carries out microwave treatment, is then freeze-dried 8h at -10 DEG C, and the active inorganic fiber powder of acicular texture is made；Tool
The inorfil powder for having acicular texture is wollastonite；Solvent is dehydrated alcohol；Surfactant is cetyl trimethyl bromine
Change ammonium；The microwave power of microwave treatment is 690W, and treatment temperature is 65 DEG C, handles time 6min；Wherein, with acicular texture
25 parts by weight of inorfil powder, 73 parts by weight of solvent, 2 parts by weight of surfactant；
(2) high amylopectin starch, ammonium persulfate/urea are caused system to be scattered in supercritical fluid, is sufficiently swollen, and carried and draw
Hair agent fully penetrates into inside starch granules, is subsequently added into active inorganic fiber powder made from step (1), carries out heating and adds
Pressure reaction, is filtered, washed after reaction, dries, needle-shaped type inorfil/high amylopectin starch composite material is made；It is overcritical
Fluid is supercritical carbon dioxide；The temperature of heating compressive reaction is 62 DEG C, pressure 21MPa, time 4.5h；Wherein, high
15 parts by weight of amylopectin, 2 parts by weight of ammonium persulfate, 3 parts by weight of urea, 55 parts by weight of supercritical fluid, active inorganic fiber
26 parts by weight of powder；
(3) by needle-shaped type inorfil/high amylopectin starch composite material made from step (2) and chemical foaming agent, nucleating agent, profit
Lubrication prescription, dispersing agent, polypropylene are added in high-speed mixer and are uniformly mixed, and are then transferred in Dual inoculation squeeze out and make
Grain, extrusion temperature are 100 DEG C and use high fondant-strength foaming concentrate to get polypropylene expanded；Chemical foaming agent is ammonium hydrogen carbonate；At
Core agent is calcium carbonate；Lubricant is butyl stearate；Dispersing agent is zinc stearate；Wherein, needle-shaped type inorfil/high branch forms sediment
70 parts by weight of powder composite material, 16 parts by weight of chemical foaming agent, 6 parts by weight of nucleating agent, 5 parts by weight of lubricant, 3 weight of dispersing agent
Part, 15 parts by weight of polypropylene.
Test method are as follows:
Expanded polypropylene melt strength: being added polypropylene matrix according to mass ratio 10% for foaming concentrate made from embodiment 2,
Mixing, which squeezes out, is made expanded polypropylene sample, measures foaming poly- third using German Rheotens71.97 type solution strength tester
The melt strength of alkene sample；
Expanded polypropylene density: polypropylene matrix, mixing is added according to mass ratio 10% in foaming concentrate made from embodiment 2
It squeezes out and expanded polypropylene sample is made, the density of expanded polypropylene sample is measured using density tester.
The melt strength of expanded polypropylene made from the foaming concentrate addition of the embodiment 2 measured as the above method and close
Degree is as shown in table 1.
Embodiment 3
Preparation process are as follows:
(1) the inorfil powder with acicular texture is added in solvent, is uniformly dispersed and suspension is made, is subsequently added into surface
Activating agent carries out microwave treatment, is then freeze-dried 3h at -30 DEG C, and the active inorganic fiber powder of acicular texture is made；Tool
The inorfil powder for having acicular texture is sepiolite；Solvent is deionized water；Surfactant is cetyl trimethyl bromine
Change ammonium；The microwave power of microwave treatment is 710W, and treatment temperature is 68 DEG C, handles time 5min；Wherein, with acicular texture
35 parts by weight of inorfil powder, 71 parts by weight of solvent, 4 parts by weight of surfactant；
(2) high amylopectin starch, ammonium persulfate/urea are caused system to be scattered in supercritical fluid, is sufficiently swollen, and carried and draw
Hair agent fully penetrates into inside starch granules, is subsequently added into active inorganic fiber powder made from step (1), carries out heating and adds
Pressure reaction, is filtered, washed after reaction, dries, needle-shaped type inorfil/high amylopectin starch composite material is made；It is overcritical
Fluid is supercritical nitrogen；The temperature of heating compressive reaction is 68 DEG C, pressure 24MPa, time 3.5h；Wherein, Gao Zhilian
17 parts by weight of starch, 4 parts by weight of ammonium persulfate, 3 parts by weight of urea, 47 parts by weight of supercritical fluid, active inorganic fiber powder
29 parts by weight；
(3) by needle-shaped type inorfil/high amylopectin starch composite material made from step (2) and chemical foaming agent, nucleating agent, profit
Lubrication prescription, dispersing agent, polypropylene are added in high-speed mixer and are uniformly mixed, and are then transferred in Dual inoculation squeeze out and make
Grain, extrusion temperature are 80 DEG C and use high fondant-strength foaming concentrate to get polypropylene expanded；Chemical foaming agent is 2,2'- azo two
Isobutyronitrile；Nucleating agent is silica；Lubricant is oleamide；Dispersing agent is calcium stearate；Wherein, needle-shaped type inorfil/
64 parts by weight of high amylopectin starch composite material, 7 parts by weight of nucleating agent, 6 parts by weight of lubricant, are divided at 19 parts by weight of chemical foaming agent
4 parts by weight of powder, 15 parts by weight of polypropylene.
