Preparation method of emulsion-polymerized styrene butadiene rubber

An emulsion polystyrene butadiene rubber, selected technology, applied in the field of preparation of emulsion polystyrene butadiene rubber, can solve the problems of fast consumption of mercaptan, molecular weight control, wide molecular weight distribution, etc., to achieve stable product performance, good molecular weight adjustment effect, good reproducibility

Inactive Publication Date: 2012-07-18
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0006] (2) The chain transfer constants of various alkyl mercaptans are quite close to vinyl monomers, therefore, it is difficult to optimize the chain transfer constants of mercaptans as chain transfer agents for vinyl monomers
Since the chain transfer constant of mercaptans to vinyl monomers is usually relatively large, when mercaptans are used in emulsion polymerization systems, there will be a large consumption of mercaptans in the early stage of polymerization, and the molecular weight of the polymer cannot be controlled in the later stage of polymerization, resulting in monomer conversion. When the rate reaches about 60%, the polymerization will be term

Method used

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  • Preparation method of emulsion-polymerized styrene butadiene rubber
  • Preparation method of emulsion-polymerized styrene butadiene rubber
  • Preparation method of emulsion-polymerized styrene butadiene rubber

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0043] Example 1

[0044] The first is the preparation of the water phase, which contains 190g of water, 4.62g of disproportionated rosin acid soap, 0.231g of phosphoric acid, 0.396g of potassium hydroxide, 0.055g of ethylenediaminetetraacetic acid tetrasodium salt, and 0.13 of sodium dinaphthylmethane disulfonate. g, 0.04 g of sodium dithionite, 0.01 g of ferrous sulfate, and 0.04 g of sodium formaldehyde sulfoxylate, add them to the reaction flask and stir well.

[0045] Next is the oil phase preparation. Dissolve 23 g of styrene monomer in 0.1 g of n-butyl-2-phenyl allyl sulfide ( figure 2 ), and dissolve evenly, then add it to the reaction flask. Then, 72 g of butadiene was added, the temperature was lowered to 5°C, and emulsification was performed for 20 minutes.

[0046] Finally, add the oxidant organic solution containing 5g styrene, 0.06g hydrogen peroxide p-menthane, and react at 5°C for 9 hours. When the conversion rate reaches 68%, add a terminator solution containing 0....

Example Embodiment

[0047] Example 2

[0048] The first is the preparation of the water phase, which contains 185g of water, 4.65g of disproportionated rosin acid soap, 0.235g of phosphoric acid, 0.4g of potassium hydroxide, 0.05g of ethylenediaminetetraacetic acid tetrasodium salt, and 0.15g of sodium dinaphthylmethane disulfonate. g, 0.05 g of sodium dithionite, 0.01 g of ferrous sulfate, and 0.03 g of sodium formaldehyde sulfoxylate, add them to the reaction flask and stir well.

[0049] Followed by the oil phase preparation, dissolve 0.15g of n-butyl-2-phenylallyl sulfide ( figure 2 ), and dissolve evenly, then add it to the reaction flask. Then, 72 g of butadiene was added, the temperature was lowered to 4°C, and emulsification was performed for 20 minutes.

[0050] Finally, add the oxidant organic solution containing 4g styrene, 0.05g hydrogen peroxide p-menthane, and react at 5°C for 10 hours. When the conversion rate reaches 70%, add the terminator solution, which contains 0.11g dithiocarbamat...

Example Embodiment

[0051] Example 3

[0052] The first is the preparation of the water phase, which contains 188g of water, 4.7g of disproportionated rosin acid soap, 0.24g of phosphoric acid, 0.4g of potassium hydroxide, 0.05g of ethylenediaminetetraacetic acid tetrasodium salt, and 0.15g of sodium dinaphthylmethane disulfonate. g, 0.05 g of sodium dithionite, 0.01 g of ferrous sulfate, and 0.03 g of sodium formaldehyde sulfoxylate, add them to the reaction flask and stir well.

[0053] Followed by the oil phase preparation, dissolve 23g of styrene monomer in 0.1g of n-dodecyl-2-phenylallyl sulfide ( figure 2 ), and dissolve evenly, then add it to the reaction flask. Then, 72 g of butadiene was added, the temperature was lowered to 6°C, and emulsification was performed for 15 minutes.

[0054] Finally, add an oxidant organic solution containing 5g styrene, 0.06g hydrogen peroxide p-menthane, and react at 6°C for 8.5 hours. When the conversion rate reaches 65%, add a terminator solution containing 0....

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Abstract

The invention provides a preparation method of emulsion-polymerized styrene butadiene rubber. The preparation method is characterized in that an irreversible addition-fragmentation chain transfer agent with the following general formula is adopted; an aqueous phase is prepared and then an oil phase is prepared; after the irreversible addition-fragmentation chain transfer agent is dissolved in styrene, butadiene is added into a reaction bottle, the temperature is reduced, and a emulsification reaction is conducted for 15 to 30 minutes; finally, an oxidant organic liquor is added into the reaction bottle; after a conversion rate reaches 60 percent to 70 percent, a terminator liquor is added into the reaction bottle and a polymerization termination reaction is conducted for 5 to 10 percents; after the polymerization termination reaction is fulfilled, a demulsification reaction is conducted with solvents of sulfuric acid and a methanol to form gel; and after the gel is milled and dried, the low temperature emulsion-polymerized styrene butadiene rubber is obtained. Compared with data of traditional emulsion-polymerized styrene butadiene rubber using tert-dodecyl mercaptan as a molecular weight regulator, the preparation method has the advantages that the comprehensive performance is not changed, odor produced by using alkyl hydrosulfide is avoided, the monomer conversion rate is increased by 5 to 8 percent, the product performance is steady, and the reproducibility is high.

Description

technical field [0001] The invention relates to a method for preparing emulsion polystyrene butadiene rubber using a molecular weight regulator based on an irreversible addition-breaking chain transfer mechanism. Background technique [0002] Emulsion polymerization technology is the only environment-friendly polymerization technology among polymerization methods. This polymerization technology has the following advantages: (1) the heat of polymerization is easy to diffuse, and the polymerization reaction temperature is easy to control; (2) the viscosity of the polymerization system is very low even in the late stage of the reaction, so it is also suitable for the preparation of high-viscosity polymers; (3) it can Obtain high molecular weight polymerization products; (4) can be used directly in the form of emulsion; (5) can simultaneously achieve high polymerization rate and high molecular weight. Therefore, emulsion polymerization technology has been widely used in importa...

Claims

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Application Information

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IPC IPC(8): C08F236/10C08F2/38C08F2/42C08F2/24
Inventor 石艳安粒惠嘉付志峰
Owner BEIJING UNIV OF CHEM TECH
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