CN102590034A - Measurement method of polypropylene powder melt index - Google Patents
Measurement method of polypropylene powder melt index Download PDFInfo
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- CN102590034A CN102590034A CN201210016893XA CN201210016893A CN102590034A CN 102590034 A CN102590034 A CN 102590034A CN 201210016893X A CN201210016893X A CN 201210016893XA CN 201210016893 A CN201210016893 A CN 201210016893A CN 102590034 A CN102590034 A CN 102590034A
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- 239000004743 Polypropylene Substances 0.000 title claims abstract description 72
- -1 polypropylene Polymers 0.000 title claims abstract description 72
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 72
- 239000000843 powder Substances 0.000 title claims abstract description 72
- 238000000691 measurement method Methods 0.000 title abstract 2
- 238000003756 stirring Methods 0.000 claims abstract description 39
- 239000002904 solvent Substances 0.000 claims abstract description 32
- 239000000203 mixture Substances 0.000 claims abstract description 25
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 24
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 23
- 235000006708 antioxidants Nutrition 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000002671 adjuvant Substances 0.000 claims description 63
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 45
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 24
- 238000012360 testing method Methods 0.000 claims description 24
- 238000002844 melting Methods 0.000 claims description 20
- 230000008018 melting Effects 0.000 claims description 20
- FGHOOJSIEHYJFQ-UHFFFAOYSA-N (2,4-ditert-butylphenyl) dihydrogen phosphite Chemical compound CC(C)(C)C1=CC=C(OP(O)O)C(C(C)(C)C)=C1 FGHOOJSIEHYJFQ-UHFFFAOYSA-N 0.000 claims description 16
- 238000003556 assay Methods 0.000 claims description 16
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical group [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 11
- 239000003381 stabilizer Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 abstract description 14
- 238000002156 mixing Methods 0.000 abstract description 12
- 239000000654 additive Substances 0.000 abstract description 5
- 230000000996 additive effect Effects 0.000 abstract description 5
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- 238000005259 measurement Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 11
- 235000019441 ethanol Nutrition 0.000 description 9
- 238000002203 pretreatment Methods 0.000 description 8
- 238000001291 vacuum drying Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 3
- ZTHYODDOHIVTJV-UHFFFAOYSA-N Propyl gallate Chemical compound CCCOC(=O)C1=CC(O)=C(O)C(O)=C1 ZTHYODDOHIVTJV-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
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- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000010525 oxidative degradation reaction Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- SPSPIUSUWPLVKD-UHFFFAOYSA-N 2,3-dibutyl-6-methylphenol Chemical compound CCCCC1=CC=C(C)C(O)=C1CCCC SPSPIUSUWPLVKD-UHFFFAOYSA-N 0.000 description 1
- YXGOYRIWPLGGKN-UHFFFAOYSA-N 2,3-ditert-butylbenzene-1,4-diol Chemical compound CC(C)(C)C1=C(O)C=CC(O)=C1C(C)(C)C YXGOYRIWPLGGKN-UHFFFAOYSA-N 0.000 description 1
- 239000004255 Butylated hydroxyanisole Substances 0.000 description 1
- 206010023126 Jaundice Diseases 0.000 description 1
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
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- CZBZUDVBLSSABA-UHFFFAOYSA-N butylated hydroxyanisole Chemical compound COC1=CC=C(O)C(C(C)(C)C)=C1.COC1=CC=C(O)C=C1C(C)(C)C CZBZUDVBLSSABA-UHFFFAOYSA-N 0.000 description 1
- 229940043253 butylated hydroxyanisole Drugs 0.000 description 1
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Abstract
The invention discloses a measurement method of polypropylene powder melt index, comprising the following steps of: dissolving an additive and polypropylene powder in a solvent according to the proportion so as to form a mixture A; stirring the mixture A to evaporate the solvent, so as to form a mixture B; drying the mixture B, so as to form a sample to be measured; and measuring the sample by using a melt index instrument. The technical scheme of the invention fully plays the anti-oxidant role, so as to prevent the polypropylene powder from being oxidized, the operation of the mixing process is convenient and during the measurement process using the melt index instrument, the data reproducibility and data parallelism are relatively good.
