CN112409681B - Polypropylene composition and preparation method thereof - Google Patents
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- 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
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- 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
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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Abstract
The invention belongs to the field of polyolefin materials, and particularly relates to a polypropylene composition and a preparation method thereof. The polypropylene composition is prepared by taking two or more polypropylenes as basic resin, adding an antioxidant, an acid-absorbing agent, a lubricant, a nucleating agent, a processing aid and the like, uniformly mixing the materials by a high-speed mixer, and then extruding and granulating the materials by a double screw to obtain the polypropylene composition. The polypropylene composition has two obvious polypropylene melting peaks of beta crystal and alpha crystal, wherein the beta crystal phase pair content is more than 75%; the polypropylene composition has excellent mechanical property and good heat resistance, and is mainly applied to the fields of trenchless power cables, communication cable conduits, other drainage pipes and the like; the preparation method is scientific, reasonable, simple and feasible.
Description
Technical Field
The invention belongs to the field of polyolefin materials, and particularly relates to a polypropylene composition and a preparation method thereof.
Background
With the improvement of the national city construction level and the acceleration of the urbanization process, the underground laying of power cables and communication cables is more and more, and the demand of plastic conduits serving as protection cables is more and more. Since the influence of construction on urban facilities, road traffic, normal life of people and the like is considered to be reduced or reduced as much as possible, the trenchless engineering technology becomes a main mode, and therefore higher requirements are put forward on the performance of the cable conduit for trenchless use. At present, the raw material of the plastic conduit for the trenchless power cable and the communication cable is mainly modified polypropylene. The modified polypropylene pipe can be welded by hot melting, the welding joint has high strength, high temperature resistance, high rigidity and good toughness, can drag the pipe by ultra-long traction force, has the advantages of excellent stratum settlement resistance, shock resistance and the like, and has the long-term use temperature of-5 ℃ to 70 ℃. The modified polypropylene pipe overcomes the defect that a Polyethylene (PE) pipe cannot resist high temperature, and the mechanical property of the PE pipe is greatly reduced after the temperature is over 40 ℃, so that the modified polypropylene pipe cannot be used for a conduit of a power cable and a communication cable; meanwhile, the modified polypropylene pipe overcomes the defects of poor stratum sedimentation resistance and incapability of construction at high traction of a chlorinated polyvinyl chloride (CPVC) pipe.
However, in the prior art, the polypropylene used is usually a wiredrawing grade homopolypropylene (such as T30S), a random copolymer polypropylene (PPR pipe material) for common cold and hot water pipes, or an injection molding grade impact copolymer polypropylene (such as K8003 or EPS 30R), the polypropylene has low strength or heat resistance, and the modification means adopted in general is that inorganic components such as calcium carbonate and glass fiber are added into the polypropylene to improve the rigidity, and components such as elastomer toughening agent or polyethylene component are added to improve the impact toughness, and often, components such as a coupling agent or a functional graft and the like are required to be added to improve the compatibility of the system, therefore, the preparation process is very complicated, the comprehensive physical property index of the obtained modified polypropylene material is difficult to meet the performance index requirement of the cable conduit at the same time, and the problems of insufficient heat resistance, low elongation at break, low strength and the like generally exist. Because the variety of the modified components is more, the process is complex, the quality stability is difficult to ensure, and because the components used by various modification manufacturers are different and the cost is controlled, the performance of the modified polypropylene material is different, and the market is more disordered.
Disclosure of Invention
The invention aims to provide a polypropylene composition which does not contain inorganic filler and has excellent and stable performance, the composition has good comprehensive performance and good heat resistance, and can meet the application field of trenchless cable ducts; the invention also provides a preparation method of the composition, which is scientific, reasonable, simple and feasible.
The polypropylene composition is prepared by taking two or more polypropylenes as basic resin, adding an antioxidant, an acid-absorbing agent, a lubricant, a nucleating agent, a processing aid and the like, uniformly mixing the materials by a high-speed mixer, and then extruding and granulating the materials by a double screw to obtain the polypropylene composition.
