CN111675848A - HDPE (high-density polyethylene) pipe and preparation method thereof - Google Patents
HDPE (high-density polyethylene) pipe and preparation method thereof Download PDFInfo
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- CN111675848A CN111675848A CN202010643946.5A CN202010643946A CN111675848A CN 111675848 A CN111675848 A CN 111675848A CN 202010643946 A CN202010643946 A CN 202010643946A CN 111675848 A CN111675848 A CN 111675848A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C08L23/0892—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms containing monomers with other atoms than carbon, hydrogen or oxygen atoms
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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
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/16—Copolymers of ethene with alpha-alkenes, e.g. EP rubbers
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- 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
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- 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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Abstract
The invention provides an HDPE (high-density polyethylene) pipe and a preparation method thereof, which are characterized in that firstly, a catalyst is prepared by mixing and reacting a vanadium-modified SBA-15 molecular sieve, titanium tetrachloride and butyl titanate, polyglutamic acid is grafted with graphene to obtain a filler, then, under the action of the catalyst, fluoroethylene, 1-octene, hydrogen, ethylene and the like are used as raw materials to carry out polymerization reaction to obtain a resin matrix, and finally, the resin matrix and the filler are melted and blended to obtain the HDPE resin.
Description
Technical Field
The invention relates to the technical field of plastic pipes, in particular to an HDPE pipe and a preparation method thereof.
Background
HDPE (high density polyethylene) is a highly crystalline, non-polar thermoplastic resin. The appearance of the original HDPE is milky white, and the micro-thin section is semitransparent to a certain degree. PE has excellent resistance to most domestic and industrial chemicals. Certain classes of chemicals cause chemical corrosion, such as corrosive oxidants (concentrated nitric acid), aromatic hydrocarbons (xylene) and halogenated hydrocarbons (carbon tetrachloride). The polymers are non-hygroscopic and have good resistance to water vapor and can be used for packaging applications. HDPE has very good electrical properties, especially high dielectric strength, making it very suitable for wire and cable applications. Medium to high molecular weight grades have excellent impact resistance, even at low temperatures of-40F at ambient temperature. The HDPE pipe has excellent mechanical strength and corrosion resistance, light weight, smooth pipe wall, low price and convenient installation, and is widely used for water supply and drainage pipes for buildings, agricultural drainage and irrigation pipes, gas tanks, blow-off pipes and the like at present.
However, the existing HDPE pipe generally has poor toughness (particularly low notched impact strength), and is difficult to meet certain special environmental requirements. In order to improve the toughness of the product, the most common method is to increase the molecular weight and increase the degree of branching, but this leads to poor processability of the HDPE resin, which in turn leads to poor other mechanical properties of the product.
Disclosure of Invention
The invention aims to provide an HDPE (high-density polyethylene) pipe and a preparation method thereof, which aim to solve the technical problem that all indexes of mechanical strength are difficult to take into consideration.
In order to realize the aim, the invention provides a preparation method of an HDPE pipe, firstly, HDPE resin is placed in a polymer pipe rotary extrusion device for melt rotary extrusion, and an extruded pipe blank is cooled and sized under traction, so that the HDPE pipe is obtained; wherein, the HDPE resin is prepared by the following method in parts by weight:
(1) adding 1-2 parts of catalyst, 3-5 parts of n-hexane and 1-2 parts of n-heptane into a polymerization kettle, and raising the temperature of the polymerization kettle to 50-60 ℃;
(2) then introducing 0.1-0.2 part of vinyl fluoride, 0.5-0.8 part of 1-octene, 1-2 parts of hydrogen and 100 parts of ethylene, reacting for 2-3 hours at 80-83 ℃ and 0.5-0.8 MPa, cooling to normal temperature, discharging, and drying to obtain a resin matrix;
(3) finally, melting and blending the resin matrix and the filler to obtain the HDPE resin;
the catalyst is obtained by mixing and reacting vanadium-modified SBA-15 molecular sieve, titanium tetrachloride and butyl titanate; the filler is obtained by grafting polyglutamic acid on graphene.
