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A kind of green synthetic method of acrylonitrile polymer

A green synthesis, acrylonitrile technology, applied in the field of polymer synthesis, can solve the problems of difficult control of radiation polymerization, and achieve the effects of avoiding complex side reactions, controllable molecular weight, and saving energy consumption

Active Publication Date: 2018-11-27
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, so far, there are only a few successful cases, and they mainly use 2-phenyl-2-propylbenzodisulfide (CDB), 2-cyanopropyl-2-ylbenzodisulfide (CPDB) , S,S-dibenzyl trithiocarbonate (DBTC), etc. as chain transfer agents, but only by thermal initiation to prepare polyacrylonitrile polymers
in addition, 60 As an environmentally friendly energy resource, Co rays can be used to prepare grafted, crosslinked polymers or to modify polymers; but such 60 Irradiation polymerization of Co ray is difficult to control

Method used

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  • A kind of green synthetic method of acrylonitrile polymer
  • A kind of green synthetic method of acrylonitrile polymer
  • A kind of green synthetic method of acrylonitrile polymer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Embodiment 1: the synthesis of RAFT reagent

[0059] 1-bromonaphthalene (22.5 g, 0.11 mol) and tetrahydrofuran (90 mL) were slowly added to a 250 mL three-necked flask with magnesium strips (2.88 g, 0.12 mol) and a small amount of iodine for about 1 hour. React for 3 hours at 40~50°C. At room temperature, carbon disulfide (8.36 g, 0.11 mol) was added to the reaction system, and then the reaction was continued for 8 hours. The reaction solution was poured into water, acidified with 2 mol / L aqueous hydrochloric acid, and then extracted with dichloromethane (40 mL×3). The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. After the solvent was removed by rotary evaporation, the crude product was dissolved in 50 mL ethyl acetate, and reacted with 2.53 g DMSO and a small amount of iodine overnight. Under ventilation, AIBN (10.8 g, 0.066 mol) and 40 mL of benzene were added to the system, and reacted at 70 °C for 15 hours. After the sol...

Embodiment 2

[0060] Embodiment 2: A kind of green synthetic method of acrylonitrile polymer

[0061]

[0062] Add the RAFT reagent obtained in Example 1, acrylonitrile (AN), and solvent ethylene carbonate (EC, 2.64 g) into a 5 mL ampoule, deoxygenate with nitrogen bubbling, and 60 The polymerization reaction occurs under the irradiation of Co-γ rays, and the acrylonitrile polymer reacts at room temperature. Stop the reaction to obtain polyacrylonitrile polymer. Table 1 shows the results of radiation-induced free radical polymerization of acrylonitrile under different conditions.

[0063] Table 1 Radiation-induced free radical polymerization results of acrylonitrile under different conditions

[0064]

[0065] Polystyrene is used as a standard sample in the GPC test; the conversion rate is calculated by weighing method; the theoretical molecular weight calculation equation is:

[0066] .

[0067] Table 1 shows some radiation-induced free radical polymerization results of acrylon...

Embodiment 3

[0072] Embodiment 3: A kind of green synthetic method of acrylonitrile polymer

[0073] Add 15.26 mg of PAN (Table 1c), 0.41 g of acrylonitrile (AN), and 1.32 g of ethylene carbonate (EC) into a 5 mL amber bottle, deoxygenate with nitrogen bubbling, in 60 The polymerization reaction occurs under the irradiation of Co-γ rays, and the reaction time is 4 hours. Then the reaction solution was dissolved in DMF (2 mL), and then dissolved in 200 mL of methanol; suction filtered, and the obtained polymer was dried in a vacuum oven at 30°C for 24 hours to obtain 123.0 mg of acrylonitrile polymer.

[0074] Figure 8 It is the GPC efflux curve before and after the polymerization of acrylonitrile monomer initiated by polyacrylonitrile as RAFT reagent, Figure 9 It is the NMR spectra of polyacrylonitrile before and after the polymerization of acrylonitrile monomer initiated by RAFT reagent; as can be seen from the figure, the molecular weight of polyacrylonitrile has changed before and a...

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Abstract

The invention discloses a green synthesis method of an acrylonitrile polymer. Specifically, the reversible addition-fragmentation chain transfer polymerization method (RAFT technology) under the condition of 60Co ray irradiation, using the initiator CPDN as the RAFT agent, achieved the controllable synthesis of polyacrylonitrile polymer (PAN) at room temperature. synthesis. At the same time, by changing the irradiation dose rate, the ratio of monomer to chain transfer agent, monomer concentration, reaction time and other conditions, a series of polymerizations are carried out to provide a new green synthesis for the preparation of PAN-based carbon fiber materials. method.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and in particular relates to a green synthesis method of polyacrylonitrile (PAN). Background technique [0002] As the precursor of carbon fiber, polyacrylonitrile (PAN) has the advantages of rigidity, tensile strength, chemical tolerance, etc., and has always played a pivotal role in aerospace, machinery manufacturing, sports equipment and other industries. As we all know, polyacrylonitrile with high molecular weight, narrow molecular weight distribution, and high tacticity is the primary condition for synthesizing high-quality carbon fiber materials. However, the fully controllable polymerization of acrylonitrile is still challenging for the prior art, mainly because of the high reactivity of acrylonitrile and the poor solubility of polyacrylonitrile. [0003] In 1961, Shindo et al. first reported the successful preparation of carbon fiber materials with PAN as the matrix. Subsequen...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/44C08F2/38C08F2/46
CPCC08F2/38C08F2/46C08F120/44C08F2438/03
Inventor 张伟张双双朱秀林殷露张正彪周年琛
Owner SUZHOU UNIV
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