CN111019048A - Modified PE material, modified PE material plug and preparation method of plug - Google Patents
Modified PE material, modified PE material plug and preparation method of plug Download PDFInfo
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- CN111019048A CN111019048A CN201911329878.9A CN201911329878A CN111019048A CN 111019048 A CN111019048 A CN 111019048A CN 201911329878 A CN201911329878 A CN 201911329878A CN 111019048 A CN111019048 A CN 111019048A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/14—Preparation of carboxylic acid esters from carboxylic acid halides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F4/00—Polymerisation catalysts
- C08F4/28—Oxygen or compounds releasing free oxygen
- C08F4/32—Organic compounds
- C08F4/34—Per-compounds with one peroxy-radical
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
- H01R13/40—Securing contact members in or to a base or case; Insulating of contact members
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
- H01R13/40—Securing contact members in or to a base or case; Insulating of contact members
- H01R13/405—Securing in non-demountable manner, e.g. moulding, riveting
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
- H01R13/46—Bases; Cases
- H01R13/502—Bases; Cases composed of different pieces
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R24/00—Two-part coupling devices, or either of their cooperating parts, characterised by their overall structure
- H01R24/28—Coupling parts carrying pins, blades or analogous contacts and secured only to wire or cable
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R43/00—Apparatus or processes specially adapted for manufacturing, assembling, maintaining, or repairing of line connectors or current collectors or for joining electric conductors
- H01R43/18—Apparatus or processes specially adapted for manufacturing, assembling, maintaining, or repairing of line connectors or current collectors or for joining electric conductors for manufacturing bases or cases for contact members
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
- H01R43/00—Apparatus or processes specially adapted for manufacturing, assembling, maintaining, or repairing of line connectors or current collectors or for joining electric conductors
- H01R43/20—Apparatus or processes specially adapted for manufacturing, assembling, maintaining, or repairing of line connectors or current collectors or for joining electric conductors for assembling or disassembling contact members with insulating base, case or sleeve
- H01R43/24—Assembling by moulding on contact members
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Abstract
The invention discloses a modified PE material, a modified PE material plug and a preparation method of the plug, and relates to the technical field of plugs, wherein the technical scheme is characterized by being prepared from the following raw materials in parts by weight: 20 parts of polyethylene; 1-1.2 parts of butyl acrylate; 3.8-4.5 parts of styrene; 0.8-1.0 part of initiator. The preparation method comprises the following steps: dissolving diisobutyronitrile peroxide in xylene, adding polyethylene, reacting at 95 deg.C for 20min to obtain swollen polyethylene, and distilling under reduced pressure to remove xylene after reaction; dissolving butyl acrylate in DMF, adding into polyethylene, adding styrene, reacting at 90-110 deg.C for 30-60min, and removing impurities to obtain modified PE. The manufactured plug comprises a plug base body, a square through hole, an insulating piece, two pins and a wiring box; two strip-shaped grooves are formed in one side of the insulating part. The invention solves the problem of poor flame retardance of the plug made of the PE material, and achieves the effect of improving the flame retardance of the PE material. In addition, the preparation method of the invention has the advantage of facilitating the grafting of the flame-retardant group on the polyethylene.
Description
Technical Field
The invention relates to the technical field of plugs, in particular to a modified PE material, a modified PE material plug and a preparation method of the plug.
Background
At present, the plug is widely applied in daily life of people. One type of conventional plug is composed of a plug base and pins fixed to the plug base, one end of each pin is exposed outside the plug base for insertion into a corresponding socket for connection to a power source, and the other end of each pin has a long-tail copper pin and passes through the plug base to be connected to a wire.
However, the conventional plug is mostly made of PE materials, most PE products are poor in heat conductivity, low in thermal expansion rate and extremely easy to burn, and therefore potential safety hazards exist in the plug made of the PE materials.
Disclosure of Invention
In view of the disadvantages of the prior art, a first object of the present invention is to provide a modified PE material, which has the advantage of improving the flame retardancy of the PE material.
A second object of the present invention is to provide a plug made of modified PE material, which has the advantage of increased creepage distance.
The third purpose of the invention is to provide a preparation method of the modified PE material, which has the advantage of facilitating the grafting of the flame retardant group on the polyethylene.
