CN109438625A - A kind of polypropylene wax high-efficient production technology - Google Patents
A kind of polypropylene wax high-efficient production technology Download PDFInfo
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- CN109438625A CN109438625A CN201811360813.6A CN201811360813A CN109438625A CN 109438625 A CN109438625 A CN 109438625A CN 201811360813 A CN201811360813 A CN 201811360813A CN 109438625 A CN109438625 A CN 109438625A
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- Prior art keywords
- polypropylene wax
- production technology
- efficient production
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- maleic anhydride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F255/00—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
- C08F255/02—Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F110/04—Monomers containing three or four carbon atoms
- C08F110/06—Propene
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Transition And Organic Metals Composition Catalysts For Addition Polymerization (AREA)
Abstract
The present invention provides a kind of polypropylene wax high-efficient production technology, belong to technical field of polymer materials, by adding maleic anhydride grafting into polypropylene wax factory formula, improve the surface polarity and processing fluidity of polypropylene wax, to improve the improvement processing flowability of the compatibilization of compatilizer, the surface activation of coupling agent and lubricant in formula simultaneously, shorten the reaction time of polypropylene wax, reduces the carbonation rate of polypropylene wax production process, improve the Production Gain rate of polypropylene wax；Simultaneously, granular polypropylene wax semi-finished product are obtained using carried metallocene catalyst catalysis bulk propylene polymerization, and polypropylene wax semi-finished granules are uniform, when solving that polypropylene wax product is discharged in prior art with melt form, due to often resulting in the technological deficiency of reactor plugs when polymer melt viscosity very big discharging, technique provided in an embodiment of the present invention, polypropylene wax product number-average molecular weight that polymerization activity height obtains is controllable and abundance narrow distribution range.
Description
Technical field
The present invention relates to technical field of polymer materials more particularly to a kind of polypropylene wax high-efficient production technologies.
Background technique
Polypropylene wax is widely used in high-tech sector, such as paper coating toner and film condensation, is also wrapped
Include the modifying agent and fabric treating of pigment dispersing agent, lubricant, the release agent of various synthetic resin molding, printing ink and coating
Auxiliary agent etc..
At present there are three ways to production polypropylene wax, the first propylene adjusts polymerization, is the routine for synthesizing polypropylene wax
Approach can accurately control molecular weight, narrow molecular weight distribution.But the method needs high temperature and pressure, and complex process, is not suitable for small rule
Mould production.Second of reactive extrursion method, this method start up and material conversion are convenient and efficient, and temperature and reaction time are easily-controllable
System.But when the method mixes difference because of polypropylene in extruder, heat transfer conditions is be easy to cause to deteriorate, crack required heat to meet
Amount, it is necessary to improve reaction temperature, yield is caused to decline, and viscous wall carbonization easily occurs, seriously affect product quality.The third stirring
Kettle pyrolysis method, this method are the current domestic methods generally used, but this method because polypropylene wax viscosity it is big, reaction is just
Phase, stirring is difficult, causes temperature inhomogenous, melt is attached to hot-spot on stirring and kettle wall and is carbonized, and carbide falls into production
Product quality is influenced in product.
Existing polypropylene wax will generally be manufactured under the catalytic condition of catalyst, complex process, in order to guarantee to urge
The activity of agent, process control condition is complicated, so that the polypropylene wax quality stability produced can be effectively ensured.
Therefore, currently, being badly in need of a kind of safe and reliable, economical and effective, tail gas qualified discharge and reaction time is short, high income, carbonation rate are low
Polypropylene wax high-efficient production technology.
Summary of the invention
In view of the above-mentioned problems, the present invention provides a kind of polypropylene wax high-efficient production technology, by matching to polypropylene wax production
Maleic anhydride grafting is added in side, improves the surface polarity and processing fluidity of polypropylene wax, to improve phase in formula simultaneously
Compatibilization, the surface activation of coupling agent and the improvement processing flowability of lubricant for holding agent, shorten polypropylene wax
The carbonation rate of polypropylene wax production process is reduced, the Production Gain rate of polypropylene wax is improved reaction time.
