CN115449018A - Maleic anhydride grafted modified ABS resin material extruded by double screw reaction and preparation method thereof - Google Patents

Maleic anhydride grafted modified ABS resin material extruded by double screw reaction and preparation method thereof Download PDF

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CN115449018A
CN115449018A CN202211305919.2A CN202211305919A CN115449018A CN 115449018 A CN115449018 A CN 115449018A CN 202211305919 A CN202211305919 A CN 202211305919A CN 115449018 A CN115449018 A CN 115449018A
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maleic anhydride
styrene
temperature
abs
zone
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汤冰炜
汤金城
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Shanghai Changya Petrochemical Co ltd
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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
    • C08F279/00—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00
    • C08F279/02—Macromolecular compounds obtained by polymerising monomers on to polymers of monomers having two or more carbon-to-carbon double bonds as defined in group C08F36/00 on to polymers of conjugated dienes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
    • C08L51/04—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to rubbers

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Abstract

The invention discloses a maleic anhydride grafted modified ABS resin material extruded by double screw reaction and a preparation method thereof, relating to the technical field of high polymer materials. The maleic anhydride graft modified ABS resin material comprises the following components in percentage by weight: 30-40% of styrene-butadiene rubber, 49.4-26.5% of styrene, 20-30% of acrylonitrile, 0.5-3% of maleic anhydride and 0.1-0.5% of initiator. The invention takes Styrene Butadiene Rubber (SBR) as a matrix polymer, takes styrene (St) monomer, maleic Anhydride (MAH) monomer and Acrylonitrile (AN) monomer as reaction monomers, and forms ABS-g-MAH graft copolymer by polymerization under the action of a free radical initiator. The ABS-g-MAH produced by the invention has extremely low free MAH content and extremely high grafting rate, and completely meets the requirement of PC/ABS alloy on ABS-g-MAH compatilizer.

Description

Maleic anhydride grafted modified ABS resin material extruded by double screw reaction and preparation method thereof
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a maleic anhydride grafted modified ABS resin material extruded by double screw reaction and a preparation method thereof.
Background
ABS (acrylonitrile/butadiene/styrene copolymer) has excellent mechanical properties as important engineering plastics, but the ABS has the disadvantage of poor heat resistance, in order to improve the heat resistance of the ABS, the ABS and polycarbonate PC are commonly modified to form PC/ABS alloy, and the PC/ABS alloy has more excellent heat resistance and impact property compared with the ABS, but the compatibility of the ABS resin and the PC resin is poor, and if no compatilizer is added, the ABS and the PC resin are difficult to disperse well in the blending process, so that the mechanical properties of the final PC/ABS alloy material are influenced.
The most commonly used compatilizer for PC/ABS alloy materials is ABS grafted maleic anhydride, the traditional production method is to carry out reaction grafting modification by a double-screw extruder, ABS resin and maleic anhydride monomer carry out melt grafting reaction in the double-screw extruder under the action of a free radical initiator, and the production process has the defects that the grafting rate of the final maleic anhydride is very low due to the low reaction activity of the maleic anhydride, and the content of free maleic anhydride in the product is extremely high, so that the use requirement cannot be met.
Disclosure of Invention
Aiming at the defects of the prior art, the invention adopts a double-screw extruder with high length-diameter ratio as a reactor, does not add any solvent, takes Styrene Butadiene Rubber (SBR) as a matrix polymer, takes a styrene (St) monomer, a Maleic Anhydride (MAH) monomer and AN Acrylonitrile (AN) monomer as reaction monomers, and polymerizes to form the ABS-g-MAH graft copolymer under the action of a free radical initiator. The ABS-g-MAH produced by the invention has extremely low free MAH content and extremely high grafting rate, and completely meets the requirement of PC/ABS alloy on ABS-g-MAH compatilizer.
The invention is realized by adopting the following technical scheme:
a maleic anhydride grafted modified ABS resin material extruded by double screw reaction comprises the following components in percentage by weight:
Figure BDA0003906006460000011
Figure BDA0003906006460000021
the sum of the weight percentages of the components is 100 percent.
