CN114163558B - Acrylate rubber and preparation method and application thereof - Google Patents

Acrylate rubber and preparation method and application thereof Download PDF

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CN114163558B
CN114163558B CN202010947445.6A CN202010947445A CN114163558B CN 114163558 B CN114163558 B CN 114163558B CN 202010947445 A CN202010947445 A CN 202010947445A CN 114163558 B CN114163558 B CN 114163558B
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acrylate rubber
acrylate
monomer
polymerization
tubular reactor
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CN114163558A (en
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杜影
齐可非
赵丽娜
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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Sinopec Beijing Research Institute of Chemical Industry
China Petroleum and Chemical Corp
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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
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1802—C2-(meth)acrylate, e.g. ethyl (meth)acrylate
    • 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
    • C08F2/001—Multistage polymerisation processes characterised by a change in reactor conditions without deactivating the intermediate polymer
    • 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
    • C08F2/01—Processes of polymerisation characterised by special features of the polymerisation apparatus used
    • 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
    • C08F2/02—Polymerisation in bulk

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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)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
  • Graft Or Block Polymers (AREA)

Abstract

The invention relates to the field of rubber preparation, and discloses acrylate rubber and a preparation method and application thereof. The preparation method comprises the following steps: s1, premixing: premixing a polymerization monomer and an initiator to obtain a premix; s2, polymerization reaction: transferring the premix obtained in the step S1 into a polymerization reaction device for polymerization reaction; wherein the polymerization reaction device is a tubular reactor and/or a double-screw extruder. The preparation method can accurately control the polymerization heat during the polymerization reaction of the acrylate rubber, realizes the continuous production of the acrylate rubber, and the acrylate rubber prepared by the method has high molecular weight, low gel content and low volatile matter.

Description

Acrylate rubber and preparation method and application thereof
Technical Field
The invention relates to the field of rubber preparation, in particular to acrylate rubber and a preparation method and application thereof.
Background
The acrylate rubber is an elastomer obtained by copolymerizing acrylate serving as a main monomer, the main chain of the acrylate rubber is a saturated carbon chain, the side group of the acrylate rubber is a polar ester group, and the acrylate rubber has excellent heat resistance, aging resistance, oil resistance, ozone resistance, ultraviolet resistance and other properties.
At present, there are two main methods for producing acrylate rubber, namely, suspension polymerization (represented by Goodrich corporation in the united states) and emulsion polymerization (represented by east asia paint corporation in japan). In addition, du Pont developed a solution polymerization process specifically for the copolymerization of acrylates with olefins. All three methods have a series of problems, such as the need of recovering a large amount of water or solvent, complex synthesis process, and unfavorable post-processing caused by the residual additives in the polymer. The conventional bulk polymerization method is difficult to industrialize because the polymerization heat is difficult to control.
Disclosure of Invention
The invention aims to overcome the problems of complex synthesis process of acrylate rubber and difficult realization of industrialization in the prior art, and provides a preparation method of acrylate rubber, the acrylate rubber and application thereof.
In order to achieve the above object, a first aspect of the present invention provides a method for producing an acrylate rubber, characterized by comprising the steps of:
s1, premixing: premixing a polymerization monomer and an initiator to obtain a premix;
s2, polymerization reaction: transferring the premix obtained in the step S1 into a polymerization reaction device for polymerization reaction;
wherein the polymerization reaction device is a tubular reactor and/or a double-screw extruder.
The second aspect of the invention provides an acrylate rubber prepared by the preparation method.
In a third aspect, the present invention provides a use of the acrylate rubber of the present invention.
Through the technical scheme, the preparation method of the acrylate rubber, the acrylate rubber and the application thereof provided by the invention have the following beneficial effects:
according to the preparation method of the acrylate rubber, a tubular reaction is adopted in the polymerization process of the acrylate rubber, the tubular reactor is internally provided with the spirally-arranged multiple layers of heat exchange tubes, reaction heat can be removed, and the materials are fully dispersed and thinned by the high-speed mixing and shearing force of the double-screw extruder, so that the heat exchange between the materials and a machine barrel is increased; meanwhile, the continuous extrusion reduces the retention time of materials, reduces the possibility of heat accumulation, and the acrylate rubber prepared by the method has controllable molecular weight and distribution, low oligomer content and stable reaction temperature, and can obtain the acrylate rubber with high molecular weight, low gel content and low volatile.
