CN102875877B - 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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- CN102875877B CN102875877B CN201210376871.4A CN201210376871A CN102875877B CN 102875877 B CN102875877 B CN 102875877B CN 201210376871 A CN201210376871 A CN 201210376871A CN 102875877 B CN102875877 B CN 102875877B
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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 PE performance.Through cross-linking modified PE, can make its performance significantly be 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 because degree of crosslinking is too high, belongs to thermosetting material, directly recycling.Meanwhile, owing to can not heat melting bonding, therefore have influence on the processed and applied of crosslinked polyethylene pipe.And heat-proof polythene is by special molecular chain structure, promoted the interior hot temperature degree of material, also can directly recycle and hot melting cohesion.But owing to not forming chemical bond between molecular chain, therefore, when high temperature, the intensity of material is less, cannot meet the service requirements under 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, it is exactly using crosslinked polyethylene as inner tube or outward appearance, and then coated one deck thermoplastic polyethylene material, reach the object that convenient processing guarantees again hose strength.For example: Chinese patent 00220438.X be exactly internal layer be crosslinked polyethylene pipe, in its end, having a skin is thermoplastic plastic layer's plastics tubing.Chinese patent 02133610.5 discloses a kind of crosslinked polyethylene that utilizes for internal layer, and heat-proof polythene is outer field hose technology.But above method, when producing, must increase equipment investment, and meanwhile, the wall thickness of flexible pipe and cohesive strength also cannot guarantee.In addition, in order to guarantee that the intensity of flexible pipe reaches the requirement of crosslinked polyethylene pipe, must increase the thickness of flexible pipe, the material cost of flexible pipe and tooling cost are obviously increased.
Summary of the invention
The object of the invention is the advantage for heat resistant polyethylene material, utilize dynamic crosslinking technology, a kind of thermoplasticity cross-linking polyethylene materials that general heat resistant polyethylene material modification is become to partial cross-linking is provided, when guaranteeing heat-proof polythene processing advantage, the performance of material is reached 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 one 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, 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, dual-tert-butyl peroxidation isopropyl benzene etc.
Described organotin can be selected from a kind of in stannous octoate, dibutyl tin laurate, dibutyl tin, tin tetraphenyl etc.
Described heat-proof polythene can adopt the common heat-proof polythene of extruding for flexible pipe (PE-RT) material on 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 comprises the following 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) by step 2) reactant that obtains mixes with heat resistant polyethylene material, then put into blending extrusion granulation in double-screw extruding pelletizing machine, obtain the dynamic crosslinking modified heat resistant polyethylene material that modification is good.
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 the condition of 85 ℃, baking 2h.
In step 3); the method of described granulation can be: by step 2) reactant that obtains mixes with heat resistant polyethylene material; put into again in 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 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), by step 2) reactant that obtains mixes with heat resistant polyethylene material, put into again blending extrusion granulation in twin screw extruder, heat resistant polyethylene material part is reacted with crosslinked polyethylene powders generation peroxide crosslinking, finally obtain the dynamic crosslinking heat resistant polyethylene material that modification is good.
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 modification promotes greatly, as shown in table 1.
Table 1
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 extrusion moulding flexible pipe.
2) dynamic crosslinking heat-proof polythene belongs to thermoplastic material, can process by second melting, facilitates the machine-shaping of flexible pipe, directly recycling of defective material simultaneously, energy-conserving and environment-protective.
3) dynamic crosslinking heat-proof polythene dosage of crosslinking agent is few, sufficient reacting.Resistates is few, reaches hygienic environment-protecting requirement.
Embodiment
Embodiment 1
According to following formula: 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 moulding product.
Concrete implementation step is:
Step 1: Low Density Polyethylene powder is taken by mass percentage, and adding stirring 5min(rotating speed in high-speed mixer is 500r/min).
Step 2: take by mass percentage vinyltrimethoxy silane coupling agent, vinyltrimethoxy silane coupling agent is sprayed onto on the Low Density Polyethylene powder in stirring uniformly.