Preferably, the initiator is a free radical initiator, and comprises at least one of azo initiators and organic peroxide initiators.
Preferably, the styrene-butadiene rubber is selected from styrene-butadiene rubbers with a styrene content of 20-40 wt%.
The invention also provides a preparation method of the maleic anhydride graft modified ABS composition by double-screw reactive extrusion, which comprises the following steps:
(1) Weighing styrene butadiene rubber according to a proportion, adding the styrene butadiene rubber into a double-screw extruder through a main feed, and stirring;
(2) Weighing the rest components in proportion, mixing to obtain uniform mixed solution, injecting the mixed solution into a double-screw extruder through a liquid material feeding port for reaction, carrying out copolymerization reaction on styrene, acrylonitrile and maleic anhydride under the initiation action of a free radical initiator under the high temperature and shearing dispersion action of a threaded element in the extruder, and then grafting a part of three monomers of styrene, acrylonitrile and maleic anhydride onto a butadiene styrene rubber molecular chain to form the ABS-g-MAH graft copolymer.
Preferably, the screw length-diameter ratio of the twin-screw extruder in step (1) is 64.
Preferably, the liquid material feeding port in the step (2) is positioned at the position where the length-diameter ratio of a screw of the twin-screw extruder is 15.
Preferably, the process parameters of the twin-screw extruder in the step (2) are as follows:
the temperature of the zone 1 is 170-180 ℃, the temperature of the zone 2 is 170-180 ℃, the temperature of the zone 3 is 180-190 ℃, the temperature of the zone 4 is 190-200 ℃, the temperature of the die head is 200-210 ℃, and the rotating speed of the screw machine is 250r/min.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, a double-screw extruder is used as a reaction container, a terpolymer is formed through a copolymer reaction among three monomers of styrene, acrylonitrile and maleic anhydride, and then the terpolymer is grafted to a styrene butadiene rubber molecular chain, and because the reactivity ratio of the copolymerization reaction among styrene/maleic anhydride is far greater than 1, free maleic anhydride hardly exists in a final product, which is equivalent to that the grafting ratio of the final maleic anhydride reaches nearly 100%, so that the grafting ratio of the ABS-g-MAH graft copolymer can be accurately controlled by adopting the method disclosed by the invention, which cannot be realized by the traditional production method, and the method has great advantages.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to make the objects, features and advantages thereof more comprehensible. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Example 1
(1) Weighing 30 kg of styrene butadiene rubber SBR-1011 (tableted), adding the styrene butadiene rubber into a double-screw extruder with the length-diameter ratio of 64;
(2) Dissolving 0.1 kg of free radical initiator AIBN and 0.5 kg of maleic anhydride monomer into 49.4 kg of styrene and 20 kg of acrylonitrile liquid to form uniform mixed liquid; then injecting the mixture into a double-screw extruder through a liquid material feeding port at the position of 15 length-diameter ratio of the extruder at 1 by using a liquid high-pressure plunger metering pump, and uniformly dispersing the mixture in the styrene butadiene rubber melt under the action of a thread element of the double-screw extruder;
weighing the rest components in proportion, mixing to obtain uniform mixed solution, injecting the mixed solution into a double-screw extruder through a liquid material feeding port for reaction, carrying out copolymerization reaction on styrene, acrylonitrile and maleic anhydride under the initiation action of a free radical initiator under the high temperature and shearing dispersion action of a threaded element in the extruder, and then grafting a part of three monomers of styrene, acrylonitrile and maleic anhydride onto a butadiene styrene rubber molecular chain to form the ABS-g-MAH graft copolymer. Under the high temperature in the extruder and the shearing and dispersing action of the screw element, styrene, acrylonitrile and maleic anhydride are subjected to copolymerization reaction under the initiation action of a free radical initiator, a part of three monomers of the styrene, the acrylonitrile and the maleic anhydride are copolymerized and then grafted to a styrene butadiene rubber molecular chain to form an ABS-g-MAH graft copolymer, and extrusion granulation is carried out to obtain the finished material finally. Wherein the technological parameters of the double-screw extruder are as follows:
the temperature of the zone 1 is 170-180 ℃, the temperature of the zone 2 is 170-180 ℃, the temperature of the zone 3 is 180-190 ℃, the temperature of the zone 4 is 190-200 ℃, the temperature of the die head is 200-210 ℃, and the rotating speed of the screw machine is 250r/min.
