CN107857927A - A kind of preparation method of environment-friendly type flame-retardant polyethylene - Google Patents
A kind of preparation method of environment-friendly type flame-retardant polyethylene Download PDFInfo
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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
- 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
- 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
- C08L2312/00—Crosslinking
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Abstract
A kind of preparation method of environment-friendly type flame-retardant polyethylene, its preparation process are as follows：By the parts by weight of high density polyethylene (HDPE) 45 ~ 68,The parts by weight of ethylene-vinyl acetate copolymer 6 ~ 8,Crosslinking agent is 5.5 ~ 8.4 parts by weight,The parts by weight of coupling agent 1 ~ 5,Antioxidant A is 2 ~ 6 parts by weight,The parts by weight of plasticizer 3 ~ 5,The parts by weight of carbon forming agent 5 ~ 7,The anti-parts by weight of molten drop agent 14,The parts by weight of process hides chromium-bearing sludge 3 ~ 7,The parts by weight of antioxidant B0.3 ~ 0.7 are well mixed,According to raw material drying,Dispensing,Mix,It is kneaded,Cool down check rod,This several processes of pelletizing are made,Particularly compounding procedure is carried out in double screw extruder,Ensure that the head pressure of double screw extruder is not less than 4Mpa,200 revs/min of screw speed,Purging vacuum degree is not more than 0.05,Six sections of barrel temperatures are to be Celsius between 180 240 DEG C,Six sections of barrel temperatures are respectively 180 DEG C Celsius,190℃,200℃,210℃,225℃,240℃,The environmental-protection flame-retardant polyethylene of acquisition.
Description
Technical field
The present invention relates to a kind of preparation method of polyethylene, particularly with regard to a kind of environment-friendly type flame-retardant polyethylene
Preparation method.
Background technology
Polyethylene (polyethylene, abbreviation PE) is a kind of aggregated obtained thermoplastic resin of ethene, and PE is five big
One of general-purpose plastics, its yield and consumption figure are occupied first of various synthetic resin, are obtained in industry, agricultural and daily life wide
General application.
Polyethylene belongs to combustible material, and particularly under the conditions of high pressure, thermal source etc., its oxygen index (OI) is 17 or so, is being burnt
When rate of release it is big, calorific value is high, flame propagation speed, decomposes and produces carbon monoxide etc., is not easy to extinguish, easily causes fire,
Huge threat is caused to the safety of life and property of the people.
Common polyethylene is carried out using inorganic combustion inhibitor or inorganic combustion inhibitor by the way of organic fire-retardant is combined
It is fire-retardant, so easily cause that fire retardant addition is big, and add PE production cost.
Patent of invention 201510830488.5 is improved poly- using high density polyethylene (HDPE), TDE, anti-dripping agent
The anti-flammability of ethene, the bright fire resistance that can significantly improve polythene material, makes its flame retardant rating reach V0。
As country is increasingly strict to environmental requirement, process hides chromium-bearing sludge is got over as the solid waste processing cost of process hides
Come higher, the tannery in Jinjiang and Haining area will be sent to the local discarded object center with processing qualification and carry out burning disposal,
The processing cost per ton for needing 2000~3000 yuan of payment, the so invisible production cost for adding process hides, it is therefore desirable to look for
To the approach of feasible reusable edible.
The content of the invention
Traditional polyethylene anti-flaming needs to add fire retardant, and of the invention is the table for making PE using the crosslinked action of crosslinking agent
Layer density is fine and close, improves its anti-flammability, reduces the dosage of fire retardant, reduces fire-retardant PE processing cost, while utilize carbon forming agent
Make the neat coal amout increase that pE burns, improve its anti-flammability, while organic matter is converted into burning in the chromium-bearing sludge of processing
Carbon containing matter.