Preferably, the rotation is any one of independent rotation of the mandrel with respect to the die, independent rotation of the die with respect to the mandrel, simultaneous co-rotation of the mandrel and the die, or simultaneous counter-rotation of the mandrel and the die, and the rotation speed is 18 to 20 rpm/min.
Preferably, the process conditions of the melt-spinning extrusion are as follows: the melting temperature is 200-230 ℃, and the temperature of the mouth mold section is 200-210 ℃.
Preferably, in the step (3), the melt blending temperature is 160 ℃, the blending time is 15 minutes, and the rotating speed of the rotor is 50 r/min.
Preferably, the preparation method of the catalyst comprises the following steps in parts by weight: dispersing 1 part of vanadium-modified SBA-15 molecular sieve in 5-8 parts of n-heptane, uniformly oscillating with ultrasonic waves, cooling to-10-15 ℃, adding 0.1-0.2 part of titanium tetrachloride, stirring and reacting for 2-3 hours, heating to 48-50 ℃, adding 0.15-0.25 part of butyl titanate, reacting for 50-80 minutes, filtering and washing to obtain the catalyst.
Further preferably, the vanadium modified SBA-15 molecular sieve is prepared by the following method in parts by weight: adding 100 parts of SBA-15 molecular sieve into 5-8 parts of vanadium-containing aqueous solution while stirring, carrying out ultrasonic oscillation for 5-10 minutes, carrying out microwave treatment for 3-5 minutes at 500-700W, and finally carrying out heat preservation grinding at 100-105 ℃ until complete drying to obtain the catalyst.
More preferably, the vanadium-containing aqueous solution is selected from any one of ammonium metavanadate, vanadyl sulfate and vanadyl oxalate, and the mass concentration of the vanadium-containing aqueous solution is 20-30%.
Preferably, the titanium tetrachloride is uniformly and slowly dripped, and the dripping time is 50-80 minutes.
Preferably, the preparation method of the filler comprises the following steps in parts by weight: adding 1 part of graphene oxide powder into 5-7 parts of N, N-dimethylformamide, uniformly dispersing by ultrasonic waves, heating to 85-88 ℃, adding 0.5-0.8 part of dicyclohexylcarbodiimide and 0.1-0.2 part of 4-dimethylaminopyridine, adding 0.7-1 part of polyglutamic acid, carrying out heat preservation stirring reaction for 5-6 hours, adding a reducing agent, continuously stirring for 80-100 minutes, filtering while hot, washing for 3-4 times by using absolute ethyl alcohol, drying for 10-12 hours at 70-80 ℃, and grinding and sieving by using a 100-mesh sieve to obtain the graphene oxide powder.
Further preferably, the graphene oxide is prepared by a modified Hummers method.
More preferably, the reducing agent is hydrazine hydrate with the mass concentration of 70-80% in 1-1.2 parts.
The HDPE pipe obtained by the preparation method.
The invention has the following beneficial effects:
according to the invention, the catalyst is prepared by mixing and reacting the vanadium modified SBA-15 molecular sieve, titanium tetrachloride and butyl titanate, the polyglutamic acid is grafted with graphene to obtain the filler, then the polymerization reaction is carried out by taking vinyl fluoride, 1-octene, hydrogen, ethylene and the like as raw materials under the action of the catalyst to obtain the resin matrix, and finally the resin matrix and the filler are melted and blended to obtain the HDPE resin, so that the flexibility of the HDPE resin is greatly improved on the premise of not influencing other mechanical strength indexes, the market vacancy is compensated, and the HDPE resin has a good market prospect.
