CN110452323B - Butyl rubber and preparation method thereof - Google Patents
Butyl rubber and preparation method thereof Download PDFInfo
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Abstract
The invention provides a preparation method of butyl rubber, wherein in the preparation process, a phenolic compound and mono-olefin are added into reaction raw materials. The method provided by the invention further widens the range of the stabilizing agent capable of being selected for synthesizing the butyl rubber, and the polymerization reaction product is uniformly dispersed in the reaction system by introducing the phenolic compound as the slurry stabilizing agent, so that the mass transfer and heat transfer of the system are effectively improved, and the monoolefine is used as the molecular weight regulator, so that the molecular weight distribution is more effectively widened, and the processing performance is improved.
Description
Technical Field
The invention belongs to the technical field of rubber, and particularly relates to butyl rubber and a preparation method thereof.
Background
Butyl rubber (IIR) is one of the synthetic rubbers, synthesized from isobutylene and a small amount of isoprene. Has good chemical stability and thermal stability, and most notably air tightness and water tightness. Its permeability to air is only 1/7 for natural rubber and 1/5 for styrene-butadiene rubber, while its permeability to steam is 1/200 for natural rubber and 1/140 for styrene-butadiene rubber. Therefore, the rubber is mainly used for manufacturing various rubber products such as various inner tubes, steam tubes, water tires, dam bottom layers, gaskets and the like. The defects of low vulcanization speed of the butyl rubber, poor mutual viscosity with other rubbers and weak action with a reinforcing agent limit the use application of the butyl rubber, and the processability of the butyl rubber is more effectively improved by adjusting the molecular weight distribution in the synthesis stage.
The polymerization of the butyl rubber is carried out by a carbocation reaction, when the polymerization temperature is higher than-85 ℃, particles in a slurry system are easy to be aggregated into blocks, the mass and heat transfer of the system are influenced, serious rubber hanging and blockage are caused, the shutdown and cleaning of a polymerization kettle are caused, the continuous operation period of the polymerization reaction is seriously influenced, the yield of the butyl rubber is reduced, and the production cost is increased.
Therefore, it is an urgent problem for those skilled in the art to discharge the heat of polymerization rapidly to control the reaction to proceed at a constant low temperature, maintain the stability of the system, and improve the mass and heat transfer of the butyl rubber polymerization system.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a butyl rubber and a preparation method thereof, wherein the preparation method provided by the present invention can effectively improve mass transfer and heat transfer in the preparation process of the butyl rubber, and can effectively widen the molecular weight distribution of the butyl rubber and improve the processability.
The invention provides a preparation method of butyl rubber, wherein in the preparation process, a phenolic compound and mono-olefin are added into reaction raw materials.
Preferably, the phenolic compound is selected from one or more of p-methyl phenol, o-methyl phenol, 2, 6-di-tert-butyl-4-methyl phenol, and 2, 2' -methylenebis (4-methyl-6-tert-butyl phenol).
Preferably, the monoolefin is selected from one or more of ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 1-heptene, 2-methyl-1-butene and 2-methyl-2-butene.
Preferably, the method comprises the following steps:
A) mixing isomonoolefin, conjugated diene, solvent, phenolic compound and monoolefine to obtain reactant solution;
B) mixing a main catalyst, a cocatalyst and a solvent to obtain a catalyst solution;
C) and mixing the catalyst solution with the reactant solution to react to obtain the butyl rubber.
Preferably, the number of carbon atoms of the isomonoolefin is 4-16; the carbon number of the conjugated diene is 4-14;
the molar ratio of the conjugated diene to the monoolefin is (0.01-0.1) 1; the mass content of the isomonoolefin in the reactant solution is 5-30 wt%.
Preferably, the mass content of the phenolic compound in the reactant solution is 1-3000 mg/Kg.
Preferably, the mass content of the monoolefine in the isomonoolefin is 10-20000 mg/Kg.
Preferably, the main catalyst is water or hydrogen chloride;
the cocatalyst is Lewis acid, such as one or more of aluminum trichloride, dichloroethylaluminum, dichlorobutylaluminum, chlorodibutylaluminum and boron trifluoride;
the molar ratio of the cocatalyst to the main catalyst is (1-10) to 1;
the molar ratio of the cocatalyst to the isomonoolefin is (0.0001-0.005): 1.
Preferably, the reaction temperature is-98 to-80 ℃, and the reaction time is 1 to 20 min.
The invention also provides the butyl rubber prepared by the preparation method.