The polypropylene composition is prepared from the following raw materials in percentage by mass:
wherein the weight sum of the homo-polypropylene or the random copolymerization polypropylene and the impact copolymerization polypropylene is 100 percent, and the dosage of other additives is calculated by the mass percent of the sum of the total weight of the polypropylene.
The melt mass flow rate MFR of the homo-polypropylene or the random co-polypropylene is 0.2-1.0g/10min, and the MFR test condition is 230 ℃ and 2.16 kg; the weight average relative molecular weight of the homo-polypropylene or random copolymer polypropylene measured by GPC method was 50X 10 4 ～90×10 4 Number average molecular weight of 8X 10 4 ～14×10 4 Z average molecular weight of 240X 10 4 ～380×10 4 (ii) a Wherein, the comonomer of the random copolymerization polypropylene is ethylene, and the mass percentage content of the ethylene is less than 0.1 percent; the melting point of the homopolymerized polypropylene is 164-169 ℃, and the melting point of the random copolymerization polypropylene is 155-160 ℃.
The impact copolymer polypropylene is an impact copolymer of propylene and ethylene, the melt mass flow rate MFR of the impact copolymer polypropylene is 0.2-0.8g/10min, and the MFR test condition is 230 ℃ and 2.16 kg; weight average relative molecular weight by GPC method was 60X 10 4 ～90×10 4 Number average molecular weight of 9X 10 4 ～14×10 4 Z average molecular weight of 260X 10 4 ～400×10 4 (ii) a In the impact-resistant copolymerized polypropylene, the mass percentage of ethylene is 2.0-5.0%; the melting point of the impact-resistant co-polypropylene is 163-168 ℃.
Preferably, the homopolymerized polypropylene is polypropylene QPH01 produced by Qilu branch petrochemical China or polypropylene B1101 produced by Yanshan branch petrochemical China; the random copolymer polypropylene is polypropylene PPH2101 or PPH4201 produced by China petrochemical Yanshan division company; the impact copolymer polypropylene adopts polypropylene QPB08 produced by Chinese petrochemical Qilu division company or polypropylene B6101 produced by Chinese petrochemical Yanshan division company.
The melting point of polypropylene is closely related to the Vicat softening point, and the melting points of the three types of polypropylene are higher, which is the root for ensuring that the polypropylene composition obtained by the invention has better heat resistance.
The antioxidant is a phenolic antioxidant and a phosphate antioxidant in a mass ratio of 1: 1, wherein the phenolic antioxidant adopts one or more of 3- (3, 5-bi-tert-butyl-4-hydroxycyclohexyl) propionate (1010), 1,3,5, tri (3, 5-di-tert-butyl, 4-hydroxybenzyl) s-triazine, 2,4,6- (1H,3H,5H) trione (3114) or 3,3,3,5,5, 5-hexa-tert-butyl-a, a, a- (1,3, 5-trimethylbenzene-2, 4, 6-triyl) tri-p-cresol (1330), and the phenolic antioxidant is preferably antioxidant 1010; the phosphate antioxidant is one or more of tris (2, 4-di-tert-butylphenyl) phosphite (168), bis (2, 4-di-tert-butylphenol) pentaerythritol diphosphite (622) or bis (2, 6-di-tert-butyl-4-methylphenyl) pentaerythritol diphosphite (PEP36), and the phosphate antioxidant is preferably the antioxidant 168.
The acid absorbent is one of stearic acid, calcium stearate or zinc stearate, and the addition amount is preferably 0.04-0.08%.
The lubricant is fatty acid ester, and the glycerol monostearate is adopted in the invention, so that the component has good lubricating effect and antistatic effect, and the problems of dust absorption, electrostatic discharge and the like of a formed product are solved.
The nucleating agent is a beta crystal form nucleating agent, and the beta-nucleating agent is one of substituted aromatic amide and substituted benzamide, rare earth nucleating agent or organic metal salt nucleating agent.
The processing aid is a fluorine-containing polymer, and can effectively improve the processing performance of the polymer. The processing aid is selected from FX9613 and FX5911 of 3M company or DA910 and DA-310ST of Japan Dajin company.
