CN110642965A - Preparation method of brominated butyl rubber - Google Patents
Preparation method of brominated butyl rubber Download PDFInfo
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Abstract
The invention provides a preparation process of brominated butyl rubber, which comprises the following steps: A) mixing butyl rubber, a dispersing agent and a solvent to obtain a glue solution; mixing liquid bromine with a hydrocarbon solvent to obtain bromine liquid; B) mixing and reacting the glue solution, the bromine solution and an oxidant to obtain an initial product; C) and (3) performing neutralization reaction on the initial product, then adding a dispersing agent, removing the solvent, and drying to obtain the brominated butyl rubber. This application is at the in-process of preparation brominated butyl rubber, has introduced the oxidant, and its oxidant as byproduct hydrogen bromide converts the bromine hydrogen into bromine simple substance, has still reduced bromine ion concentration when reducing bromine simple substance, and then has reduced brominated butyl rubber's whole running cost to the added value of brominated butyl rubber has been improved.
Description
Technical Field
The invention relates to the technical field of brominated butyl rubber, in particular to a preparation method of brominated butyl rubber.
Background
Brominated butyl rubber is a product of substitution reaction of bromine and butyl rubber, and is a modified product of butyl rubber with high densityIs 0.92g/cm3The appearance was a white to beige massive solid. The brominated butyl rubber is mainly applied to an air-tight layer and a medical rubber plug of a tubeless tire, the brominated butyl rubber is more and more favored by the tire industry with excellent performance, and along with the development of the domestic tire industry, the demand of the brominated butyl rubber is more and more large, so that various domestic and foreign brominated butyl rubber production plants are built and expanded, and an effective way for improving the competitiveness is not only to improve the quality of products, but also to continuously reduce the material consumption and reduce the cost.
As shown in fig. 1, fig. 1 is a traditional process flow diagram of brominated butyl rubber, wherein 1 is a bromine storage tank, 2 is a bromination reactor, 3 is a retention tank, 4 is a neutralization system, 5 is a washing system, 6 is a flash tank, 7 is a stripping tower, and the specific process is as follows: the liquid bromine is stored in a special storage tank provided with a nitrogen sealing system and is pumped to a reactor through a bromine metering pump, and in order to reduce the density of reactants and improve the distribution of the reactants in the reactor, bromine needs to be diluted by a hydrocarbon solvent, wherein the mass ratio of the bromine to the hydrocarbon solvent is 10-15 wt%; the flow rate of the butyl rubber solution is kept constant through a flow controller, the flow controller is connected with a flow ratio controller, the flow rate of the liquid bromine is set in a cascade mode through a speed control system acting on a metering pump, and the butyl rubber solution and the diluted bromine are injected from different injection ports on a reactor; controlling the temperature of a bromination reactor at 30-50 ℃, then stabilizing the product through a retention tank, sending the reaction product to a neutralization reactor, and carrying out a neutralization reaction on a byproduct, namely hydrogen bromide and unreacted bromine in a halogenation reaction and a neutralization solution (sodium hydroxide); and then the reaction product is washed by a washing system, wherein all equipment for bromination reaction and neutralization reaction are arranged in a factory building to protect the external environment.
In the above-mentioned reaction of bromine and butyl rubber, the theoretical maximum proportion of bromine injected into the reactor to the butyl rubber chain is 50% by weight, that is, 1mol of elemental bromine participates in the reaction, 0.5mol of elemental bromine is combined with the butyl rubber, and 0.5mol of hydrogen bromide is generated. The bromine utilization rate is reduced due to the loss of the rest bromine caused by the generation of the byproduct hydrogen bromide, and the hydrogen bromide is very corrosive and is one of the reasons for the deterioration of the quality of the brominated butyl rubber, for example, the brominated butyl rubber is discolored due to too strong acidity. Alkali liquor (sodium hydroxide or potassium hydroxide) is added in the subsequent reaction to convert the bromine into bromine salt. The hydrogen bromide and the double bond react to form a saturated structure containing tertiary bromine, which does not contribute to sulfuration and is referred to as a bromine-ineffective or hydrobrominated structure. The acidity caused by hydrogen bromide is one of the parameters that promote the isomerization (rearrangement) from the exomethylene structure (II) to the endo methylene structure (III); therefore, when the acidity is too strong, the rearrangement of the exomethylene structure to the endo methylene structure is promoted, and the effective bromine structure content of the brominated butyl rubber is reduced.