Compared with the prior art, the invention provides a preparation method of butyl rubber, and in the preparation process, phenolic compounds and mono-olefin are added into reaction raw materials. The method provided by the invention further widens the range of the stabilizing agent capable of being selected for synthesizing the butyl rubber, and the polymerization reaction product is uniformly dispersed in the reaction system by introducing the phenolic compound as the slurry stabilizing agent, so that the mass transfer and heat transfer of the system are effectively improved, and the monoolefine is used as the molecular weight regulator, so that the molecular weight distribution is more effectively widened, and the processing performance is improved.
Drawings
FIG. 1 is a nuclear magnetic spectrum of the butyl rubber prepared in example 1.
Detailed Description
The invention provides a preparation method of butyl rubber, wherein in the preparation process, a phenolic compound and mono-olefin are added into reaction raw materials.
During the reaction, phenolic compound is used as slurry stabilizer and mono-olefin is used as molecular weight regulator. The phenolic compound and the monoolefine are introduced in the preparation process, so that the dispersion state of a polymerization system can be effectively improved, the mass transfer and the heat transfer of the polymerization system are enhanced, the butyl rubber is uniformly dispersed in the system, frequent start and stop in the production process are avoided, the stability of the product is improved, the molecular weight distribution of the butyl rubber product can be effectively widened, and the processability of the butyl rubber is improved.
Wherein the phenolic compound is selected from one or more of p-methyl phenol, o-methyl phenol, 2, 6-di-tert-butyl-4-methyl phenol and 2, 2' -methylene bis (4-methyl-6-tert-butyl phenol), and is preferably methyl phenol or 2, 6-di-tert-butyl-4-methyl phenol.
The monoolefin is selected from one or more of ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 1-heptene, 2-methyl-1-butene and 2-methyl-2-butene, and is preferably 1-butene or 1-heptene.
Specifically, the preparation method comprises the following steps:
A) mixing isomonoolefin, conjugated diene, solvent, phenolic compound and monoolefine to obtain reactant solution;
B) mixing a main catalyst, a cocatalyst and a solvent to obtain a catalyst solution;
C) and mixing the catalyst solution with the reactant solution to react to obtain the butyl rubber.
Firstly, mixing isomonoolefin, a solvent, a phenolic compound and the monoolefine to obtain a mixed solution;
then, adding conjugated diene into the mixed solution, and uniformly mixing to obtain a reactant solution.
Wherein the number of carbon atoms of the isomonoolefin is 4-16, preferably 4-10, and more preferably 4-6;
the number of carbon atoms of the conjugated diene is 4-14, preferably 4-8, and more preferably 4-6;
the solvent used for dissolving the monomer is selected from methane chloride;
the molar ratio of the conjugated diene to the monoolefin is (0.01-0.1): 1, preferably (0.01-0.8): 1, more preferably (0.01-0.5): 1.
The mass content of the isomonoolefin in the reactant solution is 5 wt% to 30 wt%, preferably 5 wt% to 25 wt%, and more preferably 19 wt% to 20 wt%.
The mass content of the phenolic compound in the reactant solution is 1-3000 mg/Kg, preferably 10-1000 mg/Kg, and more preferably 20-100 mg/Kg.
The mass content of the mono-olefin in the isomonoolefin is 10-20000 mg/Kg, preferably 100-5000 mg/Kg, and more preferably 1000-2000 mg/Kg.
Mixing a main catalyst, a cocatalyst and a solvent to obtain a catalyst solution;
the main catalyst is water or hydrogen chloride;
the cocatalyst is Lewis acid, such as one or more of aluminum trichloride, ethyl aluminum dichloride, butyl aluminum dichloride, dibutyl aluminum monochloride and boron trifluoride, and is preferably Lewis acid;
the solvent for dissolving the main catalyst and the cocatalyst is one or more selected from methane chloride, dichloromethane and n-hexane, and preferably methane chloride.
The molar ratio of the cocatalyst to the main catalyst is (1-10): 1, preferably (1-5): 1, more preferably (2-5): 1;
the molar ratio of the cocatalyst to the isomonoolefin is (0.0001-0.005): 1, preferably (0.0001-0.002): 1, more preferably (0.0005-0.001): 1.
Mixing a catalyst solution with a reactant solution to react, wherein the reaction temperature is-98 to-80 ℃, preferably-85 to-98 ℃, and more preferably-92 to-97.5 ℃; the reaction time is 1-20 min, preferably 5-15 min, and more preferably 6-10 min.
