CN109180868A - The production method of cis-butenedioic anhydride graft type the third ground rubber of second - Google Patents
The production method of cis-butenedioic anhydride graft type the third ground rubber of second Download PDFInfo
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- CN109180868A CN109180868A CN201810923826.3A CN201810923826A CN109180868A CN 109180868 A CN109180868 A CN 109180868A CN 201810923826 A CN201810923826 A CN 201810923826A CN 109180868 A CN109180868 A CN 109180868A
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- rubber
- butenedioic anhydride
- useless
- production method
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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
- C08F255/04—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 on to ethene-propene copolymers
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- 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
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
-
- 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
- C08K5/10—Esters; Ether-esters
- C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids
Abstract
The invention discloses the production methods of cis-butenedioic anhydride graft type the third ground rubber of second.This method is to be uniformly mixed cis-butenedioic anhydride, auxiliary agent, useless the third rubber powder of second in a high speed mixer；Subsequently into multi-functional rubber and plastic processing unit (plant), under microwave action, second the third rubber powder chain rupture regeneration of giving up, while graft reaction occurs for cis-butenedioic anhydride and the third glue of second, and the third ground rubber of graft type second is made.Production method of the invention avoids the autohemagglutination of grafted monomers under hot conditions, polymer decomposes and volatile organic gases generates, and is conducive to environmental protection, while improving material property.
Description
Technical field
The present invention relates to the production methods of cis-butenedioic anhydride graft type the third ground rubber of second, belong to high molecular material graft modification technology
Field.
Background technique
Non-polar polymer and other materials, such as polar polymer, inorganic filler compatibility are very poor, can not prepare useful
Intermingling material.Expanding material that is previously prepared or being formed in situ is added, script incompatible polymers can be made to be formed with any
The blend for the peculiar property that component does not have.
So far, due to cheap, high activity and good processability, maleic anhydride grafted polymer is most important function
Can change material, improve the interfacial adhesion in blend between dispersed phase and continuous phase, it blend polymer, polymer/
Inorganic filler, polymer/organic fiber, composite reinforcing material and binder etc. are all widely used.Maleic anhydride with
Polyolefine material has good grafting performance, while can assign its polarity and new reactivity and be widely used, on the one hand
Determined by the structure of its carbon-to-carbon double bond, radical reaction and photochemical reaction can be participated in, on the other hand acid anhydrides as contained by it or
The reactivity of carboxylic acid group, some groups or molecule can occur amidation, esterification etc. with it and react.
Although EP rubbers has very high elasticity, excellent ageing-resistant performance, its polarity is low, (such as with polar resin
PET, PBT, PA etc.) poor compatibility, serious two-phase laminated flow can occur after simple blend, lead to the degradation of blend, therefore
EP rubbers must be modified.
It is functionalized the reactive acid anhydrides or carboxylic acid group of EP rubbers polarized on side chain, can be had with polar resin
Preferable compatibility, and can be chemically reacted with polar resin；And main chain and EP rubbers have good compatibility,
Therefore the performance of blend can be greatlyd improve after being added.The preparation method of functionalization EP rubbers has very much, such as fusion-grafting
Method, solution grafting, solid-state grafting etc..
Since melt grafting is without using solvent, continuous life can be formed using continuous mixing device (such as double screw extruder)
It produces, preparation method is simple, without post-processing, it has also become be functionalized the mainstream preparation method of EP rubbers.Melt grafting at present
The method of preparation functionalization EP rubbers, is being usually to be generated under EP rubbers is in a molten state by decomposition of initiator
Living radical, and then cause and generated free radicals on EP rubbers macromolecular chain, then occur certainly with double bond containing carboxylic acid or acid anhydrides
By base graft reaction, to obtain graft product.This method is mainly in consersion units such as screw extruder, mixer, open mills
Middle progress.
Melt grafting has several serious urgent need to resolve: 1) unsaturated carboxylic acid or acid anhydrides are easily waved at high temperature
Hair, the micro-tapping volatilized is larger, is harmful to the human body, and not only affects environment, but also reduce the service efficiency of raw material；2) anti-
Answer temperature high, radical initiator not only can initiation grafting reaction, can similarly cause the crosslinking of EP rubbers, free radical causes
The increase of agent dosage can improve the gel content of graft, so that poor processability；Although 3) improve radical initiator
Grafting rate can be improved in dosage, but in order to control gel content, usually controls the dosage of radical initiator in reduced levels,
The functionalization EP rubbers grafting rate prepared is very low.
To solve the above problems, present invention research, develop the production of cis-butenedioic anhydride graft type the third ground rubber of second
Method.