A kind of preparation method of environment-friendly type flame-retardant polyethylene, its preparation process are as follows：By high density polyethylene (HDPE) 45~68
Parts by weight, the parts by weight of ethene-vinyl acetate vinegar copolymer 6~8, crosslinking agent are 5.5~8.4 parts by weight, the weight of coupling agent 1~5
Part, antioxidant A is 2~6 parts by weight, the parts by weight of plasticizer 3~5, the parts by weight of carbon forming agent 5~7, anti-molten drop agent 1-4 parts by weight,
The parts by weight of the parts by weight of process hides chromium-bearing sludge 3~7, antioxidant B0.3~0.7 are well mixed, according to raw material drying, dispensing, mixing
This several stirring, mixing, cooling check rod, pelletizing processes are made, and particularly compounding procedure is carried out in double screw extruder,
Ensureing that the head pressure of double screw extruder is not less than 4Mpa, 200 revs/min of screw speed, purging vacuum degree is not more than 0.05,
Six sections of barrel temperatures to be Celsius between 180-240 DEG C, six sections of barrel temperatures be respectively it is Celsius 180 DEG C, 190 DEG C, 200 DEG C, 210
DEG C, 225 DEG C, 240 DEG C, the flame-proof polyethylene product of acquisition.
Coupling agent is vinyltrimethoxy silane, methyl vinyl diethoxysilane, 3- mercapto hydroxypropyl methyl dimethoxies
Any one of base silane；Plasticizer is dioctyl phthalate, diisooctyl phthalate, triethylene-glycol hexichol
Any one of formic acid esters, Diethylene Glycol Dibenzoate；Antioxidant A is 2,6 BHTs, 4- hydroxyls ten
Any one of two alkanoic acid anilids, antioxidant 1076, antioxidant 264；Antioxidant B preparation method is：By second
Double (2- amino-ethyls ether) the tetraacethyl 7.9g of glycol are added in reactor, are added potassium permanganate 5g and water 13g, are stirred at 40 DEG C
Reaction 1h is mixed, adds glucose 15g, phthalimide 2.5g and three (nonyl is for phenyl) phosphite ester 2.1g, reacts 2h,
Filtering, obtains antioxidant B；Polymeric aluminum sulfate silicate 6.3g, hexamethylolmelamine 2.3g are added in 15g water, 60 DEG C of reactions
2h, titanium sulfate 1.2g and p-Hydroxybenzoic acid isopropyl ester 0.7g are added, adjust pH to 8,70 DEG C of reaction 1.5h, be spray-dried,
Obtain crosslinking agent；Maleic anhydride 32g, X 2-1401 16g are added in the reactor equipped with agitator and thermometer,
70 DEG C of stirrings add phosphatase 11 68g again, and heating response thing is warming up to 80 DEG C, insulation reaction 2h, adds carbamic acid 12.3g and 2-
Methyl-2-propanol 6.2g, 70 DEG C of reaction 1h, obtains carbon forming agent.
Advantage of the invention is that：
(1) double (the 2- amino-ethyls ether) tetraacethyls of ethylene glycol are oxidized multiple carboxyls, grape in the presence of potassium permanganate
The more remaining potassium permanganate reduction of sugar, phthalimide, three (nonyl is for phenyl) phosphite esters carry out aiding in anti-oxidant, drop
Low chromium-bearing sludge is oxidized to the possibility of Cr VI.
(2) complexing of p-Hydroxybenzoic acid isopropyl ester increase polymeric aluminum sulfate silicate, hexamethylolmelamine, titanium sulfate, it is raw
Into stable crosslinking agent.
(3) anti-molten drop agent of the invention is prepared using 201180043011.2 embodiment (1).
(4) present invention used in process hides chromium-bearing sludge be Hebei Dongming tannery process hides chromium-bearing sludge, chrome green
Content is 24.5%, and is dried in vacuo, it is therefore prevented that trivalent chromium has changed Cr VI.
Embodiment
Example 1
A kind of preparation method of environment-friendly type flame-retardant polyethylene, its preparation process are as follows：By high density polyethylene (HDPE) 45kg, second
Alkene-vinyl acetate copolymer 6kg, crosslinking agent 5.5kg, vinyltrimethoxy silane 1kg, 2,6 BHTs
For 2kg, dioctyl phthalate 3kg, carbon forming agent 5kg, anti-molten drop agent 1kg, process hides chromium-bearing sludge 3kg, antioxidant
B0.3kg is well mixed, make according to this several raw material drying, dispensing, mixing, mixing, cooling check rod, pelletizing processes and
Into particularly compounding procedure is carried out in double screw extruder, it is ensured that the head pressure of double screw extruder is not less than 4Mpa,
200 revs/min of screw speed, purging vacuum degree are not more than 0.05, and to be Celsius between 180-240 DEG C, six sections are expected six sections of barrel temperatures
Cylinder temperature be respectively it is Celsius 180 DEG C, 190 DEG C, 200 DEG C, 210 DEG C, 225 DEG C, 240 DEG C, the flame-proof polyethylene product of acquisition.
