CN106750940A - Modified polypropylene flame redardant foamed board of a kind of hydridization melamino-formaldehyde silica aerogel and preparation method thereof - Google Patents

Modified polypropylene flame redardant foamed board of a kind of hydridization melamino-formaldehyde silica aerogel and preparation method thereof Download PDF

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Publication number
CN106750940A
CN106750940A CN201611195807.0A CN201611195807A CN106750940A CN 106750940 A CN106750940 A CN 106750940A CN 201611195807 A CN201611195807 A CN 201611195807A CN 106750940 A CN106750940 A CN 106750940A
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hydridization
silica aerogel
preparation
carbamide
foamed board
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唐晋
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Fuyang Three Packing Materials Co Ltd
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Fuyang Three Packing Materials Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/12—Polypropene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • 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
    • 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
    • C08J9/102—Azo-compounds
    • C08J9/103—Azodicarbonamide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00—Foams characterized by the expanding agent
    • C08J2203/04—N2 releasing, ex azodicarbonamide or nitroso compound
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/10—Homopolymers or copolymers of propene
    • C08J2323/12—Polypropene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2361/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
    • C08J2361/04—Condensation polymers of aldehydes or ketones with phenols only
    • C08J2361/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2461/00—Characterised by the use of condensation polymers of aldehydes or ketones; Derivatives of such polymers
    • C08J2461/04—Condensation polymers of aldehydes or ketones with phenols only
    • C08J2461/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/14—Applications used for foams
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)

Abstract

Polypropylene flame redardant foamed board being modified the invention discloses a kind of hydridization melamino-formaldehyde silica aerogel and preparation method thereof, the expanded material has good toughness and more preferable heat endurance, and melt strength is improved；The hydridization melamino-formaldehyde silica aerogel of addition has unique nano-porous structure, it is adsorbable in resin melt in foaming process, not only can further improve melt strength, the heat-proof combustion-resistant performance of resinite can also effectively be improved, this hybrid aerogel can play good synergistic effect to the fire retardant in system, and the consumption of fire retardant is effectively controlled；The PP foam material feature of environmental protection prepared by the present invention is good, and frothing percentage is high, light thermal-insulation, hydrophobic corrosion protection, economy and durability, has greatly widened the use scope of conventional polypropylene expanded material.

