CN107141551A - A kind of preparation method of high reliability graphene PE pipes - Google Patents

A kind of preparation method of high reliability graphene PE pipes Download PDF

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Publication number
CN107141551A
CN107141551A CN201710221143.9A CN201710221143A CN107141551A CN 107141551 A CN107141551 A CN 107141551A CN 201710221143 A CN201710221143 A CN 201710221143A CN 107141551 A CN107141551 A CN 107141551A
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China
Prior art keywords
graphene
vermiculite
magnesia
pipes
high reliability
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CN201710221143.9A
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Chinese (zh)
Inventor
江锦春
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Zhejiang Weihao Energy Technology Co Ltd
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Zhejiang Weihao Energy Technology Co Ltd
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Priority to CN201710221143.9A priority Critical patent/CN107141551A/en
Publication of CN107141551A publication Critical patent/CN107141551A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/10—Esters; Ether-esters
    • C08K5/101—Esters; Ether-esters of monocarboxylic acids
    • C08K5/103—Esters; Ether-esters of monocarboxylic acids with polyalcohols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/02—Ingredients treated with inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/18—Applications used for pipes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00—Properties characterising the ingredient of the composition
    • C08L2207/06—Properties of polyethylene
    • C08L2207/062—HDPE

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Rigid Pipes And Flexible Pipes (AREA)

Abstract

The invention provides a kind of preparation method of high reliability graphene PE pipes, this method is by vermiculite and magnesia, aluminum oxide and the common ball milling of ethene, inside the layer structure for being conducive to magnesia, aluminum oxide and ethene immersion vermiculite；Under 1,800 2000 DEG C of ultra-high temperature condition; even if ethene has certain protective effect to vermiculite; but vermiculite can still expand 68 times rapidly; it is changed into expanded vermiculite; so magnesia, aluminum oxide will be under ultra-high temperature conditions; there are the time of abundance and the graphite alkene reaction of space and ethylene synthesis; complete the magnesium aluminium ion doping of graphene; so as to generate magnesia-alumina spinel structure in graphenic surface; impact resistance and the resistance to elevated temperatures of graphene are substantially increased, high reliability graphene PE pipes limited oxygen index of the invention can reach 30 32% after tested.

