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Novel method for preparing itaconic anhydride-styrene monomer alternating copolymer

A technology of alternating copolymers and styrenes, which is applied in the field of self-stabilizing precipitation polymerization to prepare alternating copolymers of itaconic anhydride and styrene monomers, achieving the effects of narrow particle size distribution, low toxicity and high conversion rate

Active Publication Date: 2013-01-02
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0015] However, using alkyl esters of organic acids as the reaction medium, selecting conventional thermal decomposition initiators, and preparing alternating copolymers of itaconic anhydride and styrene monomers through self-stabilizing precipitation polymerization, there have been few reports so far.

Method used

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  • Novel method for preparing itaconic anhydride-styrene monomer alternating copolymer
  • Novel method for preparing itaconic anhydride-styrene monomer alternating copolymer
  • Novel method for preparing itaconic anhydride-styrene monomer alternating copolymer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] The monomer molar ratio is 1:1, the total concentration is 1mol / L, styrene (St) 2.4ml, itaconic anhydride (ITA) 2.24g, initiator azobisisobutyronitrile (AIBN) 0.0432g, acetic acid isoamyl Put 40ml of ester into a 100ml three-necked flask to fully dissolve, and keep the reaction temperature at 70°C under the protection of nitrogen and a condensation device, and react for 6h. After the reaction, the polymer was separated from the emulsion by centrifugation (3500rpm, 30min), dried in a vacuum oven at 50°C, and washed three times with isoamyl acetate to remove oligomers adsorbed on the surface of the microspheres. A pure alternating copolymer is obtained.

[0057] Gained polymer microsphere particle diameter is 570nm, and particle diameter distribution coefficient is 4.53%, and productive rate is 79.35%, and the number-average molecular weight of polymkeric substance recorded with GPC is 10200g / mol, and its scanning electron micrograph is as follows figure 1 shown.

Embodiment 2

[0059] The molar ratio of monomers is 1:1, the total concentration is 1mol / L, St 2.4ml, ITA 2.24g, initiator dibenzoyl peroxide (BPO) 0.0638g, isoamyl acetate 40ml, add to a 100ml three-necked flask Fully dissolve, under the protection of nitrogen and condensing device, keep the reaction temperature at 70°C, and react for 8 hours. After the reaction, the polymer was separated from the emulsion by centrifugation (3500rpm, 30min), dried in a vacuum oven at 50°C, and washed three times with isoamyl acetate to remove oligomers adsorbed on the surface of the microspheres. A pure alternating copolymer is obtained.

[0060] Gained polymer microsphere particle diameter is 590nm, and particle size distribution coefficient is 5.99%, and productive rate is 81.15%, and the number-average molecular weight of polymkeric substance recorded with GPC is 9500g / mol, and its scanning electron micrograph is as follows figure 2 shown.

Embodiment 3

[0062] Monomer molar ratio 1:1, total concentration 1mol / L, A: St 2.4ml, ITA 2.24g, AIBN 0.0432g, n-pentyl acetate 40ml, B: St 2.4ml, ITA 2.24g, AIBN 0.0432g, acetic acid Butyl ester 40ml, C:St 2.4ml, ITA 2.24g, AIBN 0.0432g, ethyl butyrate 40ml. The reactants were added to three 100ml three-neck flasks according to the formulas A, B, and C, and fully dissolved. Under the protection of nitrogen and a condensation device, the reaction temperature was kept at 70°C for 6 hours. After the reaction, the polymer was separated from the emulsion by centrifugation (3500rpm, 30min), dried in a vacuum oven at 50°C, and washed three times with the corresponding reaction medium to remove the oligomers adsorbed on the surface of the microspheres. A pure alternating copolymer is obtained.

[0063] The particle size of the polymer microsphere obtained by formula A is 595nm, the particle size distribution coefficient is 6.46%, and the yield is 76.33%, and the particle size of the polymer micr...

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Abstract

The invention discloses a novel method for preparing an itaconic anhydride-styrene monomer alternating copolymer, which belongs to the field of polymer. The method comprises the following steps of: once adding itaconic anhydride, styrene monomers, an initiator and a reaction medium into a reaction vessel for complete dissolution and shaking up, performing reaction at 60 to 70 DEG C for 6 to 8 hours under the protection of nitrogen, separating a product out of emulsion in a centrifugation way, and oven-drying the product in a vacuum drying oven of 50 DEG C to obtain the white powder of the itaconic anhydride-styrene monomer alternating copolymer, wherein the reaction medium may be an organic acid alkyl ester, or the mixed solution of the organic acid alkyl ester and acetone or cyclohexane;and the initiator is a conventional thermally-decomposed initiator. In the method of the invention, stirring and the addition of any stabilizing agent are avoided, and the reaction medium has low toxicity; microspheres with cleaning surfaces and the particle sizes of 350 to 1,000nm can be directly obtained; the copolymer has high thermal properties; and the microspheres with the particle sizes ofmore than 800nm can be synthesized by adding a crosslinker, and the gel content can reach 75 percent.

Description

technical field [0001] The invention relates to a method for preparing an alternating copolymer of itaconic anhydride and styrene monomers through self-stabilizing precipitation polymerization, which belongs to the field of polymer materials. Background technique [0002] Itaconic anhydride is an important monomer for synthetic polymer materials, widely used in the production of synthetic resins, synthetic fibers, ion exchange resins, surfactants, boiler descaling agents, lubricating additives, adhesives and non-toxic packaging materials. Itaconic anhydride is produced by fermenting carbohydrates under the liquid surface, or itaconic acid is obtained by heating and decomposing citric acid aqueous solution under pressure, and then reacts with thionyl chloride to form itaconic anhydride. [0003] After the oil crisis, modern people are increasingly concerned about energy issues, and green, non-toxic and renewable raw materials have aroused widespread interest. At present, mal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F222/04C08F212/08C08F212/14C08F2/06
Inventor 杨万泰杨坤
Owner BEIJING UNIV OF CHEM TECH