Composition based on crystalline polypropylene copolymer, sheets and plates, film, layered material

 

(57) Abstract:

Describes a composition based on crystalline polypropylene copolymer comprising a copolymer of propylene with ethylene and a copolymer of propylene with ethylene and C4-C8- alpha-olefin, characterized in that as a copolymer of propylene with ethylene, it contains a copolymer with ethylene content of 1-5 wt.%, and as a copolymer of propylene with ethylene and C4-C8- alpha-olefin - copolymer with ethylene content of 1-5 wt.% and C4-C8-alpha-olefin 6-15 wt.% in the following ratio, wt. %: copolymer of propylene with ethylene 20-60, a copolymer of propylene with ethylene and C4-C8- alpha-olefin 40-80 when the total content of ethylene in the composition of 1-5 wt.% and C4-C8- alpha-olefin 2,4-12.0 wt. %. Describes sheets and plates , as well as layered material. The technical result is an increase in adhesion to printing inks and improved performance. 4 C. and 5 C.p. f-crystals, 1 table.

The present invention relates to compositions based on crystalline propylene polymer suitable for the production of films, sheets and laminates, amenable to welding and printing ink, and the way the floor is Variani crystalline copolymers of propylene with other olefins (mainly ethylene, 1-butene, or both), or mixtures of such copolymers with other polyolefins. These crystalline copolymers produced by polymerization of propylene with small amounts of other olefinic comonomers in the presence of coordination catalysts. In the finished copolymer chains of polymerized comonomers are distributed statistically, and the melting point of the obtained copolymer is lower than crystalline homopolymer propylene. However, the presence of units of comonomers adversely affect the crystalline structure of the polymer, resulting in a relatively high content of the polymer fraction soluble at room temperature (25oC) in cold xylene. In turn, this negatively affects the mechanical properties of the polymer. When it is used to produce multilayer films and layered materials by coextrusion, for example, with crystal homopolymer propylene, weld strength can be poor due to incompatibility with polypropylene layer. In addition, the presence of a relatively large number of substances soluble in xylene, is the reason that the polymer readily reacts with organic substances, making it the disadvantages cannot be overcome by the application of the mixtures mentioned crystalline propylene copolymers or their mixtures with other olefin polymers, because the ability to weld due to the nature and proportions of crystalline and fractions, soluble at room temperature in xylene, and possibly with the distribution of the fractions in the polymer.

In addition, achieving a homogeneous distribution of components by mechanical mixing of melts in comparison with the formation of the mixture in the polymerization process is more energy intensive and lengthy process, not least because of the need to melt extruding and granulating the finished polymer. In addition, the mechanical mixing of melts creates a thermal background of the composition, as evidenced by some decomposition. This can be avoided by obtaining a polymer composition in the polymerization process.

In the published application for the European patent 483523 described compositions obtained directly in polymerization process and having a low initial temperature welding, as well as a low content of fraction soluble at room temperature in xylene or at the 50oC in n-hexane. These compositions contain (wt.%):

A) 30-65% of a copolymer of about 80 to 98% propylene with C4-C8-olefin;

B) 35-70% of a copolymer of propylene with ethylene and perhaps with 1-10% C4-C80,5-5%, if any.

However, as will be shown hereinafter in the examples, the composition has low adhesion to the printing ink even after intensive treatment of a surface designated for printing. For example, for processing the film surface by corona discharge to achieve some degree of adhesion to the printing ink must be the voltage at which the film holes and increases the initial temperature welding.

Adhesion to the printing ink is an important property of the welded polyolefin compositions, because they are often used as the two outer layers in the production of multilayer films for packaging and in many cases, in particular for food packaging, this film should be printed.

The aim of the present invention is to solve these problems by developing composition containing a copolymer of propylene with ethylene and a copolymer of propylene with ethylene and C4-C8-olefin, in which the content of ethylene and C4-C8-olefin is within such limits, in which the composition has not only a low initial temperature welding and contains a small amount of the fraction soluble at 504
-C8-olefin, as the amount of C4-8-olefins required for low temperature welding, so great that the adhesion of these materials to the printing ink is difficult to achieve. This is true for compositions on the application for a European patent 483523. On the other hand, if you apply only the copolymers of propylene/ethylene or triple polymers of propylene/ethylene/C4-C8- -olefin, there are the above-described difficulties.