In order to achieve the first object, the invention provides the following technical scheme:
a modified PE material is prepared from the following raw materials in parts by weight: 20 parts of polyethylene; 1-1.2 parts of butyl acrylate; 3.8-4.5 parts of styrene; 0.8-1.0 part of initiator.
By adopting the technical scheme, after the initiator is added into the polyethylene, the hydrogen atoms in the polyethylene are abstracted by the free radicals formed by the initiator, and the polyethylene forms high molecular free radicals. Then butyl acrylate and styrene are added into the polymer free radical to carry out polymerization reaction, and polyethylene grafted with polybutyl acrylate and polystyrene is generated. The polybutyl acrylate and the polystyrene are added into the polyethylene, so that the flame retardant property of the polyethylene can be improved, and the flame retardant property of the plug taking the polyethylene as the material is improved.
The invention is further configured to: the butyl acrylate is prepared from the following raw materials in parts by weight: 1.1-1.4 parts of acryloyl chloride; 0.9-1.1 parts of n-butyl alcohol; 0.3-0.5 part of anhydrous sodium bicarbonate; 0.2 part of hydroquinone.
By adopting the technical scheme, acryloyl chloride reacts with n-butyl alcohol to generate butyl acrylate, and anhydrous sodium bicarbonate is added to neutralize hydrochloric acid in a product so as to push the reaction to be carried out in the positive direction; hydroquinone is used as a polymerization inhibitor for preventing the generation of polymers, so that the generation of butyl acrylate is facilitated, and the PE material can be further modified by the butyl acrylate to improve the flame retardant property of the PE material.
The invention is further configured to: the initiator is diisobutyryl peroxide.
By adopting the technical scheme, the-O-O-bond of the diisobutyronitrile peroxide is broken under the heating condition to form two free radicals, and each free radical takes hydrogen atoms in the polyethylene to form isobutyric acid, so that the polyethylene can form high-molecular free radicals, the polyethylene grafting reaction is promoted, and the flame retardant property of the polyethylene is improved.
In order to achieve the second object, the invention provides the following technical scheme:
a modified PE material plug comprises a plug base body, a square through hole formed in one side of the plug base body, an insulating piece embedded in the square through hole, two pins embedded in one side of the insulating piece and a wire harness box fixed at the bottom of the plug base body; two strip-shaped grooves which are arranged in parallel are formed in one side, close to the pin, of the insulating part.
Through adopting above-mentioned technical scheme, through seting up the bar groove on the insulating part, increase creepage distance.
The invention is further configured to: one side of the wire bundling box, which is far away from the pin, is provided with a square groove.
Through adopting above-mentioned technical scheme, set up the easy perk of wire in the plug base member in to the plug base member in-process of moulding plastics, through setting up square groove, square preforming on the mould can pass square groove and inwards press the wire, reduces the possibility that the wire perk.
In order to achieve the third object, the invention provides the following technical solutions: a preparation method of a modified PE material plug comprises the following steps:
dissolving diisobutyryl peroxide in xylene, wherein the solid-to-liquid ratio is 1: 20, adding polyethylene, wherein the weight ratio of the polyethylene to the diisobutyryl peroxide is 20: 0.8-1.0, reacting at 95 ℃ for 20min to obtain swollen polyethylene, and distilling the product under reduced pressure with the vacuum degree of 6mmHg after the reaction is finished to obtain 160 ℃ fraction to obtain swollen polyethylene;
dissolving butyl acrylate in DMF, and adding into the swelled polyethylene, wherein the weight ratio of the butyl acrylate to the polyethylene is 1-1.2: 20, continuously adding styrene, wherein the weight ratio of the styrene to the polyethylene is 3.8-4.5: reacting at the temperature of 20, 90-110 ℃ for 30-60min, adding a saturated sodium chloride solution with the same volume as DMF after the reaction to wash and remove the DMF solvent, and washing the product with deionized water to obtain modified PE;
the modified PE, the zinc borate and the antioxidant 168 are mixed according to the mass ratio of 12: 0.5: 0.25, pouring the mixture into a double-screw extruder for melt extrusion, wherein the melting temperature of a first area of the double-screw extruder is 190 ℃, the melting temperature of a second area of the double-screw extruder is 205 ℃, the melting temperature of a third area of the double-screw extruder is 200 ℃, the head temperature of the double-screw extruder is 190 ℃, the rotating speed of a screw is 250-300rpm, and the retention time is 2-3 min;
pouring the extruded modified PE into a mold for compression molding treatment, wherein the mold temperature is 65-80 ℃, the compression molding temperature is 190-;
injecting the molten polyethylene terephthalate into the square through hole for compression molding treatment, wherein the mold temperature is 75 ℃, the compression molding temperature is 200 ℃, the compression molding time is 30s, and the compression molding pressure is 750 bar.
