CN107344983A - A kind of atactic copolymerized polypropene for laminated film hot sealing layer and preparation method thereof - Google Patents
A kind of atactic copolymerized polypropene for laminated film hot sealing layer and preparation method thereof Download PDFInfo
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- CN107344983A CN107344983A CN201610294615.9A CN201610294615A CN107344983A CN 107344983 A CN107344983 A CN 107344983A CN 201610294615 A CN201610294615 A CN 201610294615A CN 107344983 A CN107344983 A CN 107344983A
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- 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
- 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
- C08F210/04—Monomers containing three or four carbon atoms
- C08F210/06—Propene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- 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
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/08—Copolymers of ethene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/10—Transparent films; Clear coatings; Transparent materials
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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
- C08L2203/16—Applications used for films
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Abstract
The invention discloses a kind of atactic copolymerized polypropene for laminated film hot sealing layer and preparation method thereof, is the butylene ternary atactic copolymerized polypropene resin of propylene and ethylene 1 for the atactic copolymerized polypropene of laminated film hot sealing layer, its comonomer includes：The 85mol% of propylene 60, the 25mol% of ethene 8 and the 15mol% of 1 butylene 7.The atactic copolymerized polypropene that the present invention is used for laminated film hot sealing layer belongs to heterophasic copolymer, its design feature is different from ethylene-propylene random copolymer, have rigidity and toughness concurrently, the addition of 3rd comonomer, reduce the order of molecular chain structure, its crystallinity reduces, the transparency of material, impact strength, resistance to low temperature have risen, the heat resistance of material declines simultaneously, show as originating the decline of heat-sealing temperature (SIT) in film, modernization fast package machinery is greatly adapted to, suitable for the hot sealing layer of film.
Description
Technical field
The present invention relates to a kind of atactic copolymerized polypropene for laminated film hot sealing layer and preparation method thereof, belongs to new material neck
Domain.
Background technology
Polypropylene invention has been widely used as having high rigidity, high heat-resisting and transparency Themoplastic molding materials so far.
In order to expand polyacrylic application field, to polypropylene carry out modification by copolymerization turn into effective way, industrially pass through frequently with
Comonomer be ethene, butylene, alkene etc., Propylene polymerization, the copolymerization of the third fourth can be produced, third be copolymerized, additionally
There are part graft copolymers.However, in the intensity of increase polypropylene coating materials, heat-sealing temperature of coating materials etc. is reduced, is used
The means of homopolymerization or binary copolymerization can not be solved, therefore elastomeric component generally is added into poly- third in order to improve these performances
Among alkene.
It is uniformly dispersed however, adding elastomeric component in polypropylene for guarantee, generally requires and mixed again by screw rod,
It is higher plus elastomer price itself, although this random polypropylene material performance for resulting in adding elastomer may use cost
It is high.
The content of the invention
The present invention provide it is a kind of with excellent heat resistance and low-temperature heat-sealing performance and pliability and shock resistance be used for it is compound
Atactic copolymerized polypropene of film hot sealing layer and preparation method thereof.
In order to solve the above technical problems, the technical solution adopted in the present invention is as follows：
A kind of atactic copolymerized polypropene for laminated film hot sealing layer, gather for propylene-ethylene -1- butylene ternary random copolymerizations
Allyl resin.
The atactic copolymerized polypropene that the application is used for laminated film hot sealing layer is preferably elastomeric phase.
The application polypropylene belongs to heterophasic copolymer, and its design feature is different from ethylene-propylene random copolymer, has rigidity and toughness concurrently
Etc. the equilibrium of a variety of premium properties, the addition of the 3rd comonomer, the order of molecular chain structure, its crystallinity drop are reduced
Low, the transparency of material, impact strength, resistance to low temperature have risen, while the heat resistance of material declines, and is making
Show as originating the decline of heat-sealing temperature (SIT) in film, modernization fast package machinery has greatly been adapted to, suitable for thin
In the hot sealing layer of film.