The present invention provides a kind of polypropylene wax high-efficient production technology
Under dry nitrogen stream, silica gel is heated 4 hours under the conditions of 700 DEG C, backward reaction flask in be passed through nitrogen
It protects spare；
Under nitrogen protection, it to 6.0g methylaluminoxane and 30mL toluene are added in churned mechanically reaction flask, stirs molten
It solves and constant temperature is to 120 DEG C, then above-mentioned processed silica gel 6.0g is slowly added into methylaluminoxane solution, with 30mL first
Benzene rinses remaining silica gel, and constant temperature stirs 3 hours, is then washed, is filtered with toluene at 120 DEG C, is dry, obtains load methyl
The silica-gel carrier of aikyiaiurnirsoxan beta；
Under nitrogen protection, 120mg dimethyl-silicon bridging α-olefins are weighed to be added to churned mechanically reaction flask
In, it adds the stirring of 25mL n-hexane and slurries is made, constant temperature is to 50 DEG C, the silica-gel carrier for then loading above-mentioned methylaluminoxane
Be added in metallocene compound slurries, rinse remaining carrier with 25ml n-hexane, and continue stirring 100 minutes, after pass through
N-hexane is washed, is filtered, being dried to obtain load metallocene catalyst 12g, wherein the Al constituent content of load metallocene catalyst
For 18% weight, Zr constituent content is 0.25% weight；
Polymeric kettle is first purged with drying nitrogen and is replaced, and the hydrogen of 0.1 ~ 0.3MPa is then passed to, later by the load of 100 ~ 300mg
Metallocene catalyst, which is suspended in 5 ~ 10ml n-hexane, to be made in slurries addition catalyst feeder, and it is dense that 3.5 ~ 6ml is then added
Degree is the triisobutyl aluminium hexane solution and maleic anhydride grafted monomers of 1mol/L, and it is raw that polypropylene wax is made in starting after mixing evenly
Production catalyst；
Above-mentioned polypropylene wax production is poured in reaction kettle with catalyst using 5 ~ 10L liquid propene, is warming up to 100-250 DEG C instead
It answers 1 hour, the heating system and blender being equipped with during the reaction using reaction kettle carry out heating and stirring, wherein stirring
Rate control is added initiator during stirring and grafting and activating agent, initiator adds in 100r/min- 250r/min
Dosage is the 1/25 ~ 1/15 of maleic anhydride grafted monomers addition quality, and the additive amount of grafting and activating agent is that maleic anhydride grafting is single
Body adds the 1/3 ~ 1/2 of quality；
Reaction complete after, by the mixture in reaction kettle using atomizer spray granulation, and in drying chamber cooling and drying it
Polypropylene wax semi-finished product are obtained afterwards；
After crushing by pulverizer by above-mentioned polypropylene wax semi-finished product and use sifted point, polypropylene wax finished product is obtained.
Optionally, the maleic anhydride monomer additive amount is the 2-10% of liquid propene additive amount.
Optionally, the initiator is dual-tert-butyl cumene hydroperoxide, benzyl peroxide or tert-butyl mistake
One of oxide is a variety of.
Optionally, the grafting and activating agent is the mixture of styrene, maleic acid monoester or both.
Optionally, the number-average molecular weight of the polypropylene wax is 3000-40000 grams/mol, and molecular weight distribution is 3 ~ 4.5.
Optionally, the methylaluminoxane solution is made of using aromatic hydrocarbon as solvent, wherein the aromatic hydrocarbon be toluene,
Dimethylbenzene and its mixture.
Optionally, the alkylaluminoxane additional amount is the 8%~80% of vehicle weight；The metallocene compound is added
Amount accounts for the 5%~8% of vehicle weight；The methylaluminoxane and the load factor of the metallocene compound are all larger than 70%.
