CN101531783B - Delayed cross-linked type silicane cross-linked polyethylene plastic - Google Patents
Delayed cross-linked type silicane cross-linked polyethylene plastic Download PDFInfo
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- CN101531783B CN101531783B CN2008102075990A CN200810207599A CN101531783B CN 101531783 B CN101531783 B CN 101531783B CN 2008102075990 A CN2008102075990 A CN 2008102075990A CN 200810207599 A CN200810207599 A CN 200810207599A CN 101531783 B CN101531783 B CN 101531783B
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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
- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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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
- B29C2948/92819—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 provides a delayed cross-linked type silicane cross-linked polyethylene plastic. The plastic is characterized in that a specific modification auxiliary agent is used for improving the influence extent of the plastic composition by the water-contained environment, improving the storage stability of the plastic and slowing down the pre-cross-link. The use of the modifying agent aims at generating a layer of hydrophobic groups on the material surface so as to delay the contact of polymers and water molecules and delay the cross-link.
Description
Technical field
The present invention relates to a kind of insulation layered material of electric wire, low middle-high density polyethylene pipe material of being used for.Relate in particular to a kind of precrosslink that improves, silane crosslinked polyethylene plastic with delayed cross-linking type.
Background technology
Polyethylene is a kind of fine industrial chemicals, by crosslinking reaction, makes the polyethylene molecule become tridimensional network from two-dirnentional structure, and the chemistry and the physical property of material are enhanced accordingly, and the heat resisting and pressure resisting performance improves.Since crosslinked polyethylene plastic have good heat resistance, carrying capacity by force, do not melt, corrosion-resistant, mechanical property is high, electrical property is excellent, do not contain carcinogenic advantages such as Pb stabilizer, is being used to substitute traditional PVC plastics in increasing electric wire, tubing manufacturing.
As everyone knows, silane crosslinked polyethylene plastic is as long as just can finish crosslinkedly in immersion or the higher environment of water capacity, so water has decisive influence to silane crosslinked polyethylene plastic.And common silane crosslinked polyethylene plastic can't strictly be controlled moisture content in process of production, produces precrosslink through regular meeting, not only needs often to shut down cleaning, has also influenced the apparent and various aspects of performance of follow-up extruding pipe material.Simultaneously, because therefore the influence of moisture in the environment also is very restricted its storage period.
Summary of the invention
The objective of the invention is keeping all advantages of original crosslinked polyethylene plastic simultaneously, improved the crosslinked condition of material in the small amount of moisture environment, the initial stage precrosslink speed of response of material is reduced greatly, the precrosslink degree of minimizing in extrusion equipment, and significantly prolong storage period of silane crosslinked polyethylene plastic.
The present invention is achieved in that this delayed cross-linking type silane crosslinked polyethylene plastic composition comprises (following each component consumption is in parts by weight):
Polyvinyl resin 100
Silane crosslinker 0.8～2.5
Cross-linked evocating agent 0.03～2.5
Crosslinking catalyst 0.1～2.5
Oxidation inhibitor 0.01～2.0
Lubricant 0.1～2.0
Modified additive 0.05～1.0
Polyvinyl resin density among the present invention is 0.900～0.970, and melting index is≤20 grams (190 ℃, 2160 grams/10 minutes).
Silane crosslinker among the present invention is to choose any one kind of them in vinyltrimethoxy silane, vinyltriethoxysilane, vinyl methyl dimethoxysilane, methyltrimethoxy silane, octyltri-ethoxysilane, Union carbide A-162, the dimethyldiethoxysilane or several.Its effect is the splitting of chain that reduces high molecular free radical in cross-linking process, makes polyethylene form cross-linked structure, improves cross-linking efficiency, improves the resistance toheat of goods.
