【摘要】：發(fā)泡劑ADC(分子式H2NCONNCONH2)是一種通用的高效發(fā)泡劑，具有發(fā)氣量大、氣泡均勻、致密，分解產(chǎn)物無毒、無臭、不助燃，無污染性殘渣等優(yōu)點(diǎn)，可廣泛用作聚氯乙烯、聚乙烯、聚丙烯、聚酰胺、氯丁膠、乙腈膠、丁基膠、丁苯膠和硅橡膠等的發(fā)泡劑，且閉孔發(fā)泡、常壓發(fā)泡和加壓發(fā)泡均可適用。國內(nèi)發(fā)泡劑ADC的生產(chǎn)工藝大多采用氯氣氧化法和氯酸鈉氧化法，但均不同程度地存在能耗高、物耗大、伴有大量污染物等缺陷。過氧化氫氧化法新工藝在氧化過程除生成發(fā)泡劑ADC外，其余產(chǎn)物為水，且過氧化氫易計量，不會有氧化不足或過量問題，生產(chǎn)過程中產(chǎn)品質(zhì)量和收率穩(wěn)定，具有無污染、無副產(chǎn)品、產(chǎn)品質(zhì)量好、產(chǎn)量高、發(fā)氣量大、無爆炸危險等優(yōu)點(diǎn)。 本文在對過氧化氫氧化聯(lián)二脲制備發(fā)泡劑ADC工藝過程進(jìn)行理論分析和小試研究的基礎(chǔ)上，在國內(nèi)首先進(jìn)行中試，并實(shí)現(xiàn)工業(yè)化。小試研究得出較佳的工藝條件為：采用新型的鐵基化合物為助催化劑，反應(yīng)液固液比為1：2.5，原料摩爾配比(聯(lián)二脲：雙氧水)為1：1.05，催化劑濃度為1.75g/l，助催化劑濃度為3.0g/l，酸濃度為3.5mol/l，反應(yīng)溫度為50℃，此時反應(yīng)收率97.44%，產(chǎn)品純度98.88%。通過理論分析給出相應(yīng)的反應(yīng)機(jī)理。同時分析表明，聯(lián)二脲氧化制備發(fā)泡劑ADC的過程中，，固液傳質(zhì)為速率控制步驟。從中試過程來看，母液回流對反應(yīng)收率和產(chǎn)品純度的影響不大，母液可以一直循環(huán)使用。中試還研究確定了工藝條件的浮動范圍為：催化劑濃度為1.65g/l~1.85g/l，助催化劑濃度為2.8g/l~3.2g/l，酸濃度為3.3mol/l~3.7mol/l，反應(yīng)溫度為48℃~52℃，此時反應(yīng)收率在95.14%以上，產(chǎn)品純度在97.25%以上。工業(yè)化研究中采用的工藝條件控制在中試所得的浮動范圍內(nèi)，經(jīng)過母液數(shù)次循環(huán)后，反應(yīng)時間為6h，反應(yīng)的收率高于92.51%，產(chǎn)品純度大于96.23%，發(fā)氣量大于211ml/g，細(xì)度篩余物(篩孔38μm)小于0.15%，分解溫度大于203℃，加熱減量小于0.21%，灰分小于0.03%，完全符合產(chǎn)品的一級品要求。 工業(yè)化實(shí)踐表明，該新方法經(jīng)濟(jì)性良好，能耗低，水資源消耗低，更加環(huán)保，生產(chǎn)利潤有較大的提升，與國內(nèi)的氯氣氧化法和氯酸鹽氧化法工藝相比處于先進(jìn)水平，具有很大的推廣和應(yīng)用意義。
[Abstract]:Foaming agent ADC (molecular formula H2NCONNCONH2) is a kind of general high efficient foaming agent. It has the advantages of large amount of gas, uniform bubble, dense, non-toxic, odorless, non-combustible, non-polluting residue and so on. It can be widely used in PVC, polyethylene, etc. Polypropylene, polyamide, chloroprene, acetonitrile, Ding Ji gum, butadiene rubber and silicone rubber foaming agent, and closed cell foaming, atmospheric pressure foaming and pressure foaming are applicable. The production process of foaming agent ADC in China mostly adopts chlorine gas oxidation method and sodium chlorate oxidation method, but there are many defects such as high energy consumption, high material consumption and large amount of pollutants. In addition to forming foaming agent ADC, the other products of the new oxidation process of hydrogen peroxide are water, and the hydrogen peroxide is easy to be measured, and there will be no problem of insufficient oxidation or excessive oxidation. The product quality and yield are stable and pollution-free during the process of production. No by-products, good product quality, high output, large amount of gas, no explosion risk and other advantages. On the basis of theoretical analysis and small scale study on the preparation of foaming agent ADC by oxidation of biuret with hydrogen peroxide, the pilot test was carried out in China, and industrialization was realized. The experimental results showed that the optimum technological conditions were as follows: the new iron-based compound was used as cocatalyst, the ratio of reaction liquid to liquid was 1: 2.5, and the molar ratio of raw material (biuret: hydrogen peroxide) was 1: 1.05. The concentration of catalyst is 1.75 g / l, the concentration of cocatalyst is 3.0 g / l, the concentration of acid is 3.5 mol / l, the reaction temperature is 50 鈩

本文編號：2345598