Example 2
(1) Weighing 32 kg of styrene butadiene rubber SBR-1011 (tableted), adding the styrene butadiene rubber into a double-screw extruder with the length-diameter ratio of 64;
(2) Dissolving 0.2 kg of free radical initiator AIBN and 1 kg of maleic anhydride monomer into 44.8 kg of styrene and 22 kg of acrylonitrile liquid to form uniform mixed liquid; then injecting the mixture into a double-screw extruder through a liquid material feeding port at the position of 15 length-diameter ratio of the extruder at 1 by using a liquid high-pressure plunger metering pump, and uniformly dispersing the mixture in the styrene butadiene rubber melt under the action of a thread element of the double-screw extruder;
weighing the rest components in proportion, mixing to obtain uniform mixed solution, injecting the mixed solution into a double-screw extruder through a liquid material feeding port for reaction, carrying out copolymerization reaction on styrene, acrylonitrile and maleic anhydride under the initiation action of a free radical initiator under the high temperature and shearing dispersion action of a threaded element in the extruder, and then grafting a part of three monomers of styrene, acrylonitrile and maleic anhydride onto a butadiene styrene rubber molecular chain to form the ABS-g-MAH graft copolymer. Under the high temperature in the extruder and the shearing and dispersing action of the screw element, styrene, acrylonitrile and maleic anhydride are subjected to copolymerization reaction under the initiation action of a free radical initiator, a part of three monomers of the styrene, the acrylonitrile and the maleic anhydride are copolymerized and then grafted to a styrene butadiene rubber molecular chain to form an ABS-g-MAH graft copolymer, and extrusion granulation is carried out to obtain the finished material finally. Wherein the technological parameters of the double-screw extruder are as follows:
the temperature of the zone 1 is 170-180 ℃, the temperature of the zone 2 is 170-180 ℃, the temperature of the zone 3 is 180-190 ℃, the temperature of the zone 4 is 190-200 ℃, the temperature of the die head is 200-210 ℃, and the rotating speed of the screw machine is 250r/min.
Example 3
(1) Weighing 35 kg of styrene butadiene rubber SBR-1011 (tableted), adding the styrene butadiene rubber SBR-1011 into a double-screw extruder with the length-diameter ratio of 64;
(2) Dissolving 0.3 kg of free radical initiator AIBN and 1.5 kg of maleic anhydride monomer into 38.2 kg of styrene and 25 kg of acrylonitrile liquid to form uniform mixed liquid; then injecting the mixture into a double-screw extruder through a liquid material feeding port at the position of 15 length-diameter ratio of the extruder at 1 by using a liquid high-pressure plunger metering pump, and uniformly dispersing the mixture in the styrene butadiene rubber melt under the action of a thread element of the double-screw extruder;
weighing the rest components in proportion, mixing to obtain uniform mixed solution, injecting the mixed solution into a double-screw extruder through a liquid material feeding port for reaction, carrying out copolymerization reaction on styrene, acrylonitrile and maleic anhydride under the initiation action of a free radical initiator under the high temperature and shearing dispersion action of a threaded element in the extruder, and then grafting a part of three monomers of styrene, acrylonitrile and maleic anhydride onto a butadiene styrene rubber molecular chain to form the ABS-g-MAH graft copolymer. Under the high temperature in the extruder and the shearing and dispersing action of the screw element, styrene, acrylonitrile and maleic anhydride are subjected to copolymerization reaction under the initiation action of a free radical initiator, a part of three monomers of the styrene, the acrylonitrile and the maleic anhydride are copolymerized and then grafted to a styrene butadiene rubber molecular chain to form an ABS-g-MAH graft copolymer, and extrusion granulation is carried out to obtain the finished material finally. Wherein the technological parameters of the double-screw extruder are as follows:
the temperature of the zone 1 is 170-180 ℃, the temperature of the zone 2 is 170-180 ℃, the temperature of the zone 3 is 180-190 ℃, the temperature of the zone 4 is 190-200 ℃, the temperature of the die head is 200-210 ℃, and the rotating speed of the screw machine is 250r/min.
