CN101987900B - Method for synthesizing special resin for polypropylene cast film - Google Patents
Method for synthesizing special resin for polypropylene cast film Download PDFInfo
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- CN101987900B CN101987900B CN2009100911140A CN200910091114A CN101987900B CN 101987900 B CN101987900 B CN 101987900B CN 2009100911140 A CN2009100911140 A CN 2009100911140A CN 200910091114 A CN200910091114 A CN 200910091114A CN 101987900 B CN101987900 B CN 101987900B
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Abstract
The invention relates to a method for synthesizing special resin for a randomly copolymerized polypropylene cast film. A second generation domestic loop pipe polypropylene device is used for synthesis, CS-2 catalyst/propylene is 0.02-0.03 g/kg, and hydrogen gas and ethylene are uniformly added into two loop pipes; triethyl aluminum/propylene is 0.14-0.24 kg/t, triethyl aluminum/electron donor is 1-8 kg/kg, the densities of a first loop pipe polymerization reactor and a second loop pipe polymerization reactor are controlled at 530-580 kg/m<3>, the concentration of hydrogen gas is controlled at 1200-1500 ppm, ethylene/propylene is 18-20 kg/t, and the melt flow rate of powder is 11-14 g/10 min; additives comprise an antioxidant, a neutralizing agent, an antiblocking agent and a slipping agent; the melt flow rate value of a product is 6-9 g/10 min, and the content of ethylene is 3.6-4.0%.
Description
Technical field
The present invention relates to the resin dedicated compound method of a kind of high ethylene content atactic copolymerized polypropene casting films, belong to the synthetic resins field.
Background technology
Polypropylene casting film (CPP) is to stretch through a kind of nothing that the quenching of melt curtain coating is produced, and nondirectional cast film is widely used in textiles, the packing of fresh flower, food, daily necessities.It is resin dedicated that the production requirement of CPP film is adopted, and resin will have certain fluidity of molten and melt tension, and general requirement resin melt speed (MFR) scope that flows is 6～12g/10min, divides homopolymer and multipolymer two class greatly.The atactic copolymerized polypropene casting films PP Pipe Compound of high ethylene content is mainly used in heat-sealing film or the use of boiling film owing to have lower fusing point with impact property preferably.Because higher ethylene content, very difficulty and quality product fluctuation are bigger to make the production of polypropylene plant LP.
Summary of the invention
The objective of the invention is to provide a kind of resin dedicated method of atactic copolymerized polypropene casting films of synthesizing the high ethylene content (3.6%-4.0%) of the casting films that is used to pack, optimised process index and additive formulations with the polypropylene plant of Spheripol (homemade) s-generation endless tube.
Resin dedicated compound method according to the invention is following:
Adopt CS-2 catalyzer (group of section produces, and staple is titanium, magnesium, chlorine, ester and a small amount of fugitive constituent etc.) on the sunny side, on the polypropylene plant of Spheripol (homemade) s-generation endless tube; Adopt a ring two rings to add the hydrogen and the ethene of equivalent simultaneously; Melt mass flow rate is controlled at 6～9g/10min, and the ethene quality control is produced the random copolymerization powder of high ethylene content 3.6～4.0%; And mix in mixing tank by formula rate with oxidation inhibitor, neutralizing agent, slipping agent, antiblocking agent; Between the extruding pelletization, 150～235 ℃ of prilling temperatures, institute's granulation material promptly gets said PP Pipe Compound through homogenizing.And in the suitability for industrialized production practice, groped the technic index that the most suitable high ethylene content atactic copolymerized polypropene casting films PP Pipe Compound is produced.Guaranteed quality product.