Composition based on crystalline copolymers of propylene according to the present invention contains (wt.%):

A) 20-60%, preferably 30-50%, of a copolymer of propylene with ethylene, containing 1-5%, mainly 2-4%, of ethylene;

B) 40-80%, preferably 50-70%, of a copolymer of propylene with ethylene and C4-C8-olefin, the ethylene content in it 1-5%, preferably 2-4%, C4-C8- olefin 6-15%, preferably 7-12%; the total content of ethylene in the composition of 1-5%, preferably 2-4%, the total content of C4-C8-olefin composition of 2.4 to 12%, preferably 3.5 to 8.4 per cent.

As C4-C8the olefin preferably using 1-butene, 1-penten and 1-octene. Most preferred is 1-butene.

As shown above composition, needs a small modification to the surface. For example, when the surface treatment by corona discharge voltage, creating a corona discharge sufficient to achieve a given value of the adhesion to the printing ink is lower than the voltage required for the composition in accordance with the application for the European patent 483523 even if the printing is applied a few days after surface modification.

Moreover, the composition of the present invention has the following advantages: the melting point of 126oC to 147oC, the initial temperature of the weld (as defined below) from the 90oC to 144oC and the mass content of the fraction soluble at 50oC in n-hexane, less than 5.5%.

"Initial temperature welding or NTS (used as the sealing temperature is the minimum temperature required to obtain a weld of one layer polypropylene film with one layer of a film obtained from the composition of the present invention, in which the seam is not broken, i.e. the film is not separated in welding, if the multilayer film to attach a weight of 200 g of the Details given in the examples.

The composition of this izobretatelstvo Ziegler-Natta. The main component of this catalyst is a solid catalyst component containing compound of titanium with at least one communication titanium-halogen, and an electron-donating compound. Both compounds put on a magnesium halide in active form. Another important component is alyuminiiorganicheskikh connection, as, for example, alkylamino connection.

Used in the method of the present invention the catalysts allow to obtain polypropylene with a measure of stereoregularity above 90%, preferably above 95%. Catalysts of this nature are well known in the patent literature.

The biggest advantages are the catalysts described in U.S. patent 4339054 and in the European patent 45977. Other examples of catalysts are described in U.S. patents 4472524 and 4473660.

Solid catalyst components used in these catalysts contain as electron donor compounds from the group consisting of ethers, ketones, lactones, compounds containing N atoms, P and/or S, and esters of mono - and dicarboxylic acids.

As the electron donors are particularly suitable esters of phthalic acid such as Diisobutyl, dioctyl-, definitively; alkyl-, cycloalkyl and arylmaleimides; alkyl and arylcarbamoyl, such as Diisobutylene, ethylvinylbenzene; and esters of succinic acid, such as mono - and diethylamine.

Other suitable electron donors are simple 1,3-diesters of the formula:

< / BR>
where RIand RIIdenote identical or different radicals: C1-18alkyl, C3-18cycloalkyl or C7-18aryl; RIIIand RIVdenote identical or different radicals: C1-4alkyl.

Ethers of this type are described in published application for the European patent 361493, corresponding to U.S. patent 5095153.

Typical examples mentioned diapiric compounds are: 2-methyl-2-isopropyl-1,3-dimethoxypropane, 2,2-Diisobutyl-1,3-dimethoxypropane, 2-isopropyl-2-cyclopentyl-1,3-dimethoxypropane, 2-isopropyl-2-isoamyl-1,3-dimethoxypropane.

The above-mentioned components of the catalyst can be prepared in several ways.

For example, the halide of magnesium (in anhydrous form, containing less than 1% water), a compound of titanium and electron-donating compound can carefully grind in terms of activating the magnesium halide. The mixture is then treated one or more times with an excess of TiCl

According to another method, the anhydrous magnesium halide pre-activate one of the known methods and then act on it by excess TiCl4containing dissolved therein electron-donor compound, at a temperature of 80-135oC. Processing TiCl4I repeat, after which hexane or other hydrocarbon solvents are washed solid fraction in order to remove traces of unreacted TiCl4.

