CN102329447A - High-efficiency heat-insulation environmentally-friendly flame-retardant modified polyolefin indoor heat-insulation foam and preparation method thereof - Google Patents
High-efficiency heat-insulation environmentally-friendly flame-retardant modified polyolefin indoor heat-insulation foam and preparation method thereof Download PDFInfo
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Abstract
The invention relates to high-efficiency heat-insulation environmentally-friendly flame-retardant modified polyolefin indoor heat-insulation foam and a preparation method thereof. The preparation method comprises the following steps of: kneading low-density polyethylene resin, a composite flame retardant, an anti-smoke agent, an antioxidant and a lubricant at normal temperature, then discharging to an internal mixer for internal mixing, then discharging to a single-screw extrusion granulator, and carrying out melting, plastication and granulation to obtain a master batch A; adding low-density polyethylene resin to a high-speed mixer, then adding azobisformamide, talc powder, a lubricant and zinc stearate, kneading at normal temperature, and then discharging to a single-screw extruder for granulating to obtain a master batch D; adding low-density polyethylene resin, ethylene-vinyl acetate copolymer, ethylene propylene terpolymer, the master batch A, a master batch B, hollow ceramic microbeads, a rheologic agent and a lubricant to a high-speed mixer, kneading at normal temperature for 3 minutes, then discharging to a single-screw extruder, and extruding into sheets; carrying out radiation cross-linking on the extruded sheets through an electronic accelerator; placing the cross-linked sheets in a foaming furnace for foaming; and coating expansible fireproof paint on the surface of the foam.
Description
Technical field
The present invention relates to a kind of effectively insulating environmental protection flame retardant modified polyolefin indoor heat insulating foam and preparation method thereof.
Background technology
The residential housing energy consumption has accounted for 32% of national energy consumption at present.The nearly 40,000,000,000 square metres building of China is the highly energy-consuming building basically, and the unit surface heating energy consumption is equivalent to 2-3 times of the close developed country of weather condition.The annual new building of China is nearly 2,000,000,000 square metres at present, surpasses the summation of all developed country's construction amounts, but is still the high energy consumption building more than 95%.Prediction is promptly arrived the year two thousand twenty 10 years of future, and China also will build up about 20,000,000,000 square metres of buildings.If or else take conservation measures, do not carry out energy-saving building materials, the year two thousand twenty building energy consumption will reach 1,100,000,000 tons of standard coal equivalents, be equivalent to build at present three times of institute's consumes energy.
Building thermal insulation material mainly contains mineral-type and organic class at present, and inorganic heat insulation material is a kind of heat insulating energy saving material that is used for external rendering in the buildings, and free glass bead is mainly arranged; Pearlstone; Closed perlite, rock wool, foamed concrete etc.; Have antifreeze, the ageing-resistant and cheap characteristics such as price of fire prevention, but the insulation poor thermal efficiency.Organic insulation material mainly is an expanded plastic; Main products is polystyrene foamed plastics, phenolic aldehyde foam and urethane foam; Main drawback is inflammable, easy drip melt, and combustion fumes is big, toxicity is big, and ignition energy produces prussic acid gas; In case presence of fire is very big to the human body toxic, and shortcoming such as heat insulation effect is bad.
Summary of the invention
It is low to the objective of the invention is to overcome the inorganic heat insulation material insulating efficiency; Shortcomings such as fire-retardant not up to standard, the not environmental protection of organic insulation material, burning fuming amount be big, discharge toxic and harmful, heat insulation effect is low, provide a kind of heat insulation and preservation effect good, reach that the fire-retardant requirement of A level, environment-protecting asepsis are tasteless, cross-linked type macromolecule foam material and preparation method thereof.
