腰果酚甜菜堿型兩性離子表面活性劑的合成與性能研究
發(fā)布時(shí)間:2018-04-16 20:03
本文選題:腰果酚 + 氯醇醚; 參考:《東北石油大學(xué)》2015年碩士論文
【摘要】:本文以腰果酚、環(huán)氧氯丙烷為原料,四丁基溴化銨為催化劑合成中間體腰果酚氯醇醚,繼而與二甲胺經(jīng)胺化合成腰果酚叔胺,產(chǎn)物再與3-氯-2-羥基丙磺酸鈉進(jìn)行最終反應(yīng),獲得產(chǎn)品--腰果酚甜菜堿,對合成的產(chǎn)品進(jìn)行了紅外表征并對表/界面張力、乳化性、熱穩(wěn)定性、與聚合物的復(fù)配性等進(jìn)行了一系列的展開研究。本實(shí)驗(yàn)是在實(shí)驗(yàn)室前人基礎(chǔ)上對合成該表面活性劑的工藝進(jìn)行了改進(jìn),將縮水甘油醚中間體法改為氯醇醚中間體法,該方法具有反應(yīng)條件低、操作簡單、催化劑使用量少、中間產(chǎn)物處理方便、叔胺轉(zhuǎn)化率高等優(yōu)點(diǎn)。最終產(chǎn)品及中間體的紅外譜圖顯示,合成的物質(zhì)均具有目標(biāo)產(chǎn)物的特征吸收峰可初步判斷為目標(biāo)產(chǎn)品。對中間產(chǎn)物腰果酚叔胺設(shè)計(jì)4因素3水平的正交試驗(yàn),以確定最佳反應(yīng)條件,實(shí)驗(yàn)結(jié)果為:n(腰果酚氯醇醚):n(二甲胺):n(氫氧化鈉)=1:2.5:1.4;反應(yīng)時(shí)間為6h;反應(yīng)溫度為40℃。在此條件下進(jìn)行3次平行試驗(yàn),腰果酚叔胺產(chǎn)率較為理想,達(dá)到90%。通過旋滴法測試表面活性劑降低油-水界面張力的性能,實(shí)驗(yàn)表明實(shí)驗(yàn)室自制的腰果酚甜菜堿可以高效地降低油水界面張力,當(dāng)濃度為0.5~3.0g/L時(shí)仍能保持良好的性能,界面張力均可達(dá)到10-4~10-3mN/m,而且在高溫(55~95℃)、高鹽(32308~64616mg/L)條件下均能滿足驅(qū)油過程中達(dá)到超低界面張力(10-3mN/m)的要求。采用滴體積法測定該表面活性劑的表面張力,實(shí)驗(yàn)表明低濃度表面活性劑溶液即可達(dá)到臨界膠束濃度,其中cmc=3.17×10-4mol/L,此時(shí)表面張力γcmc=32.86mN/m。通過分水時(shí)間法來反映表面活性劑的乳化性能,實(shí)驗(yàn)表明單一的該表面活性劑乳化性能較差,在0.5~3.0g/L濃度范圍內(nèi),分水時(shí)間短,約為35s左右,該性能仍亟待提高。通過測試表面活性劑在42天模擬地層溫度(85℃)的條件下界面張力的變化來反映該表面活性劑熱穩(wěn)定,實(shí)驗(yàn)表明,該表面活性劑的表面活性會(huì)隨著時(shí)間的推移有所降低,導(dǎo)致油-水界面張力的增長,但仍能保持10-3mN/m,可以滿足采油需要。與聚丙烯酰胺的復(fù)配使用使其性能更為優(yōu)越:加入一定量(0.5~1.5g/L)的聚合物可使界面張力達(dá)到10-6~10-4mN/m;cmc有所降低,對γcmc無太大影響:聚合物濃度為0.5g/L時(shí)cmc=2.75×10-4mol/L,γcmc=34.96mN/m;聚合物濃度為1.5g/L時(shí)cmc=1.38×10-4mol/L,γcmc=35.72m N/m;聚合物濃度為1.0~1.5g/L時(shí),分水時(shí)間大幅度提高(約為200~1200s),乳化性能得到改善;聚合物的加入使體系熱穩(wěn)定性更佳,基本呈穩(wěn)定狀態(tài),且在一定程度上降低界面張力至10-5~10-4mN/m。
[Abstract]:In this paper, cashew fruit phenol and epichlorohydrin were used as raw materials, and tetra ammonium bromide was used as catalyst to synthesize the intermediate cashew fruit phenol chlorol ether, which was then aminated with dimethylamine to synthesize cashew phenol tertiary amine, and the final reaction was carried out with sodium 3-chloro-2-hydroxypropyl sulfonate.The synthesized product was characterized by IR and a series of studies were carried out on the surface / interfacial tension, emulsification, thermal stability and the compatibility with polymer.In this experiment, the synthetic process of the surfactant was improved on the basis of laboratory predecessors. The method was changed from the intermediate of glycidyl ether to the intermediate of chloroalcohol ether. The method has the advantages of low reaction conditions, simple operation and less catalyst usage.The intermediate product is easy to deal with and the conversion rate of tertiary amine is high.The infrared spectra of the final product and the intermediate show that the synthesized substance has the characteristic absorption peak of the target product and can be preliminarily judged as the target product.The orthogonal design of 4 factors and 3 levels of the intermediate product cashew fruit phenol tertiary amine was carried out to determine the optimum reaction conditions. The experimental results showed that the reaction temperature was 40 鈩,
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