CN102516628A - High-density polyethylene composite material and preparation method thereof - Google Patents
High-density polyethylene composite material and preparation method thereof Download PDFInfo
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- CN102516628A CN102516628A CN2011103980864A CN201110398086A CN102516628A CN 102516628 A CN102516628 A CN 102516628A CN 2011103980864 A CN2011103980864 A CN 2011103980864A CN 201110398086 A CN201110398086 A CN 201110398086A CN 102516628 A CN102516628 A CN 102516628A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/78—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
- B29C48/875—Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92514—Pressure
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92561—Time, e.g. start, termination, duration or interruption
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92819—Location or phase of control
- B29C2948/92857—Extrusion unit
- B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
- B29C2948/92895—Barrel or housing
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Abstract
The invention is applicable to the technical field of engineering plastics, and provides a high-density polyethylene composite material and a preparation method thereof. The high-density polyethylene composite material utilizes an antidropping agent of a constitutional formula I. By adopting the constitutional formula I, effective flame retardant effect can be realized through fluorine; high flame retardant grade and high chemical property can be realized through Oxazole ring; and the preparation method of the high-density polyethylene composite material is simple to operate, has low cost, and is very suitable for the industrialized production.
Description
Technical field
The invention belongs to the engineering plastics field, relate in particular to a kind of high-density polyethylene composite material and preparation method thereof.
Background technology
High density polyethylene(HDPE) (HDPE) is a kind of general synthetic resin of excellent performance, all has been widely used in fields such as industrial or agricultural, national defence, construction industry and daily necessities.Along with the development of petrochemical complex, the HDPE increase of production is very fast, and YO at present only is lower than new LDPE (film grade) (LDPE) and SE (PVC).But the HDPE oxygen index is very low, and flame retardant effect is very poor, has limited its further widespread use.
HDPE is accompanied by the vertical phenomenon of violent melt droplets in combustion processes, need a high proportion of fire retardant of interpolation and anti-dripping agent could improve this problem.Anti-dripping agent general on the market is the ptfe micropowder of surface-treated, receives the influence of process for modifying surface, and this type of anti-dripping agent has the adding proportion height, with the shortcoming of resin compatible difference.
Summary of the invention
The object of the present invention is to provide a kind of high-density polyethylene composite material, consistency is poor between anti-dripping agent that solution prior art middle-high density composite polyethylene material is added and the high density polyethylene(HDPE), the technical problem that mechanical property is low.
The present invention is achieved in that
A kind of high-density polyethylene composite material comprises following components in weight percentage content:
Said anti-dripping agent has following structural formula I:
And,
Above-specified high density composite polyethylene material preparation method comprises the steps:
Following components in weight percentage content is provided:
Said anti-dripping agent has following structural formula I:
Said component mixing is obtained mixture, said mixture is extruded processing, obtain high-density polyethylene composite material.
High-density polyethylene composite material of the present invention uses said structure formula I anti-dripping agent, effectively plays fire retardation through fluorine element; Tong Guo oxazole heterocycle makes it have higher flame retardant rating and mechanical property simultaneously; High-density polyethylene composite material preparation method of the present invention, simple to operate, with low cost, be very suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is an embodiment of the invention preparation method schema.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearer,, the present invention is further elaborated below in conjunction with accompanying drawing and embodiment.Should be appreciated that specific embodiment described herein only in order to explanation the present invention, and be not used in qualification the present invention.
The embodiment of the invention provides a kind of high-density polyethylene composite material, comprises the component of following parts by weight:
Said anti-dripping agent has following structural formula I:
In the employed anti-dripping agent of embodiment of the invention high-density polyethylene composite material, contain fluorine element or/and other halogenss, wherein fluorine element content is high, can play very excellent flame-retardant; Further; Go back Bao Kuo You oxazole heterocycle in this anti-dripping agent; Nitrogen element wherein not only has anti-flaming function; Also can be capable become hydrogen bond crosslinked, and then improved the consistency of anti-dripping agent and high density polyethylene(HDPE), make high-density polyethylene composite material have higher flame retardant rating and mechanical property simultaneously with the Wasserstoffatoms in the high density polyethylene(HDPE).
The preparation method of this anti-dripping agent comprises the steps:
Step 1, supply raw materials:
Respectively structural formula
the compound A and structural formula
compound B;
Step 2, dehydration reaction:
With mol ratio is that 2.05～2.1: 1 compd A and compd B are added in the PPA solvent; At oxygen free condition and temperature is to react 9～12 hours under 185～195 ℃ of conditions; Obtain the anti-dripping agent of structural formula I; Structural formula I is
wherein, and X is a halogens.
