CN115926034A - Preparation method of high-strength waterproof polyethylene film - Google Patents
Preparation method of high-strength waterproof polyethylene film Download PDFInfo
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- CN115926034A CN115926034A CN202211498991.1A CN202211498991A CN115926034A CN 115926034 A CN115926034 A CN 115926034A CN 202211498991 A CN202211498991 A CN 202211498991A CN 115926034 A CN115926034 A CN 115926034A
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- ethylene
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- hexene
- octene
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- 239000004698 Polyethylene Substances 0.000 title claims abstract description 24
- -1 polyethylene Polymers 0.000 title claims abstract description 24
- 229920000573 polyethylene Polymers 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000005977 Ethylene Substances 0.000 claims abstract description 41
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 37
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000001257 hydrogen Substances 0.000 claims abstract description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 15
- 239000012968 metallocene catalyst Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 11
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000005303 weighing Methods 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000000498 cooling water Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 229920000642 polymer Polymers 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 6
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 230000001276 controlling effect Effects 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000004078 waterproofing Methods 0.000 claims 1
- 229920005989 resin Polymers 0.000 abstract description 8
- 239000011347 resin Substances 0.000 abstract description 8
- 229920013716 polyethylene resin Polymers 0.000 abstract description 7
- 238000012545 processing Methods 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 238000007334 copolymerization reaction Methods 0.000 abstract description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 abstract 1
- 230000008901 benefit Effects 0.000 description 3
- 238000012512 characterization method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000006353 environmental stress Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 229920006027 ternary co-polymer Polymers 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Abstract
The invention discloses a preparation method of a high-strength waterproof polyethylene film, which comprises the following steps: under the catalysis of metallocene catalyst, the concentration of ethylene and hydrogen, the concentration of octene-1 and the concentration ratio of hexene-1 to ethylene are adjusted in the ternary copolymerization reaction of ethylene and hexene-1/octene-1 slurry, different polymerization process conditions are established, the rapid and stable regulation and control of polymerization reaction and product indexes are realized, the technical performance of the prepared polyethylene product is closer to the performance index of waterproof coiled material resin of imported factories, and the flow rate of the polyethylene resin melt is higher, which shows that the processing performance is better, and can provide theoretical technical basis for the industrial production of high-strength waterproof polyethylene film.
Description
Technical Field
The invention relates to a preparation method of a polyethylene film, in particular to a preparation method of a high-strength waterproof polyethylene film, belonging to the field of petrochemical industry.
Background
The high-strength waterproof membrane can be bonded with concrete under a certain condition, can be maximally sealed with a main body structure, has the advantages of good waterproof effect, convenience in construction, outstanding impact resistance and the like, is suitable for various waterproof fields of industrial and civil buildings, rail transit, underground excavated tunnels and the like, has very strict requirements on the puncture resistance strength of industrial-grade waterproof membranes in national standards, and can be produced by a few manufacturers meeting related technical indexes.
At present, the market demand of the special resin in China is more than 20 million tons, the annual consumption of typical users such as Kelun corporation of Jiangsu is about 2 million tons, no special resin capable of meeting the requirements exists at present, downstream manufacturers need to blend other types of resin for production, but the problems of low melt flow rate of main resin, large fluctuation of processing performance, poor batch quality stability of coiled materials, thicker sheets, higher cost and the like exist, the using effect can not reach the expectation all the time, the requirements of the manufacturers on the high-quality special resin are very urgent, and if the development of the waterproof polyethylene film is successful, the waterproof polyethylene film has better economic benefit prospect.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the preparation method of the high-strength waterproof polyethylene film, which has the technical characteristics that the flow rate of the polyethylene resin melt is higher, the processability is better, a theoretical technical basis can be provided for the industrial production of the high-strength waterproof polyethylene film, and the like.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of a high-strength waterproof polyethylene film comprises the following steps: under the catalysis of metallocene catalyst, the concentration of ethylene and hydrogen, the concentration of octene-1 and the concentration ratio of hexene-1 to ethylene are regulated in the ternary polymerization reaction of ethylene and hexene-1/octene-1 slurry, and different polymerization conditions are established to realize the fast and stable regulation of polymerization reaction and product index.
Preferably, the specific steps are as follows: on a 2L-scale intermittent polymerization device, respectively pressurizing the system to 0.5MPa and 1.0MPa by using nitrogen for air tightness, and after ensuring that the system has no leakage, replacing the system by using nitrogen firstly and then replacing the system by using ethylene for 3 times;
controlling the system pressure after replacement at a set pressure, heating the high-pressure polymerization kettle to a set temperature of 80 ℃, and adding quantitative hexane, ethylene, hexene-1, octene-1 and hydrogen into the high-pressure polymerization kettle in sequence under slow stirring;
stirring and premixing for 3min, quickly adding a supported metallocene catalyst, quickly increasing the rotating speed to react for 2 hours, cooling, taking out solid polyethylene powder and weighing.
