CN108794858A - A kind of preparation method of flame-retardant and anti-static polyethylene resin - Google Patents
A kind of preparation method of flame-retardant and anti-static polyethylene resin Download PDFInfo
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- CN108794858A CN108794858A CN201810616512.9A CN201810616512A CN108794858A CN 108794858 A CN108794858 A CN 108794858A CN 201810616512 A CN201810616512 A CN 201810616512A CN 108794858 A CN108794858 A CN 108794858A
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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
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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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
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/066—LDPE (radical process)
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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
- C08L2314/00—Polymer mixtures characterised by way of preparation
- C08L2314/06—Metallocene or single site catalysts
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Abstract
The invention discloses a kind of preparation methods of flame-retardant and anti-static polyethylene resin, powder will be made with carbon black, toughener hybrid reaction after starch dissolution, as starch-carbon black composite powder, composite powder is reacted with the suspension of alundum (Al2O3), nano silicon dioxide, expansible graphite later, after different base polyethylenes is blended with epoxy resin mixed melting, it is squeezed out with modified carbon black powder, other auxiliary agent melt blendings of preparation, up to flame-retardant and anti-static polyethylene resin after tie rod, water cooling, pelletizing.The present invention is blended by being modified to carbon black with by the polyvinyl resin of different densities so that the uniform cutter of resin has anti-flammability and anlistatig characteristic, good mechanical performance.
Description
Technical field
The invention belongs to compound resin manufacture fields, and in particular to a kind of preparation side of flame-retardant and anti-static polyethylene resin
Method.
Background technology
Polyethylene be one kind by vinyl monomer by polymer made of free crowd, polyethylene can be abbreviated as PE
（polyethylene).Polyethylene has the following mainly unique property, when light weight when compared with metal material, second is that making
Nontoxic to human body and environment, harmless in, third, electrical insulating property and chemical resistance are all good, four are machined to type conveniently, because
This polyethylene is widely used in chemical material industry, electric appliance equipment industry, machine-building, food processing industry and agricultural planting
Etc. various aspects.
Carbon black is developed and is applied as more early in a kind of widely used industrial chemicals and human material's scientific development
Nano material, and conductive black as a kind of typical function kind of carbon black because of its good electric conductivity and higher sexual valence
Than being widely used in conductive and antistatic product.
Invention content
The present invention provides a kind of preparation method of flame-retardant and anti-static polyethylene resin, and the present invention is by being modified carbon black
It is blended with by the polyvinyl resin of different densities so that the uniform cutter of resin has anti-flammability and anlistatig characteristic, mechanics
Function admirable.
The present invention is achieved by the following technical solutions：
A kind of preparation method of flame-retardant and anti-static polyethylene resin, which is characterized in that include the following steps：
（1）Starch-carbon black toughening is compound
a）Stirring and dissolving in suitable deionized water is added in 30-50 weight starch by room temperature, until aqueous solution is clarified;
b）20-30 parts by weight of carbon black per and 3-13 parts by weight toughener are added into amidin, is transferred in high pressure water heating kettle,
It is put into the electric drying oven with forced convection for being set in advance 200-250 DEG C, reaction is taken out after 130-140 minutes, after cooling, is hanged
Supernatant liquid is filtered, and is washed three times, is put into 68-72 DEG C of drying box and is dried 3 hours, the powder of obtained brown, for use；
（2）Modified carbon black
By 5-13 parts by weight alundum (Al2O3), 1-2 parts by weight nano silicon dioxide, 3-5 parts by weight expansible graphite water-baths 40-60
DEG C stirring and dissolving is sufficiently stirred to form uniform suspension, is then gradually added into the ammonia of 3-8% in appropriate tetrahydrofuran solution
Aqueous solution, until the pH value of solution is between 7.5-11, by step（1）The powder of gained pours into dispersion, and is uniformly mixed, warp
Fully filtration drying after washing, for use；
（3）Melt blending
After the different base polyethylene of 80-160 parts by weight is distributed according to the ratio, addition is mixed with 5-25 parts by weight epoxy resin
It is carried out in melt blending to torque rheometer, blending temperature is 180-190 DEG C, screw speed 50r/min, and incorporation time is
10-15 minutes, for use；
（4）It squeezes out
By step（3）The material and step of the melt blending of gained（2）Material, 1-10 parts by weight nucleating agent, the 1.1-1.5 of gained
It is added into double screw extruder after parts by weight lubricant, 1-1.5 parts by weight antioxidant, the mixing of 1-2 parts by weight anti ultraviolet agents
Middle melt blending, up to flame-retardant and anti-static polyethylene resin after tie rod, water cooling, pelletizing.