Particularly, in the step 1, the name of compd A is called 4 '-halogenated benzoic acid (4-XBA), for example, fluorinated acid, chlorinated benzene formic acid, bromobenzene formic acid or iodobenzoic acid, compd A can obtain from buying on the market.The name of compd B is called two (3-amino-4-phenylor) HFC-236fas (6F-BAHP), and compd B can obtain from buying on the market.
Particularly, in the step 2, the mol ratio of this compd A and compd B is 2.05～2.1: 1, is preferably 2: 1.
Particularly, this PPA solvent is meant poly phosphoric acid solution, and in this poly phosphoric acid solution, the weight percentage of Vanadium Pentoxide in FLAKES is 85%～90%.The concentration of buying the poly phosphoric acid solution that obtains on the market is less than above-mentioned concentration; Above-mentioned weight percentage passes through adding the Vanadium Pentoxide in FLAKES solid in the poly phosphoric acid solution; Be heated to thickly again through oil bath etc., Vanadium Pentoxide in FLAKES be dissolved in the poly phosphoric acid solution fully obtain.
Particularly, being reflected under the oxygen free condition of compd A and compd B carried out in the step 2, and this oxygen free condition is restriction not, for example, through in reactor drum, feeding nitrogen, makes reactor drum keep oxygen-free environment.In this step, temperature of reaction is 185～195 ℃, and for example, 190 ℃, the reaction times is 9～12 hours, for example 10 hours.The reaction formula of step 2 is expressed as:
Further, after reaction finishes, will react back liquid cooling, stopped reaction.Deionized water is injected into the solid product that obtains grey black in the reactor drum, and hot-water soak, flushing are till leacheate is neutrality.After activated carbon decolorizing, recrystallization, vacuum-drying, obtain the product of white, the anti-dripping agent of the structural formula I that uses in the high-density polyethylene composite material promptly of the present invention.
Particularly, among the structural formula I, halogens is selected from fluorine, chlorine, bromine or iodine.
Particularly, halogen-free flame retardants is the composite expansion type flame retardant of phosphorus-nitrogen, as 10200, and the place of production: go up Hai'an protruding plastics additive ltd; HFR-041, the place of production; Foshan Wei Kede chemical materials ltd.
Particularly, this lubricant is strong polarity organic molecule, for example, and like ethylene bis-fatty acid amides (TAF, TAS-2A etc.).
Particularly, this oxidation inhibitor is restriction not, and for example 1010,186 etc.
See also Fig. 1, Fig. 1 shows that the embodiment of the invention advances high-density polyethylene composite material preparation method schema, comprises the steps:
Step S01, supply raw materials:
Following components in weight percentage content is provided:
Said anti-dripping agent has following structural formula I:
wherein, X is a halogens;
Step S02, extrude processing:
Said component mixing is obtained mixture, said mixture is extruded processing, obtain high-density polyethylene composite material.
Particularly, among the structural formula I, halogens is selected from fluorine, chlorine, bromine or iodine.
Particularly, halogen-free flame retardants is the composite expansion type flame retardant of phosphorus-nitrogen, as 10200, and the place of production: go up Hai'an protruding plastics additive ltd; HFR-041, the place of production; Foshan Wei Kede chemical materials ltd.
Particularly, this lubricant is strong polarity organic molecule, for example, and like ethylene bis-fatty acid amides (TAF, TAS-2A etc.).
Particularly, this oxidation inhibitor is restriction not, and for example 1010,186 etc.
Particularly
Particularly, this anti-dripping agent prepares through preceding method, and the weight percentage of this anti-dripping agent is 0.1%～0.5%, is preferably 0.2%～0.4%.
Concrete, among the step S02, the raw materials mix that step S01 is provided is even, obtains mixture, then this mixture is melt extruded processing with twin screw extruder or single screw extrusion machine process, extrudes in the treatment step, and processing condition are following:
One district temperature 130-140 ℃, two district temperature 170-180 ℃, three district temperature 180-190 ℃, four district temperature 175-185 ℃, head 180-190 ℃, the residence time 1～2min, pressure are 20-30MPa.Through extruding processing, cooling, granulation, obtain embodiment of the invention high-density polyethylene composite material.
Embodiment of the invention high-density polyethylene composite material preparation method; Simple to operate, with low cost, be very suitable for suitability for industrialized production; The prepared high-density polyethylene composite material that obtains uses said structure formula I anti-dripping agent, effectively plays fire retardation through fluorine element; Tong Guo oxazole heterocycle makes it have higher flame retardant rating and mechanical property simultaneously.
Below in conjunction with specific embodiment above-specified high density composite polyethylene material preparation method is set forth in detail.
