TWI626211B - 提取劑及其製備方法 - Google Patents

提取劑及其製備方法 Download PDF

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TWI626211B
TWI626211B TW101108954A TW101108954A TWI626211B TW I626211 B TWI626211 B TW I626211B TW 101108954 A TW101108954 A TW 101108954A TW 101108954 A TW101108954 A TW 101108954A TW I626211 B TWI626211 B TW I626211B
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potassium
manganese
oil
extracting agent
water
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凌永健
劉人銪
張馨云
黃怡慈
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國立清華大學
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Abstract

本發明係關於一種製備提取劑的方法，該方法包括下列步驟：將鉀、錳、硫以及氧以可溶於水的形式溶於水中，以得到一水溶液；以及利用加熱該水溶液以得到該提取劑。

Description

提取劑及其製備方法
本發明係關於一種提取劑及其製備方法，尤指一種油提取劑及其製備方法。
石油是一種不可再生且無法循環使用的能源，具備光合作用碳循環利用以及高土地利用效率的藻類來取代有限的原油是未來驅勢，微藻製油具有1.產油率高、2.對環境有益、以及3.不佔用耕地等優勢，且有些微藻還能在鹽鹼環境下生長，所以一些鹽鹼化土地也能用作培養微藻的場所，充分利用原本無法利用之鹽鹼化土地。世界各國如美、中皆在微藻製油中投入大量經費與研究。一般採取藻油主要是殺掉藻類再通過加入化學物質來提取藻油，但這樣的成本過高。目前創新的方向包含利用一百奈米尺寸圓形矽球以及利用基因工程使藻類自動分泌油脂到細胞外收集等，但一百奈米圓形矽球沒有展現出選擇性吸附油卻不吸附水的能力，而分泌油脂到細胞外仍尚未成功商業化。
奈米材料是近年來最受關注的新興材料，由於構成物質的基本尺寸在達到奈米尺度以後，其性能將產生一系列變化即奈米效應(如小尺寸效應、體積效應、表面效應、量子尺寸效應、宏觀量子隧道效應等)，因此奈米材料表現出許多不同於常規材料的新奇特性，具有廣闊的應用前景。國內外學者已經開始將奈米材料應用於石油工業領域的研究，如深部調剖、稠油降黏、低油滲透等，在提高萃油效率方面，也已經出現了奈米膜驅油劑、奈米乳液驅油劑等，但是現有的奈米膜驅油劑、奈米乳液驅油劑等的驅油效果是鎖定巨觀油脂體系，無法縮小到可滲透到藻類體內萃取藻油，預期效果不理想。除了這些方向外，仍需要更低能耗、更簡易、更綠色的製備方法來提高對藻油的採收率，並且減少在提取過程中對藻類的傷害。因此一種價格低廉、環境友好、可提取藻油、選擇性吸附油脂能力好的新型奈米藻油提取劑有待開發。
本案之主要目的在於提供製備一油提取劑的方法，包括下列步驟：(a)將重量百分比0.1%～30%的硫酸鉀、0.1%～30%的過硫酸鉀以及0.1%～30%的硫酸錳溶於水中；(b)利用微波加熱合成一化合物；(c)冷卻該化合物至室溫；以及(d)將該化合物低溫烘烤除水。
本案之另一目的在於提供一種製備一提取劑的方法，包括下列步驟：將鉀、錳、硫以及氧以可溶於水的形式溶於水中，以得到一水溶液；以及利用加熱該水溶液以得到該提取劑。
本發明之又一目的在於提供一種提取劑，其係具有一鉀錳硫氧之複鹽。
本發明所提供之奈米藻油提取劑，其價格低廉、安全環保、吸附油選擇性高。具體技術方案是：所述合成後之提取劑為一奈米線，奈米線的材料優選為鉀錳硫氧之複鹽。奈米線材料的加入能夠降低油水介面張力，同時作為吸附劑提高油脂在水溶液內的分離，另外由於奈米線材料尺寸小，可與藻類體內的藻油產生吸附作用，接著再利用油類與水密度差來回收藻油以提高驅油效率。
所述奈米線材料以鉀、錳、硫、氧為主要原料，合成出具有極強的憎水親油性能以及相對於水的對三酸甘油脂的高選擇性吸附，因此能夠降低油水介面張力，使藻油很容易地被萃取出來。
所述奈米線材料在越高極性溶劑環境中會呈現聚集現象，而在越低極性溶劑中會呈現低於一微米的尺寸大小分佈。低於一微米的奈米線材料能夠降低油水介面張力，從而穿透藻類的細胞膜或細胞壁，由藻類中自由進出並採出其體內那部分不易流出的油脂。
所述奈米線材料的微波合成優選為利用多批次的間歇性微波合成，一方面縮短傳統合成奈米線的時間，一方面也可以減少連續微波時產生過高的高溫導致奈米線組合成塊狀的形成，從而合成出具有較大表面積之奈米線以提高採油率。