Antioxidant B preparation method is：Double (2- amino-ethyls ether) the tetraacethyl 7.9g of ethylene glycol are added to reactor
In, add potassium permanganate 5g and water 13g, stirring reaction 1h at 40 DEG C, add glucose 15g, phthalimide 2.5g
With three (nonyl is for phenyl) phosphite ester 2.1g, 2h is reacted, filtering, obtains antioxidant B；
The preparation method of crosslinking agent is：Polymeric aluminum sulfate silicate 6.3g, hexamethylolmelamine 2.3g are added to 15g water
In, 60 DEG C of reaction 2h, titanium sulfate 1.2g and p-Hydroxybenzoic acid isopropyl ester 0.7g are added, adjust pH to 8,70 DEG C of reactions
1.5h, spray drying, obtains crosslinking agent；
The preparation method of carbon forming agent is：Maleic anhydride 32g, ring-type are added in the reactor equipped with agitator and thermometer
Dimethyl silicone polymer 16g, then 70 DEG C of stirrings add phosphatase 11 68g, and heating response thing is warming up to 80 DEG C, insulation reaction 2h, adds
Carbamic acid 12.3g and 2- methyl-2-propanol 6.2g, 70 DEG C of reaction 1h, obtains carbon forming agent.
Example 2
A kind of preparation method of environment-friendly type flame-retardant polyethylene, its preparation process are as follows：By high density polyethylene (HDPE) 68kg, second
Alkene-vinyl acetate copolymer 8kg, crosslinking agent 8.4kg, methyl vinyl diethoxysilane 5kg, 4- hydroxy-dodecanoic acid
Anilid is 6kg, diisooctyl phthalate 5kg, carbon forming agent 7kg, anti-molten drop agent 4kg, process hides chromium-bearing sludge 7kg, anti-
Oxidant B0.7kg is well mixed, according to this several raw material drying, dispensing, mixing, mixing, cooling check rod, pelletizing processes
It is made, particularly compounding procedure is carried out in double screw extruder, it is ensured that the head pressure of double screw extruder is not small
In 4Mpa, 200 revs/min of screw speed, purging vacuum degree is not more than 0.05, six sections of barrel temperatures to be Celsius between 180-240 DEG C,
Six sections of barrel temperatures be respectively it is Celsius 180 DEG C, 190 DEG C, 200 DEG C, 210 DEG C, 225 DEG C, 240 DEG C, the flame-proof polyethylene system of acquisition
Product.
Antioxidant B preparation method is：Double (2- amino-ethyls ether) the tetraacethyl 7.9g of ethylene glycol are added to reactor
In, add potassium permanganate 5g and water 13g, stirring reaction 1h at 40 DEG C, add glucose 15g, phthalimide 2.5g
With three (nonyl is for phenyl) phosphite ester 2.1g, 2h is reacted, filtering, obtains antioxidant B；
The preparation method of crosslinking agent is：Polymeric aluminum sulfate silicate 6.3g, hexamethylolmelamine 2.3g are added to 15g water
In, 60 DEG C of reaction 2h, titanium sulfate 1.2g and p-Hydroxybenzoic acid isopropyl ester 0.7g are added, adjust pH to 8,70 DEG C of reactions
1.5h, spray drying, obtains crosslinking agent；
The preparation method of carbon forming agent is：Maleic anhydride 32g, ring-type are added in the reactor equipped with agitator and thermometer
Dimethyl silicone polymer 16g, then 70 DEG C of stirrings add phosphatase 11 68g, and heating response thing is warming up to 80 DEG C, insulation reaction 2h, adds
Carbamic acid 12.3g and 2- methyl-2-propanol 6.2g, 70 DEG C of reaction 1h, obtains carbon forming agent.