Furthermore, the preparation of the acrylate rubber is realized by bulk polymerization, so that the use of a solvent is avoided, the process flow is simplified, and the product is pure.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a preparation method of acrylate rubber, which is characterized by comprising the following steps:
s1, premixing: premixing a polymerization monomer and an initiator to obtain a premix;
s2, polymerization reaction: transferring the premix obtained in the step S1 into a polymerization reaction device for polymerization reaction;
wherein the polymerization reaction device is a tubular reactor and/or a double-screw extruder.
According to the invention, a polymerization monomer and an initiator are premixed and then subjected to bulk polymerization in a tubular reactor and/or a double-screw extruder to obtain the acrylate rubber.
In the invention, the polymerization monomer containing the acrylate monomer is subjected to bulk polymerization in the tubular reactor and/or the twin-screw extruder, so that the aggregation of polymerization heat caused by difficult diffusion of heat generated by polymerization in the polymerization process can be remarkably reduced; and through the high-speed mixing and high shearing force of the double-screw extruder, the heat exchange between a polymerization system and the external environment is further increased, the possibility of heat accumulation is reduced, and the stability of the product quality is ensured.
The acrylate rubber prepared by the preparation method has controllable molecular weight and distribution, low oligomer content and stable reaction temperature, and can obtain the acrylate rubber with high molecular weight, low gel content and low volatile.
Meanwhile, the continuous polymerization reaction is realized through the matching of the tubular reactor and/or the double-screw extruder, the retention time of materials is reduced, and the stability of the quality of the final product is further ensured.
In the invention, the method also comprises the step of weighing the polymerization monomer and the initiator according to the proportion.
In the present invention, the premixing may be carried out in a mixing apparatus conventional in the art, and may be, for example, a stirred mixing tank.
In the present invention, the temperature of the premixing is not particularly limited, and the temperature of the premixing is preferably 20 to 80 ℃ and preferably 40 to 60 ℃.
According to the present invention, the tubular reactor may be a tubular reactor which is conventional in the art. Preferably, the tubular reactor contains a plurality of layers of heat exchange tubes which are spirally arranged. Further, the length to diameter ratio of the tubular reactor is from 4 to 48, preferably from 8 to 24.
In the present invention, the twin-screw extruder has a length to diameter ratio of 7 to 64, preferably 12 to 48.
According to the invention, in step S2, the premix is subjected to a polymerization reaction sequentially through a tubular reactor and a twin-screw extruder.
According to the invention, the polymerization temperature of the tubular reactor is between 40 and 90 ℃, preferably between 50 and 80 ℃; the polymerization time is from 0.5 to 2 hours, preferably from 0.5 to 1.5 hours.
According to the invention, the polymerization temperature of the twin-screw extruder is 50 to 100 ℃, preferably 60 to 90 ℃; the shearing speed of the double-screw extruder is 50-90r/min, preferably 60-80r/min; the extrusion time is 5-40min, preferably 10-30min.
In the present invention, the twin-screw extruder comprises a reaction section and an extrusion section.
Preferably, the temperature of the reaction section is different from the temperature of the extrusion section, specifically, the temperature of the reaction section is 40-90 ℃, preferably 50-80 ℃; the temperature of the extrusion section is 50 to 100 ℃, preferably 60 to 90 ℃.
According to the invention, the conversion of the polymerized monomers in the tubular reactor is between 30 and 70%, preferably between 40 and 60%.
In the present invention, the conversion of the monomer was measured by a differential weight method.
According to the invention, the polymerization temperature of the tubular reactor is lower than the polymerization temperature of the twin-screw extruder.
In the invention, the polymerization temperature of the tubular reactor is controlled to be lower than that of the double-screw extruder, so that the reaction speed is stable, and the gel content in the product is effectively controlled.
Further, when the polymerization temperature of the tubular reactor is 5 to 25 ℃ lower than that of the reaction section of the twin-screw extruder, an acrylate rubber having more excellent properties can be obtained.
According to the present invention, the polymeric monomer includes an acrylate monomer and a monomer having a crosslinking reactive group.
