CN102875877A - Dynamic crosslinked modified heat-proof polyethylene material and preparation method and application thereof - Google Patents
Dynamic crosslinked modified heat-proof polyethylene material and preparation method and application thereof Download PDFInfo
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- CN102875877A CN102875877A CN2012103768714A CN201210376871A CN102875877A CN 102875877 A CN102875877 A CN 102875877A CN 2012103768714 A CN2012103768714 A CN 2012103768714A CN 201210376871 A CN201210376871 A CN 201210376871A CN 102875877 A CN102875877 A CN 102875877A
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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
- B29C48/001—Combinations of extrusion moulding with other shaping operations
- B29C48/0022—Combinations of extrusion moulding with other shaping operations combined with cutting
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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
- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/04—Particle-shaped
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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
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
- B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
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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
-
- 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
- B29C2948/9258—Velocity
- B29C2948/9259—Angular velocity
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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
- B29C2948/92885—Screw or gear
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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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- 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
- B29C2948/92923—Calibration, after-treatment or cooling zone
Abstract
The invention discloses a dynamic crosslinked modified heat-proof polyethylene material and a preparation method and an application thereof and relates to a plastic material. Raw materials of the dynamic crosslinked modified heat-proof polyethylene material comprise polyethylene powders, a silane coupling agent, organic peroxides, organic tin and heat-proof polyethylene. The preparation method includes (1) mixing and stirring the polyethylene powders, the silane coupling agent, the organic peroxides and the organic tin to obtain a mixture; (2) drying and baking the mixture of the step (1) to subject the polyethylene powders to a silane crosslinking reaction to obtain a reaction product; and (3) mixing the reaction product obtained in the step (2) and the heat-proof polyethylene material to obtain a mixture, and adding the mixture in a double-screw extruder pelletizer for blending extrusion granulation to obtain the modified dynamic crosslinked modified heat-proof polyethylene material. According to the dynamic crosslinked modified heat-proof polyethylene material and the preparation method and the application thereof, a general heat-proof polyethylene material is modified to form a local crosslinked thermoplastic crosslinked polyethylene material, processing advantages of heat-proof polyethylene are guaranteed, and simultaneously the property of the material reaches to or even exceeds that of crosslinked polyethylene.
Description
Technical field
The present invention relates to a kind of plastic material, especially relate to a kind of dynamic crosslinking modified heat resistant polyethylene material and preparation method thereof and application.
Background technology
Crosslinking technological is a kind of important technology that improves the PE performance.Through cross-linking modified PE its performance is significantly improved, the over-all propertieies such as mechanical property, environmental stress cracking resistance, resistance to corrosive chemicals energy, creep resistance and electrical property of PE have not only been significantly improved, and improved very significantly temperature resistant grade, the heat resisting temperature that can make PE is brought up to more than 100 ℃ from 70 ℃, thereby has greatly widened the range of application of PE.
In household and sanitary ware industry, a large amount of polyethylene hoses be can use, crosslinked polyethylene (PEX) and heat-proof polythene (PE-RT) mainly contained.But general crosslinked polyethylene (PEX) material belongs to thermosetting material, directly recycling because degree of crosslinking is too high.Simultaneously, owing to can not heat melt bonding, therefore have influence on the processed and applied of crosslinked polyethylene pipe.And heat-proof polythene has promoted the interior hot temperature of material by special molecular chain structure, also can directly recycle and hot melting cohesion.But owing to do not form chemical bond between the molecular chain, therefore when high temperature, the intensity of material is less, can't satisfy the service requirements under the high-temperature and high-pressure conditions.
In order to bring into play the advantage of cross-linking polyethylene materials, people have invented the multiple-unit tube that crosslinked polyethylene and general thermoplastic polyethylene combination of materials form, be exactly as inner tube or outward appearance crosslinked polyethylene, and then coat one deck thermoplastic polyethylene material, reach the purpose that convenient processing guarantees again hose strength.For example: Chinese patent 00220438.X be exactly internal layer be crosslinked polyethylene pipe, have one outer to be thermoplastic plastic layer's plastics tubing in its end.Chinese patent 02133610.5 discloses a kind of crosslinked polyethylene that utilizes and is internal layer, and heat-proof polythene is outer field hose technology.But above method when producing, must increase equipment investment, and simultaneously, the wall thickness of flexible pipe and cohesive strength also can't guarantee.In addition, for the intensity that guarantees flexible pipe reaches the requirement of crosslinked polyethylene pipe, must increase the thickness of flexible pipe, so that the material cost of flexible pipe and tooling cost obviously increase.