Step 3: take by mass percentage dicumyl peroxide, dicumyl peroxide is added on the Low Density Polyethylene powder in stirring.
Step 4: take by mass percentage stannous octoate, stannous octoate is added on the Low Density Polyethylene powder in stirring.
Step 5: continuing to stir 20min(rotating speed is 500r/min), take out the powder being stirred.Be positioned over baking reaction in loft drier, temperature is 85 ℃, and the time is 2h.
Step 6: baked powder is taken out, take heat-proof polythene according to formula rate and put into therewith that to mix 10min(rotating speed in homogenizer be 500r/min);
Step 7: the resulting mixing raw material of step 6 is put in double-screw extruding pelletizing machine, through melt extruding into line, cooling, pelletizing obtains dynamic crosslinking heat resistant polyethylene material, processing parameter is: utilize auxiliary feed system to add mixing raw material, rate of feeding is 80r/min; Main-machine screw rotating speed is 260r/min; One 190 ℃ of district's temperature, two 190 ℃ of district's temperature, three 190 ℃ of district's temperature, four 200 ℃ of district's temperature, five 200 ℃ of district's temperature, six 210 ℃ of district's temperature, seven 215 ℃ of district's temperature, eight 215 ℃ of district's temperature, nine 220 ℃ of district's temperature, ten 220 ℃ of 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 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 of temperature, 200 ℃ of two sections of temperature, 210 ℃ of three sections of temperature, 220 ℃ of four sections of temperature, 220 ℃ of nozzle temperature, rate of feeding is 80r/min, pulling speed 100r/min.
Step 9: the flexible pipe obtaining is carried out to the test of high temperature burst pressure, and under the water temperature of 82 ℃, flexible pipe can bear the pressure of 1405PSI.
Table 2
Embodiment 2
According to following formula: 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 moulding product.
Concrete steps are:
Step 1: Low Density Polyethylene powder is taken by mass percentage, and adding stirring 5min(rotating speed in high-speed mixer is 500r/min).
Step 2: take by mass percentage vinyltrimethoxy silane coupling agent, vinyltrimethoxy silane coupling agent is sprayed onto on the Low Density Polyethylene powder in stirring uniformly.
Step 3: take by mass percentage dicumyl peroxide, dicumyl peroxide is added on the Low Density Polyethylene powder in stirring.
Step 4: take by mass percentage stannous octoate, stannous octoate is added on the Low Density Polyethylene powder in stirring.
Step 5: continuing to stir 20min(rotating speed is 500r/min), take out the powder being stirred.Be positioned over baking reaction in loft drier, temperature is 85 ℃, and the time is 2h.
Step 6: baked powder is taken out, take heat-proof polythene according to formula rate and put into therewith that to mix 10min(rotating speed in homogenizer be 500r/min);
Step 7: the resulting mixing raw material of step 6 is put in double-screw extruding pelletizing machine, through melt extruding into line, cooling, pelletizing obtains dynamic crosslinking heat resistant polyethylene material, processing parameter is: utilize auxiliary feed system to add mixing raw material, rate of feeding is 80r/min; Main-machine screw rotating speed is 260r/min; One 190 ℃ of district's temperature, two 190 ℃ of district's temperature, three 190 ℃ of district's temperature, four 200 ℃ of district's temperature, five 200 ℃ of district's temperature, six 210 ℃ of district's temperature, seven 215 ℃ of district's temperature, eight 215 ℃ of district's temperature, nine 220 ℃ of district's temperature, ten 220 ℃ of 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 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 of temperature, 200 ℃ of two sections of temperature, 210 ℃ of three sections of temperature, 220 ℃ of four sections of temperature, 220 ℃ of nozzle temperature, rate of feeding is 80r/min, pulling speed 100r/min.
Step 9: the flexible pipe obtaining is carried out to the test of high temperature burst pressure, and under the water temperature of 82 ℃, flexible pipe can bear the pressure of 1534PSI.