The different base polyethylenes are HDPE, LLDPE, LDPE-1, and LDPE-2, mPE press 3:2:1:1:1.
The lubricant is oleamide, erucyl amide, stearmide, ethylenebisstearamide, alkylidene two are hard
It is a kind of in acyl amine.
The antioxidant is three monooctyl esters, three last of the ten Heavenly stems esters, four (β-(3,5- three-level butyl -4- hydroxy phenyls) propionic acid) Ji Wusi
It is a kind of in alcohol ester, o-phenol or hydroquinone.
It is an advantage of the invention that：
Powder will be made with carbon black, toughener hybrid reaction after starch dissolution in the present invention, as starch-carbon black composite powder, it
Composite powder is reacted with the suspension of alundum (Al2O3), nano silicon dioxide, expansible graphite afterwards, by different poly- second
After alkenyl body is blended with epoxy resin mixed melting, squeezes out, draw with modified carbon black powder, other auxiliary agent melt blendings of preparation
Up to flame-retardant and anti-static polyethylene resin after item, water cooling, pelletizing.The present invention by using after starch dissolution with carbon black, toughener
Hybrid reaction is made powder, starch and toughener fit closely in the rough surface of carbon black or embedded carbon black micropore and
In mesoporous, complex is formed, alundum (Al2O3), nano silicon dioxide, expansible graphite mixing, tetrahydrofuran is as organic molten
Agent forms the uniform suspension of solute, is combined later with carbon black, increase the roughness of carbon blacksurface, and increase charcoal
The high energy active site on black surface, to improve compatibility and flame retardant property of the modified carbon black in resin matrix, different densities
Polyethylene mixed melting be blended into basis material, the crystallinity for the matrix resin for being it is higher and with filler have it is good compatible
Property, continue to squeeze out later simple for process when being blended, easy to operation, improve polyvinyl resin is easy to charge enrichment, low temperature
The shortcomings of defect poor toughness so that material is also provided with anlistatig effect.The present invention by carbon black be modified with will not
Polyvinyl resin with density is blended so that the uniform cutter of resin has anti-flammability and anlistatig characteristic, mechanical property excellent
It is good.
Specific implementation mode
A kind of preparation method of flame-retardant and anti-static polyethylene resin, which is characterized in that include the following steps：
（1）Starch-carbon black toughening is compound
a）Stirring and dissolving in suitable deionized water is added in 40 weight starch by room temperature, until aqueous solution is clarified;
b）20 parts by weight of carbon black per and 14 parts by weight toughener are added into amidin, is transferred in high pressure water heating kettle, is put into
It has been set in advance in 230 DEG C of electric drying oven with forced convection, reaction is taken out after 135 minutes, after cooling, obtained suspension, was carried out
Filter, and wash three times, it is put into 70 DEG C of drying boxes and dries 3 hours, the powder of obtained brown, for use；
（2）Modified carbon black
By 10 parts by weight alundum (Al2O3)s, 1.5 parts by weight nano silicon dioxides, 4 parts by weight expansible graphite water-bath, 50 DEG C of stirrings
It is dissolved in appropriate tetrahydrofuran solution, is sufficiently stirred to form uniform suspension, be then gradually added into 5% ammonia spirit,
To solution pH value between 7.5-11, by step（1）The powder of gained pours into dispersion, and is uniformly mixed, through fully washing
Rear filtration drying is washed, for use；
（3）Melt blending
After the different base polyethylene of 120 parts by weight is distributed according to the ratio, it is mixed to join and turns with 15 parts by weight epoxy resin
Square rheometer carries out in melt blending, and blending temperature is 185 DEG C, screw speed 50r/min, and incorporation time is 12 minutes, is waited for
With；
（4）It squeezes out
By step（3）The material and step of the melt blending of gained（2）The material of gained, 5 parts by weight nucleating agents, 1.2 parts by weight
Melting is added into double screw extruder altogether after lubricant, 1.2 parts by weight antioxidant, the mixing of 1.5 parts by weight anti ultraviolet agents
It is mixed, up to flame-retardant and anti-static polyethylene resin after tie rod, water cooling, pelletizing.
The different base polyethylenes are HDPE, LLDPE, LDPE-1, and LDPE-2, mPE press 3:2:1:1:1.
The lubricant is oleamide, erucyl amide, stearmide, ethylenebisstearamide, alkylidene two are hard
It is a kind of in acyl amine.
The antioxidant is three monooctyl esters, three last of the ten Heavenly stems esters, four (β-(3,5- three-level butyl -4- hydroxy phenyls) propionic acid) Ji Wusi
It is a kind of in alcohol ester, o-phenol or hydroquinone.