Adding an alcohol compound into the reaction slurry obtained by the reaction to terminate the reaction, wherein the alcohol compound is methanol or ethanol, preferably ethanol solution, and the volume fraction of the ethanol aqueous solution is preferably 35-45%.
And removing the solvent from the reaction slurry to obtain the butyl rubber. The method for removing the solvent is not particularly limited in the present invention, and a method known to those skilled in the art may be used.
The invention also provides the butyl rubber prepared by the preparation method.
The method provided by the invention further widens the range of the stabilizing agent capable of being selected for synthesizing the butyl rubber, and the polymerization reaction product is uniformly dispersed in the reaction system by introducing the phenolic compound as the slurry stabilizing agent, so that the mass transfer and heat transfer of the system are effectively improved, and the monoolefine is used as the molecular weight regulator, so that the molecular weight distribution is more effectively widened, and the processing performance is improved.
For further understanding of the present invention, the following examples are provided to illustrate the butyl rubber and the preparation method thereof, and the scope of the present invention is not limited by the following examples.
Example 1
0.1g of 2, 6-di-tert-butyl-4-methylphenol and 0.75g of 1-heptene are weighed and added into 99.15g of methane chloride at the temperature of-70 ℃ to prepare a methane chloride solution, so that the 2, 6-di-tert-butyl-4-methylphenol and 1-heptene can be conveniently added, and after stirring for 30min, the solution is cooled to-95 ℃ to obtain a 2, 6-di-tert-butyl-4-methylphenol and 1-heptene solution.
0.1g of 20% dichloroethylaluminum solution is weighed at-70 ℃ and added into 5g of 0.05wt% HCl methane chloride solution to be uniformly mixed to obtain catalyst solution, and after the catalyst solution is aged at-92 ℃ for 30min, the temperature is reduced to-95 ℃.
The reactor temperature was-95 ℃ and 11.25g of isobutylene, 63.75g of methyl chloride, 2g of 2, 6-di-tert-butyl-4-methylphenol and 1-heptene solution were sequentially added, followed by 0.5g of isoprene and mixed uniformly to obtain a reactant solution. After stirring for 15min, the above catalyst solution was added.
Adding the catalytic system into the reactant solution to react for 10min at the temperature of-95 ℃ to obtain the granular uniformly-dispersed slurry.
1g of ethanol is added to terminate the reaction, the obtained reaction product is dried under vacuum at 40 ℃ for 48 hours, the yield is 87%, the obtained product is subjected to nuclear magnetic analysis (see figure 1, figure 1 is a nuclear magnetic spectrum diagram of the butyl rubber prepared in example 1) and gel permeation chromatography, the unsaturation degree of the obtained butyl rubber is 1.72 mol%, the weight average molecular weight is 21000, the molecular weight distribution is 5.9, the rubber 300% elongation is 7.2MPa, and the tensile strength is 17.5 MPa.
Example 2
0.1g of p-methylphenol and 0.75g of 1-heptene are weighed and added into 99.15g of methane chloride at the temperature of-70 ℃ to prepare methane chloride solution, so that the p-methylphenol and the 1-heptene can be conveniently added, and after stirring for 30min, the solution is cooled to-95 ℃ to obtain the p-methylphenol and 1-heptene solution.
0.1g of 20% dichloroethylaluminum solution is weighed at-70 ℃ and added into 5g of 0.05wt% HCl methane chloride solution to be uniformly mixed to obtain catalyst solution, and after the catalyst solution is aged at-92 ℃ for 30min, the temperature is reduced to-95 ℃.
The reactor temperature was-95 ℃ and 11.25g of isobutylene, 63.75g of methyl chloride, 2g of p-methylphenol and 1-heptene solution were sequentially added, followed by 0.5g of isoprene and mixed uniformly to obtain a reactant solution. After stirring for 15min, the above catalyst solution was added.
Adding the catalytic system into the reactant solution to react for 10min at the temperature of-95 ℃ to obtain the granular uniformly-dispersed slurry.
Adding 1g of ethanol to terminate the reaction, drying the obtained reaction product at 40 ℃ in vacuum for 48h, wherein the yield is 84%, carrying out nuclear magnetic analysis and gel permeation chromatograph test on the obtained product, and obtaining the butyl rubber with the unsaturation degree of 1.70 mol%, the weight average molecular weight of 18500, the molecular weight distribution of 5.7, the rubber with the 300% definite elongation of 7.0MPa and the tensile strength of 17.0 MPa.