Description
Technical field
The present invention relates to the polypropylene production field, in particular to the assay method of polypropylene powder melting index.
Background technology
Melting index is a melt flow rate, is meant to use special-purpose determining instrument, and under certain temperature and pressure load, molten mass passed through the amount of a standard die orifice in ten minutes.Melting index is directly related with the mean molecular weight of polymkeric substance, and the big more melting index of molecular weight is more little, otherwise the more little melting index of molecular weight is big more.Melting index is general as the first association index of dividing the high molecular polymer trade mark, also is an important indicator of the concrete purposes of decision high molecular polymer.Therefore, measure melting index exactly quality in kind and the practical use of judging had crucial meaning.
For a long time; The mensuration of polypropylene powder melting index is a very complicated problems always; Maximum problem is that polypropylene powder is very unstable under hot conditions, is easy to take place chemical reaction, and the consequence that causes is exactly that collimation is very poor as a result for the mensuration of melting index; Therefore when measuring the melting index of melt, in sample, add suitable anti-oxidant; Sample is carried out stabilization processes, in the mensuration process, can oxidizedly not degrade, just can measure the melting index of polypropylene powder sample to guarantee sample.But; In most polypropylene powder melt index determination tests, take directly to add adjuvant; Manually shake up in the process and to exist owing to shake a bottle angle difference, shake a bottle dynamics difference, mixing time is different; The equal reason of operating personnel's technical skill and make adjuvant and test powder fail abundant mixing, thus the inaccurate problem of melt index determination result caused.
The polypropylene powder melting index is to instruct the most important index of explained hereafter; Therefore easy, the needs accurately of seeking that a kind of assay method can satisfy that polypropylene is measured in the suitability for industrialized production; Can solve polypropylene powder again and at high temperature be prone to oxidation to cause measuring the result inaccurate, and the uneven problem of the mixing of adjuvant and polypropylene powder is imperative.
Summary of the invention
The present invention aims to provide a kind of method of measuring the polypropylene powder melting index, and polypropylene powder at high temperature is prone to oxidation in the prior art to solve, and anti-oxidant mixes inhomogeneous with powder, make the result's problem devious of measuring.
To achieve these goals, according to an aspect of the present invention, a kind of assay method of polypropylene powder melting index is provided, has may further comprise the steps: 1) adjuvant and polypropylene powder have been dissolved in the solvent in proportion, form potpourri A; 2) A that stirs the mixture makes solvent evaporates, forms potpourri B; 3) potpourri B is dry, form testing sample; 4) and utilize the molten appearance that refers to that testing sample is measured.
Further, above-mentioned steps 1) comprising: adjuvant is added in the solvent, carry out the first time and stir, dissolve fully to adjuvant, form mixture C; Polypropylene powder is joined in the mixture C, carry out the second time and stir, form potpourri A.
Further, the above-mentioned stirring second time comprises: a. stirred 20～40 seconds along clockwise direction; B. along counterclockwise stirring 20～40 seconds; And c. repeating step a and step b20～40 time.
Further, above-mentioned steps 3) further comprise: at 120～130 ℃, drying is 10～20 minutes under the vacuum condition with said mixture B.
Further, the concentration of adjuvant is that every liter of solvent contains 17.5～25 gram adjuvants among the said mixture C.
Further, above-mentioned solvent is absolute ethyl alcohol, isopropyl alcohol, methyl alcohol, acetone.
Further, the mass ratio of adjuvant and polypropylene powder is an adjuvant among the said mixture A: polypropylene powder=2.5～3.5: 150～250.
Further, above-mentioned adjuvant comprises main anti-oxidant, helps anti-oxidant and stabilizing agent.
Further, above-mentioned main anti-oxidant is three [2.4-di-tert-butyl-phenyl] phosphite ester, and helping anti-oxidant is 1,3,5-trimethyl-2,4, and 6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene, stabilizing agent is a zinc paste.