Example 3
A kind of preparation method of environment-friendly type flame-retardant polyethylene, its preparation process are as follows：By high density polyethylene (HDPE) 56.5kg,
Ethene-vinyl acetate vinegar copolymer 7kg, crosslinking agent 7kg, 3- mercapto hydroxypropyl methyl dimethoxysilane 3kg, antioxidant 1076
For 4kg, triethylene-glycol dibenzoate 4kg, carbon forming agent 6kg, anti-molten drop agent 2.5kg, process hides chromium-bearing sludge 5kg, antioxygen
Agent B0.5kg is well mixed, according to raw material drying, dispensing, mixing, mixing, cooling check rod, pelletizing this several process systems
Form, particularly compounding procedure is carried out in double screw extruder, it is ensured that the head pressure of double screw extruder is not less than
4Mpa, 200 revs/min of screw speed, purging vacuum degree are not more than 0.05, and six sections of barrel temperatures are to be Celsius between 180-240 DEG C, and six
Section barrel temperature be respectively it is Celsius 180 DEG C, 190 DEG C, 200 DEG C, 210 DEG C, 225 DEG C, 240 DEG C, the flame-proof polyethylene product of acquisition.
Antioxidant B preparation method is：Double (2- amino-ethyls ether) the tetraacethyl 7.9g of ethylene glycol are added to reactor
In, add potassium permanganate 5g and water 13g, stirring reaction 1h at 40 DEG C, add glucose 15g, phthalimide 2.5g
With three (nonyl is for phenyl) phosphite ester 2.1g, 2h is reacted, filtering, obtains antioxidant B；
The preparation method of crosslinking agent is：Polymeric aluminum sulfate silicate 6.3g, hexamethylolmelamine 2.3g are added to 15g water
In, 60 DEG C of reaction 2h, titanium sulfate 1.2g and p-Hydroxybenzoic acid isopropyl ester 0.7g are added, adjust pH to 8,70 DEG C of reactions
1.5h, spray drying, obtains crosslinking agent；
The preparation method of carbon forming agent is：Maleic anhydride 32g, ring-type are added in the reactor equipped with agitator and thermometer
Dimethyl silicone polymer 16g, then 70 DEG C of stirrings add phosphatase 11 68g, and heating response thing is warming up to 80 DEG C, insulation reaction 2h, adds
Carbamic acid 12.3g and 2- methyl-2-propanol 6.2g, 70 DEG C of reaction 1h, obtains carbon forming agent.
Example 1-3 data are detected, using the limited oxygen index instrument of Jiangning, Nanjing analytical instrument factory.
Table 1 detects data
Detected using the common PE Plastic Drum of Qingdao Lu Zhou plastic bottles factory, wherein common PE is unsatisfactory for UL-94
Standard, found from table 1, what present invention gained environment-friendly PE Flame Retardancy can be higher than the anti-flammability of common PE is more, and can reach
To UL-94 V-1 and V-0 rank.
Table 2 does not add the data of crosslinking agent
All it is on the basis of instantiation example 1-3 of the present invention is kept to example 1-3 from table 2, has simply added friendship less
Join the experimental data obtained by agent, its anti-flammability fall is than adding the big of crosslinking agent as can be found from Table 2.
Table 3 has added crosslinking agent but has not added the data of carbon forming agent
All it is on the basis of instantiation example 1-3 of the present invention is kept to example 1-3, has simply lacked carbon forming agent, other
The data that sample has, as known from Table 3, not plus the Flame Retardancy of carbon forming agent declines to a great extent, wherein oxygen index (OI) be reduced to 32 with
Under.
Table 4 has added crosslinking agent but has not added the data of p-Hydroxybenzoic acid isopropyl ester
All it is on the basis of instantiation example 1-3 of the present invention is kept to example 1-3, has simply lacked P-hydroxybenzoic acid
Isopropyl ester, the data that other samples have, other have similar explanation.
The data of table 5 (not plus antioxidant B)
All it is on the basis of instantiation example 1-3 of the present invention is kept to example 1-3, has simply lacked antioxidant agent B, sends out
Now antioxidant B has the probability for preventing trivalent chromium conversion Cr VI.
The data of table 6 (not plus phthalimide)
All it is on the basis of instantiation example 1-3 of the present invention is kept to example 1-3, has simply lacked phthalyl Asia
Amine, find not add the content of 6-valence Cr ions of phthalimide higher.