Table 1 synthesis technique index
Table 2 extruding workshop section technic index
The method that guarantees high ethylene content random copolymerization technology long-period stable operation is following:
Adding Atmer163 in 8 hours in advance when HOPP is changed the line of production high ethylene content atactic copolymerized polypropene and adding concentration in 24 hours in advance is 100% electron donor, and guarantees that the add-on of Atmer163 is not less than 0.5kg/h.Flash tank (D2301) the baiting valve latch up phenomenon that occurs when taking the polypropylene plant of Spheripol (homemade) s-generation endless tube after this measure to produce the atactic copolymerized polypropene powder significantly reduces.And the vapor temperature of adjustment entering steamer (D2501), the vapor temperature that gets into steamer is controlled at below 110 ℃.Make device steamer washing tower (T2501) fine powder when producing random thing significantly reduce.And the discharge line of having transformed the polypropylene plant T2501 of Spheripol (homemade) s-generation endless tube transform 2 turnings as by 5 turnings, and drainage speed is accelerated.Long-term operation when having guaranteed that device is produced random material.Guarantee the long-term operation of random copolymerized units.
The said polypropylene plant of the present invention is the polypropylene plant of Spheripol (homemade) s-generation endless tube.
The said catalyzer of the present invention is the CS-2 catalyzer of the group of section that faces south,
The said ethene of the present invention is that purity is greater than 99.9%.
The said TEAL of the present invention is a triethyl aluminum, and molecular formula is (C
2H
5)
3Al,
The said DONORO of the present invention is electron donor Donor C, and name is called cyclohexyl, methyl, dimethoxy silane, and molecular formula is C
9H
20O
2Si.
The said Atmer163 of the present invention, Chinese are oxyethyl group alkyl amine.
The said prescription of the present invention is the additive adding proportion, and by 100 weight parts, oxidation inhibitor is 0.1～0.3 part in the atactic copolymerized polypropene powder, and neutralizing agent is 0.03～0.1 part, and antiblocking agent is 0.1～0.3 part, and slipping agent is 0.06～0.1 part.
The said homogenizing of the present invention is that institute's granulation material is one batch by 200 tons, in the homogenizing storehouse, mixes 4～8 hours, to keep the homogeneity of PP Pipe Compound performance.
The said oxidation inhibitor of the present invention is composite antioxidant, is made up of in 1: 2 ratio antioxidant 1010 and 168.
The said antioxidant 1010 of the present invention is [3-(3.5 a pairs of tertiary butyl-4-hydroxy-cyclohexyls) propionic ester], and 168 is (2,4 dual-tert-butyl phenol) phosphorous acid ester.
The said neutralizing agent of the present invention is a calcium stearate.
The said antiblocking agent of the present invention be median size at 0.5 μ m, purity is greater than the silicon-dioxide more than 99%.
The said slipping agent of the present invention is an erucamid erucyl amide.
The invention effect:
Adopt the polypropylene plant of Spheripol (homemade) s-generation endless tube,, the hydrogen add-on, confirmed triethyl aluminum/propylene and triethyl aluminum/electron donor optimum control value through control ethene add-on.Realized the stabilization of industry scale prodn of the random copolymerization PP Pipe Compound of high ethylene content 3.6-4.0%,, realized the production long-period stable operation of random copolymerization casting films resin through Optimizing operation technology.But realized the optimum balance of plyability and resistance to blocking in the processing film process, improved the processibility and the use properties of PP Pipe Compound.The atactic copolymerized polypropene casting films PP Pipe Compound of exploitation becomes the excellent system raw material that domestic casting films producer is approved because of having excellent physical and mechanical properties, heat sealability and the transparency.