Further, the molar ratio of each component is three [2.4-di-tert-butyl-phenyl] phosphite ester in the above-mentioned adjuvant: 1,3, and 5-trimethyl-2,4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene: zinc paste=1.5～2.5: 1～3: 0.5～1.5.
The technique effect that the present invention reached is: the effect that technical scheme of the present invention is given full play to anti-oxidant makes polypropylene powder not oxidized, and mixed process is easy and simple to handle, and when testing with molten finger appearance, data repeatability and collimation are better.
Except top described purpose, feature and advantage, the present invention also has other purpose, feature and advantage.To do further detailed explanation to the present invention with reference to embodiment below.
Embodiment
To carry out detailed explanation to the technical scheme in the embodiments of the invention below, but following embodiment only is in order to understanding the present invention, and can not limits the present invention, the multitude of different ways that the present invention can be defined by the claims and cover is implemented.
In a kind of typical embodiment of the present invention, the assay method of polypropylene powder melting index may further comprise the steps: 1) adjuvant and polypropylene powder are dissolved in the solvent in proportion, form potpourri A; 2) stir said mixture A, make solvent evaporates, form potpourri B; 3) said mixture B is dry, form testing sample; 4) utilize the molten appearance that refers to that testing sample is measured.
The present invention makes the two disperse more even at liquid environment through adopting dissolution with solvents adjuvant and polypropylene powder; And, make contacting of adjuvant and polypropylene powder more abundant through stirring, promote mixed effect; Simultaneously; Stirring impels solvent to quicken volatilization; Thereby obtain comprising the potpourri B of adjuvant and polypropylene powder; Adjuvant and polypropylene powder are more even compared to the prior art mixing among the potpourri B, utilize this moment the molten appearance that refers to that this polypropylene powder melting index is tested, and can access and measure the result more accurately.
Preferably, in the assay method of above-mentioned polypropylene powder melting index, step 1) further comprises, adjuvant is added in the solvent, carries out the first time and stirs, and dissolves fully to adjuvant, forms mixture C; Polypropylene powder is joined among the said mixture C, carry out the second time and stir, form said mixture A.In this mode, with adjuvant and polypropylene powder in order, successively join in the solvent, promoting adjuvant and the diffusion area of polypropylene powder in solvent, and then make adjuvant and polypropylene powder mixing more even.Particularly, earlier adjuvant is joined in the solvent, through stirring adjuvant is uniformly dispersed in solvent, the mixture C of formation; Then, in mixture C, add polypropylene powder, at this moment; Mixture C is a fluent meterial; Wherein adjuvant has been in a liquid state and has been dispersed in the solvent, is the equal of that polypropylene powder is put in the fluent meterial, and through stirring it is dispersed in this fluent meterial.This mode has increased the contact area of adjuvant and polypropylene powder, has avoided local adjuvant to assemble and has caused polypropylene powder and adjuvant to mix the appearance of uneven problem.
The present invention is when stirring for the second time, and concrete grammar is that a. stirred 20～40 seconds along clockwise direction; B. along counterclockwise stirring 20～40 seconds; And c. repeating said steps a and said step b20～40 time.Stir the mixing that not only helps adjuvant and powder repeatedly through different directions, and quickened the volatilization of solvent, shorten the time that polypropylene powder exposes in air, avoid in mixed process powder oxidized.
The condition that the present invention is dry with said mixture B is: 100～150 ℃, vacuum condition was dried 10～30 minutes down.Potpourri B placed vacuum environment is dry had both avoided sample oxidized under the high temperature of dry run, can accelerate the volatilization of moisture among the potpourri B and adjuvant again, use to reach the requirement of instrument short as far as possible drying time testing sample humidity.Preferably, baking temperature is 120～130 ℃, vacuum condition dry 10～20 minutes down.