The present invention at least has the following beneficial effects:
The present invention provides a kind of polypropylene wax high-efficient production technologies, by adding maleic anhydride into polypropylene wax factory formula
Grafting, improves the surface polarity and processing fluidity of polypropylene wax, to improve the compatibilization of compatilizer, idol in formula simultaneously
Join the surface activation of agent and the improvement processing flowability of lubricant, shorten the reaction time of polypropylene wax, reduces poly- third
The carbonation rate of alkene wax production process improves the Production Gain rate of polypropylene wax；Meanwhile it being catalyzed using carried metallocene catalyst
Bulk propylene polymerization obtains granular polypropylene wax semi-finished product, and polypropylene wax semi-finished granules are uniform, relative to existing skill
Preparation method in art, when solving that polypropylene wax product is discharged in prior art with melt form, since polymer melt is glutinous
Spend the technological deficiency that reactor plugs are often resulted in when very big discharging, technique provided in an embodiment of the present invention, polymerization activity
Polypropylene wax product number-average molecular weight that height obtains is controllable and abundance narrow distribution range.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described reality
Applying example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field
Those of ordinary skill's every other embodiment obtained without making creative work, belongs to guarantor of the present invention
The range of shield.
A kind of polypropylene wax high-efficient production technology provided in an embodiment of the present invention includes the following steps:
Under dry nitrogen stream, silica gel is heated 4 hours under the conditions of 700 DEG C, backward reaction flask in be passed through nitrogen
It protects spare；
Under nitrogen protection, it to 6.0g methylaluminoxane and 30mL toluene are added in churned mechanically reaction flask, stirs molten
It solves and constant temperature is to 120 DEG C, then above-mentioned processed silica gel 6.0g is slowly added into methylaluminoxane solution, with 30mL first
Benzene rinses remaining silica gel, and constant temperature stirs 3 hours, is then washed, is filtered with toluene at 120 DEG C, is dry, obtains load methyl
The silica-gel carrier of aikyiaiurnirsoxan beta；
Under nitrogen protection, 120mg dimethyl-silicon bridging α-olefins are weighed to be added to churned mechanically reaction flask
In, it adds the stirring of 25mL n-hexane and slurries is made, constant temperature is to 50 DEG C, the silica-gel carrier for then loading above-mentioned methylaluminoxane
Be added in metallocene compound slurries, rinse remaining carrier with 25ml n-hexane, and continue stirring 100 minutes, after pass through
N-hexane is washed, is filtered, being dried to obtain load metallocene catalyst 12g, wherein the Al constituent content of load metallocene catalyst
For 18% weight, Zr constituent content is 0.25% weight；
Polymeric kettle is first purged with drying nitrogen and is replaced, and the hydrogen of 0.1 ~ 0.3MPa is then passed to, later by the load of 100 ~ 300mg
Metallocene catalyst, which is suspended in 5 ~ 10ml n-hexane, to be made in slurries addition catalyst feeder, and it is dense that 3.5 ~ 6ml is then added
Degree is the triisobutyl aluminium hexane solution and maleic anhydride grafted monomers of 1mol/L, and it is raw that polypropylene wax is made in starting after mixing evenly
Production catalyst；
Above-mentioned polypropylene wax production is poured in reaction kettle with catalyst using 5 ~ 10L liquid propene, is warming up to 100-250 DEG C instead
It answers 1 hour, the heating system and blender being equipped with during the reaction using reaction kettle carry out heating and stirring, wherein stirring
Rate control is added initiator during stirring and grafting and activating agent, initiator adds in 100r/min- 250r/min
Dosage is the 1/25 ~ 1/15 of maleic anhydride grafted monomers addition quality, and the additive amount of grafting and activating agent is that maleic anhydride grafting is single
Body adds the 1/3 ~ 1/2 of quality；
Reaction complete after, by the mixture in reaction kettle using atomizer spray granulation, and in drying chamber cooling and drying it
Polypropylene wax semi-finished product are obtained afterwards；
After crushing by pulverizer by above-mentioned polypropylene wax semi-finished product and use sifted point, polypropylene wax finished product is obtained.
