CN112457436A - High-melt index polypropylene and preparation method thereof - Google Patents
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Abstract
The invention relates to high-melt index polypropylene and a preparation method thereof. The melt index of the high-melt index polypropylene is 400-2500 g/10min, the isotactic index is 90-98%, the molecular weight distribution Mw/Mn is 4-5.6, the ash content is less than or equal to 0.02 wt%, and the high-melt index polypropylene does not contain phthalate compounds. The high-melt-index polypropylene is a propylene homopolymer or a propylene-comonomer random copolymer containing 0-8 mass% of ethylene or butylene. The high-melt-index polypropylene is prepared by the steps of carrying out catalyst prereduction, prepolymerization and polymerization on a propylene raw material on a ring pipe polypropylene production device in the presence of a polypropylene catalyst, an external electron donor and an activating agent, and then carrying out separation treatment processes of flash evaporation, steaming, filtering and drying. The invention adopts HR catalyst, proper hydrogen concentration and proper T/D ratio, optimizes the polypropylene technological condition, raises the melt index of polypropylene, produces polypropylene product with high melt index, low ash content, and improved shock resistance and toughness.
Description
Technical Field
The invention belongs to the technical field of chemical production, relates to a polypropylene production technology, and particularly relates to high-melt index polypropylene and a preparation method thereof.
Background
High melt index (MFR) polypropylenes are used in a wide variety of applications, such as in the production of meltblown fabrics and in the modification of polypropylene resins. Whether polypropylene can be used in melt blown nonwoven depends primarily on melt index, and polypropylene pellets used to produce melt blown fabrics are required to have very good melt flow.
The prior art for producing high-melt-index polypropylene (MFR: >100g/10min) adopts a method for degrading medium-low melt-index polypropylene by adding a degrading agent peroxide, so that the phenomena of odor and yellowing of products are easily caused in the production process, the performance of the high-melt-index polypropylene produced by the method is unstable (the melt index fluctuation is large), the production and the quality of products are influenced, and the peroxide has the risk of explosion and spontaneous combustion in the storage and production processes.
The melt index of the melt-blown fabric is improved, so that the addition of a degradation agent in the fabric spraying process can be reduced or avoided, and the quality of the melt-blown fabric is improved. The method for preparing the polypropylene with high melt index mainly comprises a hydrogen regulation method and a degradation method, wherein the hydrogen regulation method is used for reducing the molecular weight of the polypropylene by increasing the adding amount of hydrogen in the propylene polymerization process so as to improve the MFR of the polypropylene. The degradation method is that peroxide degradation agent is added after polypropylene powder produced by a polymerization device, MFR of polypropylene is further degraded to be more than 45g/10min, and nucleating agent with proper concentration is added to improve various performance indexes of the product as in the case of hydrogen regulation granulation, but the product quality is not stable in the hydrogen regulation method, and the appearance is easy to appear yellowish and easy to become brittle.
Disclosure of Invention
The invention aims to provide high-melt index polypropylene to improve the melt index of the polypropylene and improve the impact resistance and the toughness of a product, and the invention also aims to provide a preparation method of the high-melt index polypropylene.
The technical scheme of the invention is as follows: the high-melting index polypropylene is 400-2500 g/10min, the isotactic index is 90-98%, the molecular weight distribution Mw/Mn is 4-5.6, the ash content is less than or equal to 0.02 wt%, and the high-melting index polypropylene does not contain phthalate compounds.
The melt index of the polypropylene is preferably 1500-2000 g/10min, and the isotactic index is preferably 92-97%. The high-melting-index polypropylene is a propylene homopolymer or a propylene-comonomer random copolymer containing 0-8 mass% of comonomer. The comonomer is ethylene or butene.