Another way adduct MgCl2nROH (in particular, in the form of spheroidal particles), where n is generally from 1 to 3 and ROH is ethanol, butanol or Isobutanol, interacts with the excess TiCl4containing dissolved therein electron-donating compound. Temperature range from 80 to 120oC. Then separated from the solid fraction and again affected by excess TiCl4, then washed aliquot doses of hydrocarbon until then, until you disappear all chlorine ions.

According to another method, magnesium alcoholate and chloralkali (in particular, chloralkali received in accordance with the method described in U.S. patent 4220554) react with excess TiCl4containing in solution electronie titanium, expressed as TiCl4as a rule, present in an amount of from 0.5 to 10 wt.%. The content of the electron-donating compound, which remains bound to the solid catalytic component, mainly, is usually from 5 to 20 mol.% in relation to dihalide magnesium.

Titanium compounds which can be used for preparation of solid catalyst components, it halides and galogenangidridy titanium. The most preferred titanium tetrachloride.

Satisfactory results can also be obtained by using trialodine of titanium compounds, especially TiCl3HR, TiCl3ARA and using galogenarenov such as TiCl3OR, where R is the phenyl radical.

In the above reaction produces magnesium halide in active form. In the literature there are other reactions which forms a magnesium halide in active form from compounds of magnesium, not being halides, e.g., carboxylates of magnesium.

The active form of the magnesium halide in the solid catalytic components can be installed on the ground that the x-ray spectrum of the component instead of the reflection with maximum intensity characteristic neaktivirovannye relatively high non-activated dihalide magnesium or on the basis of that reflection with maximum intensity has a width at half height of at least 30% more than Deaktivierung halide of magnesium. The most active forms are those in which x-ray spectrum of the solid catalytic component appears above the halo.

Among Gulidov preferred magnesium is magnesium chloride. When the highest activity of magnesium chloride in the x-ray spectrum of the solid catalytic component is observed halo instead of reflection, which in the spectrum of non-activated chloride is located at a distance of 2.56 .

Alkylamine compounds used as acetalization represent Al-trialkyl such as Al-triethyl, Al-triisobutyl, Al-tri-n-butyl, and linear or cyclic alkylamine compounds containing two or more Al atoms linked to each other through the O or N atoms, or through groups SO4and SO.

Examples of such compounds are the compounds of formula:

< / BR>
where n is a number from 1 to 20.

In addition, you can use connection AlR2OR', where R' is aryl, substituted in one or more positions, R - containing 1-6 carbon atoms alkyl radical, and also link the quantities to the ratio of Al/Ti was from 1 to 1000.

Electron-donor compounds that can be used as external donors include esters of aromatic acids, such as alkylbenzoates, and, in particular, silicon compounds containing at least one bond of Si-OR (R = hydrocarbon radical), 2,2,6,6-tetramethylpiperidine and 2,6-diisopropylaniline.

Examples of silicon compounds: (tert-butyl)2-Si(OCH3)2, (cyclohexyl)2Si(OCH3)3, (phenyl)2Si(OCH3)2and (cyclopentyl)2Si(OCH3)2. You can also apply a simple 1.3 diesters having the above formula. If one of these diesters is an internal donor, you can do without external donors.

The polymerization of components (a) and (B) can be done in at least two successive stages for each individual modes in the presence of the polymer obtained in the previous phase, and the catalyst used in the previous phase. The catalyst is added only at the first stage. However, its activity is such that it remains active at all subsequent stages. Thus, all subsequent stages do not add any catalysts.

The time and temperature of reaction in relation to the two stages is not critical. However, it is better if the temperature is chosen in the range from 20 to 100oC. regulation of the molecular weight by prominent regulators, in particular with hydrogen.

The catalysts can be pre-contact with small quantities of olefin (prepolymerisation). Prepolymerisation improves as the quality of the catalysts, and the structure of the obtained polymers.