In the present invention, the acrylate monomer is selected from substituted or unsubstituted alkyl acrylates (particularly, C1-C6 alkyl acrylates), and the substituted group is preferably an alkoxy group (particularly, a C1-C4 alkoxy group).
Preferably, the acrylate monomer is selected from one or more of Butyl Acrylate (BA), ethyl Acrylate (EA), methoxyethyl acrylate (MOEA), and ethoxyethyl acrylate (EEA).
According to the invention, the monomer having a crosslinking reactive group is selected from vulcanizable monomers which are copolymerizable with the acrylate monomers.
Preferably, the monomer having a crosslinking reactive group is selected from one or more of Acrylonitrile (AN), acrylic Acid (AA), itaconic Acid (IA), monobutyl Itaconate (IBA), vinyl Chloroacetate (VCA), glycidyl Acrylate (GA), and Ethylidene Norbornene (ENB).
According to the invention, the initiator is selected from peroxide initiators and/or oxidation-reduction initiators.
Preferably, the initiator is selected from one or more of azobisisobutyronitrile, cumene hydroperoxide and benzoyl peroxide or di-tert-butyl peroxide.
According to the present invention, the monomer having a crosslinking reactive group is used in an amount of 1 to 10wt%, preferably 2 to 6wt%, based on the total weight of the polymerized monomers; the amount of the acrylate monomer is 90 to 99wt%, preferably 94 to 98wt%.
The initiator is used in an amount of 0.01 to 1wt%, preferably 0.015 to 0.5wt%, based on the total weight of the polymerized monomers.
One embodiment of the present invention is: adding an acrylate monomer, a monomer with a crosslinking active group and a monomer initiator into a stirring type mixing kettle, mixing, sequentially feeding into a tubular reactor through a metering pump, and then feeding into a double-screw extruder for continuous reaction and extrusion reaction to obtain the acrylate rubber.
The second aspect of the invention provides an acrylate rubber prepared by the preparation method.
According to the invention, the acrylate rubber comprises a structural unit A provided by an acrylate monomer and a structural unit B provided by a monomer with a crosslinking active group;
wherein the content of the structural unit A is 90-99wt% based on the total weight of the structural unit of the acrylate rubber; the content of structural unit B is 1-10wt%.
According to the invention, the content of structural units A is 94 to 98 wt.%, based on the total weight of the structural units of the acrylate rubber; the content of structural units B is from 2 to 6% by weight.
In the invention, the content of each structural unit in the acrylate rubber is measured by adopting a nuclear magnetic hydrogen spectrum.
According to the invention, the number-average molecular weight of the acrylate rubber is 10X 10 4 -80×10 4 Excellence inIs selected to be 15 × 10 4 -60×10 4 (ii) a The molecular weight distribution is from 2 to 8, preferably from 2.5 to 6.
In the present invention, the gel content of the acrylate rubber is less than 10wt%, preferably 1 to 5wt%. In the present invention, the volatile matter of the acrylate rubber is less than 3wt%, preferably 0.1 to 1.5wt%.
The third aspect of the invention provides the application of the acrylate rubber in high-temperature-resistant and oil-resistant sealing materials.
The present invention will be described in detail below by way of examples. In the following examples of the present invention,
the dosage of each raw material is calculated by weight portion;
the number average molecular weight and the molecular weight distribution of the acrylate rubber were measured according to the following methods: adopting a gel permeation chromatograph produced by American Water company, taking tetrahydrofuran as a mobile phase and taking a polystyrene standard molecular weight sample as a standard sample;
the conversion of the polymerized monomers was determined by the differential weight method.
The content of the structural unit of the acrylate rubber is measured by adopting a nuclear magnetic hydrogen spectrum method;
measuring the gel content of the acrylate rubber by a Soxhlet extraction method;
the volatile content of the acrylate rubber is measured by adopting thermogravimetric analysis;
the raw materials used in the examples and comparative examples are all commercially available products.
Example 1
100 parts of ethyl acrylate, 2.5 parts of vinyl chloroacetate and 0.06 part of azobisisobutyronitrile are put into a stirring type mixing kettle with the temperature controlled below 40 ℃ for full mixing at one time, and the mixture enters a tubular reactor (the length-diameter ratio is 4:1) through a metering pump after being mixed, the reaction time of the tubular reactor is controlled at 60 ℃ for 1h, the conversion rate of a polymerization monomer in the tubular reactor is 50%, and then the mixture enters a double-screw extruder (the length-diameter ratio is 32. Wherein the polymerization temperature of the tubular reactor is 20 ℃ lower than that of the twin-screw extruder.