The preparation method of the polypropylene composition comprises the following steps:
(1) mixing materials: placing the raw materials in a high-speed stirrer, stirring for 3-5min at the rotating speed of 1000-1500 r/min, and uniformly mixing;
(2) and (3) extruding and granulating: adding the uniformly mixed materials into a co-rotating double-screw extruder for melting and mixing, and extruding and granulating to obtain a product; wherein the highest section temperature of the extruder is 190-230 ℃, the rotating speed of the extruder main machine is 150-230 r/min, and the feeding rotating speed is 30-50 r/min.
The invention has the following beneficial effects:
1. the polypropylene composition obtained by the invention has two obvious polypropylene melting peaks which are a beta crystal form melting peak at the temperature of 147-153 ℃ and an alpha crystal form melting peak at the temperature of 164-167 ℃, wherein the beta crystal phase pair content is more than 75%.
2. The polypropylene composition does not contain inorganic filler, has excellent mechanical property and good heat resistance, has the tensile strength of 32-35 MPa, the fracture nominal strain of more than 410 percent and the notch impact strength of a normal-temperature simple supported beam of 100kJ/m 2 The material has the bending modulus of 1200MPa, the bending strength of 30MPa, the load thermal deformation temperature of 100-105 ℃ and the Vicat softening temperature of 151-157 ℃, and can be applied to the fields of trenchless power cables, communication cable plastic conduits, drainage pipes and the like.
3. The preparation method provided by the invention is scientific, reasonable, simple and feasible.
Drawings
FIG. 1 is a graph showing the melting profile of the polypropylene composition obtained according to the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which are not intended to limit the practice of the invention.
Example 1
73 parts of homopolymerized polypropylene (MFR is 0.24g/10min), 27 parts of impact-resistant copolymerized polypropylene (MFR is 0.40g/10min), 0.2 part of antioxidant, 0.05 part of acid acceptor, 0.06 part of lubricant, 0.05 part of aromatic amide beta nucleating agent and 0.08 part of processing aid.
Wherein the homopolymerized polypropylene is polypropylene QPH01 produced by Chinese petrochemical Qilu division company; the impact copolymer polypropylene adopts polypropylene B6101 produced by China petrochemical Yanshan division. The antioxidant is 1010 and 168 produced by BASF corporation; the acid absorbent is commercially available calcium stearate; the lubricant was commercially available glycerol monostearate and the processing aid was FX5911 from 3M.
The preparation method comprises the following steps:
(1) mixing materials: placing the raw materials in a high-speed stirrer, stirring at 1500r/min for 3min, and mixing well;
(2) and (3) extruding and granulating: adding the uniformly mixed materials into a co-rotating double-screw extruder for melting and mixing, and extruding and granulating to obtain a product; wherein the highest section temperature of the extruder is 230 ℃, the rotating speed of the extruder host is 230r/min, and the feeding rotating speed is 40 r/min.
Example 2
65 portions of random copolymerized polypropylene (MFR is 0.35g/10min, the content of ethylene is 0.6 percent), 35 portions of impact-resistant copolymerized polypropylene (MFR is 0.35g/10min), 0.2 portion of antioxidant, 0.05 portion of acid absorbent, 0.06 portion of lubricant, 0.06 portion of organic acid metal salt beta nucleating agent NAB-82 and 0.06 portion of processing aid.
Wherein, the polypropylene random copolymer is polypropylene PPH4201 produced by China petrochemical Yanshan division company; the impact copolymer polypropylene adopts polypropylene QPB08 produced by Chinese petrochemical Qilu division. The antioxidant adopts 1010 and 168 produced by BASF corporation; the acid absorbent is commercially available calcium stearate; the lubricant was commercially available glycerol monostearate and the processing aid was FX5911 from 3M.
The preparation method is the same as that of example 1.
Example 3
55 parts of homopolymerized polypropylene (MFR is 0.22g/10min), 45 parts of impact-resistant copolymerized polypropylene (MFR is 0.35g/10min), 0.2 part of antioxidant, 0.05 part of acid acceptor, 0.06 part of lubricant, 0.08 part of rare earth organic complex type beta nucleating agent WBG-II and 0.08 part of processing aid.
