CN106947039A - A kind of isobutene isoprene Petropols and preparation method - Google Patents
A kind of isobutene isoprene Petropols and preparation method Download PDFInfo
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- CN106947039A CN106947039A CN201710206160.5A CN201710206160A CN106947039A CN 106947039 A CN106947039 A CN 106947039A CN 201710206160 A CN201710206160 A CN 201710206160A CN 106947039 A CN106947039 A CN 106947039A
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- isoprene
- petropols
- isobutene
- isobutylene
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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
- C08F297/00—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer
- C08F297/02—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the anionic type
-
- 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
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/04—Monomers containing three or four carbon atoms
- C08F210/08—Butenes
- C08F210/10—Isobutene
- C08F210/12—Isobutene with conjugated diolefins, e.g. butyl rubber
-
- 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
- C08F236/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds
- C08F236/02—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds
- C08F236/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds the radical having only two carbon-to-carbon double bonds conjugated
- C08F236/08—Isoprene
-
- 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
- C08F240/00—Copolymers of hydrocarbons and mineral oils, e.g. petroleum resins
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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)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention discloses a kind of isobutene isoprene Petropols and preparation method, including the following raw material:Isoprene, isobutene, atent solvent, age resistor, initiator, terminator.Preparation method includes:First weigh isoprene to be dissolved in atent solvent, add initiator and start to trigger isoprene polymerization, prepare poly- 3,4 isoprene blocks;After isoprene polymerization is fully completed, the isobutene containing polar additive is added, starts to prepare polyisobutene block;After isobutene polymerisation is fully completed, age resistor and terminator are added, and glue is post-processed, purifies, produces the isobutene isoprene Petropols.Petropols of the present invention are applied in compound resin system processing technology, that is, can guarantee that the excellent mechanical and physical property of resin system, and the reaction environment compared with low viscosity can be provided for resin system, with preferable application value.
Description
Technical field
The present invention relates to Petropols technical field, and in particular to a kind of isobutylene-isoprene Petropols and preparation
Method.
Background technology
Petropols are that, with the C5 of cracking of ethylene byproduct in process, C9 cuts are a kind of thermoplastic of main polymerizable raw material
Property resin.C5 series Petropols are that, by petroleum cracking byproduct, light dydrocarbon series Petropols are widely used, available for manufacture pressure
Sensitive adhesive, PUR flux, hot-melt coating encapsulating material, hot melt traffic sign coating, rubber tackifier, paint and varnish,
Printing-ink etc..
With developing rapidly for composite industry, new method for processing forming is continued to bring out, to used resin base
Body proposes higher requirement.Such as RTM (ResinTransferMolding) technique, because RTM techniques are low pressure molding process,
Resin is not required nothing more than with higher mechanical property and physical property, and resin only has a step impregnation process to fiber, also
Seeking resin has very low viscosity, to meet resin to the abundant infiltration of fiber and flowing mold filling.The resin used at present due to
Viscosity is higher, limits its application in RTM moulding process.For this problem, research meets the low viscous of RTM technological requirements
Degree, high performance resin system can not only widen the application field of RTM techniques, while the performance of composite can be improved greatly.
Therefore, study it is a kind of can either ensure that resin system has excellent performance, and have simultaneously Petropols compared with low viscosity into
Also to have preferable application prospect and use value.
The content of the invention
For defect of the prior art, it is an object of the invention to provide a kind of isobutylene-isoprene Petropols and
Preparation method, the Petropols are applied in compound resin system processing technology, that is, can guarantee that the excellent mechanical of resin system
And physical property, and the reaction environment compared with low viscosity can be provided for resin system, with preferable application value.
The present invention solves technical problem and adopted the following technical scheme that:
The present invention relates to each raw material of a kind of isobutylene-isoprene Petropols, including following parts by weight:Isoprene 20 ~
40 parts, 30 ~ 50 parts of isobutene, 80 ~ 150 parts of atent solvent, 0.6 ~ 2.2 part of age resistor, 0.05 ~ 0.8 part of initiator, terminator 1 ~
3 parts.
Preferably, 30 parts of the isoprene, 45 parts of isobutene, 90 parts of atent solvent, 1.5 parts of age resistor, initiator 0.2
Part, 1.5 parts of terminator.
Preferably, the atent solvent is any of hexamethylene, toluene, dimethylbenzene.
Preferably, the age resistor is phenol antiager.
Preferably, the initiator is alkyl lithium initiator.
Preferably, the terminator is any of water, methanol, ethanol.
