CN1300237C - Ethylene copolymer particle - Google Patents

Ethylene copolymer particle Download PDF

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Publication number
CN1300237C
CN1300237C CNB2004100072059A CN200410007205A CN1300237C CN 1300237 C CN1300237 C CN 1300237C CN B2004100072059 A CNB2004100072059 A CN B2004100072059A CN 200410007205 A CN200410007205 A CN 200410007205A CN 1300237 C CN1300237 C CN 1300237C
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Prior art keywords
ethylene
ethylene copolymer
particle
lubricant
unsaturated fatty
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Expired - Fee Related
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CNB2004100072059A
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CN1530394A (en
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坂野博英
雪冈聪
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Tosoh Corp
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Tosoh Corp
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B4/00—Separating solids from solids by subjecting their mixture to gas currents
    • B07B4/02—Separating solids from solids by subjecting their mixture to gas currents while the mixtures fall
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B13/00—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices
    • B07B13/08—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices according to weight
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B13/00—Grading or sorting solid materials by dry methods, not otherwise provided for; Sorting articles otherwise than by indirectly controlled devices
    • B07B13/14—Details or accessories
    • B07B13/16—Feed or discharge arrangements
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B07—SEPARATING SOLIDS FROM SOLIDS; SORTING
    • B07B—SEPARATING SOLIDS FROM SOLIDS BY SIEVING, SCREENING, SIFTING OR BY USING GAS CURRENTS; SEPARATING BY OTHER DRY METHODS APPLICABLE TO BULK MATERIAL, e.g. LOOSE ARTICLES FIT TO BE HANDLED LIKE BULK MATERIAL
    • B07B9/00—Combinations of apparatus for screening or sifting or for separating solids from solids using gas currents; General arrangement of plant, e.g. flow sheets
    • B07B9/02—Combinations of similar or different apparatus for separating solids from solids using gas currents

Abstract

Ethylene copolymer pellets having improved unsusceptibility to blocking are provided. The ethylene copolymer pellets comprising a mixture of: (a) 100 parts by weight of an ethylene copolymer; (b) 0.01-0.5 part by weight of an unsaturated fatty acid bisamide having a melting point of 100-180 DEG C; and (c) 0.01-0.5 part by weight of a lubricant having a melting point of 60-90 DEG C, which, when used in combination with ingredient (b), lowers the melting point of ingredient (b) by at least 20 DEG C.

