CN111057172A - Octene-modified linear low-density polyethylene resin, multi-layer co-extruded packaging film comprising the same, and preparation method thereof - Google Patents
Octene-modified linear low-density polyethylene resin, multi-layer co-extruded packaging film comprising the same, and preparation method thereof Download PDFInfo
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- CN111057172A CN111057172A CN201811210186.8A CN201811210186A CN111057172A CN 111057172 A CN111057172 A CN 111057172A CN 201811210186 A CN201811210186 A CN 201811210186A CN 111057172 A CN111057172 A CN 111057172A
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- B65D65/38—Packaging materials of special type or form
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Abstract
The invention provides an octene modified linear low-density polyethylene resin, a multilayer co-extrusion packaging film containing the same and a preparation method thereof. The resin density of the octene modified linear low density polyethylene resin is 0.917-0.923 g/cm3The melt index is 0.7-1.3 g/10min, the content of octene units is 1.6-2.0 mol%, and the melt ratio of molecular weight distribution is 2.9-3.1. Because the octene modified linear low-density polyethylene resin has longer side chains and the side chains have the same effect as knotted molecules, the toughness and the shock resistance of the octene modified linear low-density polyethylene resin are greatly improved. Octene LLDPE resins improve to 300% in impact and tear properties for a given resin at the same melt index and density. While the incorporation of octene in linear low density polyethylene is also beneficial in improving its formationThe transparency, shrinkage rate, heat sealing performance and other comprehensive properties of the film.
Description
Technical Field
The invention relates to the field of organic synthesis, in particular to an octene modified linear low-density polyethylene resin, a multilayer co-extrusion packaging film containing the same and a preparation method thereof.
Background
POF is a multilayer co-extruded polyolefin heat shrinkable film, which is prepared by plasticizing and extruding linear low-density polyethylene (LLDPE) serving as an intermediate layer and copolymerized propylene (PP) serving as an inner layer and an outer layer by three extruders, and then carrying out die head molding, film bubble blowing and other special processes. The packaging film is mainly used for packaging products with regular and irregular shapes, and has the characteristics of no toxicity, environmental protection, high transparency, high shrinkage rate, good heat sealing performance, high surface glossiness, good toughness, high tear strength, uniform heat shrinkage, suitability for full-automatic high-speed packaging and the like, and corners of a sealing part are soft after shrink packaging; the heat sealing adhesive has no toxicity, and does not generate toxic gas during heat sealing processing; the coating is thin and tough, uniform in thickness, soft in texture, better in moisture resistance, excellent in cold resistance, not hard in winter, not brittle and not easy to break in transportation. After shrink-wrapping, the tightening force can not change, and the packaged material can not be deformed after being stored for a long time. The product can be widely applied to the products such as automobile articles, plastic products, stationery, books, electronics, circuit boards, MP3, VCD, artware, photo frames and other wooden products, toys, insecticides, daily necessities, food, cosmetics, canned beverages, dairy products, medicines, cassette tapes, video tapes and the like.
POF heat shrinkable films have basically replaced PVC heat shrinkable film packages and become the mainstream product in heat shrinkable packaging materials. The thermal contraction film is designed by adopting a macromolecular chain stretching and orienting principle and is formed by a rapid cooling and shaping method. The physical principle is as follows: when the polymer is in a high elastic state, it is oriented by stretching, then the polymer is quenched to below the glass transition temperature, the molecular orientation is frozen, and when the article is heated in the packaging process, the molecules are restored to the original state due to the relaxation of the stress caused by the molecular motion, and the shrinkage is generated.
Nova chemical company marketed As a series of LLDPE resins produced using a novel Advanced Sclairtech solution process and a specialized catalyst under the trade designation Sclair As TuteFP120The octene LLDPE film-grade high-grade resin produced by a chemical plant with the annual capacity of 37 ten thousand tons in an Eberba tower has 5 marks. These grades all have a resin density of 0.92g/cm3The melt index is 1.0, and the method is mainly used for producing various high-grade films, such as food packaging films, special product packaging films, laminated films, co-extruded films, heavy-duty shipping packaging bags and the like. These grades are described to have excellent dart impact strength, puncture resistance, tear strength, sealing properties, optical properties, etc., while having excellent melt stability, improved processability in blown film, and less gel particles.