Description

A kind of modified polypropylene flame redardant foamed board of hydridization carbamide silica aerogel And preparation method thereof
Technical field
The present invention relates to High-molecular flame-retardant foam material technical field, more particularly to a kind of hydridization carbamide silicon Modified polypropylene flame redardant foamed board of aeroge and preparation method thereof.
Background technology
High molecular foam material is a kind of special material constituted by polymer and comprising gas cells, with general polymer Material is compared to having that density is low, specific strength is high, sound insulation damping, the advantage such as heat-insulated, answered extensively in fields such as commodity packaging, pads With.The high molecular foam material as packaging common in the market has polyethylene foam-material, PP foam material, gathers Styrene expanded material, EVA expanded materials etc., wherein PP foam material are a kind of environment-friendly type expanded materials, cost performance is excellent, Can repeatedly recycle, application prospect is preferable.Difficult point polypropylene expanded at present is that after processing temperature exceedes fusing point, PP's is molten The very fast decline of body intensity, the ability of melt parcel gas declines, and causes abscess to collapse, it is difficult to qualified foaming product is obtained.Remove Outside this, the inflammability of organic foam material be also user must not careless problem, expanded material is carried out flame-retardant modified With important practical application meaning.
In order to improve the anti-flammability of PP foam material, many researchers have done substantial amounts of work, most common method The flame retardant effect of material is improved for addition fire retardant, also has multiple material synergy to improve polyacrylic anti-flammability, Wherein expansion type flame retardant（IFR）There is the high and low cigarette of flame retarding efficiency, low toxicity, but itself and PP poor compatibilities, usage amount Greatly, the easy moisture absorption, it will usually cause polyacrylic mechanical property to substantially reduce, will also produce bad shadow to melt in foaming process Ring, foaming effect is poor, so as to influence performance.《Nano silicon activeness and quietness expansion type flame-retarding COPP performance Research》One text is by the mechanical property of adding the method for nano silicon to improve expansion type inflaming retarding polypropylene, nanometer two The addition of silica improving harmful effect that fire retardant is produced to polypropylene to a certain degree, but there are some researches show receiving Rice silica consumption have vital influence to polypropylene expanded process, when consumption is excessive nano-particle easily reunite and Cause frothing percentage low, but too low nano material not can overcome the disadvantages that harmful effect of the fire retardant to system, finally occur in that product Foaming effect is good, poor fire, otherwise flame retardant effect is preferably, but the predicament of foaming effect difference.
The distinctive nanoporous network structure of aeroge makes it show to be permitted in optics, calorifics, electricity, acoustics etc. field Many unique properties, with SiO2Aeroge is that the aerogel products of representative show huge application prospect in multiple fields, It has the multi-effect such as heat-insulated, insulation, fire-retardant, if being applied in high molecular foam material, by the foaming to material Journey has a good facilitation, but SiO2Mechanical Properties of Aerogels is not good, and fragility is larger, it is necessary to be further modified to it Treatment.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of hydridization carbamide silicon airsetting Modified polypropylene flame redardant foamed board of glue and preparation method thereof, it is special using the unique mechanical property of hybridized aerogel material and structure Point, treatment is modified to resin melt, obtains the expanded polypropylene material with good flame retardant effect and mechanical property.
The present invention is achieved by the following technical solutions：
A kind of modified polypropylene flame redardant foamed board of hydridization carbamide silica aerogel, the expanded material is by following weight The raw material of part is obtained：Polypropylene 65-80, maleic anhydride stem grafting polyolefin elastomer 10-14, ethylene-vinyl acetate copolymer 8- 12nd, PIC 4-5, pentaerythrite 4-8, organic phosphorus flame retardant 1-2, blowing agent AC 1-5, antioxidant 0.1-0.2, trimerization Cyanamide 2-5, mass fraction are formalin 2-5, appropriate natrium carbonicum calcinatum, tetraethyl orthosilicate 2-3, the absolute ethyl alcohol of 37-40% 5-8, silane coupler 0.1-0.2, concentration are oxalic acid solution 10-12, the deionized water 15-20 of 0.01mol/L.
Described organic phosphorus flame retardant is phosphate toluene diphenyl ester, triphenyl phosphate, IPPP, bis-phenol One or more in A- double (diphenyl phosphoester), tricresyl phosphate, tricresyl phosphate (2- chloropropyls) ester, annular phosphates Mixing.
A kind of preparation method bag of the modified polypropylene flame redardant foamed board of described hydridization carbamide silica aerogel Include following steps：