Preferably, on a 2L-scale batch polymerization device, the pressure control range of a polymerization reaction kettle is 1.0MPa, the temperature of the reaction kettle is controlled at 80 ℃, the nitrogen concentration control range is 30-45%, the ethylene concentration control range is 50-60%, the hydrogen concentration control range is 150-200 ppm, the octene-1 concentration control range is 1-5%, the hexene-1/ethylene concentration ratio control range is 0.005-0.008, and acidified ethanol with the mass fraction of 10% is added to terminate the reaction after the reaction is carried out for 2 hours; cooling with cooling water and releasing the pressure of the high-pressure kettle to normal pressure; adding 500ml of acidified ethanol solution to precipitate a polymer, carrying out suction filtration, drying, carrying out vacuum drying at 70 ℃ for 6 hours, and weighing the obtained product.
Has the advantages that: the technical performance of the prepared polyethylene product is closer to the performance index of the waterproof coiled material resin of an imported factory, and the melt flow rate of the polyethylene resin is higher, so that the processing performance of the polyethylene resin is better, and a theoretical technical basis can be provided for the industrial production of the high-strength waterproof polyethylene film.
Detailed Description
The present invention will be further described with reference to the following examples, but the present invention is not limited to the following examples.
The technical content of the application is as follows: in the reaction of ethylene and hexene-1/octene-1 slurry ternary copolymerization catalyzed by metallocene catalyst, the concentration of ethylene and hydrogen, the concentration of octene-1 and the concentration ratio of hexene-1 to ethylene are adjusted, different polymerization process conditions are established, and the rapid and stable regulation and control of polymerization reaction and product index are realized.
Evaluation of polymerization: on a 2L-scale intermittent polymerization device, respectively pressurizing the system to 0.5MPa and 1.0MPa by using nitrogen for air tightness, and after ensuring that the system has no leakage, replacing the system by using nitrogen firstly and then replacing the system by using ethylene for 3 times; controlling the system pressure after replacement at a set pressure, heating the high-pressure polymerization kettle to a set temperature of 80 ℃, and adding quantitative hexane, ethylene, hexene-1, octene-1 and hydrogen into the high-pressure polymerization kettle in sequence under slow stirring; stirring and premixing for 3min, quickly adding a supported metallocene catalyst, quickly increasing the rotating speed to react for 2 h, cooling, taking out solid polyethylene powder and weighing.
On a 2L-scale intermittent polymerization device, adding acidified ethanol with the mass fraction of 10% to terminate the reaction after reacting for 2 hours, wherein the pressure control range of a polymerization reaction kettle is 1.0MPa, the temperature of the reaction kettle is 80 ℃, the nitrogen concentration control range is 30-45%, the ethylene concentration control range is 50-60%, the hydrogen concentration control range is 150-200 ppm, the octene-1 concentration control range is 1-5%, and the hexene-1/ethylene concentration ratio control range is 0.005-0.008; cooling with cooling water and releasing the pressure of the high-pressure kettle to normal pressure; adding 500ml of acidified ethanol solution to precipitate out a polymer, carrying out suction filtration, drying, carrying out vacuum drying at 70 ℃ for 6 hours, and weighing the obtained product.
Polymerization evaluation procedure and results:
the performance of the obtained polymer resin is tested and the structure is analyzed by the coordinated regulation and control of polymerization process parameters such as ethylene and hydrogen concentration, ethylene/hexene-1 concentration ratio and the like.
The first scheme is as follows: the metallocene catalyst catalyzes ethylene and hexene-1/octene-1 slurry ternary polymerization, control hydrogen, octene-1, hexene-1/ethylene concentration addition constant, ethylene concentration is added into polymerization reactor according to 50%, 55%, 60%, 65% proportion separately in order; after reacting for 2 hours, adding acidified ethanol with the mass fraction of 10 percent to terminate the reaction; cooling with cooling water and releasing the pressure of the high-pressure kettle to normal pressure; adding 500ml of acidified ethanol solution to precipitate out a polymer, carrying out suction filtration, drying, carrying out vacuum drying at 70 ℃ for 6 hours, and weighing the obtained product.
Scheme II: the metallocene catalyst catalyzes ethylene and hexene-1/octene-1 slurry ternary polymerization, control ethylene concentration, octene-1, hexene-1/ethylene concentration ratio addition constant, the hydrogen concentration is added into polymerization reactor according to 150ppm, 160ppm, 170ppm, 180ppm, 190ppm, 200ppm respectively in order; after reacting for 2 hours, adding acidified ethanol with the mass fraction of 10 percent to terminate the reaction; cooling with cooling water and releasing the pressure of the high-pressure kettle to normal pressure; adding 500ml of acidified ethanol solution to precipitate out a polymer, carrying out suction filtration, drying, carrying out vacuum drying at 70 ℃ for 6 hours, and weighing the obtained product.