Table 3
Embodiment 3
According to following formula: 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 moulding product.
Concrete implementation step is:
Step 1: Low Density Polyethylene powder is taken by mass percentage, and adding stirring 5min(rotating speed in high-speed mixer is 500r/min).
Step 2: take by mass percentage vinyltrimethoxy silane coupling agent, vinyltrimethoxy silane coupling agent is sprayed onto on the Low Density Polyethylene powder in stirring uniformly.
Step 3: take by mass percentage dicumyl peroxide, dicumyl peroxide is added on the Low Density Polyethylene powder in stirring.
Step 4: take by mass percentage stannous octoate, stannous octoate is added on the Low Density Polyethylene powder in stirring.
Step 5: continuing to stir 20min(rotating speed is 500r/min), take out the powder being stirred.Be positioned over baking reaction in loft drier, temperature is 85 ℃, and the time is 2h.
Step 6: baked powder is taken out, take heat-proof polythene according to formula rate and put into therewith that to mix 10min(rotating speed in homogenizer be 500r/min).
Step 7: the resulting mixing raw material of step 6 is put in double-screw extruding pelletizing machine, through melt extruding into line, cooling, pelletizing obtains dynamic crosslinking heat resistant polyethylene material, processing parameter is: utilize auxiliary feed system to add mixing raw material, rate of feeding is 80r/min; Main-machine screw rotating speed is 260r/min; One 190 ℃ of district's temperature, two 190 ℃ of district's temperature, three 190 ℃ of district's temperature, four 200 ℃ of district's temperature, five 200 ℃ of district's temperature, six 210 ℃ of district's temperature, seven 215 ℃ of district's temperature, eight 215 ℃ of district's temperature, nine 220 ℃ of district's temperature, ten 220 ℃ of 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 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 of temperature, 200 ℃ of two sections of temperature, 210 ℃ of three sections of temperature, 220 ℃ of four sections of temperature, 220 ℃ of nozzle temperature, rate of feeding is 80r/min, pulling speed 100r/min.
Step 9: the flexible pipe obtaining is carried out to the test of high temperature burst pressure, and under the water temperature of 82 ℃, flexible pipe can bear the pressure of 1316PSI.
Table 4
Embodiment 4
According to following formula: 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 moulding product.
Concrete implementation step is:
Step 1: Low Density Polyethylene powder is taken by mass percentage, and adding stirring 5min(rotating speed in high-speed mixer is 500r/min).
Step 2: take by mass percentage vinyltrimethoxy silane coupling agent, vinyltrimethoxy silane coupling agent is sprayed onto on the Low Density Polyethylene powder in stirring uniformly.
Step 3: take by mass percentage dicumyl peroxide, dicumyl peroxide is added on the Low Density Polyethylene powder in stirring.
Step 4: take by mass percentage stannous octoate, stannous octoate is added on the Low Density Polyethylene powder in stirring.
Step 5: continuing to stir 20min(rotating speed is 500r/min), take out the powder being stirred.Be positioned over baking reaction in loft drier, temperature is 85 ℃, and the time is 2h.
Step 6: baked powder is taken out, take heat-proof polythene according to formula rate and put into therewith that to mix 10min(rotating speed in homogenizer be 500r/min);
Step 7: the resulting mixing raw material of step 6 is put in double-screw extruding pelletizing machine, through melt extruding into line, cooling, pelletizing obtains dynamic crosslinking heat resistant polyethylene material, processing parameter is: utilize auxiliary feed system to add mixing raw material, rate of feeding is 80r/min; Main-machine screw rotating speed is 260r/min; One 190 ℃ of district's temperature, two 190 ℃ of district's temperature, three 190 ℃ of district's temperature, four 200 ℃ of district's temperature, five 200 ℃ of district's temperature, six 210 ℃ of district's temperature, seven 215 ℃ of district's temperature, eight 215 ℃ of district's temperature, nine 220 ℃ of district's temperature, ten 220 ℃ of 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 hose extruder, by following technique extrusion moulding external diameter 9.6mm, the flexible pipe of internal diameter 6.2mm: 190 ℃ of one section of temperature, 200 ℃ of two sections of temperature, 210 ℃ of three sections of temperature, 220 ℃ of four sections of temperature, 220 ℃ of nozzle temperature, rate of feeding is 80r/min, pulling speed 100r/min.