In summary, the conventional bromination process has the following disadvantages: firstly, the unit consumption of bromine is high, and the production cost is high; consumption of hydrogen bromide as a byproduct and consumption of alkali liquor; the bromide ion concentration of the bromide waste water generated after neutralization is high, the bromide treatment load is increased, and the operation cost is high; and the brominated butyl rubber has low physical properties such as strength and the like. Therefore, it is urgently needed to provide a production process of brominated butyl rubber, which can effectively reduce the unit consumption of bromine, so as to improve the product quality of the brominated butyl rubber.
Disclosure of Invention
The invention aims to provide a preparation method of brominated butyl rubber, which can reduce bromine unit consumption, reduce the concentration of bromide ions and improve the quality of the brominated butyl rubber.
In view of the above, the present application provides a preparation process of brominated butyl rubber, comprising the following steps:
A) mixing butyl rubber, a dispersing agent and a solvent to obtain a glue solution;
mixing liquid bromine with a hydrocarbon solvent to obtain bromine liquid;
B) mixing and reacting the glue solution, the bromine solution and an oxidant to obtain an initial product;
C) and (3) performing neutralization reaction on the initial product, then adding a dispersing agent, removing the solvent, and drying to obtain the brominated butyl rubber.
Preferably, the oxidant is hydrogen peroxide.
Preferably, the concentration of the hydrogen peroxide is 25-40 wt%, and the filling amount of the hydrogen peroxide is 10-22 kg/t of brominated butyl rubber.
Preferably, the concentration of the hydrogen peroxide is 30-35 wt%, and the filling amount of the hydrogen peroxide is 12-20 kg/t of brominated butyl rubber.
Preferably, the unsaturation degree of the butyl rubber is 1.65 mol% to 1.85 mol%.
Preferably, the unsaturation degree of the butyl rubber is 1.70 mol% to 1.80 mol%.
Preferably, the dispersing agent is calcium stearate; in the step A), the content of the calcium stearate is 0.3-0.6 wt% of the butyl rubber; in the step C), the content of the calcium stearate is 1.5-3.0 wt% of the brominated butyl rubber.
Preferably, the concentration of the glue solution is 10 wt% -30 wt%.
Preferably, the reaction temperature is 20-60 ℃, and the reaction time is 3-10 min.
Preferably, the drying is carried out in a double-screw expansion drying extruder, and the temperature of a die head of the double-screw expansion drying extruder is 90-160 ℃.
The application provides a preparation method of brominated butyl rubber, which comprises the steps of firstly preparing a glue solution containing butyl rubber and a bromine solution containing liquid bromine, and then mixing and reacting the glue solution, the bromine solution and an oxidant to obtain the brominated butyl rubber; in the process of preparing the brominated butyl rubber, the oxidant is introduced and is used as the oxidant of the hydrogen bromide, so that the byproduct hydrogen bromide can be converted into a raw material bromine simple substance, the unit consumption of bromine is reduced, the concentration of bromine ions can be reduced, the cost of the brominated butyl rubber is reduced, and the tensile strength of the brominated butyl rubber is improved. The experimental results show that: the preparation process of the brominated butyl rubber can reduce the unit consumption of bromine simple substances by 30-45 wt%, the amount of neutralizing alkali liquor is reduced by 20-25 wt%, the concentration of bromide ions is reduced by 20-45 wt%, the microstructure content of the brominated butyl rubber is adjusted, the content of II structures (outer methylene) is improved to more than 60%, the content of III structures (inner methylene) is reduced to less than 8%, the content of functional bromine (effective bromine) is improved to more than 1.00 mol%, the tensile strength is improved to more than 16MPa, and the 300% definite elongation is improved to more than 7.4 MPa.
Drawings
FIG. 1 is a flow diagram of a conventional process for preparing brominated butyl rubber;
FIG. 2 is a flow diagram of a process for preparing brominated butyl rubber of the present invention.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention by way of example, and it is to be understood that the description is intended to further illustrate features and advantages of the invention, and not to limit the scope of the claims.
In view of the problems of high unit consumption of bromine in brominated butyl rubber and a series of problems of hydrogen bromide as a byproduct in the prior art, the application provides a preparation method of brominated butyl rubber, and an oxidant is introduced in the method, so that the conversion rate of bromination reaction is improved, and the unit consumption of bromine simple substances and a series of problems caused by subsequent bromination can be reduced. Specifically, the embodiment of the invention discloses a preparation process of brominated butyl rubber, which comprises the following steps:
A) mixing butyl rubber, a dispersing agent and a solvent to obtain a glue solution;
mixing liquid bromine with a hydrocarbon solvent to obtain bromine liquid;
B) mixing and reacting the glue solution, the bromine solution and an oxidant to obtain an initial product;
C) and adjusting the pH value of the initial product, removing the solvent, and drying to obtain the brominated butyl rubber.