Cross-linked evocating agent among the present invention is benzoyl peroxide, α, α-two (tert-butyl peroxy base) diisopropylbenzene(DIPB), 1, two (tert-butyl peroxy base) diisopropylbenzene(DIPB)s of 4-, dicumyl peroxide, 2,5-dimethyl-2,5 pairs of (tert-butyl peroxy base) hexanes, 2, choose any one kind of them in 5-dimethyl-2,5 pair (tert-butyl peroxy base) hexin-3, ditertiary butyl peroxide, the tert-butyl peroxide or several.Its effect is at a certain temperature, excites the free radical of superoxide, and the H-H reaction on free radical and the carbochain forms new free radical, with the silane crosslinker grafting.
Crosslinking catalyst among the present invention is a dibutyl tin laurate, chooses any one kind of them in lauric acid toxilic acid dibutyl tin, Bis(lauroyloxy)dioctyltin, two (toxilic acid list zinc ester) di-n-butyl tin or several.Its effect is the activity by catalyst themselves, generation and the raising speed of response that water-absorbent is quickened crosslinking reaction, guarantees that product reaches certain degree of crosslinking within a certain period of time.
Oxidation inhibitor among the present invention is that four [3-(3 ', 5 '-di-t-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester, 4,4 '-thiobis-(the 6-tertiary butyl-3-methylphenol), 4,4 '-thiobis (6-tertiary butyl meta-cresol), N, N '-hexamethylene two (3,5-di-t-butyl-4-hydroxyl propionic acid amide), thio-2 acid two laurel tallows, thio-2 acid distearyl alcohol ester, β-(4-hydroxyl-3, the 5-di-tert-butyl-phenyl) the positive octadecanol ester of propionic acid, 2,2 '-thiobis [3,-(3, the 5-di-tert-butyl-hydroxy phenyl) ethyl propionate] in choose any one kind of them or several.Its effect is to suppress goods to wear out, and improves the heat resistance of goods.
Lubricant among the present invention is to choose any one kind of them in polyethylene wax, Poly Propylene Wax, oxidized polyethlene wax, Zinic stearas, calcium stearate, lead stearate, stearylamide, organo-silicone rubber, siloxanes, silicone, fluoroelastomer, stearin, the amide waxe or several.Its effect is to produce inside and outside lubrication, and is few to the processing units wearing and tearing, and reduces energy consumption.
Modified additive among the present invention is to choose any one kind of them in ethylene-propylene acid sodium-salt ionic copolymer, ethylene-propylene acid potassium salt ionic copolymer, ethylene-acrylic acid lithium salts ionic copolymer, ethylene-methyl methacrylate sodium salt ionic copolymer, ethylene-methyl methacrylate sylvite ionic copolymer, ethylene-methyl methacrylate lithium salts ionic copolymer, polyvinyl alcohol, Sodium dodecylbenzene sulfonate, the m-nitrobenzene sodium sulfonate or several.Its effect is to produce the non-hydrophilic group of one deck at material surface, and the slow polymkeric substance of resistance contacts delayed cross-linking speed with water molecules.
The preparation method of the vinyon of the delayed cross-linking type crosslinked with silicane among the present invention is a two step method, comprises preparation A material and B material, and the mixing of A material and B material, and the A material is the silane grafted material, and the B material is catalyst masterbatch.
Preparation process is:
The preparation of a, A material: the polyvinyl resin pre-treatment is dried to below the moisture 400ppm, then with silane crosslinker, cross-linked evocating agent, oxidation inhibitor, modified additive thorough mixing, enter the forcing machine extruding pelletization at 100 ℃～250 ℃, the later finished product of granulation is dried to moisture content less than below the 250ppm, is stored in the vacuum packaging bag.
The preparation of b, B material: polyvinyl resin, oxidation inhibitor, crosslinking catalyst, lubricant are entered the forcing machine granulation with compound behind the thorough mixing in the high-speed mixer of 80～250 rev/mins of rotating speeds, moisture content of finished products content after the granulation is less than below the 200ppm, be stored in the vacuum packaging bag 80 ℃～200 ℃ of extruder temperatures.
