Polyacrylonitrile resin with controllable molecular weight and distribution and high regularity, and preparation method thereof
A technology of polyacrylonitrile resin and polyacrylonitrile, applied in the field of polyacrylonitrile resin with controllable molecular weight and distribution, high regularity and its preparation, which can solve the problem of limited space for improving carbon fiber performance, uncertain copolymer sequence structure, The free radical copolymerization process is complicated, etc., to achieve good hydrophilicity and pre-oxidation cyclization reaction activity, which is beneficial to the control of molecular weight and its distribution, and the effect of less molecular structure defects
Active Publication Date: 2020-05-05
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology
However, the process of free radical copolymerization is complicated. Since the reactivity ratio of comonomers is greatly affected by temperature and solvent environment, the controllability of the reaction is poor, and the composition and sequence structure of the obtained copolymers are both uncertain and unstable, resulting in low quality of the original silk in the later stage. , which further limits the space for carbon fiber performance improvement
Method used
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Embodiment 1～16
[0019] Using a certain mass fraction of sodium thiocyanate (NaSCN) aqueous solution as the solvent, azobisisobutyronitrile (AIBN) as the initiator, S,S'-bis(α,α'-dimethyl-α″-acetic acid) Trithiocarbonate (TRIT) is a RAFT reagent. The material composed of acrylonitrile monomer, initiator, RAFT reagent and solvent is added to the reactor, nitrogen gas is passed through for oxygen removal treatment, and then RAFT is carried out at a certain reaction temperature. Polymerization, reaction time 6~24 hours.With the weight of whole polymerization system as a basis, the concentration of acrylonitrile monomer is shown in Table 1; Taking monomer weight as a basis, initiator dosage and RAFT dosage are shown in Table 1 Polymerization temperature, polymerization reaction The time is shown in Table 1. Finally, the residual monomer and air bubbles are removed to obtain polyacrylonitrile resin.
[0020] Table 1
[0021]
[0022]
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Abstract
The invention discloses polyacrylonitrile resin with controllable molecular weight and distribution and high regularity, and a preparation method thereof. The polyacrylonitrile resin with controllablemolecular weight and distribution and high regularity is prepared through a reversible addition / fragmentation chain transfer (RAFT) free radical polymerization process and a polymerization reaction by taking trithiocarbonate (TRIT) containing carboxyl groups at two ends as an RAFT reagent. The polyacrylonitrile resin has the advantages of high molecular weight, narrow molecular weight distribution, high molecular chain structure regularity and few molecular structure defects. The hydrophilicity of the polyacrylonitrile resin prepared by the method is obviously improved, the oxidative cyclization activity is improved, and the polyacrylonitrile resin is suitable for preparing protofilaments for high-performance carbon fibers.
Description
technical field [0001] The invention relates to a polyacrylonitrile resin with controllable molecular weight and distribution and high regularity and a preparation method thereof, in particular to the preparation of high molecular weight and narrow distribution polypropylene by reversible addition-fragmentation chain transfer radical polymerization (RAFT) technology The method of nitrile resin, and involves adopting the reagent that contains carboxyl functional group as RAFT reagent to prepare the polyacrylonitrile resin that end contains carboxyl group, thereby improves the structural regularity of polyacrylonitrile resin molecular chain, reduces molecular structure defect, obtains hydrophilicity The polyacrylonitrile resin is obviously improved and the oxidation cyclization activity is improved. The acrylonitrile resin with controllable molecular weight and distribution and high regularity is suitable for preparing high-performance carbon fiber precursors. Background techni...
Claims
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IPC IPC(8): C08F120/44C08F2/38C08F2/10
CPCC08F120/44C08F2/38C08F2/10C08F2438/03
Inventor 宋文迪黄翔宇吴嵩义袁玉红季春晓王平
Owner CHINA PETROLEUM & CHEM CORP
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