Test method are as follows:
Expanded polypropylene melt strength: being added polypropylene matrix according to mass ratio 10% for foaming concentrate made from embodiment 3,
Mixing, which squeezes out, is made expanded polypropylene sample, measures foaming poly- third using German Rheotens71.97 type solution strength tester
The melt strength of alkene sample；
Expanded polypropylene density: polypropylene matrix, mixing is added according to mass ratio 10% in foaming concentrate made from embodiment 3
It squeezes out and expanded polypropylene sample is made, the density of expanded polypropylene sample is measured using density tester.
The melt strength of expanded polypropylene made from the foaming concentrate addition of the embodiment 3 measured as the above method and close
Degree is as shown in table 1.
Embodiment 4
Preparation process are as follows:
(1) the inorfil powder with acicular texture is added in solvent, is uniformly dispersed and suspension is made, is subsequently added into surface
Activating agent carries out microwave treatment, is then freeze-dried 6h at -15 DEG C, and the active inorganic fiber powder of acicular texture is made；Tool
The inorfil powder for having acicular texture is shepardite；Solvent is dehydrated alcohol；Surfactant is cetyl trimethyl bromine
Change ammonium；The microwave power of microwave treatment is 680W, and treatment temperature is 60 DEG C, handles time 6min；Wherein, with acicular texture
20 parts by weight of inorfil powder, 78 parts by weight of solvent, 2 parts by weight of surfactant；
(2) high amylopectin starch, ammonium persulfate/urea are caused system to be scattered in supercritical fluid, is sufficiently swollen, and carried and draw
Hair agent fully penetrates into inside starch granules, is subsequently added into active inorganic fiber powder made from step (1), carries out heating and adds
Pressure reaction, is filtered, washed after reaction, dries, needle-shaped type inorfil/high amylopectin starch composite material is made；It is overcritical
Fluid is Supercritical Ethanol；The temperature of heating compressive reaction is 60 DEG C, pressure 20MPa, time 5h；Wherein, high branch forms sediment
14 parts by weight of powder, 2 parts by weight of ammonium persulfate, 2 parts by weight of urea, 57 parts by weight of supercritical fluid, active inorganic fiber powder 25
Parts by weight；
(3) by needle-shaped type inorfil/high amylopectin starch composite material made from step (2) and chemical foaming agent, nucleating agent, profit
Lubrication prescription, dispersing agent, polypropylene are added in high-speed mixer and are uniformly mixed, and are then transferred in Dual inoculation squeeze out and make
Grain, extrusion temperature are 100 DEG C and use high fondant-strength foaming concentrate to get polypropylene expanded；Chemical foaming agent is azoformic acid
Diisopropyl ester；Nucleating agent is calcium oxide；Lubricant is ethylene bis stearamide；Dispersing agent is cadmium stearate；Wherein, needle-shaped type without
Machine fiber/73 parts by weight of high amylopectin starch composite material, 15 parts by weight of chemical foaming agent, 5 parts by weight of nucleating agent, 4 weight of lubricant
Measure part, 3 parts by weight of dispersing agent, 15 parts by weight of polypropylene.