Summary of the invention
Microwave heat and induced chemical reaction in terms of be widely used, application is more especially in terms of induced chemical reaction
By force.Microwave heating be using heated material polar molecule in microwave electromagnetic field (frequency 2450MHz) fast steering and
It aligns, to generate tearing and phase mutual friction and generate heat.Microwave induction catalytic reaction is by high-intensitive short pulse microwave spoke
It penetrates and focuses on the solid catalyst bed surface containing certain " substance ", due to the strong work of surface metal point and microwave energy
With microwave energy will be converted heat, to make certain surface points be selectively heated to very high temperature quickly, in reactor
Material can react when contacting with the surface point being stimulated.
Microwave technology Heterosis exists: (1) microwave has very strong penetrability, and homogeneous heating can directly act on and be added
Hot substance makes to heat and act on together inside and outside it, and moment can reach predetermined temperature；(2) it is transported at a high speed under microwave electromagnetic field action
It is dynamic, the contact probability of auxiliary agent and material is greatly increased, contact interface is constantly updated, thus can increase substantially reaction speed,
And auxiliary agent is made to be fully used.(3) microwave treatment be not in hot-spot, it is partially carbonized, agglomeration phenomena such as, it is easy to accomplish
Automation, mitigates the working strength of operator.
The multi-functional rubber and plastic processing unit (plant) that the present invention uses is the entitled multi-functional rubber and plastic processing unit (plant) (patent No.
CN201720960911 the equipment described in).
Therefore, the present invention provides the production technology schemes of following cis-butenedioic anhydride graft type the third ground rubber of second:
The production method of cis-butenedioic anhydride graft type the third ground rubber of second, it is characterised in that: (1) by cis-butenedioic anhydride, auxiliary agent, useless the third rubber powder of second in height
It is uniformly mixed in fast mixing machine；(2) under nitrogen protection state, cis-butenedioic anhydride, auxiliary agent, useless second the third rubber powder mixture are added multi-functional
It is preheated under rubber and plastic processing unit (plant) stirring；(3) start microwave generator, reacted 10-150 minutes under microwave action, make to give up
Second the third rubber powder chain rupture regeneration, while making cis-butenedioic anhydride and EP rubbers molecule that graft reaction occur, the third ground rubber of graft type second is made.
The partial size of useless the third rubber powder of second is -100 mesh of 20 mesh.
Cis-butenedioic anhydride additional amount is the 0.3-10% of useless the third rubber powder of second quality.
Auxiliary agent is the mixture of peroxide cumyl peroxide Yu filler phthalic acid ester；Peroxide peroxide
Change the 0-0.10% that diisopropylbenzene (DIPB) additional amount is useless the third rubber powder of second quality, filler phthalic acid ester additional amount is useless the third glue of second
The 0-10% of silty amount.
Cis-butenedioic anhydride, auxiliary agent, useless second the third rubber powder mixture are 30 DEG C -70 DEG C in the preheating temperature of multi-functional rubber and plastic processing unit (plant).
The thermos have the advantages that
1, using high-speed mixer, cis-butenedioic anhydride, auxiliary agent, useless the third rubber powder of second can be made to be sufficiently mixed uniformly.
2, using nitrogen protection, it can prevent material from oxidation side reaction occurs.
3, cis-butenedioic anhydride, auxiliary agent, useless the third rubber powder of second mixture preheating temperature are 30 DEG C -70 DEG C, microwave can be made directly to make
With.
4, the microwave generator of multi-functional rubber and plastic processing unit (plant) can not only make useless second the third rubber powder chain rupture regeneration, but also can make suitable
Graft reaction occurs for acid anhydride and rubber molecule.
Specific embodiment
Below with reference to embodiment, the invention will be further described, and embodiment is merely to illustrate the present invention rather than limitation
The scope of the present invention, after having read content of the present invention, those skilled in the art to the present invention make it is various change or
Modification, such equivalent forms equally fall within following claims limited range.
Embodiment
1, it is as follows to prepare equipment, facility: (1) high-speed mixer is used in 10 liters of experiments；(2) 10 liters of experiment electricity consumption heated multi-functions
Rubber and plastic process equipment (air-cooled microwave generator power: 2000 watts)；(3) industrial nitrogen (99%).
2, following components is weighed according to parts by weight: (1) useless the third rubber powder of second of 40 mesh: 3000 grams；(2) cis-butenedioic anhydride (99.5%): 90
Gram；(3) repefral (99%): 110 grams；(4) peroxide cumyl peroxide DCP(98%): 2.0 grams.
3, above-mentioned cis-butenedioic anhydride, auxiliary agent, useless the third rubber powder of second are blended 2-5 minutes in 10 liters of experiment high-speed mixers, are made
Temperature of charge is not higher than 50 DEG C.
