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Preparation method of brominated butyl rubber under action of phase transfer agent

A technology of brominated butyl rubber and phase transfer agent, which is applied in the field of butyl rubber, can solve the problem of low utilization rate of bromine element, and achieve the effect of increasing bromination reaction speed and utilization rate

Pending Publication Date: 2022-07-26
山东京博中聚新材料有限公司
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

Therefore, the utilization rate of bromine element in bromobutyl rubber is low at present

Method used

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  • Preparation method of brominated butyl rubber under action of phase transfer agent
  • Preparation method of brominated butyl rubber under action of phase transfer agent

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preparation example Construction

[0026] In the present invention, the preparation method of bromobutyl rubber under the action of the phase transfer agent specifically comprises the following steps:

[0027] Mix the butyl rubber solution, the oxidant and the phase transfer agent to obtain a mixed glue; wherein the mass ratio of the butyl rubber to the oxidant and the phase transfer agent is 100:(0.01-10):(0.001-5) to obtain the mixed glue ;

[0028] Wherein, the butyl rubber solution is a non-polar or weakly polar organic solution of butyl rubber, and the non-polar or weakly polar organic solvent used is C5~C30 straight chain alkane, branched chain alkane or cyclic alkane Alkanes or their mixtures, the concentration of the butyl rubber solution is any value between 10wt% and 25wt%. The mass ratio of butyl rubber to weak polar or non-polar alkane is any value in (11-35):100,

[0029] After obtaining the butyl rubber solution, add an oxidizing agent and a phase transfer agent to the butyl rubber solution and ...

Embodiment 1

[0050] (1) Configure 20kg of 20% butyl rubber glue, (Mooney 35, 1.7% unsaturation), 2.5kg of 5% bromine-n-hexane solution, 200g of 30% hydrogen peroxide solution, an appropriate amount of 2% sodium hydroxide solution, Phase transfer agent tetradecyltrimethylammonium chloride.

[0051] (2) Add 0.4% dry glue mass oxidant solution, 0.1% dry glue mass phase transfer agent and a small amount of distilled water to the glue solution to control the water content of the system to about 1%.

[0052] (3) Control the flow rate of glue solution at 200ml / min and bromine solution at 28ml / min.

[0053] (4) control 45 ℃ in the bromination reaction still, rotating speed 300rpm, at this moment, the residence time in the still is about 9min, control and neutralize 45 ℃ in the reaction still, rotating speed 300rpm, this moment material stays about 5min, the reaction system after the lye neutralization pH is 7-10

[0054] (5) Add 2.2%, 1.3%, 0.1% calcium stearate, epoxidized soybean oil, and anti...

Embodiment 2

[0056] (1) Prepare 20kg of 15% butyl rubber glue (Mooney 35, 1.7% unsaturation), 2kg of 5% bromine-n-hexane solution, and an appropriate amount of 2% sodium hydroxide solution, prepare solid sodium hypochlorite, phase transfer agent three Butylamine.

[0057] (2) Add sodium hypochlorite with 0.1% dry glue mass, phase transfer agent with 0.15% dry glue mass and a small amount of distilled water to the glue solution, and control the water content of the system to about 0.5%.

[0058] (3) Control the flow rate of glue solution at 190ml / min and bromine solution at 18ml / min.

[0059] (4) control 50 ℃ in bromination reaction kettle, rotating speed 300rpm, at this moment, the residence time in kettle is about 10min, control neutralization reaction kettle at 45 ℃, rotating speed 300rpm, material stays about 5min now, and the system is neutral.

[0060] (5) Add 2.2%, 1.3%, 0.1% calcium stearate, epoxidized soybean oil, and antioxidant 1076 to the neutralized glue solution after drying...

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Abstract

The invention provides a preparation method of brominated butyl rubber under the action of a phase transfer agent. According to the method, the brominated butyl rubber is prepared by taking weak polar or non-polar alkane as a solvent and using a solution method, and the bromine content and the microstructure in the brominated butyl rubber are analyzed mainly by using general methods such as 1H NMR and the like. According to the method, firstly, an oxidizing agent and a phase transfer agent solution are added into a butyl rubber solution according to a certain proportion, then the mixture is mixed with an alkane solution of liquid bromine for a bromination reaction, the oxidizing agent can oxidize reaction byproducts into elemental bromine to further participate in the reaction, the phase transfer agent accelerates oil-water two-phase mass transfer, and the bromine utilization rate and the reaction rate are increased. After the reaction is finished, adding an alkaline solution to enable the system to be neutral or alkalescent; the bromine content in the obtained brominated butyl rubber is 0.85-1.05%, and the ratio of primary bromine to secondary bromine is less than 0.2: 1. The method has more competitive production cost and less industrial wastewater, and the product performance can meet the use requirements of industrial products such as automobile tires and medical rubber plugs.

Description

technical field [0001] The invention belongs to the technical field of butyl rubber, and in particular relates to a preparation method of bromobutyl rubber under the action of a phase transfer agent. Background technique [0002] Bromobutyl rubber (BIIR) has the advantages of fast vulcanization, good mutual adhesion and compatibility, and can be vulcanized with zinc oxide alone. It has gradually replaced ordinary butyl rubber in various applications, such as radial tires, heat-resistant inner tubes. , container liners, pharmaceutical stoppers and machine liners and other industrial products. [0003] Since this reaction is a substitution reaction of bromine, the utilization rate of bromine element is only 40-50%, and the rest is discharged in the form of bromine salt. Therefore, the utilization rate of bromine element in bromobutyl rubber is low at present. SUMMARY OF THE INVENTION [0004] In view of this, the technical problem to be solved by the present invention is t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F8/22C08F210/12
CPCC08F8/22C08F210/12
Inventor 韩飞陈铁龙张杰荆帅林谢晴李立霞黄启谷郑红兵任学斌
Owner 山东京博中聚新材料有限公司
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