The number-average molecular weight of the acrylate rubber A1 was found to be 3.8X 10 5 The molecular weight distribution was 2.9. The gel content was 1.5% by weight, and the volatile matter was 0.18% by weight, and the results are shown in Table 1. In the acrylate rubber, the content of the structural unit A was 98.1% by weight, and the content of the structural unit B was 1.9% by weight.
Example 2
100 parts of ethyl acrylate, 2.5 parts of vinyl chloroacetate and 0.1 part of azobisisobutyronitrile are put into a stirring type mixing kettle with the temperature controlled below 40 ℃ for full mixing at one time, the mixture enters a tubular reactor (the length-diameter ratio is 4:1) through a metering pump after being mixed, the tubular reaction is controlled at 60 ℃ for 0.8h, the conversion rate of a polymerization monomer in the tubular reactor is 55%, the mixture enters a double-screw extruder (the length-diameter ratio is 32. Wherein the polymerization temperature of the tubular reactor is 20 ℃ lower than that of the twin-screw extruder.
The number average molecular weight of the acrylate rubber was tested to be 2.75X 10 5 The molecular weight distribution was 3.5, the gel content was 2% by weight, and the volatile matter was 0.15% by weight, the results are shown in Table 1. In the acrylate rubber, the content of the structural unit A was 98wt%, and the content of the structural unit B was 2wt%.
Example 3
100 parts of ethyl acrylate, 2.5 parts of vinyl chloroacetate and 0.15 part of azobisisobutyronitrile are put into a stirring type mixing kettle controlled at a temperature below 40 ℃ for full mixing at one time, the mixture enters a tubular reactor (length-diameter ratio 4:1) through a metering pump after being mixed, the tubular reaction is controlled at 60 ℃, the reaction time is 0.5h, the conversion rate of a polymerization monomer in the tubular reactor is 60%, and then the mixture enters a double-screw extruder (length-diameter ratio 32. The shearing speed of the extruder is 65r/min, the extrusion time is 10min, and the acrylate rubber A3 is prepared. Wherein the polymerization temperature of the tubular reactor is 20 ℃ lower than that of the twin-screw extruder.
The number-average molecular weight of the acrylate rubber A3 was found to be 2.02X 10 5 The molecular weight distribution was 4, the gel content was 1.9% by weight, and the volatile matter was 0.18% by weight, the results are shown in Table 1. In the acrylate rubber, the content of the structural unit A was 98.1% by weight, and the content of the structural unit B was 1.9% by weight.
Example 4
100 parts of ethyl acrylate, 2.5 parts of vinyl chloroacetate and 0.1 part of azobisisobutyronitrile are put into a stirring type mixing kettle with the temperature controlled below 40 ℃ for full mixing at one time, the mixture enters a tubular reactor (length-diameter ratio 4:1) through a metering pump after being mixed, the tubular reaction is controlled at 60 ℃, the reaction time is 1h, the conversion rate of a polymerization monomer in the tubular reactor is 60%, and then the mixture enters a double-screw extruder (length-diameter ratio 32. The shearing speed of the extruder is 80r/min, and the extrusion time is 10min, so that the acrylate rubber A4 is prepared. Wherein the polymerization temperature of the tubular reactor is 20 ℃ lower than that of the twin-screw extruder.
The number-average molecular weight of the acrylate rubber A4 was found to be 2.16X 10 5 The molecular weight distribution was 3.7. The gel content was 2.1% by weight, and the volatile matter was 0.16% by weight, and the results are shown in Table 1. In the acrylate rubber, the content of the structural unit A was 98.2% by weight, and the content of the structural unit B was 1.8% by weight.
Example 5
An acrylate rubber A5 was prepared according to the method of example 1, except that: the mixed monomer and initiator directly enter a double-screw extruder through a metering pump. The temperature of the reaction section of the double-screw extruder is controlled to be 80 ℃, and the temperature of the extrusion section of the double-screw extruder is controlled to be 70 ℃. The shearing speed of the extruder is 80r/min, and the extrusion time is 30min, so that the acrylate rubber A5 is prepared.