At present, no enterprise for producing the special material for the octene copolymer polyethylene POF film exists in China. The octene copolymer polyethylene material is mainly used for producing high-grade heat-packing shrink film materials. The film produced by the copolymer has excellent strength and tear resistance, and the octene copolymer is in great demand on the market.
Aiming at the domestic blank that POF raw materials in the market of heat-shrinkable packaging films all depend on foreign products, in particular octene copolymerized POF resin. The ethylene and 1-octene copolymerized LLDPE heat-shrinkable special resin has excellent dart impact strength, puncture resistance, tearing strength, sealing performance and optical performance, and simultaneously has excellent melt stability, and can be used for producing various high-grade films. The heat shrinkable film packaging material can gradually replace imported products to meet the requirements of downstream users on high-quality special materials, has the remarkable characteristics of high transparency, high shrinkage, good heat sealing performance and the like, and has the advantages and the advantages of a PP film and a PE film, so that the product performance of the heat shrinkable film packaging material is far superior to that of a pure PP film and a pure PE film, and the heat shrinkable film packaging material is widely popularized and used in the international market at present and is an environment-friendly heat shrinkable film packaging material approved by the European and American markets.
Disclosure of Invention
The invention mainly aims to provide an octene modified linear low-density polyethylene resin, a multilayer co-extrusion packaging film containing the same and a preparation method thereof, and aims to solve the problems that the existing packaging film material is poor in transparency, shrinkage rate and heat sealing performance.
To achieve the above object, according to one aspect of the present invention, there is provided a method of manufacturing a semiconductor deviceThe octene-modified linear low density polyethylene resin has a resin density of 0.917 to 0.923g/cm3The melt index is 0.7-1.3 g/10min, the content of octene units is 1.6-2.0 mol%, and the melt ratio of molecular weight distribution is 2.9-3.1.
Further, the raw materials for preparing the octene modified linear low density polyethylene resin comprise 98.4-98.0 mol% of ethylene monomer and 1.6-2.0 mol% of octene monomer in parts by weight.
The application also provides a multilayer co-extrusion packaging film, which comprises a material layer prepared from the octene modified linear low-density polyethylene resin.
The present application also provides a preparation method of the octene-modified linear low density polyethylene resin, which comprises the following steps: under the action of a Ziegler Natta catalyst, ethylene monomer and octene monomer are subjected to copolymerization reaction to obtain octene modified linear low density polyethylene resin.
Further, the reaction temperature of the polymerization reaction is 270-300 ℃, and the reaction pressure is 11-16 MPa.
Further, the preparation method also comprises the following steps: adding an antioxidant into the reaction system of the polymerization reaction.
Further, the antioxidant is selected from 1010 and/or 168.
Further, before adding the antioxidant, the preparation method further comprises the following steps: mixing an organic solvent and an antioxidant to prepare a mixed solution; then adding the mixed solution into a reaction system of polymerization reaction; preferably, the organic solvent is cyclohexane.
Further, the preparation method also comprises the following steps: adding hydrogen into a reaction system of the polymerization reaction; preferably, the adding amount of the hydrogen is 3-5 ppm.
Furthermore, the dosage of the Ziegler Natta catalyst is 16-20 ppm.
By applying the technical scheme of the invention, the octene modified linear low density polyethylene resin has longer side chains, and the side chains have the same effect as knotted molecules, so that the toughness and the shock resistance of the octene modified linear low density polyethylene resin are greatly improved. Octene LLDPE resins improve to 300% in impact and tear properties for a given resin at the same melt index and density. Meanwhile, the octene is doped into the linear low-density polyethylene, so that the comprehensive properties of the film formed by the octene, such as transparency, shrinkage rate, heat sealing property and the like, can be improved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 shows a schematic view of an apparatus for synthesizing an octene-modified linear low density polyethylene resin provided according to an exemplary embodiment of the present invention.
Wherein the figures include the following reference numerals:
10. a copolymerization reactor; 20. a low-boiling column; 30. a high boiling column; 40. a grease tower.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail with reference to examples.