Summary of the invention
The objective of the invention is the advantage for heat resistant polyethylene material, utilize the dynamic crosslinking technology, a kind of thermoplasticity cross-linking polyethylene materials that general heat resistant polyethylene material modification is become partial cross-linking is provided, when guaranteeing the heat-proof polythene processing advantage, so that the performance of material reaches even surmount the dynamic crosslinking modified heat resistant polyethylene material and preparation method thereof and application of crosslinked polyethylene performance.
The raw material of described dynamic crosslinking modified heat resistant polyethylene material forms:
Polyethylene powders 5% ~ 20%;
Silane coupling agent 0.1% ~ 0.4%;
Organo-peroxide 0.01% ~ 0.1%;
Organotin 0.01% ~ 0.04%;
Surplus is heat-proof polythene.
Described polyethylene powders can be selected from Low Density Polyethylene (LDPE) powder, medium-density polyethylene (MDPE) powder, high density polyethylene(HDPE) (HDPE) powder, at least a in ultrahigh molecular weight polyethylene(UHMWPE) (UHMWPE) powder etc.
The particle diameter of described polyethylene powders can be 1～100 μ m.
Described silane coupling agent can be selected from a kind of in vinyltriethoxysilane, vinyltrimethoxy silane, vinyl three (2-methoxy ethoxy) silane, vinyl silane triisopropoxide, octyltri-ethoxysilane, β-(3,4 epoxycyclohexyl)-ethyl trimethoxy silane, γ-glycidyl ether oxygen propyl methyldiethoxysilane, the methyltrimethoxy silane etc.
Described organo-peroxide can be selected from dicumyl peroxide, 2, a kind of in 2-di-tert-butyl peroxide butane, tert-butyl peroxide propyl benzene, the dual-tert-butyl peroxidation isopropyl benzene etc.
Described organotin can be selected from a kind of in stannous octoate, dibutyl tin laurate, dibutyl tin, the tin tetraphenyl etc.
Described heat-proof polythene can adopt common heat-proof polythene (PE-RT) material of extruding for flexible pipe on the market, for example: the DX800 of Korea S SK company, the DOWLEX 2344,2388 of U.S. DOW chemical company, the XRT70 of Dao Daer petro-chemical corporation etc.
The preparation method of described dynamic crosslinking modified heat resistant polyethylene material may further comprise the steps:
1) polyethylene powders is mixed with silane coupling agent, organo-peroxide and organotin, stir;
2) mixture of step 1) is dry, baking makes the reaction of polyethylene powders generation crosslinked with silicane;
3) with step 2) reactant that obtains mixes with heat resistant polyethylene material, puts into blending extrusion granulation in the double-screw extruding pelletizing machine again, obtains the good dynamic crosslinking modified heat resistant polyethylene material of modification.
In step 1), the condition of described stirring can be, and rotating speed is 500r/min, and the time is 5～20min.
In step 2) in, the condition of described baking can be under 85 ℃ condition, baking 2h.
In step 3); the method of described granulation can be: with step 2) reactant that obtains mixes with heat resistant polyethylene material; put into again in the double-screw extruding pelletizing machine, through melt extruding into line, cooling; the processing parameter of pelletizing is: utilize auxiliary feed system to add mixing raw material; rate of feeding is 40～120r/min, and the main-machine screw rotating speed is 200～300r/min, and processing temperature is 190～220 ℃; die pressure is 1.0～6.0MPa, and dicing machine pelletizing speed is 200～400r/min.
In step 3), with step 2) reactant that obtains mixes with heat resistant polyethylene material, put into again blending extrusion granulation in the twin screw extruder, so that local with the crosslinked polyethylene powders generation peroxide crosslinking reaction of heat resistant polyethylene material finally obtains the good dynamic crosslinking heat resistant polyethylene material of modification.
Described dynamic crosslinking modified heat resistant polyethylene material can be used for preparing flexible pipe etc.