In order to further improve the heat resistance of product and low-temperature heat-sealing performance, it is preferable that for the random common of laminated film hot sealing layer
Gather polyacrylic comonomer to include：Propylene 60-85mol%, ethene 8-25mol% and 1- butylene 7-15mol%, further
Preferably, propylene 70-85mol%, ethene 8-19mol% and 1- butylene 7-11mol%, more preferably, propylene 73-85mol%,
Ethene 8-17mol% and 1- butylene 7-10mol%.
The application is used for inherent viscosity of the atactic copolymerized polypropene of laminated film hot sealing layer in 135 DEG C of naphthalane
0.1-15dl/g, preferably 0.5-15dl/g, it is preferably 1.2-15dl/g.
The application is used for the atactic copolymerized polypropene of laminated film hot sealing layer, melt flow rate (MFR) 0.1-400g/10min.
Preferably 1-80g/10min, 190 DEG C, 21.6kg.
Measured by gel permeation chromatography (GPC) for the application for the atactic copolymerized polypropene of laminated film hot sealing layer
Molecular weight distribution is not more than 4, preferably 1.8-3.5, more preferably 2.1-2.7.
Degree of randomness：Indicate the parameter B of the atactic copolymerized polypropene for laminated film hot sealing layer of comonomer sequence distribution
It is worth for 1.0-2.0, preferably 1.0-1.5, more preferably 1.0-1.2.
Parameter B values are mentioned by B.D.Cole-man and T.G.FOX in J.Polym.Sci., Al, 3188 (1963)
Cross, the parameter can be obtained by following formula：
B=P12/ (2P1*P2)
Wherein, P1 is the first content of monomer component, and P2 is second comonomer content component, and P12 is that the first monomer subtracts second
The ratio of sequence monomer and total binary sequence arranges.
In B=1, Bernoulli Jacob's statistics is used for copolymer；In B ＜ 1, copolymer tends to block；In B>When 1,
Copolymer tends to replace；As B=2, copolymer is alternate copolymer.
The fusing point Tm that propylene-ethylene -1- butylene ternary atactic copolymerized polypropene resins are measured by differential scanning calorimetry is
80-130 DEG C, preferably 117-130 DEG C.
In the atactic copolymerized polypropene that the application is used for laminated film hot sealing layer, the crystallinity that is measured by X-ray diffraction method
C and comonomer Component units content M (mol%) meet following relations：C≥-1.5M+75.
The application is used for the atactic copolymerized polypropene of laminated film hot sealing layer by propylene monomer, vinyl monomer and 1- butene monomers
Copolymerization forms, and polymerization process uses solid polyolefin hydrocarbon catalyst；Polymerization pressure is that air is depressed into 100kg/cm2, preferably greatly
Air pressure is to 60kg/cm2。
The each component of catalyst mixes in polymer reactor, or is added after premix in reactor；If premixing,
Mixing temperature is -50 DEG C -160 DEG C, is preferably -20-110 DEG C, time of contact is 1-1500 minutes, is preferably 4-500
Minute；Mixing temperature can change in mixed process.
Polymerization can be carried out with any liquid polymerization method or gas phase polymerization process.
In liquid phase polymerization, usable unreactive hydrocarbons solvent can also be used propylene to be used as solvent in itself.
In suspension polymerisation, polymerization temperature is usually -50-150 DEG C, preferably 10-90 DEG C；In solution polymerization, temperature
Degree is usually 0-250 DEG C, preferably 30-180 DEG C；During gas phase polymerization, temperature is usually 0-130 DEG C, preferably
For 20-90 DEG C.
Polymerization pressure is usually that air is depressed into 100kg/cm2, preferably air is depressed into 60kg/cm2.Polymerisation can in batches,
It is semicontinuous or be carried out continuously.Polymerization also can under the conditions of differential responses in two steps or multistep carry out.
The molecular weight of obtained propylene-ethylene -1- butylene ternary atactic copolymers can by into polymerization system add hydrogen or
Change polymerization temperature or polymerization pressure and be controlled.
