CN106633393A - High-rigidity oxidation-resistant polypropylene synergistically regulated and controlled by molecular sieve/phosphate sodium salt and preparation method thereof - Google Patents
High-rigidity oxidation-resistant polypropylene synergistically regulated and controlled by molecular sieve/phosphate sodium salt and preparation method thereof Download PDFInfo
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- CN106633393A CN106633393A CN201611113687.5A CN201611113687A CN106633393A CN 106633393 A CN106633393 A CN 106633393A CN 201611113687 A CN201611113687 A CN 201611113687A CN 106633393 A CN106633393 A CN 106633393A
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- polypropylene
- molecular sieve
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- oxidation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/04—Ingredients characterised by their shape and organic or inorganic ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/13—Phenols; Phenolates
- C08K5/134—Phenols containing ester groups
- C08K5/1345—Carboxylic esters of phenolcarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses high-rigidity oxidation-resistant polypropylene synergistically regulated and controlled by a molecular sieve/phosphate sodium salt and a preparation method thereof. The high-rigidity oxidation-resistant polypropylene is prepared from the following ingredients in parts by weight: 100 parts of polypropylene, 0.1 to 20 parts of powdery molecular sieves, 0.01 to 1.0 part of nucleating agents, 0.01 to 1.0 part of antioxidants and 0.1 to 5.0 parts of lubricating agents. The preparation method is one of a direct mixing preparation method, a pre-dispersing preparation method and a dipping-absorbing preparation method. A prepared high-rigidity oxidation-resistant polypropylene composite material uses the nucleating agent, so that the rigidity of the polypropylene is effectively improved; the toughness of the polypropylene is stabilized through the molecular sieve; meanwhile, the molecular sieve disperses the oxygen concentration of a polypropylene base body through the adsorption effect of pore passages on oxygen; is, so that the thermal oxidation stability of a polymer material is improved. The high-rigidity oxidation-resistant polypropylene can be widely applied to industries of automobiles, household appliances and the like.
Description
Technical field
The present invention relates to it is a kind of with good rigid, thermo-oxidative stability PP composite material and preparation method thereof,
Specifically related to a kind of high just resistance to oxidation polypropylene and preparation method thereof by molecular sieve/phosphoric acid ester sodium coordinated regulation, belongs to
Polymeric material field.
Background technology
Polypropylene is excellent with good mechanical property, light weight, heat-resisting and easy processing molding etc. as a kind of semi-crystalline polymer
Good characteristic, and its low in raw material price, in recent years its commercial value is growing, has been widely used in automobile making, household electric
Device, articles for daily use and packaging material etc., but because polyacrylic crystallization rate is slow, molding cycle is long, product gloss and the transparency
It is poor so as to which that application is very limited.However, polyacrylic spherocrystal pattern and spherulite size decide its mechanical property and light
Performance is learned, reduces the mechanical property that spherulite size is more beneficial for RPP.In order to overcome the shortcomings of in polyacrylic performance
So as to meet application requirement, it is a kind of effective method to change its mechanical performance using nucleator.
With the α nucleators that 2,2 '-di-2-ethylhexylphosphine oxide (4,6- di-tert-butyl-phenyl) sodium phosphate (NA-40) is representative, Neng Gouyou
Effect ground reduces polyacrylic spherulite size, the stretching of RPP and bending property.But nucleator price is compared to polypropylene
Costliness is a lot, about the 40 of polypropylene price times, and China's polypropylene art is going into second and expands energy peak period, the degree of self-sufficiency
Higher, the problem of product homogeneity undoubtedly which increases polyacrylic cost than more significant so that the market competitiveness significantly under
Drop.Therefore, it is the heat more paid close attention at present to find a kind of new nucleator system of high quality and at a reasonable price and can substitute NA-40 nucleators
Point.
Molecular sieve is a kind of porous material different from other inorganic material, and Jiang etc. has found that molecular sieve can induce poly- third
Alkene generates α spherocrystals, and effectively lifts polyacrylic crystallization temperature.Lv Zhi equalitys have studied variety classes molecular sieve in polypropylene
Nucleating effect, although finding that molecular sieve can promote the lifting of Mechanical Properties of PP, lift amplitude relative to phosphate ester
Sodium salt nucleator is very limited.