As described in the background art, the existing packaging film materials have problems of being deficient in transparency, shrinkage and heat-sealing property. In order to solve the technical problem, the application provides an octene-modified linear low-density polyethylene resin, wherein the resin density of the octene-modified linear low-density polyethylene resin is 0.917-0.923 g/cm3The melt index is 0.7-1.3 g/10min, the content of octene units is 1.6-2.0 mol%, and the melt ratio of molecular weight distribution is 2.9-3.1.
Because the octene modified linear low-density polyethylene resin has longer side chains and the side chains have the same effect as knotted molecules, the toughness and the shock resistance of the octene modified linear low-density polyethylene resin are greatly improved. Octene LLDPE resins improve to 300% in impact and tear properties for a given resin at the same melt index and density. Meanwhile, the octene is doped into the linear low-density polyethylene, so that the comprehensive properties of the film formed by the octene, such as transparency, shrinkage rate, heat sealing property and the like, can be improved.
In a preferred embodiment, the raw material for preparing the octene modified linear low density polyethylene resin comprises 98.4-98.0 parts by weight of ethylene monomer and 1.6-2.0 parts by weight of octene monomer. The weight ratio of the ethylene monomer to the octene monomer includes, but is not limited to, the above range, and it is advantageously defined within the above range to further improve the overall properties of the octene-modified linear low density polyethylene resin.
For a better understanding of the present application, another aspect of the present application also provides a method for preparing the above-described octene-modified linear low density polyethylene resin, the method comprising: under the action of a Ziegler Natta catalyst, ethylene monomer and octene monomer are subjected to copolymerization reaction to obtain octene modified linear low density polyethylene resin.
The linear low-density polyethylene resin modified by the octenes is prepared by taking the ethylene as the raw material and the octenes as the comonomer. Because the octene modified resin has longer side chains and the side chains have the same effect as knotted molecules, the toughness and the impact resistance of the octene modified resin can be greatly improved. For a given resin at the same melt index and density, the octene-modified linear low density polyethylene resin improves to 300% in impact and tear properties. Meanwhile, the octene is doped into the linear low-density polyethylene, so that the comprehensive properties of the film formed by the octene, such as transparency, shrinkage rate, heat sealing property and the like, can be improved.
In a preferred embodiment, the polymerization temperature is 270-300 deg.C and the reaction pressure is 11-16 MPa. The reaction temperature and reaction pressure of the polymerization reaction include, but are not limited to, the above ranges, and limiting the same to the above ranges is advantageous for further improving the reaction degree of the polymerization reaction, thereby contributing to improvement of the conversion rate of the reaction raw materials and the combination of the impact resistance and toughness of the octene-modified resin.
In a preferred embodiment, the ratio of the number of moles of ethylene to the number of moles of octene is (1.6 to 2.0). The ratio of the number of moles of ethylene to the number of moles of octene includes, but is not limited to, the above range, and it is preferable to limit it to the above range in order to further improve the overall properties of the octene-modified resin.
In a preferred embodiment, the above preparation method further comprises: adding an antioxidant into a reaction system of the polymerization reaction. The antioxidant is added into a reaction system of the polymerization reaction, so that the aging resistance of the octene modified resin is improved, and the service life of the octene modified resin is prolonged.
In the above polymerization, antioxidants commonly used in the art can be used. To further improve the aging resistance of the octene modified resin, preferably, antioxidants include, but are not limited to 1010 and/or 168.
More preferably, the above preparation method further comprises, before adding the antioxidant: mixing an organic solvent and an antioxidant to prepare a mixed solution; then adding the mixed solution into a reaction system of the polymerization reaction. The antioxidant was diluted with cyclohexane and added to the reaction system. When an antioxidant is added in the preparation process, the obtained octene modified linear low density polyethylene resin also contains the antioxidant, which is beneficial to improving the oxidation resistance and prolonging the service life. Preferably, the organic solvent is cyclohexane.
In a preferred embodiment, the above preparation method further comprises: hydrogen is added to the reaction system of the polymerization reaction. The addition of hydrogen in the polymerization reaction system is favorable for adjusting the melt index of the octene modified linear polyethylene, and is further favorable for improving the comprehensive performance of the octene modified linear polyethylene. More preferably, the amount of hydrogen added is 3 to 5 ppm.
In the polymerization reaction process, the addition of the Ziegler Natta catalyst is beneficial to improving the reaction activity of reaction raw materials and further is beneficial to shortening the reaction time. In a preferred embodiment, the Ziegler Natta catalyst is used in an amount of 16 to 20 ppm.