The improvement of flexibility mainly depends on the following aspects: firstly, 1-octene is introduced into a resin matrix and has a long-chain structure, so that the structure is properly branched and crosslinked, and the improvement of the flexibility of a product is facilitated; secondly, adding hydrogen when preparing the resin matrix, and adjusting the molecular weight of the resin matrix, wherein the larger the molecular weight is, the stronger the entanglement among molecular chains is, and the better the flexibility is; and thirdly, the graphene is introduced into the filler, so that the graphene has good toughness and is beneficial to improving the flexibility of the product, but the compatibility of the graphene and a resin matrix is poor.
The resin matrix is obtained by polymerizing vinyl fluoride, 1-octene, hydrogen, ethylene and the like serving as raw materials, and besides monomer ethylene, vinyl fluoride and 1-octene are introduced for copolymerization, so that on one hand, the introduction of 1-octene enables the product structure to be properly branched and enhances toughness, and on the other hand, the vinyl fluoride brings fluorine which can form hydrogen bond action with filler components, and the compatibility is improved. The addition of proper hydrogen can regulate the molecular weight of the resin matrix and give consideration to the flexibility and other mechanical performance indexes of the product. When the resin matrix is prepared, n-hexane and n-heptane are added as dispersing solvents, so that the catalyst is uniformly dispersed, the catalytic active center is fully exposed, and a better catalytic effect is achieved.
The catalyst is prepared by mixing and reacting vanadium-modified SBA-15 molecular sieve, titanium tetrachloride and butyl titanate, wherein the SBA-15 molecular sieve has a two-dimensional hexagonal through hole structure, is large in specific surface area and uniform in pore diameter distribution, facilitates transportation of reactants in pores, facilitates reaction, and plays a role in catalysis. The SBA-15 molecular sieve is modified by vanadium to bring unfilled d-orbits, titanium is introduced after the SBA-15 molecular sieve is mixed with titanium tetrachloride and butyl titanate for reaction, the unfilled d-orbits exist, electron clouds on the molecular orbits are delocalized, the ethylene structure is symmetrical, polarization is not easy to induce, the activation energy of the polymerization reaction is high, and the polymerization reaction is not easy to occur; in addition, the alkyl in the 1-octene belongs to an electron-donating group, the fluorine in the fluoroethylene belongs to an electron-withdrawing group, the polymerization of cations and anions tends to be realized respectively, and the electron cloud delocalization effect of the catalyst is favorable for enhancing the stability of the intermediate and promoting the formation of the intermediate, so that the polymerization reaction is carried out, and the catalytic effect is enhanced.
The filler is obtained by grafting polyglutamic acid on graphene, the graphene is a hexagonal honeycomb-lattice two-dimensional carbon nano material consisting of carbon atoms, and the graphene has good toughness, but the compatibility of the graphene and a resin matrix is poor. According to the invention, polyglutamic acid grafted graphene is utilized, and a large amount of hydroxyl, imino and the like are introduced, so that hydrogen bonds can be formed with fluorine and the like in a resin matrix, the compatibility is enhanced, and the mechanical properties of the product are improved.
In addition to the objects, features and advantages described above, other objects, features and advantages of the present invention are also provided. The present invention will be described in further detail below.
Detailed Description
The following is a detailed description of embodiments of the invention, but the invention can be implemented in many different ways, as defined and covered by the claims.
Example 1:
the preparation method of the HDPE pipe comprises the steps of firstly, putting HDPE resin into a polymer pipe rotary extrusion device for melt rotary extrusion, and cooling and sizing an extruded pipe blank under traction to obtain the HDPE pipe; wherein, the HDPE resin is prepared by the following method in parts by weight:
(1) firstly, adding 1 part of catalyst, 5 parts of normal hexane and 1 part of normal heptane into a polymerization kettle, and raising the temperature of the polymerization kettle to 60 ℃;
(2) then introducing 0.1 part of vinyl fluoride, 0.8 part of 1-octene, 1 part of hydrogen and 100 parts of ethylene, reacting for 3 hours at 83 ℃ and 0.5MPa, cooling to normal temperature, discharging and drying to obtain a resin matrix;
(3) finally, melting and blending the resin matrix and the filler to obtain the HDPE resin;
the catalyst is obtained by mixing and reacting vanadium-modified SBA-15 molecular sieve, titanium tetrachloride and butyl titanate; the filler is obtained by grafting polyglutamic acid on graphene.
