CN107722415A - A kind of preparation and its application of polyolefin nucleating agent composition - Google Patents
A kind of preparation and its application of polyolefin nucleating agent composition Download PDFInfo
- Publication number
- CN107722415A CN107722415A CN201711095768.1A CN201711095768A CN107722415A CN 107722415 A CN107722415 A CN 107722415A CN 201711095768 A CN201711095768 A CN 201711095768A CN 107722415 A CN107722415 A CN 107722415A
- Authority
- CN
- China
- Prior art keywords
- polyolefin
- nucleating agent
- agent composition
- preparation
- polyolefin nucleating
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920000098 polyolefin Polymers 0.000 title claims abstract description 58
- 239000002667 nucleating agent Substances 0.000 title claims abstract description 34
- 239000000203 mixture Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000002425 crystallisation Methods 0.000 claims abstract description 18
- 230000008025 crystallization Effects 0.000 claims abstract description 18
- -1 cyclohexyl dicarboxylic acid's salt Chemical class 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000344 soap Substances 0.000 claims abstract description 9
- 238000002844 melting Methods 0.000 claims abstract description 4
- 230000008018 melting Effects 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 229920005989 resin Polymers 0.000 claims description 6
- 239000011347 resin Substances 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 239000011575 calcium Substances 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 4
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 4
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 239000004411 aluminium Substances 0.000 claims description 4
- 229910052782 aluminium Inorganic materials 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052788 barium Inorganic materials 0.000 claims description 4
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052744 lithium Inorganic materials 0.000 claims description 4
- 229910052749 magnesium Inorganic materials 0.000 claims description 4
- 239000011777 magnesium Substances 0.000 claims description 4
- 229910021645 metal ion Inorganic materials 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 2
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 claims description 2
- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 claims 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- 238000003756 stirring Methods 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 159000000007 calcium salts Chemical class 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 241001269238 Data Species 0.000 description 1
- 239000013032 Hydrocarbon resin Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229920006270 hydrocarbon resin Polymers 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 150000004291 polyenes Chemical class 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/24—Crystallisation aids
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of polyolefin nucleating agent composition, take out standby after cyclohexyl dicarboxylic acid's salt is stirred 3 60 minutes with soap in homogenizer, the mass fraction proportioning of the soap and cyclohexyl dicarboxylic acid's salt is 1:5—5:1.The present invention discloses a kind of polyolefin nucleating agent composition prepared according to the method described above.The application process is that the polyolefin nucleating agent composition that this method is prepared is well mixed into melting mixing with polyolefin, in the case of addition identical, polyolefin nucleating agent composition prepared by the present invention has more preferable nucleating effect, significantly reduce semicrystalline polyolefin crystallization time, the crystalline rate of polyolefin is accelerated, improves the crystallinity of polyolefin.
Description
Technical field
The invention belongs to technical field of polymer materials, and in particular to a kind of preparation of polyolefin nucleating agent composition and its
Using.
Background technology
Addition nucleator is the major way of current improved polyalkene crystal property.Nucleator initial stage can in polyolefin crystallization
Effectively to provide nucleus, heterogeneous nucleating effect is played, makes molecular polyolefin chain apposition growth.Therefore, nucleator can be effective
Increase the crystallization temperature and crystallization rate of polyolefin, it is crystallized at a higher temperature, so as to shorten the process-cycle, and and this
Crystal grain thinning simultaneously, improves the physics such as the rigid, transparent of polyolefin, lustrous surface, dimensional stability and processing characteristics.
At present, nucleator kind is mostly single inorganic material and organic compound kind and high polymer material, for
Compound kind is rarely reported.The nucleator of single variety can not often play optimal efficacy, can not meet carrying for universality energy
Height, therefore, the Composite of nucleator are imperative.
The content of the invention
The present invention is intended to provide a kind of preparation and its application of polyolefin nucleating agent composition, by selecting different hexamethylenes
The compounding of dicarboxylate and soap and different proportion obtains a kind of polyolefin nucleating agent composition, compared to single hexamethylene
Dicarboxylate nucleator, the polyolefin nucleating agent composition of this method synthesis overcome salt nucleator and disperse hardly possible in resin
Shortcoming, its surface is activated by soap, improve dispersiveness of cyclohexyl dicarboxylic acid's salt nucleator in resin, enter
One step improves the efficiency of cyclohexyl dicarboxylic acid's salt nucleator, accelerates the crystalline rate of polyolefin, improves the crystallization of polyolefin
Degree.
The present invention adopts the following technical scheme that：
A kind of preparation method of polyolefin nucleating agent composition, comprises the following steps：Under normal temperature, by cyclohexyl dicarboxylic acid's salt and fat
Hydrochlorate takes out standby, described cyclohexyl dicarboxylic acid's salt after 3-60 minutes are stirred in homogenizer and the quality of soap is divided
Counting proportioning is：1:5—5:1.
Metal ion corresponding to cyclohexyl dicarboxylic acid's salt is at least one of calcium, magnesium, barium, zinc, aluminium, lithium.
The soap can be saturation or unsaturated fatty acid salt, and its carbon number is：5-28.
