Separation and detection method for sulfurol-containing additive in styrene butadiene rubber

Abstract

The invention discloses a separation method for a sulfurol-containing additive in styrene butadiene rubber. The separation method at least comprises the following steps of sulfonating, wherein sulfonated styrene butadiene rubber is obtained from styrene butadiene rubber through a sulfonation reaction; separating, wherein water is added into the sulfonated styrene butadiene rubber to form a mixed solution; crosslinking, wherein polyphosphoric acid is added into the mixed solution to enable the sulfonated styrene butadiene rubber to be subjected to curing crosslinking, and then undissolved substances are separated out. According to the separation method, the sulfurol-containing additive in the styrene butadiene rubber can be accurately separated.

Description

technical field

[0001] The present invention relates to a method for separating and detecting additives in styrene-butadiene rubber, in particular to a method for separating and detecting sulfur-containing thiazole additives in styrene-butadiene rubber. Background technique

[0002] Styrene-butadiene rubber (SBR), as the most consumed general-purpose synthetic rubber (SR) variety, is widely used in the production of tires and tire products, footwear, hoses, tapes, medical equipment, auto parts, wires and cables with its excellent properties. Various other industrial rubber products. SBR is a general-purpose synthetic rubber synthesized from butadiene and styrene as monomers. Its processing performance is good, and its performance is close to that of natural rubber after being made into a finished product, and its physical and mechanical properties are good. Before the vulcanization of styrene-butadiene rubber, there is no cross-linking between the molecules, so it lacks go...

Examples

preparation example Construction

[0046] In one embodiment, the preparation method of the sulfonated styrene-butadiene rubber at least comprises the following steps:

[0047] Provide styrene butadiene rubber;

[0048] Provide sulfonation reagents;

[0049] The styrene-butadiene rubber is contacted with the sulfonating agent, and the sulfonated styrene-butadiene rubber is obtained through a sulfonation process.

[0050] Sulfonation process

[0051] The sulfonation process refers to the introduction of sulfonic acid groups into styrene-butadiene rubber through sulfonation reagents.

[0052] There are many types of sulfonation reagents and different reaction mechanisms. Some are electrophilic reactions, such as sulfuric acid, sulfur trioxide, oleum, etc.; some are nucleophilic reactions, such as sodium sulfite, sodium bisulfite, etc.; some are free radical reactions, such as sulfur dioxide and chlorine, sulfur dioxide and oxygen, etc. Sulfonation on the benzene ring is an electrophilic reaction. First, the...

Embodiment 1

[0094] The sample is styrene-butadiene rubber containing 1 % mass fraction of 2-mercaptobenzothiazole.

[0095] 1. Weigh 10 g of the sample, crush the sample, dissolve the sample in 50 mL of chloroform, and stir at room temperature until the styrene-butadiene rubber is completely dissolved to obtain a mixed solution;

[0096] 2. Add the above mixed solution into a three-necked flask with a reflux, stirring and temperature control system, and control the sulfonation reaction temperature to be 0°C. Under vigorous stirring, slowly add 0.50g of chlorosulfonic acid dropwise to the system. After the addition, nitrogen was continuously introduced into the system, and the sulfonation time was 1 h to obtain a sulfonated styrene-butadiene rubber solution (the sulfonation degree of the styrene-butadiene rubber was 20%).

[0097] 3. Add 100 mL of water to the sulfonated styrene-butadiene rubber solution, and after shaking, add 5 g of pyrophosphoric acid to the sulfonated styrene-butadiene...

Embodiment 2

[0104] The sample is styrene-butadiene rubber containing 1 % mass fraction of 2-mercaptobenzothiazole.

[0105] 1. Weigh 10 g of the sample, crush the sample, dissolve the sample in 50 mL of chloroform, and stir at room temperature until the styrene-butadiene rubber is completely dissolved to obtain a mixed solution;

[0106] 2. Add the above mixed solution into a three-necked flask with a reflux, stirring and temperature control system, and control the sulfonation reaction temperature to be 10°C. Under vigorous stirring, slowly add 0.50g of concentrated sulfuric acid dropwise to the system, add dropwise After the completion, nitrogen was continuously introduced into the system, and the sulfonation time was: 4 h to obtain a sulfonated styrene-butadiene rubber solution (the sulfonation degree of the styrene-butadiene rubber was 45%).

