CN114426688A - Method for preparing rubber aid dispersion liquid, brominated butyl rubber and preparation method thereof - Google Patents
Method for preparing rubber aid dispersion liquid, brominated butyl rubber and preparation method thereof Download PDFInfo
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- CN114426688A CN114426688A CN202011101904.5A CN202011101904A CN114426688A CN 114426688 A CN114426688 A CN 114426688A CN 202011101904 A CN202011101904 A CN 202011101904A CN 114426688 A CN114426688 A CN 114426688A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/205—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
- C08J3/21—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase
- C08J3/215—Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the polymer being premixed with a liquid phase at least one additive being also premixed with a liquid phase
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/26—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment
- C08J2323/28—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment by reaction with halogens or halogen-containing compounds
Abstract
The invention relates to the field of rubber, and discloses a method for preparing a rubber auxiliary agent dispersion liquid, a preparation method of brominated nitrile rubber and brominated butyl rubber prepared by the method. The method for preparing the rubber auxiliary agent dispersion liquid comprises the following steps: under the conditions of first stirring and first ultrasonic treatment, carrying out first contact on an antioxidant and an organic solvent to obtain a rubber auxiliary dispersion liquid; wherein the temperature of the first contact is 10-60 ℃. The rubber assistant dispersion liquid prepared by the method can improve the absorption rate of the assistant and improve the dispersion stability of the assistant in rubber, particularly brominated butyl rubber.
Description
Technical Field
The invention relates to the field of rubber, in particular to a method for preparing a rubber auxiliary agent dispersion liquid, a preparation method of brominated nitrile rubber and brominated butyl rubber prepared by the method.
Background
Most industrial organic materials such as plastics, rubbers, fibers, adhesives, foods and feeds, etc. have the property of reacting with oxygen. The reacted substances partially change their original properties, and oxidation phenomena can cause discoloration, weight loss, transparency loss, surface cracking and the like of the polymer and simultaneously cause the loss of mechanical properties of the polymer. There are many methods for industrially preventing the oxidation of organic substances, including modification of polymer structure, obtaining physical stability by orientation of polymer, addition of antioxidant, etc. Among them, the addition of an antioxidant is the simplest and most effective method. The antioxidant is one of the common additives for the high polymer material, and the reasonable use of the antioxidant can play an obvious role in reducing the autoxidation reaction speed of the high polymer material and delaying the aging degradation of the high polymer material.
Butyl rubber (halogenated butyl rubber-containing) is the fourth rubber in the synthetic rubber in the world and is an irreplaceable raw material for the rubber industry. Chlorinated butyl rubber (CIIR)/brominated butyl rubber (BIIR) is obtained by the halogenated modification of butyl rubber, both of which are collectively referred to as halogenated butyl rubber. The halogenated butyl rubber also retains the inherent advantages of butyl rubber due to its backbone. In addition, a small amount of H atoms on the isoprene are partially replaced by active halogen atoms, so that better vulcanization characteristics are provided for the halogenated butyl rubber. This makes the halogenated butyl rubber compatible with other rubbers and vulcanize, greatly expanding its application field. BIIR has more excellent reactivity and vulcanization speed than CIIR, so that BIIR is more dominant in productivity. BIIR is subject to degradation by exposure to various factors such as high temperature, oxygen, high pressure, solvents, etc. during manufacture, processing and use. Since it is mainly applied to inner tubes and inner liners of tires for automobiles, experimental results show that the damage form of tires is mainly thermal damage (the working environment temperature may be higher than 100 ℃). In general, the aging of rubber is retarded and inhibited by adding antioxidant in industrial production, and with the increasing environmental protection concept, the requirement of antioxidant is more strict. The method has the advantages that the anti-aging performance of the rubber is improved, the development of the antioxidant which is more efficient, low (non-) toxic and environment-friendly is one direction for improving the butyl bromide process, and meanwhile, the addition mode of the antioxidant is changed, so that the antioxidant has higher yield, and can meet the requirements under the condition of low addition amount and is one direction for research.