Although additionally, phosphoric acid ester sodium can significantly lift polyacrylic rigidity, while polypropylene toughness can be caused
It is decreased obviously.
Further, since containing substantial amounts of tertiary carbon hydrogen in the middle of polypropylene molecule, it is during processing and use due to being subject to
Machinery, heat effect be easy to occur molecule chain break and degrade, it is therefore desirable to add antioxidant ensure its processing and
Stability during use.For high firm polypropylene uses temperature higher due to it, then propose to the stability of antioxidant
Higher requirement, because organic antioxidant thermostability is poor, uses at relatively high temperatures, it is easy to decompose and volatilize,
Not only reduce antioxygen property but also health can be produced potentially hazardous.Therefore, enter while polypropylene rigidity is improved
One step improves its thermo-oxidative stability becomes the key point that high just polypropylene is finally able to apply.
The content of the invention
For the defect of prior art, the present invention is regulated and controled by the synergism of molecular sieve and phosphoric acid ester sodium nucleator
Polyacrylic mechanical performance so as to while ensureing that substantially rigidity is lifted, with good toughness.Solve and use merely phosphorus
Sodium salt nucleator is expensive, and the problem of toughness is had a strong impact on while polypropylene rigidity is improved；And adopting
While improving polypropylene rigidity with molecular sieve and phosphoric acid ester sodium collaboration, polyacrylic oxidation is improved by molecular sieve and is started
Temperature, improves polyacrylic thermo-oxidative stability so that high just polypropylene is possibly realized in the use of wide range of areas.
The invention aims to overcome the above-mentioned deficiency of prior art, and a kind of Gao Gang, the resistance to oxidation poly- third for providing
Alkene material simultaneously provides its preparation method.
Above-mentioned purpose can be achieved through the following technical solutions：
A kind of firm antioxygen polypropylene of height of molecular sieve/phosphoric acid ester sodium coordinated regulation, it is characterised in that the high just oxytolerant
Changing polypropylene includes following component and ratio of weight and number：
Wherein, described polypropylene is melt flow rate (MFR) (test condition：230 DEG C, 2.16Kg) 0.5-20g/min's
Polypropylene,
Described nucleator is phosphoric acid ester sodium α crystalline substance nucleators,
Described molecular sieve is silicon substrate molecular sieve or Si-Al molecular sieve of the particle diameter in 1-10 microns,
The antioxidant includes primary antioxidant and auxiliary antioxidant, and primary antioxidant is hindered phenol antioxygen, auxiliary antioxidant
For phosphite ester,
Described lubricant is the one kind in liquid paraffin, Tissuemat E, stearic acid and its ester.
One kind in the preferred 13X molecular sieves of described molecular sieve, 5A molecular sieves, SBA-15 molecular sieves.
The preferred NA-40 nucleators of described nucleator.
One or several in described primary antioxidant preferred Irgnox1076, Irgnox1010 and Irgnox3114,
Auxiliary antioxidant preferred Irgafos168 or HP-10.
The present invention also provides the described height just polyacrylic preparation method of resistance to oxidation.
A kind of height polyacrylic preparation method of firm antioxygen of molecular sieve/phosphoric acid ester sodium coordinated regulation, it is characterised in that institute
The method of stating is the one kind being directly mixed with method, pre-dispersed preparation method and dipping absorption preparation method.
The described method that is directly mixed with is comprised the following steps：
(1) raw material is weighed according to ratio of weight and number,
(2) by polypropylene, nucleator, molecular sieve, antioxidant and lubricant in 5-10 point of super mixer high speed mixing
Clock,
(3) raw material of mixing is placed in the middle of double screw extruder, melting extrusion, pelletize is carried out at 200-250 DEG C, obtained
To the described firm resistance to oxidation polypropylene of height.
Described dipping absorption preparation method is comprised the following steps：
1) by the ratio of weight and number, first the dissolving of phosphoric acid ester sodium nucleator is configured in organic solvent sodium phosphate
Saline solution, being subsequently adding molecular sieve carries out ultrasonic disperse 2 hours, after solvent is steamed, described organic solvent is methanol, phosphoric acid
The concentration of ester sodium salt solution is 0.02g/ml；
2) and then, in step 1) nucleator and molecular sieve mixture in add antioxidant, lubricant and polypropylene, altogether
Mix 5-10 minutes with super mixer high speed, the raw material for mixing is placed in the middle of double screw extruder, in 200-250
Melting extrusion, pelletize are carried out at DEG C, described height just resistance to oxidation polypropylene is obtained.