The NM technology of the present invention is with reference to prior art.
The atactic copolymerized polypropene that the present invention is used for laminated film hot sealing layer belongs to heterophasic copolymer, and its design feature is different from
Ethylene-propylene random copolymer, has rigidity and toughness concurrently, the addition of the 3rd comonomer, reduces the order of molecular chain structure,
Its crystallinity reduces, and the transparency of material, impact strength, resistance to low temperature have risen, while the heat resistance of material
Decline, show as originating the decline of heat-sealing temperature (SIT) in film, greatly adapted to modernization fast package machinery,
Suitable for the hot sealing layer of film, and cost is cheap.
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but present disclosure
It is not limited solely to the following examples.
The measurement of propylene-ethylene -1- butylene ternary atactic copolymer properties：
1. content of monomer：Measured with 13C-NMR.
2. inherent viscosity：Measure in 135 DEG C of decahydronaphthalene and represented with dl/g.
3. molecular weight distribution：As follows with the gpc measurement of Millipore Co. productions.
Use the TSK-GNH-HT splitters that a diameter of 27 millimeters and length are 600 millimeters.Column temperature is set as 140 DEG C,
Mobile phase used is the o- dichlorotoleune (WAKO containing 0.025% (weight) BHT (Takeda chemical companies) antioxidant
Junyaku Kogyo k.k), flow rate 1.0ml/min.500 microlitre of 0.1% (weight) sample solution is introduced should
Post, differential refractometer are counted as detection.
Purchased from TOSO Co., Ltd polystyrene is used as Mw<1000 and Mw>4*106Molecular weight standard, be purchased from
The polystyrene of Pressure chemical companies is used as 1000<Mw<4*106Molecular weight standard.
4.B values (monomer distribution)
200mg copolymers are measured in the 13CNMR spectrum of the homogeneous sample solution of 1 milliliter of hexachlorobutadiene, coupon used
For diameter 10mm, measuring condition used is usually：120 DEG C, frequency 25.05MHz, frequency spectrum 1500Hz of temperature, filter
Width 1500Hz, pulse recurring temporal 4.2s, time of integration 2000-5000.
5. fusing point (Tm)
The DSC-7 type instrument tests that fusing point is produced using PE Co. as follows.About 5mg sample is mounted in aluminium dish
200 DEG C are heated to, 5min is kept, -40 DEG C, then the speed with 10 DEG C/min is then cooled to 10 DEG C/min speed
Heating, has obtained the exotherm of sample, has determined Tm.
6. crystallinity
Available thickness is that the X- diffraction spectras of 1.0mm tabletting determine that tabletting stores at least 24h after pressing.
Embodiment 1
900ml hexanes and 65g1- butylene are being added with the thorough purged 2L autoclaves of nitrogen, is adding 1 mM
Triethyl aluminum, system temperature is increased to 70 DEG C, is passed through propylene (intake is determined by the pressure being finally achieved) and 50ml
Ethene, gross pressure is set to reach 7kg/cm2, add 0.3 mM of MAO and 0.001 mM (in terms of zirconium atom)
Dichloro-dimethyl silicylene-bis- [1- (2- methyl 4-phenyls indenyls)] zirconium, carry out 30 minutes polymerisations；When
After reaction terminates, autoclave is vented, with Methanol Recovery polymer, 12h is dried under 110 DEG C of vacuum, produces propylene-second
Alkene -1- butylene ternary atactic copolymers, performance are shown in Table 1.
Embodiment 2
900ml hexanes and 25g1- butylene are being added with the thorough purged 2L autoclaves of nitrogen, is adding 1 mM
Triethyl aluminum, system temperature is increased to 70 DEG C, propylene and 20ml ethene is passed through, gross pressure is reached 7kg/cm2, then add
Enter the dichloro-dimethyl silicylene of 0.3 mM of MAO and 0.001 mM (in terms of zirconium atom)-bis-
[1- (2- methyl 4-phenyls indenyl)] zirconium, carry out 30 minutes polymerisations；After reaction terminates, autoclave is vented,
With Methanol Recovery polymer, 12h is dried under 110 DEG C of vacuum, produces propylene-ethylene -1- butylene ternary atactic copolymers, property
1 can be shown in Table.