Test method are as follows:
Expanded polypropylene melt strength: being added polypropylene matrix according to mass ratio 10% for foaming concentrate made from embodiment 4,
Mixing, which squeezes out, is made expanded polypropylene sample, measures foaming poly- third using German Rheotens71.97 type solution strength tester
The melt strength of alkene sample；
Expanded polypropylene density: polypropylene matrix, mixing is added according to mass ratio 10% in foaming concentrate made from embodiment 4
It squeezes out and expanded polypropylene sample is made, the density of expanded polypropylene sample is measured using density tester.
The melt strength of expanded polypropylene made from the foaming concentrate addition of the embodiment 4 measured as the above method and close
Degree is as shown in table 1.
Embodiment 5
Preparation process are as follows:
(1) the inorfil powder with acicular texture is added in solvent, is uniformly dispersed and suspension is made, is subsequently added into surface
Activating agent carries out microwave treatment, is then freeze-dried 7h at -18 DEG C, and the active inorganic fiber powder of acicular texture is made；Tool
The inorfil powder for having acicular texture is glass fibre；Solvent is deionized water；Surfactant is cetyl trimethyl
Ammonium bromide；The microwave power of microwave treatment is 720W, and treatment temperature is 80 DEG C, handles time 5min；Wherein, there is acicular texture
40 parts by weight of inorfil powder, 56 parts by weight of solvent, 4 parts by weight of surfactant；
(2) high amylopectin starch, ammonium persulfate/urea are caused system to be scattered in supercritical fluid, is sufficiently swollen, and carried and draw
Hair agent fully penetrates into inside starch granules, is subsequently added into active inorganic fiber powder made from step (1), carries out heating and adds
Pressure reaction, is filtered, washed after reaction, dries, needle-shaped type inorfil/high amylopectin starch composite material is made；It is overcritical
Fluid is supercritical water；The temperature of heating compressive reaction is 70 DEG C, pressure 25MPa, time 3h；Wherein, high amylopectin starch
18 parts by weight, 4 parts by weight of ammonium persulfate, 4 parts by weight of urea, 44 parts by weight of supercritical fluid, 30 weight of active inorganic fiber powder
Measure part；
(3) by needle-shaped type inorfil/high amylopectin starch composite material made from step (2) and chemical foaming agent, nucleating agent, profit
Lubrication prescription, dispersing agent, polypropylene are added in high-speed mixer and are uniformly mixed, and are then transferred in Dual inoculation squeeze out and make
Grain, extrusion temperature are 90 DEG C and use high fondant-strength foaming concentrate to get polypropylene expanded；Chemical foaming agent is sodium bicarbonate；At
Core agent is carbon black；Lubricant is stearic acid；Dispersing agent is magnesium stearate；Wherein, needle-shaped type inorfil/high amylopectin starch is compound
61 parts by weight of material, 8 parts by weight of nucleating agent, 6 parts by weight of lubricant, 5 parts by weight of dispersing agent, are gathered at 20 parts by weight of chemical foaming agent
18 parts by weight of propylene.
Test method are as follows:
Expanded polypropylene melt strength: being added polypropylene matrix according to mass ratio 10% for foaming concentrate made from embodiment 5,
Mixing, which squeezes out, is made expanded polypropylene sample, measures foaming poly- third using German Rheotens71.97 type solution strength tester
The melt strength of alkene sample；
Expanded polypropylene density: polypropylene matrix, mixing is added according to mass ratio 10% in foaming concentrate made from embodiment 5
It squeezes out and expanded polypropylene sample is made, the density of expanded polypropylene sample is measured using density tester.
The melt strength of expanded polypropylene made from the foaming concentrate addition of the embodiment 5 measured as the above method and close
Degree is as shown in table 1.
