CN104341667A - Polyethylene halogen-free flame-retarding foaming master batch and preparation method thereof - Google Patents
Polyethylene halogen-free flame-retarding foaming master batch and preparation method thereof Download PDFInfo
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C2948/00—Indexing scheme relating to extrusion moulding
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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
- C08J2423/02—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
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Abstract
The invention relates to a polyethylene halogen-free flame-retarding foaming master batch and a preparation method thereof. The polyethylene halogen-free flame-retarding foaming master batch is characterized in that raw materials for preparing the master batch benchmarked, by taking the weight of carrier resin as reference, comprise 100 parts of carrier resin, 15-30 parts of dispersing agent, 0.5-10 parts of nucleating agent, 10-30 parts of filter, 110-150 parts of halogen-free flame retardant, 20-40 parts of flame-retarding modifying agent, 20-40 parts of organic foaming agent and 5-10 parts of foaming activating agent. According to the halogen-free flame-retarding foaming master batch prepared by the method provided by the invention, as a multifunctional master batch, a certain flame retarding performance of a product is realized while the density of a polyethylene product is obviously lowered, and the processing performance and the mechanical performance of the product are improved; the application of polyethylene resin in more fields such as building, traffic, electric appliance and communication are widened.
Description
Technical field
The present invention relates to a kind of masterbatch and preparation method thereof, relate to halogen-free flame-retardant expanded masterbatch of a kind of polyethylene and preparation method thereof.
Background technology
In the processing industry of plastics, people are finding a kind of novel method that can adapt to modern processing always, thus reach save time, the object of improve effects.In line with this spirit, various functional plastics masterbatch arises at the historic moment.Plastic matrix is the enriched material of various plastics additive, namely additives for plastics is exceeded conventional addition (routine about 20%, in masterbatch, auxiliary agent mostly is more than 50%) join in vector resin, it is mixing or plasticate together with processing aid, formed by twin screw extruder extruding pelletization.When producing plastic prod, directly add master batch and both solve the difficult problems such as ordinary adjuvants bad dispersibility, dust from flying, metering be inaccurate, in turn simplify production process, reduce the wearing and tearing to equipment, conservation, make raw material mix convenience, mixing is even, thus improve the performance index of production efficiency and product.Compare with American-European countries, the output of China's plastic matrix is lower, also there is very large gap.At present, consumer plastic amount is still lower than world average level per capita in China, and plastic matrix market potential is large, and development prospect is wide.
Foaming concentrate is a kind of novel expanded plastic processing aid just grown up in recent years, research at home starts from the mid-90 in last century, it has multiple efficacies in foaming technique, as helped the functions such as foaming, resisted shrinkage, lubrication, plasticising, rebound resilience, increase surface brightness, there is comprehensive advantage such as raising foam article performance and processing characteristics etc.
Plastic prod is while having various excellent application performance, and but have and hold incendive shortcoming, particularly polyolefins plastics, Plastics Combustion easily causes the heavy losses of fire and personnel and material.For polyethylene, its oxygen index (OI) only about 18, belong to inflammable substance, poor fire limits the application of PE in more areas such as building, traffic, electrical equipment, communications.Add the halogenated flame retardant containing haloid element, if clorafin, decabromodiphenyl oxide, tetrabromo-bisphenol and antimonous oxide etc. are the methods of raising Flame Retardancy energy conventional at present.But halogen family fire retardant can discharge the extremely strong poisonous corrosive hydrogen halides gas of toxicity when fire occurs, may cause the secondary pollution of larger harm, thus make it apply and be very limited.Halogen, eliminates smoke and has become the developing direction of high molecular fire retardant.Compare with halogenated flame retardant, the halogen-free flame retardants of exploitation at present also also exists big gap in flame retardant resistance, processing characteristics, mechanical property and price etc.Under state-of-the art and market situation, halogen system, low halogen and halogen-free flame retardants will be in and the situation of depositing over a period to come.
In today of Polymer Industry high speed development, single masterbatch often cannot meet the many-sided needs of material, add multiple masterbatch, sometimes cannot play the function of each functional master batch completely, cost also can be caused to remain high, therefore be necessary to develop multi-functional masterbatch, by once adding, making material possess several functions, reducing costs, Simplified flowsheet, widens the Application Areas of material.