Wherein the homopolymerized polypropylene is polypropylene B1101 produced by China petrochemical Yanshan division company; the impact copolymer polypropylene adopts polypropylene QPB08 produced by Chinese petrochemical Qilu division. The antioxidant adopts 1010 and 168 produced by BASF corporation; the acid absorbent is commercially available calcium stearate; the lubricant was commercially available glycerol monostearate and the processing aid was FX5911 from 3M.
The preparation method is the same as that of example 1.
Comparative example 1
30 parts of homopolymerized polypropylene (the trade name is T30S, the MFR is 3.0g/10min), 52 parts of impact-resistant copolymerized polypropylene (the trade name is K8003, and the MFR is 2.4g/10min), 3 parts of linear low-density polyethylene (the trade name is 7042, the MFR is 2.0g/10min under the conditions of 190 ℃ and 2.16 kg), 15 parts of activated calcium carbonate, 0.3 part of antioxidant, 0.05 part of alpha-reinforcing nucleating agent, 0.05 part of acid absorbent, 0.07 part of lubricant and 0.06 part of processing aid.
Wherein, the antioxidant adopts 1010 and 168 sold in the market, the alpha stiffening nucleating agent is a product sold in the market, the acid absorbent is calcium stearate sold in the market, the active calcium carbonate is a product sold in the market with the grain diameter of 2000 meshes, the talcum powder is a product sold in the market with the grain diameter of 1250 meshes, the lubricant is glycerol monostearate sold in the market, and the processing aid is fluorine-containing polymer sold in the market.
The preparation method is the same as that of example 1.
Comparative example 2
70 parts of random copolymer polypropylene (the mark is 4220, and the MFR is 0.26g/10min), 20 parts of impact copolymer polypropylene (the mark is K8003, and the MFR is 2.4g/10min), 10 parts of talcum powder, 0.2 part of antioxidant, 0.08 part of alpha-stiffening nucleating agent, 0.05 part of acid acceptor, 0.06 part of lubricant, and 0.08 part of processing aid.
Wherein, the antioxidant adopts 1010 and 168 sold in the market, the alpha stiffening nucleating agent is a product sold in the market, the acid absorbent is calcium stearate sold in the market, the active calcium carbonate is a product sold in the market with the grain diameter of 2000 meshes, the talcum powder is a product sold in the market with the grain diameter of 1250 meshes, the lubricant is glycerol monostearate sold in the market, and the processing aid is fluorine-containing polymer sold in the market.
The preparation method is the same as that of example 1.
The results of the physical property tests of the polypropylene modified materials prepared in the examples and the comparative examples are shown in Table 1, and the results of the physical property tests of the pipes prepared from the modified materials obtained in the examples 1 and the comparative examples 1 are shown in Table 2.
TABLE 1 results of performance test of examples and comparative examples
TABLE 2 results of the performance tests of the pipes (specification DS 100X 6mm) prepared in example 1 and comparative example 1
The test method is characterized by comprising the following steps of:
Melt Mass Flow Rate (MFR): proceeding according to GB/T3682-2000;
the impact strength of the gap of the simply supported beam is tested according to GB/T1043-;
the tensile property is tested according to GB/T1040.2-2006;
the bending performance is tested according to GB/T9341-;
the load deflection temperature was tested in accordance with GB/T1634.2-2004.
The Vicat softening temperature GB/T1633-2000 test.