Example 3
0.1g of 2, 6-di-tert-butyl-4-methylphenol and 0.75g of 1-butene are weighed and added into 99.15g of methane chloride at the temperature of minus 70 ℃ to prepare a methane chloride solution, so that the 2, 6-di-tert-butyl-4-methylphenol and 1-butene can be conveniently added, the solution is cooled to minus 95 ℃ after being stirred for 30min, and the solution of the 2, 6-di-tert-butyl-4-methylphenol and the 1-butene is obtained.
0.1g of 20% dichloroethylaluminum solution is weighed at-70 ℃ and added into 5g of 0.05wt% HCl methane chloride solution to be uniformly mixed to obtain catalyst solution, and after the catalyst solution is aged at-92 ℃ for 30min, the temperature is reduced to-95 ℃.
The reactor temperature was-95 ℃ and 11.25g of isobutylene, 63.75g of methyl chloride, 2g of 2, 6-di-tert-butyl-4-methylphenol and 1-butene solution were sequentially added, followed by 0.5g of isoprene and mixed uniformly to obtain a reactant solution. After stirring for 15min, the above catalyst solution was added.
Adding the catalytic system into the reactant solution to react for 10min at the temperature of-95 ℃ to obtain the granular uniformly-dispersed slurry.
Adding 1g of ethanol to terminate the reaction, drying the obtained reaction product at 40 ℃ in vacuum for 48h, wherein the yield is 80%, carrying out nuclear magnetic analysis and gel permeation chromatograph test on the obtained product, and obtaining the butyl rubber with the unsaturation degree of 1.68 mol%, the weight average molecular weight of 18000, the molecular weight distribution of 5.5, the 300% definite elongation of the rubber of 6.8MPa and the tensile strength of 16.7 MPa.
Example 4
0.1g of 2, 6-di-tert-butyl-4-methylphenol and 1g of 1-heptene are weighed and added into 98.9g of methane chloride at the temperature of-70 ℃ to prepare methane chloride solution, so that the 2, 6-di-tert-butyl-4-methylphenol and 1-heptene can be conveniently added, the solution is cooled to-95 ℃ after being stirred for 30min, and then the 2, 6-di-tert-butyl-4-methylphenol and 1-heptene solution is obtained.
0.1g of 40% dichloroethylaluminum solution is weighed at-70 ℃ and added into 5g of 0.05wt% HCl methane chloride solution to be uniformly mixed to obtain catalyst solution, and after the catalyst solution is aged at-92 ℃ for 30min, the temperature is reduced to-95 ℃.
At a reactor temperature of-95 ℃, 11.25g of isobutene, 63.75g of methyl chloride, 3g of 2, 6-di-tert-butyl-4-methylphenol and 1-heptene solution are sequentially added, and then 0.5g of isoprene is added and mixed uniformly to obtain a reactant solution. After stirring for 15min, the above catalyst solution was added.
Adding the catalytic system into the reactant solution to react for 10min at the temperature of-95 ℃ to obtain the granular uniformly-dispersed slurry.
Adding 1g of ethanol to terminate the reaction, drying the obtained reaction product at 40 ℃ in vacuum for 48h, wherein the yield is 75%, carrying out nuclear magnetic analysis and gel permeation chromatograph test on the obtained product, and obtaining the butyl rubber with the unsaturation degree of 1.64 mol%, the weight average molecular weight of 16950, the molecular weight distribution of 5.4, the rubber with the 300% definite elongation of 6.9MPa and the tensile strength of 16.7 MPa.
Example 5
0.1g of 2, 6-di-tert-butyl-4-methylphenol and 0.3g of 1-heptene are weighed and added into 99.6g of methane chloride at the temperature of-70 ℃ to prepare a methane chloride solution, so that the 2, 6-di-tert-butyl-4-methylphenol and 1-heptene can be conveniently added, and after stirring for 30min, the solution is cooled to-95 ℃ to obtain a 2, 6-di-tert-butyl-4-methylphenol and 1-heptene solution.
0.1g of 40% dichloroethylaluminum solution is weighed at-70 ℃ and added into 5g of 0.05wt% HCl methane chloride solution to be uniformly mixed to obtain catalyst solution, and after the catalyst solution is aged at-92 ℃ for 30min, the temperature is reduced to-95 ℃.
The reactor temperature was-95 ℃ and 11.25g of isobutylene, 63.75g of methyl chloride, 2g of 2, 6-di-tert-butyl-4-methylphenol and 1-heptene solution were sequentially added, followed by 0.5g of isoprene and mixed uniformly to obtain a reactant solution. After stirring for 15min, the above catalyst solution was added.