Among the present invention in the mixture C concentration of adjuvant be every liter of solvent contain 17.5～25 the gram adjuvants.The concentration of adjuvant is in this scope in the control mixture C, both guaranteed that solvent adjuvant and polypropylene powder before volatilization fully mixed, and can too much not cause unnecessary waste because of solvent again, mix and the prolongation of drying time.
Organic solvent used in the present invention includes but not limited to absolute ethyl alcohol, isopropyl alcohol, amylalcohol, methyl alcohol, acetone, wherein preferably uses absolute ethyl alcohol, isopropyl alcohol, methyl alcohol, acetone.This be because employed organic solvent be can solubilising additive and also not with the volatile organic solvent of additive reaction; The organic solvent of solubilized adjuvant has guaranteed that adjuvant evenly disperses in solvent; The chemical inertness of organic solvent and adjuvant can not destroyed the original performance of adjuvant, and the effumability of organic solvent makes the married operation step simply again can be in testing sample not residual to measuring the result or instrument exerts an influence.Take all factors into consideration the factor of technique effect, solvent cost and toxicity size, further preferred absolute ethyl alcohol, isopropyl alcohol are solvent of the present invention.
The present invention selects the mass ratio of adjuvant and polypropylene powder to be: adjuvant: polypropylene powder=2.5～3.5: 150～250; In this scope, make the performance of polypropylene material not receive the influence of adjuvant can keep higher antioxygenic property and stability again; Can be because of adjuvant; For example the addition of three [2.4-di-tert-butyl-phenyl] phosphite ester too much makes the jaundice of polypropylene material, and also can polypropylene material fragility not increased because of addition influences testing result.Take all factors into consideration practical operation condition, testing cost and adjuvant to the polypropylene powder Effect on Performance, the mass ratio of adjuvant and polypropylene powder further is preferably: adjuvant: polypropylene powder=3: 200.
Adjuvant of the present invention comprises main anti-oxidant, helps anti-oxidant and stabilizing agent.Wherein can be used for anti-oxidant of the present invention and include but not limited to butylated hydroxy anisole, three [2.4-di-tert-butyl-phenyl] phosphite ester, dibutyl hydroxy toluene, n-propyl gallate, ditert-butylhydro quinone, 1,3,5-trimethyl-2; 4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene; Wherein main anti-oxidant preferably uses three [2.4-di-tert-butyl-phenyl] phosphite ester, helps anti-oxidant preferably to use 1,3; 5-trimethyl-2,4,6-three (3; The 5-di-tert-butyl-4-hydroxyl benzyl) benzene can be used for stabilizing agent of the present invention but is not limited to lead salt, mixed metal salt, organotin, zinc paste, wherein preferably uses zinc paste.Adopt above-mentioned main anti-oxidant in the present invention, help anti-oxidant and stabilizing agent, primary antioxidant can be caught the active free radical that produces in the oxidative degradation, thereby interrupts the chain type degradation reaction, reaches anti-oxidant purpose.Auxiliary antioxidant can be decomposed into the intermediate product of oxidative degradation the non-free radical product.Stabilizing agent has that to stop plastics that degradation takes place because of being heated common, main and auxiliary antioxidant with and stabilizing agent and usefulness, reach best antioxidant effect through mutual cooperative effect.
More specifically, the molar ratio of each component is in the adjuvant of the present invention: three [2.4-di-tert-butyl-phenyl] phosphite ester: 1,3, and 5-trimethyl-2; 4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene: zinc paste=1.5～2.5: 1～3: 0.5～1.5; Each component ratio of adjuvant further is preferably: three [2.4-di-tert-butyl-phenyl] phosphite ester: 1,3, and 5-trimethyl-2; 4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene: zinc paste=2: 2: 1.Select the ratio of the adjuvant of suitable this explained hereafter according to explained hereafter.
Below will combine embodiment 1-6 and Comparative Examples 1 to further specify the beneficial effect of polypropylene powder melt index determination method of the present invention.