The data molecular weight of the acrylate rubber A5 was found to be 4.87X 10 5 The molecular weight distribution was 2.73, the gel content was 4.5wt%, and the volatile matter was 0.2wt%, the results are shown in Table 1. The content of the structural unit A was 98% by weight, and the content of the structural unit B was 2% by weight.
Example 6
An acrylate rubber A6 was prepared as in example 1, except that: the mixed monomers and initiator are polymerized only in the tubular reactor. The tubular reactor is controlled at 60 ℃ and the reaction time is 2h, and the acrylate rubber A6 is prepared.
The data molecular weight of the acrylate rubber A6 was tested to be 2.62X 10 5 The molecular weight distribution was 4.3. The gel content was 2.3% by weight, and the volatile matter was 2% by weight, and the results are shown in Table 1. The content of the structural unit A was 98.1% by weight, and the content of the structural unit B was 1.9% by weight.
Example 7
An acrylate rubber A7 was prepared according to the method of example 1, except that: the temperature of the tubular reactor is controlled at 60 ℃, the temperature of the reaction section of the double-screw extruder is 100 ℃, namely the polymerization temperature of the tubular reactor is 40 ℃ lower than that of the reaction section of the double-screw extruder, and the acrylate rubber A7 is prepared.
The data molecular weight of the acrylate rubber A7 was tested to be 1.12X 10 5 The molecular weight distribution was 2.3. The gel content was 11wt%, and the volatile matter was 0.16wt%, the results are shown in Table 1. The content of the structural unit A was 97.8% by weight, and the content of the structural unit B was 2.2% by weight.
Example 8
50 parts of ethyl acrylate, 30 parts of butyl acrylate, 20 parts of methoxyethyl acrylate, 2.5 parts of vinyl chloroacetate and 0.06 part of azobisisobutyronitrile are put into a stirring type mixing kettle with the temperature controlled below 40 ℃ for full mixing at one time, the mixture enters a tubular reactor (the length-diameter ratio is 4:1) through a metering pump after being mixed, the tubular reactor is controlled at 60 ℃, the reaction time is 1h, the conversion rate of a polymerization monomer in the tubular reactor is 60%, the mixture enters a double-screw extruder (the length-diameter ratio is 32%, the temperature of a reaction section of the double-screw extruder is controlled at 70 ℃, the temperature of an extrusion section of the double-screw extruder is controlled at 70 ℃, the shearing speed of the extruder is 65r/min, and the extrusion time is 15min, so that the acrylic rubber A1 is prepared. Wherein the polymerization temperature of the tubular reactor is 10 ℃ lower than that of the twin-screw extruder.
The number average molecular weight of the acrylate rubber A1 was determined6.8×10 5 The molecular weight distribution was 3.12. The gel content was 1.5% by weight, and the volatile matter was 0.15% by weight, and the results are shown in Table 1. In the acrylate rubber, the content of the structural unit A was 97.5% by weight, and the content of the structural unit B was 2.5%.
Comparative example 1
100 parts of ethyl acrylate, 2.5 parts of vinyl chloroacetate and 0.15 part of azobisisobutyronitrile are subjected to emulsion polymerization at the reaction temperature of 60 ℃ for 3 hours to obtain the acrylate rubber D1.
The number-average molecular weight of the acrylate rubber D1 was found to be 8.2X 10 4 The molecular weight distribution was 1.92. The gel content was 1.7% by weight, and the volatile matter was 3.5% by weight, the results are shown in Table 1. In the acrylate rubber, the content of the structural unit A was 98wt%, and the content of the structural unit B was 2wt%.
TABLE 1
Number average molecular weight Molecular weight distribution Gel content, wt% Volatile matter, wt%
Example 1 3.8×10 5 2.9 1.5 0.18
Example 2 2.75×10 5 3.5 2 0.15
Example 3 2.02×10 5 4 1.9 0.18
Example 4 2.16×10 5 3.7 2.1 0.16
Example 5 4.87×10 5 2.73 4.5 0.2
Example 6 2.62×10 5 4.3 2.3 2
Example 7 1.12×10 5 2.3 11 0.16
Example 8 6.8×10 5 3.12 1.5 0.15
Comparative example 1 8.2×10 4 1.92 1.7 3.5
As can be seen from Table 1, the acrylate rubbers obtained in examples 1 to 8 according to the present invention have higher number average molecular weights and lower gel contents and volatile contents than those obtained in comparative example 1, i.e., the acrylate rubbers obtained in examples 1 to 8 according to the present invention have more excellent overall properties.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.