By adopting the technical scheme, under the heating condition, the-O-O-bond of the diisobutyronitrile peroxide is broken to form two free radicals, and each free radical takes hydrogen atoms in the polyethylene to enable the polyethylene to form a high-molecular free radical; meanwhile, the peroxyacetyl undergoes decarboxylation reaction to generate methyl free radicals and carbon dioxide, so that the subsequent grafting reaction is facilitated; the plug is prepared by melt extrusion after polyethylene modification. The flame retardant property of the PE material is enhanced by grafting butyl acrylate, and the flame retardant property of the plug is improved by modifying the PE material to prepare the plug.
The invention is further configured to: the preparation process of butyl acrylate comprises the following steps: mixing n-butanol, hydroquinone and anhydrous sodium bicarbonate according to a weight ratio of 0.9-1.1: 0.2: 0.3-0.5, dripping acryloyl chloride under stirring, wherein the weight ratio of the added acryloyl chloride to the n-butyl alcohol is (1.1-1.4): reacting at 0.9-1.1 and 0-5 ℃ for 2h, and removing impurities to obtain butyl acrylate.
By adopting the technical scheme, the reaction activity of the n-butyl alcohol and the acryloyl chloride is higher, and the reaction temperature is controlled to be 0-5 ℃ so as to control the reaction to be carried out, thereby facilitating the generation of the butyl acrylate product.
The invention is further configured to: the impurity removal process of butyl acrylate comprises the following steps: adding benzene with the same volume as the n-butyl alcohol into the reaction product to dissolve redundant n-butyl alcohol, extracting to remove a benzene layer, washing the product with a saturated sodium carbonate solution with the same volume as the n-butyl alcohol to remove generated acid, standing for layering, and retaining an organic layer to obtain the butyl acrylate.
By adopting the technical scheme, excessive n-butyl alcohol is added in the reaction of the n-butyl alcohol and the acryloyl chloride to reduce the occurrence of side reaction, the excessive n-butyl alcohol is dissolved by benzene, after a benzene layer is removed by extraction, the excessive n-butyl alcohol is removed along with the benzene layer, and a product is washed by a saturated sodium carbonate solution to remove generated acid.
In summary, compared with the prior art, the invention has the following beneficial effects:
1. by selecting diisobutyryl peroxide as an initiator, hydrogen atoms in polyethylene are abstracted by free radicals formed by the initiator, so that the polyethylene forms high-molecular free radicals;
2. in the reaction process of the n-butyl alcohol and the acryloyl chloride, the reaction temperature is controlled to be 0-5 ℃ so as to control the reaction to be carried out, and the butyl acrylate product is conveniently generated;
3. through seting up the bar groove increase creepage distance on the insulating part, through setting up square groove, be convenient for inwards press the wire, reduce the possibility of the in-process wire perk of moulding plastics.
Drawings
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic view of the protruding square groove of the present invention.
In the figure: 1. a plug base body; 2. a square through hole; 3. an insulating member; 4. a pin; 5. a wire bundling box; 6. a strip-shaped groove; 7. a square groove.
Detailed Description
Examples
Example 1:
a modified PE material is prepared from the following raw materials in parts by weight: 20 parts of polyethylene; 1.1 parts of butyl acrylate; 4.2 parts of styrene; and 0.9 part of an initiator.
The butyl acrylate is prepared from the following raw materials in parts by weight: 1.3 parts of acryloyl chloride; 1.0 part of n-butyl alcohol; 0.4 part of anhydrous sodium bicarbonate; 0.2 part of hydroquinone.