Claims (4)
1. a kind of preparation method of flame-retardant and anti-static polyethylene resin, which is characterized in that include the following steps：
（1）Starch-carbon black toughening is compound
a）Stirring and dissolving in suitable deionized water is added in 30-50 weight starch by room temperature, until aqueous solution is clarified;
b）20-30 parts by weight of carbon black per and 3-13 parts by weight toughener are added into amidin, is transferred in high pressure water heating kettle,
It is put into the electric drying oven with forced convection for being set in advance 200-250 DEG C, reaction is taken out after 130-140 minutes, after cooling, is hanged
Supernatant liquid is filtered, and is washed three times, is put into 68-72 DEG C of drying box and is dried 3 hours, the powder of obtained brown, for use；
（2）Modified carbon black
By 5-13 parts by weight alundum (Al2O3), 1-2 parts by weight nano silicon dioxide, 3-5 parts by weight expansible graphite water-baths 40-60
DEG C stirring and dissolving is sufficiently stirred to form uniform suspension, is then gradually added into the ammonia of 3-8% in appropriate tetrahydrofuran solution
Aqueous solution, until the pH value of solution is between 7.5-11, by step（1）The powder of gained pours into dispersion, and is uniformly mixed, warp
Fully filtration drying after washing, for use；
（3）Melt blending
After the different base polyethylene of 80-160 parts by weight is distributed according to the ratio, addition is mixed with 5-25 parts by weight epoxy resin
It is carried out in melt blending to torque rheometer, blending temperature is 180-190 DEG C, screw speed 50r/min, and incorporation time is
10-15 minutes, for use；
It squeezes out
By step（3）The material and step of the melt blending of gained（2）Material, 1-10 parts by weight nucleating agent, the 1.1-1.5 of gained
It is added into double screw extruder after parts by weight lubricant, 1-1.5 parts by weight antioxidant, the mixing of 1-2 parts by weight anti ultraviolet agents
Middle melt blending, up to flame-retardant and anti-static polyethylene resin after tie rod, water cooling, pelletizing.
2. according to a kind of preparation method of flame-retardant and anti-static polyethylene resin of claim 1, which is characterized in that described is different
Base polyethylene is HDPE, LLDPE, LDPE-1, and LDPE-2, mPE press 3:2:1:1:1.
3. according to a kind of preparation method of flame-retardant and anti-static polyethylene resin of claim 1, which is characterized in that the lubricant
It is a kind of in oleamide, erucyl amide, stearmide, ethylenebisstearamide, alkylidene distearyl amide.
4. according to a kind of preparation method of flame-retardant and anti-static polyethylene resin of claim 1, which is characterized in that the antioxidant
For three monooctyl esters, three last of the ten Heavenly stems esters, four (β-(3,5- three-level butyl -4- hydroxy phenyls) propionic acid) pentaerythritol ester, o-phenols or to benzene
It is a kind of in diphenol.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810616512.9A CN108794858A (en) | 2018-06-15 | 2018-06-15 | A kind of preparation method of flame-retardant and anti-static polyethylene resin |
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| CN201810616512.9A CN108794858A (en) | 2018-06-15 | 2018-06-15 | A kind of preparation method of flame-retardant and anti-static polyethylene resin |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103849024A (en) * | 2012-12-04 | 2014-06-11 | 青岛三利中德美水设备有限公司 | Antistatic and flame-retardant modified polyethylene powder and preparation method thereof |
| CN103881180A (en) * | 2012-12-20 | 2014-06-25 | 青岛欣展塑胶有限公司 | Flame-retardant antistatic bifunctional modified polyethylene composite material and its preparation method |
| CN108752695A (en) * | 2018-06-05 | 2018-11-06 | 芜湖市艾德森自动化设备有限公司 | A kind of preparation method of flame-retardant and anti-static polyethylene resin |
-
2018
- 2018-06-15 CN CN201810616512.9A patent/CN108794858A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103849024A (en) * | 2012-12-04 | 2014-06-11 | 青岛三利中德美水设备有限公司 | Antistatic and flame-retardant modified polyethylene powder and preparation method thereof |
| CN103881180A (en) * | 2012-12-20 | 2014-06-25 | 青岛欣展塑胶有限公司 | Flame-retardant antistatic bifunctional modified polyethylene composite material and its preparation method |
| CN108752695A (en) * | 2018-06-05 | 2018-11-06 | 芜湖市艾德森自动化设备有限公司 | A kind of preparation method of flame-retardant and anti-static polyethylene resin |
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Application publication date: 20181113 |