The instrument that in the embodiment of the invention and Comparative Examples, adopts is: CEAST 21844
The testing standard of selecting for use is: ISOBp, and concrete parameter is set to: test temperature: 230 ℃, mouthful mould internal diameter: 2.095mm; Mouth mould height: 8.00mm, preheating time: 240s, beginning height: 50.00mm; Measuring height: 30.00mm, measure quantity: 8, weighing load: 2.16kg.
Comparative Examples 1
According to traditional disposal route polypropylene powder is carried out pre-treatment: get 1.200 gram three [2.4-di-tert-butyl-phenyl] phosphite esters, 1.200 grams 1,3 respectively, 5-trimethyl-2; 4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene and 0.0600 gram zinc paste are in surface plate; After stirring 3 minutes with stirring rod; To wherein adding the 20g trade mark is that the polypropylene powder of L5E89 continue to stir 5 minutes, then this potpourri is inserted vacuum drying chamber, and drying is 15 minutes under 125 ℃ of following vacuum states.The gained sample is a comparative sample 1.
According to the molten preceding inspection of starting shooting successively of appearance working specification, start, the instrument self checking of referring to; Set testing standard, the instrument auto-programming is warming up to design temperature, treats to carry out application of sample by instrument prompting and standard-required behind the temperature stabilization; Sample add and compacting after insert the piston rod have flag, should guarantee that the scale mark on the piston rod is higher than the adiabatic table top of instrument, is put in the working position with displacement transducer and counterweight frame this moment; Press " START " key and begin experiment, measurement finishes, the automatic display result of instrument.Test result is seen table 1.
Embodiment 1
Polypropylene powder is carried out pre-treatment: get 1.200 gram three [2.4-di-tert-butyl-phenyl] phosphite esters, 1.200 grams 1 respectively; 3,5-trimethyl-2,4; 6-three (3; The 5-di-tert-butyl-4-hydroxyl benzyl) benzene, 0.0600 gram zinc paste and the 20g trade mark be the polypropylene powder of L5E89 in the surface plate that fills 15ml ethanol, stirred along clockwise direction 30 seconds, then along counterclockwise stirring 30 seconds; Repeat behind the aforesaid operations 30 times this potpourri to be inserted vacuum drying chamber, drying is 15 minutes under 125 ℃ of following vacuum states.The gained sample is a sample 1.
The molten operation that refers to appearance operation repetition Comparative Examples 1.Test result is seen table 1.
Embodiment 2
Polypropylene powder is carried out pre-treatment: get 0.1200 gram three [2.4-di-tert-butyl-phenyl] phosphite ester, 0.1200 gram 1,3 respectively, 5-trimethyl-2; 4, in 6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene and 10 milliliters the ethanol of 0.0600 gram zinc paste in surface plate; Obtain the solution of adjuvant and ethanol mixing after 60 seconds with the stirring rod stirring; To wherein adding the polypropylene powder that the 20g trade mark is L5E89, stirred along clockwise direction 30 seconds, then along counterclockwise stirring 30 seconds; Repeat behind the aforesaid operations 25 times this potpourri to be inserted vacuum drying chamber, drying is 15 minutes under 125 ℃ of following vacuum states.The gained sample is a sample 2.
The molten operation that refers to appearance operation repetition Comparative Examples 1.Test result is seen table 1.
Embodiment 3
Polypropylene powder is carried out pre-treatment: get 0.1200 gram three [2.4-di-tert-butyl-phenyl] phosphite ester, 0.1200 gram 1,3 respectively, 5-trimethyl-2; 4, in 6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene and 10 milliliters the isopropyl alcohol of 0.0600 gram zinc paste in surface plate; Obtain the solution of adjuvant and isopropyl alcohol mixing after 40 seconds with the stirring rod stirring; To wherein adding the polypropylene powder that the 15g trade mark is L5E89, stirred along clockwise direction 20 seconds, then along counterclockwise stirring 20 seconds; Repeat behind the aforesaid operations 40 times this potpourri to be inserted vacuum drying chamber, drying is 15 minutes under 125 ℃ of following vacuum states.The gained sample is a sample 3.
The molten operation that refers to appearance operation repetition Comparative Examples 1.Test result is seen table 1.