Compare with existing heat resistant polyethylene material, the prepared described dynamic crosslinking modified heat resistant polyethylene material of the present invention has the following advantages:
1) the dynamic crosslinking heat resistant polyethylene material performance after the modification promotes greatly, and is as shown in table 1.
Table 1
By as seen from Table 1, adopt the heat-proof polythene of dynamic crosslinking modification, higher than the intensity of general crosslinked polyethylene, and more soft, be more suitable for the extrusion moulding flexible pipe.
2) the dynamic crosslinking heat-proof polythene belongs to thermoplastic material, can process by second melting, makes things convenient for the machine-shaping of flexible pipe, simultaneously directly recycling of defective material, energy-conserving and environment-protective.
3) dynamic crosslinking heat-proof polythene dosage of crosslinking agent is few, sufficient reacting.Resistates is few, reaches the hygienic environment-protecting requirement.
Embodiment
Embodiment 1
According to following prescription: Low Density Polyethylene powder 5%; Vinyltrimethoxy silane coupling agent 0.15%; Dicumyl peroxide 0.015%; Stannous octoate 0.01%; Surplus is heat-proof polythene.Blending extrusion is a granulated into dynamic crosslinking heat resistant polyethylene material and moulding product.
The implementation step is:
Step 1: the Low Density Polyethylene powder is taken by weighing by mass percentage, and adding the interior 5min(of stirring of high-speed mixer rotating speed is 500r/min).
Step 2: take by weighing by mass percentage the vinyltrimethoxy silane coupling agent, the vinyltrimethoxy silane coupling agent is sprayed onto on the Low Density Polyethylene powder in the stirring uniformly.
Step 3: take by weighing by mass percentage dicumyl peroxide, dicumyl peroxide is added on the Low Density Polyethylene powder in the stirring.
Step 4: take by weighing by mass percentage stannous octoate, stannous octoate is added on the Low Density Polyethylene powder in the stirring.
Step 5: continuing to stir the 20min(rotating speed is 500r/min), take out the powder that stirs.Be positioned over baking reaction in the loft drier, temperature is 85 ℃, and the time is 2h.
Step 6: baked powder is taken out, take by weighing heat-proof polythene according to formula rate and put into therewith that to mix the 10min(rotating speed in the homogenizer be 500r/min);
Step 7: the resulting mixing raw material of step 6 is put in the double-screw extruding pelletizing machine, obtain the dynamic crosslinking heat resistant polyethylene material through melt extruding into line, cooling, pelletizing, processing parameter is: utilize auxiliary feed system to add mixing raw material, rate of feeding is 80r/min; The main-machine screw rotating speed is 260r/min; 190 ℃ of one district's temperature, 190 ℃ of two district's temperature, 190 ℃ of three district's temperature, 200 ℃ of four district's temperature, 200 ℃ of five district's temperature, 210 ℃ of six district's temperature, 215 ℃ of seven district's temperature, 215 ℃ of eight district's temperature, 220 ℃ of nine district's temperature, 220 ℃ of ten district's temperature, 220 ℃ of die head temperatures; Dicing machine pelletizing speed is 300r/min.Material property is as shown in table 2.
Step 8: dynamic crosslinking heat resistant polyethylene material pellet is put in the hose extruder, by 9.6 millimeters of following technique extrusion moulding external diameters, the flexible pipe that internal diameter is 6.2 millimeters: 190 ℃ of one section temperature, 200 ℃ of two sections temperature, 210 ℃ of three sections temperature, 220 ℃ of four sections temperature, 220 ℃ of nozzle temperature, rate of feeding is 80r/min, pulling speed 100r/min.
Step 9: the flexible pipe that obtains is carried out the test of high temperature burst pressure, and under 82 ℃ water temperature, flexible pipe can bear the pressure of 1405PSI.
Table 2
Embodiment 2
According to following prescription: Low Density Polyethylene powder 10%; Vinyltrimethoxy silane coupling agent 0.2%; Dicumyl peroxide 0.02%; Stannous octoate 0.015%; Surplus is heat-proof polythene.Blending extrusion is a granulated into dynamic crosslinking heat resistant polyethylene material and moulding product.