A preparation method of a modified PE material comprises the following steps:
n-butyl alcohol, hydroquinone serving as a polymerization inhibitor and anhydrous sodium bicarbonate are mixed according to the weight ratio of 1.3: 0.2: 0.4, putting into a three-neck flask, slowly dropwise adding acryloyl chloride under the stirring state, wherein the weight ratio of the added acryloyl chloride to n-butyl alcohol is 1.3: 1.0, placing the three-neck flask in a water bath condition at the temperature of 3 ℃ for reaction for 2 hours. And after the reaction is finished, adding benzene with the same volume as the n-butyl alcohol into the three-neck flask to dissolve redundant n-butyl alcohol, extracting to remove a benzene layer, continuously adding saturated sodium carbonate solution with the same volume as the n-butyl alcohol to remove generated acid, standing for layering, and keeping an organic layer to obtain butyl acrylate.
Dissolving an initiator of diisobutyronitrile peroxide in xylene, wherein the solid-to-liquid ratio is 1: 20, adding polyethylene, wherein the weight ratio of the polyethylene to the initiator is 20: 0.9, heating to 95 ℃ in an oil bath for reaction for 20min to obtain polyethylene swelled by the initiator, and distilling the product under reduced pressure at the vacuum degree of 6mmHg after the reaction is finished to obtain 160 ℃ fraction to obtain the swelled polyethylene.
Dissolving butyl acrylate in DMF, and adding into the swelled polyethylene, wherein the weight ratio of the butyl acrylate to the polyethylene is 1.1: 20, continuing to add styrene, wherein the weight ratio of the styrene to the polyethylene is 4.2: performing oil bath reaction at 20 and 100 ℃ for 45 min; and after the reaction is finished, adding a saturated sodium chloride solution with the same volume as the DMF into the product, filtering to remove the filtrate, and washing the product with deionized water to obtain the modified PE.
The modified PE, the zinc borate and the antioxidant 168 are mixed according to the mass ratio of 12: 0.5: 0.25, pouring the mixture into a double-screw extruder for melt extrusion, wherein the melting temperature of a first area of the double-screw extruder is 190 ℃, the melting temperature of a second area of the double-screw extruder is 205 ℃, the melting temperature of a third area of the double-screw extruder is 200 ℃, the head temperature of the double-screw extruder is 190 ℃, the rotating speed of a screw is 275rpm, and the residence time of the double-screw extruder is 2.5 min.
Pouring the extruded modified PE into a mold for compression molding treatment, wherein the mold temperature is 75 ℃, the compression molding temperature is 195 ℃, the compression molding time is 30s, the compression molding pressure is 800bar, cooling at room temperature to form a plug base body 1, and welding the lead and the pins 4 into the square through holes 2 of the plug base body 1.
Injecting the molten polyethylene terephthalate into the square through hole 2 for compression molding treatment, wherein the mold temperature is 75 ℃, the compression molding temperature is 200 ℃, the compression molding time is 30s, and the compression molding pressure is 750 bar.
A plug made of modified PE material is shown in figures 1 and 2 and comprises a plug base body 1, a square through hole 2 arranged on one side of the plug base body 1, an insulating part 3 embedded in the square through hole 2, two pins 4 embedded on one side of the insulating part 3 and a wire harness box 5 fixed at the bottom of the plug base body 1 and communicated with the plug base body 1. Two strip-shaped grooves 6 which are arranged in parallel are arranged on one side of the insulating part 3 close to the pin 4. The wiring box 5 is provided with a square groove 7 at one side far away from the pin 4.
Example 2: example 2 differs from example 1 in that a modified PE material is made from raw materials comprising, in parts by weight: 20 parts of polyethylene; 1 part of butyl acrylate; 4.2 parts of styrene; and 0.9 part of an initiator.
Example 3: example 3 differs from example 1 in that a modified PE material is made from raw materials comprising, in parts by weight: 20 parts of polyethylene; 1.2 parts of butyl acrylate; 4.2 parts of styrene; and 0.9 part of an initiator.
Example 4: example 4 differs from example 1 in that a modified PE material is made from raw materials comprising, in parts by weight: 20 parts of polyethylene; 1.1 parts of butyl acrylate; 3.8 parts of styrene; and 0.9 part of an initiator.
Example 5: example 5 differs from example 1 in that a modified PE material is made from raw materials comprising, in parts by weight: 20 parts of polyethylene; 1.1 parts of butyl acrylate; 4.5 parts of styrene; and 0.9 part of an initiator.