The invention further relates to a kind of method for preparing isobutylene-isoprene Petropols, comprise the following steps:
(1)Isoprene is weighed respectively according to proportioning, and is dissolved in atent solvent, wherein, monomer concentration is 40% ~
60%, mixed liquor is added in reactor, 40 ~ 75 DEG C are warming up to, initiator is added and starts to trigger isoprene polymerization, prepare poly-
3,4- isoprene blocks;
(2)After isoprene polymerization is fully completed, the isobutene containing polar additive is added, starts to prepare polyisobutene embedding
Section, wherein polyisobutene/poly- 3,4- isoprene blocks ratio are 40/60-80/20 (weight ratio);
(3)After isobutene polymerisation is fully completed, age resistor and terminator are added, and glue is post-processed, isobutyl is obtained
Alkene -3,4- isoprene block oligomer;
(4)By step(3)In reaction product carry out purification processes, remove solvent and other small molecular weight impurities, produce described different
Butylene-isoprene Petropols.
Preferably, the step(2)Middle polar additive in oxygen-containing, nitrogenous, sulfur-bearing, phosphorous polar compound one
Plant or several mixtures.
Preferably, the step(2)The isobutene of middle addition for dissolving in a solvent, monomer concentration for 40% ~ 60% it is mixed
Close liquid.
Preferably, the step(4)Middle method of purification is vacuum distillation, to remove atent solvent and unreacted monomer.
Compared with prior art, the present invention has following beneficial effect:
(1)Isobutylene-isoprene Petropols of the present invention, by by isobutene and isoprene block copolymer, adjusting
The block ratio of isobutene and isoprene is saved, the Petropols of low viscosity is obtained, the Petropols is applied to compound tree
In resin system processing technology, that is, the excellent mechanical and physical property of resin system are can guarantee that, and can provide relatively low for resin system
The reaction environment of viscosity, with preferable application value.
(2)The preparation technology of isobutylene-isoprene Petropols of the present invention is simple, and reaction condition is gentle, behaviour
Facilitate, and production process will not produce crosslinking insoluble matter, it is to avoid remove the processing step of solid insoluble, reduce production
Difficulty, is adapted to popularization and application.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.These embodiments be merely to illustrate the present invention and without
In limitation the scope of the present invention.The experimental method of unreceipted actual conditions in the following example, generally according to normal condition, for example
Sambrook equimoleculars are cloned:Laboratory manual(New York:Cold Spring Harbor Laboratory Press,
1989)Described in condition, or according to the condition proposed by manufacturer.
Embodiment 1:
A kind of isobutylene-isoprene Petropols and preparation method of the preferred embodiment of the present invention;
The isobutylene-isoprene Petropols, are prepared from by each raw material of following parts by weight:
30 parts of isoprene;
45 parts of isobutene;
90 parts of atent solvent;
1.5 parts of age resistor;
0.2 part of initiator;
1.5 parts of terminator.
The atent solvent is hexamethylene.
The age resistor is phenol antiager.
The initiator is alkyl lithium initiator.
The terminator is water.
The method of the present invention for preparing isobutylene-isoprene Petropols, comprises the following steps:
(1)Isoprene is weighed respectively according to proportioning, and is dissolved in atent solvent, wherein, monomer concentration is 50%, will
Mixed liquor is added in reactor, is warming up to 60 DEG C, is added initiator and is started to trigger isoprene polymerization, prepares poly- 3,4- isoamyls two
Alkene block;
(2)After isoprene polymerization is fully completed, the isobutene containing polar additive is added, starts to prepare polyisobutene embedding
Section, wherein polyisobutene/poly- 3,4- isoprene blocks ratio are 40/60-80/20 (weight ratio);
(3)After isobutene polymerisation is fully completed, age resistor and terminator are added, and glue is post-processed, isobutyl is obtained
Alkene -3,4- isoprene block oligomer;
(4)By step(3)In reaction product carry out purification processes, remove solvent and other small molecular weight impurities, produce described different
Butylene-isoprene Petropols.
Step(2)One or several kinds of the middle polar additive in oxygen-containing, nitrogenous, sulfur-bearing, phosphorous polar compound
Mixture.
Step(2)For dissolving in a solvent, monomer concentration is 50% mixed liquor to the isobutene of middle addition.
Step(4)Middle method of purification is vacuum distillation, to remove atent solvent and unreacted monomer.