Description

Ethylene copolymer pellets
The present invention relates to a kind of ethylene copolymer pellets that particle fusion bonding (hereinafter being referred to as " particle bond ") is had the insensitivity of raising.
Ethylene copolymer pellets, promptly ethylene/vinyl acetate copolymer (after this being abbreviated as " EVA ") is in processes such as particle manufacture or follow-up storage, transportation, because their high viscosity can be strengthened luming each other.Another problem of particle is the flowability owing to their extreme differences, and particle manufacture and package handling need a large amount of work.In processes such as over a long time storage, transportation, a lot of difficulties have been run into.Technology as these problems of elimination has proposed various particle disposal methods up to now.
Stop the method for particle caking to comprise: wherein use inorganic substance, for example, and talcum or silicon-dioxide, tiny polyolefin particles, polyethylene wax or their dispersion are coated to the method for particle surface; With with itself and higher fatty acid or salt, N, N '-ethylenebisoleoamide, N, N '-ethylenebis erucicamide, N, N '-two oil base adipimides or N, N '-two savoy adipimide phase blended methods.But these diverse ways all have many problems.
For example, inorganic substance for example talcum or silicon-dioxide mix with EVA and adhere under the situation on the EVA, essentially add a large amount of inorganic substance to obtain mobility of particle.But the use of this a large amount of inorganic substance can produce a problem, promptly because it is very poor with the consistency of EVA, therefore understands the performance of havoc the finished product.
The problem that has with the method for the water-based slurry coated polymer particles of tiny polyolefin particles is, because the tiny dispersed extreme difference of polyolefin particles in water-based system, be unsuitable on particle and adhere to, therefore this technology can not reach the level (referring to for example, No. 3528841 United States Patent (USP)) that viscosity is reduced to substantially the flowability of satisfaction guaranted.
In the coating EVA particulate examples such as dispersion that with polyethylene wax or with the polyethylene wax are main component,, can not obtain the flowability of actual needs though this method can be eliminated viscosity to a certain extent effectively.Another problem of this method is that when the particle after applying melted, melting thing was lactous.Because these problems, using according to the particulate through applying of this technology is limited (referring to for example, the 5667029A Japanese Patent).
In addition, apply under the situation of high viscosity ethylene polymer particles in dispersion with low viscosity EVA, the problem that exists is the coated particle that can not obtain to eliminate viscosity in fact and have satisfied flowability, this is low because of the fusing point of the EVA that is used as coating material, although this relevant with the vinyl acetate content in the coating material (referring to for example 4832939A Japanese Patent).
The someone proposes a kind of method (referring to for example 56136374A Japanese Patent) and a kind of N of being selected from of fusion that mixes higher fatty acid or its salt, N '-ethylenebisoleoamide, N, N '-ethylenebis erucicamide, N, N '-two oil base adipimides or N, the method for the additive of N '-two savoy adipimides (referring to for example 57200434A Japanese Patent).But the shortcoming of these methods is the bleed speed deficiencies owing to additive, therefore stops the weak effect of particle initial stage caking.
Therefore, an object of the present invention is to provide a kind of ethylene copolymer pellets that the particle caking is had the insensitivity of raising.
The present inventor has carried out the investigation of concentrating at these problems.As a result, find by adding the caking that specific lubricant can reduce ethylene copolymer pellets to ethylene copolymer.Finished the present invention based on this discovery.
The present invention relates to comprise the ethylene copolymer pellets of following mixture:
(a) ethylene copolymer of 100 weight parts;
(b) fusing point of 0.01-0.5 weight part is 100-180 ℃ a unsaturated fatty acids bisamide; With
(c) fusing point of 0.01-0.5 weight part is 60-90 ℃ a lubricant, and when itself and composition (b) when being used in combination, and this lubricant reduces at least 20 ℃ of the fusing points of composition (b).
To explain the present invention in detail below.
The ethylene copolymer (a) that uses among the present invention is not particularly limited, the example comprises the polymkeric substance that is called ethylene copolymer, ethylene/alpha for example, beta-unsaturated carboxylic acid ester copolymer, ethylene/vinyl base ester copolymer, ethylene/vinyl base ester/α, beta-unsaturated carboxylic acid ester terpolymer, and ethylene/alpha-olefin copolymer.The object lesson of ethylene copolymer comprises ethene/Methane Carboxylic Acid ester copolymer, ethene/ethyl propylene acid ester copolymer, ethylene/methacrylic acid methyl terpolymer, ethylene/methacrylic acid ethyl ester multipolymer, ethene/butene-1 copolymer, ethene/1-hexene copolymer, ethene/1-octene copolymer, ethene/4 methyl 1 pentene copolymer, ethylene/propylene copolymer rubber, ethylene/propylene/diene copolymer rubber and ethylene/butylene copolymers rubber.Wherein, the preferred use has the ethylene/vinyl acetate copolymer of low softening point.
Its vinyl acetate content (VAc) of measuring according to JIS K6924-1 (1997) be 27-50wt%, and to satisfy the ethylene/vinyl acetate copolymer of following relationship formula more preferred according to the body flow rate (MFR) of melting of JIS K6924-1 (1997) measurement.
MFR＞431.98×(VAc) -0.7731
Therefore, the ethylene/vinyl acetate copolymer that preferably has easy caking trend (that is, having high VAc content and high MFR).