Example 6: example 6 differs from example 1 in that a modified PE material is made from raw materials comprising, in parts by weight: 20 parts of polyethylene; 1.1 parts of butyl acrylate; 4.2 parts of styrene; and 0.8 part of an initiator.
Example 7: example 7 differs from example 1 in that a modified PE material is made from raw materials comprising, in parts by weight: 20 parts of polyethylene; 1.1 parts of butyl acrylate; 4.2 parts of styrene; 1.0 part of an initiator.
Example 8: a modified PE material is prepared from the following raw materials in parts by weight: 20 parts of polyethylene; 1.1 parts of butyl acrylate; 4.2 parts of styrene; and 0.9 part of an initiator.
The butyl acrylate is prepared from the following raw materials in parts by weight: 1.1 parts of acryloyl chloride; 0.9 part of n-butyl alcohol; 0.3 part of anhydrous sodium bicarbonate; 0.2 part of hydroquinone.
A preparation method of a modified PE material comprises the following steps:
n-butyl alcohol, hydroquinone serving as a polymerization inhibitor and anhydrous sodium bicarbonate are mixed according to the weight ratio of 0.9: 0.2: 0.3, putting into a three-neck flask, slowly dropwise adding acryloyl chloride under the stirring state, wherein the weight ratio of the added acryloyl chloride to n-butyl alcohol is 1.1: 0.9, placing the three-neck flask in a water bath condition at 0 ℃ for reaction for 2 h. And after the reaction is finished, adding benzene with the same volume as the n-butyl alcohol into the three-neck flask to dissolve redundant n-butyl alcohol, extracting to remove a benzene layer, continuously adding saturated sodium carbonate solution with the same volume as the n-butyl alcohol to remove generated acid, standing for layering, and keeping an organic layer to obtain butyl acrylate.
Dissolving an initiator of diisobutyronitrile peroxide in xylene, wherein the solid-to-liquid ratio is 1: 20, adding polyethylene, wherein the weight ratio of the polyethylene to the initiator is 20: 0.9, heating to 95 ℃ in an oil bath for reaction for 20min to obtain polyethylene swelled by the initiator, and distilling the product under reduced pressure at the vacuum degree of 6mmHg after the reaction is finished to obtain 160 ℃ fraction to obtain the swelled polyethylene.
Dissolving butyl acrylate in DMF, and adding into the swelled polyethylene, wherein the weight ratio of the butyl acrylate to the polyethylene is 1.1: 20, continuing to add styrene, wherein the weight ratio of the styrene to the polyethylene is 4.2: performing oil bath reaction at 20 and 90 ℃ for 30 min; and after the reaction is finished, adding a saturated sodium chloride solution with the same volume as the DMF into the product, filtering to remove the filtrate, and washing the product with deionized water to obtain the modified PE.
The modified PE, the zinc borate and the antioxidant 168 are mixed according to the mass ratio of 12: 0.5: 0.25, pouring the mixture into a double-screw extruder for melt extrusion, wherein the melting temperature of a first area of the double-screw extruder is 190 ℃, the melting temperature of a second area of the double-screw extruder is 205 ℃, the melting temperature of a third area of the double-screw extruder is 200 ℃, the head temperature of the double-screw extruder is 190 ℃, the rotating speed of a screw is 250rpm, and the residence time of the double-screw extruder is 2 min.
Pouring the extruded modified PE into a mold for compression molding treatment, wherein the mold temperature is 65 ℃, the compression molding temperature is 190 ℃, the compression molding time is 30s, the compression molding pressure is 650bar, cooling at room temperature to form a plug base body 1, and welding the lead and the pins 4 into the square through holes 2 of the plug base body 1.
Injecting the molten polyethylene terephthalate into the square through hole 2 for compression molding treatment, wherein the mold temperature is 75 ℃, the compression molding temperature is 200 ℃, the compression molding time is 30s, and the compression molding pressure is 750 bar.
A plug made of modified PE material is shown in figures 1 and 2 and comprises a plug base body 1, a square through hole 2 arranged on one side of the plug base body 1, an insulating part 3 embedded in the square through hole 2, two pins 4 embedded on one side of the insulating part 3 and a wire harness box 5 fixed at the bottom of the plug base body 1 and communicated with the plug base body 1. Two strip-shaped grooves 6 which are arranged in parallel are arranged on one side of the insulating part 3 close to the pin 4. The wiring box 5 is provided with a square groove 7 at one side far away from the pin 4.