Disclosure of Invention
The invention aims to overcome the defects of low yield, insufficient stability and difficulty in uniform mixing of an auxiliary agent when the auxiliary agent is added into rubber in the prior art, and provides a method for preparing a rubber auxiliary agent dispersion liquid, brominated butyl rubber and a preparation method thereof. The rubber assistant dispersion liquid prepared by the method can improve the absorption rate of the assistant and improve the dispersion stability of the assistant in rubber, particularly brominated butyl rubber.
In order to achieve the above object, a first aspect of the present invention provides a method for preparing a rubber auxiliary dispersion, comprising:
under the conditions of first stirring and first ultrasonic treatment, carrying out first contact on an antioxidant and an organic solvent to obtain a rubber auxiliary dispersion liquid; wherein the temperature of the first contact is 10-60 ℃.
In a second aspect, the present invention provides a process for preparing brominated butyl rubber, said process comprising the steps of:
(1) under the conditions of second stirring and second ultrasonic wave, carrying out second contact on the rubber auxiliary dispersion liquid and the neutralized brominated butyl rubber glue liquid to obtain a first contact material;
(2) under the conditions of second heating and second ultrasonic treatment, removing the organic solvent in the second contact material;
wherein the rubber aid dispersion liquid is prepared by the method.
In a third aspect, the present invention provides a process for producing brominated butyl rubber, characterized in that the process comprises the steps of:
s1, under the conditions of third stirring and third ultrasonic treatment, carrying out third contact on an antioxidant and the neutralized brominated butyl rubber liquid to obtain a third contact material;
s2, under the third heating and third ultrasonic treatment conditions, removing the organic solvent in the third contact material.
In a fourth aspect, the present invention provides a brominated butyl rubber produced by the above process.
By the technical scheme, the rubber aid dispersion liquid, the brominated butyl rubber and the preparation method thereof provided by the invention have the following beneficial effects:
the rubber auxiliary agent dispersion liquid prepared by the process method not only solves the problems of easy dust pollution, difficult transportation and low solubility of the powder antioxidant in an organic solvent of solid powder auxiliary agents, especially the antioxidant and the like, but also solves the problems of low yield and instability of the antioxidant, so that the antioxidant can meet the production requirement under the condition of low addition amount, and has higher economic benefit.
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.
In a first aspect, the present invention provides a method for preparing a rubber auxiliary dispersion, comprising:
under the conditions of first stirring and first ultrasonic treatment, carrying out first contact on an antioxidant and an organic solvent to obtain a rubber auxiliary dispersion liquid; wherein the temperature of the first contact is 10-60 ℃.
In the invention, the inventor researches and discovers that the rubber auxiliary agent dispersion liquid prepared by the method can effectively improve the dispersibility of the rubber auxiliary agent in an organic solvent, and when the rubber auxiliary agent dispersion liquid is used as an auxiliary agent system for preparing the brominated butyl rubber, the rubber auxiliary agent dispersion liquid not only can avoid dust pollution caused by addition of the auxiliary agent in the traditional technology, but also can obviously improve the absorption rate and the dispersion stability of the auxiliary agent in the brominated butyl rubber, so that the antioxidant can meet the production requirement under the condition of low addition amount, and has higher economic benefit.
According to the invention, the temperature of the first contact is between 20 and 60 ℃.
According to the invention, the conditions of the first stirring comprise: stirring for 1-30 min; the rotation speed of the stirring is 100-500 rpm.
Further, the conditions of the first stirring include: the stirring time is preferably 5-15 min; the rotation speed of the stirring is preferably 200-400 rpm.
According to the invention, the conditions of the first sonication include: the ultrasonic frequency is 20-80 kHz; the ultrasonic treatment time is 1-30 min.
Further, the conditions of the first sonication include: the frequency of the ultrasound is preferably 30-50 kHz; the time of ultrasound is preferably 15-30 min.