The preparation method of the high-melt index polypropylene comprises the following steps of carrying out catalyst prereduction, prepolymerization and polymerization on a propylene raw material on a ring pipe polypropylene production device in the presence of a polypropylene catalyst, an external electron donor and an activating agent:
mixing a catalyst, an external electron donor and an activating agent in a catalyst pre-reduction tank 6 to perform a catalyst pre-reduction reaction, wherein the pre-reduction reaction temperature is 8-20 ℃, and preferably 10-12 ℃; the adding amount of the catalyst is as follows: the mass ratio of the catalyst to the total feeding amount of propylene in the prepolymerization and polymerization processes is 0.00001-0.000014: 1, and the addition amount of the activating agent is as follows: the mass ratio of the activating agent to the total propylene feed in the prepolymerization and polymerization processes is 0.00016-0.0002: 1, the mass ratio of the activating agent to the external electron donor is 1-2000: 1, preferably 20 to 1000: 1, further selecting 20-80;
overflowing and discharging the material after the pre-reduction of the catalyst from a catalyst pre-reduction tank, mixing the material with propylene in a catalyst on-line mixer, and then feeding the mixture into a prepolymerization reactor for prepolymerization reaction; the prepolymerization is propylene bulk polymerization, wherein in the prepolymerization, the addition of propylene is 1500-3500 kg/h, the reaction temperature is 15-30 ℃, the preference is 18-20 ℃, and the reaction time is 10-15 minutes;
the reaction product in the prepolymerization reactor, fresh propylene and hydrogen enter a tubular polymerization reactor together for polymerization reaction; the prepolymerization is propylene bulk polymerization or propylene-comonomer random copolymerization, and in the polymerization, the addition amount of propylene is as follows: 17000-27000 kg/h (depending on the reaction load), the hydrogen addition was: 3000-20000 mg of hydrogen/kg of propylene (adjusted according to the target melt index), the reaction temperature is 60-75 ℃, preferably 65-70 ℃, the reaction pressure is 3.2-4.1 MPa, and the reaction time is 1-1.5 hours;
and fourthly, separating the reaction product of the polymerization reactor to a separating unit to obtain the high-melt index polypropylene powder.
The catalyst is HR catalyst, the activator is triethyl aluminum or triisobutyl aluminum, and the external electron donor is at least one of cyclohexyl methyl dimethoxy silane, diisopropyl dimethoxy silane, di-n-butyl dimethoxy silane, diisobutyl dimethoxy silane, diphenyl dimethoxy silane, methyl tert-butyl dimethoxy silane, dicyclopentyl dimethoxy silane, cyclohexyl trimethoxy silane, tert-butyl trimethoxy silane and tert-hexyl trimethoxy silane.
In the polymerization process, a comonomer is added to carry out random copolymerization of propylene-comonomer, wherein the comonomer is ethylene or butylene. The addition amount of ethylene is as follows: the mass ratio of ethylene to propylene is 0-4.5: 100, adding the butene in an amount of 0-9 mass ratio of the butene to the propylene: 100.
the separation treatment process comprises flash evaporation, steaming, filtration and drying, and the separation unit comprises a flash evaporation tank, a bag filter, a steam evaporation tank and a dryer. The ring pipe polypropylene production device is a single ring pipe polypropylene production device or a double ring pipe polypropylene production device. The high-melting index polypropylene is used for producing melt-blown cloth or is blended with other polypropylene resin for modifying the polypropylene resin.
The isotactic index of polypropylene is the mass percent of polymer insoluble in boiling n-heptane under specified conditions, and is determined by adopting a heptane extraction method (boiling extraction for 6 hours by heptane), namely 2g of dried polymer sample is placed in an extractor and is extracted for 6 hours by boiling heptane, then the residue is dried to constant weight, and the ratio of the mass (g) of the obtained polymer to 2 is the isotactic index. The melt index of polypropylene is determined according to ASTM D1238-99. Molecular weight distribution of polypropylene: the measurement was carried out by using Shimadzu LC-10AT Gel Permeation Chromatograph (GPC), in which trichlorobenzene was used as a mobile phase and the temperature was 150 ℃. The ash content of polypropylene was determined according to the method of GB/T9345.1-2008.