配方中的鉀錳硫氧材料按照合理比例與合成條件的搭配，合成出具有選擇性吸附油而不吸附水的特性之奈米線，鑑於其吸附油之功效，可應用於廚房、浴室之去污清潔劑，以及汽機車機油之吸附處理，同時延伸到採取藻油的應用範圍，使藻類藻油的採收成本大大降低。
本案之功效與目的，可藉由下列實施方式說明，俾有更深入之了解。
 實施例1
將0.1%~30%的鉀、0.1%~30%的錳、0.1%~30%的硫、0.1%~30%的氧以可溶於水的形式溶於100 mL水中，以批次微波加熱的方式總共加熱10分鐘，微波加熱功率為最大功率的80%(最大功率為1000W)，加熱結束後即產生奈米線材料。
實施例2
按照如下重量百分比配備原料：0.1%~30%的鉀、0.1%~30%的錳、0.1%~30%的硫、0.1%~30%氧配置前驅物；將奈米材料前驅物充分混合後利用批次微波加熱合成提取劑。批次加熱的方式包含以下之一：將奈米材料的前驅物溶解於100 mL水的燒瓶中並置於微波爐中，以批次加熱之方式總共加熱20分鐘，微波加熱功率為最大功率的60%(最大功率為1000W)，加熱結束後產生奈米材料，接著冷卻至室溫後用去離子水洗淨產物，接著低溫烘烤去除奈米材料沾附的多餘水分，即得奈米線形貌之提取劑。
實施例3
按照如下重量百分比配備原料：0.1%~30%的鉀、0.1%~30%的錳、0.1%~30%的硫、0.1%~30%氧配置前驅物；將奈米材料前驅物充分混合後利用批次加熱合成。批次加熱的方式包含以下之一：將奈米材料的前驅物溶解於100 mL水中，以批次加熱之方式總共加熱30分鐘，加熱功率為400W，加熱結束後產生奈米材料，接著冷卻至室溫後用去離子水洗淨產物，接著低溫烘烤去除奈米材料沾附的多餘水分，即得奈米線形貌之提取劑。
實施例4
將0.1%~30%的硫酸鉀、0.1%~30%的過硫酸鉀、0.1%~30%的硫酸錳混合後溶解於100 mL水的燒瓶中，以微波加熱的方式每加熱30秒取出攪拌均勻再繼續加熱，總共加熱10分鐘，微波加熱功率為最大功率的80%(最大功率為1000W)，加熱結束後產生奈米材料，接著冷卻至室溫後用去離子水洗淨產物，接著低溫烘烤去除奈米材料沾附的多餘水分，即得無水鉀錳礬類複鹽(K2Mn2(SO4)3)，如第1圖所示之奈米線。
實施例5：提取劑之提油效率
首先將10 ml的水與3 ml的油混合，置入前述實驗所得之奈米材料0.066 g並上下前後搖晃均勻，然後將奈米線材料與油水液分離，靜置使油水分層以供選擇性吸附量的辨別，靜置兩分鐘後發現水完全沒有吸附，油卻被吸附了1 mL。
實施例6：奈米線進出藻類細胞壁
取0.001 g的奈米線，加入在10 mL水的綠球藻，等待約1天後，取出藻類在顯微鏡下觀察，發現黑色的奈米線出現在綠球藻的細胞壁內，如第2圖所示。累積在藻類體內的藻油，其尺寸會大於可穿透細胞壁的一微米通道，因此被侷限在藻類體內，一般萃取藻油都需要利用疏水性溶劑或者氣體(超臨界流體)打破藻類後或者穿透藻類取得藻油，本案利用小於一微米的奈米線，進入藻類體內吸附藻油，因為奈米線體積小所以可以將藻油自藻類體內攜帶出來，利用油水之密度差而漂浮上水面。
實施例
1.　一種製備一油提取劑的方法，包括下列步驟：
(a)將重量百分比0.1%～30%的硫酸鉀、0.1%～30%的過硫酸鉀以及0.1%～30%的硫酸錳溶於水中；
(b)利用微波加熱合成一化合物；
(c)冷卻該化合物至室溫；以及
(d)將該化合物低溫烘烤除水。
2.　根據實施例1所述之方法，其中該微波加熱為批次加熱。
3.　根據實施例1-2所述之方法，其中該油提取劑為一奈米線。
4.　根據實施例1-3所述之方法，其中該微波加熱之微波功率介於400～800W之間，該微波加熱之加熱時間介於20～40分鐘之間。
5.　一種製備一提取劑的方法，包括下列步驟：將鉀、錳、硫以及氧以可溶於水的形式溶於水中，以得到一水溶液；以及利用加熱該水溶液以得到該提取劑。
6.　根據實施例5所述之方法，其中該鉀、錳、硫以及氧分別具有重量百分比0.1%～30%，該加熱方式係為微波加熱，以及該提取劑係為一油提取劑。
7.　一種提取劑，其係具有一鉀錳硫氧之複鹽。
8.　根據實施例7所述之提取劑，其中該鉀錳硫氧之複鹽為無水鉀錳礬類複鹽(K2Mn2(SO4)3)，且其具有重量百分比0.1%～30%的鉀、0.1%～30%的錳、0.1%～30%的硫以及0.1%～30%的氧。
9.　根據實施例7-8所述之提取劑，其具有親油憎水之特性。
10.　根據實施例7-9所述之提取劑，係應用於藻類藻油之提取。
以上所述係利用較佳實施例詳細說明本發明，而非限制本發明的範圍，因此熟知此技藝的人士應能明瞭，適當而作些微的改變與調整，仍將不失本發明之要義所在，亦不脫離本發明之精神和範圍，故都應視為本發明的進一步實施狀況。謹請貴審查委員明鑑，並祈惠准，是所至禱。
本案得由熟習此技術之人士任施匠思而為諸般修飾，然皆不脫本案申請專利範圍所欲保護者。
第1圖：本發明一較佳實施例中掃瞄式電子顯微鏡下所觀察到合成之無水鉀錳礬類複鹽，其外形為一奈米線。
第2圖：本發明一較佳實施例中顯微鏡下所觀察之奈米線進出藻類細胞壁。