For realizing above purpose, technical solution of the present invention is: a kind of preparation method of effectively insulating environmental protection flame retardant modified polyolefin indoor heat insulating foam, and this preparation method may further comprise the steps successively:
The first step: the preparation of fire-retardant master granule A: get the ldpe resin of 20 weight parts, the composite flame-retardant agent of 30 weight parts, the smoke suppressor of 8 weight parts, the antioxidant 1010 of 0.3 weight part, the lubricant of 0.6 weight part earlier; Normal temperature was mediated 3 – 5 minutes down; Enter the material group after banburying in the Banbury mixer gets banburying then; The banburying temperature is 100 ± 5 ℃; The banburying time is 6 – 8 minutes, the group of the material after the banburying is entered in single screw extruder pelletizer through forced feed again, and the fusion plastification granulation makes flame-retardant master batch A; Said composite flame-retardant agent is the compound of micro encapsulation ammonium polyphosphate and zinc borate, and this compound is mixed by the micro encapsulation ammonium polyphosphate of 90wt% and the zinc borate of 10wt%; Said lubricant is a polyethylene wax; Said smoke suppressor is an ammonium octamolybdate;
Second step: the preparation of foaming concentrate B: the ldpe resin of getting 50 weight parts earlier adds in the high mixer; Add the AC whipping agent Cellmic C 121 of 15 weight parts, the talcum powder of 0.8 weight part, the lubricant of 2 weight parts, the Zinic stearas of 1 weight part again; Normal temperature was mediated 3 minutes down, entered the single screw extrusion machine granulation then to obtain foaming concentrate D;
The 3rd step: the preparation of sheet material C: get the ldpe resin of 5 –, 20 weight parts, the Yi Xi – acetate ethylene copolymer of 23 –, 30 weight parts, the terpolymer EP rubber of 2 –, 10 weight parts, the flame-retardant master batch A of 20-30 weight part, the foaming concentrate B of 8 –, 20 weight parts; The lubricant of the rheological agent of the hollow ceramic microspheres of 10-15 weight part, 2-3 weight part, 2-3 weight part; Join in the high-speed mixer; Normal temperature was mediated 3 minutes down, entered single screw extrusion machine then and was extruded into sheet material;
The 4th step: the cross-linking radiation of product: carry out cross-linking radiation to the sheet material that extrudes through rumbatron; Irradiation dose: 15-18 megarad.
The 5th step: the foaming of product: the sheet material after crosslinked is put into foaming furnace foam, the temperature of foaming is 260 ± 10 ℃.
The 6th step: through the foam surface-coated expanding fire-proof paint after the foaming of the 5th step.
The working temperature of single screw extruder pelletizer is in the said the first step: 105 ℃ in a district, 115 ℃ in two districts, 125 ℃ in three districts, 135 ℃ in four districts, 125 ℃ in five districts;
The working temperature of single screw extruder pelletizer is in said second step: 90 ℃ in a district, 95 ℃ in two districts, 100 ℃ in three districts, 105 ℃ in four districts;
The working temperature of single screw extrusion machine is in said the 3rd step: 80 ℃ in a district, 85 ℃ in two districts, 95 ℃ in three districts, 90 ℃ in four districts.
Single screw extrusion machine is a BM type screw extrusion press in said the 3rd step.
The effectively insulating environmental protection flame retardant modified polyolefin indoor heat insulating foam that makes by aforesaid method.
This product employing blend, low temperature are extruded, prepared such as electron accelerator irradiation is crosslinked, foaming furnace foamable form; The finished product form fine and closely woven unicellular structure; Select the heat shielding additives hollow ceramic microspheres for use, blend is extruded through low temperature, makes it be dispersed in the system uniformly; Make product become good heat-insulation and heat-preservation material, thereby save the energy significantly.Use in the buildings of this product, can effectively completely cut off the conduction of heat energy, make buildings possess automatic attemperation, really accomplish cool in summer and warm in winter.The gordian technique of preparation is: 1, selected hollow ceramic microspheres for use, and success is dispersed in uniformly in the macromolecular material; 2, adopt the forcing machine of BM screw-rod structure, material can be extruded at a lower temperature, guarantee that whipping agent is not decomposed in advance; 3, material possesses high flame resistance, and burning is not fuming.The finished product are nonpoisonous and tasteless, environmental protection flame retardant, effectively insulating are energy-conservation, to human body and environmentally friendly, are the energy-conserving and environment-protective products of a new generation, can substitute traditional macromolecular material foaming thermal-insulating and inorganic heat insulation material.
Principle explanation of the present invention as follows
:
1, one of technological innovation of the present invention is to have adopted heat shielding additives: hollow ceramic microspheres is a kind of type material of excellent performance, and staple is a borosilicate; Granularity is that 10-250 micron, wall thickness are the hollow ball of 1-2 micron; Just as vacuum miniature hot-water bottle one by one, they form firm resist at body surface on the hollow ceramic microspheres microcosmic, and it is reflected effectively and reflect heat energy; This material has light weight, low heat conduction, intensity is high and good advantages such as chemicalstability; Through special processing, have oleophylic, hydrophobicity performance, be very easy to be scattered in the organic materials such as resin.