If components (a) and (B) received directly by sequential polymerization, the composition of the present invention has the appearance of extrodianry particles or, in other words, a view of polymerized particles, i.e. particles discharged from the reactor. Components (a) and (B) in these particles are evenly distributed between them, which allows us to use the composition to obtain a suitable for welding of plastic films, sheets and laminates without mixing of melts for a better distribution of the components of the copolymer.

The preferred form extrodianry compositions are Sparrow particles from 0.5 to 3.5 mm, which constitute at least 90% of the total mass of the particles. Such spherical particles can be obtained, for example, using the catalysts described in U.S. patent 4472524.

The compositions of the present invention may contain such additives as antioxidants, light stabilizers, depletability, dyes and fillers.

As mentioned above, the compositions of the present invention is particularly suitable for the manufacture of films, sheets and laminates.

It is assumed that the film has a thickness of less than 100 microns, and the sheets and plates of 100 microns or more. In layered materials of the present invention at least one of the layers contains a composition of the present invention, possibly in a mixture with, for example, polyethylene or polypropylene homopolymer. In layered materials, each layer that does not contain the composition according to this invention, may be from other polyolefins, such as polyethylene or another polyolefin homopolymer. In short, layered materials according to this invention can be manufactured by known technologies: extrusion, calendering. Specific examples of films and layered materials containing compositions according to the present examples, not limiting the present invention, illustrate the features of preparation of the compositions and process of sequential polymerization.

The preparation of the solid catalytic component

In a two-liter autoclave with a stirrer turbine type and the exhaust pipe load in the atmosphere of inert gas at room temperature, 48 g of anhydrous magnesium chloride, 77 g of anhydrous ethyl alcohol and 830 ml of kerosene.

The contents of the autoclave with continuous stirring, heated to 120oC, forming the product of the interaction of MgCl2and alcohol, which is then melted and remains in kerosene as the variance.

In support autoclave nitrogen pressure of 15 ATM. The exhaust pipe has an internal diameter of 1 mm and a length of 3 m, outside heated with the help of shirts.

The finished dispersion is produced through the tube with a speed of 7 m/s At the outlet of tube dispersion is collected in a five-liter flask containing 2.5 liters of kerosene, with continuous stirring. The flask was cooled from the outside by means of a shirt, which set the initial temperature -40oC. the Final temperature variance 0oC.

The solid product in the form of particles speeches doses of hexane, then dried.

All these operations are conducted in an atmosphere of inert gas.

The result is 130 g of adduct MgCl23C2H5OH in the form of solid spherical particles. It is subjected to vacuum drying. If after drying for two hours in the weight of the solid adduct is 105 g, the drying is complete. For the most complete removal of alcohol from its adduct is heated in a stream of nitrogen to 60oC, resulting in a gain adduct MgCl22,1 C2H5OH. This adduct is used to obtain a solid catalytic component as follows.

In a glass flask with a fridge, a mechanical stirrer and a thermometer was loaded with stirring, at a temperature of 0oC in dry nitrogen atmosphere 625 ml of TiCl4and 25 g of adduct MgCl22,1 C2H5OH.

The contents of the flask are heated to 100oC for one hour. When the temperature reaches 40oC in flask enter 9 mmol of diisobutylphthalate. Temperature 100oC is maintained for two hours after which the contents provide an opportunity to settle and the liquid phase is sucked off. Add 550 ml of TiCl4and the mixture is heated for one hour to 120oC. content Then allow to settle, and LM is C and 3 times at room temperature. The resulting product is a solid catalytic component.

Catalytic system and prepolymerisation processing

Before loading in the polymerization reactors, the solid catalytic component is injected for 5 minutes at a temperature of 5oC in contact with triethylaluminium (TEAl) and dicyclopentadienyliron (DCPHS) (mass ratio TEAL/DCPHS is approximately equal to 5) used in such quantities, in which the molar ratio of TEAl/Ti solid catalytic component is equal to 65.

Then before introduction into the first polymerization reactor catalytic system is subjected to prepolymerisation by its suspension in liquid propylene at 20oC for about 20 minutes.