Description of drawings
Fig. 1 polypropylene plant schematic flow sheet
Wherein: D2201 contacts jar, Z2203 on-line mixing device, R2200 pre-polymerization reactor, R2201 one loop polymerization reactor, R2202 two loop polymerization reactor, D2301 flash tank, F2301 deep bed filter, D2501 steamer, D2502 moisture eliminator, EX2801 extrusion machine in advance
Embodiment
Synthetic with home-made s-generation endless tube polypropylene plant; Catalyzer, triethyl aluminum and electron donor are fully mixed the formation complex compound at 10 ℃ in contact in advance jar, the complex compound that from preparatory contact jar, overflows in the on-line mixing device with entering prepolymerization reactor after 20 ℃ propylene mixes, at 20 ℃; 3.4Mpa under the pressure, reaction 4min gets into a loop polymerization reactor; Add ethene and hydrogen, a part of propylene carries out polymerization, and polymer concentration is controlled at 50-55%wt; Ethene, the hydrogen of polymkeric substance, propylene and the adding of coming out from a loop polymerization reactor get into two loop polymerization reactor; Add oxyethyl group alkyl amine to be not less than 0.5kg/h from the outlet of two loop polymerization reactor simultaneously, one, two endless tube polymeric reaction temperatures are 69-71 ℃, and pressure is 3.3～3.4Mpa; The material that two loop polymerization reactor are discharged; After the flash line of jacket steam heating heated up, entering pressure was that the flash tank of 1.8Mpa carries out gas solid separation earlier, and isolated polymkeric substance gets into steamer through strainer and makes the remainder catalyst inactivation; Steam the monomer of powder absorption, obtain the atactic copolymerized polypropene powder after the drying; In atactic copolymerized polypropene grain weight amount is 100 parts, adds 0.1～0.3 part in oxidation inhibitor, 0.03～0.1 part of neutralizing agent, and 0.1～0.3 part of antiblocking agent, 0.06～0.1 part of slipping agent is sent into the extrusion machine extruding pelletization after the mixing, 150～235 ℃ of prilling temperatures;
Catalyzer/propylene is 0.02～0.03g catalyzer/kg propylene; Triethyl aluminum/propylene is 0.14～0.24kg/t, and triethyl aluminum/electron donor is 1～8kg/kg, and density of hydrogen is controlled at 1200～1500ppm; Ethylene/propene is 18～20kg/t; The vapor temperature of steamer is controlled at 100～110 ℃, and the powder melt flow rate(MFR) is controlled at 11～14g/10min, and the ethylene content of atactic copolymerized polypropene powder is controlled at 3.6～4.0%;
Electron donor is cyclohexyl, methyl or dimethoxy silane;
Oxidation inhibitor is composite antioxidant, by antioxidant 1010 [3-(3.5 pairs of tertiary butyl-4-hydroxy-cyclohexyls) propionic ester], with 168 (2,4 dual-tert-butyl phenol) phosphorous acid ester by weight 1: 2 ratio form;
Neutralizing agent is a calcium stearate;
Antiblocking agent be median size at 0.5 μ m, purity is greater than the silicon-dioxide more than 99%;
Slipping agent is an erucamid erucyl amide.
Embodiment 1
(device load 6t/h): Primary Catalysts (120g/h), (105g/h～840g/h) in about 10 ℃, fully mixes the formation complex compound in contact jar D2201 in advance for triethyl aluminum (840g/h) and electron donor.The complex compound that from D2201, overflows (6t/h) mixes the back with cold propylene (20 ℃) and gets into pre-polymerization reactor R2200 in Z2203 (on-line mixing device); At 20 ℃; 3.4Mpa under the pressure, about reaction 4min, get among the annular-pipe reactor R2201; Simultaneously the hydrogen of ethene (about 116kg/h) and control molecular weight is imported an annular-pipe reactor R2201 together, in an annular-pipe reactor, carry out polyreaction.70 ℃ of service temperatures, pressure 3.4Mpa, a part of propylene carries out polymerization, and the remaining liquid propylene is as the flowing carrier of solid polymer simultaneously, and slurry concentration is controlled at 50-55%wt.The slurry that comes out from R2201, propylene and get into two annular-pipe reactor R2202 from the ethene (116kg/h) and the hydrogen of battery limit (BL).And to be not less than 0.5kg/h from R2202 outlet adding Atmer163.The slurry that two annular-pipe reactor R2202 discharge; Earlier after the flash line of jacket steam heating heats up; Entering pressure is that the flash tank D2301 of 1.8Mpa carries out gas solid separation; Isolated gas enters into propylene washing tower through dynamic separator, and the collected polymkeric substance in flash tank D2301 bottom then under material level control, is discharged to deep bed filter F2301.Polymkeric substance among the F2301 relies on gravity to get in the moving-bed type steamer D2501; D2501 has slow stirrer, and steam gets into D2501 equably by grid distributor with holes, makes progress through steam; Powder is to " convection current " form that moves down; Make the remainder catalyst inactivation, and steam the monomer of powder absorption, thereby improve the quality of products.D2501 working pressure 0.02Mpa, 100～110 ℃ of temperature.Through the closed circuit hot nitrogen recycle system, will in fluidized bed dryer D2502, remove from the moisture content of the polymer surfaces of D2501.