The high-melt-index polypropylene adopts the HR catalyst, the proper hydrogen concentration and the proper T/D ratio (the ratio of the cocatalyst to the external electron donor), optimizes the process conditions for producing the polypropylene, improves the melt index of the polypropylene, and produces the polypropylene product with high melt index and low ash content. In the polymerization process, the comonomer is added to carry out the random copolymerization of the propylene-comonomer, thereby improving the impact resistance and the toughness of the product. The produced high-melting-index polypropylene is used for producing melt-blown cloth or is blended with other polypropylene resin for modifying the polypropylene resin, so that the application of the product is expanded. The preparation method of the high-melt-index polypropylene of the invention produces the high-melt-index polypropylene through the catalyst pre-reduction, the prepolymerization and the polymerization reaction processes, optimizes the production process of the polypropylene, and adopts a single-ring tube polymerization reactor or a double-ring tube polymerization reactor as a polypropylene production device to increase the production selectivity.
Description of the drawings:
FIG. 1 is a schematic flow diagram of a double-ring pipe polypropylene production apparatus;
FIG. 2 is a schematic flow diagram of a single loop pipe polypropylene production plant;
wherein: 1-catalyst storage tank, 2-activator storage tank, 3-electron donor storage tank, 4-catalyst on-line mixer, 5-prepolymerization reactor, 6-catalyst pre-reduction tank, 7-first loop polymerization reactor, 8-second loop polymerization reactor, 9-flash tank, 10-bag filter, 11-steam tank, 12-dryer.
Detailed Description
The present invention will now be described in detail with reference to the following examples and accompanying drawings. The scope of protection of the invention is not limited to the embodiments, and any modification made by those skilled in the art within the scope defined by the claims also falls within the scope of protection of the invention.
Example 1
The invention relates to a preparation method of high-melt index polypropylene, which is used for producing propylene homopolymerized high-melt index polypropylene and is used as a production raw material of melt-blown cloth. As shown in fig. 1, the double-loop pipe polypropylene production device comprises a catalyst storage tank 1, an activator storage tank 2, an electron donor storage tank 3, a catalyst on-line mixer 4, a prepolymerization reactor 5, a catalyst pre-reduction tank 6, a first loop polymerization reactor 7, a second loop polymerization reactor 8, a flash tank 9, a bag filter 10, a steam distillation tank 11 and a dryer. The prepolymerization reactor is a small single-loop reactor.
The catalyst storage tank 1, the activator storage tank 2 and the electron donor storage tank 3 are connected to a catalyst pre-reduction tank 6, the catalyst pre-reduction tank is connected to a prepolymerization reactor through a catalyst online mixer 4, the prepolymerization reactor is sequentially connected with a first loop polymerization reactor 8 and a second loop polymerization reactor 8, and a reaction material outlet of the second loop polymerization reactor sequentially passes through a flash tank 9, a bag filter 10, a steam distillation tank 11 and is connected to a dryer. The dryer is provided with a propylene powder outlet which is connected to a further refining process. The propylene feed line is connected to the catalyst in-line mixer 4, the first loop polymerization reactor 7 and the second loop polymerization reactor 8, respectively, and the hydrogen line is connected to the first loop polymerization reactor.