Summary of the invention
Technical problem to be solved by this invention is for above shortcomings in prior art, provides a kind of multi-functional foaming concentrate and preparation method thereof, and this foaming concentrate is containing halogen-free flame retardants, and flame retardant effect is good, and cost is lower, and preparation technology is simple.
The technical scheme of the halogen-free flame-retardant expanded masterbatch of polyethylene of the present invention is:
The starting material preparing the halogen-free flame-retardant expanded masterbatch of this polyethylene, comprising for benchmark with the weight of vector resin:
By such scheme, described vector resin is the mixture of one or more in LDPE (Low Density Polyethylene), LLDPE (LLDPE), HDPE (high density polyethylene(HDPE)), EVA (ethylene-vinyl acetate copolymer), and its DSC fusing point is 105-130 DEG C.
By such scheme, described dispersion agent is the mixture of one or more in solid paraffin, stearic acid, polyethylene wax; Described nucleator is the mixture of one or more in silicon-dioxide, talcum powder, titanium dioxide; Described filler is the mixture of one or more in calcium carbonate superfine powder, superfine talcum powder, barium sulfate, polynite.
By such scheme, described halogen-free flame retardants is one or more mixtures in magnesium hydroxide, aluminium hydroxide, ammonium polyphosphate; Described flame-proof modifier is the mixture of one or more in vinylformic acid, methacrylic acid, MALEIC ANHYDRIDE, methyl propenoic acid glycidyl ether.
By such scheme, described organic blowing agent is the mixture of one or more in Cellmic C 121 (AC), two this sulfonyl hydrazide (OBSH) of 4,4-oxos, dinitrosopentamethlyene tetramine (DPT), Diisopropyl azodicarboxylate (AIBN); Described blowing activator is the mixture of one or more in zinc oxide, magnesium oxide, plumbous oxide, citric acid, stearic acid, Zinic stearas, calcium stearate.
The preparation method of the halogen-free flame-retardant expanded masterbatch of polyethylene of the present invention is:
After the starting material preparing the halogen-free flame-retardant expanded masterbatch of polyethylene are weighed in proportion, first add in high speed mixer and mix, then add in mill and plasticate, form finally by twin screw extruder extruding pelletization, the weight proportion of each component of starting material with the weight of vector resin for benchmark, for:
By such scheme, the technique mixed in described high speed mixer is 40-45 DEG C of mixing 8-10 minute.
By such scheme, in described mill, the time of plasticating is 6-10 minute, and temperature is 60-90 DEG C.
By such scheme, described twin screw extruder expressing technique is: the screw speed of forcing machine is 40 revs/min, feed rate 15 ~ 20 revs/min, each district temperature: first paragraph 100 DEG C, second segment 110 DEG C, the 3rd section 115 DEG C, 4th section 120 DEG C, 5th section 125 DEG C, the 6th section 120 DEG C, head temperature 115 DEG C.
Beneficial effect of the present invention is: 1, compare with traditional halogenated flame retardant, halogen-free flame retardants has good flame retardation effect, eco-friendly advantage, but general addition is very large in resin, easy appearance is reunited, the shortcoming of bloom, the present invention reduces the surface energy of fire retardant by adding flame-proof modifier, fire retardant is formed coated, improve the dispersiveness of fire retardant, flame-proof modifier introduces polarity or functionalization side base on nonpolar molecular polyolefin on the other hand, improve the consistency of resin and fire retardant, in addition, flame-proof modifier contains a large amount of active function groups, hydrogen bond is formed with the hydrophilic hydroxy group of filling surface, reduce the surface energy of filler, promote the dispersion of filler, improve the mechanical property of product, 2, the present invention adopts blowing activator and organic blowing agent to carry out the decomposition temperature of composite reduction whipping agent, improve gas forming amount, improve decomposability and the froth stability of whipping agent, that improves whipping agent can processed-type, for polyethylene, AC whipping agent is a kind of Exothermic blowing agents, its decomposition temperature is 195-220 DEG C, blowing activator is adopted to reduce foaming agent decomposition temperature to 150 DEG C, save energy, balance foaming, add this foaming concentrate to polyvinyl resin with the addition of 8-18% and produce, obtaining density is 0.70-0.84g/cm
3foam material, 3, preparation method's technique provided by the invention is simple, and the halogen-free flame-retardant expanded masterbatch of prepared polyethylene is a kind of multifunctional concentrate, easy to use, can directly add in polyvinyl resin, pass through injection moulding, mold pressing, the explained hereafter flame retardant type polyethylene foam product such as to extrude, enormously simplify production process, significantly reducing polyethylene product density, improve Product processing performance, give product certain flame retardant properties while mechanical property, widened the application of polyvinyl resin in more areas such as building, traffic, electrical equipment, communications.