The fusing point of the unsaturated fatty acids bisamide (b) that uses among the present invention is 100-180 ℃.The example of unsaturated fatty acids bisamide (b) comprises ethylenebisstearamide, ethylenebisoleoamide, ethylenebis erucicamide and ethylenebis laurylamide.Wherein, from considering more preferably to use ethylenebisoleoamide with the consistency and the bleed angle of ethylene copolymer.
In the ethylene copolymer (a) of per 100 weight parts, the consumption of unsaturated fatty acids bisamide (b) is the 0.01-0.5 weight part, preferred 0.05-0.2 weight part.When the consumption of unsaturated fatty acids bisamide (b) during less than 0.01 weight part, particulate agglomeration resistance weak effect.On the other hand, when its consumption surpassed 0.5 weight part, As time goes on unsaturated fatty acids bisamide (b) was exuded to the surface in a large number, and this causes for example problem of cohesive strength reduction.
Be used for lubricant of the present invention (c) and be not particularly limited, if it to be fusing point be 60-90 ℃ lubricant and when with unsaturated fatty acids bisamide (b) when being used in combination, at least 20 ℃ of the fusing points of this lubricant reduction unsaturated fatty acids bisamide (b).The example of lubricant (c) comprises lipid acid and fatty amide.When the fusing point of lubricant (c) is lower than 60 ℃, particulate agglomeration resistance weak effect.On the other hand, when its fusing point surpasses 90 ℃, particulate initial stage agglomeration resistance weak effect.The object lesson of lubricant (c) comprises saturated fatty acid for example stearic acid, palmitinic acid Huo docosoic, and the unsaturated fatty acids acid amides is erucicamide or oleylamide for example.These compounds may be used singly or in combin.In the lubricant, the unsaturated fatty acids acid amides that preferred use is moved to the surface rapidly and had good anti-caking performance more preferably uses the erucicamide that improves unsaturated fatty acids bisamide (b) bleed performance.
In the ethylene copolymer (a) of per 100 weight parts, the consumption of lubricant (c) is the 0.01-0.5 weight part, is preferably the 0.05-0.2 weight part.When the amount of lubricant (c) during less than 0.01 weight part, particulate agglomeration resistance weak effect.On the other hand, when its amount surpassed 0.5 weight part, As time goes on lubricant was exuded to the surface in a large number, caused for example problem of cohesive strength reduction.
Consider that from the bleed angle of unsaturated fatty acids bisamide (b) unsaturated fatty acids bisamide (b) is preferably 70/30-30/70 with the weight ratio (b)/(c) of lubricant (c).
The method that is used to add lubricant (c) among the present invention is not particularly limited, and any suitable method all can be used for obtaining particle.The example of method comprises: wherein composition is to carry out melt with extrusion machine, Banbury mixer, kneader etc. to mix the method for pinching; Wherein use for example method of the lubricant covering particle surface of dispersion form; Wherein lubricant and particle are done the method for mixing.Preferably mix the method for pinching and obtain particle, because they have good insensitivity to caking by melt.
From anti-stick effect, mobile equal angles, preferably has the surface roughness Ra of the about 1.0-2.5 μ m that measures according to JIS B0601 (1994) according to ethylene polymer particles of the present invention.The method of the coarse surface that can use in the present invention is, for example, through cutting, for example the particle that obtains of cutting, twisted wire cutting or hot cutting under water is by with the transport pipe with recess and projection of dot matrix arranged in patterns (nurling) or with the method for the transport pipe transmission with recess and projection of annular style arrangement (repetition).
Surface roughness Ra value of the present invention is to obtain by color laser microscope VK-8500 (being made by Keyence).
If desired or necessary, ethylene copolymer pellets of the present invention can comprise dyestuff, pigment, antioxidant, lubricant, protective agent, antisticking agent, various stablizer, mineral filler etc.
To describe the present invention in detail with reference to the following example and comparative example, but these examples are not construed as limiting to the present invention.
In the following example and the comparative example, carry out benchmark test according to following method.
(1) particle caking test
To mix the 100g ethylene copolymer pellets pinch acquisition by fusion, to place internal capacity be that 60 * 60 * 60 test sample is produced case.Place the load of 68.6N on it, this case kept 48 hours down at 30 ℃, kept 24 hours down at 23 ℃ then.Exert pressure with the measurement required overall loading of breaking to the test sample that obtains with the speed of 10mm/min.Then, the ethylene copolymer pellets that kept 1 month is carried out identical test under 23 ℃ of normal atmosphere.The test block that cake strength is lower than 490N is labeled as " good ", and those cake strength are 490N or are higher than then being labeled as of 490N " poor ".Test-results is shown in table 2.
(2) measurement of fusing point reduction
Measure the DSC curve of unsaturated fatty acids bisamide (b), the temperature that is equivalent to the summit of peak melting point side on the curve is called Tm1.The melt of measuring unsaturated fatty acids bisamide (b) and lubricant (c) mixes the DSC curve of pinching mixture, and the temperature that is equivalent to the summit of peak melting point side on the curve is called Tm2.Difference between Tm1 and the Tm2 is fusing point and reduces.This test the results are shown in table 2.
Embodiment 1
According to the prescription shown in the table 1, MFR is that 400g/10min, VAc content are that the ethylene/vinyl acetate copolymer (Ultrathene (Nipoflex) 0B54B, by Tosoh company produce) of 100 weight parts of 33wt% is carried out melt with the erucicamide of the ethylenebisoleoamide of 0.1 weight part and 0.1 weight part and mixed and pinch.Water cutting down cuts the mixture that makes such acquisition.The particle surface that alligatoring obtains.Having obtained surface roughness like this is the particle of 1.6 μ m.The particle that obtains is carried out the cake strength evaluation.The fusing point of ethylenebisoleoamide, Tm1 are 120 ℃, and the fusing point of erucicamide is 82 ℃.The fusing point of ethylenebisoleoamide and erucicamide 50/50 (wt%) mixture, Tm2 is 75 ℃.Fusing point reduces measuring result and the cake strength measuring result all is shown in table 2.