The catalyst in the catalyst storage tank 1 is a medium petrochemical catalyst HR catalyst of Beijing Ouda division, the activator in the activator storage tank 2 is triethyl aluminum, and the external electron donor in the electron donor storage tank 3 is cyclohexyl methyl dimethoxy silane. The preparation process of the high-melt index polypropylene comprises the following steps:
mixing a catalyst, an external electron donor and an activating agent in a catalyst pre-reduction tank 6 for pre-reduction reaction, wherein the pre-reduction reaction temperature is 8-20 ℃; the adding amount of the catalyst is as follows: the mass ratio of the catalyst to the total feeding amount of propylene in the prepolymerization and polymerization processes is 0.00001-0.000014: 1, and the addition amount of the activating agent is as follows: the mass ratio of the activating agent to the total propylene feed in the prepolymerization and polymerization processes is 0.00016-0.0002: 1, the mass ratio of the activating agent to the external electron donor is 20-80: 1;
overflowing and discharging the material after the pre-reduction of the catalyst from a catalyst pre-reduction tank 6, mixing the material with propylene in a catalyst on-line mixer 4, and then feeding the mixture into a prepolymerization reactor 5 for prepolymerization reaction; the prepolymerization is propylene bulk polymerization, wherein in the prepolymerization, the addition of propylene is 1500-3500 kg/h, the reaction temperature is 15-30 ℃, the preference is 18-20 ℃, and the reaction time is 10-15 minutes;
the reaction product in the prepolymerization reactor 5, fresh propylene and hydrogen enter a first loop polymerization reactor 7 together for polymerization reaction; the reaction product of the first loop polymerization reactor 7 and fresh propylene enter a second loop polymerization reactor 8 to continue polymerization; the polymerization is bulk polymerization of propylene, and in the polymerization, the adding amount of the propylene is as follows: 17000-27000 kg/h (depending on the reaction load), the hydrogen addition was: 3000-20000 mg hydrogen/kg propylene (adjusted according to the target melt index), the reaction temperature is 60-75 ℃, preferably 65-70 ℃, and the reaction pressure is 3.2-4.1 MPa; the total reaction time of the materials in the first loop polymerization reactor and the second loop polymerization reactor is 1-1.5 hours;
fourth, the reaction product of the second loop polymerization reactor is separated by a flash tank 9, a bag filter 10, a steam evaporation tank 11 and a dryer, and then high-melt index polypropylene is produced and further processed and refined in a refining process. The operating temperature of the steam steaming tank 11 is 110 +/-5 ℃, and the material level of the steam steaming tank is controlled to be 50 +/-5%.
4 batches of production are carried out according to the steps and the process requirements, the data of the process conditions for preparing the high-melt index polypropylene in each batch are shown in tables 1 and 2, and the data of the quality of the polypropylene products in 4 batches are shown in table 3. To show the results, data of the polypropylene products of the prior art are shown in tables 1, 2, 3 for comparison, the catalyst of the comparative example being a DQC catalyst.
TABLE 1 dosage of catalyst, activator and external Electron donor
TABLE 2 Process conditions for the respective reactors
TABLE 3 high melt index Polypropylene Properties
The results in table 3 show that the high-melt index polypropylene prepared by the invention has the characteristics of high melt index and low ash content, and the ultrahigh-melt index polypropylene is directly prepared on a ring pipe polypropylene device through polymerization reaction, so that compared with the prior degradation technology through peroxide, the production cost is reduced, the phenomena that the degradation technology is easy to cause yellowing and odor of products are particularly avoided, and the high-melt index polypropylene can be directly used for producing melt-blown fabric.
Example 2
Another embodiment of the present invention produces a random copolymer of propylene-ethylene monomers with an ethylene to propylene mass ratio of 3: 100. as shown in fig. 2, the device is a single loop polypropylene production device, and comprises a catalyst storage tank 1, an activator storage tank 2, an electron donor storage tank 3, a catalyst on-line mixer 4, a prepolymerization reactor 5, a catalyst pre-reduction tank 6, a first loop polymerization reactor 7, a flash tank 9, a bag filter 10, a steam distillation tank 11 and a dryer. The prepolymerization reactor is a small single-loop reactor.