Comparative example 1
Preparation process are as follows:
(1) the inorfil powder with acicular texture is added in solvent, is uniformly dispersed and suspension is made, is subsequently added into surface
Activating agent carries out microwave treatment, is then freeze-dried 5h at -20 DEG C, and the active inorganic fiber powder of acicular texture is made；Tool
The inorfil powder for having acicular texture is nepheline；Solvent is dehydrated alcohol；Surfactant is cetyl trimethyl bromination
Ammonium；The microwave power of microwave treatment is 700W, and treatment temperature is 70 DEG C, handles time 5.5min；Wherein, with acicular texture
30 parts by weight of inorfil powder, 67 parts by weight of solvent, 3 parts by weight of surfactant；
(2) by the active inorganic fiber powder of acicular texture made from step (1) and chemical foaming agent, nucleating agent, lubricant, point
Powder, polypropylene are added in high-speed mixer and are uniformly mixed, and are then transferred in Dual inoculation and carry out extruding pelletization, squeeze out temperature
Degree is for 100 DEG C to get foaming concentrate；Chemical foaming agent is diisopropyl azodiformate；Nucleating agent is mica；Lubricant is hard
Resin acid butyl ester；Dispersing agent is copper stearate；Wherein, 67 parts by weight of active inorganic fiber powder, the chemical foaming agent of acicular texture
18 parts by weight, 6 parts by weight of nucleating agent, 5 parts by weight of lubricant, 4 parts by weight of dispersing agent, 15 parts by weight of polypropylene.
Test method are as follows:
Expanded polypropylene melt strength: being added polypropylene matrix according to mass ratio 10% for foaming concentrate made from comparative example 1,
Mixing, which squeezes out, is made expanded polypropylene sample, measures foaming poly- third using German Rheotens71.97 type solution strength tester
The melt strength of alkene sample；
Expanded polypropylene density: polypropylene matrix, mixing is added according to mass ratio 10% in foaming concentrate made from comparative example 1
It squeezes out and expanded polypropylene sample is made, the density of expanded polypropylene sample is measured using density tester.
The melt strength of expanded polypropylene made from the foaming concentrate addition of the comparative example 1 measured as the above method and close
Degree is as shown in table 1.
Table 1:
Claims (10)
1. a kind of polypropylene expanded preparation method with high fondant-strength foaming concentrate, which comprises the following steps:
(1) the inorfil powder with acicular texture is added in solvent, is uniformly dispersed and suspension is made, is subsequently added into surface
Activating agent carries out microwave treatment, and 3 ~ 8h is then freeze-dried at -10 ~ -30 DEG C, and the active inorganic fiber powder of acicular texture is made
Body；
(2) high amylopectin starch, ammonium persulfate/urea are caused system to be scattered in supercritical fluid, is sufficiently swollen, and carried and draw
Hair agent fully penetrates into inside starch granules, is subsequently added into active inorganic fiber powder made from step (1), carries out heating and adds
Pressure reaction, so that introducing large number of grafted chain on needle-shaped type inorfil surface, is filtered, washed after reaction, dries,
Needle-shaped type inorfil/high amylopectin starch composite material is made；
(3) by needle-shaped type inorfil/high amylopectin starch composite material made from step (2) and chemical foaming agent, nucleating agent, profit
Lubrication prescription, dispersing agent, polypropylene are added in high-speed mixer and are uniformly mixed, and are then transferred in Dual inoculation squeeze out and make
Grain, extrusion temperature are 80-100 DEG C and use high fondant-strength foaming concentrate to get polypropylene expanded.
2. a kind of polypropylene expanded preparation method with high fondant-strength foaming concentrate, feature exist according to claim 1
In: step (1) the inorfil powder with acicular texture is calcium carbonate crystal whisker, wollastonite, sepiolite, shepardite, glass
At least one of glass fiber, pyrophillite, nepheline, the solvent are one of deionized water, dehydrated alcohol, and the surface is living
Property agent be cetyl trimethylammonium bromide.
3. a kind of polypropylene expanded preparation method with high fondant-strength foaming concentrate, feature exist according to claim 1
In: the microwave power of step (1) described microwave treatment is 680 ~ 720W, and treatment temperature is 60 ~ 80 DEG C, handles 5 ~ 6min of time.