According to the invention, the mass-volume ratio of the antioxidant to the organic solvent is (50-150):1 g/mL. When the mass-to-volume ratio of the antioxidant to the organic solvent satisfies the above range, the amount of the antioxidant to be added can be significantly increased while ensuring the dispersibility of the antioxidant in the organic solvent. Further, the preferable mass volume ratio of the antioxidant to the organic solvent is (80-120):1 g/mL.
According to the present invention, the organic solvent is at least one selected from the group consisting of cyclohexane, n-hexane, pentane, heptane, toluene, benzene, p-toluene, and cyclopentane.
In the present invention, the antioxidant may be an antioxidant which is conventional in the art, for example, a solid antioxidant and/or a liquid antioxidant. Specifically, the solid powder antioxidant is at least one selected from antioxidant 1010, antioxidant 1076 and antioxidant 1330; the liquid antioxidant is selected from antioxidant 1520 and/or antioxidant FT-NOX 3036.
According to the invention, the ultrasound treatment is carried out in an ultrasonic oscillator and/or an ultrasonic cleaner.
In a second aspect, the present invention provides a process for preparing brominated butyl rubber, said process comprising the steps of:
(1) under the conditions of second stirring and second ultrasonic wave, carrying out second contact on the rubber auxiliary dispersion liquid and the neutralized brominated butyl rubber liquid to obtain a second contact material;
(2) under the conditions of second heating and second ultrasonic treatment, removing the organic solvent in the second contact material;
wherein the rubber aid dispersion liquid is prepared by the method.
According to the invention, the organic solvent in the second contact material is removed under the conditions of heating and second ultrasonic treatment, so that the absorption rate of the antioxidant can be improved, and the dispersion stability of the antioxidant in the brominated butyl rubber is further improved.
According to the present invention, in step (1), the second contact temperature is 30 to 90 ℃, preferably 40 to 80 ℃.
According to the invention, in step (1), the second stirring conditions include: stirring for 1-30min, preferably 10-20 min; the rotational speed of the stirring is 100 to 500rpm, preferably 200 to 400 rpm.
According to the present invention, in the step (2), the temperature of the second heating is 30 to 90 ℃, preferably 40 to 80 ℃.
In the present invention, the second contact temperature and the second heating temperature may be the same or different, and preferably the same.
According to the invention, the conditions of the second sonication include: the frequency of the ultrasound is 20-80kHz, preferably 30-50 kHz.
In the present invention, the ultrasonic treatment time is such that the content of the organic solvent in the second contact material is less than 0.5 wt%, preferably such that the content of the organic solvent in the second contact material is 0 wt%.
According to the invention, the rubber aid dispersion liquid and the brominated butyl rubber glue solution are used in an amount such that the antioxidant is used in an amount of 0.02 to 0.5 wt% relative to the brominated butyl rubber.
According to the invention, in the step (2), the heating mode is direct heating and/or flash evaporation.
In the invention, the method also comprises the step of carrying out open milling on the brominated butyl rubber after the organic solvent is removed to prepare a rubber product.
In a third aspect, the present invention provides a process for producing brominated butyl rubber, characterized in that the process comprises the steps of:
s1, under the conditions of third stirring and third ultrasonic treatment, carrying out third contact on an antioxidant and the neutralized brominated butyl rubber liquid to obtain a third contact material;
s2, under the third heating and third ultrasonic treatment conditions, removing the organic solvent in the third contact material.
According to the invention, the organic solvent in the second contact material is removed under the conditions of heating and second ultrasonic treatment, so that the absorption rate of the antioxidant can be improved, and the dispersion stability of the antioxidant in the brominated butyl rubber is further improved.
According to the invention, the antioxidant and the brominated butyl rubber glue solution are used in an amount of 0.02 to 0.5 wt% relative to the brominated butyl rubber.
According to the invention, the temperature of the third contact in step S1 is between 30 and 90 ℃, preferably between 40 and 80 ℃.
According to the invention, in step S2, the temperature of the third heating is 30 to 90 ℃, preferably 40 to 80 ℃.