Step 9: the flexible pipe obtaining is carried out to the test of high temperature burst pressure, and under the water temperature of 82 ℃, flexible pipe can bear the pressure of 1458PSI.
Claims (7)
1. a dynamic crosslinking modified heat resistant polyethylene material, is characterized in that its raw material forms and is by mass percentage:
Surplus is heat-proof polythene;
Described polyethylene powders is selected from Low Density Polyethylene powder, medium-density polyethylene powder, high-density polyethylene powder, at least one in ultrahigh molecular weight polyethylene(UHMWPE) powder;
The particle diameter of described polyethylene powders is 1～100 μ m;
Described a kind of dynamic crosslinking modified heat resistant polyethylene material is prepared by following methods:
1) polyethylene powders is mixed with silane coupling agent, organo-peroxide and organotin, stir;
2) by step 1) mixture dry, baking, makes the reaction of polyethylene powders generation crosslinked with silicane;
3) by step 2) reactant that obtains mixes with heat resistant polyethylene material, then put into blending extrusion granulation in double-screw extruding pelletizing machine, obtain the dynamic crosslinking modified heat resistant polyethylene material that modification is good; The method of described granulation is: by step 2) reactant that obtains mixes with heat resistant polyethylene material; put into again in 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; 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.
2. a kind of dynamic crosslinking modified heat resistant polyethylene material as claimed in claim 1, it 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, methyltrimethoxy silane.
3. 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-bis-(tert-butyl hydroperoxide) butane, tert-butyl peroxide propyl benzene, dual-tert-butyl peroxidation isopropyl benzene.
4. 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, tin tetraphenyl.
5. the preparation method of a kind of dynamic crosslinking modified heat resistant polyethylene material as claimed in claim 1, is characterized in that comprising the following steps:
1) polyethylene powders is mixed with silane coupling agent, organo-peroxide and organotin, stir;
2) by step 1) mixture dry, baking, makes the reaction of polyethylene powders generation crosslinked with silicane;
3) by step 2) reactant that obtains mixes with heat resistant polyethylene material, then put into blending extrusion granulation in double-screw extruding pelletizing machine, obtain the dynamic crosslinking modified heat resistant polyethylene material that modification is good; The method of described granulation is: by step 2) reactant that obtains mixes with heat resistant polyethylene material; put into again in 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; 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.
6. the preparation method of a kind of dynamic crosslinking modified heat resistant polyethylene material as claimed in claim 5, is characterized in that in step 1) in, the condition of described stirring is, and rotating speed is 500r/min, and the time is 5～20min.
7. the preparation method of a kind of dynamic crosslinking modified heat resistant polyethylene material as claimed in claim 5, is characterized in that in step 2) in, the condition of described baking is to toast 2h under the condition of 85 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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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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| FR3020440B1 (en) | 2014-10-14 | 2017-02-10 | Technip France | FLEXIBLE SUBMARINE CONDUIT COMPRISING A LAYER COMPRISING A 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 |
| CN106985362B (en) * | 2017-04-20 | 2023-05-23 | 厦门大学嘉庚学院 | Electrical apparatus for producing polyethylene and use method thereof |
| 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 |
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| GB1526398A (en) * | 1974-12-06 | 1978-09-27 | Maillefer Sa | Manufacture of extruded products |
| CN1239835C (en) * | 2002-08-15 | 2006-02-01 | 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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| TW201412855A (en) | 2014-04-01 |
| TWI494361B (en) | 2015-08-01 |
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