The soap is preferably stearate, and the metal ion of the stearate is calcium, magnesium, barium, zinc, aluminium, lithium
At least one of.
The polyolefin nucleating agent composition that present invention protection is prepared according to preparation method as described above.
The present invention also protects application of the said polyolefins nucleating agent compositions in polyolefin crystallization modification.
Application of the polyolefin nucleating agent composition in polyolefin crystallization modification, its concrete application method are：By institute
State polyolefin nucleating agent composition and melting mixing is well mixed with polyolefin, the polyolefin nucleating agent composition is in polyolefin tree
Addition in fat is：300ppm-5000ppm resin quality fractions.
Beneficial effects of the present invention：The polyolefin nucleating agent of more single cyclohexyl dicarboxylic acid's salt, polyolefin of the invention nucleation
Agent composition can not only provide nucleus, particularly can also effectively help strand preferably mobile and ordered arrangement, further carry
The high efficiency of cyclohexyl dicarboxylic acid's salt nucleator, the crystalline rate of polyolefin is accelerated, further increases the efficiency of nucleator,
The crystalline rate of polyolefin is accelerated, improves the crystallinity of polyolefin；The polyolefin nucleating agent composition of the present invention is in polyene
Dispersion rate is high in hydrocarbon resin, and energy rapid dispersion is uniform, solves single cyclohexyl dicarboxylic acid's salt nucleator difficult point in resin
The problem of dissipating；The polyolefin nucleating agent composition prepared using the inventive method is shown in the application that polyolefin crystallization is modified
More preferable nucleating effect.
Embodiment
The present invention is described in further detail with reference to embodiment, it should be appreciated that these embodiments are only used for
Illustrate the application of the present invention rather than the limitation present invention.
Embodiment
（1）Cyclohexyl dicarboxylic acid's calcium is weighed up in proportion with zinc stearate first；
（2）In homogenizer, stirred 20 minutes under normal temperature；
（3）Polyolefin nucleating agent composition is obtained, is taken out standby（It is shown in Table 1）.
Table 1
By polypropylene（Commercially available powder melts finger：230 DEG C, under 2.16Kg, 2.52g/10min）It is nucleated with the polyolefin of above-mentioned preparation
Empirically ratio puts into torque rheometer for agent composition and one-component cyclohexyl dicarboxylic acid's calcium salt nucleator（Breathe out general electricity in Harbin
Gas technology Co., Ltd）In be well mixed melting mixing（200 DEG C, 80rpm, 4min).
Sample preparation ratio is as shown in table 2:
Table 2
Method of testing：
The present invention uses differential scanning calorimeter（DSC, plum Teller-support benefit）, crystallization temperature is evaluated using following procedure section
And crystallinity.Crystallization temperature is higher, and crystallization is faster, and molding cycle is shorter.
（1）Use differential scanning calorimeter（DSC, plum Teller-support benefit）, during using following procedure section to evaluate hypocrystalline
Between.Flexible chain：In the case of isothermal crystal, crystallization reaches the time needed for half, is weigh Resin crystallization speed one
Individual important indicator.
Program segment：210 DEG C of insulation 3min, subsequent fast cooling to 138 DEG C of guarantors are risen to from 25 DEG C with 20 DEG C/min speed
Hold 15 minutes.
Test simultaneously result of calculation such as table 3.
Table 3
（2）The present invention uses differential scanning calorimeter（DSC, plum Teller-support benefit）, crystallization temperature is evaluated using following procedure section
Degree.
Program segment：210 DEG C of insulation 3min are risen to from 25 DEG C with 20 DEG C/min speed, then press 10 DEG C/min and 40 respectively
DEG C/min rate of temperature fall is down to 25 DEG C, survey its Crystallization peak temperature.
Test simultaneously result of calculation such as table 4.
Table 4
It is further compared to one-component cyclohexyl dicarboxylic acid's calcium salt nucleator, polyolefin nucleating agent composition from the point of view of test data
The crystallization temperature of polyolefin is improved, and shortens flexible chain；Thus two item datas can illustrate, polyolefin nucleating agent group
Compound can preferably shorten molding cycle and the production cycle of actual processing process polyolefin.Meanwhile the addition of soap
The usage amount of nucleator can effectively be reduced, reduce the production cost of nucleator.
Described above is only the better embodiment of the present invention, therefore all constructions according to described in present patent application scope,
The equivalent change or modification that feature and principle are done, it is included in present patent application scope.
Claims (8)
1. a kind of preparation method of polyolefin nucleating agent composition, it is characterised in that comprise the following steps：Under normal temperature, by hexamethylene
Dicarboxylate takes out standby, described cyclohexyl dicarboxylic acid's salt and fat after stirring 3-60 minutes in homogenizer with soap
The mass fraction of fat hydrochlorate matches：1:5—5:1.
A kind of 2. preparation method of polyolefin nucleating agent composition according to claim 1, it is characterised in that：The hexamethylene
Metal ion corresponding to dicarboxylate is at least one of calcium, magnesium, barium, zinc, aluminium, lithium.
A kind of 3. preparation method of polyolefin nucleating agent composition according to claim 1, it is characterised in that：The fat
The carbon number of hydrochlorate is 5-28.