Among step a and the step b, polyvinyl resin is used for the A material and is 80%～98% weight percent of its total amount, is used for the B material and is 2%～20% weight percent of its total amount.Oxidation inhibitor is used for the A material and is 75%～85% weight percent of its total amount, is used for the B material and is 15%～25% weight percent of its total amount.
A, B material thorough mixing enters forcing machine and makes cable or pipe material product when c, use, and product is finished the cross-linking process of crosslinked with silicane plastics in water-bath more than 85 ℃.
Compared with prior art, the present invention has following advantage:
A, the present invention have possessed all advantages of crosslinked polyethylene wire cable material and tube material.
B, the present invention use novel modified additive, have reduced in electric wire and the tubing extrusion precrosslink particulate and have led to a phenomenon, and give goods bright and clean apparent.
C, the present invention have prolonged the cleaning cycle of extrusion screw rod, have solved electric wire, short defective of tubing continuous production cycle.
But d, the present invention have prolonged the preservation valid period of the vinyon A material of crosslinked with silicane, have improved stability of material, have improved product property, and it is convenient to bring to the user.
In conjunction with the embodiments content of the present invention is described further.
Table one embodiment
Silane crosslinker is a vinyltrimethoxy silane; Cross-linked evocating agent is 1, two (tert-butyl peroxy base) diisopropylbenzene(DIPB)s of 4-; The crosslinking catalyst dibutyl tin laurate; Oxidation inhibitor is β-positive octadecanol ester of (4-hydroxyl-3,5-di-tert-butyl-phenyl) propionic acid; Lubricant is oxidized polyethlene wax, polydimethylsiloxanepolymer polymer; Modified additive is Sodium dodecylbenzene sulfonate, ethylene-acrylic acid lithium salts ionic copolymer.
More than the rate of crosslinking (degree of crosslinking over time rate) of product (getting the thick batten of 1mm) in 85 ℃ of water-baths of three examples as follows:
Table two rate of crosslinking change list
Example 1 is used for the short period of time domestic demand is reached occasion than high-crosslinking-degree, as electric wire.
Example 2 is used for to the long-term apparent occasion that has higher requirements of goods, as electric wire, tubing.
Example 3 is used for the internal structure complexity, is difficult for the often occasion of cleaning extrusion equipment, as electric wire, corrugated tube, tubing.
Claims (8)
1. the silane crosslinked polyethylene plastic of a delayed cross-linking type, it is characterized in that: use specific modification auxiliary agent to improve this plastics composite and be subjected to the aqueous environment effect, improve its package stability and reduce its precrosslink speed, in the main polymer polyvinyl resin is 100 weight parts, and the composition of described silane crosslinked polyethylene plastic comprises:
Weight part
Polyvinyl resin 100
Silane crosslinker 0.8～2.5
Cross-linked evocating agent 0.03～2.5
Crosslinking catalyst 0.1～2.5
Oxidation inhibitor 0.01～2.0
Lubricant 0.1～2.0
Modified additive 0.05～1.0;
Described modified additive is selected from: one or more in ethylene-propylene acid sodium-salt ionic copolymer, ethylene-propylene acid potassium salt ionic copolymer, ethylene-acrylic acid lithium salts ionic copolymer, ethylene-methyl methacrylate sodium salt ionic copolymer, ethylene-methyl methacrylate sylvite ionic copolymer, ethylene-methyl methacrylate lithium salts ionic copolymer, polyvinyl alcohol, Sodium dodecylbenzene sulfonate, the m-nitrobenzene sodium sulfonate.
2. silane crosslinked polyethylene plastic according to claim 1 is characterized in that: described polyvinyl resin relative density is 0.900～0.970, and at 190 ℃, the melting index that records under the 2160g/10min condition is 18～20g.