The rotation was carried out using a mandrel rotating independently of the die at a speed of 18 rpm/min.
The technological conditions of the melt rotary extrusion are as follows: the melting temperature is 230 ℃, and the temperature of the die section is 200 ℃.
In the step (3), the melt blending temperature is 160 ℃, the blending time is 15 minutes, and the rotating speed of a rotor is 50 r/min.
The preparation method of the catalyst comprises the following steps of: dispersing 1 part of vanadium modified SBA-15 molecular sieve in 8 parts of n-heptane, uniformly oscillating by ultrasonic waves, cooling to-10 ℃, adding 0.2 part of titanium tetrachloride, stirring for reacting for 2 hours, heating to 50 ℃, adding 0.15 part of butyl titanate, reacting for 80 minutes, filtering and washing to obtain the catalyst.
The vanadium modified SBA-15 molecular sieve is prepared by the following method in parts by weight: adding 100 parts of SBA-15 molecular sieve into 5 parts of vanadium-containing aqueous solution while stirring, oscillating for 10 minutes by ultrasonic waves, processing for 5 minutes by 500W microwaves, and finally grinding at 100 ℃ in a heat preservation manner until the mixture is completely dried to obtain the vanadium-containing aqueous solution.
The vanadium-containing aqueous solution is ammonium metavanadate, and the mass concentration of the ammonium metavanadate is 30%.
The titanium tetrachloride should be uniformly and slowly added dropwise for 50 minutes.
The preparation method of the filler comprises the following steps of: adding 1 part of graphene oxide powder into 7 parts of N, N-dimethylformamide, uniformly dispersing by ultrasonic waves, heating to 85 ℃, adding 0.8 part of dicyclohexylcarbodiimide and 0.1 part of 4-dimethylaminopyridine, adding 1 part of polyglutamic acid, carrying out heat preservation stirring reaction for 5 hours, adding a reducing agent, continuously stirring for 100 minutes, filtering while hot, washing for 3 times by using absolute ethyl alcohol, drying for 10 hours at 80 ℃, grinding and sieving by using a 100-mesh sieve to obtain the graphene oxide.
The graphene oxide is prepared by adopting an improved Hummers method.
The reducing agent is 1.2 parts of hydrazine hydrate with the mass concentration of 70%.
The HDPE pipe obtained by the preparation method.
Example 2:
the preparation method of the HDPE pipe comprises the steps of firstly, putting HDPE resin into a polymer pipe rotary extrusion device for melt rotary extrusion, and cooling and sizing an extruded pipe blank under traction to obtain the HDPE pipe; wherein, the HDPE resin is prepared by the following method in parts by weight:
(1) firstly, adding 2 parts of catalyst, 3 parts of normal hexane and 2 parts of normal heptane into a polymerization kettle, and raising the temperature of the polymerization kettle to 50 ℃;
(2) then introducing 0.2 part of vinyl fluoride, 0.5 part of 1-octene, 2 parts of hydrogen and 100 parts of ethylene, reacting for 2 hours at 80 ℃ and 0.8MPa, cooling to normal temperature, discharging and drying to obtain a resin matrix;
(3) finally, melting and blending the resin matrix and the filler to obtain the HDPE resin;
the catalyst is obtained by mixing and reacting vanadium-modified SBA-15 molecular sieve, titanium tetrachloride and butyl titanate; the filler is obtained by grafting polyglutamic acid on graphene.
The rotation adopts the mode that the core rod and the neck mold rotate in the same direction at the same time, and the rotating speed is 20 rpm/min.
The technological conditions of the melt rotary extrusion are as follows: the melting temperature is 200 ℃, and the die section temperature is 210 ℃.
In the step (3), the melt blending temperature is 160 ℃, the blending time is 15 minutes, and the rotating speed of a rotor is 50 r/min.