Table 1
Kind MFR (g/10min) Co-monomer content (wt%) The unsaturated fatty acids bisamide Consumption (weight part) Lubricant Consumption (weight part) Addition means Surface roughness (μ m)
Embodiment 1 EVA 400 33 Ethylenebisoleoamide 0.1 Erucicamide 0.1 Melt mixes and pinches 1.6
Embodiment 2 EVA 400 33 Ethylenebisoleoamide 0.5 Erucicamide 0.5 Melt mixes and pinches 1.6
Embodiment 3 EVA 400 33 Ethylenebisoleoamide 0.05 Erucicamide 0.05 Melt mixes and pinches 1.6
Embodiment 4 EVA 400 33 Ethylenebisoleoamide 0.1 Oleylamide 0.1 Melt mixes and pinches 1.6
Comparative example 1 EVA 400 33 - - - - - 1.6
Comparative example 2 EVA 400 33 Ethylenebisoleoamide 0.2 - - Melt mixes and pinches 1.6
Comparative example 3 EVA 400 33 - - Erucicamide 0.2 Melt mixes and pinches 1.6
Comparative example 4 EVA 400 33 Ethylenebisoleoamide 0.15 Erucicamide 0.05 Melt mixes and pinches 1.6
Table 2
Tm1 (℃) Tm2 (℃) Fusing point decline (℃) Cake strength (N)
Harsh postpartum After 1 month
Embodiment 1 120 75 45 206 Good 186 Good
Embodiment 2 120 75 45 78 Good 59 Good
Embodiment 3 120 75 45 441 Good 392 Good
Embodiment 4 120 85 35 294 Good 274 Good
Comparative example 1 - - - ＞490 Difference ＞490 Difference
Comparative example 2 - - - ＞490 Difference 314 Good
Comparative example 3 - - - ＞490 Difference ＞490 Difference
Comparative example 4 120 103 17 ＞490 Difference 196 Good
Embodiment 2
MFR is that 400g/10min, VAc content are that 100 parts by weight of ethylene/vinyl acetate copolymer (Ultrathene (Nipoflex) 0B54B, by Tosoh company produce) of 33wt% carries out melt with the erucicamide of the ethylenebisoleoamide of 0.5 weight part and 0.5 weight part and mixes and pinch.Water cutting down cuts the mixture that obtains.The particle surface that alligatoring obtains.Having obtained surface roughness like this is the particle of 1.6 μ m.The particle that obtains is carried out the cake strength evaluation.It the results are shown in table 2.
Embodiment 3
MFR is that 400g/10min, VAc content are that 100 parts by weight of ethylene/vinyl acetate copolymer (Ultrathene (Nipoflex) 0B54B, by Tosoh company produce) of 33wt% carries out melt with the erucicamide of the ethylenebisoleoamide of 0.05 weight part and 0.05 weight part and mixes and pinch.Water cutting down cuts the mixture that obtains.The particle surface that alligatoring obtains.Having obtained surface roughness like this is the particle of 1.6 μ m.The particle that obtains is carried out the cake strength evaluation.It the results are shown in table 2.
Embodiment 4
MFR is that 400g/10min, VAc content are that 100 parts by weight of ethylene/vinyl acetate copolymer (Ultrathene (Nipoflex) 0B54B, by Tosoh company produce) of 33wt% carries out melt with the oleylamide of the ethylenebisoleoamide of 0.05 weight part and 0.05 weight part and mixes and pinch.Water cutting down cuts the mixture that obtains.The particle surface that alligatoring obtains.Having obtained surface roughness like this is the particle of 1.6 μ m.The particle that obtains is carried out the cake strength evaluation.0.1 the fusing point decline measuring result of the mixture of weight part ethylenebisoleoamide and 0.1 weight part oleylamide and the measuring result of cake strength are shown in table 2.
Comparative example 1
To MFR is that 400g/10min, VAc content are that alligatoring is carried out on the surface of the ethylene/vinyl acetate copolymer particle (Ultrathene (Nipoflex) 0B54B, by Tosoh company produce) of 33wt%.Having obtained surface roughness like this is the particle of 1.6 μ m.The particle that obtains is carried out the cake strength evaluation.The results are shown in table 2.Because particulate cake strength height, so these particles are unpractical.
Comparative example 2
MFR is that 400g/10min, VAc content are that 100 parts by weight of ethylene/vinyl acetate copolymer (Ultrathene (Nipoflex) 0B54B, by Tosoh company produce) of 33wt% carries out melt with the ethylenebisoleoamide of 0.2 weight part and mixes and pinch.Water cutting down cuts the mixture that obtains.The particle surface that alligatoring obtains.Having obtained surface roughness like this is the particle of 1.6 μ m.The particle that obtains is carried out the cake strength evaluation.The results are shown in table 2.Because the cake strength height of these particles after just producing, so they are unpractical.
Comparative example 3
MFR is that 400g/10min, VAc content are that 100 parts by weight of ethylene/vinyl acetate copolymer (Ultrathene (Nipoflex) 0B54B, by Tosoh company produce) of 33wt% carries out melt with the erucicamide of 0.2 weight part and mixes and pinch.Then, cutting is cut the mixture that obtains under the water.The particle surface that alligatoring obtains.Having obtained surface roughness like this is the particle of 1.6 μ m.The particle that obtains is carried out the cake strength evaluation.The results are shown in table 2.Because these particulate cake strength height, so they are unpractical.
Comparative example 4
MFR is that 400g/10min, VAc content are that 100 parts by weight of ethylene/vinyl acetate copolymer (Ultrathene (Nipoflex) 0B54B, by Tosoh company produce) of 33wt% carries out melt with the erucicamide of the ethylenebisoleoamide of 0.15 weight part and 0.05 weight part and mixes and pinch.Water cutting down cuts the mixture that obtains.The particle surface that alligatoring obtains.Having obtained surface roughness like this is the particle of 1.6 μ m.The particle that obtains is carried out the cake strength evaluation.0.15 the fusing point decline measuring result of the mixture of weight part ethylenebisoleoamide and 0.05 weight part erucicamide and the measuring result of cake strength are shown in table 2.Because the cake strength height of these particles after just producing, so they are unpractical.
The anti-caking effect that can have as mentioned above, raising according to ethylene copolymer pellets of the present invention.