In the process of preparing the brominated butyl rubber, firstly, preparing raw materials, mixing the butyl rubber, a dispersing agent and a solvent to obtain a glue solution, and similarly, mixing liquid bromine and a hydrocarbon solvent to obtain a bromine solution; in the process, the process of obtaining the glue solution can be divided into two stages: firstly, mixing butyl rubber and a dispersing agent to obtain colloidal particle water, and mixing the colloidal particle water with a solvent to obtain a glue solution; the unsaturation degree of the butyl rubber is 1.65-1.85 mol%, in a specific embodiment, the unsaturation degree of the butyl rubber is 1.70-1.80 mol%, the unsaturation degree represents the mole fraction of unsaturated double bonds on a molecular chain, the bromination reaction conversion rate is low when the unsaturation degree is too low, and the aging resistance of a product is reduced when the unsaturation degree is too high; the dispersant is selected from calcium stearate in a specific embodiment, and the content of the calcium stearate is 0.3-0.6 wt%, and the content of the calcium stearate is 0.4-0.5 wt%; if the content of the calcium stearate is too low, the dispersing effect is poor, the colloidal particles form a rubber blanket, the risk of sticking together a kettle is increased, and if the content of the calcium stearate is too high, the polymerized colloidal particle water returns when being sent to a bromination dewatering screen; the concentration of the glue solution is 10-30 wt%, in a specific embodiment, the concentration of the glue solution is 15-25 wt%, when the concentration of the glue solution is too low, the substitution reaction probability of bromine is reduced, the production efficiency is reduced, along with the increase of the concentration of the glue solution, the substitution reaction probability of bromine is increased, and when the concentration of the glue solution is too high, the viscosity of the glue solution is also higher, which is not beneficial to the delivery of a pump and is also not beneficial to the bromination reaction. The solvent is well known to those skilled in the art as long as it is capable of achieving dissolution of the butyl rubber, and in particular embodiments, the solvent is selected from hexane. In the process of preparing the bromine liquid, the liquid bromine is a raw material well known to those skilled in the art, and the present application is not particularly limited, and the hydrocarbon solvent is selected from solvents well known to those skilled in the art, and the present application is not particularly limited.
After the raw materials are prepared, mixing the glue solution, the bromine solution and an oxidant, and reacting to obtain an initial product; in the process, elemental bromine and butyl rubber are subjected to bromination reaction to obtain brominated butyl rubber, and a byproduct hydrogen bromide is generated; the oxidant is introduced as the oxidant of the hydrogen bromide, the byproduct hydrogen bromide after the reaction of bromine and butyl rubber can be converted into a bromine simple substance, and the bromine simple substance is used as the raw material again, so that the unit consumption of bromine is reduced, and the concentration of bromine ions can also be reduced. The initial product is the acidic product. In order to not introduce additional impurities, the oxidant is selected from hydrogen peroxide, the concentration of the hydrogen peroxide is 25-40 wt%, and the filling amount of the hydrogen peroxide is 10-22 kg/t of brominated butyl rubber, in a specific embodiment, the concentration of the oxidant is 30-35 wt%, and the filling amount of the hydrogen peroxide is 12-20 kg/t of brominated butyl rubber; the utilization rate of bromine cannot be obviously improved when the adding amount of the oxidant is too low. The temperature of the reaction is 20-60 ℃, and the time is 3-10 min; in a specific embodiment, the reaction temperature is 30-50 ℃, and the reaction time is 5-8 min; the reaction temperature is too low, the viscosity of the glue solution is obviously increased, the mixing of the glue solution and bromine is not facilitated, the reaction degree of the glue solution and the bromine is continuously increased along with the increase of the reaction temperature, but the temperature is too high, and the bromination side reaction is increased; the reaction time is too short, the bromination reaction is insufficient, the reaction time is too long, and the long-time acidic environment increases the bromination side reaction and seriously affects the microstructure proportion of the final product. In the process, the mass ratio of the dispersing agent to the generated brominated butyl rubber is 1.5 wt% to 3.0 wt%, in a specific embodiment, the dispersing agent is 2.0 wt% to 2.5 wt% of the brominated butyl rubber, and the dispersing agent also reacts with hydrogen bromide, which can be regarded as a deacidification agent, and the proper content of the deacidification agent is beneficial to the adjustment of the effective bromine structure content of the final product.