The preparation method of the catalyst comprises the following steps of: dispersing 1 part of vanadium modified SBA-15 molecular sieve in 5 parts of n-heptane, uniformly oscillating by ultrasonic waves, cooling to-15 ℃, adding 0.1 part of titanium tetrachloride, stirring for reaction for 3 hours, heating to 48 ℃, adding 0.25 part of butyl titanate, reacting for 50 minutes, filtering and washing to obtain the catalyst.
The vanadium modified SBA-15 molecular sieve is prepared by the following method in parts by weight: adding 100 parts of SBA-15 molecular sieve into 8 parts of vanadium-containing aqueous solution while stirring, oscillating for 5 minutes by ultrasonic waves, treating for 3 minutes by 700W microwaves, and finally grinding at 105 ℃ in a heat preservation manner until the mixture is completely dried to obtain the vanadium-containing aqueous solution.
The vanadium-containing aqueous solution is vanadyl sulfate, and the mass concentration of the vanadyl sulfate is 20%.
The titanium tetrachloride should be uniformly and slowly added dropwise for 80 minutes.
The preparation method of the filler comprises the following steps of: adding 1 part of graphene oxide powder into 5 parts of N, N-dimethylformamide, uniformly dispersing by ultrasonic waves, heating to 88 ℃, adding 0.5 part of dicyclohexylcarbodiimide and 0.2 part of 4-dimethylaminopyridine, adding 0.7 part of polyglutamic acid, carrying out heat preservation and stirring reaction for 6 hours, adding a reducing agent, continuously stirring for 80 minutes, filtering while hot, washing with absolute ethyl alcohol for 4 times, drying at 70 ℃ for 12 hours, and grinding and sieving with a 100-mesh sieve to obtain the graphene oxide.
The graphene oxide is prepared by adopting an improved Hummers method.
The reducing agent is 1 part of hydrazine hydrate with the mass concentration of 80%.
The HDPE pipe obtained by the preparation method.
Example 3:
the preparation method of the HDPE pipe comprises the steps of firstly, putting HDPE resin into a polymer pipe rotary extrusion device for melt rotary extrusion, and cooling and sizing an extruded pipe blank under traction to obtain the HDPE pipe; wherein, the HDPE resin is prepared by the following method in parts by weight:
(1) firstly, adding 1.5 parts of catalyst, 4 parts of normal hexane and 1.5 parts of normal heptane into a polymerization kettle, and raising the temperature of the polymerization kettle to 55 ℃;
(2) then introducing 0.15 part of vinyl fluoride, 0.6 part of 1-octene, 1.5 parts of hydrogen and 100 parts of ethylene, reacting for 2.5 hours at 82 ℃ and 0.7MPa, cooling to normal temperature, discharging and drying to obtain a resin matrix;
(3) finally, melting and blending the resin matrix and the filler to obtain the HDPE resin;
the catalyst is obtained by mixing and reacting vanadium-modified SBA-15 molecular sieve, titanium tetrachloride and butyl titanate; the filler is obtained by grafting polyglutamic acid on graphene.
The core rod and the neck ring mold rotate reversely at the same time in the rotating mode, and the rotating speed is 19 rpm/min.
The technological conditions of the melt rotary extrusion are as follows: the melting temperature was 220 ℃ and the die section temperature was 205 ℃.
In the step (3), the melt blending temperature is 160 ℃, the blending time is 15 minutes, and the rotating speed of a rotor is 50 r/min.
The preparation method of the catalyst comprises the following steps of: dispersing 1 part of vanadium modified SBA-15 molecular sieve in 6 parts of n-heptane, uniformly oscillating by ultrasonic waves, cooling to-12 ℃, adding 0.15 part of titanium tetrachloride, stirring for reaction for 2.5 hours, heating to 49 ℃, adding 0.2 part of butyl titanate, reacting for 70 minutes, filtering and washing to obtain the catalyst.