Concrete steps are:
Step 1: the Low Density Polyethylene powder is taken by weighing by mass percentage, and adding the interior 5min(of stirring of high-speed mixer rotating speed is 500r/min).
Step 2: take by weighing by mass percentage the vinyltrimethoxy silane coupling agent, the vinyltrimethoxy silane coupling agent is sprayed onto on the Low Density Polyethylene powder in the stirring uniformly.
Step 3: take by weighing by mass percentage dicumyl peroxide, dicumyl peroxide is added on the Low Density Polyethylene powder in the stirring.
Step 4: take by weighing by mass percentage stannous octoate, stannous octoate is added on the Low Density Polyethylene powder in the stirring.
Step 5: continuing to stir the 20min(rotating speed is 500r/min), take out the powder that stirs.Be positioned over baking reaction in the loft drier, temperature is 85 ℃, and the time is 2h.
Step 6: baked powder is taken out, take by weighing heat-proof polythene according to formula rate and put into therewith that to mix the 10min(rotating speed in the homogenizer be 500r/min);
Step 7: the resulting mixing raw material of step 6 is put in the double-screw extruding pelletizing machine, obtain the dynamic crosslinking heat resistant polyethylene material through melt extruding into line, cooling, pelletizing, processing parameter is: utilize auxiliary feed system to add mixing raw material, rate of feeding is 80r/min; The main-machine screw rotating speed is 260r/min; 190 ℃ of one district's temperature, 190 ℃ of two district's temperature, 190 ℃ of three district's temperature, 200 ℃ of four district's temperature, 200 ℃ of five district's temperature, 210 ℃ of six district's temperature, 215 ℃ of seven district's temperature, 215 ℃ of eight district's temperature, 220 ℃ of nine district's temperature, 220 ℃ of ten district's temperature, 220 ℃ of die head temperatures; Dicing machine pelletizing speed is 300r/min.Material property is as shown in table 3.
Step 8: dynamic crosslinking heat resistant polyethylene material pellet is put in the hose extruder, by 9.6 millimeters of following technique extrusion moulding external diameters, the flexible pipe that internal diameter is 6.2 millimeters: 190 ℃ of one section temperature, 200 ℃ of two sections temperature, 210 ℃ of three sections temperature, 220 ℃ of four sections temperature, 220 ℃ of nozzle temperature, rate of feeding is 80r/min, pulling speed 100r/min.
Step 9: the flexible pipe that obtains is carried out the test of high temperature burst pressure, and under 82 ℃ water temperature, flexible pipe can bear the pressure of 1534PSI.
Table 3
Embodiment 3
According to following prescription: ultrahigh molecular weight polyethylene(UHMWPE) powder 5%; Vinyltriethoxysilane coupling agent 0.15%; Dicumyl peroxide 0.015%; Dibutyl tin laurate 0.01%; Surplus is heat-proof polythene.Blending extrusion is a granulated into dynamic crosslinking heat resistant polyethylene material and moulding product.
The implementation step is:
Step 1: the Low Density Polyethylene powder is taken by weighing by mass percentage, and adding the interior 5min(of stirring of high-speed mixer rotating speed is 500r/min).
Step 2: take by weighing by mass percentage the vinyltrimethoxy silane coupling agent, the vinyltrimethoxy silane coupling agent is sprayed onto on the Low Density Polyethylene powder in the stirring uniformly.
Step 3: take by weighing by mass percentage dicumyl peroxide, dicumyl peroxide is added on the Low Density Polyethylene powder in the stirring.
Step 4: take by weighing by mass percentage stannous octoate, stannous octoate is added on the Low Density Polyethylene powder in the stirring.
Step 5: continuing to stir the 20min(rotating speed is 500r/min), take out the powder that stirs.Be positioned over baking reaction in the loft drier, temperature is 85 ℃, and the time is 2h.
Step 6: baked powder is taken out, take by weighing heat-proof polythene according to formula rate and put into therewith that to mix the 10min(rotating speed in the homogenizer be 500r/min).