[0107] 3. Add 100 mL of water to the sulfonated styrene-butadiene rubber solution, and after shaking, add 10 g of pyrophosphoric acid to the sul...

technical field

[0001] The present invention relates to a method for separating and detecting additives in styrene-butadiene rubber, in particular to a method for separating and detecting sulfur-containing thiazole additives in styrene-butadiene rubber. Background technique

[0002] Styrene-butadiene rubber (SBR), as the most consumed general-purpose synthetic rubber (SR) variety, is widely used in the production of tires and tire products, footwear, hoses, tapes, medical equipment, auto parts, wires and cables with its excellent properties. Various other industrial rubber products. SBR is a general-purpose synthetic rubber synthesized from butadiene and styrene as monomers. Its processing performance is good, and its performance is close to that of natural rubber after being made into a finished product, and its physical and mechanical properties are good. Before the vulcanization of styrene-butadiene rubber, there is no cross-linking between the molecules, so it lacks go...

Examples

preparation example Construction

[0046] In one embodiment, the preparation method of the sulfonated styrene-butadiene rubber at least comprises the following steps:

[0047] Provide styrene butadiene rubber;

[0048] Provide sulfonation reagents;

[0049] The styrene-butadiene rubber is contacted with the sulfonating agent, and the sulfonated styrene-butadiene rubber is obtained through a sulfonation process.

[0050] Sulfonation process

[0051] The sulfonation process refers to the introduction of sulfonic acid groups into styrene-butadiene rubber through sulfonation reagents.

[0052] There are many types of sulfonation reagents and different reaction mechanisms. Some are electrophilic reactions, such as sulfuric acid, sulfur trioxide, oleum, etc.; some are nucleophilic reactions, such as sodium sulfite, sodium bisulfite, etc.; some are free radical reactions, such as sulfur dioxide and chlorine, sulfur dioxide and oxygen, etc. Sulfonation on the benzene ring is an electrophilic reaction. First, the...

Embodiment 1

[0094] The sample is styrene-butadiene rubber containing 1 % mass fraction of 2-mercaptobenzothiazole.

[0095] 1. Weigh 10 g of the sample, crush the sample, dissolve the sample in 50 mL of chloroform, and stir at room temperature until the styrene-butadiene rubber is completely dissolved to obtain a mixed solution;

[0096] 2. Add the above mixed solution into a three-necked flask with a reflux, stirring and temperature control system, and control the sulfonation reaction temperature to be 0°C. Under vigorous stirring, slowly add 0.50g of chlorosulfonic acid dropwise to the system. After the addition, nitrogen was continuously introduced into the system, and the sulfonation time was 1 h to obtain a sulfonated styrene-butadiene rubber solution (the sulfonation degree of the styrene-butadiene rubber was 20%).

[0097] 3. Add 100 mL of water to the sulfonated styrene-butadiene rubber solution, and after shaking, add 5 g of pyrophosphoric acid to the sulfonated styrene-butadiene...

Embodiment 2

[0104] The sample is styrene-butadiene rubber containing 1 % mass fraction of 2-mercaptobenzothiazole.

[0105] 1. Weigh 10 g of the sample, crush the sample, dissolve the sample in 50 mL of chloroform, and stir at room temperature until the styrene-butadiene rubber is completely dissolved to obtain a mixed solution;

[0106] 2. Add the above mixed solution into a three-necked flask with a reflux, stirring and temperature control system, and control the sulfonation reaction temperature to be 10°C. Under vigorous stirring, slowly add 0.50g of concentrated sulfuric acid dropwise to the system, add dropwise After the completion, nitrogen was continuously introduced into the system, and the sulfonation time was: 4 h to obtain a sulfonated styrene-butadiene rubber solution (the sulfonation degree of the styrene-butadiene rubber was 45%).

[0107] 3. Add 100 mL of water to the sulfonated styrene-butadiene rubber solution, and after shaking, add 10 g of pyrophosphoric acid to the sul...

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