Wherein, the maleic anhydride monomer additive amount used in above-mentioned steps causes for the 2-10% of liquid propene additive amount
Agent is one of dual-tert-butyl cumene hydroperoxide, benzyl peroxide or tert-butyl peroxide or a variety of.It connects
Branch activator is the mixture of styrene, maleic acid monoester or both, and methylaluminoxane solution is using aromatic hydrocarbon as solvent system
At, wherein aromatic hydrocarbon is toluene, dimethylbenzene and its mixture.Alkylaluminoxane additional amount used in the embodiment of the present invention is to carry
The 8%~80% of body weight；Metallocene compound additional amount accounts for the 5%~8% of vehicle weight；Methylaluminoxane and metallocene
The load factor for closing object is all larger than 70%.
The number-average molecular weight for the polypropylene wax for using the technique of the embodiment of the present invention to prepare for 3000-40000 grams/mol,
Molecular weight distribution is 3 ~ 4.5.
A kind of polypropylene wax high-efficient production technology of the embodiment of the present invention carries out graft reaction using reaction kettle equipment, mentions
The high haptoreaction time of polypropylene wax and maleic anhydride monomer, and by pressing proper proportion maleic anhydride monomer and initiator
Measure to strengthen effective dispersion of maleic anhydride monomer and initiator, these be all conducive to improve maleic anhydride monomer it is effective
Grafting rate；Also, during entire technological reaction, make carrier to residual in product using inert gas under the stirring of blender
It stays monomer and peculiar smell to be removed, ensure that going on smoothly for reaction.
The present invention provides a kind of polypropylene wax high-efficient production technologies, by adding Malaysia into polypropylene wax factory formula
Acid anhydrides grafting, improves the surface polarity and processing fluidity of polypropylene wax, so that the increase-volume for improving compatilizer in formula simultaneously is made
With, the improvement processing flowability of the surface activation of coupling agent and lubricant, shortens the reaction time of polypropylene wax, reduce
The carbonation rate of polypropylene wax production process improves the Production Gain rate of polypropylene wax；Meanwhile using carried metallocene catalyst
Catalysis bulk propylene polymerization obtains granular polypropylene wax semi-finished product, and polypropylene wax semi-finished granules are uniform, relative to
There is the preparation method in technology, when solving that polypropylene wax product is discharged in prior art with melt form, since polymer is molten
Body viscosity very big discharging when often result in the technological deficiencies of reactor plugs, technique provided in an embodiment of the present invention, polymerization reaction
Polypropylene wax product number-average molecular weight that active height obtains is controllable and abundance narrow distribution range.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (7)
1. a kind of polypropylene wax high-efficient production technology, which is characterized in that the polypropylene wax high-efficient production technology includes:
Under dry nitrogen stream, silica gel is heated 4 hours under the conditions of 700 DEG C, backward reaction flask in be passed through nitrogen
It protects spare；
Under nitrogen protection, it to 6.0g methylaluminoxane and 30mL toluene are added in churned mechanically reaction flask, stirs molten
It solves and constant temperature is to 120 DEG C, then above-mentioned processed silica gel 6.0g is slowly added into methylaluminoxane solution, with 30mL first
Benzene rinses remaining silica gel, and constant temperature stirs 3 hours, is then washed, is filtered with toluene at 120 DEG C, is dry, obtains load methyl
The silica-gel carrier of aikyiaiurnirsoxan beta；
Under nitrogen protection, 120mg dimethyl-silicon bridging α-olefins are weighed to be added to churned mechanically reaction flask
In, it adds the stirring of 25mL n-hexane and slurries is made, constant temperature is to 50 DEG C, the silica-gel carrier for then loading above-mentioned methylaluminoxane
Be added in metallocene compound slurries, rinse remaining carrier with 25ml n-hexane, and continue stirring 100 minutes, after pass through
N-hexane is washed, is filtered, being dried to obtain load metallocene catalyst 12g, wherein the Al constituent content of load metallocene catalyst
For 18% weight, Zr constituent content is 0.25% weight；
Polymeric kettle is first purged with drying nitrogen and is replaced, and the hydrogen of 0.1 ~ 0.3MPa is then passed to, later by the load of 100 ~ 300mg
Metallocene catalyst, which is suspended in 5 ~ 10ml n-hexane, to be made in slurries addition catalyst feeder, and it is dense that 3.5 ~ 6ml is then added
Degree is the triisobutyl aluminium hexane solution and maleic anhydride grafted monomers of 1mol/L, and it is raw that polypropylene wax is made in starting after mixing evenly
Production catalyst；
Above-mentioned polypropylene wax production is poured in reaction kettle with catalyst using 5 ~ 10L liquid propene, is warming up to 100-250 DEG C instead
It answers 1 hour, the heating system and blender being equipped with during the reaction using reaction kettle carry out heating and stirring, wherein stirring
Rate control is added initiator during stirring and grafting and activating agent, initiator adds in 100r/min- 250r/min
Dosage is the 1/25 ~ 1/15 of maleic anhydride grafted monomers addition quality, and the additive amount of grafting and activating agent is that maleic anhydride grafting is single
Body adds the 1/3 ~ 1/2 of quality；
Reaction complete after, by the mixture in reaction kettle using atomizer spray granulation, and in drying chamber cooling and drying it
Polypropylene wax semi-finished product are obtained afterwards；
After crushing by pulverizer by above-mentioned polypropylene wax semi-finished product and use sifted point, polypropylene wax finished product is obtained.