Claims (6)
1. A process for the preparation of a polypropylene composition, characterized in that: the polypropylene composition is prepared from the following raw materials in percentage by mass:
wherein the weight sum of the homo-polypropylene or the random copolymerization polypropylene and the impact copolymerization polypropylene is 100 percent, and the dosage of other additives is calculated by the mass percentage of the sum of the total weight of the polypropylene;
the melting point of the homopolymerized polypropylene is 164-169 ℃; the melting point of the random copolymerization polypropylene is 155-160 ℃;
the melting point of the impact-resistant co-polypropylene is 163-168 ℃;
the melt mass flow rate MFR of the homo-polypropylene or the random co-polypropylene is 0.2-1.0g/10min, and the MFR test condition is 230 ℃ and 2.16 kg; the weight average relative molecular weight of the homo-polypropylene or random copolymer polypropylene measured by GPC method was 50X 10 4 ～90×10 4 Number average molecular weight of 8X 10 4 ～14×10 4 Z average molecular weight of 240X 10 4 ～380×10 4 (ii) a Wherein, the comonomer of the random copolymerization polypropylene is ethylene, and the mass percentage content of the ethylene is 0.6 percent;
the impact copolymer polypropylene is an impact copolymer of propylene and ethylene, the melt mass flow rate MFR of the copolymer is 0.2-0.8g/10min, and the MFR test condition is 230 ℃ and 2.16 kg; weight average relative molecular weight by GPC method was 60X 10 4 ～90×10 4 Number average molecular weight of 9X 10 4 ～14×10 4 Z average molecular weight of 260X 10 4 ～400×10 4 (ii) a In the impact-resistant copolymerized polypropylene, the mass percentage of ethylene is 2.0-5.0%;
the nucleating agent is a beta crystal form nucleating agent;
the preparation method of the polypropylene composition comprises the following steps:
(1) mixing materials: placing the raw materials in a high-speed stirrer, stirring for 3-5min at the rotating speed of 1000-1500 r/min, and uniformly mixing;
(2) and (3) extruding and granulating: adding the uniformly mixed materials into a co-rotating double-screw extruder for melting and mixing, and extruding and granulating to obtain a product; wherein the highest section temperature of the extruder is 190-230 ℃, the rotating speed of the extruder main machine is 150-230 r/min, and the feeding rotating speed is 30-50 r/min.
2. The method for preparing a polypropylene composition according to claim 1, wherein: the antioxidant is a phenolic antioxidant and a phosphate antioxidant in a mass ratio of 1: 1 mixed formulation.
3. The method for preparing a polypropylene composition according to claim 2, wherein: the phenolic antioxidant is one or more of antioxidant 1010, antioxidant 3114 or antioxidant 1330; the phosphate antioxidant is one or more of antioxidant 168, antioxidant 622 or antioxidant PEP 36.
4. The method for preparing a polypropylene composition according to claim 1, wherein: the acid absorbent is one of stearic acid, calcium stearate or zinc stearate.
5. The method for preparing a polypropylene composition according to claim 1, wherein: the lubricant is glycerol monostearate.
6. The method for preparing a polypropylene composition according to claim 1, wherein: the processing aid is one of FX9613, FX5911, DA910 or DA-310 ST.
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| EP1364986A1 (en) * | 2002-05-21 | 2003-11-26 | Borealis Technology Oy | Polypropylene compositions especially for pipes |
| CN101698729B (en) * | 2009-10-27 | 2012-12-05 | 中国石油化工股份有限公司 | Polypropylene composition for chemical pipelines and preparation method thereof |
| CN102952329B (en) * | 2011-08-30 | 2015-07-15 | 中国石油化工股份有限公司 | Polypropylene composition and preparation method thereof |
| CN102558683B (en) * | 2011-12-31 | 2014-01-22 | 广州呈和科技有限公司 | Polypropylene beta crystal form nucleating agent composition and application thereof |
| CN103665587B (en) * | 2012-09-21 | 2016-03-30 | 中国石油化工股份有限公司 | A kind of polypropene composition and polypropylene granules and preparation method thereof and polypropylene pressure pipeline |
| CN104327369B (en) * | 2013-07-22 | 2017-06-23 | 中国石油化工股份有限公司 | A kind of polypropene composition and polypropylene granules |
| CN104558859B (en) * | 2013-10-28 | 2017-03-08 | 中国石油化工股份有限公司 | Polypropene composition and preparation method thereof and tubing prepared therefrom |
| CN107540953B (en) * | 2016-06-28 | 2020-04-14 | 中国石油化工股份有限公司 | Polypropylene resin composition for medical syringe and preparation method thereof |
| CN106893204A (en) * | 2016-07-17 | 2017-06-27 | 佛山瑞箭体育器材有限公司 | A kind of high rigidity polypropene composition |
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| CN108976589B (en) * | 2017-05-31 | 2021-03-02 | 中国石油化工股份有限公司 | Polypropylene toughening master batch and preparation method thereof |
| CN109486031A (en) * | 2018-10-09 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of rigidity-toughness balanced high-transparency polypropylene composition |
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