4, the cis-butenedioic anhydride mixed, auxiliary agent, useless the third rubber powder of second mixture are added to 10 liters of experiment electricity consumption heated multi-function rubbers
It moulds in process equipment, opens nitrogen protection valve, be passed through nitrogen.
5, starting stirs, is heated to 50 DEG C, starts microwave generator, microwave treatment material 15 minutes, closes microwave
Device.
6, nitrogen protection is stirred for 5 minutes, and blowing obtains the third ground rubber of second of cis-butenedioic anhydride grafting.
Claims (5)
1. the production method of cis-butenedioic anhydride graft type the third ground rubber of second, it is characterised in that: (1) by the measured cis-butenedioic anhydride of poidometer, auxiliary agent,
Useless the third rubber powder of second is uniformly mixed in a high speed mixer；(2) under nitrogen protection state, by cis-butenedioic anhydride, auxiliary agent, useless the third glue of second
Powder mixture is added under multi-functional rubber and plastic processing unit (plant) stirring and preheats；(3) start microwave generator, it is anti-under microwave action
It answers 10-150 minutes, makes useless second the third rubber powder chain rupture regeneration, while making cis-butenedioic anhydride and EP rubbers molecule that graft reaction occur, be made and connect
Branch type the third ground rubber of second.
2. the production method of cis-butenedioic anhydride graft type the third ground rubber of second, it is characterised in that: the partial size of useless the third rubber powder of second is 20 mesh -100
Mesh.
3. the production method of cis-butenedioic anhydride graft type the third ground rubber of second, it is characterised in that: cis-butenedioic anhydride additional amount is useless the third rubber powder of second quality
0.3-10%.
4. the production method of cis-butenedioic anhydride graft type the third ground rubber of second, it is characterised in that: auxiliary agent is peroxide peroxidating diisopropyl
The mixture of benzene and filler phthalic acid ester；Peroxide cumyl peroxide additional amount is useless the third rubber powder of second quality
0-0.10%, filler phthalic acid ester additional amount are the 0-10% of useless the third rubber powder of second quality.
5. the production method of cis-butenedioic anhydride graft type the third ground rubber of second, it is characterised in that: cis-butenedioic anhydride, auxiliary agent, useless the third rubber powder of second mixture
It is 30 DEG C -70 DEG C in the preheating temperature of multi-functional rubber and plastic process equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810923826.3A CN109180868A (en) | 2018-08-11 | 2018-08-11 | The production method of cis-butenedioic anhydride graft type the third ground rubber of second |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810923826.3A CN109180868A (en) | 2018-08-11 | 2018-08-11 | The production method of cis-butenedioic anhydride graft type the third ground rubber of second |
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| Publication Number | Publication Date |
|---|---|
| CN109180868A true CN109180868A (en) | 2019-01-11 |
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| CN201810923826.3A Withdrawn CN109180868A (en) | 2018-08-11 | 2018-08-11 | The production method of cis-butenedioic anhydride graft type the third ground rubber of second |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999048960A1 (en) * | 1998-03-23 | 1999-09-30 | Chandrasekaran Pillai | Process for the manufacture of quality reclaimed rubber |
| CN1974621A (en) * | 2006-12-07 | 2007-06-06 | 武汉工程大学 | Modified rubber powder and its prepn and use |
| CN101580558A (en) * | 2008-05-13 | 2009-11-18 | 住友橡胶工业株式会社 | Modified natural rubber, method for producing modified natural rubber, rubber composition, and tire |
| CN107033385A (en) * | 2017-05-06 | 2017-08-11 | 洛阳和梦科技有限公司 | Scrap rubber regenerated environment protecting method |
| CN206999371U (en) * | 2017-05-06 | 2018-02-13 | 洛阳和梦科技有限公司 | Multi-functional plastic cement processing unit (plant) |
-
2018
- 2018-08-11 CN CN201810923826.3A patent/CN109180868A/en not_active Withdrawn
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999048960A1 (en) * | 1998-03-23 | 1999-09-30 | Chandrasekaran Pillai | Process for the manufacture of quality reclaimed rubber |
| CN1974621A (en) * | 2006-12-07 | 2007-06-06 | 武汉工程大学 | Modified rubber powder and its prepn and use |
| CN101580558A (en) * | 2008-05-13 | 2009-11-18 | 住友橡胶工业株式会社 | Modified natural rubber, method for producing modified natural rubber, rubber composition, and tire |
| CN107033385A (en) * | 2017-05-06 | 2017-08-11 | 洛阳和梦科技有限公司 | Scrap rubber regenerated environment protecting method |
| CN206999371U (en) * | 2017-05-06 | 2018-02-13 | 洛阳和梦科技有限公司 | Multi-functional plastic cement processing unit (plant) |
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Application publication date: 20190111 |