Embodiment
For making those skilled in the art understand technical scheme of the present invention better, below in conjunction with embodiment, the present invention is described in further detail.
In embodiment, the testing method of flame retardant properties is tested with reference to Plastics Combustion performance test standard GB/T2406-1993 and GB 8332-1987.
The DSC fusing point of the embodiment of the present invention LDPE, LLDPE, HDPE, EVA used or its mixture is 105-130 DEG C.The expressing technique of twin screw extruder used is: the screw speed of forcing machine is 40 revs/min, feed rate 15 ~ 20 revs/min, each district temperature: first paragraph 100 DEG C, second segment 110 DEG C, the 3rd section 115 DEG C, the 4th section 120 DEG C, 5th section 125 DEG C, the 6th section 120 DEG C, head temperature 115 DEG C.
Embodiment 1
Double centner LDPE is added successively in high speed mixer, 15 kilograms of stearic acid, 4 kilograms of silicon-dioxide and 1 kilogram of titanium dioxide, 20 kilograms of calcium carbonate superfine powders, 120 kg of hydrogen magnesium oxide, 30 kilograms of MALEIC ANHYDRIDE, 35 kilograms of whipping agent Cellmic C 121s, the mixture (the two mass ratio is 3:1) of 8 grams of zinc oxide and barium stearate, mixes 10 minutes, mixing temperature 45 DEG C.First mixed thing is added to the 6-10 minute that to plasticate in mill, at twin screw extruder extruding pelletization after discharging, polyethylene anti-flaming foaming concentrate can be obtained.By masterbatch with 8% addition add polyvinyl resin to and produce, obtain density 0.70g/cm
3, oxygen index is 25, the product of flame retardant rating V-2 level.
Embodiment 2
70 kilograms of LLDPE and 30 kilogram EVA are added successively in high speed mixer, 25 kilograms of solid paraffins, 6 kilograms of titanium dioxide, 15 kilograms of superfine talcum powders and 5 kilo sulfuric acid barium, the mixture of 60 kg of hydrogen magnesium oxide and 50 kg of hydrogen aluminum oxide, 35 kilograms of methacrylic acids, 15 kilograms of Cellmic C 121s and 10 kilograms of dinitrosopentamethlyene tetramines, 3 kilograms of zinc oxide and 3 kilograms of citric acids, mix 10 minutes, mixing temperature 45 DEG C.First mixed thing is added to the 6-10 minute that to plasticate in mill, at twin screw extruder extruding pelletization after discharging, polyethylene anti-flaming foaming concentrate can be obtained.By masterbatch with 12% addition add polyvinyl resin to and produce, obtain density 0.75g/cm
3, oxygen index is 27, the product of flame retardant rating V-1 level.
Embodiment 3
70 kilograms of HDPE and 30 kilogram EVA are added successively in high speed mixer, 15 kilograms of stearic acid and 15 kilograms of polyethylene waxs, 0.5 kilogram of talcum powder, 30 kilo sulfuric acid barium, 90 kg of hydrogen magnesium oxide and 60 kilograms of ammonium polyphosphate mixtures, 20 kilograms of vinylformic acid, 10 kilogram of 4,4-oxo these sulfonyl hydrazide two and 10 kilograms of Diisopropyl azodicarboxylates, 3 kilograms of calcium stearates and 2 kilograms of Zinic stearass, mix 10 minutes, mixing temperature 45 DEG C.First mixed thing is added to the 6-10 minute that to plasticate in mill, at twin screw extruder extruding pelletization after discharging, polyethylene anti-flaming foaming concentrate can be obtained.By masterbatch with 16% addition add polyvinyl resin to and produce, obtain density 0.8g/cm
3, oxygen index is 30, the product of flame retardant rating V-0 level.