Adding the catalytic system into the reactant solution to react for 10min at the temperature of-95 ℃ to obtain the granular uniformly-dispersed slurry.
Adding 1g of ethanol to terminate the reaction, drying the obtained reaction product at 40 ℃ in vacuum for 48h, wherein the yield is 68%, carrying out nuclear magnetic analysis and gel permeation chromatograph test on the obtained product, and obtaining the butyl rubber with the unsaturation degree of 1.62 mol%, the weight average molecular weight of 16000, the molecular weight distribution of 5.1, the rubber with the 300% definite elongation of 6.6MPa and the tensile strength of 16.2 MPa.
Example 6
0.01g of 2, 6-di-tert-butyl-4-methylphenol and 0.75g of 1-heptene are weighed and added into 99.24g of methane chloride at the temperature of-70 ℃ to prepare a methane chloride solution, so that the 2, 6-di-tert-butyl-4-methylphenol and 1-heptene can be conveniently added, and after stirring for 30min, the solution is cooled to-95 ℃ to obtain a 2, 6-di-tert-butyl-4-methylphenol and 1-heptene solution.
0.1g of 20% dichloroethylaluminum solution is weighed at-70 ℃ and added into 5g of 0.05wt% HCl methane chloride solution to be uniformly mixed to obtain catalyst solution, and after the catalyst solution is aged at-92 ℃ for 30min, the temperature is reduced to-95 ℃.
The reactor temperature was-95 ℃ and 11.25g of isobutylene, 63.75g of methyl chloride, 2g of 2, 6-di-tert-butyl-4-methylphenol and 1-heptene solution were sequentially added, followed by 0.5g of isoprene and mixed uniformly to obtain a reactant solution. After stirring for 15min, the above catalyst solution was added.
Adding the catalytic system into the reactant solution to react for 10min at the temperature of-95 ℃ to obtain spherical uniformly dispersed slurry.
Adding 1g of ethanol to terminate the reaction, drying the obtained reaction product at 40 ℃ in vacuum for 48h, wherein the yield is 80%, carrying out nuclear magnetic analysis and gel permeation chromatograph test on the obtained product, and obtaining the butyl rubber with the unsaturation degree of 1.66 mol%, the weight average molecular weight of 20000, the molecular weight distribution of 5.8, the rubber with the 300% definite elongation of 7.1MPa and the tensile strength of 17.6 MPa.
Example 7
0.5g of 2, 6-di-tert-butyl-4-methylphenol and 0.75g of 1-heptene are weighed and added into 98.75g of methane chloride at the temperature of-70 ℃ to prepare methane chloride solution, so that the 2, 6-di-tert-butyl-4-methylphenol and 1-heptene can be conveniently added, and after stirring for 30min, the solution is cooled to-95 ℃ to obtain 2, 6-di-tert-butyl-4-methylphenol and 1-heptene solution.
0.1g of 20% dichloroethylaluminum solution is weighed at-70 ℃ and added into 5g of 0.05wt% HCl methane chloride solution to be uniformly mixed to obtain catalyst solution, and after the catalyst solution is aged at-92 ℃ for 30min, the temperature is reduced to-95 ℃.
The reactor temperature was-95 ℃ and 11.25g of isobutylene, 63.75g of methyl chloride, 2g of 2, 6-di-tert-butyl-4-methylphenol and 1-heptene solution were sequentially added, followed by 0.5g of isoprene and mixed uniformly to obtain a reactant solution. After stirring for 15min, the above catalyst solution was added.
Adding the catalytic system into the reactant solution to react for 10min at the temperature of-95 ℃ to obtain the granular uniformly-dispersed slurry.
Adding 1g of ethanol to terminate the reaction, drying the obtained reaction product at 40 ℃ in vacuum for 48h, wherein the yield is 55%, performing nuclear magnetic analysis and gel permeation chromatography tests on the obtained product, and obtaining the butyl rubber with the unsaturation degree of 1.68 mol%, the weight average molecular weight of 18000, the molecular weight distribution of 5.5, the 300% definite elongation of the rubber of 7.0MPa and the tensile strength of 17.2 MPa.
Comparative example 1
The process flow and the steps are the same as those of the example 1, and the difference from the example 1 is that 2, 6-di-tert-butyl-4-methylphenol and 1-heptene are not added. The reaction begins with product agglomeration on the stirring paddle and the kettle wall.