（1）First by tetraethyl orthosilicate input absolute ethyl alcohol, oxalic acid aqueous solution is added after being uniformly mixed, in 50-60 DEG C of water Stirring reaction 3-5h under the conditions of bath, is made Ludox standby；
（2）And natrium carbonicum calcinatum will be added to adjust successively by melamine, formalin, deionized water input reaction vessel Section system pH is 8-9, stirring reaction 20-30min is continued after then system heating stirring is completely dissolved to melamine, most System is cooled to room temperature afterwards, and adds step（1）The Ludox of preparation, well mixed rear system is placed in 50-60 DEG C of condition 30-40h, takes out gel successively through water, ethanol cleaning displacement 2-3 times after gel is complete, and solvent and unreacted reactant are removed completely Material, is finally processed gel using Supercritical Drying Technology, at 45-50 DEG C, 4-5h is dried under conditions of 10-15MPa, is obtained Hydridization carbamide silica aerogel is standby；
（3）By step（2）The hydridization carbamide silica aerogel of preparation mix with silane coupler after ball-milling treatment 30- 50min, crosses 100 mesh sieves, is well mixed during resulting material is put into high-speed mixer together with other surplus stocks, then will be mixed The material for getting togather is delivered in extruder, material heated melting, mixing, extruding, foaming in screw cylinder, then extruded machine Product is obtained final product after extrusion, mould shape, wherein barrel temperature is 185-205 DEG C, and screw speed is 40-50 revs/min, mould temperature It is 165-180 DEG C to spend, and pressure is 1-5MPa.
PP foam material prepared by the present invention uses polypropylene, maleic anhydride stem grafting polyolefin elastomer, ethene-vinegar , used as resin binder, this resin binder improves conventional polypropylene compatibility difference for sour ethylene copolymer and PIC Defect, with good toughness and more preferable heat endurance, melt strength is improved；The hydridization carbamide of addition Silica aerogel has unique nano-porous structure, adsorbable in resin melt in foaming process, not only can be further Improve melt strength, moreover it is possible to which the effective heat-proof combustion-resistant performance for improving resinite, this hybrid aerogel can be to the resistance in system Good synergistic effect is played in combustion agent, and the consumption of fire retardant is effectively controlled；PP foam material ring prepared by the present invention Guarantor property is good, and frothing percentage is high, light thermal-insulation, hydrophobic corrosion protection, economy and durability, has greatly widened making for conventional polypropylene expanded material Use scope.
Specific embodiment
A kind of modified polypropylene flame redardant foamed board of hydridization melamino-formaldehyde silica aerogel, the expanded material is by following heavy The raw material for measuring part is obtained：Polypropylene 65, maleic anhydride stem grafting polyolefin elastomer 10, ethylene-vinyl acetate copolymer 8, poly- isocyanide Acid esters 4, pentaerythrite 4, phosphate toluene diphenyl ester 1, blowing agent AC 1, antioxidant 0.1, melamine 2, mass fraction are 37% Formalin 2, appropriate natrium carbonicum calcinatum, tetraethyl orthosilicate 2, absolute ethyl alcohol 5, silane coupler 0.1, concentration be The oxalic acid solution 10 of 0.01mol/L, deionized water 15.
The preparation method of the polypropylene flame redardant foamed board is comprised the following steps：
（1）First by tetraethyl orthosilicate input absolute ethyl alcohol, oxalic acid aqueous solution is added after being uniformly mixed, in 50 DEG C of water-bath bars Stirring reaction 3h under part, is made Ludox standby；
（2）And natrium carbonicum calcinatum will be added to adjust successively by melamine, formalin, deionized water input reaction vessel Section system pH is 8, and stirring reaction 20min is continued after then system heating stirring is completely dissolved to melamine, finally will System is cooled to room temperature, and adds step（1）The Ludox of preparation, system places 30h in 50 DEG C of conditions after being well mixed, and waits to coagulate Glue takes out gel successively through water, ethanol cleaning displacement 2 times afterwards completely, solvent and unreacted material is removed completely, finally using super Critical dry technology is processed gel, at 45 DEG C, 4h is dried under conditions of 10MPa, obtains hydridization melamino-formaldehyde silicon gas Gel is standby；
（3）By step（2）The hydridization melamino-formaldehyde silica aerogel of preparation mix with silane coupler after ball-milling treatment 30min, crosses 100 mesh sieves, is well mixed during resulting material is put into high-speed mixer together with other surplus stocks, then will be mixed The material for getting togather is delivered in extruder, material heated melting, mixing, extruding, foaming in screw cylinder, then extruded machine Product is obtained final product after extrusion, mould shape, wherein barrel temperature is 185 DEG C, and screw speed is 50 revs/min, and mold temperature is 165 DEG C, pressure is 1MPa.
Prepared foamed board is taken into standard specimen, and follows relevant criterion carries out performance test, and test result is：
Cell density：6.25×106Individual/cm3；
Melt mass flow rate：0.70g/10min ；
Shore A hardness：76.4；
Tensile strength：17.4MPa；
Elongation percentage：602%；
UL94 flame retardant ratings：V0；
Limited oxygen index：28.3.