Described pre-dispersed preparation method is comprised the following steps：
The phosphoric acid ester sodium nucleator and molecular sieve for weighing respective amount mixes under conditions of 100HZ in the middle of high-speed mixer
10 minutes, then polypropylene, antioxidant and lubricant are mixed into 5-10 minutes in super mixer high speed, the raw material of mixing is put
In the middle of double screw extruder, melting extrusion, pelletize are carried out at 200-250 DEG C, obtain described height just resistance to oxidation polypropylene.
The present invention is ensured on the basis of phosphate ester α crystalline substance nucleator raising polypropylene is rigid by the collaboration of molecular sieve
Polypropylene has enough toughness, and the adsorption by molecular sieve pore passage to oxygen, reduces resin in the middle of compound system and connects
The oxygen concentration of continuous phase, improves the thermo-oxidative stability of compound system so that heat proof material has enough service life.
It is an advantage of the invention that：
1st, the present invention suppresses nucleator to increase the decline of firm Pp System toughness using molecular sieve.
2nd, the present invention is while ensureing that polypropylene has enough rigidity and toughness so as to higher thermal oxidation stability
Property.
The preparation method of the PP composite material that the 3rd, the present invention relates to is simple, low production cost.
Specific embodiment：
With reference to embodiment, the present invention is described in further detail：
Embodiment 1：
It is raw materials used as follows：100 parts of HOPP, melt flow rate (MFR) is 0.5-20g/min (test conditions：230
DEG C, 2.16Kg)；0.04 part of 13X molecular sieves, particle diameter is in 3-4 microns, Shanghai Jiu Zhou Chemical Co., Ltd.s；NA-40 nucleators 0.16
Part, Shanghai Sheng Pan new materials Science and Technology Ltd.；0.05 part of Irganox1010 antioxidant, BASF AG；Irgafos168 is aided in
0.05 part of antioxidant, BASF AG；0.05 part of calcium stearate.
First resin and various additives are mixed into 5-10min in high-speed mixer, then in double screw extruder
Melting extrusion, pelletize are carried out at 220 DEG C.Vacuum drying of the polypropylene particles of pelletize at 100 DEG C will according to the method described above be completed
It is dried in the middle of case 2 hours, then dried particle is carried out on injection machine injection mo(u)lding sample preparation.
Embodiment 2：
Molecular sieve consumption in embodiment 1 is changed to into 0.1 part, nucleator consumption is changed to 0.1 part.Remaining raw material dosage is with real
Apply example 1.
Embodiment 3：
Antioxidant consumption in embodiment 1 is changed to into 0.Remaining raw material dosage is with embodiment 1.
Embodiment 4：
Molecular sieve consumption in embodiment 1 is changed to into 5A molecular sieves, remaining raw material type is with consumption with embodiment 1.Implement
Example 5：
Molecular sieve consumption in embodiment 1 is changed to into SBA-15 molecular sieves, remaining raw material type is with consumption with embodiment 1.
Embodiment 6：
The combination of molecular sieve in the middle of embodiment and nucleator is made into, dipping adsorbs preparation, remaining raw material and consumption
With embodiment 1.
Comparative example 1：
Molecular sieve consumption in embodiment 1 is changed to into 0 part, nucleator consumption is changed to 0.2 part.Remaining raw material dosage is with enforcement
Example 1.
Comparative example 2：
Molecular sieve consumption in embodiment 1 is changed to into 0 part, nucleator consumption is changed to 0 part.The same embodiment of remaining raw material dosage
1。
Comparative example 3
All make the various additives in the middle of embodiment 1 into 0 part.