The catalyst storage tank 1, the activator storage tank 2 and the electron donor storage tank 3 are connected to a catalyst pre-reduction tank 6, the catalyst pre-reduction tank is connected to a prepolymerization reactor through a catalyst online mixer 4, the prepolymerization reactor is sequentially connected with a first loop polymerization reactor 8, and a reaction material outlet of the first loop polymerization reactor sequentially passes through a flash tank 9, a bag filter 10, a steam distillation tank 11 and is connected to a dryer. The dryer is provided with a propylene powder outlet which is connected to a further refining process. The propylene feed line was connected to the catalyst in-line mixer 4 and the first loop polymerization reactor 7, respectively, the hydrogen line was connected to the first loop polymerization reactor, and the ethylene line was connected to the first loop polymerization reactor.
The catalyst in the catalyst storage tank 1 is a medium petrochemical catalyst HR catalyst of Beijing Odada division, the activator in the activator storage tank 2 is triisobutyl aluminum, and the external electron donor in the electron donor storage tank 3 is methyl tert-butyl dimethoxysilane. The preparation process of the high-melt index polypropylene comprises the following steps:
mixing a catalyst, an external electron donor and an activating agent in a catalyst pre-reduction tank 6 for pre-reduction reaction, wherein the pre-reduction reaction temperature is 15 ℃, and the pre-reduction reaction temperature is preferably 12 ℃; the adding amount of the catalyst is as follows: the mass ratio of the catalyst to the total propylene feed during prepolymerization and polymerization was 0.000011:1, the amount of activator added was: the mass ratio of activator to total propylene feed in prepolymerization and polymerization was 0.00018: 1, the mass ratio of the activating agent to the external electron donor is 50: 1;
overflowing and discharging the pre-reduced materials from a catalyst pre-reduction tank 6, mixing the materials with propylene in a catalyst on-line mixer 4, and then feeding the mixture into a prepolymerization reactor 5 for prepolymerization reaction; the prepolymerization is propylene bulk polymerization, wherein in the prepolymerization, the addition of propylene is 2500 kg/h, the reaction temperature is 20 ℃, the preference is 20 ℃, and the reaction time is 15 minutes;
the reaction product in the prepolymerization reactor 5, fresh propylene, ethylene and hydrogen enter a first loop polymerization reactor 7 together for polymerization reaction; the polymerization is propylene-ethylene random copolymerization, and in the polymerization, the addition amount of propylene is as follows: 20000 kg/h, the ethylene addition is: 700 kg/h, hydrogen addition: 3000-20000 mg of hydrogen/kg of propylene (adjusted according to the target melt index), the reaction temperature is 66-68 ℃, and the reaction pressure is 3.9 MPa; the total reaction time of the materials in the first loop polymerization reactor and the second loop polymerization reactor is 1.0 hour;
fourth, the reaction product of the second loop polymerization reactor is separated by a flash tank 9, a bag filter 10, a steam evaporation tank 11 and a dryer, and then high-melt index polypropylene is produced and further processed and refined in a refining process. The operating temperature of the steam steaming tank 11 is 110 +/-5 ℃, and the material level of the steam steaming tank is controlled to be 50 +/-5%.
In the polymerization process, the comonomer is added to carry out the random copolymerization of the propylene-comonomer, thereby improving the impact resistance and the toughness of the product. The produced high-melting-index polypropylene is used for producing melt-blown cloth or is blended with other polypropylene resin for modifying the polypropylene resin, so that the application of the product is expanded.
Claims (10)
1. High melt index polypropylene, which is characterized in that: the melt index of the high-melt index polypropylene is 400-2500 g/10min, the isotactic index is 90-98%, the molecular weight distribution Mw/Mn is 4-5.6, the ash content is less than or equal to 0.02 wt%, and the high-melt index polypropylene does not contain phthalate compounds.
2. The high melt index polypropylene of claim 1, wherein: the melt index is 1500-2000 g/10min, and the isotacticity index is 92-97%.
3. The high melt index polypropylene of claim 1, wherein: the high-melt-index polypropylene is a propylene homopolymer or a propylene-comonomer random copolymer containing 0-8 mass% of comonomer.