Step 7: the resulting mixing raw material of step 6 is put in the double-screw extruding pelletizing machine, obtain the dynamic crosslinking heat resistant polyethylene material through melt extruding into line, cooling, pelletizing, processing parameter is: utilize auxiliary feed system to add mixing raw material, rate of feeding is 80r/min; The main-machine screw rotating speed is 260r/min; 190 ℃ of one district's temperature, 190 ℃ of two district's temperature, 190 ℃ of three district's temperature, 200 ℃ of four district's temperature, 200 ℃ of five district's temperature, 210 ℃ of six district's temperature, 215 ℃ of seven district's temperature, 215 ℃ of eight district's temperature, 220 ℃ of nine district's temperature, 220 ℃ of ten district's temperature, 220 ℃ of die head temperatures; Dicing machine pelletizing speed is 300r/min.Material property is as shown in table 4.
Step 8: dynamic crosslinking heat resistant polyethylene material pellet is put in the hose extruder, by 9.6 millimeters of following technique extrusion moulding external diameters, the flexible pipe that internal diameter is 6.2 millimeters: 190 ℃ of one section temperature, 200 ℃ of two sections temperature, 210 ℃ of three sections temperature, 220 ℃ of four sections temperature, 220 ℃ of nozzle temperature, rate of feeding is 80r/min, pulling speed 100r/min.
Step 9: the flexible pipe that obtains is carried out the test of high temperature burst pressure, and under 82 ℃ water temperature, flexible pipe can bear the pressure of 1316PSI.
Table 4
Embodiment 4
According to following prescription: ultrahigh molecular weight polyethylene(UHMWPE) powder 10%; Vinyltriethoxysilane coupling agent 0.3%; Dicumyl peroxide 0.03%; Dibutyl tin laurate 0.02%; Surplus is heat-proof polythene.Blending extrusion is a granulated into dynamic crosslinking heat resistant polyethylene material and moulding product.
The implementation step is:
Step 1: the Low Density Polyethylene powder is taken by weighing by mass percentage, and adding the interior 5min(of stirring of high-speed mixer rotating speed is 500r/min).
Step 2: take by weighing by mass percentage the vinyltrimethoxy silane coupling agent, the vinyltrimethoxy silane coupling agent is sprayed onto on the Low Density Polyethylene powder in the stirring uniformly.
Step 3: take by weighing by mass percentage dicumyl peroxide, dicumyl peroxide is added on the Low Density Polyethylene powder in the stirring.
Step 4: take by weighing by mass percentage stannous octoate, stannous octoate is added on the Low Density Polyethylene powder in the stirring.
Step 5: continuing to stir the 20min(rotating speed is 500r/min), take out the powder that stirs.Be positioned over baking reaction in the loft drier, temperature is 85 ℃, and the time is 2h.
Step 6: baked powder is taken out, take by weighing heat-proof polythene according to formula rate and put into therewith that to mix the 10min(rotating speed in the homogenizer be 500r/min);
Step 7: the resulting mixing raw material of step 6 is put in the double-screw extruding pelletizing machine, obtain the dynamic crosslinking heat resistant polyethylene material through melt extruding into line, cooling, pelletizing, processing parameter is: utilize auxiliary feed system to add mixing raw material, rate of feeding is 80r/min; The main-machine screw rotating speed is 260r/min; 190 ℃ of one district's temperature, 190 ℃ of two district's temperature, 190 ℃ of three district's temperature, 200 ℃ of four district's temperature, 200 ℃ of five district's temperature, 210 ℃ of six district's temperature, 215 ℃ of seven district's temperature, 215 ℃ of eight district's temperature, 220 ℃ of nine district's temperature, 220 ℃ of ten district's temperature, 220 ℃ of die head temperatures; Dicing machine pelletizing speed is 300r/min.Material property is as shown in table 5.
Table 5
Step 8: dynamic crosslinking heat resistant polyethylene material pellet is put in the hose extruder, by following technique extrusion moulding external diameter 9.6mm, the flexible pipe of internal diameter 6.2mm: 190 ℃ of one section temperature, 200 ℃ of two sections temperature, 210 ℃ of three sections temperature, 220 ℃ of four sections temperature, 220 ℃ of nozzle temperature, rate of feeding is 80r/min, pulling speed 100r/min.
Step 9: the flexible pipe that obtains is carried out the test of high temperature burst pressure, and under 82 ℃ water temperature, flexible pipe can bear the pressure of 1458PSI.