Sample in above-described embodiment and comparative example is tested according to following：
Tensile property is carried out according to ASTM D638-00, and specimen size is 165 × 12.7 × 3.2, and draw speed is 50mm/
min；Bending property is carried out according to ASTM D790-10, and specimen size is 127 × 12.7 × 3.2, and rate of bending is 1.3mm/
Min, span is 51.2；Impact property is carried out according to ASTM D256, specimen size 64 × 12.7 × 3.2；Heat distortion temperature according to
ASTM D648 are carried out, specimen size 127 × 13 × 3.2, load 0.455MPa, 2 DEG C/min of heating rate；Thermo-oxidative stability is pressed
Carry out according to ASTM E2009-99, take sample 2-3mg as DSC planchets in the middle of, with the speed of 20 DEG C/min in oxygen atmosphere
The temperature that sample produces obvious oxidation Decomposition is warming up to, this temperature is heated and recorded in stopping.Embodiment and property indices
The results are shown in Table 1.
In sum, the purpose of patent of the present invention be in order to overcome the deficiencies in the prior art, and provide a kind of high rigidity,
Heat-resisting, antioxidation PP composite material, it is adopted nucleator to effectively improve polypropylene rigidity, poly- third is stablized by molecular sieve
The toughness of alkene, while adsorption of the molecular sieve passing hole channel to oxygen, disperses the oxygen concentration of polypropylene matrix, so as to improve polymerization
The thermo-oxidative stability of thing material.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
Member, without departing from the inventive concept of the premise, can also make some improvements and modifications, and these improvements and modifications also should be regarded as
In protection scope of the present invention.
Embodiment 1-4 of table 1 and comparative example 1,2 test results
According to table 1, the comparison for never adding the comparative example 3 of any additive and the comparative example 2 of an addition antioxidant is right
According to the addition that can be seen that antioxidant the oxidation induction temperature of material can be caused to improve 12 DEG C, effect is obvious；Simultaneously from contrast
Example 3 and only plus phosphoric acid ester sodium/molecular sieve collaboration system, without the embodiment 3 of antioxidant control can be seen that comprising point
The addition of the collaboration system of son sieve not only can substantially embody polyacrylic rigidity and thermostability, while polyacrylic oxygen can be caused
Change inducing temperature and improve 18 DEG C, exceeded collaboration antioxidant system and stablized polyacrylic inducing temperature.Therefore, molecular sieve and phosphoric acid
Ester sodium salt collaboration is used can be so that PP composite material has good rigid, thermostability and antioxidation.
Claims (8)
1. a kind of just antioxygen polypropylene of the height of molecular sieve/phosphoric acid ester sodium coordinated regulation, it is characterised in that the high just resistance to oxidation
Polypropylene includes following component and ratio of weight and number：
Polypropylene 100
Mealy molecular sieve 0.1-20
Nucleator 0.01-1.0
Antioxidant 0-1.0
Lubricant 0.1-5.0
Wherein, described polypropylene is polypropylene of the melt flow rate (MFR) in 0.5-20g/min,
Described nucleator is phosphate ester α crystalline substance nucleators,
Described mealy molecular sieve is silicon substrate molecular sieve or Si-Al molecular sieve of the particle diameter in 1-10 microns,
The antioxidant includes primary antioxidant and auxiliary antioxidant, and primary antioxidant is hindered phenol antioxygen, and auxiliary antioxidant is Asia
Phosphate ester,
Described lubricant is the one kind in liquid paraffin, Tissuemat E, stearic acid and its ester.
2. a kind of high just antioxygen polypropylene as claimed in claim 1, it is characterised in that described molecular sieve be 13X molecular sieves,
One kind in 5A molecular sieves, SBA-15 molecular sieves.
3. a kind of high just antioxygen polypropylene as claimed in claim 1, it is characterised in that described nucleator is NA-40 nucleation
Agent.
4. a kind of high just antioxygen polypropylene as claimed in claim 1, it is characterised in that described primary antioxidant is
One or several in Irgnox1076, Irgnox1010 and Irgnox3114, auxiliary antioxidant is Irgafos168 or HP-
10。
5. the just polyacrylic preparation side of antioxygen of the height of a kind of molecular sieve as claimed in claim 1/phosphoric acid ester sodium coordinated regulation
Method, it is characterised in that methods described is the one kind being directly mixed with method, pre-dispersed preparation method and dipping absorption preparation method.