4. A high melt index polypropylene according to claim 3, wherein: the comonomer is ethylene or butylene.
5. A process for producing the high melt index polypropylene according to claim 1, wherein: in the presence of a polypropylene catalyst, an external electron donor and an activator, a propylene raw material is subjected to catalyst prereduction, prepolymerization and polymerization reaction on a loop polypropylene production device, and the method specifically comprises the following steps:
mixing a catalyst, an external electron donor and an activating agent in a catalyst pre-reduction tank (6) to perform a catalyst pre-reduction reaction, wherein the pre-reduction reaction temperature is 8-20 ℃, and preferably 10-12 ℃; the addition amount of the catalyst is as follows: the mass ratio of the catalyst to the total feeding amount of propylene in the prepolymerization and polymerization processes is 0.00001-0.000014: 1, and the addition amount of the activating agent is as follows: the mass ratio of the activating agent to the total propylene feed in the prepolymerization and polymerization processes is 0.00016-0.0002: 1, the mass ratio of the activating agent to the external electron donor is 1-2000: 1, preferably 20 to 1000: 1, further selecting 20-80;
overflowing the pre-reduced material of the catalyst from a catalyst pre-reduction tank (6), mixing the material with propylene in a catalyst on-line mixer (4) and then entering a prepolymerization reactor (5) for prepolymerization reaction; in the prepolymerization reaction, the adding amount of propylene is 1500-3500 kg/h, the reaction temperature is 15-30 ℃, the preference is 18-20 ℃, and the reaction time is 10-15 minutes;
the reaction product in the prepolymerization reactor (5) and fresh propylene and hydrogen enter a loop polymerization reactor together for polymerization reaction; in the polymerization reaction, the addition amount of propylene is as follows: 17000 and 27000 kg/h, the adding amount of hydrogen is as follows: 3000-20000 mg of hydrogen/kg of propylene, the reaction temperature is 60-75 ℃, preferably 65-70 ℃, the reaction pressure is 3.2-4.1 MPa, and the reaction time is 1-1.5 hours;
and fourthly, separating the reaction product of the annular polymerization reactor to a separating unit to obtain the high-melt index polypropylene powder.
6. The process for producing high melt index polypropylene according to claim 5, wherein: the catalyst is an HR catalyst, the activator is triethylaluminum or triisobutylaluminum, and the external electron donor is at least one of cyclohexylmethyldimethoxysilane, diisopropyldimethoxysilane, di-n-butyldimethoxysilane, diisobutyldimethoxysilane, diphenyldimethoxysilane, methyl-tert-butyldimethoxysilane, dicyclopentyldimethoxysilane, cyclohexyltrimethoxysilane, tert-butyltrimethoxysilane and tert-hexyltrimethoxysilane.
7. The process for producing high melt index polypropylene according to claim 5, wherein: in the polymerization process, a comonomer is added to carry out random copolymerization of propylene-comonomer, wherein the comonomer is ethylene or butylene.
8. The process for producing high melt index polypropylene according to claim 7, wherein: the addition amount of the ethylene is as follows: the mass ratio of ethylene to propylene is 0-4.5: 100, adding the butene in an amount of 0-9 mass ratio of the butene to the propylene: 100.
9. the process for producing high melt index polypropylene according to claim 5, wherein: the separation process comprises flash evaporation, steaming, filtration and drying, and the separation unit comprises a flash evaporation tank (9), a bag filter (10), a steaming tank (11) and a dryer (12).
10. The process for producing high melt index polypropylene according to claim 5, wherein: the ring pipe polypropylene production device is a single ring pipe polypropylene production device or a double ring pipe polypropylene production device.
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| CN115368855A (en) * | 2021-08-03 | 2022-11-22 | 广州波塞冬材料科技有限公司 | High-temperature-resistant hot melt adhesive for air filter and preparation method thereof |
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Application publication date: 20210309 |