Embodiment 3
850ml hexanes and 30g1- butylene are being added with the thorough purged 2L autoclaves of nitrogen, is adding 1 mM
Triethyl aluminum, system temperature is increased to 70 DEG C, propylene and 40ml ethene is passed through, gross pressure is reached 7kg/cm2, then add
Enter the dichloro-dimethyl silicylene of 0.3 mM of MAO and 0.001 mM (in terms of zirconium atom)-bis-
[1- (2- methyl 4-phenyls indenyl)] zirconium, carry out 30 minutes polymerisations；After reaction terminates, autoclave is vented,
With a large amount of Methanol Recovery polymer, 12h is dried under 110 DEG C of vacuum, produces propylene-ethylene -1- butylene ternary atactic copolymers,
Performance is shown in Table 1.
Embodiment 4
870ml hexanes and 35g1- butylene are being added with the thorough purged 2L autoclaves of nitrogen, is adding 1 mM
Triethyl aluminum, system temperature is increased to 70 DEG C, propylene and 30ml ethene is passed through, gross pressure is reached 7kg/cm2, then add
Enter the dichloro-dimethyl silicylene of 0.3 mM of MAO and 0.001 mM (in terms of zirconium atom)-bis-
[1- (2- methyl 4-phenyls indenyl)] zirconium, carry out 20 minutes polymerisations；After reaction terminates, autoclave is vented,
With a large amount of Methanol Recovery polymer, 12h is dried under 110 DEG C of vacuum, produces propylene-ethylene -1- butylene ternary atactic copolymers,
Performance is shown in Table 1.
Embodiment 5
890ml hexanes and 45g1- butylene are being added with the thorough purged 2L autoclaves of nitrogen, is adding 1 mM
Triethyl aluminum, system temperature is increased to 70 DEG C, propylene and 50ml ethene is passed through, gross pressure is reached 7kg/cm2, then add
Enter the dichloro-dimethyl silicylene of 0.3 mM of MAO and 0.001 mM (in terms of zirconium atom)-bis-
[1- (2- methyl 4-phenyls indenyl)] zirconium, carry out 30 minutes polymerisations；After reaction terminates, autoclave is vented,
With a large amount of Methanol Recovery polymer, 12h is dried under 110 DEG C of vacuum, produces propylene-ethylene -1- butylene ternary atactic copolymers,
Performance is shown in Table 1.
Embodiment 6
880ml hexanes and 55g1- butylene are being added with the thorough purged 2L autoclaves of nitrogen, is adding 1 mM
Triethyl aluminum, system temperature is increased to 70 DEG C, propylene and 50ml ethene is passed through, gross pressure is reached 7kg/cm2, then add
Enter the dichloro-dimethyl silicylene of 0.3 mM of MAO and 0.001 mM (in terms of zirconium atom)-bis-
[1- (2- methyl 4-phenyls indenyl)] zirconium, carry out 15 minutes polymerisations；After reaction terminates, autoclave is vented,
With a large amount of Methanol Recovery polymer, 12h is dried under 110 DEG C of vacuum, produces propylene-ethylene -1- butylene ternary atactic copolymers,
Performance is shown in Table 1.
Embodiment 7
870ml hexanes and 45g1- butylene are being added with the thorough purged 2L autoclaves of nitrogen, is adding 1 mM
Triethyl aluminum, system temperature is increased to 70 DEG C, propylene and 20ml ethene is passed through, gross pressure is reached 7kg/cm2, then add
Enter the dichloro-dimethyl silicylene of 0.3 mM of MAO and 0.001 mM (in terms of zirconium atom)-bis-
[1- (2- methyl 4-phenyls indenyl)] zirconium, carry out 30 minutes polymerisations；After reaction terminates, autoclave is vented,
With a large amount of Methanol Recovery polymer, 12h is dried under 110 DEG C of vacuum, produces propylene-ethylene -1- butylene ternary atactic copolymers,
Performance is shown in Table 1-2.