Embodiment one
The embodiment of the invention one high-density polyethylene composite material preparation method comprises the steps:
It is 83.9% HDPE (below be weight percentage) that weight percentage is provided, the anti-dripping agent of the structural formula I of 15% halogen-free flame retardants 10200,0.1%, 0.5% lubricant, 0.5% oxidation inhibitor;
With weight percentage is 83.9% HDPE (below be weight percentage), the anti-dripping agent of the structural formula I of 15% halogen-free flame retardants 10200,0.1%; 0.5% lubricant; 0.5% oxidation inhibitor mixes, and the material that mixes is joined in the hopper of twin screw extruder, through melt blending; Extruding pelletization obtains high-density polyethylene composite material.Wherein, screw rod is respectively distinguished the temperature setting and is respectively: twin screw extruder one district temperature 130-140 ℃, two district temperature 170-180 ℃, three district temperature 180-190 ℃, four district temperature 175-185 ℃, head 180-190 ℃, the residence time 1～2min, pressure are 20-30MPa.
Embodiment two
The embodiment of the invention two high-density polyethylene composite material preparing methods comprise the steps:
It is 81.6% HDPE (below be weight percentage) that weight percentage is provided, the anti-dripping agent of the structural formula I of 17% halogen-free flame retardants 10200,0.2%, 0.6% lubricant, 0.6% oxidation inhibitor;
The HDPE weight percentage is 81.6% (below be weight percentage); Halogen-free flame retardants 1020017%, the anti-dripping agent 0.2% of structural formula I, lubricant 0.6%; Oxidation inhibitor 0.6% mixes; The material that mixes is joined in the hopper of twin screw extruder, through melt blending, extruding pelletization becomes.Wherein, screw rod is respectively distinguished the temperature setting and is respectively: twin screw extruder one district temperature 130-140 ℃, two district temperature 170-180 ℃, three district temperature 180-190 ℃, four district temperature 175-185 ℃, head 180-190 ℃, the residence time 1～2min, pressure are 20-30MPa.
Embodiment three
The embodiment of the invention three high-density polyethylene composite material preparing methods comprise the steps:
It is 79.3% HDPE (below be weight percentage) that weight percentage is provided, the anti-dripping agent of the structural formula I of 19% halogen-free flame retardants 10200,0.3%, 0.7% lubricant, 0.7% oxidation inhibitor;
The HDPE weight percentage is 79.3% (below be weight percentage); Halogen-free flame retardants 1020019%, the anti-dripping agent 0.3% of structural formula I, lubricant 0.7%; Oxidation inhibitor 0.7% mixes; The material that mixes is joined in the hopper of twin screw extruder, through melt blending, extruding pelletization becomes.Wherein, screw rod is respectively distinguished the temperature setting and is respectively: twin screw extruder one district temperature 130-140 ℃, two district temperature 170-180 ℃, three district temperature 180-190 ℃, four district temperature 175-185 ℃, head 180-190 ℃, the residence time 1～2min, pressure are 20-30MPa.
Embodiment four
The embodiment of the invention four high-density polyethylene composite material preparing methods comprise the steps:
It is 75% HDPE (below be weight percentage) that weight percentage is provided, the anti-dripping agent of the structural formula I of 23% halogen-free flame retardants 10200,0.4%, 0.8% lubricant, 0.8% oxidation inhibitor;
The HDPE weight percentage is 75% (below be weight percentage); Halogen-free flame retardants HFR-04123%, the anti-dripping agent 0.4% of structural formula I, lubricant 0.8%; Oxidation inhibitor 0.8% mixes; The material that mixes is joined in the hopper of twin screw extruder, through melt blending, extruding pelletization becomes.Wherein, screw rod is respectively distinguished the temperature setting and is respectively: twin screw extruder one district temperature 130-140 ℃, two district temperature 170-180 ℃, three district temperature 180-190 ℃, four district temperature 175-185 ℃, head 180-190 ℃, the residence time 1～2min, pressure are 20-30MPa.
Embodiment five
The embodiment of the invention five high-density polyethylene composite material preparing methods comprise the steps:
It is 72.5% HDPE (below be weight percentage) that weight percentage is provided, the anti-dripping agent of the structural formula I of 25% halogen-free flame retardants 10200,0.5%, 1% lubricant, 1% oxidation inhibitor;
The HDPE weight percentage is 72.5% (below be weight percentage); Halogen-free flame retardants HFR-04125%, the anti-dripping agent 0.5% of structural formula I, lubricant 1%; Oxidation inhibitor 1% mixes; The material that mixes is joined in the hopper of twin screw extruder, through melt blending, extruding pelletization becomes.Wherein, screw rod is respectively distinguished the temperature setting and is respectively: twin screw extruder one district temperature 130-140 ℃, two district temperature 170-180 ℃, three district temperature 180-190 ℃, four district temperature 175-185 ℃, head 180-190 ℃, the residence time 1～2min, pressure are 20-30MPa.