4. a kind of polypropylene expanded preparation method with high fondant-strength foaming concentrate, feature exist according to claim 1
In: in step (1), 20 ~ 40 parts by weight of inorfil powder, 56 ~ 78 parts by weight of solvent, surfactant with acicular texture
2 ~ 4 parts by weight.
5. a kind of polypropylene expanded preparation method with high fondant-strength foaming concentrate, feature exist according to claim 1
In: step (2) supercritical fluid be supercritical water, supercritical carbon dioxide, supercritical nitrogen, one in Supercritical Ethanol
Kind.
6. a kind of polypropylene expanded preparation method with high fondant-strength foaming concentrate, feature exist according to claim 1
In: the temperature of step (2) the heating compressive reaction is 60 ~ 70 DEG C, and pressure is 20 ~ 25MPa, and the time is 3 ~ 5h.
7. a kind of polypropylene expanded preparation method with high fondant-strength foaming concentrate, feature exist according to claim 1
In: in step (2), 14 ~ 18 parts by weight of high amylopectin starch, 2 ~ 4 parts by weight of ammonium persulfate, 2 ~ 4 parts by weight of urea, supercritical fluid
44 ~ 57 parts by weight, 25 ~ 30 parts by weight of active inorganic fiber powder.
8. a kind of polypropylene expanded preparation method with high fondant-strength foaming concentrate, feature exist according to claim 1
It is that sodium bicarbonate, ammonium hydrogen carbonate, 2,2'- azodiisobutyronitrile, azoformic acid two are different in: step (3) chemical foaming agent
One of propyl ester, the nucleating agent be talcum powder, calcium carbonate, silica, calcium oxide, magnesia, carbon black, in mica extremely
Few one kind, the lubricant are at least one of stearic acid, butyl stearate, oleamide, ethylene bis stearamide, described point
Powder is at least one of barium stearate, zinc stearate, calcium stearate, cadmium stearate, magnesium stearate, copper stearate.
9. a kind of polypropylene expanded preparation method with high fondant-strength foaming concentrate, feature exist according to claim 1
In: in step (3), needle-shaped type inorfil/61 ~ 73 parts by weight of high amylopectin starch composite material, 15 ~ 20 weight of chemical foaming agent
Part, 5 ~ 8 parts by weight of nucleating agent, 4 ~ 6 parts by weight of lubricant, 3 ~ 5 parts by weight of dispersing agent, polypropylene 10-20 parts by weight.
It is foamed 10. one kind that any one of claim 1 ~ 9 preparation method is prepared is polypropylene expanded with high fondant-strength
Masterbatch.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102604223A (en) * | 2012-03-16 | 2012-07-25 | 武汉富蒂亚新型材料有限公司 | Polypropylene resin foam concentrate and preparation method thereof |
| CN105566831A (en) * | 2016-03-07 | 2016-05-11 | 惠州市环美盛新材料有限公司 | Water-foamed, antibacterial and air-permeable microporous film masterbatch, film and preparation method thereof |
| CN106432897A (en) * | 2015-08-07 | 2017-02-22 | 现代自动车株式会社 | Foamable masterbatch and polyolefin resin composition with excellent expandability and direct metallizing property |
| US20180002505A1 (en) * | 2016-07-04 | 2018-01-04 | Hyundai Motor Company | Polypropylene resin composition with improved foaming capability |
-
2019
- 2019-04-28 CN CN201910349795.XA patent/CN110028695A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102604223A (en) * | 2012-03-16 | 2012-07-25 | 武汉富蒂亚新型材料有限公司 | Polypropylene resin foam concentrate and preparation method thereof |
| CN106432897A (en) * | 2015-08-07 | 2017-02-22 | 现代自动车株式会社 | Foamable masterbatch and polyolefin resin composition with excellent expandability and direct metallizing property |
| CN105566831A (en) * | 2016-03-07 | 2016-05-11 | 惠州市环美盛新材料有限公司 | Water-foamed, antibacterial and air-permeable microporous film masterbatch, film and preparation method thereof |
| US20180002505A1 (en) * | 2016-07-04 | 2018-01-04 | Hyundai Motor Company | Polypropylene resin composition with improved foaming capability |
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