Description

A kind of preparation method of high reliability graphene PE pipes
Technical field
The present invention relates to PE Manifold technologies field, it particularly relates to a kind of preparation method of high reliability graphene PE pipes.
Background technology
PE（Polyethylene）Pipeline is one of most common pipeline, and it has low-temperature impact resistance, resistant to chemical etching, wear-resisting etc. Advantage, feedwater, draining, heat supply, for combustion gas, agricultural irrigation, hydraulic engineering and various commercial plants in be all used widely. In order to improve the mechanical property of PE pipes, its application is expanded, extends its service life, it is necessary to a kind of high reliability stone is researched and developed Black alkene PE pipes.
The content of the invention
In view of this, it is an object of the invention to provide a kind of preparation method of high reliability graphene PE pipes, this method is big It is big to improve magnesia, the using effect of aluminum oxide.
A kind of preparation method of high reliability graphene PE pipes, comprises the following steps：
A, calcium carbonate superfine powder is dried and silane-modified processing is carried out, activation modification calcium carbonate superfine powder powder is made；
B, by magnesia, aluminum oxide and ethene vermiculite be template under conditions of, generate magnalium doped graphene；
C, by high density polyethylene (HDPE), activation modification calcium carbonate superfine powder powder, magnalium doped graphene, pentaerythrite Stearyl Amine and Granulated after antioxidant is well mixed, obtain polyethylene master batch；
D, polyethylene master batch by tube-forming machine extruded into-sizing-traction-cooling and shaping-cutting, tubing is made.
It is preferred that, described antioxidant is Hinered phenols antioxidant.
It is preferred that, the step B comprises the following steps：
Step 1: vermiculite and magnesia, aluminum oxide are put into pulverizer, powdery is crushed to, 250 mesh sieves is crossed, screenings is put Enter in wet ball mill, add ethene, be ground using ball-milling method, obtain compound；
Step 2: compound is poured into quartz reactor, under the conditions of protective gas is added, 1800-2000 DEG C of reaction 6- Compound is poured out after 10min, cooling；
Step 3: removing vermiculite and reacting incomplete magnesia, aluminum oxide compound with being cleaned again with clear water after acid cleaning And ethene.
It is preferred that, in described step two, vermiculite and magnesia, the particle diameter of aluminum oxide are respectively less than 50 μm.
It is preferred that, in described step two, described protective gas is any one in argon gas, nitrogen and helium.
It is preferred that, the weight proportion of each raw material is in the step C：
Magnalium doped graphene：0.1-0.5%
Calcium carbonate superfine powder powder：6-12%
Pentaerythrite Stearyl Amine：0.5-1%
Antioxidant 1-2%
High density polyethylene (HDPE)：Surplus.
The preparation method of high reliability graphene PE pipes provided by the present invention, this method is by vermiculite and magnesia, oxidation Inside aluminium and the common ball milling of ethene, the layer structure for being conducive to magnesia, aluminum oxide and ethene immersion vermiculite；In 1800-2000 DEG C ultra-high temperature condition under, even if ethene has certain protective effect to vermiculite, but vermiculite can still expand 6-8 times rapidly, be changed into Expanded vermiculite, such magnesia, aluminum oxide under ultra-high temperature condition, will have the time of abundance and the stone of space and ethylene synthesis Black alkene reaction, completes the magnesium aluminium ion doping of graphene, so as to generate magnesia-alumina spinel structure in graphenic surface, greatly improves The impact resistance of graphene and resistance to elevated temperatures, after tested high reliability graphene PE pipes limited oxygen index of the invention can reach To 30-32%.
Embodiment
Following examples, to further labor of the invention：
Embodiment 1
A kind of preparation method of high reliability graphene PE pipes, comprises the following steps：
A, calcium carbonate superfine powder is dried and silane-modified processing is carried out, activation modification calcium carbonate superfine powder powder is made；
B, by magnesia, aluminum oxide and ethene vermiculite be template under conditions of, generate magnalium doped graphene；
C, by high density polyethylene (HDPE), activation modification calcium carbonate superfine powder powder, magnalium doped graphene, pentaerythrite Stearyl Amine and Granulated after antioxidant is well mixed, obtain polyethylene master batch；
D, polyethylene master batch by tube-forming machine extruded into-sizing-traction-cooling and shaping-cutting, tubing is made.
The step B, comprises the following steps：
Step 1: vermiculite and magnesia, aluminum oxide are put into pulverizer, powdery is crushed to, 250 mesh sieves is crossed, screenings is put Enter in wet ball mill, add ethene, be ground using ball-milling method, obtain compound；
Step 2: compound is poured into quartz reactor, under the conditions of protective gas is added, 1950 DEG C of reaction 8min, cooling After pour out compound；
Step 3: removing vermiculite and reacting incomplete magnesia, aluminum oxide compound with being cleaned again with clear water after acid cleaning And ethene.
In described step two, vermiculite and magnesia, the particle diameter of aluminum oxide are respectively less than 50 μm.
In described step two, described protective gas is argon gas.
The weight proportion of each raw material is in the step C：
Magnalium doped graphene：0.3%
Calcium carbonate superfine powder powder：8%
Pentaerythrite Stearyl Amine：0.8%
Antioxidant 1.5%
High density polyethylene (HDPE)：Surplus.
Described antioxidant is Hinered phenols antioxidant.
Embodiment 2
A kind of preparation method of high reliability graphene PE pipes, comprises the following steps：
A, calcium carbonate superfine powder is dried and silane-modified processing is carried out, activation modification calcium carbonate superfine powder powder is made；
B, by magnesia, aluminum oxide and ethene vermiculite be template under conditions of, generate magnalium doped graphene；
C, by high density polyethylene (HDPE), activation modification calcium carbonate superfine powder powder, magnalium doped graphene, pentaerythrite Stearyl Amine and Granulated after antioxidant is well mixed, obtain polyethylene master batch；
D, polyethylene master batch by tube-forming machine extruded into-sizing-traction-cooling and shaping-cutting, tubing is made.
The step B, comprises the following steps：
Step 1: vermiculite and magnesia, aluminum oxide are put into pulverizer, powdery is crushed to, 250 mesh sieves is crossed, screenings is put Enter in wet ball mill, add ethene, be ground using ball-milling method, obtain compound；
Step 2: compound is poured into quartz reactor, under the conditions of protective gas is added, 1800 DEG C of reaction 10min, cooling After pour out compound；
Step 3: removing vermiculite and reacting incomplete magnesia, aluminum oxide compound with being cleaned again with clear water after acid cleaning And ethene.
In described step two, vermiculite and magnesia, the particle diameter of aluminum oxide are respectively less than 50 μm.
In described step two, described protective gas is nitrogen.
The weight proportion of each raw material is in the step C：
Magnalium doped graphene：0.1%
Calcium carbonate superfine powder powder：12%
Pentaerythrite Stearyl Amine：0.5%
Antioxidant 2%
High density polyethylene (HDPE)：Surplus.
Described antioxidant is Hinered phenols antioxidant.
Embodiment 3
A kind of preparation method of high reliability graphene PE pipes, comprises the following steps：
A, calcium carbonate superfine powder is dried and silane-modified processing is carried out, activation modification calcium carbonate superfine powder powder is made；
B, by magnesia, aluminum oxide and ethene vermiculite be template under conditions of, generate magnalium doped graphene；
C, by high density polyethylene (HDPE), activation modification calcium carbonate superfine powder powder, magnalium doped graphene, pentaerythrite Stearyl Amine and Granulated after antioxidant is well mixed, obtain polyethylene master batch；
D, polyethylene master batch by tube-forming machine extruded into-sizing-traction-cooling and shaping-cutting, tubing is made.
The step B, comprises the following steps：
Step 1: vermiculite and magnesia, aluminum oxide are put into pulverizer, powdery is crushed to, 250 mesh sieves is crossed, screenings is put Enter in wet ball mill, add ethene, be ground using ball-milling method, obtain compound；
Step 2: compound is poured into quartz reactor, under the conditions of protective gas is added, 2000 DEG C of reaction 6min, cooling After pour out compound；
Step 3: removing vermiculite and reacting incomplete magnesia, aluminum oxide compound with being cleaned again with clear water after acid cleaning And ethene.
In described step two, vermiculite and magnesia, the particle diameter of aluminum oxide are respectively less than 50 μm.
In described step two, described protective gas is helium.
The weight proportion of each raw material is in the step C：
Magnalium doped graphene：0.5%
Calcium carbonate superfine powder powder：6%
Pentaerythrite Stearyl Amine：1%
Antioxidant 1%
High density polyethylene (HDPE)：Surplus.
Described antioxidant is Hinered phenols antioxidant.
After testing, the tensile strength of PE pipes of the invention is 35-40Mpa, and tensile elongation is 250-260%, and limit oxygen refers to Number is 30-30%.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto, Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.