Example 4
(1) Weighing 37 kg of styrene butadiene rubber SBR-1011 (tableted), adding the styrene butadiene rubber into a double-screw extruder with the length-diameter ratio of 64;
(2) Dissolving 0.2 kg of free radical initiator BPO, 0.2 kg of free radical initiator AIBN and 2 kg of maleic anhydride monomer into 33.6 kg of styrene and 27 kg of acrylonitrile liquid to form uniform mixed liquid; then injecting the mixture into a double-screw extruder through a liquid material feeding port at the position of 15 length-diameter ratio of the extruder at 1 by using a liquid high-pressure plunger metering pump, and uniformly dispersing the mixture in the styrene butadiene rubber melt under the action of a thread element of the double-screw extruder;
weighing the rest components in proportion, mixing to obtain a uniform mixed solution, injecting the mixed solution into a double-screw extruder through a liquid material feeding port for reaction, carrying out copolymerization reaction on styrene, acrylonitrile and maleic anhydride under the initiating action of a free radical initiator under the high temperature and shearing dispersion action of a threaded element in the extruder, and then grafting a part of three monomers of styrene, acrylonitrile and maleic anhydride onto a styrene butadiene rubber molecular chain to form the ABS-g-MAH graft copolymer. Under the high temperature in the extruder and the shearing dispersion action of the thread element, styrene, acrylonitrile and maleic anhydride are subjected to copolymerization reaction under the initiation action of a free radical initiator, a part of three monomers of styrene, acrylonitrile and maleic anhydride are copolymerized and then grafted onto a styrene butadiene rubber molecular chain to form an ABS-g-MAH graft copolymer, and extrusion granulation is carried out to obtain the finished product material finally. Wherein the technological parameters of the double-screw extruder are as follows:
the temperature of the zone 1 is 170-180 ℃, the temperature of the zone 2 is 170-180 ℃, the temperature of the zone 3 is 180-190 ℃, the temperature of the zone 4 is 190-200 ℃, the temperature of the die head is 200-210 ℃, and the rotating speed of the screw machine is 250r/min.
Example 5
(1) Weighing 40 kg of styrene butadiene rubber SBR-1011 (tableted), adding the styrene butadiene rubber into a double-screw extruder with the length-diameter ratio of 64;
(2) Dissolving 0.25 kg of free radical initiator BPO, 0.25 kg of free radical initiator AIBN and 3 kg of maleic anhydride monomer into 26.5 kg of styrene and 30 kg of acrylonitrile liquid to form uniform mixed liquid; then injecting the mixture into a double-screw extruder through a liquid material feeding port at the position of 15 length-diameter ratio of the extruder at 1 by using a liquid high-pressure plunger metering pump, and uniformly dispersing the mixture in the styrene butadiene rubber melt under the action of a thread element of the double-screw extruder;
weighing the rest components in proportion, mixing to obtain uniform mixed solution, injecting the mixed solution into a double-screw extruder through a liquid material feeding port for reaction, carrying out copolymerization reaction on styrene, acrylonitrile and maleic anhydride under the initiation action of a free radical initiator under the high temperature and shearing dispersion action of a threaded element in the extruder, and then grafting a part of three monomers of styrene, acrylonitrile and maleic anhydride onto a butadiene styrene rubber molecular chain to form the ABS-g-MAH graft copolymer. Under the high temperature in the extruder and the shearing and dispersing action of the screw element, styrene, acrylonitrile and maleic anhydride are subjected to copolymerization reaction under the initiation action of a free radical initiator, a part of three monomers of the styrene, the acrylonitrile and the maleic anhydride are copolymerized and then grafted to a styrene butadiene rubber molecular chain to form an ABS-g-MAH graft copolymer, and extrusion granulation is carried out to obtain the finished material finally. Wherein the technological parameters of the double-screw extruder are as follows:
the temperature of the zone 1 is 170-180 ℃, the temperature of the zone 2 is 170-180 ℃, the temperature of the zone 3 is 180-190 ℃, the temperature of the zone 4 is 190-200 ℃, the temperature of the die head is 200-210 ℃, and the rotating speed of the screw machine is 250r/min.