Example 9: a modified PE material is prepared from the following raw materials in parts by weight: 20 parts of polyethylene; 1.1 parts of butyl acrylate; 4.2 parts of styrene; and 0.9 part of an initiator.
The butyl acrylate is prepared from the following raw materials in parts by weight: 1.4 parts of acryloyl chloride; 1.1 parts of n-butyl alcohol; 0.5 part of anhydrous sodium bicarbonate; 0.2 part of hydroquinone.
A preparation method of a modified PE material comprises the following steps:
n-butyl alcohol, hydroquinone serving as a polymerization inhibitor and anhydrous sodium bicarbonate are mixed according to the weight ratio of 1.1: 0.2: 0.5, putting into a three-neck flask, slowly dropwise adding acryloyl chloride under the stirring state, wherein the weight ratio of the added acryloyl chloride to n-butyl alcohol is 1.4: 1.1, placing the three-neck flask in a water bath condition at 5 ℃ for reaction for 2 h. And after the reaction is finished, adding benzene with the same volume as the n-butyl alcohol into the three-neck flask to dissolve redundant n-butyl alcohol, extracting to remove a benzene layer, continuously adding saturated sodium carbonate solution with the same volume as the n-butyl alcohol to remove generated acid, standing for layering, and keeping an organic layer to obtain butyl acrylate.
Dissolving an initiator of diisobutyronitrile peroxide in xylene, wherein the solid-to-liquid ratio is 1: 20, adding polyethylene, wherein the weight ratio of the polyethylene to the initiator is 20: 0.9, heating to 95 ℃ in an oil bath for reaction for 20min to obtain polyethylene swelled by the initiator, and distilling the product under reduced pressure at the vacuum degree of 6mmHg after the reaction is finished to obtain 160 ℃ fraction to obtain the swelled polyethylene.
Dissolving butyl acrylate in DMF, and adding into the swelled polyethylene, wherein the weight ratio of the butyl acrylate to the polyethylene is 1.1: 20, continuing to add styrene, wherein the weight ratio of the styrene to the polyethylene is 4.2: carrying out oil bath reaction at 20 and 110 ℃ for 60 min; and after the reaction is finished, adding a saturated sodium chloride solution with the same volume as the DMF into the product, filtering to remove the filtrate, and washing the product with deionized water to obtain the modified PE.
The modified PE, the zinc borate and the antioxidant 168 are mixed according to the mass ratio of 12: 0.5: 0.25, pouring the mixture into a double-screw extruder for melt extrusion, wherein the melting temperature of a first area of the double-screw extruder is 190 ℃, the melting temperature of a second area of the double-screw extruder is 205 ℃, the melting temperature of a third area of the double-screw extruder is 200 ℃, the head temperature of the double-screw extruder is 190 ℃, the rotating speed of a screw is 300rpm, and the residence time of the double-screw extruder is 3 min.
Pouring the extruded modified PE into a mold for compression molding treatment, wherein the mold temperature is 80 ℃, the compression molding temperature is 200 ℃, the compression molding time is 30s, the compression molding pressure is 950bar, cooling at room temperature to form a plug base body 1, and welding the lead and the pins 4 into the square through holes 2 of the plug base body 1.
Injecting the molten polyethylene terephthalate into the square through hole 2 for compression molding treatment, wherein the mold temperature is 75 ℃, the compression molding temperature is 200 ℃, the compression molding time is 30s, and the compression molding pressure is 750 bar.
A plug made of modified PE material is shown in figures 1 and 2 and comprises a plug base body 1, a square through hole 2 arranged on one side of the plug base body 1, an insulating part 3 embedded in the square through hole 2, two pins 4 embedded on one side of the insulating part 3 and a wire harness box 5 fixed at the bottom of the plug base body 1 and communicated with the plug base body 1. Two strip-shaped grooves 6 which are arranged in parallel are arranged on one side of the insulating part 3 close to the pin 4. The wiring box 5 is provided with a square groove 7 at one side far away from the pin 4.