In the present invention, the third contact temperature and the third heating temperature may be the same or different, and preferably the same.
According to the invention, in step S1, the third stirring conditions include: stirring for 1-30min, preferably 10-20 min; the rotational speed of the stirring is 100 to 500rpm, preferably 200 to 400 rpm.
According to the invention, the conditions of the ultrasonication comprise: the frequency of the ultrasound is 20-80kHz, preferably 30-50 kHz.
In the present invention, the ultrasonic treatment time is such that the content of the organic solvent in the third contact material is less than 0.5 wt%, preferably such that the content of the organic solvent in the third contact material is 0 wt%.
In a preferred embodiment of the present invention, the process for producing brominated butyl rubber comprises the steps of:
s1, under the conditions of third stirring and third ultrasonic treatment, carrying out third contact on the liquid antioxidant and the neutralized brominated butyl rubber liquid to obtain a third contact material;
s2, under the third heating and third ultrasonic treatment conditions, removing the organic solvent in the third contact material.
In the invention, the method also comprises the step of carrying out open milling on the brominated butyl rubber after the organic solvent is removed to prepare a rubber product.
The "brominated butyl rubber glue solution" in the invention is a raw material in the method for preparing brominated butyl rubber in the second aspect of the invention and the method for producing brominated butyl rubber in the third aspect of the invention.
In the invention, the brominated butyl rubber glue solution can be purchased from the market, and can also be obtained by the following steps:
(a1) under the condition of stirring, mixing butyl rubber with a solvent to obtain a butyl rubber glue solution;
(a2) under the heating condition, carrying out bromination reaction on the butyl rubber glue solution, and then adding an alkali solution for neutralization reaction to obtain a neutralized brominated butyl rubber glue solution;
(a3) and washing the neutralized brominated butyl rubber glue solution, and adding a stabilizer to obtain the brominated butyl rubber glue solution.
In the present invention, the solvent in the step (a1) is the same as the organic solvent, and is at least one selected from the group consisting of cyclohexane, n-hexane, pentane, heptane, toluene, benzene, p-toluene and cyclopentane.
In a fourth aspect, the present invention provides a brominated butyl rubber produced by the above process.
In the brominated butyl rubber provided by the invention, the content of the antioxidant is stable and easy to adjust, and the absorption rate of the antioxidant is more than or equal to 75%.
The present invention will be described in detail below by way of examples.
The preparation method of the brominated butyl rubber glue solution in the following examples and comparative examples is as follows:
preparing glue solution: accurately weighing 40g of butyl rubber 1751, cutting the butyl rubber into fragments, putting the fragments into a bromination reaction kettle in a laboratory, adding 320ml of hexane into the reaction kettle, stirring and dissolving at a low rotating speed at room temperature for 12 hours to obtain a butyl rubber glue solution with the mass fraction of 15 wt%;
bromination stage and neutralization of the gum solution: heating in water bath, keeping the temperature of the glue solution in the reaction kettle constant at 50 ℃, stirring at low speed for 2h, diluting 0.67ml of liquid bromine with 20ml of hexane in a constant-pressure funnel during bromination, carrying out light-shielding treatment on the reaction kettle, increasing the rotation speed of the glue solution, quickly adding the bromine diluent into the glue solution, adding 30ml of sodium hydroxide solution with the mass fraction of 5% after reacting for 2min to neutralize HBr generated by the reaction, continuing to react for 13min, stopping stirring after the reaction is finished, opening the reaction kettle, and transferring the glue solution to a 5L big beaker.
BIIR post-treatment: and (3) washing the glue solution in the big beaker for 3-5 times by using a large amount of deionized water until the pH value of the system is alkalescent, and adding a stabilizer to obtain the brominated butyl rubber glue solution.
Examples and comparative examples all other materials were commercially available.