The application then subjects the initial product to a neutralization reaction. In the process, adjusting the pH of the initial product by using alkali liquor, namely adjusting the unoxidized hydrogen bromide by using alkali liquor, wherein the pH value is 5-12, and in a specific embodiment, the pH value is 7-10; if the pH value is too low, residual acidic substances in the product are remained, the content of the external methylene structure (II) is low, the content of the internal methylene structure (III) is high, the vulcanization process is influenced, and the final strength and other physical properties of the brominated butyl rubber are influenced; when the pH value is too high, the alkali liquor is excessive, and generates a substance easy to foam with the dispersing agent, and the subsequent condensation and product drying are not facilitated.
And the product enters a washing system for washing, and then enters a flash evaporation and stripping system for recovering the solvent. A dispersant is added into the flash tank, the mass ratio of the dispersant to the generated brominated butyl rubber is 1.5-3.0 wt% in the process, in a specific embodiment, the dispersant is 2.0-2.5 wt% of the brominated butyl rubber, and the dispersant can react with possibly residual hydrogen bromide besides the function of dispersing colloidal particles, and can be regarded as a deacidification agent, and the proper content of the deacidification agent is beneficial to the adjustment of the effective bromine structure content of the final product.
The application carries out a post-treatment drying unit after removing the solvent; through three-stage and fluidized bed dehydration, the volatile component of the brominated butyl rubber is within a qualified range, specifically, a third-stage drying unit, namely a double-screw expansion drying extruder, is dehydrated by utilizing shearing force, and the opening of a die hole is adjusted to control the volatile component, so that the product is seriously debrominated when the temperature is too high; the temperature of the die head is generally controlled to be 90-160 ℃, preferably 110-140 ℃, when the temperature is too low, the volatile component can not meet the requirement, the devolatilization pressure is transferred to the fluidized bed, and the output can be limited when the load of the fluidized bed is increased; too high a temperature can cause severe debromination of the product, thereby affecting the usability of the product for downstream customers.
FIG. 2 is a process flow diagram of a bromination reaction of the present application; and (2) allowing the glue solution, the oxidant and the bromine solution to enter a bromination reactor for bromination reaction, allowing the reacted product to enter a retention tank, allowing the reacted product to enter a neutralization system for reacting unoxidized hydrogen bromide, washing by a washing system, allowing the washed product to pass through a flash tank and a stripper, adding various auxiliaries, recovering the solvent, and performing aftertreatment, dehydration and drying on the glue solution to obtain the brominated butyl rubber.
The preparation of the brominated butyl rubber is characterized in that an injection port of an oxidant is added in an original bromination reactor, a proper oxidant is selected, preferably hydrogen peroxide, and the bromination conversion rate is improved, so that the unit consumption of a bromine simple substance can be reduced by 30-45 wt%, the conversion rate of the bromine simple substance can be improved to 80 wt%, the amount of a neutralization alkali solution is reduced by 20-25 wt%, the concentration of bromine ions is reduced by 20-45 wt%, the microstructure content of a product is adjusted, the content of a structure II (outer methylene) is improved to more than 60%, the content of a structure III (inner methylene) is reduced to less than 8%, the content of functional bromine (effective bromine) is improved to more than 1.00 mol%, the tensile strength is improved to more than 16MPa, and the 300% definite elongation is improved to more than 7.4 MPa.
For further understanding of the present invention, the following examples are provided to illustrate the preparation of the brominated butyl rubber of the present invention, and the scope of the present invention is not limited by the following examples.
Example 1
Obtaining a base rubber with the unsaturation degree of 1.70 mol% by adjusting the mass ratio of isobutene to isoprene, wherein the adding amount of calcium stearate serving as a dispersing agent in a polymerization flash tank is 0.4 wt% of butyl rubber to obtain colloidal particle water; 5 wt% of colloidal particle water enters a dewatering screen of a bromination process, then hexane is adopted for sol, the concentration of a glue solution before entering a bromination reactor is controlled to be 15 wt%, an oxidant metering tank is added on the basis of the original bromination reaction, an injection port is added on the bromination reactor, hydrogen peroxide is selected as an oxidant, the purity of the hydrogen peroxide is 30 wt%, the unit consumption of the hydrogen peroxide is controlled to be 12kg/t, the bromination reaction temperature is controlled to be 30 ℃, the reaction residence time is 5min, the neutralization pH value is controlled to be 7.0, and the calcium stearate content of a brominated dispersant is 2.2 wt% of that of brominated butyl rubber; feeding the mixture into a halogenation flash tank and a stripping tower to recover and remove the solvent, and adding calcium stearate into the flash tank; the solvent is effectively removed and then recycled; and (3) carrying out aftertreatment and drying on the mixed glue solution, controlling the temperature of a die head of a double-screw expansion extruder of a drying unit to be 110 ℃, measuring the total bromine content of the product by a fluorescence method to be 2.0 wt%, further calculating to obtain that the bromine conversion rate is 55 wt%, and detecting to obtain that the II structure content, the III structure content and the functional bromine content of the final product are 60%, 7.9% and 1.00 mol%. In addition, the bromine ion concentration is reduced to 7.8 wt%, so that the bromine salt wastewater treatment load is reduced, the operation cost is effectively reduced, and the tensile strength of the product is improved to 16.2 MPa.