Examples 1 and 2

In the first reactor gas-phase polymerization get a statistical copolymer of propylene and ethylene [component (A)] by filing a continuous and constant flow prepolymerized catalyst system, hydrogen to control molecular weight and monomer of propylene and ethylene in a gas. The conditions of polymerization, the molar ratio of the reactants and the composition of the obtained copolymer are shown in table. The copolymer obtained in the first reactor of 40 continuous flow serves in the second gas-phase reactor with constant number of streams of hydrogen and propylene monomers, ethylene and 1-butene in the form of gases. Tripolymer formed from a propylene/ethylene/1-butene in the second reactor [component (B)], get in the amount of 60 wt.% of the total composition. Reaction conditions and molar ratio of reactants for each example in the table.

Leaving the second reactor polymer composition is treated with steam to remove unreacted monomers and volatile substances, and then dried.

The table shows the composition and some physical and chemical characteristics of the compositions, which correspond to the properties of the compositions according to this invention.

The table shows that the composition of example 1 component (b) contains 3,23 wt.% ethylene (C2-) and 8.8 wt.% butene (C4-at the same time as the composition of example 2 component (C) contains 3,53 wt.% ethylene and 7.5 wt.% butene.

Comparative examples 3 and 4

The composition in comparative example 3 was obtained similarly to examples 1 and 2, but without using as co monomer is 1-butene. In the first and second reactors were thus obtained 2 copolymer of propylene/ethylene in quantity (each) 50 wt.%.

The conditions of polymerization, molar sootnosheniyu 4 was prepared by obtaining in the first reactor copolymer of propylene/1-butene in the amount of 48% of the total composition, and in the second reactor copolymer of propylene/ethylene in the amount of 52% of the total composition.

The conditions of polymerization, the composition and characteristics given in the table.

You can clearly see that the composition in comparative example 3, having an extremely high content of ethylene (in the absence of 1-butene), does not meet the requirements due to the high content of polymeric fraction, extracted with n-hexane (22 wt.% compared to 4 wt.% in examples 1 and 2).

On the other hand, the composition in comparative example 4, having an excess of 1-butene does not stand up to tests for adhesion to the printing ink (voltage of 17.5/17.5 of > 20 kV compared to 12,5/12,5/12,5 kV for sample 1 and 2).

In addition, the relatively smaller values of the melting temperature of the compositions obtained in comparative examples 3 and 4, suggests that they are less technologically sophisticated than the compositions of examples 1 and 2.

The data given in the table are obtained using the following analytical methods.

- The molar ratio of the gaseous raw material

Gas chromatography

The content of ethylene and 1-butene in polymers

Infrared spectroscopy

- Flow index of races the RA crystallization (that is Christ.)

Using a differential scanning calorimeter.

- Solubility in N-hexane

The sample film thickness of 100 microns from the study of the composition was placed in an autoclave with an excess of hexane at 50oC for 2 hours, then evaporated hexane and weighing the dry residue.

- The initial temperature of the welding

Is determined as follows.

Prototyping film

Film thickness of 50 microns is produced by extrusion of each study composition at about 200oC.

Each of the obtained film placed on a polypropylene film of a thickness of 500 μm with a measure of stereoregularity 97 (in boiling n-hexane) with MFR of 4.5 g/10 min.

Superimposed on each film pressed on the tiled press under 200oC with a force of 9000 kg, excerpt 5 minutes.

The obtained two-layer film is pulled along and across, that is subjected to biaxial orientation by stretching ratio of 6 using the device for drawing long films TM to obtain a film thickness of 16 μm.

From this multi-layer film cut samples with sizes 5x10 see

Determining the initial temperature of the welding NTS.

This procedure requires Ave the I of each of the two tests described above specimen impose one on another along the length, moreover, the adjacent layers are films of the tested compositions. Folded so the samples welded along one of the short sides (5 cm) on the welding machine company Sentinel Combination Laboratory model 12-12 A. weld 5 at a pressure of 1.2 ATM, joint width, and 2.5 refer to the welding Temperature increase from sample to sample 2oC. From each of the welded sample cut out pieces of size 2,5x10 see In each trial Nazarene free long ends of the samples are attached to a dynamometer and make every effort equivalent to a load of 200 g

Thus to set the minimum sealing temperature at which the seam is not broken at a load of 200 g Is the initial temperature of the welding NTS test composition.