Claims (10)
1. dynamic crosslinking modified heat resistant polyethylene material is characterized in that its raw material forms and is by mass percentage:
Polyethylene powders 5% ~ 20%;
Silane coupling agent 0.1% ~ 0.4%;
Organo-peroxide 0.01% ~ 0.1%;
Organotin 0.01% ~ 0.04%;
Surplus is heat-proof polythene.
2. a kind of dynamic crosslinking modified heat resistant polyethylene material as claimed in claim 1, it is characterized in that described polyethylene powders is selected from the Low Density Polyethylene powder, the medium-density polyethylene powder, high-density polyethylene powder, at least a in the ultrahigh molecular weight polyethylene(UHMWPE) powder.
3. a kind of dynamic crosslinking modified heat resistant polyethylene material as claimed in claim 1 or 2, the particle diameter that it is characterized in that described polyethylene powders is 1～100 μ m.
4. a kind of dynamic crosslinking modified heat resistant polyethylene material as claimed in claim 1 is characterized in that described silane coupling agent is selected from a kind of in vinyltriethoxysilane, vinyltrimethoxy silane, vinyl three (2-methoxy ethoxy) silane, vinyl silane triisopropoxide, octyltri-ethoxysilane, β-(3,4 epoxycyclohexyl)-ethyl trimethoxy silane, γ-glycidyl ether oxygen propyl methyldiethoxysilane, the methyltrimethoxy silane.
5. a kind of dynamic crosslinking modified heat resistant polyethylene material as claimed in claim 1, it is characterized in that described organo-peroxide is selected from dicumyl peroxide, 2, a kind of in 2-di-tert-butyl peroxide butane, tert-butyl peroxide propyl benzene, the dual-tert-butyl peroxidation isopropyl benzene.
6. a kind of dynamic crosslinking modified heat resistant polyethylene material as claimed in claim 1 is characterized in that described organotin is selected from a kind of in stannous octoate, dibutyl tin laurate, dibutyl tin, the tin tetraphenyl.
7. the preparation method of a kind of dynamic crosslinking modified heat resistant polyethylene material as claimed in claim 1 is characterized in that may further comprise the steps:
1) polyethylene powders is mixed with silane coupling agent, organo-peroxide and organotin, stir;
2) mixture of step 1) is dry, baking makes the reaction of polyethylene powders generation crosslinked with silicane;
3) with step 2) reactant that obtains mixes with heat resistant polyethylene material, puts into blending extrusion granulation in the double-screw extruding pelletizing machine again, obtains the good dynamic crosslinking modified heat resistant polyethylene material of modification.
8. the preparation method of a kind of dynamic crosslinking modified heat resistant polyethylene material as claimed in claim 7 is characterized in that in step 1), and the condition of described stirring is, rotating speed is 500r/min, and the time is 5～20min.
9. the preparation method of a kind of dynamic crosslinking modified heat resistant polyethylene material as claimed in claim 7 is characterized in that in step 2) in, the condition of described baking is to toast 2h under 85 ℃ condition.
10. the preparation method of a kind of dynamic crosslinking modified heat resistant polyethylene material as claimed in claim 7; it is characterized in that in step 3); the method of described granulation is: with step 2) reactant that obtains mixes with heat resistant polyethylene material; put into again in the double-screw extruding pelletizing machine; through melt extruding into line; cooling; the processing parameter of pelletizing is: utilize auxiliary feed system to add mixing raw material; rate of feeding is 40～120r/min; the main-machine screw rotating speed is 200～300r/min; processing temperature is 190～220 ℃, and die pressure is 1.0～6.0MPa, and dicing machine pelletizing speed is 200～400r/min.