The antioxidant content in the brominated butyl rubber is measured by a high performance liquid chromatograph, the model of which is Agilent 1100 type high performance liquid chromatograph, and a diode array detector is arranged. The determination method comprises the following steps: dissolving a rubber sample with tetrahydrofuran, adding methanol for extraction, shaking uniformly, taking a filtrate for sample injection, taking acetonitrile/water as a mobile phase, carrying out gradient elution, carrying out OSD column separation, detecting by a diode array detector, and quantifying the result by an external standard method.
Preparation example 1
Solid powder antioxidant 1076 in an amount of 0.05% by weight of the brominated butyl rubber was mixed with 10ml of hexane at 30 ℃ under the following conditions: stirring for 2min at the rotation speed of 200rpm, and then ultrasonically vibrating for 5min by ultrasonic waves with the frequency of 30kHz to uniformly disperse the antioxidant in the solvent to obtain the rubber auxiliary dispersion liquid Z1.
The other preparation examples adopt the same procedures as the preparation example 1, only the process conditions are different, and the specific process conditions are listed in table 1.
TABLE 1
Comparative example 1
And (3) contacting the brominated butyl rubber glue solution with antioxidant 1076 powder accounting for 0.05 wt% of the brominated butyl rubber at the temperature of 30 ℃, fully stirring to uniformly disperse the brominated butyl rubber glue solution, carrying out contact reaction for 15min, carrying out flash evaporation by using boiling water, carrying out vacuum drying, and carrying out open milling by using an open mill to obtain a rubber finished product.
Comparative example 2
Brominated butyl rubber was prepared using the procedure of comparative example 1, except that: antioxidant 1076 was replaced with antioxidant 1520.
Example 1
And (2) stirring the brominated butyl rubber glue solution and the rubber aid dispersion solution obtained in the preparation example 1 at the temperature of 60 ℃ in Z1 for 10min at the rotating speed of 200rpm, performing ultrasonic vibration at the frequency of 30kHz to obtain a first contact material, removing the organic solvent under the heating condition of ultrasonic vibration and matching, and performing vacuum drying and open milling in an open mill to obtain a finished product A1 of the brominated butyl rubber.
Examples 2 to 8
Brominated butyl rubbers A2-A8 were prepared in the same manner as in example 1, except that: rubber aid dispersion Z2-Z8 was used in place of rubber aid dispersion Z1.
Example 9
Brominated butyl rubber article A9 was prepared according to the method of example 1, except that: and ultrasonically vibrating the stirred brominated butyl rubber glue solution for 10min, contacting to obtain a first contact material, and then carrying out flash evaporation in boiling water, vacuum drying and open milling in an open mill to obtain a rubber finished product A9.
The process flow of examples 1-9 and comparative examples 1-2 is shown in Table 2.
TABLE 2
Test example
Test examples are provided to illustrate the absorbance of the antioxidant in the brominated butyl rubber prepared in the above examples and comparative examples, and the results are shown in Table 3.
TABLE 3
As can be seen from Table 3, the brominated butyl rubber obtained by contacting the rubber aid dispersion liquid provided by the invention with the brominated butyl rubber glue solution has stable and easily adjustable antioxidant content, and the antioxidant absorption rate is more than or equal to 75%.
Example 10
And (3) stirring the brominated butyl rubber glue solution and a liquid antioxidant 1520 at the temperature of 60 ℃ for 10min at the rotating speed of 200rpm, contacting by ultrasonic vibration with the frequency of 30kHz to obtain a third contact material, removing the organic solvent under the heating condition of ultrasonic vibration matched with heating, and then carrying out vacuum drying and open milling by an open mill to obtain a finished product A10 of the brominated butyl rubber.
The process flow for examples 10-15 is described in Table 4.
TABLE 4
Test example
Test examples are provided to illustrate the absorbance of the antioxidant in the brominated butyl rubber prepared in the above examples, and the results are shown in Table 5.
TABLE 5
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 (14)
1. A method of formulating a rubber aid dispersion, said method comprising:
under the conditions of first stirring and first ultrasonic treatment, carrying out first contact on an antioxidant and an organic solvent to obtain a rubber auxiliary dispersion liquid; wherein the temperature of the first contact is 10-60 ℃.