3. silane crosslinked polyethylene plastic according to claim 1 is characterized in that: described silane crosslinker is selected from: one or more in vinyltrimethoxy silane, vinyltriethoxysilane, vinyl methyl dimethoxysilane, methyltrimethoxy silane, octyltri-ethoxysilane, Union carbide A-162 or the dimethyldiethoxysilane.
4. silane crosslinked polyethylene plastic according to claim 1, it is characterized in that: described cross-linked evocating agent is selected from: benzoyl peroxide, α, α-two (tert-butyl peroxy base) diisopropylbenzene(DIPB), 1, two (tert-butyl peroxy base) diisopropylbenzene(DIPB)s of 4-, dicumyl peroxide, 2,5-dimethyl-2,5 pairs of (tert-butyl peroxy base) hexanes, 2, one or more in 5-dimethyl-2,5 pair (tert-butyl peroxy base) hexin-3, ditertiary butyl peroxide or the tert-butyl peroxide.
5. silane crosslinked polyethylene plastic according to claim 1, it is characterized in that: described crosslinking catalyst is selected from: dibutyl tin laurate, one or more in lauric acid toxilic acid dibutyl tin, Bis(lauroyloxy)dioctyltin or two (toxilic acid list zinc ester) di-n-butyl tin.
6. silane crosslinked polyethylene plastic according to claim 1, it is characterized in that: described oxidation inhibitor is selected from: four [3-(3 ', 5 '-di-t-butyl-4 '-hydroxy phenyl) propionic acid] pentaerythritol ester, 4,4 '-thiobis-(the 6-tertiary butyl-3-methylphenol), 4,4 '-thiobis (6-tertiary butyl meta-cresol), N, N '-hexamethylene two (3,5-di-t-butyl-4-hydroxyl propionic acid amide), thio-2 acid two laurel tallows, thio-2 acid distearyl alcohol ester, β-(4-hydroxyl-3, the 5-di-tert-butyl-phenyl) the positive octadecanol ester of propionic acid or 2, in 2 '-thiobis [3 ,-(3, the 5-di-tert-butyl-hydroxy phenyl) ethyl propionate] one or more.
7. silane crosslinked polyethylene plastic according to claim 1 is characterized in that: described lubricant is selected from: one or more in polyethylene wax, Poly Propylene Wax, oxidized polyethlene wax, Zinic stearas, calcium stearate, lead stearate, stearylamide, organo-silicone rubber, siloxanes, silicone, fluoroelastomer, stearin or the amide waxe.
8. preparation method according to the described silane crosslinked polyethylene plastic of claim 1, it is characterized in that, described preparation method is a two step method, that is: the first step prepares A material and B material respectively, second step was the mixing of A material and B material, and wherein, the A material is the silane grafted material, the B material is catalyst masterbatch, and concrete steps are:
The preparation of a, A material: the polyvinyl resin pre-treatment is dried to below the moisture 400ppm, then with silane crosslinker, cross-linked evocating agent, oxidation inhibitor, modified additive thorough mixing, enter the forcing machine extruding pelletization at 100 ℃～250 ℃, the later finished product of granulation is dried to moisture content less than below the 250ppm, is stored in the vacuum packaging bag;
The preparation of b, B material: polyvinyl resin, oxidation inhibitor, crosslinking catalyst, lubricant are entered the forcing machine granulation with compound behind the thorough mixing in the high-speed mixer of 80～250 rev/mins of rotating speeds, moisture content of finished products content after the granulation is less than below the 200ppm, be stored in the vacuum packaging bag 80 ℃～200 ℃ of extruder temperatures;
Among step a and the step b, polyvinyl resin is used for the A material and is 80%～98% weight percent of its total amount, be used for the B material and be 2%～20% weight percent of its total amount, oxidation inhibitor is used for the A material and is 75%～85% weight percent of its total amount, is used for the B material and is 15%～25% weight percent of its total amount.
A, B material thorough mixing enters forcing machine and makes cable or pipe material product when c, use, and product is finished the cross-linking process of crosslinked with silicane plastics in water-bath more than 85 ℃.
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