Produce 200 tons of atactic copolymerized polypropene pellets in each batch; 1920kg polypropylene powder, oxidation inhibitor 200kg, neutralizing agent 60kg, antiblocking agent 200kg, slipping agent 120kg thorough mixing are delivered to mixer with the polymkeric substance from D2502 through WT-MSR continuously pari passu in the additive tank, deliver to extrusion machine EX2801 again.Send into the homogenizing feed bin then and carry out homogenizing, homogenizing 8 hours gets product.Product melt flow rate(MFR) numerical value is 6～9g/10min, and ethylene content is 3.6～4.0%.
Embodiment 2
(device load 6t/h): Primary Catalysts (150g/h), (142.5g/h～1140g/h) in about 10 ℃, fully mixes the complexing center that forms in contact jar D2201 in advance for triethyl aluminum (1140g/h) and electron donor.The complex compound that from D2201, overflows (6t/h) mixes the back with cold propylene (20 ℃) and gets into prepolymerization reactor R2200 in Z2203 (on-line mixing device); At 20 ℃; 3.4Mpa under the pressure, about reaction 4min, get among the loop polymerization reactor R2201; Simultaneously the hydrogen of ethene (about 116kg/h) and control molecular weight is imported a loop polymerization reactor R2201 together, in a loop polymerization reactor, carry out polyreaction.70 ℃ of service temperatures, pressure 3.4Mpa, a part of propylene carries out polymerization, and the remaining liquid propylene is as the flowing carrier of solid polymer simultaneously, and slurry concentration is controlled at 50-55%wt.The slurry that comes out from R2201, propylene and get into two loop polymerization reactor R2202 from the ethene (116kg/h) and the hydrogen of battery limit (BL).And to be not less than 0.5kg/h from R2202 outlet adding Atmer163.The slurry that two loop polymerization reactor R2202 discharge; Earlier after the flash line of jacket steam heating heats up; Entering pressure is that the flash tank D2301 of 1.8Mpa carries out gas solid separation; Isolated gas enters into propylene washing tower through dynamic separator, and the collected polymkeric substance in flash tank D2301 bottom then under material level control, is discharged to deep bed filter F2301.Polymkeric substance among the F2301 relies on gravity to get in the moving-bed type steamer D2501; D2501 has slow stirrer, and steam gets into D2501 equably by grid distributor with holes, makes progress through steam; Powder is to " convection current " form that moves down; Make the remainder catalyst inactivation, and steam the monomer of powder absorption, thereby improve the quality of products.D2501 working pressure 0.02Mpa, 100～110 ℃ of temperature.Through the closed circuit hot nitrogen recycle system, will in fluidized bed dryer D2502, remove from the moisture content of the polymer surfaces of D2501.
Produce 200 tons of atactic copolymerized polypropene pellets in each batch; 1410kg polypropylene powder, oxidation inhibitor 400kg, neutralizing agent 130kg, antiblocking agent 400kg, slipping agent 160kg thorough mixing are delivered to mixer with the polymkeric substance from D2502 through WT-MSR continuously pari passu in the additive tank, deliver to extrusion machine EX2801 again.Send into the homogenizing feed bin then and carry out homogenizing, homogenizing 8 hours gets product.Product melt flow rate(MFR) numerical value is 6～9g/10min, and ethylene content is 3.6～4.0%.