Performance table obtained by 1 each embodiment of table
Performance table obtained by 2 each embodiment of table
Claims (10)
- A kind of 1. atactic copolymerized polypropene for laminated film hot sealing layer, it is characterised in that：For propylene-ethylene -1- butylene Ternary atactic copolymerized polypropene resin.
- 2. it is used for the atactic copolymerized polypropene of laminated film hot sealing layer as claimed in claim 1, it is characterised in that：It is common Polycondensation monomer includes：Propylene 60-85mol%, ethene 8-25mol% and 1- butylene 7-15mol%.
- 3. it is used for the atactic copolymerized polypropene of laminated film hot sealing layer as claimed in claim 2, it is characterised in that：It is common Polycondensation monomer includes：Propylene 70-85mol%, ethene 8-19mol% and 1- butylene 7-11mol%.
- 4. it is used for the atactic copolymerized polypropene of laminated film hot sealing layer as claimed in claim 3, it is characterised in that：It is common Polycondensation monomer includes：Propylene 73-85mol%, ethene 8-17mol% and 1- butylene 7-10mol%.
- 5. the atactic copolymerized polypropene for laminated film hot sealing layer as described in claim 1-4 any one, its feature It is：Its inherent viscosity in 135 DEG C of naphthalane is 0.1-15dl/g.
- 6. the atactic copolymerized polypropene for laminated film hot sealing layer as described in claim 1-4 any one, its feature It is：Its molecular weight distribution is not more than 4；Melt flow rate (MFR) is 0.1-400g/10min.
- 7. the atactic copolymerized polypropene for laminated film hot sealing layer as described in claim 1-4 any one, its feature It is：It indicates that the degree of randomness parameter B values of comonomer sequence distribution are 1.0-2.0.
- 8. the atactic copolymerized polypropene for laminated film hot sealing layer as described in claim 1-4 any one, its feature It is：Its fusing point is 80-130 DEG C.
- 9. the atactic copolymerized polypropene for laminated film hot sealing layer as described in claim 1-4 any one, its feature It is：C >=-1.5M+75, wherein, C is crystallinity, and M is the content of comonomer Component units, unit mol%.
- 10. the preparation side of the atactic copolymerized polypropene for laminated film hot sealing layer described in claim 1-9 any one Method, it is characterised in that：Formed by the copolymerization of propylene monomer, vinyl monomer and 1- butene monomers, polymerization process is gathered using solid Alkene catalyst, polymerization pressure are that air is depressed into 100kg/cm2；The each component of catalyst mixes in polymer reactor, or is added after premix in reactor；If premixing, Mixing temperature is -50 DEG C -160 DEG C, and time of contact is 1-1500 minutes；It is polymerized to polymerisation in solution, suspension polymerisation or gas-phase polymerization；If polymerisation in solution, using unreactive hydrocarbons as solvent or with propylene , as solvent, polymerization temperature is 0-250 DEG C for this；If suspension polymerisation, polymerization temperature is -50-150 DEG C；If vapor phase method Polymerization, polymerization temperature are 0-130 DEG C.
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| CN109868953A (en) * | 2019-01-21 | 2019-06-11 | 桐城市桐佳装饰有限公司 | A kind of oil stain preventing function wallpaper for kitchen use |
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| CN105330778A (en) * | 2014-08-14 | 2016-02-17 | 中国石化扬子石油化工有限公司 | Polypropylene resin used for heat-sealing layer of film |
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| CN105330778A (en) * | 2014-08-14 | 2016-02-17 | 中国石化扬子石油化工有限公司 | Polypropylene resin used for heat-sealing layer of film |
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|---|---|---|---|---|
| CN109868953A (en) * | 2019-01-21 | 2019-06-11 | 桐城市桐佳装饰有限公司 | A kind of oil stain preventing function wallpaper for kitchen use |
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