The vanadium modified SBA-15 molecular sieve is prepared by the following method in parts by weight: adding 100 parts of SBA-15 molecular sieve into 6 parts of vanadium-containing aqueous solution while stirring, oscillating for 8 minutes by ultrasonic waves, processing for 4 minutes by 600W microwaves, and finally grinding at the temperature of 102 ℃ in a heat preservation manner until the mixture is completely dried to obtain the vanadium-containing aqueous solution.
The vanadium-containing aqueous solution is vanadyl oxalate with the mass concentration of 25 percent.
The titanium tetrachloride should be uniformly and slowly added dropwise for 60 minutes.
The preparation method of the filler comprises the following steps of: adding 1 part of graphene oxide powder into 6 parts of N, N-dimethylformamide, uniformly dispersing by ultrasonic waves, heating to 87 ℃, adding 0.6 part of dicyclohexylcarbodiimide and 0.15 part of 4-dimethylaminopyridine, adding 0.8 part of polyglutamic acid, carrying out heat preservation stirring reaction for 5.5 hours, adding a reducing agent, continuously stirring for 90 minutes, filtering while hot, washing with absolute ethyl alcohol for 3 times, drying at 75 ℃ for 11 hours, and grinding and sieving with a 100-mesh sieve to obtain the graphene oxide powder.
The graphene oxide is prepared by adopting an improved Hummers method.
The reducing agent is 1.1 part of hydrazine hydrate with the mass concentration of 75%.
The HDPE pipe obtained by the preparation method.
Comparative example 1
The catalyst is obtained by mixing SBA-15 molecular sieve, titanium tetrachloride and butyl titanate for reaction;
the rest is the same as example 1.
Comparative example 2
The filler is graphene;
the rest is the same as example 1.
Comparative example 3
The filler is ethylenediamine grafted graphene, and ethylenediamine is directly used for replacing polyglutamic acid during preparation.
The rest is the same as example 1.
Comparative example 4
Vinyl fluoride is omitted in the preparation of HDPE resins;
the rest is the same as example 1.
Comparative example 5
1-octene was omitted when making HDPE resin;
the rest is the same as example 1.
Test examples
With reference to GB/T13663-92, the pipe materials (outer diameter is 100mm) obtained in examples 1-3 or comparative examples 1-5 are examined for properties including bending (QB/T2803-.
TABLE 1 Performance test results
As can be seen from Table 1, the pipe obtained in examples 1 to 3 has low bending, high tensile yield stress, low longitudinal shrinkage, no cracking and no leakage in a hydraulic test, and is suitable for use as a pipe for water supply inside and outside buildings (overhead or buried). The catalyst of the comparative example 1 is obtained by mixing and reacting an SBA-15 molecular sieve, titanium tetrachloride and butyl titanate, the filler of the comparative example 2 is graphene, the filler of the comparative example 3 is ethylenediamine grafted graphene, the ethylenediamine is directly used for replacing polyglutamic acid during preparation, the fluoroethylene is omitted during preparation of HDPE resin in the comparative example 4, the 1-octene is omitted during preparation of HDPE resin in the comparative example 5, and all mechanical properties of the product are obviously poor.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The preparation method of the HDPE pipe is characterized in that the HDPE resin is placed in a polymer pipe rotary extrusion device for melt rotary extrusion, and the extruded pipe blank is cooled and sized under traction, so that the HDPE pipe is obtained; wherein, the HDPE resin is prepared by the following method in parts by weight:
(1) adding 1-2 parts of catalyst, 3-5 parts of n-hexane and 1-2 parts of n-heptane into a polymerization kettle, and raising the temperature of the polymerization kettle to 50-60 ℃;
(2) then introducing 0.1-0.2 part of vinyl fluoride, 0.5-0.8 part of 1-octene, 1-2 parts of hydrogen and 100 parts of ethylene, reacting for 2-3 hours at 80-83 ℃ and 0.5-0.8 MPa, cooling to normal temperature, discharging, and drying to obtain a resin matrix;
(3) finally, melting and blending the resin matrix and the filler to obtain the HDPE resin;
the catalyst is obtained by mixing and reacting vanadium-modified SBA-15 molecular sieve, titanium tetrachloride and butyl titanate; the filler is obtained by grafting polyglutamic acid on graphene.