Embodiment 4
Double centner HDPE is added successively in high speed mixer, 25 kilograms of polyethylene waxs, 9 kilograms of titanium dioxide, 10 kilograms of polynites, 70 kg of hydrogen magnesium oxide and 60 kilograms of ammonium polyphosphate mixtures, 25 kilograms of vinylformic acid and 15 kilograms of methyl propenoic acid glycidyl ethers, 20 kilograms of Cellmic C 121s and 20 kilogram of 4,4-oxo this sulfonyl hydrazide two, 8 kilograms of stearic acid and 2 kilograms of Zinic stearass, mix 10 minutes, mixing temperature 45 DEG C.First mixed thing is added to the 6-10 minute that to plasticate in mill, at twin screw extruder extruding pelletization after discharging, polyethylene anti-flaming foaming concentrate can be obtained.By masterbatch with 18% addition add polyvinyl resin to and produce, obtain density 0.84g/cm
3, oxygen index is 33, the product of flame retardant rating V-0 level.
Claims (9)
1. the halogen-free flame-retardant expanded masterbatch of polyethylene, the starting material that it is characterized in that preparing the halogen-free flame-retardant expanded masterbatch of this polyethylene, comprising for benchmark with the weight of vector resin:
2. the halogen-free flame-retardant expanded masterbatch of polyethylene according to claim 1, it is characterized in that described vector resin is the mixture of one or more in LDPE, LLDPE, HDPE, EVA, its DSC fusing point is 105-130 DEG C.
3. the halogen-free flame-retardant expanded masterbatch of polyethylene according to claim 1, is characterized in that described dispersion agent is the mixture of one or more in solid paraffin, stearic acid, polyethylene wax; Described nucleator is the mixture of one or more in silicon-dioxide, talcum powder, titanium dioxide; Described filler is the mixture of one or more in calcium carbonate superfine powder, superfine talcum powder, barium sulfate, polynite.
4. the halogen-free flame-retardant expanded masterbatch of polyethylene according to claim 1, is characterized in that described halogen-free flame retardants is one or more mixtures in magnesium hydroxide, aluminium hydroxide, ammonium polyphosphate; Described flame-proof modifier is the mixture of one or more in vinylformic acid, methacrylic acid, MALEIC ANHYDRIDE, methyl propenoic acid glycidyl ether.
5. the halogen-free flame-retardant expanded masterbatch of polyethylene according to claim 1, it is characterized in that described organic blowing agent is the mixture of one or more in Cellmic C 121,4,4-oxos this sulfonyl hydrazide two, dinitrosopentamethlyene tetramine, Diisopropyl azodicarboxylate; Described blowing activator is the mixture of one or more in zinc oxide, magnesium oxide, plumbous oxide, citric acid, stearic acid, Zinic stearas, calcium stearate.
6. the preparation method of the halogen-free flame-retardant expanded masterbatch of polyethylene, it is characterized in that: after the starting material preparing the halogen-free flame-retardant expanded masterbatch of polyethylene are weighed in proportion, first add in high speed mixer and mix, add in mill again and plasticate, form finally by twin screw extruder extruding pelletization, the weight proportion of each component of starting material with the weight of vector resin for benchmark, for:
7. the preparation method of the halogen-free flame-retardant expanded masterbatch of polyethylene according to claim 6, is characterized in that: the technique mixed in described high speed mixer is 40-45 DEG C of mixing 8-10 minute.
8. the preparation method of the halogen-free flame-retardant expanded masterbatch of polyethylene according to claim 6, is characterized in that: in described mill, the time of plasticating is 6-10 minute, and temperature is 60-90 DEG C.
9. the preparation method of the halogen-free flame-retardant expanded masterbatch of polyethylene according to claim 6, it is characterized in that, described twin screw extruder expressing technique is: the screw speed of forcing machine is 40 revs/min, feed rate 15 ~ 20 revs/min, each district temperature: first paragraph 100 DEG C, second segment 110 DEG C, 3rd section 115 DEG C, the 4th section 120 DEG C, the 5th section 125 DEG C, 6th section 120 DEG C, head temperature 115 DEG C.
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Application publication date: 20150211 |