Claims (9)

  1. 一種製備一油提取劑的方法，包括下列步驟：(a)將重量百分比0.1%~30%的硫酸鉀、0.1%~30%的過硫酸鉀以及0.1%~30%的硫酸錳溶於水中；(b)利用微波加熱合成一化合物；(c)冷卻該化合物至室溫；以及(d)將該化合物低溫烘烤除水以得到一奈米線。
  2. 如申請專利範圍第1項所述之方法，其中該微波加熱為批次加熱。
  3. 如申請專利範圍第1項所述之方法，其中該微波加熱之微波功率介於400~800W之間，該微波加熱之加熱時間介於20~40分鐘之間。
  4. 一種製備一提取劑的方法，包括下列步驟：將鉀、錳、硫以及氧以可溶於水的形式溶於水中，以得到一水溶液，其中該鉀、錳、硫以及氧分別具有重量百分比0.1%~30%；以及利用加熱該水溶液以得到該提取劑，其中該提取劑為一奈米線。
  5. 如申請專利範圍第4項所述之方法，該加熱方式係為微波加熱，以及該提取劑係為一油提取劑。
  6. 一種提取劑，其係具有一鉀錳硫氧之複鹽，其中該提取劑為一奈米線，且該鉀錳硫氧之複鹽具有重量百分比0.1%~30%的鉀、0.1%~30%的錳、0.1%~30%的硫以及0.1%~30%的氧。
  7. 如申請專利範圍第6項所述之提取劑，其中該鉀錳硫氧之複鹽為無水鉀錳礬類複鹽(K2Mn2(SO4)3)。
  8. 如申請專利範圍第6項所述之提取劑，其具有親油憎水之特性。
  9. 如申請專利範圍第6項所述之提取劑，係應用於藻類藻油、煉油或化工製程廢污水中碳氫化合物之提取。
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