Another aspect of the present application also provides a multilayer co-extruded packaging film comprising a material layer made of the above octene-modified linear low density polyethylene resin.
Because the octene modified linear low-density polyethylene resin has longer side chains and the side chains have the same effect as knotted molecules, the toughness and the shock resistance of the octene modified linear low-density polyethylene resin are greatly improved. Octene LLDPE resins improve to 300% in impact and tear properties for a given resin at the same melt index and density. Meanwhile, the octene is doped into the linear low-density polyethylene, so that the comprehensive properties of the film formed by the octene, such as transparency, shrinkage rate, heat sealing property and the like, can be improved. Therefore, the multilayer co-extrusion packaging film containing the material layer prepared from the octene modified linear low density polyethylene resin has excellent strength, tear resistance and heat sealability.
The present application is described in further detail below with reference to specific examples, which should not be construed as limiting the scope of the invention as claimed.
Example 1
An octene-modified linear low density polyethylene resin was synthesized using an apparatus as shown in FIG. 1.
The specific synthesis method comprises the following steps:
taking ethylene as a raw material (with the feeding speed of 8t/h) and octene as a comonomer (with the feeding speed of 0.88t/h), and carrying out polymerization reaction in a copolymerization reactor 10 to obtain a polymerization product; wherein in the polymerization reaction process, the average reaction temperature is 237 ℃, the system pressure is 10MPA, and the total conversion rate is 94%. And after 40min of adding octene, testing the resin density and melt index by contacting an analysis station, and further adjusting the reaction according to the values provided by the analysis (the operation index, the finished product index and the target value are shown in table 1). Antioxidant (1010) and hydrogen were added at the beginning of the reaction in the amounts of 1000ppm and 5ppm in that order.
The polymerization product (with the feed rate of 8.3t/h) and the octene (with the feed rate of 8t/h) are conveyed to a low-boiling tower 20 for isomerization reaction to obtain an isomerization product system (two systems); the pressure at the top of the low-boiling tower is 17-18 kg/cm3, the temperature at the top of the tower is 95-100 ℃, and the temperature at the bottom of the tower is 225-229 ℃.
The above-mentioned isomerization product system in which the flow rates of octene-1 and octene-2 were 7.84t/h and 0.16t/h in this order was fed to a high boiling column 30 to separate the isomerization product from the solvent, and the isomerization product was discharged from the bottom of the column to be dissolvedThe agent is discharged from the top of the tower; the overhead pressure of the high-boiling column was 6.8kg/cm3The temperature at the top of the column was 180 ℃ and the temperature at the bottom of the column was 220 ℃.
Conveying the isomerization product to a grease tower 40 for separation to obtain octene modified linear low density polyethylene resin; the pressure at the top of the grease tower is 3.40-3.8 kg/cm3The temperature at the top of the tower is 180-190 ℃, and the temperature at the bottom of the tower is 190-210 ℃.
The multilayer co-extruded POF material (FX120) is prepared from the octene modified linear low density polyethylene resin. The POF material is mainly prepared by taking linear PE and random copolymerization PP as main materials, namely the middle layer is LLDPE (the product) which is a special material for octene-1 copolymerization, the heat sealing layer is ethylene and propylene random polymerization PP, and the POF material is prepared by blow molding extrusion.
Example 2
Taking ethylene as a raw material (with the feeding speed of 8t/h) and octene as a comonomer (with the feeding speed of 0.88t/h), and carrying out polymerization reaction in a copolymerization reactor 10 to obtain a polymerization product; wherein in the polymerization reaction process, the average reaction temperature is 280 ℃, the system pressure is 12MPA, and the total conversion rate is 94%. And after 40min of adding octene, testing the resin density and melt index by contacting an analysis station, and further adjusting the reaction according to the values provided by the analysis (the operation index, the finished product index and the target value are shown in table 1). Antioxidant (1010) and hydrogen were added at the beginning of the reaction in the amounts of 1000ppm and 5ppm in that order.