2, expanding fire-proof paint is under flame or high temperature, and the coating charing of acutely foaming forms one and can completely cut off the direct heating of extraneous flame to base material than the former flame-retardant foam charring layer that is coated with tens times of thickness even hundred times, plays fire retardation.When coating was charing expanded, the thermal conductivity of coating reduced, and had intercepted the conduction through expansion charcoal course base material heat.
3, the screw-rod structure problem of machining at low temperature sheet forming: owing to require the AC whipping agent can not have differential to separate phenomenon in the extrusion process of this product, extruding the mold temperature of processing, to extrude production than routine low at least more than 40 ℃.This has just caused the extrusion plasticizing problem of LDPE-EVA-EPDM compound system, how under the processing temperature that the AC whipping agent allows, to make the extrusion sheet plasticizing good, becomes an important technological problems.This project is through the contrast to various different structure screw rods, and the blend of selecting for use BM type screw rod (like the barrier divergence type screw rod with mixing pin of core water flowing) can satisfy LDPE-EVA-EPDM compound system is better extruded.
The effect of main raw material(s) is following among the present invention:
The present invention through a large amount of prescriptions have a competition, starting material simultaneous test and practical experience, drawn present production formula and production technique, selected starting material all are best, contribution also is best to performance of products.
Polyolefine: at present in the crosslinking reaction than being easier to crosslinked long-chain branch olefin material, the present invention elite with new LDPE (film grade), EVA (ethylene-vinyl acetate copolymer), ethylene-propylene diene copolymer EPDM as the crosslinked base-material of environment friendly non-halogen.
Composite flame-retardant agent: select environment friendly halogen-free fireproof agent micro encapsulation ammonium polyphosphate and zinc borate for use, nontoxic, heavy metal free, (micro encapsulation ammonium polyphosphate 90%+ zinc borate 10%)
Heat shielding additives: select hollow ceramic microspheres for use.
Smoke suppressor: ammonium octamolybdate is not fuming material combustion.
Whipping agent: select the AC whipping agent for use, because of its foaming effect best, and environment-protecting asepsis.
Fire-proof dilatation: the flame retardant resistance that increases material.
Rheological agent: make the material extrusion temperature lower.
Oxidation inhibitor: prevent material oxidation in use.
Lubricant: material is extruded in the course of processing easily.
Zinic stearas: acvator makes the whipping agent foaming fully.
The product that the present invention produces not only has flame retardant properties preferably, and the combustionproperty grade is: A2-s1, d1; The t0 level; The burning be not fuming, thermal conductivity reach 0.015
, well below other lagging material; In addition; The expansion ratio of product reaches 5 – 30, and shore hardness reaches 15 – 60A, and over-all properties is stronger.
Embodiment
Embodiment 1: a kind of preparation method of effectively insulating environmental protection flame retardant modified polyolefin indoor heat insulating foam, and this preparation method may further comprise the steps successively:
The first step: the preparation of fire-retardant master granule A: get the ldpe resin of 20 weight parts, the composite flame-retardant agent of 30 weight parts, the smoke suppressor of 8 weight parts, the antioxidant 1010 of 0.3 weight part, the lubricant of 0.6 weight part earlier; Normal temperature was mediated 3 – 5 minutes down; Enter banburying in the Banbury mixer then, the banburying temperature is 100 ± 5 ℃, and the banburying time is 6 – 8 minutes; The group of the material after the banburying is entered in single screw extruder pelletizer through forced feed, the fusion plastification granulation makes flame-retardant master batch A again; Said composite flame-retardant agent is the compound of micro encapsulation ammonium polyphosphate and zinc borate, and pale powder, said lubricant are polyethylene wax (Honeywell A-C316A); Said smoke suppressor is an ammonium octamolybdate, the white powder, (place of production: the Kunshan, Jiangsu).
Wherein the working temperature of single screw extruder pelletizer is: 105 ℃ in a district, 115 ℃ in two districts, 125 ℃ in three districts, 135 ℃ in four districts, 125 ℃ in five districts.
Second step: the preparation of foaming concentrate B: the ldpe resin of getting 50 weight parts earlier adds in the high mixer; Add the AC whipping agent Cellmic C 121 of 15 weight parts, the talcum powder of 0.8 weight part, the lubricant (with the step 1 lubricant) of 2 weight parts, the Zinic stearas of 1 weight part again; Normal temperature was mediated 3 minutes down, entered the single screw extrusion machine granulation then to obtain foaming concentrate D;
Wherein the working temperature of single screw extruder pelletizer is: 90 ℃ in a district, 95 ℃ in two districts, 100 ℃ in three districts, 105 ℃ in four districts.