Embodiment 3
(device load 6t/h): Primary Catalysts (180g/h), triethyl aluminum (1440g/h) and electron donor (180～1440g/h) in contact jar D2201 in advance in about 10 ℃, fully mix the complexing center that forms.The complex compound that from D2201, overflows (6t/h) mixes the back with cold propylene (20 ℃) and gets into prepolymerization reactor R2200 in Z2203 (on-line mixing device); At 20 ℃; 3.4Mpa under the pressure, about reaction 4min, get among the loop polymerization reactor R2201; Simultaneously the hydrogen of ethene (about 116kg/h) and control molecular weight is imported a loop polymerization reactor R2201 together, in a loop polymerization reactor, carry out polyreaction.70 ℃ of service temperatures, pressure 3.4Mpa, a part of propylene carries out polymerization, and the remaining liquid propylene is as the flowing carrier of solid polymer simultaneously, and slurry concentration is controlled at 50-55%wt.The slurry that comes out from R2201, propylene and get into two annular-pipe reactor R2202 from the ethene (116kg/h) and the hydrogen of battery limit (BL).And to be not less than 0.5kg/h from R2202 outlet adding Atmer163.The slurry that two loop polymerization reactor R2202 discharge; Earlier after the flash line of jacket steam heating heats up; Entering pressure is that the flash tank D2301 of 1.8Mpa carries out gas solid separation; Isolated gas enters into propylene washing tower through dynamic separator, and the collected polymkeric substance in flash tank D2301 bottom then under material level control, is discharged to deep bed filter F2301.Polymkeric substance among the F2301 relies on gravity to get in the moving-bed type steamer D2501; D2501 has slow stirrer, and steam gets into D2501 equably by grid distributor with holes, makes progress through steam; Powder is to " convection current " form that moves down; Make the remainder catalyst inactivation, and steam the monomer of powder absorption, thereby improve the quality of products.D2501 working pressure 0.02Mpa, 100～110 ℃ of temperature.Through the closed circuit hot nitrogen recycle system, will in fluidized bed dryer D2502, remove from the moisture content of the polymer surfaces of D2501.
Produce 200 tons of atactic copolymerized polypropene pellets in each batch; 900kg polypropylene powder, oxidation inhibitor 600kg, neutralizing agent 200kg, antiblocking agent 600kg, slipping agent 200kg thorough mixing are delivered to mixer with the polymkeric substance from D2502 through WT-MSR continuously pari passu in the additive tank, deliver to extrusion machine EX2801 again.Send into the homogenizing feed bin then and carry out homogenizing, homogenizing 8 hours gets product.Product melt flow rate(MFR) numerical value is 6～9g/10min, and ethylene content is 3.6～4.0%.