Embodiment 2:
A kind of isobutylene-isoprene Petropols and preparation method of the preferred embodiment of the present invention;
The isobutylene-isoprene Petropols, are prepared from by each raw material of following parts by weight:
20 parts of isoprene;
30 parts of isobutene;
60 parts of atent solvent;
0.6 part of age resistor;
0.05 part of initiator;
1 part of terminator.
The atent solvent is toluene.
The age resistor is phenol antiager.
The initiator is alkyl lithium initiator.
The terminator is ethanol.
The method of the present invention for preparing isobutylene-isoprene Petropols, comprises the following steps:
(1)Isoprene is weighed respectively according to proportioning, and is dissolved in atent solvent, wherein, monomer concentration is 40%, will
Mixed liquor is added in reactor, is warming up to 40 DEG C, is added initiator and is started to trigger isoprene polymerization, prepares poly- 3,4- isoamyls two
Alkene block;
(2)After isoprene polymerization is fully completed, the isobutene containing polar additive is added, starts to prepare polyisobutene embedding
Section, wherein polyisobutene/poly- 3,4- isoprene blocks ratio are 40/60-80/20 (weight ratio);
(3)After isobutene polymerisation is fully completed, age resistor and terminator are added, and glue is post-processed, isobutyl is obtained
Alkene -3,4- isoprene block oligomer;
(4)By step(3)In reaction product carry out purification processes, remove solvent and other small molecular weight impurities, produce described different
Butylene-isoprene Petropols.
Step(2)One or several kinds of the middle polar additive in oxygen-containing, nitrogenous, sulfur-bearing, phosphorous polar compound
Mixture.
Step(2)For dissolving in a solvent, monomer concentration is 40% mixed liquor to the isobutene of middle addition.
Step(4)Middle method of purification is vacuum distillation, to remove atent solvent and unreacted monomer.
Embodiment 3:
A kind of isobutylene-isoprene Petropols and preparation method of the preferred embodiment of the present invention;
The isobutylene-isoprene Petropols, are prepared from by each raw material of following parts by weight:
40 parts of isoprene;
50 parts of isobutene;
110 parts of atent solvent;
2.2 parts of age resistor;
0.8 part of initiator;
3 parts of terminator.
The atent solvent is dimethylbenzene.
The age resistor is phenol antiager.
The initiator is alkyl lithium initiator.
The terminator is methanol.
The method of the present invention for preparing isobutylene-isoprene Petropols, comprises the following steps:
(1)Isoprene is weighed respectively according to proportioning, and is dissolved in atent solvent, wherein, monomer concentration is 60%, will
Mixed liquor is added in reactor, is warming up to 75 DEG C, is added initiator and is started to trigger isoprene polymerization, prepares poly- 3,4- isoamyls two
Alkene block;
(2)After isoprene polymerization is fully completed, the isobutene containing polar additive is added, starts to prepare polyisobutene embedding
Section, wherein polyisobutene/poly- 3,4- isoprene blocks ratio are 40/60-80/20 (weight ratio);
(3)After isobutene polymerisation is fully completed, age resistor and terminator are added, and glue is post-processed, isobutyl is obtained
Alkene -3,4- isoprene block oligomer;
(4)By step(3)In reaction product carry out purification processes, remove solvent and other small molecular weight impurities, produce described different
Butylene-isoprene Petropols.
Step(2)One or several kinds of the middle polar additive in oxygen-containing, nitrogenous, sulfur-bearing, phosphorous polar compound
Mixture.
Step(2)For dissolving in a solvent, monomer concentration is 60% mixed liquor to the isobutene of middle addition.
Step(4)Middle method of purification is vacuum distillation, to remove atent solvent and unreacted monomer.
Isobutylene-isoprene Petropols of the present invention, by by isobutene and isoprene block copolymer, adjusting
The block ratio of isobutene and isoprene is saved, the Petropols of low viscosity is obtained, the Petropols is applied to compound tree
In resin system processing technology, that is, the excellent mechanical and physical property of resin system are can guarantee that, and can provide relatively low for resin system
The reaction environment of viscosity, with preferable application value.
The preparation technology of isobutylene-isoprene Petropols of the present invention is simple, and reaction condition is gentle, operation side
Just, and production process will not produce crosslinking insoluble matter, it is to avoid remove the processing step of solid insoluble, reduce production difficult
Degree, is adapted to popularization and application.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substance of the present invention.
Claims (10)
1. a kind of isobutylene-isoprene Petropols, it is characterised in that:Each raw material including following parts by weight:Isoprene
20 ~ 40 parts, 30 ~ 50 parts of isobutene, 80 ~ 150 parts of atent solvent, 0.6 ~ 2.2 part of age resistor, 0.05 ~ 0.8 part of initiator, terminate
1 ~ 3 part of agent.
