本文選題：不溶性硫黃 + 熔融法��； 參考：《華東理工大學(xué)》2015年碩士論文

【摘要】：不溶性硫黃(簡稱IS)是性能優(yōu)良、應(yīng)用廣泛的橡膠硫化劑。本論文對(duì)熔融法制取不溶性硫黃新技術(shù)進(jìn)行了研究。 首先考察了硫黃原料對(duì)熔融法反應(yīng)合成IS的影響,結(jié)果表明：以普光氣田硫黃反應(yīng)合成的IS轉(zhuǎn)化率為37.9%,120℃熱穩(wěn)定性相對(duì)較高,達(dá)13.2%。 其次,對(duì)反應(yīng)產(chǎn)物IS萃取提濃技術(shù)進(jìn)行考察。采用動(dòng)態(tài)平衡法測(cè)定硫黃在氯苯中的溶解度,結(jié)果表明：隨著溫度的升高,氯苯對(duì)硫黃的溶解能力明顯提升,在80。C時(shí)氯苯對(duì)硫黃的溶解能力為17.8g/100g,超過文獻(xiàn)[61]報(bào)道的萃取劑1,1,1-三氯乙烷/四氯乙烯混合液對(duì)硫黃的溶解能力。 在上述基礎(chǔ)上,對(duì)氯苯一級(jí)平衡萃取提高IS含量的工藝進(jìn)行優(yōu)化,結(jié)果表明：在萃取溫度為80。C,溶劑比為10：1,萃取時(shí)間為30min的條件下,新鮮氯苯對(duì)Is的萃取率為98.10%,高于萃取劑1,1,1-三氯乙烷/四氯乙烯混合液的萃取率85.08%。經(jīng)六次循環(huán)回收利用的氯苯對(duì)IS的萃取率為93.40%,略低于新鮮氯苯。氯苯的萃取效果接近二硫化碳(C82),且安全、低毒、環(huán)保。 最后,對(duì)填充油的基屬、充油穩(wěn)定劑和充油方式進(jìn)行考察優(yōu)選,結(jié)果表明：以環(huán)烷基油作為填充油,以0.5%的六氯丁二烯作為穩(wěn)定劑,以石油醚分散填充油對(duì)含量達(dá)97.2%、120。C熱穩(wěn)定性為38.1%的IS進(jìn)行充油,充油IS的120℃熱穩(wěn)定性為43%,較充油前提高了4.9%,接近Crystex-OT20產(chǎn)品。
[Abstract]:Insoluble sulfur (IS) is a rubber vulcanizing agent with excellent properties and wide application.
The effect of sulfur raw materials on the synthesis of IS by melting reaction was investigated. The results showed that the conversion rate of IS was 37.9%, and the thermal stability was relatively high at 120 C, reaching 13.2%..
Secondly, the extraction concentration technology of the reaction product IS extraction was investigated. The solubility of sulfur in chlorobenzene was determined by dynamic equilibrium method. The results showed that the solubility of chlorobenzene to sulfur was obviously improved with the increase of temperature, and the solubility of chlorobenzene to sulfur was 17.8g/100g at 80.C, which was more than that of 1,1,1- three chloroethane, an extractant reported in [61]. / dissolving capacity of four chloroethylene mixture on sulphur.
On the basis of the above basis, the process of improving the content of IS by the first class equilibrium extraction of chlorobenzene was optimized. The results showed that the extraction rate of fresh chlorobenzene to Is was 98.10% under the conditions of 80.C, 10:1 and 30min, which was higher than that of the extractant 1,1,1- three chloroethane / four chloroethylene mixture. The extraction rate of 85.08%. was followed by six times. The extraction rate of chlorobenzene recycled by ring is 93.40%, slightly lower than that of fresh chlorobenzene. The extraction effect of chlorobenzene is close to carbon disulfide (C82), and is safe, low toxic and environmental friendly. IS
Finally, the base genera, oil filling stabilizers and oil filling methods were investigated and optimized. The results showed that the naphthenic oil was used as filling oil and 0.5% hexahchlorbutadiene was used as stabilizer. The oil filled oil was 97.2% and the thermal stability of 120.C was 38.1%. The thermal stability of the oil filled IS was 43%, and the oil filled oil was 43%, and the oil filled oil was 43%. The previous increase was 4.9%, close to the Crystex-OT20 product.

【學(xué)位授予單位】：華東理工大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2015
【分類號(hào)】：TQ125.116

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