Example 3
Taking ethylene as a raw material (with the feeding speed of 8t/h) and octene as a comonomer (with the feeding speed of 0.88t/h), and carrying out polymerization reaction in a copolymerization reactor 10 to obtain a polymerization product; wherein in the polymerization reaction process, the average reaction temperature is 237 ℃, the system pressure is 10MPA, and the total conversion rate is 94%. And after 40min of adding octene, testing the resin density and melt index by contacting an analysis station, and further adjusting the reaction according to the values provided by the analysis (the operation index, the finished product index and the target value are shown in table 1). Antioxidant (168) and hydrogen were added at the beginning of the reaction in an amount of 1000ppm, 5ppm in that order.
Example 4
Taking ethylene as a raw material (with the feeding speed of 8t/h) and octene as a comonomer (with the feeding speed of 0.1t/h), and carrying out polymerization reaction in a copolymerization reactor 10 to obtain a polymerization product; wherein in the polymerization reaction process, the average reaction temperature is 237 ℃, the system pressure is 10MPA, and the total conversion rate is 94%. And after 40min of adding octene, testing the resin density and melt index by contacting an analysis station, and further adjusting the reaction according to the values provided by the analysis (the operation index, the finished product index and the target value are shown in table 1). Antioxidant (1010) and hydrogen were added at the beginning of the reaction in the amounts of 1000ppm and 5ppm in that order.
Example 5
Taking ethylene as a raw material (with the feeding speed of 8t/h) and octene as a comonomer (with the feeding speed of 0.88t/h), and carrying out polymerization reaction in a copolymerization reactor 10 to obtain a polymerization product; wherein in the polymerization reaction process, the average reaction temperature is 237 ℃, the system pressure is 10MPA, and the total conversion rate is 94%. And after 40min of adding octene, testing the resin density and melt index by contacting an analysis station, and further adjusting the reaction according to the values provided by the analysis (the operation index, the finished product index and the target value are shown in table 1). Antioxidant (1010) and hydrogen were added at the beginning of the reaction in an amount of 1000ppm, 2ppm in that order.
TABLE 1
And (3) performance testing:
the products obtained in examples 1 to 5 and comparative example 1 (existing product, Dow 2045G) were subjected to performance tests, the results of which are as follows:
(1) molecular weight and GPC distribution.
The molecular weight and distribution test results of examples 1 to 5 and comparative example 1 are shown in Table 2, using ASTM D6474 gel permeation chromatography.
TABLE 2
| Sample (I) | Weight average molecular weight Mw | Number average molecular weight Mn | Molecular weight distribution PD |
| COMPARATIVE EXAMPLE 1 (US 2045G Dow) | 15.7 | 3.8 | 4.1 |
| Example 1(FX120) | 13.7 | 3.4 | 4.1 |
| Example 2 | 14.0 | 3.3 | 4.2 |
| Example 3 | 13.6 | 3.3 | 4.1 |
| Example 4 | 15.4 | 3.5 | 4.4 |
| Example 5 | 12.8 | 3.7 | 3.5 |
(2) And testing the basic performance of the POF material.
The test methods are described in GB/T3682, and the melt index and melt flow ratio in examples 1 to 5 and comparative example 1 are shown in Table 3.
TABLE 3
(3) DSC analysis of POF material.
The test method is shown in GB/T19466.6-2009, and the thermal performance test results of examples 1-5 and comparative examples are shown in Table 4.
TABLE 4
(4) Mechanical properties of the POF material.
The test method is shown in GB/T1042.2-2006, and the mechanical property test results of examples 1-5 and comparative examples are shown in Table 5.
TABLE 5
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
comparing examples 1 to 5 with comparative example 1, it can be seen that the POF material prepared from the octene-modified low-density linear polyethylene prepared by the preparation method provided by the application has higher elasticity and tensile property.
Comparing examples 1 and 2, it is known that limiting the average reaction temperature and pressure of the polymerization reaction to the preferred ranges herein is advantageous for improving the overall properties of the POF material.
Comparing examples 1, 4 and 5, it is found that limiting the feeding ratio of ethylene to octene and the amount of hydrogen added to the preferred ranges of the present application is advantageous for improving the overall performance of the POF material.
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 (10)
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| CN115947898A (en) * | 2021-10-09 | 2023-04-11 | 中国石油天然气股份有限公司 | A kind of coating grade low-density polyethylene and its preparation method and application |
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Application publication date: 20200424 |