Claims (7)
1. a kind of preparation method of environment-friendly type flame-retardant polyethylene, its preparation process are as follows：By the weight of high density polyethylene (HDPE) 45~68
Part is measured, the parts by weight of ethene-vinyl acetate vinegar copolymer 6~8, crosslinking agent are 5.5~8.4 parts by weight, the parts by weight of coupling agent 1~5,
Antioxidant A is 2~6 parts by weight, the parts by weight of plasticizer 3~5, the parts by weight of carbon forming agent 5~7, anti-molten drop agent 1-4 parts by weight, is made
The parts by weight of leather chromium-bearing sludge 3~7 parts by weight, antioxidant B0.3~0.7 are well mixed, and are stirred according to raw material drying, dispensing, mixing
Mix, be kneaded, cooling down check rod, this several processes of pelletizing are made, particularly compounding procedure is carried out in double screw extruder,
Ensure that the head pressure of double screw extruder is not less than 4Mpa, 200 revs/min of screw speed, purging vacuum degree is not more than 0.05, six
Section barrel temperature be it is Celsius between 180-240 DEG C, six sections of barrel temperatures be respectively it is Celsius 180 DEG C, 190 DEG C, 200 DEG C, 210 DEG C,
225 DEG C, 240 DEG C, the environmental-protection flame-retardant polyethylene of acquisition.
2. the preparation method of a kind of environment-friendly type flame-retardant polyethylene as described in right 1, it is characterised in that described coupling agent is
Any one of vinyltrimethoxy silane, methyl vinyl diethoxysilane, 3- mercapto hydroxypropyl methyl dimethoxysilanes.
3. the preparation method of a kind of environment-friendly type flame-retardant polyethylene as described in right 1, it is characterised in that described plasticizer is
Dioctyl phthalate, diisooctyl phthalate, triethylene-glycol dibenzoate, diglycol hexichol first
Any one of acid esters.
A kind of 4. preparation method of environment-friendly type flame-retardant polyethylene as described in right 1, it is characterised in that described antioxidant
A be 2,6 BHTs, 4- hydroxy-dodecanoic acids anilid, antioxidant 1076, antioxidant 264 it is any one
Kind.
A kind of 5. preparation method of environment-friendly type flame-retardant polyethylene as described in right 1, it is characterised in that described antioxidant
B preparation method is：Double (2- amino-ethyls ether) the tetraacethyl 7.9g of ethylene glycol are added in reactor, add potassium permanganate
5g and water 13g, stirring reaction 1h at 40 DEG C, it is sub- to add glucose 15g, phthalimide 2.5g and three (nonyl is for phenyl)
Phosphate 2.1g, 2h is reacted, filtering, obtains antioxidant B.
6. the preparation method of a kind of environment-friendly type flame-retardant polyethylene as described in right 1, it is characterised in that described crosslinking agent
Preparation method is：Polymeric aluminum sulfate silicate 6.3g, hexamethylolmelamine 2.3g are added in 15g water, 60 DEG C of reaction 2h, then added
Enter titanium sulfate 1.2g and p-Hydroxybenzoic acid isopropyl ester 0.7g, adjust pH to 8,70 DEG C of reaction 1.5h, spray drying, must be crosslinked
Agent.
A kind of 7. preparation method of environment-friendly type flame-retardant polyethylene as described in right 1, it is characterised in that：The preparation side of carbon forming agent
Method is：Maleic anhydride 32g, X 2-1401 16g, then 70 are added in the reactor equipped with agitator and thermometer
DEG C stirring adds phosphatase 11 68g, and heating response thing is warming up to 80 DEG C, insulation reaction 2h, add carbamic acid 12.3g and 2- methyl-
2- propyl alcohol 6.2g, 70 DEG C of reaction 1h, obtains carbon forming agent.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1886453A (en) * | 2003-11-25 | 2006-12-27 | 纳幕尔杜邦公司 | Flame retardant, halogen-free compositions |
| CN106750721A (en) * | 2015-11-25 | 2017-05-31 | 青岛格润得新型材料有限公司 | Flame retardant polyethylene material |
-
2017
- 2017-11-15 CN CN201711135553.8A patent/CN107857927A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1886453A (en) * | 2003-11-25 | 2006-12-27 | 纳幕尔杜邦公司 | Flame retardant, halogen-free compositions |
| CN106750721A (en) * | 2015-11-25 | 2017-05-31 | 青岛格润得新型材料有限公司 | Flame retardant polyethylene material |
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Application publication date: 20180330 |