Comparative example 1
After 99.4 kg of ABS 750A (tableted), 0.5 kg of maleic anhydride monomer and 0.1 kg of free radical initiator AIBN are mixed uniformly, a reaction type double-screw extruder with the length-diameter ratio of 64 is added through a main feed, and the extrusion temperature of each section is as follows:
the temperature of the zone 1 is 170-180 ℃, the temperature of the zone 2 is 170-180 ℃, the temperature of the zone 3 is 180-190 ℃, the temperature of the zone 4 is 190-200 ℃, the temperature of the die head is 200-210 ℃, and the rotating speed of the screw machine is 250r/min.
Under the shearing dispersion of the screw element of the double-screw extruder and the initiation action of an initiator, a part of maleic anhydride monomer is self-polymerized, and a part of maleic anhydride monomer is graft copolymerized to an ABS molecular chain, and then extrusion granulation is carried out, and finally the finished product material is obtained.
Comparative example 2
98.8 kg of ABS 709 (tabletization), 1 kg of maleic anhydride monomer and 0.2 kg of free radical initiator AIBN are mixed uniformly and added into a reaction type double-screw extruder with the length-diameter ratio of 64 through main feeding, and the extrusion temperature of each section is as follows:
the temperature of the zone 1 is 170-180 ℃, the temperature of the zone 2 is 170-180 ℃, the temperature of the zone 3 is 180-190 ℃, the temperature of the zone 4 is 190-200 ℃, the temperature of the die head is 200-210 ℃, and the rotating speed of the screw machine is 250r/min.
Under the shearing dispersion of the screw element of the double-screw extruder and the initiation action of an initiator, a part of maleic anhydride monomer is self-polymerized, and a part of maleic anhydride monomer is graft copolymerized to an ABS molecular chain, and then extrusion granulation is carried out, and finally the finished product material is obtained.
Comparative example 3
98.2 kg of ABS 0215A (Taiwan), 1.5 kg of maleic anhydride monomer and 0.3 kg of free radical initiator BPO are mixed uniformly and added into a reaction type double-screw extruder with the length-diameter ratio of 64 through a main feed, and the extrusion temperature of each section is as follows:
the temperature of the zone 1 is 170-180 ℃, the temperature of the zone 2 is 170-180 ℃, the temperature of the zone 3 is 180-190 ℃, the temperature of the zone 4 is 190-200 ℃, the temperature of the die head is 200-210 ℃, and the rotating speed of the screw machine is 250r/min.
Under the shearing dispersion of the screw element of the double-screw extruder and the initiation action of an initiator, a part of maleic anhydride monomer is self-polymerized, and a part of maleic anhydride monomer is graft copolymerized to an ABS molecular chain, and then extrusion granulation is carried out, and finally the finished product material is obtained.
Comparative example 4
97.6 kg of ABS 0150 (tabletization), 2 kg of maleic anhydride monomer, 0.2 kg of free radical initiator BPO and 0.2 kg of free radical initiator AIBN are uniformly mixed and then added into a reaction type double-screw extruder with the length-diameter ratio of 64 through a main feeding, and the extrusion temperature of each section is as follows:
the temperature of the zone 1 is 170-180 ℃, the temperature of the zone 2 is 170-180 ℃, the temperature of the zone 3 is 180-190 ℃, the temperature of the zone 4 is 190-200 ℃, the temperature of the die head is 200-210 ℃, and the rotating speed of the screw machine is 250r/min.
