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Preparation method of butyl acrylate-styrene-acrylonitrile graft copolymer

A technology of butyl acrylate and graft copolymer, applied in the field of polymers, can solve problems such as imperfect control of core/shell structure technology

Inactive Publication Date: 2010-10-20
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] In China, the research on poly(butyl acrylate-styrene-acrylonitrile ASA) graft polymers began in the 1990s, and the research institutes of Lanhua Company, Zhejiang University, Fudan University, Jilin University, etc. The basic research work in synthesis and performance research is all based on emulsion polymerization. Due to the imperfect technology in controlling the core / shell structure, the domestic graft polymerization of poly(butyl acrylate-styrene-acrylonitrile ASA) There is a certain gap with foreign countries in biological research

Method used

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  • Preparation method of butyl acrylate-styrene-acrylonitrile graft copolymer

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preparation example Construction

[0052] (1) The preparation of the rubber phase latex is a multi-step seed emulsion polymerization method.

[0053] Preparation of rubber phase seed latex: at room temperature, add a certain amount of deionized water and emulsifier to react

[0054] In the kettle, start stirring, fix the stirring speed at 300r / m, and stir for 30min; then add the rubber phase monomer, pass nitrogen protection for 30min, and remove the oxygen in the reaction system; time. Sampling to measure conversion rate.

[0055] At normal temperature, in a reaction kettle with a stirring device, the stirring speed is fixed at 300r / m, and a certain amount of deionized water, emulsifier and seed emulsion are added in sequence. Control the temperature of the reaction system, add the rubber phase monomer, crosslinking agent, grafting agent, and initiation system under the condition of nitrogen protection, and react for a certain period of time. Sampling to measure conversion rate.

[0056] (2) Preparation of...

Embodiment 1

[0085] 1. Pre-emulsification

[0086] Accurately weigh 1g of sodium dodecyl sulfate (SDS), dissolve it in 70ml of water and put it into a 250ml three-neck flask, add 79g of butyl acrylate (BA) and 1g of methacrylic acid (MAA) in sequence, and stir rapidly (1000r / min) for 8h spare.

[0087] 2. Polymerization reaction

[0088] (1) Synthetic Seed

[0089] Weigh 0.25g of SDS and add 68ml of water to fully dissolve it, then add it to a 500ml four-neck flask, pass condensed water, adjust the pH value of the sodium hydroxide solution to 9-10, raise the temperature to 75°C, add 5% pre-emulsion, and then slowly add persulfuric acid Potassium (KPS) 0.25g / 25ml (water) solution, stirred for ten minutes. Raise the temperature to 80°C and react for 60 minutes.

[0090] (2) Another 0.25g / 25ml (water) solution of KPS and the remaining 95% pre-emulsion were added dropwise to the system at the same time using a dropping funnel, and the dropwise addition was completed within 2 hours. Contin...

Embodiment 2

[0096] 1. Pre-emulsification

[0097] Accurately weigh 0.8g of fatty alcohol polyoxyalkylene ether sodium sulfate (AES), dissolve it in 70ml of water and add it to a 250ml three-neck flask, add 79g of butyl acrylate (BA), 1g of methacrylic acid (MAA), isopropyl hydrogen peroxide Benzene 0.212g. Stir rapidly (1000r / min) for 8h for later use.

[0098] Prepare the initiator solution: Dissolve 0.121g of disodium salt of ethylenediaminetetraacetic acid (EDTA), 0.086g of sodium formaldehyde sulfoxylate (SFS), and 0.008g of ferrous sulfate (FES) in 75ml of water, and set aside.

[0099] 2. Polymerization reaction

[0100] (1) Seed Synthesis

[0101] Weigh 0.2g of AES and add 68ml of water to fully dissolve it, then add it to a 500ml four-neck flask, pass condensed water and nitrogen. Heat up to 50°C, add 5% pre-emulsion, and add 10ml of initiator solution. Reaction 60min.

[0102] (2) nuclear layer synthesis

[0103] Control the reaction temperature to 50°C and blow nitrogen. ...

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Abstract

The invention relates to a preparation method of a butyl acrylate-styrene-acrylonitrile graft copolymer. In the method, a nucleus layer, a cross-linking agent, a shell layer, a emulsifier and an initiator are involved, wherein the nucleus layer is cross-linked acrylic ester, the cross-linking agent is a monomer with a cross-linking function, the shell layer is a monomer with a plastic function, and the formation of a nucleus / shell structure can be controlled by firstly adding a nucleus monomer and then adding a shell monomer. The cross-linking agent is methacrylic acid. A proper amount of methacrylic acid is added to the nucleus layer, a long-chain molecular structure can be formed through carboxyl dehydration, or polyacrylate rubber with a cross-linking structure can be formed; and by utilizing the methacrylic acid unreacted in the nucleus layer and the added methacrylic acid, the carboxyl is dehydrated to form nucleus / shell chemical binding.

Description

technical field [0001] The invention relates to the technical field of polymers, in particular to a preparation method of butyl acrylate-styrene-acrylonitrile graft copolymer. Background technique [0002] Core-shell structure poly(butyl acrylate-styrene-acrylonitrile, abbreviated as ASA) graft copolymer, which has the same structure as poly(butadiene-styrene-acrylonitrile, abbreviated as ABS) graft copolymer . In terms of composition, polyacrylate rubber with saturated structure is used to replace polybutadiene rubber with unsaturated structure, and the rest of the components are the same. Since the rubber phase of the poly(butyl acrylate-styrene-acrylonitrile) graft copolymer is a saturated structure and does not contain residual double bonds, the hydrogen dissociation energy of the rubber phase is as high as 380KJ / mol, and it can only be used in high-energy light with a wavelength below 300nm. Lower dissociation (absent in sun rays). Therefore, it has excellent weather...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F265/04C08F2/24
Inventor 林润雄李荣勋李超芹丁乃秀
Owner QINGDAO UNIV OF SCI & TECH