The prepared butyl rubber product is subjected to nuclear magnetic analysis and gel permeation chromatography test, the obtained butyl rubber has the unsaturation degree of 1.50 mol%, the weight average molecular weight of 13000, the molecular weight distribution of 4.1, the 300% definite elongation of the rubber of 6.3MPa and the tensile strength of 16.1 MPa.
Comparative example 2
The process flow and the steps are the same as those of the example 1, and the difference from the example 1 is that 1-heptene is not added. The reaction polymerization product is granular in the diluent, and the glue hanging phenomenon in the reaction is weakened.
The prepared butyl rubber product is subjected to nuclear magnetic analysis and gel permeation chromatography test, the obtained butyl rubber has the unsaturation degree of 1.60 mol%, the weight average molecular weight of 14500, the molecular weight distribution of 4.0, the rubber 300% elongation of 76.5MPa and the tensile strength of 16.0 MPa.
Comparative example 3
The process flow and the steps are the same as those of the example 1, and the difference from the example 1 is that 2, 6-di-tert-butyl-4-methylphenol is not added. The reaction begins with product agglomeration on the stirring paddle and the kettle wall.
The prepared butyl rubber product is subjected to nuclear magnetic analysis and gel permeation chromatography test, the obtained butyl rubber has the unsaturation degree of 1.58 mol%, the weight average molecular weight of 16000, the molecular weight distribution of 5.6, the rubber 300% definite elongation of 7.1MPa and the tensile strength of 16.9 MPa.
After the phenolic compound and the mono-olefin are introduced into the reaction system, the polymerization product can be granular in the diluent, the phenomenon of glue hanging in the reaction is weakened, and the molecular weight and the distribution are effectively adjusted. The processing performance of the product is improved.
The invention provides a preparation method of butyl rubber, which introduces phenolic compounds and mono-olefin in the preparation process, effectively changes the mass transfer and heat transfer of a reaction system, ensures the continuous production of the butyl rubber, avoids frequent startup and shutdown in the production process, and ensures the good quality stability of products. Meanwhile, the molecular weight and the distribution are effectively adjusted, and the processing performance of the product is improved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (4)
1. The preparation method of the butyl rubber is characterized by comprising the following steps:
A) mixing isomonoolefin, conjugated diene, solvent, phenolic compound and monoolefine to obtain reactant solution; the monoolefin is selected from one or more of ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 1-heptene, 2-methyl-1-butene and 2-methyl-2-butene;
B) mixing a main catalyst, a cocatalyst and a solvent to obtain a catalyst solution;
C) mixing the catalyst solution with the reactant solution for reaction to obtain the butyl rubber
The phenolic compound is selected from one or more of p-methyl phenol, o-methyl phenol, 2, 6-di-tert-butyl-4-methyl phenol and 2, 2' -methylene bis (4-methyl-6-tert-butyl phenol);
the mass content of the phenolic compound in the reactant solution is 1-3000 mg/Kg;
the mass content of the mono-olefin in the isomonoolefin is 10-20000 mg/Kg;
the main catalyst is water or hydrogen chloride.
2. The process for preparing butyl rubber according to claim 1, wherein the co-catalyst is a lewis acid;
the molar ratio of the cocatalyst to the main catalyst is (1-10) to 1;
the molar ratio of the cocatalyst to the isomonoolefin is (0.0001-0.005): 1.
3. The method for preparing butyl rubber according to claim 2, wherein the cocatalyst is selected from one or more of aluminum trichloride, ethyl aluminum dichloride, butyl aluminum dichloride, dibutyl aluminum monochloride and boron trifluoride.
4. The method for preparing butyl rubber according to claim 1, wherein the reaction temperature is-98 to-80 ℃, and the reaction time is 1 to 20 min.
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| US2344213A (en) * | 1938-05-24 | 1944-03-14 | Otto Michael | Production of polymerization products from isobutylene |
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| CN108219050A (en) * | 2017-12-29 | 2018-06-29 | 黄河三角洲京博化工研究院有限公司 | A kind of preparation method of butyl rubber |
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| CN1523045A (en) * | 2003-02-17 | 2004-08-25 | 中国石油化工股份有限公司 | Process for polymerizing isoolefine cation |
| CN102140147A (en) * | 2010-02-03 | 2011-08-03 | 中国石油天然气股份有限公司 | Method for preparing butyl rubber by catalytic polymerization |
| CN108219050A (en) * | 2017-12-29 | 2018-06-29 | 黄河三角洲京博化工研究院有限公司 | A kind of preparation method of butyl rubber |
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