Under the shearing dispersion of the screw element of the double-screw extruder and the initiation action of an initiator, a part of maleic anhydride monomer is polymerized by self, and a part of maleic anhydride monomer is grafted and copolymerized to an ABS molecular chain, and then extrusion granulation is carried out, thus finally obtaining the finished product material.
Comparative example 5
96.5 kg of ABS 750N (tabletization), 3 kg of maleic anhydride monomer, 0.25 kg of free radical initiator BPO and 0.25 kg of free radical initiator AIBN are uniformly mixed and then added into a reaction type double-screw extruder with the length-diameter ratio of 64 through a main feed, and the extrusion temperature of each section is controlled as follows:
the temperature of the zone 1 is 170-180 ℃, the temperature of the zone 2 is 170-180 ℃, the temperature of the zone 3 is 180-190 ℃, the temperature of the zone 4 is 190-200 ℃, the temperature of the die head is 200-210 ℃, and the rotating speed of the screw machine is 250r/min.
Under the shearing dispersion of the screw element of the double-screw extruder and the initiation action of an initiator, a part of maleic anhydride monomer is self-polymerized, and a part of maleic anhydride monomer is graft copolymerized to an ABS molecular chain, and then extrusion granulation is carried out, and finally the finished product material is obtained.
After 10 total materials of comparative examples 1 to 5 and examples 1 to 5 were passed through a Soxhlet extractor to remove free maleic anhydride, the final graft ratio of maleic anhydride was determined by titration, as detailed in Table 1.
TABLE 1 maleic anhydride graft ratio of comparative and example materials
Figure BDA0003906006460000071
Figure BDA0003906006460000081
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (7)

1. A maleic anhydride grafted modified ABS resin material extruded by double screw reaction is characterized by comprising the following components in percentage by weight:
Figure FDA0003906006450000011
the sum of the weight percentages of the components is 100 percent.
2. The twin-screw reactive extrusion maleic anhydride graft modified ABS resin material of claim 1 wherein the initiator is a free radical initiator including at least one of azo type initiators, organic peroxide type initiators.
3. The maleic anhydride graft-modified ABS resin material as claimed in claim 1, wherein the styrene-butadiene rubber is selected from styrene-butadiene rubbers having a styrene content of 20-40 wt%.
4. The preparation method of the maleic anhydride graft modified ABS composition by the twin-screw reactive extrusion according to any one of claims 1 to 3, characterized by comprising the steps of:
(1) Weighing styrene butadiene rubber according to a proportion, and adding the styrene butadiene rubber into a double-screw extruder through a main feed to be stirred;
(2) Weighing the rest components in proportion, mixing to obtain uniform mixed solution, and injecting the mixed solution into a double-screw extruder through a liquid material feeding port for reaction to obtain the maleic anhydride grafted modified ABS resin material.
5. The production method according to claim 4, wherein the screw length-diameter ratio of the twin-screw extruder in step (1) is 64.
6. The method for preparing the rubber composition according to claim 4, wherein the liquid material feeding port in the step (2) is positioned at a length-diameter ratio of 15.
7. The preparation method according to claim 4, wherein the twin-screw extruder of step (2) has the following process parameters:
the temperature of the zone 1 is 170-180 ℃, the temperature of the zone 2 is 170-180 ℃, the temperature of the zone 3 is 180-190 ℃, the temperature of the zone 4 is 190-200 ℃, the temperature of the die head is 200-210 ℃, and the rotating speed of the screw machine is 250r/min.
CN202211305919.2A 2022-10-24 2022-10-24 Maleic anhydride grafted modified ABS resin material extruded by double screw reaction and preparation method thereof Pending CN115449018A (en)

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