A kind of 4. preparation method of polyolefin nucleating agent composition according to claim 1, it is characterised in that：The fat
Hydrochlorate is stearate.
A kind of 5. preparation method of polyolefin nucleating agent composition according to claim 4, it is characterised in that：The tristearin
Metal ion corresponding to hydrochlorate is at least one of calcium, magnesium, barium, zinc, aluminium, lithium.
6. a kind of preparation method of polyolefin nucleating agent composition according to any one of claims 1 to 5 is prepared poly-
Alkene nucleating agent compositions.
7. application of the polyolefin nucleating agent composition according to claim 6 in polyolefin crystallization modification.
8. a kind of application of the polyolefin nucleating agent composition according to claim 7 in polyolefin crystallization modification, it is special
Sign is that its concrete application method is：The polyolefin nucleating agent composition is well mixed melting mixing with polyolefin, it is described
Addition of the polyolefin nucleating agent composition in vistanex be：300ppm-5000ppm resin quality fractions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711095768.1A CN107722415A (en) | 2017-11-09 | 2017-11-09 | A kind of preparation and its application of polyolefin nucleating agent composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711095768.1A CN107722415A (en) | 2017-11-09 | 2017-11-09 | A kind of preparation and its application of polyolefin nucleating agent composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107722415A true CN107722415A (en) | 2018-02-23 |
Family
ID=61214270
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711095768.1A Pending CN107722415A (en) | 2017-11-09 | 2017-11-09 | A kind of preparation and its application of polyolefin nucleating agent composition |
Country Status (1)
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Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030236332A1 (en) * | 2002-06-14 | 2003-12-25 | Dotson Darin L. | Bimolecular nucleation methods for thermoplastics |
| CN1500117A (en) * | 2001-03-29 | 2004-05-26 | Metalsalts of hexahydrophthalic acid as nucleating additives for crystalline thermoplatics | |
| CN1525992A (en) * | 2001-03-29 | 2004-09-01 | Disodium hexahydrophthalate salt compositions and nucleated polymers comprising such compositions | |
| US20050038155A1 (en) * | 2003-08-12 | 2005-02-17 | Stephane Berghmans | Thermoplastics exhibiting excellent long-term hydrostatic strength for high-pressure applications |
| CN101054448A (en) * | 2007-06-06 | 2007-10-17 | 北京化工大学 | Nucleater, composition and preparation method thereof |
| WO2008005143A1 (en) * | 2006-07-03 | 2008-01-10 | Milliken & Company | Compositions comprising metal salts of hexahydrophthalic acid and methods of employing such compositions in polyolefin resins |
| KR20130001770A (en) * | 2011-06-28 | 2013-01-07 | 호남석유화학 주식회사 | Polypropylene resin composition for high tenacity fiber and high tenacity fiber manufactured by using the same |
| CN104974377A (en) * | 2014-04-14 | 2015-10-14 | 中国石油化工股份有限公司 | Nucleating agent composition containing cyclic carboxylic acid metal salt |
| CN106810714A (en) * | 2015-11-27 | 2017-06-09 | 中国石油化工股份有限公司 | A kind of nucleating agent compositions and its application |
-
2017
- 2017-11-09 CN CN201711095768.1A patent/CN107722415A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1500117A (en) * | 2001-03-29 | 2004-05-26 | Metalsalts of hexahydrophthalic acid as nucleating additives for crystalline thermoplatics | |
| CN1525992A (en) * | 2001-03-29 | 2004-09-01 | Disodium hexahydrophthalate salt compositions and nucleated polymers comprising such compositions | |
| EP1383831B1 (en) * | 2001-03-29 | 2007-09-12 | Milliken & Company | Disodium hexahydrophthalate salt compositions and nucleated polymers comprising such compositions |
| US20030236332A1 (en) * | 2002-06-14 | 2003-12-25 | Dotson Darin L. | Bimolecular nucleation methods for thermoplastics |
| US20050038155A1 (en) * | 2003-08-12 | 2005-02-17 | Stephane Berghmans | Thermoplastics exhibiting excellent long-term hydrostatic strength for high-pressure applications |
| WO2008005143A1 (en) * | 2006-07-03 | 2008-01-10 | Milliken & Company | Compositions comprising metal salts of hexahydrophthalic acid and methods of employing such compositions in polyolefin resins |
| CN101054448A (en) * | 2007-06-06 | 2007-10-17 | 北京化工大学 | Nucleater, composition and preparation method thereof |
| KR20130001770A (en) * | 2011-06-28 | 2013-01-07 | 호남석유화학 주식회사 | Polypropylene resin composition for high tenacity fiber and high tenacity fiber manufactured by using the same |
| CN104974377A (en) * | 2014-04-14 | 2015-10-14 | 中国石油化工股份有限公司 | Nucleating agent composition containing cyclic carboxylic acid metal salt |
| CN106810714A (en) * | 2015-11-27 | 2017-06-09 | 中国石油化工股份有限公司 | A kind of nucleating agent compositions and its application |
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| PB01 | Publication | ||
| PB01 | Publication | ||
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Application publication date: 20180223 |