The preparation processes of the embodiments 2 to 3 are the same as those of the embodiment 1, except that: the unsaturation degree of the polymerization base glue, the content of a dispersing agent, the concentration of the glue solution, the unit consumption of an oxidant, the bromination reaction temperature, the retention time, the neutralization pH value, the content of calcium stearate and the post-treatment drying temperature are different, and the specific control process conditions are shown in the following table 1:
TABLE 1 data Table of relevant parameters of the preparation of brominated butyl rubbers of examples 1 to 3
On the premise of ensuring that the total bromine content of the product is 2.0 wt%, the conversion rate of bromine is respectively calculated, the microstructure content of the product in the examples 1-3 and the bromine ion concentration, microstructure content, bromine ion concentration and tensile strength in bromine brine are detected, and the results are shown in table 2:
TABLE 2 data Table for products prepared in examples 1-3
| Bromine conversion/wt% | Content of II Structure | III structural content | Content of functional bromine | Bromide ion concentration/wt% | Tensile strength/MPa | |
| Example 1 | 55 | 60 | 7.9 | 1.00 | 7.8 | 16.2 |
| Example 2 | 70 | 62 | 7.3 | 1.03 | 6.7 | 16.6 |
| Example 3 | 80 | 63 | 7.0 | 1.05 | 5.5 | 17.1 |
From the above calculation and detection results, in the bromination reaction process provided by the invention, the unsaturation degree of the polymerization base rubber, the concentration of the rubber solution, the reaction temperature, the residence time and the operating conditions of the neutralization pH value are controlled, and the amount of the dispersing agent, the unit consumption of the oxidizing agent and the outlet temperature of the double-screw drying extruder are adjusted, so that the structure II and structure III content and the functional bromine content of the product reach the international leading level, the conversion rate of bromine is greatly improved, the ion concentration of bromine brine is reduced, the operating cost is reduced, the market competitiveness is improved, and the environmental protection is facilitated.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A preparation process of brominated butyl rubber comprises the following steps:
A) mixing butyl rubber, a dispersing agent and a solvent to obtain a glue solution;
mixing liquid bromine with a hydrocarbon solvent to obtain bromine liquid;
B) mixing and reacting the glue solution, the bromine solution and an oxidant to obtain an initial product;
C) and (3) performing neutralization reaction on the initial product, then adding a dispersing agent, removing the solvent, and drying to obtain the brominated butyl rubber.
2. The preparation process according to claim 1, wherein the oxidant is hydrogen peroxide.
3. The preparation process of claim 2, wherein the concentration of the hydrogen peroxide is 25-40 wt%, and the filling amount of the hydrogen peroxide is 10-22 kg/t of the brominated butyl rubber.
4. The preparation process according to claim 2 or 3, wherein the concentration of the hydrogen peroxide is 30-35 wt%, and the filling amount of the hydrogen peroxide is 12-20 kg/t of the brominated butyl rubber.
5. The process according to claim 1, wherein the butyl rubber has an unsaturation degree of 1.65 to 1.85 mol%.
6. The process according to claim 1 or 5, wherein the butyl rubber has an unsaturation degree of 1.70 mol% to 1.80 mol%.
7. The process according to claim 1, wherein the dispersant is calcium stearate; in the step A), the content of the calcium stearate is 0.3-0.6 wt% of the butyl rubber; in the step C), the content of the calcium stearate is 1.5-3.0 wt% of the brominated butyl rubber.
8. The preparation process according to claim 1, wherein the concentration of the glue solution is 10 wt% to 30 wt%.
9. The preparation process according to claim 1, wherein the reaction temperature is 20-60 ℃ and the reaction time is 3-10 min.
10. The method for preparing the rubber composition according to claim 1, wherein the drying is performed in a twin-screw expansion drying extruder, and the temperature of a die head of the twin-screw expansion drying extruder is 90-160 ℃.
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| CN112142884B (en) * | 2020-09-01 | 2023-06-09 | 中北大学 | Brominated butyl rubber synthesis device and process |
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