Claims (5)

1. ethylene copolymer pellets comprises following mixture:
(a) ethylene/vinyl acetate copolymer of 100 weight parts;
(b) fusing point of 0.01-0.5 weight part is 100-180 ℃ a unsaturated fatty acids bisamide; With
(c) fusing point of 0.01-0.5 weight part is 60-90 ℃ a lubricant, and when itself and composition (b) when being used in combination, at least 20 ℃ of the fusing points of this lubricant reduction composition (b), unsaturated fatty acids bisamide (b) is 70/30-30/70 with the weight ratio of lubricant (c), and this ethylene copolymer pellets has the surface roughness Ra of the 1.0-2.5 μ m that measures according to JISB0601 (1994), the therein ethylene multipolymer is that a kind of vinyl acetate content VAc that has according to JIS K6924-1 (1997) measurement is 27-50wt%, and the melt flow rate value of measuring according to JISK6924-1 (1997), MFR, satisfy the ethylene/vinyl acetate copolymer of following relationship formula:
MFR＞431.98×(VAc) -0.7731。
2. ethylene copolymer pellets as claimed in claim 1, this particle are to mix by melt to pinch the mixture of acquisition.
3. ethylene copolymer pellets as claimed in claim 1 or 2, wherein unsaturated fatty acids bisamide (b) is an ethylenebisoleoamide.
4. ethylene copolymer pellets as claimed in claim 1 or 2, wherein lubricant (c) is the unsaturated fatty acids acid amides.
5. ethylene copolymer pellets as claimed in claim 4, wherein the unsaturated fatty acids acid amides is an erucicamide.
CNB2004100072059A 2003-02-27 2004-02-27 Ethylene copolymer particle Expired - Fee Related CN1300237C (en)

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JP2003050893A JP4192628B2 (en) 2003-02-27 2003-02-27 Ethylene copolymer pellets
JP050893/03 2003-02-27

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US20070221268A1 (en) * 2006-03-21 2007-09-27 Hasch Bruce M Encapsulants for electronic components
JP7236563B2 (en) 2019-11-28 2023-03-09 三井・ダウポリケミカル株式会社 Resin pellet, method for producing resin pellet, gravure ink and wire coating material
JP7326404B2 (en) * 2021-06-16 2023-08-15 長春石油化學股▲分▼有限公司 Ethylene-vinyl alcohol copolymer resin composition
CN115477801B (en) * 2021-06-16 2023-12-05 长春石油化学股份有限公司 Ethylene-vinyl alcohol copolymer resin composition, ethylene-vinyl alcohol copolymer film formed therefrom, and multilayer structure comprising the same

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JPH05140363A (en) * 1991-11-22 1993-06-08 Hitachi Chem Co Ltd Production of foamed styrenic resin particle
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Granted publication date: 20070214