2. The production method according to claim 1, wherein the rotation is 18 to 20rpm/min, and the rotation is any one of independent rotation of the core rod with respect to the die, independent rotation of the die with respect to the core rod, simultaneous co-rotation of the core rod and the die, or simultaneous counter-rotation of the core rod and the die.
3. The preparation method according to claim 1, wherein the process conditions of the melt-spinning extrusion are as follows: the melting temperature is 200-230 ℃, and the temperature of the mouth mold section is 200-210 ℃.
4. The production method according to claim 1, wherein in the step (3), the melt blending temperature is 160 ℃, the blending time is 15 minutes, and the rotation speed of the rotor is 50 r/min.
5. The method of claim 1, wherein the catalyst is prepared by the following steps in parts by weight: dispersing 1 part of vanadium-modified SBA-15 molecular sieve in 5-8 parts of n-heptane, uniformly oscillating with ultrasonic waves, cooling to-10-15 ℃, adding 0.1-0.2 part of titanium tetrachloride, stirring and reacting for 2-3 hours, heating to 48-50 ℃, adding 0.15-0.25 part of butyl titanate, reacting for 50-80 minutes, filtering and washing to obtain the catalyst.
6. The preparation method of claim 5, wherein the vanadium modified SBA-15 molecular sieve is prepared by the following method in parts by weight: adding 100 parts of SBA-15 molecular sieve into 5-8 parts of vanadium-containing aqueous solution while stirring, carrying out ultrasonic oscillation for 5-10 minutes, carrying out microwave treatment for 3-5 minutes at 500-700W, and finally carrying out heat preservation grinding at 100-105 ℃ until complete drying to obtain the catalyst.
7. The method of claim 1, wherein the filler is prepared by the following method in parts by weight: adding 1 part of graphene oxide powder into 5-7 parts of N, N-dimethylformamide, uniformly dispersing by ultrasonic waves, heating to 85-88 ℃, adding 0.5-0.8 part of dicyclohexylcarbodiimide and 0.1-0.2 part of 4-dimethylaminopyridine, adding 0.7-1 part of polyglutamic acid, carrying out heat preservation stirring reaction for 5-6 hours, adding a reducing agent, continuously stirring for 80-100 minutes, filtering while hot, washing for 3-4 times by using absolute ethyl alcohol, drying for 10-12 hours at 70-80 ℃, and grinding and sieving by using a 100-mesh sieve to obtain the graphene oxide powder.
8. An HDPE pipe obtained by the preparation method of any one of claims 1-7.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010643946.5A CN111675848A (en) | 2020-07-07 | 2020-07-07 | HDPE (high-density polyethylene) pipe and preparation method thereof |
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| CN202010643946.5A CN111675848A (en) | 2020-07-07 | 2020-07-07 | HDPE (high-density polyethylene) pipe and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113071086A (en) * | 2021-03-09 | 2021-07-06 | 浙江联景塑胶有限公司 | Antibacterial, anti-aging and high-temperature-resistant PSP steel-plastic composite pipe and preparation method thereof |
-
2020
- 2020-07-07 CN CN202010643946.5A patent/CN111675848A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113071086A (en) * | 2021-03-09 | 2021-07-06 | 浙江联景塑胶有限公司 | Antibacterial, anti-aging and high-temperature-resistant PSP steel-plastic composite pipe and preparation method thereof |
| CN113071086B (en) * | 2021-03-09 | 2022-10-21 | 浙江联景塑胶有限公司 | Antibacterial, anti-aging and high-temperature-resistant PSP steel-plastic composite pipe and preparation method thereof |
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Application publication date: 20200918 |
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