Comparative example
Comparative example 1: comparative example 1 differs from example 1 in that a modified PE material is made from raw materials comprising, in parts by weight: 20 parts of polyethylene; 0.5 part of butyl acrylate; 4.2 parts of styrene; 1.0 part of an initiator.
Comparative example 2: comparative example 2 differs from example 1 in that a modified PE material is made from raw materials comprising, in parts by weight: 20 parts of polyethylene; 2 parts of butyl acrylate; 4.2 parts of styrene; 1.0 part of an initiator.
Comparative example 3: comparative example 3 differs from example 1 in that no butyl acrylate was added.
Comparative example 4: comparative example 4 differs from example 1 in that a modified PE material is made from raw materials comprising, in parts by weight: 20 parts of polyethylene; 1.1 parts of butyl acrylate; 3.5 parts of styrene; 1.0 part of an initiator.
Comparative example 5: comparative example 5 differs from example 1 in that a modified PE material is made from raw materials comprising, in parts by weight: 20 parts of polyethylene; 1.1 parts of butyl acrylate; 5 parts of styrene; 1.0 part of an initiator.
Comparative example 6: comparative example 6 differs from example 1 in that no styrene was added.
Comparative example 7: comparative example 7 differs from example 1 in that a modified PE material is made from raw materials comprising, in parts by weight: 20 parts of polyethylene; 1.1 parts of butyl acrylate; 4.2 parts of styrene; and 0.5 part of an initiator.
Comparative example 8: comparative example 8 differs from example 1 in that a modified PE material is made from raw materials comprising, in parts by weight: 20 parts of polyethylene; 1.1 parts of butyl acrylate; 4.2 parts of styrene; and 2 parts of an initiator.
Comparative example 9: comparative example 9 differs from example 1 in that no initiator is added.
Performance test
The Limiting Oxygen Index (LOI) of the examples and comparative examples was determined according to GB/T2406.2-2009, respectively;
the UL-94 ratings of the examples and comparative examples were determined according to GB/T2408/IEC 60695-2003, respectively; the test results are shown in table 1.
TABLE 1
| UL-94 rating | LOI/% | UL-94 rating | LOI/% | ||
| Example 1 | V-0 | 32.3 | Comparative example 1 | V-2 | 22.4 |
| Example 2 | V-0 | 31.1 | Comparative example 2 | V-0 | 34.3 |
| Example 3 | V-0 | 34.5 | Comparative example 3 | NR | 17.6 |
| Example 4 | V-0 | 32.5 | Comparative example 4 | V-1 | 27.4 |
| Example 5 | V-0 | 32.9 | Comparative example 5 | V-0 | 31.8 |
| Example 6 | V-0 | 30.7 | Comparative example 6 | NR | 18.1 |
| Example 7 | V-0 | 33.4 | Comparative example 7 | V-2 | 20.6 |
| Example 8 | V-0 | 31.0 | Comparative example 8 | V-0 | 33.9 |
| Example 9 | V-0 | 32.1 | Comparative example 9 | NR | 18.4 |
The limiting oxygen index refers to the volume fraction concentration of oxygen in the polymer in the oxygen and nitrogen mixture when it is just capable of supporting its combustion. As can be seen from Table 1, the limiting oxygen index of the product gradually increases with increasing butyl acrylate or initiator content; when the content of the butyl acrylate is lower than the range defined by the examples or the butyl acrylate is not added in the reactants, the limiting oxygen index of the product is obviously reduced; when the content of styrene is lower than the range defined in the examples, the limiting oxygen index of the product is reduced to 27.4, and when no styrene is added in the reactants, the limiting oxygen index of the product is obviously reduced; when the content of the initiator is below the range defined in the examples or when no initiator is added to the reactants, the limiting oxygen index of the product is significantly reduced.
The UL-94 rating is used to evaluate the ability of a material to extinguish after being ignited. The UL-94 ratings of examples 1-9 were all V-0; when the addition amount of butyl acrylate or styrene or the initiator in the reactants is lower than the range defined in the examples, the UL-94 rating of the product is reduced to different degrees; when no butyl acrylate or styrene or initiator is added to the reactants, the product has no flame retardant capability.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments, and all technical solutions belonging to the idea of the present invention belong to the protection scope of the present invention. It should be noted that modifications and embellishments within the scope of the invention may occur to those skilled in the art without departing from the principle of the invention, and are considered to be within the scope of the invention.