2. isobutylene-isoprene Petropols according to claim 1, it is characterised in that:30 parts of the isoprene,
45 parts of isobutene, 90 parts of atent solvent, 1.5 parts of age resistor, 0.2 part of initiator, 1.5 parts of terminator.
3. isobutylene-isoprene Petropols according to claim 1, it is characterised in that:The atent solvent is ring
Any of hexane, toluene, dimethylbenzene.
4. isobutylene-isoprene Petropols according to claim 1, it is characterised in that:The age resistor is phenols
Age resistor.
5. isobutylene-isoprene Petropols according to claim 1, it is characterised in that:The initiator is alkyl
Lithium initiator.
6. isobutylene-isoprene Petropols according to claim 1, it is characterised in that:The terminator is water, first
Any of alcohol, ethanol.
7. the method that one kind prepares the isobutylene-isoprene Petropols as described in any one of claim 1 ~ 6, its feature exists
In:Comprise the following steps:
(1)Isoprene is weighed respectively according to proportioning, and is dissolved in atent solvent, wherein, monomer concentration is 40% ~
60%, mixed liquor is added in reactor, 40 ~ 75 DEG C are warming up to, initiator is added and starts to trigger isoprene polymerization, prepare poly-
3,4- isoprene blocks;
(2)After isoprene polymerization is fully completed, the isobutene containing polar additive is added, starts to prepare polyisobutene embedding
Section, wherein polyisobutene/poly- 3,4- isoprene blocks ratio are 40/60-80/20 (weight ratio);
(3)After isobutene polymerisation is fully completed, age resistor and terminator are added, and glue is post-processed, isobutyl is obtained
Alkene -3,4- isoprene block oligomer;
(4)By step(3)In reaction product carry out purification processes, remove solvent and other small molecular weight impurities, produce described different
Butylene-isoprene Petropols.
8. the preparation method of isobutylene-isoprene Petropols according to claim 7, it is characterised in that:The step
Suddenly(2)One or several kinds of mixtures of the middle polar additive in oxygen-containing, nitrogenous, sulfur-bearing, phosphorous polar compound.
9. the preparation method of isobutylene-isoprene Petropols according to claim 7, it is characterised in that:The step
Suddenly(2)For dissolving in a solvent, monomer concentration is 40% ~ 60% mixed liquor to the isobutene of middle addition.
10. the preparation method of isobutylene-isoprene Petropols according to claim 7, it is characterised in that:The step
Suddenly(4)Middle method of purification is vacuum distillation, to remove atent solvent and unreacted monomer.
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Citations (5)
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---|---|---|---|---|
CN1242379A (en) * | 1999-07-28 | 2000-01-26 | 北京燕山石油化工公司研究院 | Three block-co-polymer of isoprene-butadiene-isoprene, and prepn. method thereof |
CN1406991A (en) * | 2001-08-21 | 2003-04-02 | 拜尔公司 | Preparation of isomeric olefine copolymer |
CN1502639A (en) * | 2002-11-21 | 2004-06-09 | 中国石油化工股份有限公司 | Method for preparing isobutylene block copolymer by sequential initiation |
CN102372810A (en) * | 2010-08-19 | 2012-03-14 | 中国石油化工股份有限公司 | Method for preparing isomonoolefin-polyene hydrocarbon copolymer |
CN103319659A (en) * | 2012-03-23 | 2013-09-25 | 天津鲁华化工有限公司 | Multicomponent copolymer petroleum resin and preparation method thereof |
-
2017
- 2017-03-31 CN CN201710206160.5A patent/CN106947039A/en active Pending
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CN1242379A (en) * | 1999-07-28 | 2000-01-26 | 北京燕山石油化工公司研究院 | Three block-co-polymer of isoprene-butadiene-isoprene, and prepn. method thereof |
CN1406991A (en) * | 2001-08-21 | 2003-04-02 | 拜尔公司 | Preparation of isomeric olefine copolymer |
CN1502639A (en) * | 2002-11-21 | 2004-06-09 | 中国石油化工股份有限公司 | Method for preparing isobutylene block copolymer by sequential initiation |
CN102372810A (en) * | 2010-08-19 | 2012-03-14 | 中国石油化工股份有限公司 | Method for preparing isomonoolefin-polyene hydrocarbon copolymer |
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Non-Patent Citations (1)
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Application publication date: 20170714 |