Claims (18)

1. The preparation method of the acrylate rubber is characterized by comprising the following steps:
s1, premixing: premixing a polymerization monomer and an initiator to obtain a premix;
s2, polymerization reaction: transferring the premix obtained in the step S1 into a polymerization reaction device for polymerization reaction;
wherein the polymerization reaction device is a tubular reactor and a double-screw extruder;
the premix sequentially passes through a tubular reactor and a double-screw extruder to carry out polymerization reaction;
wherein the polymerization temperature of the tubular reactor is 50-80 ℃; the polymerization time is 0.5-1.5h;
the polymerization temperature of the double-screw extruder is 60-90 ℃; the shearing speed of the double-screw extruder is 60-80r/min; the extrusion time is 10-30min;
the polymerization temperature of the tubular reactor is 5-25 ℃ lower than that of the reaction section of the double-screw extruder;
wherein, in the tubular reactor, the conversion rate of the polymerization monomer is 40-60%;
wherein the polymerization monomer comprises an acrylate monomer and a monomer with a crosslinking active group.
2. The production method according to claim 1, wherein the length-to-diameter ratio of the tubular reactor is 4 to 48.
3. The production method according to claim 2, wherein the length-to-diameter ratio of the tubular reactor is 8 to 24.
4. The method of claim 1, wherein the twin screw extruder has an aspect ratio of 7 to 64.
5. The production method according to claim 4, wherein the twin-screw extruder has an aspect ratio of 12 to 48.
6. The method according to any one of claims 1 to 5, wherein the acrylic monomer is one or more selected from butyl acrylate, ethyl acrylate, methoxyethyl acrylate, and ethoxyethyl acrylate.
7. The production method according to any one of claims 1 to 5, wherein the monomer having a crosslinking reactive group is one or more selected from acrylonitrile, acrylic acid, itaconic acid, monobutyl itaconate, vinyl chloroacetate, glycidyl acrylate, and ethylidene norbornene.
8. The production method according to any one of claims 1 to 5, wherein the initiator is selected from one or more of azobisisobutyronitrile, cumene hydroperoxide, benzoyl peroxide and di-tert-butyl peroxide.
9. The preparation method of claim 1, wherein the monomer having the crosslinking reactive group is used in an amount of 1 to 10wt% based on the total weight of the polymerized monomers.
10. The preparation method according to claim 9, wherein the monomer having a crosslinking-reactive group is used in an amount of 2 to 6wt% based on the total weight of the polymerized monomers.
11. The preparation method of claim 1, wherein the initiator is used in an amount of 0.01 to 1% based on the total weight of the polymerized monomers.
12. The preparation method of claim 11, wherein the initiator is used in an amount of 0.015 to 0.5wt% based on the total weight of the polymerized monomers.
13. An acrylate rubber obtained by the production method according to any one of claims 1 to 12.
14. The acrylate rubber according to claim 13, wherein the acrylate rubber comprises structural units a provided by an acrylate monomer and structural units B provided by a monomer having a crosslinking reactive group;
wherein the content of the structural unit A is 90-99wt% based on the total weight of the structural unit of the acrylate rubber; the content of structural unit B is 1-10wt%.
15. The acrylate rubber according to claim 14, wherein the content of the structural unit a is 94 to 98wt%, based on the total weight of the structural units of the acrylate rubber; the content of structural units B is from 2 to 6% by weight.
16. The acrylate rubber according to any of claims 13-15, wherein the number average molecular weight of the acrylate rubber is 1.0 x 10 5 -8.0×10 5 (ii) a The molecular weight distribution is 2-8.
17. The acrylate rubber according to claim 16, wherein the number average molecular weight of the acrylate rubber is 1.5 x 10 5 -6.0×10 5 (ii) a The molecular weight distribution is 2.5-6.
18. Use of the acrylate rubber according to any of claims 13-16 in high temperature resistant, oil resistant sealing materials.
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