Embodiment 4
Polypropylene powder is carried out pre-treatment: get 0.1250 gram three [2.4-di-tert-butyl-phenyl] phosphite ester, 0.0833 gram 1,3 respectively, 5-trimethyl-2; 4, in 6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene and 15 milliliters the ethanol of 0.0417 gram zinc paste in surface plate; Obtain the solution of adjuvant and ethanol mixing after 40 seconds with the stirring rod stirring; To wherein adding the polypropylene powder that the 15g trade mark is L5E89, stirred along clockwise direction 40 seconds, then along counterclockwise stirring 40 seconds; Repeat behind the aforesaid operations 20 times this potpourri to be inserted vacuum drying chamber, drying is 20 minutes under 120 ℃ of following vacuum states.The gained sample is a sample 4.
The molten operation that refers to appearance operation repetition Comparative Examples 1.Test result is seen table 1.
Embodiment 5
Polypropylene powder is carried out pre-treatment: get 0.1200 gram three [2.4-di-tert-butyl-phenyl] phosphite ester, 0.1200 gram 1 respectively; 3,5-trimethyl-2,4; 6-three (3; The 5-di-tert-butyl-4-hydroxyl benzyl) in benzene and 0.0600 gram 10 milliliters the ethanol of zinc paste in surface plate, stirs the solution that obtains adjuvant and ethanol mixing after 60 seconds with stirring rod, to wherein adding the polypropylene powder that the 20g trade mark is L5E89; A direction stirred after 5 minutes inserts vacuum drying chamber with this potpourri, and drying is 20 minutes under 125 ℃ of following vacuum states.The gained sample is a sample 5.
The molten operation that refers to appearance operation repetition Comparative Examples 1.Test result is seen table 1.
Embodiment 6
Polypropylene powder is carried out pre-treatment: get 0.1250 gram three [2.4-di-tert-butyl-phenyl] phosphite ester, 0.1500 gram 1,3 respectively, 5-trimethyl-2; 4; In 6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene and 20 milliliters the ethanol of 0.0750 gram zinc paste in surface plate, obtain homogeneous solution after 90 seconds with the stirring rod stirring; To wherein adding the 25g trade mark is that the polypropylene powder of L5E89 stirred 40 seconds along clockwise direction; Then along counterclockwise stirring 40 seconds, repeat behind the aforesaid operations 30 times this potpourri to be inserted vacuum drying chamber, drying is 10 minutes under 130 ℃ of following vacuum states.The gained sample is a sample 6.
The molten operation that refers to appearance operation repetition Comparative Examples 1.Test result is seen table 1.
The test result of Comparative Examples 1 and embodiment 1-6 is seen table 1.
Table 1
Can know from the data analysis of table 1: with ethanol and isopropyl alcohol is that solvent carries out pre-treatment to polypropylene powder; The standard deviation of the polyacrylic melt index determination value that obtains is between 0.0025 and 0.0046; The standard deviation of the polyacrylic melt index determination value that traditional pre-treating method that directly additive package is mixed with polypropylene powder obtains is 0.0098; This standard deviation is obviously greater than the standard deviation that obtains through the present techniques scheme; The repeatability and the collimation that show the mensuration result that the technical scheme of utilizing the application obtains have all reached higher level, measure the result comparatively accurately and reliably.
Can find out from above description; The above embodiments of the present invention have realized following technique effect: proportionally be dissolved in additive package and polypropylene powder in the solvent; Make the abundant mixing of adjuvant and powder; And then with molten its melting index of appearance mensuration that refers to, data repeatability and collimation are better.
The above is merely the preferred embodiments of the present invention, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.All within spirit of the present invention and principle, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the assay method of a polypropylene powder melting index is characterized in that, may further comprise the steps:
1) adjuvant and polypropylene powder are dissolved in the solvent in proportion, form potpourri A;
2) stir said potpourri A, make said solvent evaporates, form potpourri B;
3) said potpourri B is dry, form testing sample; And
4) utilize the molten appearance that refers to that said testing sample is measured.