Claims (6)

1. a kind of preparation method of high reliability graphene PE pipes, it is characterised in that comprise the following steps：
A, calcium carbonate superfine powder is dried and silane-modified processing is carried out, activation modification calcium carbonate superfine powder powder is made；
B, by magnesia, aluminum oxide and ethene vermiculite be template under conditions of, generate magnalium doped graphene；
C, by high density polyethylene (HDPE), activation modification calcium carbonate superfine powder powder, magnalium doped graphene, pentaerythrite Stearyl Amine and Granulated after antioxidant is well mixed, obtain polyethylene master batch；
D, polyethylene master batch by tube-forming machine extruded into-sizing-traction-cooling and shaping-cutting, tubing is made.
2. the preparation method of high reliability graphene PE pipes as claimed in claim 1, it is characterised in that described antioxidant is Hinered phenols antioxidant.
3. the preparation method of high reliability graphene PE pipes as claimed in claim 1, it is characterised in that the step B, including Following steps：
Step 1: vermiculite and magnesia, aluminum oxide are put into pulverizer, powdery is crushed to, 250 mesh sieves is crossed, screenings is put Enter in wet ball mill, add ethene, be ground using ball-milling method, obtain compound；
Step 2: compound is poured into quartz reactor, under the conditions of protective gas is added, 1800-2000 DEG C of reaction 6- Compound is poured out after 10min, cooling；
Step 3: removing vermiculite and reacting incomplete magnesia, aluminum oxide compound with being cleaned again with clear water after acid cleaning And ethene.
4. the preparation method of high reliability graphene PE pipes as claimed in claim 3, it is characterised in that described step two In, vermiculite and magnesia, the particle diameter of aluminum oxide are respectively less than 50 μm.
5. the preparation method of high reliability graphene PE pipes as claimed in claim 3, it is characterised in that described step two In, described protective gas is any one in argon gas, nitrogen and helium.
6. the preparation method of high reliability graphene PE pipes as claimed in claim 1, it is characterised in that each in the step C The weight proportion of raw material is：
Magnalium doped graphene：0.1-0.5%
Calcium carbonate superfine powder powder：6-12%
Pentaerythrite Stearyl Amine：0.5-1%
Antioxidant 1-2%
High density polyethylene (HDPE)：Surplus.
CN201710221143.9A 2017-04-06 2017-04-06 A kind of preparation method of high reliability graphene PE pipes Pending CN107141551A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108485021A (en) * 2018-02-02 2018-09-04 桂林理工大学 A kind of graphene/liquid crystal collaboration reinforced thermoplastics pipe and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103408828A (en) * 2013-09-03 2013-11-27 武汉麟青管业有限公司 Preparation method of halogen-free flame-retardant polyethylene (PE) pipe

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103408828A (en) * 2013-09-03 2013-11-27 武汉麟青管业有限公司 Preparation method of halogen-free flame-retardant polyethylene (PE) pipe

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108485021A (en) * 2018-02-02 2018-09-04 桂林理工大学 A kind of graphene/liquid crystal collaboration reinforced thermoplastics pipe and preparation method thereof
CN108485021B (en) * 2018-02-02 2019-07-23 桂林理工大学 A kind of graphene/liquid crystal collaboration reinforced thermoplastics pipe and preparation method thereof

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Application publication date: 20170908