Comparative Examples:
This Comparative Examples high-density polyethylene composite material preparation method comprises the steps:
It is 75% HDPE (below be weight percentage) that weight percentage is provided, the commodity anti-dripping agent DB105 of 23% halogen-free flame retardants 10200,0.4%, 0.8% lubricant, 0.8% oxidation inhibitor;
The HDPE weight percentage is 75% (below be weight percentage); Halogen-free flame retardants HFR-04123%, commodity anti-dripping agent DB1050.4%, lubricant 0.8%; Oxidation inhibitor 0.8% mixes; The material that mixes is joined in the hopper of twin screw extruder, through melt blending, extruding pelletization becomes.Wherein, screw rod is respectively distinguished the temperature setting and is respectively: twin screw extruder one district temperature 130-140 ℃, two district temperature 170-180 ℃, three district temperature 180-190 ℃, four district temperature 175-185 ℃, head 180-190 ℃, the residence time 1～2min, pressure are 20-30MPa.
Performance test:
Tensile strength is tested by ASTM D-638 standard.Specimen types is the I type, batten size (mm): (176 ± 2) (length) * (12.6 ± 0.2) (end width) * (3.05 ± 0.2) (thickness), and draw speed is 50mm/min;
Flexural strength and modulus in flexure are tested by ASTM D-790 standard.Specimen types is specimen size (mm): (128 ± 2) * (12.67 ± 0.2) * (3.11 ± 0.2), rate of bending are 20mm/min;
The socle girder notched Izod impact strength is tested by ASTM D-256 standard.Specimen types is the I type, specimen size (mm): (63 ± 2) * (12.45 ± 0.2) * (3.1 ± 0.2); The breach type is a category-A, and the breach residual thickness is 1.9mm;
Flame retardant properties is tested by UL94, test size (mm): (128 ± 2) * (12.67 ± 0.2) * (3.11 ± 0.2), and flame height 20mm, test bars thickness is respectively 3.2mm, 1.6mm and 0.8mm
Embodiment one～five and Comparative Examples prescription and material property are seen table 1:
Table 1
Can find out that by table 1 anti-dripping agent of structural formula I has higher flame retardant effect to the HDPE resin, when adding proportion 0.2% when above, can effectively suppress the molten of HDPE melt and hang down, make the fire-retardant rank of HDPE bring up to V0 by V2.Compare with similar anti-dripping agent on the market, homemade anti-dripping agent and resin compatible are good, therefore can make material reach higher fire-retardant rank down than few additive, make material have good comprehensive mechanical properties simultaneously.
The above is merely preferred embodiment of the present invention, not in order to restriction the present invention, all any modifications of within spirit of the present invention and principle, being done, is equal to and replaces and improvement etc., all should be included within protection scope of the present invention.
Claims (5)
1. high-density polyethylene composite material comprises following components in weight percentage content:
Said anti-dripping agent has following structural formula I:
wherein, X is a halogens.
2. high-density polyethylene composite material as claimed in claim 1 is characterized in that halogens is selected from fluorine, chlorine, bromine or iodine in the said anti-dripping agent.
3. a high-density polyethylene composite material preparation method comprises the steps:
Following components in weight percentage content is provided:
Said anti-dripping agent has following structural formula I:
Said component mixing is obtained mixture, said mixture is extruded processing, obtain high-density polyethylene composite material.
4. high-density polyethylene composite material preparation method as claimed in claim 3 is characterized in that said halogens is selected from fluorine, chlorine, bromine or iodine.
5. high-density polyethylene composite material as claimed in claim 4 is characterized in that, the said treatment condition of extruding are:
One district temperature 130-140 ℃, two district temperature 170-180 ℃, three district temperature 180-190 ℃, four district temperature 175-185 ℃, head 180-190 ℃, the residence time 1～2min, pressure are 20-30MPa.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107973961A (en) * | 2017-12-08 | 2018-05-01 | 广东技塑新材料股份有限公司 | It is micro- to be crosslinked super stress crack resistant non halogen flame retardant polyolefin composite and preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050026969A1 (en) * | 2003-08-01 | 2005-02-03 | Cheng Jie Fei | Heterocyclic compounds useful as malonyl-CoA decarboxylase inhibitors |
| CN101469089A (en) * | 2008-06-19 | 2009-07-01 | 上海化工研究院 | Halogen-free polyvinyl composite for manufacturing pipes and manufacturing method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050026969A1 (en) * | 2003-08-01 | 2005-02-03 | Cheng Jie Fei | Heterocyclic compounds useful as malonyl-CoA decarboxylase inhibitors |
| CN101469089A (en) * | 2008-06-19 | 2009-07-01 | 上海化工研究院 | Halogen-free polyvinyl composite for manufacturing pipes and manufacturing method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107973961A (en) * | 2017-12-08 | 2018-05-01 | 广东技塑新材料股份有限公司 | It is micro- to be crosslinked super stress crack resistant non halogen flame retardant polyolefin composite and preparation method |
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