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Method for preparing rosin-based regular polymers

A polymer, rosin-based technology, applied in the field of preparation of rosin-based regular polymers, can solve the problem of no rosin-like substance polymerization and the like

Inactive Publication Date: 2012-05-02
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition to common monomers, protic monomers such as acrylic acid, sodium p-vinylbenzenesulfonate, hydroxyethyl methacrylate, and aminoethyl methacrylate, or acidic and basic monomers can be polymerized smoothly, but there is no For the polymerization of rosin substances

Method used

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  • Method for preparing rosin-based regular polymers
  • Method for preparing rosin-based regular polymers
  • Method for preparing rosin-based regular polymers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 10 g of DAME monomer, 66 mg of RAFT reagent (CDB, cumyl dithiobenzoate) and 4.0 mg of AIBN (azobisisobutyronitrile) in molar ratio ([DAE]:[CDB]:[ AIBN]=[100]:[1]:[0.1]) was added to 20 ml of toluene, the solution was transferred to an eggplant-shaped reaction flask, and nitrogen was bubbled to remove oxygen for 15 minutes. After reacting at 70 °C for 24 hours, the monomer conversion rate was 95%. Polymer Molecular Weight:M n (GPC): 25600 g / mol, PDI = 1.22. Mn (NMR): 37800 g / mol.

[0039]

Embodiment 2

[0041] Add 10 g of DAME monomer, 66 mg of RAFT reagent (CDB, cumyl dithiobenzoate) and 4.0 mg of AIBN (azobisisobutyronitrile) in a molar ratio ([DAME]:[CDB]:[ AIBN]=[100]:[1]:[0.1]) was added to 20 ml of toluene, the solution was transferred to an eggplant-shaped reaction flask, and nitrogen was bubbled to remove oxygen for 15 minutes. After reacting at 100 °C for 12 hours, the monomer conversion rate was 35%. Polymer Molecular Weight: M n (GPC): 10,600 g / mol, PDI = 1.29. M n (NMR): 12900 g / mol.

[0042] After 24 hours of reaction, the monomer conversion was 45%. Polymer Molecular Weight: M n (GPC): 15,300 g / mol, PDI = 1.67. M n (NMR): 17900 g / mol.

[0043] Can find out from the reaction, with toluene as solvent, react at 100 DEG C, reaction is in the time that conversion rate is lower than 35%, polymerization reaction process is controllable, when conversion rate continues to increase, PDI increases, and structure changes Uncontrollable.

[0044]

Embodiment 3

[0046] Add 10 g of DAME monomer, 66 mg of RAFT reagent (CDB, cumyl dithiobenzoate) and 4.0 mg of AIBN (azobisisobutyronitrile) in a molar ratio ([DAME]:[CDB]:[ AIBN]=[100]:[1]:[0.1]) into 20 ml tetrahydrofuran, transfer the solution into an eggplant-shaped reaction flask, and deoxygenate by bubbling nitrogen gas for 15 minutes. After reacting at 80 ° C for 12 hours, the polymer was precipitated in methanol, then filtered and dried to obtain rosin-based polymers with different molecular weights, and the monomer conversion rate was 42%. Polymer Molecular Weight: M n (GPC): 8600 g / mol, PDI = 1.46. M n (NMR): 17000 g / mol

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Abstract

The invention discloses a method for preparing rosin-based regular polymers. The method comprises the following steps of: dissolving a rosin-based monomer, an initiator for free radical polymerization, and a reversible addition-fragmentation chain transfer reagent in a certain molar mass ratio in a solvent, introducing nitrogen to remove oxygen, reacting at the temperature of between 50 and 120 DEG C for 1 to 24h, precipitating polymers in methanol, and filtering and drying to obtain rosin-based polymers with different molecular weights, wherein the rosin-based monomer is a rosin derivative which can be subjected to free radical polymerization reaction. By the method, the rosin-based regular polymers with different molecular weights and molecular weight distributions (PDI) can be obtained. The polymers are taken as prepolymers of a functional rosin block polymer.

Description

technical field [0001] The invention relates to a preparation method of a rosin-based regular polymer, in particular to the application of a new polymerization method in the synthesis of a rosin-based polymer. Background technique [0002] Rosin is an important renewable material and one of the main forestry products in my country. The annual output of rosin in the world is about 1.2 million tons, and the annual output of rosin in my country is about 800,000 tons. Rosin is mainly composed of resin acid and some neutral substances, and carboxyl group and conjugated double bond are the main functional groups in resin acid. Disproportionated rosin, hydrogenated rosin, maleic rosin, acrylic rosin and various rosin esters have been synthesized through chemical modification of carboxyl and conjugated double bonds, including some free radical polymerizable monomers (CN101215445, CN101492591, CN101265392, CN101066918). As follows: [0003] [0004] DAE DAME DAB DAA D...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F122/14C08F2/38C08F118/12C08F293/00
Inventor 储富祥王基夫唐传兵王春鹏
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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