14C-labeled polystyrene (PS) and synthesis method thereof
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A technology of polystyrene and styrene, applied in the field of synthesis of 14C-labeled polystyrene, which can solve the problem of low degree of polymerization
Active Publication Date: 2015-09-09
NANJING UNIV
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[0006] to solve 14 In the synthesis of C-labeled polystyrene, the reaction time is long, difficult to control, and the degree of polymerization is low, which reduces the 14 C mark polystyrene synthesis cost, the present invention provides micro-synthesis 14 C is a method for labeling polystyrene, which uses high temperature and high pressure to overcome the disadvantage of low polymerization degree under normal pressure; the starting marker raw materials are easily available in the market, the synthesis steps are simple, and the synthesis method is universal; the marking sites are respectively On the benzene ring or branch chain, the benzene ring labeling site has not been reported yet, and there is no corresponding product on the market
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Embodiment 1
[0050] Example 1: branched chain 14 C-labeled [β- 14 C]-polystyrene ([β- 14 Synthesis of C]-PS)(IV)
[0053] Set the specific activity to 2.1×10 9 Bq mmol -1 of 14 C-labeled malonate 14 CH 2 (COOH) 2 (1) and appropriate unmarked malonic acid are dissolved in pyridine, join in the 25mL pear-shaped bottle, obtain specific activity and be 4.2 * 10 7 Bq mmol -1 of 14 C-malonic acid. Add 0.1128 g of benzaldehyde and 177.5 μL of piperidine in sequence, 14 CH 2 (COOH) 2 (1) The molar ratio with benzaldehyde is 1:1.2~1.5, nitrogen protection, magnetic stirring, oil bath 105 ℃, react for 14 hours. After the reaction, cool to room temperature, add 20 mL of 1M hydrochloric acid for acidification, and make the pH of the solution acidic. Extracted 9 time...
Embodiment 2
[0059] Example 2: benzene ring 14 C marked [U-ring- 14 C6]-polystyrene ([U-ring- 14 Synthesis of C6]-PS)(VII)
[0060] combine figure 1 , 2, benzene ring 14 C marked [U-ring- 14 C6]-polystyrene ([U-ring- 14 C6]-PS)
[0061] The synthetic steps of (VII) are:
[0062] (1) Synthesis of benzene ring 14 C labeled styrene ([U-ring- 14 C6]-styrene) (VI)
[0063] Take the specific activity as 1.3×10 8 Bq mmol -1 benzene ring 14 C-labeled cinnamic acid [U-ring- 14 C6]-cinnamic acid (V) and an appropriate amount of non-labeled cinnamic acid were added to a 25mL pear-shaped bottle, dissolved in 1mL DMAc (dimethylacetamide), and the specific activity was obtained: 1.3×10 7 Bq mmol -1 The [U-ring- 14 C6]-cinnamic acid. Add silver acetate 0.0029g, anhydrous potassium carbonate 0.0036g, [U-ring- 14 C6]-cinnamic acid, silver acetate and potassium carbonate in a molar ratio of 1:0.2 to 0.5:0.3 to 0.8, nitrogen protection, magnetic stirring, oil bath at 160°C, and reaction for...
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Abstract
The invention discloses 14C-labeled polystyrene (PS) and its synthesis method and belongs to the field of radioactive isotope 14C-labeled compounds. According to the invention, 14C radioactive isotope label is introduced into the structure of polystyrene (PS). A 14C-labeled site is on a branched chain or a phenyl ring, and is respectively named [beta-14C]-PS and [U-ring-14C6]-PS. The general structural formula is as shown in the Figure 1, wherein * indicates the 14C-labeled site. The synthesis method comprises the following steps: adding the 14C-labeled styrene into non-labeled styrene for dilution, putting into a high-temperature and high-pressure reactor and reacting at 118-123 DEG C for 8-12 h; dissolving reaction products with chloroform, washing with methanol, depositing and purifying to obtain the 14C-labeled polystyrene. The synthesis method has the following advantages: reaction materials are easily available, unreacted raw materials can be recovered, and synthesis cost is low; reaction time is short and efficiency is high; and reaction conditions are mild, operation technique is safe, and the preparation technology is simple. Radioactive purity of the 14C-labelled polystyrene synthesized by the method reaches more than 99%.
Description
technical field [0001] The present invention relates to radioisotopes 14 The field of synthesis of C-labeled compounds, especially 14 Synthesis of C-labeled polystyrene. It can be used in the trace research of the degradation and transformation of polystyrene in the environment in the field of environmental science. Background technique [0002] Polystyrene (Polystyrene, PS) is a polymer formed by free radical addition polymerization of styrene monomer. It is widely used in communication equipment, optical instruments, transparent molds, food packaging materials and daily necessities. Discarded polystyrene plastic fragments may be accidentally eaten by organisms, causing obstruction of the digestive tract, resulting in reduced food intake, and may also be transferred to the internal circulatory system to cause harm to organisms, and may be passed along the food chain to higher trophic levels. Therefore, it is of great significance to study the environmental behavior of po...
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