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| CN201210376871.4A CN102875877B (en) | 2012-09-27 | 2012-09-27 | Dynamic crosslinked modified heat-proof polyethylene material and preparation method and application thereof |
| TW102124514A TW201412855A (en) | 2012-09-27 | 2013-07-09 | Dynamic crosslinked modified heat-proof polyethylene material and preparation method and application thereof |
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| CN201210376871.4A CN102875877B (en) | 2012-09-27 | 2012-09-27 | Dynamic crosslinked modified heat-proof polyethylene material and preparation method and application thereof |
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| CN102875877A true CN102875877A (en) | 2013-01-16 |
| CN102875877B CN102875877B (en) | 2014-08-13 |
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| CN201210376871.4A Active CN102875877B (en) | 2012-09-27 | 2012-09-27 | Dynamic crosslinked modified heat-proof polyethylene material and preparation method and application thereof |
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| CN (1) | CN102875877B (en) |
| TW (1) | TW201412855A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105972337A (en) * | 2016-06-23 | 2016-09-28 | 康泰塑胶科技集团有限公司 | Abrasion-resisting, heat-resisting, antibacterial and scale-preventing steel wire skeleton pipe and manufacturing method thereof |
| CN106366398A (en) * | 2016-08-27 | 2017-02-01 | 潍坊市宏源防水材料有限公司 | Peroxide cross-linked polyolefin waterproof coiled material and preparation technology thereof |
| CN106985362A (en) * | 2017-04-20 | 2017-07-28 | 厦门大学嘉庚学院 | Polyethylene production electrical appliance and its application method |
| CN110452435A (en) * | 2019-07-09 | 2019-11-15 | 武汉材料保护研究所有限公司 | A kind of wear resistant composite material and preparation method thereof of tetraphenyltin modified ultra-high molecular weight polyethylene |
| EP3206866B1 (en) | 2014-10-14 | 2020-04-29 | Technip France | Flexible underwater pipe including a layer including a cross-linked polyethylene with increased thermal resistance |
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| US4117195A (en) * | 1974-12-06 | 1978-09-26 | Bicc Limited | Manufacture of extruded products |
| CN1396399A (en) * | 2002-08-15 | 2003-02-12 | 甘国工 | Composite pipe made of non-cross-linking refractory polyethylene and cross-linking polyethylene |
| US20060093769A1 (en) * | 2004-10-29 | 2006-05-04 | Ghislain Biebuyck | Multilayer tube assembly and methods for forming and using the same |
| CN202074138U (en) * | 2011-06-17 | 2011-12-14 | 爱康企业集团(上海)有限公司 | Heat-resisting polyethylene and composite cross-linked polyethylene piping material |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US4117195A (en) * | 1974-12-06 | 1978-09-26 | Bicc Limited | Manufacture of extruded products |
| US4117195B1 (en) * | 1974-12-06 | 1982-09-21 | ||
| CN1396399A (en) * | 2002-08-15 | 2003-02-12 | 甘国工 | Composite pipe made of non-cross-linking refractory polyethylene and cross-linking polyethylene |
| US20060093769A1 (en) * | 2004-10-29 | 2006-05-04 | Ghislain Biebuyck | Multilayer tube assembly and methods for forming and using the same |
| CN202074138U (en) * | 2011-06-17 | 2011-12-14 | 爱康企业集团(上海)有限公司 | Heat-resisting polyethylene and composite cross-linked polyethylene piping material |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3206866B1 (en) | 2014-10-14 | 2020-04-29 | Technip France | Flexible underwater pipe including a layer including a cross-linked polyethylene with increased thermal resistance |
| CN105972337A (en) * | 2016-06-23 | 2016-09-28 | 康泰塑胶科技集团有限公司 | Abrasion-resisting, heat-resisting, antibacterial and scale-preventing steel wire skeleton pipe and manufacturing method thereof |
| CN106366398A (en) * | 2016-08-27 | 2017-02-01 | 潍坊市宏源防水材料有限公司 | Peroxide cross-linked polyolefin waterproof coiled material and preparation technology thereof |
| CN106985362A (en) * | 2017-04-20 | 2017-07-28 | 厦门大学嘉庚学院 | Polyethylene production electrical appliance and its application method |
| CN110452435A (en) * | 2019-07-09 | 2019-11-15 | 武汉材料保护研究所有限公司 | A kind of wear resistant composite material and preparation method thereof of tetraphenyltin modified ultra-high molecular weight polyethylene |
| CN110452435B (en) * | 2019-07-09 | 2022-02-01 | 武汉材料保护研究所有限公司 | Tetraphenyltin modified ultra-high molecular weight polyethylene wear-resistant composite material and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| TW201412855A (en) | 2014-04-01 |
| TWI494361B (en) | 2015-08-01 |
| CN102875877B (en) | 2014-08-13 |
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