The 3rd step: the preparation of sheet material C: the flame-retardant master batch A that gets terpolymer EP rubber 20 weight parts of the ldpe resin of 5 weight parts, the Yi Xi – acetate ethylene copolymer of 23 weight parts (be and raise sub-petrochemical industry-BASF Ltd product), 2 weight parts; The lubricant of the rheological agent of the foaming concentrate B of 8 weight parts, the hollow ceramic microspheres of 10 weight parts, 2 weight parts (Qingdao Wei Dongke rubber and plastic Science and Technology Ltd.), 2 weight parts adds in the high mixer; Normal temperature was mediated 3 minutes down, entered BM type screw extrusion press (Nanjing Jie Ya company) then and was extruded into sheet material.Said hollow ceramic microspheres is a white powder, and rheological agent is a white powder.
Wherein the working temperature of single screw extrusion machine is: 80 ℃ in a district, 85 ℃ in two districts, 95 ℃ in three districts, 90 ℃ in four districts.
The 4th step: the cross-linking radiation of product: carry out cross-linking radiation to the sheet material that extrudes through rumbatron.Irradiation dose: 15-18 megarad.
The 5th step: the foaming of product: the sheet material after crosslinked is put into foaming furnace foam, the temperature of foaming is 260 ± 10 ℃.
The 6th goes on foot: the coating of not firing frie retardant coating: directly get into to be equipped with through the foam after the foaming of the 5th step and do not fire frie retardant coating (expanding fire-proof paint; Model: the coating equipment WL-01 finishing fire retardant paint); Carry out surface-coated; Because sheet material is in elastic state, frie retardant coating is easy to be bonded in sheet surface, forms firm coat.
The key technical indexes of gained insulation foam product:
Outward appearance: smooth no color differnece;
Product expansion ratio: 5;
Product shore hardness: 15A;
Thermal conductivity: 0.015
;
The combustionproperty grade is: A2-s1, d1, t0 level;
Plumbous (Pb) content :≤5PPM;
Cadmium (Cd) content :≤5PPM;
Sexavalent chrome (Cr) content :≤5PPM;
Mercury (Hg) content :≤5PPM;
PBBs content :≤5PPM;
PBBs ethers content :≤5PPM.
Embodiment 2:
The first step, second step, the 4th step, the 5th step are with embodiment 1; Different was the 3rd step: the ldpe resin in the preparation of sheet material C is that 20 weight parts, Yi Xi – acetate ethylene copolymer are that 30 weight parts, terpolymer EP rubber are that 10 weight parts, flame-retardant master batch A are 30 weight parts; Foaming concentrate B is 20 weight parts, and hollow ceramic microspheres is that 15 weight parts, rheological agent are that 3 weight parts, lubricant are that 3 weight parts add in the high mixer.
The key technical indexes of gained insulation foam product:
Outward appearance: smooth no color differnece;
Product expansion ratio: 30;
Product shore hardness: 60A;
Thermal conductivity: 0.015
;
The combustionproperty grade is: A2-s1, d1, t0 level;
Plumbous (Pb) content :≤5PPM;
Cadmium (Cd) content :≤5PPM;
Sexavalent chrome (Cr) content :≤5PPM;
Mercury (Hg) content :≤5PPM;
PBBs content :≤5PPM;
PBBs ethers content :≤5PPM.
Embodiment 3:
The first step, second step, the 4th step, the 5th step with embodiment 1 different be the 3rd step: ldpe resin is that 15 weight parts, Yi Xi – acetate ethylene copolymer are that 25 weight parts, terpolymer EP rubber are that 7 weight parts, flame-retardant master batch A are that 25 weight parts, foaming concentrate B are that 13 weight parts, hollow ceramic microspheres are that 12 weight parts, rheological agent are that 2.5 weight parts, lubricant are 2.5 weight parts in the preparation of sheet material C.
The key technical indexes of gained insulation foam product:
Outward appearance: smooth no color differnece;
Product expansion ratio: 15;
Product shore hardness: 40A;
Thermal conductivity: 0.015
;
The combustionproperty grade is: A2-s1, d1, t0 level;
Plumbous (Pb) content :≤5PPM;
Cadmium (Cd) content :≤5PPM;
Sexavalent chrome (Cr) content :≤5PPM;
Mercury (Hg) content :≤5PPM;
PBBs content :≤5PPM;
PBBs ethers content :≤5PPM.