The third scheme is as follows: the metallocene catalyst catalyzes ethylene and hexene-1/octene-1 slurry ternary polymerization reaction to control ethylene concentration, octene-1, hydrogen concentration to be invariable, the hexene-1/ethylene concentration ratio is added into a polymerization reactor according to 0.008, 0.007, 0.006, 0.005 respectively in turn; after reacting for 2 hours, adding acidified ethanol with the mass fraction of 10 percent to terminate the reaction; cooling with cooling water and releasing the pressure of the high-pressure kettle to normal pressure; adding 500ml of acidified ethanol solution to precipitate out a polymer, carrying out suction filtration, drying, carrying out vacuum drying at 70 ℃ for 6 hours, and weighing the obtained product.
And the scheme is as follows: the metallocene catalyst catalyzes ethylene and hexene-1/octene-1 slurry ternary polymerization reaction to control ethylene concentration, hydrogen concentration, hexene-1/ethylene concentration ratio is invariable, octene-1 concentration is added into the polymerization reactor according to 1%, 2%, 3%, 4%, 5% respectively in turn; after reacting for 2 hours, adding acidified ethanol with the mass fraction of 10 percent to terminate the reaction; cooling with cooling water and releasing the pressure in the high-pressure kettle to normal pressure; adding 500ml of acidified ethanol solution to precipitate out a polymer, carrying out suction filtration, drying, carrying out vacuum drying at 70 ℃ for 6 hours, and weighing the obtained product.
Under the synergistic regulation and control of the four different process parameters, the metallocene catalyst is used for catalyzing ethylene and hexene-1/octene-1 slurry ternary copolymer products to carry out performance test and structural characterization, and the following table is shown:
polyethylene product performance test and structure characterization results
Imported sample 1 was Dow chemical 5538G and imported sample 2 was EXXON corporation 4009MC.
The technical performance of the polyethylene product obtained by testing is closer to the performance index of the waterproof coiled material resin of an imported factory, and the flow rate of the polyethylene resin melt is higher, which shows that the polyethylene resin melt has better processing performance, and can provide theoretical technical basis for the industrial production of the high-strength waterproof polyethylene film. In the slurry ternary polymerization of ethylene and hexene-1/octene-1, the added comonomer octene-1 can effectively improve the extensibility, tensile property, impact strength and environmental stress crack resistance of polyethylene resin melt, and the mechanical processing property, heat resistance, flexibility, transparency and the like of polyethylene; and compared with slurry copolymerization of ethylene and hexene-1, the method can reduce the consumption of the comonomer under the condition of obtaining products with the same density, and is favorable for saving the cost.
Finally, it should be noted that the present invention is not limited to the above embodiments, and many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (3)
1. A preparation method of a high-strength waterproof polyethylene film is characterized by comprising the following steps: under the catalysis of metallocene catalyst, the concentration of ethylene and hydrogen, the concentration of octene-1 and the concentration ratio of hexene-1 to ethylene are regulated in the ternary polymerization reaction of ethylene and hexene-1/octene-1 slurry, and different polymerization conditions are established to realize the fast and stable regulation of polymerization reaction and product index.
2. The preparation method of the high-strength waterproof polyethylene film according to claim 1, which is characterized by comprising the following steps: on a 2L-scale intermittent polymerization device, respectively pressurizing the system to 0.5MPa and 1.0MPa by using nitrogen for air tightness, and after ensuring that the system has no leakage, replacing the system by using nitrogen firstly and then replacing the system by using ethylene for 3 times;
controlling the system pressure after replacement at a set pressure, heating the high-pressure polymerization kettle to a set temperature of 80 ℃, and adding quantitative hexane, ethylene, hexene-1, octene-1 and hydrogen into the high-pressure polymerization kettle in sequence under slow stirring;
stirring and premixing for 3min, quickly adding a supported metallocene catalyst, quickly increasing the rotating speed to react for 2 h, cooling, taking out solid polyethylene powder and weighing.
3. The method for preparing a high-strength polyethylene film for waterproofing according to claim 1 or 2, characterized in that: on a 2L-scale intermittent polymerization device, adding acidified ethanol with the mass fraction of 10% to terminate the reaction after reacting for 2 hours, wherein the pressure control range of a polymerization reaction kettle is 1.0MPa, the temperature of the reaction kettle is 80 ℃, the nitrogen concentration control range is 30-45%, the ethylene concentration control range is 50-60%, the hydrogen concentration control range is 150-200 ppm, the octene-1 concentration control range is 1-5%, and the hexene-1/ethylene concentration ratio control range is 0.005-0.008; cooling with cooling water and releasing the pressure of the high-pressure kettle to normal pressure; adding 500ml of acidified ethanol solution to precipitate out a polymer, carrying out suction filtration, drying, carrying out vacuum drying at 70 ℃ for 6 hours, and weighing the obtained product.
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| CN202211498991.1A CN115926034A (en) | 2022-11-28 | 2022-11-28 | Preparation method of high-strength waterproof polyethylene film |
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