6. the just polyacrylic preparation side of antioxygen of the height of a kind of molecular sieve as claimed in claim 5/phosphoric acid ester sodium coordinated regulation
Method, it is characterised in that the described method that is directly mixed with is comprised the following steps：
(1) raw material is weighed according to the ratio of weight and number,
(2) by polypropylene, nucleator, mealy molecular sieve, antioxidant and lubricant in 5-10 point of super mixer high speed mixing
Clock,
(3) raw material of mixing is placed in the middle of double screw extruder, melting extrusion, pelletize is carried out at 200-250 DEG C, obtain institute
The firm resistance to oxidation polypropylene of height stated.
7. the just polyacrylic preparation side of antioxygen of the height of a kind of molecular sieve as claimed in claim 5/phosphoric acid ester sodium coordinated regulation
Method, it is characterised in that described dipping absorption preparation method is comprised the following steps：
1) by the ratio of weight and number, first the dissolving of phosphoric acid ester sodium nucleator is configured in organic solvent phosphoric acid ester sodium molten
Liquid, being subsequently adding molecular sieve carries out ultrasonic disperse 2 hours, after solvent is steamed, described organic solvent is methanol, sodium phosphate
The concentration of saline solution is 0.02g/ml；
2) and then, in step 1) nucleator and molecular sieve mixture in add antioxidant, lubricant and polypropylene, exist jointly
Super mixer high speed mixes 5-10 minutes, the raw material for mixing is placed in the middle of double screw extruder, at 200-250 DEG C
Melting extrusion, pelletize are carried out, described height just resistance to oxidation polypropylene is obtained.
8. the just polyacrylic preparation side of antioxygen of the height of a kind of molecular sieve as claimed in claim 5/phosphoric acid ester sodium coordinated regulation
Method, it is characterised in that described pre-dispersion method is：
According to the ratio of weight and number, phosphoric acid ester sodium nucleator and molecular sieve are first weighed, the 100HZ in the middle of high-speed mixer
Under the conditions of mix 10 minutes, then polypropylene, antioxidant and lubricant are mixed into 5-10 minutes in super mixer high speed, will be mixed
The raw material of conjunction is placed in the middle of double screw extruder, and melting extrusion, pelletize are carried out at 200-250 DEG C, obtains described height just resistance to
Its chlorinated polypropylene.
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| CN201611113687.5A CN106633393A (en) | 2016-12-07 | 2016-12-07 | High-rigidity oxidation-resistant polypropylene synergistically regulated and controlled by molecular sieve/phosphate sodium salt and preparation method thereof |
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| CN201611113687.5A CN106633393A (en) | 2016-12-07 | 2016-12-07 | High-rigidity oxidation-resistant polypropylene synergistically regulated and controlled by molecular sieve/phosphate sodium salt and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107163378A (en) * | 2017-05-22 | 2017-09-15 | 华东理工大学 | Phosphate/molecular sieve is self-assembled into application of the nuclear system in high just polypropylene preparation |
| CN109535545A (en) * | 2018-10-22 | 2019-03-29 | 山东京博石油化工有限公司 | A kind of novel high just polypropylene modified material and preparation method thereof |
| CN111393749A (en) * | 2020-04-30 | 2020-07-10 | 宁夏大学 | Polypropylene composite material and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558812A (en) * | 2013-10-10 | 2015-04-29 | 中国石油化工股份有限公司 | Ternary composite nucleating agent and its application in preparation of reinforced polypropylene |
-
2016
- 2016-12-07 CN CN201611113687.5A patent/CN106633393A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104558812A (en) * | 2013-10-10 | 2015-04-29 | 中国石油化工股份有限公司 | Ternary composite nucleating agent and its application in preparation of reinforced polypropylene |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107163378A (en) * | 2017-05-22 | 2017-09-15 | 华东理工大学 | Phosphate/molecular sieve is self-assembled into application of the nuclear system in high just polypropylene preparation |
| CN109535545A (en) * | 2018-10-22 | 2019-03-29 | 山东京博石油化工有限公司 | A kind of novel high just polypropylene modified material and preparation method thereof |
| CN111393749A (en) * | 2020-04-30 | 2020-07-10 | 宁夏大学 | Polypropylene composite material and preparation method thereof |
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Application publication date: 20170510 |