2. assay method according to claim 1 is characterized in that, said step 1) further comprises:
Said adjuvant is added in the said solvent, carry out the first time and stir, extremely said adjuvant dissolves fully, forms mixture C;
Said polypropylene powder is joined in the said mixture C, carry out the second time and stir, form said potpourri A.
3. assay method according to claim 2 is characterized in that, stirs the said second time further to comprise:
A. stirred along clockwise direction 20～40 seconds;
B. along counterclockwise stirring 20～40 seconds; And
C. repeating said steps a and said step b20～40 time make said solvent evaporates.
4. assay method according to claim 1 is characterized in that, said step 3) further comprises:
At 120～130 ℃, drying is 10～20 minutes under the vacuum condition with said potpourri B.
5. assay method according to claim 2 is characterized in that, the concentration of adjuvant described in the said mixture C is that every liter of said solvent contains the said adjuvant of 17.5～25 grams.
6. assay method according to claim 5 is characterized in that, said solvent is an absolute ethyl alcohol, isopropyl alcohol, methyl alcohol, acetone.
7. according to each described assay method among the claim 1-4, it is characterized in that the mass ratio of adjuvant and polypropylene powder is an adjuvant among the said potpourri A: polypropylene powder=2.5～3.5: 150～250.
8. assay method according to claim 1 is characterized in that, said adjuvant comprises main anti-oxidant, helps anti-oxidant and stabilizing agent.
9. assay method according to claim 8 is characterized in that, said main anti-oxidant is three [2.4-di-tert-butyl-phenyl] phosphite ester, and the said anti-oxidant that helps is 1; 3,5-trimethyl-2,4; 6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene, said stabilizing agent is a zinc paste.
10. assay method according to claim 9; It is characterized in that the molar ratio of each component is three [2.4-di-tert-butyl-phenyl] phosphite ester in the said adjuvant: 1,3; 5-trimethyl-2; 4,6-three (3, the 5-di-tert-butyl-4-hydroxyl benzyl) benzene: zinc paste=1.5～2.5: 1～3: 0.5～1.5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105067658A (en) * | 2015-08-12 | 2015-11-18 | 上海天洋热熔粘接材料股份有限公司 | Method for evaluating melting rate of hot-melt adhesive |
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| JPS5682820A (en) * | 1979-12-10 | 1981-07-06 | Tokuyama Soda Co Ltd | Adhesion of additive to polypropylene powder and granule |
| CN1394223A (en) * | 2000-11-02 | 2003-01-29 | 旭电化工业株式会社 | Granular composite additive for polyolefin, process for producing the same, and polyolefin composition containing the same |
| JP2008201976A (en) * | 2007-02-22 | 2008-09-04 | Sumitomo Chemical Co Ltd | Method for stabilization of polyolefin powder |
| CN101597398A (en) * | 2008-06-05 | 2009-12-09 | 中国石化上海石油化工股份有限公司 | A kind of preparation method who makes the acrylic resin of high-transparency and high-rigidity cigarette packaging film |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5682820A (en) * | 1979-12-10 | 1981-07-06 | Tokuyama Soda Co Ltd | Adhesion of additive to polypropylene powder and granule |
| CN1394223A (en) * | 2000-11-02 | 2003-01-29 | 旭电化工业株式会社 | Granular composite additive for polyolefin, process for producing the same, and polyolefin composition containing the same |
| JP2008201976A (en) * | 2007-02-22 | 2008-09-04 | Sumitomo Chemical Co Ltd | Method for stabilization of polyolefin powder |
| CN101597398A (en) * | 2008-06-05 | 2009-12-09 | 中国石化上海石油化工股份有限公司 | A kind of preparation method who makes the acrylic resin of high-transparency and high-rigidity cigarette packaging film |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105067658A (en) * | 2015-08-12 | 2015-11-18 | 上海天洋热熔粘接材料股份有限公司 | Method for evaluating melting rate of hot-melt adhesive |
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