The analytical procedure of each item index in the embodiment of the invention:
1, melt flow rate(MFR) testing method: GB/T 3682
2, ethylene content testing method: Q/SY DS 0240.118-2004
Claims (1)
1. the compound method that polypropylene casting film is resin dedicated is characterized in that: synthetic with home-made s-generation endless tube polypropylene plant; CS-2 catalyzer, triethyl aluminum and electron donor are fully mixed the formation complex compound at 10 ℃ in contact in advance jar, the complex compound that from preparatory contact jar, overflows in the on-line mixing device with entering pre-polymerization reactor after 20 ℃ propylene mixes, at 20 ℃; 3.4Mpa under the pressure, reaction 4min gets into a loop polymerization reactor; Add ethene and hydrogen, a part of propylene carries out polymerization, and polymer concentration is controlled at 50-55wt%; The polymkeric substance that comes out from a loop polymerization reactor, propylene and get into two loop polymerization reactor from ethene, the hydrogen of battery limit (BL); Add oxyethyl group alkyl amine to be not less than 0.5kg/h from the outlet of two loop polymerization reactor simultaneously, one, two endless tube polymeric reaction temperatures are 69-71 ℃, and pressure is 3.3～3.4Mpa; The material that two loop polymerization reactor are discharged; After the flash line of jacket steam heating heated up, entering pressure was that the flash tank of 1.8Mpa carries out gas solid separation earlier, and isolated polymkeric substance gets into steamer through strainer and makes the remainder catalyst inactivation; Steam the monomer of powder absorption, obtain the atactic copolymerized polypropene powder after the drying; In atactic copolymerized polypropene grain weight amount is 100 parts, adds 0.1～0.3 part in oxidation inhibitor, 0.03～0.1 part of neutralizing agent, and 0.1～0.3 part of antiblocking agent, 0.06～0.1 part of slipping agent is sent into the extrusion machine extruding pelletization after the mixing, 150～235 ℃ of prilling temperatures;
CS-2 catalyzer/propylene is 0.02～0.03g/kg; Triethyl aluminum/propylene is 0.14～0.24kg/t, and triethyl aluminum/electron donor is 1～8kg/kg, and density of hydrogen is controlled at 1200～1500ppm; Ethylene/propene is 18～20kg/t; The vapor temperature of steamer is controlled at 100～110 ℃, and the powder melt flow rate(MFR) is controlled at 11～14g/10min, melt flow rate(MFR) testing method: GB/T 3682; The ethylene content of atactic copolymerized polypropene powder is controlled at 3.6～4.0wt%, and one, two loop polymerization reactor density are controlled at 530～580Kg/m
3
Electron donor is cyclohexyl, methyl or dimethoxy silane;
Oxidation inhibitor is composite antioxidant, by antioxidant 1010 and 168 by weight 1: 2 ratio form;
Neutralizing agent is a calcium stearate;
Antiblocking agent be median size at 0.5 μ m, purity is greater than the silicon-dioxide more than 99%;
Slipping agent is an erucamid erucyl amide.
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| CN102827450B (en) * | 2011-06-17 | 2014-04-02 | 中国石油天然气股份有限公司 | Synthesizing method of high-ethylene-content polypropylene injection molding tank special-purposed resin |
| CN102992934A (en) * | 2011-09-17 | 2013-03-27 | 天华化工机械及自动化研究设计院有限公司 | Nitrogen closed-loop cyclic regeneration type propylene dehydration method and device |
| CN109553863B (en) * | 2018-10-09 | 2022-09-09 | 中国石油化工股份有限公司 | Polypropylene material for extrusion and preparation method thereof |
| CN109575171B (en) * | 2018-10-09 | 2022-09-09 | 中国石油化工股份有限公司 | Preparation method of polypropylene cast film resin |
| CN109438834B (en) * | 2018-10-09 | 2022-09-09 | 中国石油化工股份有限公司 | Polypropylene casting film material and preparation method thereof |
| CN109467825B (en) * | 2018-10-09 | 2022-09-09 | 中国石油化工股份有限公司 | Polypropylene material for stretched film and preparation method thereof |
| CN113088004B (en) * | 2021-04-13 | 2023-03-10 | 中国石油化工股份有限公司 | Special radiation-resistant sterilization polypropylene injection molding material and preparation method thereof |
| WO2024025742A1 (en) | 2022-07-25 | 2024-02-01 | Exxonmobil Chemical Patents Inc. | Purged polymer, process and apparatus for production thereof |
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| WO2002072649A1 (en) * | 2001-03-12 | 2002-09-19 | Idemitsu Petrochemical Co., Ltd. | Process for producing polyolefin resin composition and polypropylene composition |
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| WO2002072649A1 (en) * | 2001-03-12 | 2002-09-19 | Idemitsu Petrochemical Co., Ltd. | Process for producing polyolefin resin composition and polypropylene composition |
| CN1737018A (en) * | 2001-06-27 | 2006-02-22 | 北方技术股份有限公司 | Propylene polymer resin with improved properties |
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