Embodiment 4:
The first step, second step, the 4th step, the 5th step with embodiment 1 different be the 3rd step: the ldpe resin in the preparation of sheet material C is that 15 weight parts, Yi Xi – acetate ethylene copolymer are that 25 weight parts, terpolymer EP rubber are that 7 weight parts, flame-retardant master batch A are 25 weight parts, and foaming concentrate B is that 18 weight parts, hollow ceramic microspheres are that 12 weight parts, rheological agent are that 2.5 weight parts, lubricant are 2.5 weight parts.
The key technical indexes of gained insulation foam product:
Outward appearance: smooth no color differnece;
Product expansion ratio: 25;
Product shore hardness: 50A;
Thermal conductivity: 0.015
;
The combustionproperty grade is: A2-s1, d1, t0 level;
Plumbous (Pb) content :≤5PPM;
Cadmium (Cd) content :≤5PPM;
Sexavalent chrome (Cr) content :≤5PPM;
Mercury (Hg) content :≤5PPM;
PBBs content :≤5PPM;
PBBs ethers content :≤5PPM.
Claims (4)
1. the preparation method of an effectively insulating environmental protection flame retardant modified polyolefin indoor heat insulating foam may further comprise the steps:
The first step: the preparation of fire-retardant master granule A: get the ldpe resin of 20 weight parts, the composite flame-retardant agent of 30 weight parts, the smoke suppressor of 8 weight parts, the antioxidant 1010 of 0.3 weight part, the lubricant of 0.6 weight part earlier; Normal temperature was mediated 3 – 5 minutes down; Enter the material group after banburying in the Banbury mixer gets banburying then; The banburying temperature is 100 ± 5 ℃, and the banburying time is 6 – 8 minutes; The group of the material after the banburying is entered in single screw extruder pelletizer through forced feed, the fusion plastification granulation makes flame-retardant master batch A again; Said composite flame-retardant agent is the compound of micro encapsulation ammonium polyphosphate and zinc borate, and this compound is mixed by the micro encapsulation ammonium polyphosphate of 90wt% and the zinc borate of 10wt%; Said lubricant is a polyethylene wax; Said smoke suppressor is an ammonium octamolybdate;
Second step: the preparation of foaming concentrate B: the ldpe resin of getting 50 weight parts earlier adds in the high mixer; Add the Cellmic C 121 of 15 weight parts, the talcum powder of 0.8 weight part, the lubricant of 2 weight parts, the Zinic stearas of 1 weight part again; Normal temperature was mediated 3 minutes down, entered the single screw extrusion machine granulation then to obtain foaming concentrate D;
The 3rd step: the preparation of sheet material C: get the ldpe resin of 5 –, 20 weight parts, the Yi Xi – acetate ethylene copolymer of 23 –, 30 weight parts, the terpolymer EP rubber of 2 –, 10 weight parts, the flame-retardant master batch A of 20-30 weight part, the foaming concentrate B of 8 –, 20 weight parts, the hollow ceramic microspheres of 10-15 weight part, the rheological agent of 2-3 weight part and the lubricant of 2-3 weight part; Join in the high-speed mixer; Normal temperature was mediated 3 minutes down, entered single screw extrusion machine then and was extruded into sheet material;
The 4th step: the cross-linking radiation of product: carry out cross-linking radiation to the sheet material that extrudes through rumbatron and get the sheet material after crosslinked; Irradiation dose: 15-18 megarad;
The 5th the step: the foaming of product: with the sheet material after crosslinked put into foaming furnace foam the foaming after foam, the temperature of foaming is 260 ± 10 ℃;
The 6th step: through the foam surface-coated expanding fire-proof paint after the foaming of the 5th step.
2. preparation method according to claim 1 is characterized in that:
The working temperature of single screw extruder pelletizer is in the said the first step: 105 ℃ in a district, 115 ℃ in two districts, 125 ℃ in three districts, 135 ℃ in four districts, 125 ℃ in five districts;
The working temperature of single screw extruder pelletizer is in said second step: 90 ℃ in a district, 95 ℃ in two districts, 100 ℃ in three districts, 105 ℃ in four districts;
The working temperature of single screw extrusion machine is in said the 3rd step: 80 ℃ in a district, 85 ℃ in two districts, 95 ℃ in three districts, 90 ℃ in four districts.
3. method according to claim 1 and 2 is characterized in that: the BM type screw extrusion press that single screw extrusion machine is in said the 3rd step.
4. the effectively insulating environmental protection flame retardant modified polyolefin indoor heat insulating foam that makes by claim 1 or 2 said methods.
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