2. polypropylene wax high-efficient production technology according to claim 1 or 2, which is characterized in that the maleic anhydride monomer
Additive amount is the 2-10% of liquid propene additive amount.
3. polypropylene wax high-efficient production technology according to claim 1 or 2, which is characterized in that the initiator is double uncles
One of butyl peroxy cumene, benzyl peroxide or tert-butyl peroxide are a variety of.
4. polypropylene wax high-efficient production technology according to claim 1 or 3, which is characterized in that the grafting and activating agent is
The mixture of styrene, maleic acid monoester or both.
5. polypropylene wax high-efficient production technology according to claim 1, which is characterized in that the number of the polypropylene wax is divided equally
Son amount is 3000-40000 grams/mol, and molecular weight distribution is 3 ~ 4.5.
6. polypropylene wax high-efficient production technology according to claim 1, which is characterized in that the methylaluminoxane solution is
It is made using aromatic hydrocarbon of solvent, wherein the aromatic hydrocarbon is toluene, dimethylbenzene and its mixture.
7. polypropylene wax high-efficient production technology according to claim 1, which is characterized in that the alkylaluminoxane is added
Amount is the 8%~80% of vehicle weight；The metallocene compound additional amount accounts for the 5%~8% of vehicle weight；The aluminium methyl
The load factor of oxygen alkane and the metallocene compound is all larger than 70%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811360813.6A CN109438625A (en) | 2018-11-15 | 2018-11-15 | A kind of polypropylene wax high-efficient production technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811360813.6A CN109438625A (en) | 2018-11-15 | 2018-11-15 | A kind of polypropylene wax high-efficient production technology |
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| CN109438625A true CN109438625A (en) | 2019-03-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201811360813.6A Pending CN109438625A (en) | 2018-11-15 | 2018-11-15 | A kind of polypropylene wax high-efficient production technology |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597358A (en) * | 2008-06-02 | 2009-12-09 | 张发饶 | A kind of preparation method of maleic anhydride inoculated polypropylene wax and device thereof |
| CN105622807A (en) * | 2014-10-28 | 2016-06-01 | 中国石油化工股份有限公司 | Preparation method of polypropylene wax |
| WO2017110633A1 (en) * | 2015-12-22 | 2017-06-29 | 日本製紙株式会社 | Modified polyolefin resin |
-
2018
- 2018-11-15 CN CN201811360813.6A patent/CN109438625A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101597358A (en) * | 2008-06-02 | 2009-12-09 | 张发饶 | A kind of preparation method of maleic anhydride inoculated polypropylene wax and device thereof |
| CN105622807A (en) * | 2014-10-28 | 2016-06-01 | 中国石油化工股份有限公司 | Preparation method of polypropylene wax |
| WO2017110633A1 (en) * | 2015-12-22 | 2017-06-29 | 日本製紙株式会社 | Modified polyolefin resin |
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Application publication date: 20190308 |