2. The method of claim 1, wherein the temperature of the first contacting is 20-60 ℃;
preferably, the conditions of the first stirring include: stirring for 1-30min, preferably 5-15 min; the stirring speed is 100-500rpm, preferably 200-400 rpm;
preferably, the conditions of the first sonication include: the ultrasonic frequency is 20-80kHz, preferably 30-50 Hz; the ultrasonic treatment time is 1-30min, preferably 15-30 min.
3. The method according to claim 1 or 2, wherein the mass to volume ratio of the antioxidant to the organic solvent is (50-150):1g/mL, preferably (80-120):1 g/mL.
4. The method according to any one of claims 1 to 3, wherein the organic solvent is selected from at least one of cyclohexane, n-hexane, pentane, heptane, toluene, benzene, p-toluene and cyclopentane.
5. The method according to any one of claims 1 to 4, wherein the antioxidant is selected from solid antioxidants and/or liquid antioxidants.
6. The method according to any one of claims 1 to 5, wherein the sonication is carried out in a sonicator and/or a sonicator.
7. A process for preparing brominated butyl rubber, the process comprising the steps of:
(1) under the conditions of second stirring and second ultrasonic treatment, carrying out second contact on the rubber auxiliary dispersion liquid and the neutralized brominated butyl rubber liquid to obtain a second contact material;
(2) under the conditions of second heating and second ultrasonic treatment, removing the organic solvent in the second contact material;
wherein the rubber auxiliary dispersion liquid is a rubber auxiliary dispersion liquid prepared by the method according to any one of claims 1 to 6.
8. The process according to claim 7, wherein in step (1), the temperature of the second contacting is 30-90 ℃, preferably 40-80 ℃;
in the step (1), the second stirring conditions include: stirring for 1-30min, preferably 10-20 min; the stirring speed is 100-500rpm, preferably 200-400 rpm;
preferably, in step (2), the temperature of the second heating is 30-90 ℃, preferably 40-80 ℃;
preferably, the conditions of the second sonication include: the frequency of the ultrasound is 20-80kHz, preferably 30-50 kHz.
9. The method according to any one of claims 7 or 8, wherein the rubber aid dispersion and the brominated butyl rubber cement are used in an amount such that the antioxidant is used in an amount of 0.02 to 0.5 wt% with respect to the brominated butyl rubber.
10. The method according to any one of claims 7 to 9, wherein in step (2), the heating is direct heating and/or flash evaporation.
11. A process for producing brominated butyl rubber, the process comprising the steps of:
s1, under the conditions of third stirring and third ultrasonic treatment, carrying out third contact on an antioxidant and the neutralized brominated butyl rubber liquid to obtain a third contact material;
s2, under the third heating and third ultrasonic treatment conditions, removing the organic solvent in the third contact material.
12. The method of claim 11, wherein the antioxidant is present in the brominated butyl rubber cement in an amount of 0.02 to 0.5 wt% relative to the brominated butyl rubber.
13. The method according to claim 11 or 12, wherein the temperature of the third contacting in step S1 is 30-90 ℃, preferably 40-80 ℃;
preferably, in step S1, the third stirring conditions include: stirring for 1-30min, preferably 10-20 min; the stirring speed is 100-500rpm, preferably 200-400 rpm;
preferably, in step S2, the temperature of the third heating is 30 to 90 ℃, preferably 40 to 80 ℃;
preferably, the conditions of the third sonication include: the frequency of the ultrasound is 20-80kHz, preferably 30-50 kHz.
14. Brominated butyl rubber produced by the process of any one of claims 7-13.
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| CN109957121A (en) * | 2017-12-14 | 2019-07-02 | 中国石油化工股份有限公司 | The preparation method of nanocomposite and the preparation method of vulcanized rubber |
| CN110229254A (en) * | 2019-07-05 | 2019-09-13 | 黄河三角洲京博化工研究院有限公司 | A kind of bromination process and brombutyl of butyl rubber |
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