Claims (3)

1. a kind of polypropylene flame redardant foamed board that hydridization carbamide silica aerogel is modified, it is characterised in that the foaming material Material is obtained by the raw material of following weight portion：Polypropylene 65-80, maleic anhydride stem grafting polyolefin elastomer 10-14, ethyl vinyl acetate Ethylene copolymer 8-12, PIC 4-5, pentaerythrite 4-8, organic phosphorus flame retardant 1-2, blowing agent AC 1-5, antioxidant 0.1-0.2, melamine 2-5, mass fraction are formalin 2-5, appropriate natrium carbonicum calcinatum, the tetraethyl orthosilicate of 37-40% 2-3, absolute ethyl alcohol 5-8, silane coupler 0.1-0.2, concentration are oxalic acid solution 10-12, the deionized water 15- of 0.01mol/L 20。
2. the polypropylene flame redardant foamed board that a kind of hydridization carbamide silica aerogel as claimed in claim 1 is modified, its It is characterised by, described organic phosphorus flame retardant is phosphate toluene diphenyl ester, triphenyl phosphate, IPPP, double One or more in phenol A- double (diphenyl phosphoester), tricresyl phosphate, tricresyl phosphate (2- chloropropyls) ester, annular phosphates Mixing.
3. the polypropylene flame redardant foamed board that a kind of hydridization carbamide silica aerogel as claimed in claim 1 is modified Preparation method, it is characterised in that described preparation method is comprised the following steps：
（1）First by tetraethyl orthosilicate input absolute ethyl alcohol, oxalic acid aqueous solution is added after being uniformly mixed, in 50-60 DEG C of water Stirring reaction 3-5h under the conditions of bath, is made Ludox standby；
（2）And natrium carbonicum calcinatum will be added to adjust successively by melamine, formalin, deionized water input reaction vessel Section system pH is 8-9, stirring reaction 20-30min is continued after then system heating stirring is completely dissolved to melamine, most System is cooled to room temperature afterwards, and adds step（1）The Ludox of preparation, well mixed rear system is placed in 50-60 DEG C of condition 30-40h, takes out gel successively through water, ethanol cleaning displacement 2-3 times after gel is complete, and solvent and unreacted reactant are removed completely Material, is finally processed gel using Supercritical Drying Technology, at 45-50 DEG C, 4-5h is dried under conditions of 10-15MPa, is obtained Hydridization carbamide silica aerogel is standby；
（3）By step（2）The hydridization carbamide silica aerogel of preparation mix with silane coupler after ball-milling treatment 30- 50min, crosses 100 mesh sieves, is well mixed during resulting material is put into high-speed mixer together with other surplus stocks, then will be mixed The material for getting togather is delivered in extruder, material heated melting, mixing, extruding, foaming in screw cylinder, then extruded machine Product is obtained final product after extrusion, mould shape, wherein barrel temperature is 185-205 DEG C, and screw speed is 40-50 revs/min, mould temperature It is 165-180 DEG C to spend, and pressure is 1-5MPa.
CN201611195807.0A 2016-12-22 2016-12-22 Modified polypropylene flame redardant foamed board of a kind of hydridization melamino-formaldehyde silica aerogel and preparation method thereof Pending CN106750940A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109174006A (en) * 2018-08-07 2019-01-11 济南大学 A kind of preparation method of ion liquid modified melamine-formaldehyde aeroge coating solid phase micro-extraction fiber
CN110387066A (en) * 2019-07-17 2019-10-29 北京化工大学 A kind of preparation of microencapsulation modified flame-retardant agent
CN112795048A (en) * 2021-02-03 2021-05-14 峰特(浙江)新材料有限公司 Mixed aerogel modified melamine foam and application thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102604202A (en) * 2011-12-26 2012-07-25 上海金发科技发展有限公司 Glass fiber reinforced halogen-free flame-retardant polypropylene composite material and preparation method thereof
CN103980624A (en) * 2014-05-19 2014-08-13 四川大学 Halogen-free flame-retardant polystyrene foam composite material and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102604202A (en) * 2011-12-26 2012-07-25 上海金发科技发展有限公司 Glass fiber reinforced halogen-free flame-retardant polypropylene composite material and preparation method thereof
CN103980624A (en) * 2014-05-19 2014-08-13 四川大学 Halogen-free flame-retardant polystyrene foam composite material and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109174006A (en) * 2018-08-07 2019-01-11 济南大学 A kind of preparation method of ion liquid modified melamine-formaldehyde aeroge coating solid phase micro-extraction fiber
CN109174006B (en) * 2018-08-07 2021-07-23 济南大学 Preparation method of ionic liquid modified melamine-formaldehyde aerogel coating solid-phase microextraction fiber
CN110387066A (en) * 2019-07-17 2019-10-29 北京化工大学 A kind of preparation of microencapsulation modified flame-retardant agent
CN112795048A (en) * 2021-02-03 2021-05-14 峰特(浙江)新材料有限公司 Mixed aerogel modified melamine foam and application thereof

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Application publication date: 20170531