Dicyclopentadienyl alkaline earth metal thiolate and its preparation method and application
A technology of dicyclopentadienyl mercaptan and dicyclopentadienyl, applied in the field of preparing thermally reversible covalently cross-linked polyvinyl chloride, which can solve problems such as the degree of difficult cross-linking
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Embodiment 1
[0080] Add 178 grams of deoxygenated 1,2-dibromoethane into an oxygen-free and water-free reactor, and add it dropwise at a rate of 0.05-0.1 ml / s under the protection of high-purity nitrogen (purity ≥ 99.999%) and stirring Concentration is 370 grams of the tetrahydrofuran solution of cyclopentadiene sodium of 15wt%; Carry out the reaction of replacing the bromine atom in 1,2 dibromoethane at a temperature of 20 ℃ for 8 hours, add 200ml to the reactor after completion of the reaction Wash the obtained product with ionic water to separate the oil phase; after washing and separating several times in this way, send the oil phase to a rotary evaporator for evaporation under reduced pressure, so that all the remaining 1,2 dibromoethane is evaporated, and at the same time Cyclopentadienyl bromide dimerization obtains 101 grams of dicyclopentadienyl bromide, and the conversion rate of cyclopentadienyl sodium is calculated to be about 92%; the infrared spectrum of this dicyclopentadieny...
Embodiment 2
[0086] At room temperature, in the absence of oxygen and under the protection of high-purity nitrogen (purity ≥ 99.999%), add all the aqueous solutions containing sodium dicyclopentadienyl ethanethiolate obtained in Example 1 to the reactor, and adjust the aqueous solution with dilute hydrochloric acid The pH is 8.2, then dropwise (speed 0.05 ~ 0.1 ml / sec) by 50 grams of barium chloride (BaCl 2 2H 2 O) Prepared saturated aqueous solution, raise the temperature from room temperature to 80°C, carry out sufficient metathesis reaction under continuous stirring for 6 hours, then cool to room temperature naturally, discard the upper aqueous phase after centrifugation to obtain precipitation; use deionized water for precipitation Wash and centrifuge 3 times each, then wash 1 time with tetrahydrofuran; vacuum-dry to obtain a white slightly yellow powder-67 grams of barium dicyclopentadienyl ethanethiolate; its infrared spectrum is shown in Figure 4 , the figure shows the character...
Embodiment 3
[0089] Plasticizer, the dicyclopentadienyl ethyl mercaptide barium obtained in Example 2, calcium-zinc composite stabilizer or dibutyltin dilaurate stabilizer are added in the mixer, at room temperature and under stirring at 100 rev / min After adding 100 parts by mass of PVC resin with a polymerization degree of 1000, mix at a high speed of 800 rpm at a temperature of 50-80°C to obtain a PVC dry mix; cool the obtained PVC dry mix and then feed it into Plasticizing at 150°C for 5 minutes on a two-roll mill; then laminating the obtained flakes under a single-layer electric tablet press at 180°C for 10 minutes to make a thermally reversible covalently cross-linked polyvinyl chloride sample, and then Cut into standard splines, test its performance in the manner listed in the present invention, the results are shown in Table 1. As a comparison, this embodiment also provides a polyvinyl chloride sample that does not contain barium dicyclopentadienyl ethanethiolate crosslinking agent....
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Abstract
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