Claims (8)
1. A modified PE material characterized by: the feed is prepared from the following raw materials in parts by weight: 20 parts of polyethylene; 1-1.2 parts of butyl acrylate; 3.8-4.5 parts of styrene; 0.8-1.0 part of initiator.
2. A modified PE material according to claim 1, characterized in that: the butyl acrylate is prepared from the following raw materials in parts by weight: 1.1-1.4 parts of acryloyl chloride; 0.9-1.1 parts of n-butyl alcohol; 0.3-0.5 part of anhydrous sodium bicarbonate; 0.2 part of hydroquinone.
3. A modified PE material according to claim 1, characterized in that: the initiator is diisobutyryl peroxide.
4. The plug made of the modified PE material according to claim 1, which comprises a plug base body (1), a square through hole (2) formed in one side of the plug base body (1), an insulating member (3) embedded in the square through hole (2), two pins (4) embedded in one side of the insulating member (3), and a binding box (5) fixed to the bottom of the plug base body (1) and communicated with the plug base body (1); two strip-shaped grooves (6) are formed in one side, close to the plug pins (4), of the insulating part (3).
5. The plug of claim 4, wherein: one side of the wire binding box (5) far away from the plug pin (4) is provided with a square groove (7).
6. A method for preparing the plug of modified PE material according to claim 1, characterized by comprising the steps of:
dissolving diisobutyryl peroxide in xylene, wherein the solid-to-liquid ratio is 1: 20, adding polyethylene, wherein the weight ratio of the polyethylene to the diisobutyryl peroxide is 20: 0.8-1.0, reacting at 95 ℃ for 20min to obtain swollen polyethylene, and distilling the product under reduced pressure with the vacuum degree of 6mmHg after the reaction is finished to obtain 160 ℃ fraction to obtain swollen polyethylene;
dissolving butyl acrylate in DMF, and adding into the swelled polyethylene, wherein the weight ratio of the butyl acrylate to the polyethylene is 1-1.2: 20, continuously adding styrene, wherein the weight ratio of the styrene to the polyethylene is 3.8-4.5: reacting at the temperature of 20, 90-110 ℃ for 30-60min, adding a saturated sodium chloride solution with the same volume as DMF after the reaction to wash and remove the DMF solvent, and washing the product with deionized water to obtain modified PE;
the modified PE, the zinc borate and the antioxidant 168 are mixed according to the mass ratio of 12: 0.5: 0.25, pouring the mixture into a double-screw extruder for melt extrusion, wherein the melting temperature of a first area of the double-screw extruder is 190 ℃, the melting temperature of a second area of the double-screw extruder is 205 ℃, the melting temperature of a third area of the double-screw extruder is 200 ℃, the head temperature of the double-screw extruder is 190 ℃, the rotating speed of a screw is 250-300rpm, and the retention time is 2-3 min;
pouring the extruded modified PE into a mold for compression molding treatment, wherein the mold temperature is 65-80 ℃, the compression molding temperature is 190-;
injecting the molten polyethylene terephthalate into the square through hole (2) for compression molding treatment, wherein the mold temperature is 75 ℃, the compression molding temperature is 200 ℃, the compression molding time is 30s, and the compression molding pressure is 750 bar.
7. The method for preparing the plug made of the modified PE material according to claim 6, wherein the method comprises the following steps: the preparation process of butyl acrylate comprises the following steps: mixing n-butanol, hydroquinone and anhydrous sodium bicarbonate according to a weight ratio of 0.9-1.1: 0.2: 0.3-0.5, dripping acryloyl chloride under stirring, wherein the weight ratio of the added acryloyl chloride to the n-butyl alcohol is (1.1-1.4): reacting at 0.9-1.1 and 0-5 ℃ for 2h, and removing impurities to obtain butyl acrylate.
8. The method for preparing a plug made of modified PE material according to claim 7, wherein the method comprises the following steps: the impurity removal process of butyl acrylate comprises the following steps: adding benzene with the same volume as the n-butyl alcohol into the reaction product to dissolve redundant n-butyl alcohol, extracting to remove a benzene layer, washing the product with a saturated sodium carbonate solution with the same volume as the n-butyl alcohol to remove generated acid, standing for layering, and retaining an organic layer to obtain the butyl acrylate.
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