Testing of adhesion to the printing ink

Manufacturing of samples for these tests are similar to the production of samples for determination of NTS. Each sample film was placed on a sheet of polypropylene with a thickness of 1 mm, which, in turn, is located between the two opposite circular electrodes with a diameter of 2.5 cm, one of which is grounded.

On the SAME device between two electrodes provide a voltage to 80 kV with a frequency of 50 Hz for one of the three samples each, cut from the same sample film, starting with the lower border of the selected voltage range, gradually increasing the voltage up to the maximum.

On the day of sample processing by corona discharge of all series of samples are selected based on one sample, put them inks and experience by removing the masking tape. 24 hours after the corona treatment, select one sample from each series and subjected to the procedure as described above. Finally, 7 days after the treatment by corona discharge, then do the same thing with the remaining samples.

During the tests on the sample surface treated by corona discharge, a rubber roller is applied one-component paint. White paint mark M 57, offered by the company Siegwerk, contains a mixture of solvents (ethanol or ethyl acetate), nitrocellulose, various pigments, polyurethane, lubrication and adhesion promoters.

After drying of the ink at room temperature for 1 hour and measure the adhesion of paint to the surface treated by corona discharge, by gluing strips of masking tape to the surface of the film coated with ink and then peel it. Then measure the quantities of the customers in relation to the amount of ink that was on the sample before removing the tape.

Comparing the share of paint remaining on the samples according to the increase of voltage, determine the minimum voltage at which the proportion of paint remaining on the sample reaches 80%. This is the adhesiveness of the film to the printing ink.

The amount of adhesion to the printing ink, expressed by kV presented in table three values. The first of three values refers to samples for which adhesion was determined on the day of treatment by corona discharge, the second value after 24 hours and the third value after 7 days.

1. Composition based on crystalline polypropylene copolymer comprising a copolymer of propylene with ethylene and a copolymer of propylene with ethylene and C4- C8-alpha-olefin, characterized in that as a copolymer of propylene with ethylene, it contains a copolymer with ethylene content of 1 to 5 wt.%, and as a copolymer of propylene with ethylene and C4- C8-alpha-olefin - copolymer with ethylene content of 1 to 5 wt.% and alpha-olefin of 6 to 15 wt.% in the following ratio, wt.%:

The copolymer of propylene with ethylene - 20 - 60

The copolymer of propylene with ethylene and C4- C8alpha-Ola is AC.%.

2. The composition according to p. 1, characterized in that it contains 30 to 50 wt.% copolymer of propylene with from 2 to 4 wt.% ethylene and 50 to 70 wt.% copolymer of propylene with from 2 to 4 wt.% ethylene and 7 - 12 wt.% C4- C8-alpha-olefin.

3. The composition according to p. 1, characterized in that it contains a copolymer of propylene with ethylene and C4- C8-alpha-olefin, selected and groups, including 1-butene, 1-penten, 1-hexene, 4-methyl-1-penten and 1-octene.

4. The sheet or plate made of a composition comprising a copolymer of propylene with ethylene and a copolymer of propylene with ethylene and C4-C alpha-olefin, characterized in that they are made from the composition under item 1.

5. The sheet or plate under item 4, characterized in that they are made from the compositions of p. 2.

6. The film is suitable for application of commercial printing, made of a composition comprising a copolymer of propylene with ethylene and a copolymer of propylene with ethylene and C4- C8-alpha-olefin, characterized in that it is made from the composition under item 1.

7. Film on p. 6, characterized in that it is made from the composition under item 2.

8. Layered material suitable for the application of commercial printing, including layer, suitable for commercial printing>- C8-alpha-olefin, characterized in that as a layer suitable for commercial printing, it contains a layer made from the composition under item 1.

9. Layered material under item 8, characterized in that as a layer suitable for commercial printing, it contains a layer made of the composition of p. 2.

 

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