TW201809240A - Biodiesel manufacturing method using microwave heater and calcium di-glycerin with which the manufacturing time is short and the conversion efficiency is high - Google Patents
Biodiesel manufacturing method using microwave heater and calcium di-glycerin with which the manufacturing time is short and the conversion efficiency is high Download PDFInfo
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- TW201809240A TW201809240A TW105128430A TW105128430A TW201809240A TW 201809240 A TW201809240 A TW 201809240A TW 105128430 A TW105128430 A TW 105128430A TW 105128430 A TW105128430 A TW 105128430A TW 201809240 A TW201809240 A TW 201809240A
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- 239000003225 biodiesel Substances 0.000 title claims abstract description 46
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 45
- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- GFIKGNHHWZZCOJ-UHFFFAOYSA-N OCC(O)CO.OCC(O)CO.[Ca] Chemical compound OCC(O)CO.OCC(O)CO.[Ca] GFIKGNHHWZZCOJ-UHFFFAOYSA-N 0.000 title abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000005809 transesterification reaction Methods 0.000 claims abstract description 25
- 239000003921 oil Substances 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 10
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 29
- 239000011575 calcium Substances 0.000 claims description 27
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 26
- 229910052791 calcium Inorganic materials 0.000 claims description 26
- 239000003925 fat Substances 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 10
- 239000002699 waste material Substances 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 7
- 150000001298 alcohols Chemical class 0.000 claims description 6
- 239000008162 cooking oil Substances 0.000 claims description 4
- 235000014593 oils and fats Nutrition 0.000 claims description 2
- 238000000746 purification Methods 0.000 abstract description 9
- 239000008157 edible vegetable oil Substances 0.000 abstract description 5
- 235000019441 ethanol Nutrition 0.000 abstract 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 13
- 235000019198 oils Nutrition 0.000 description 13
- UQDUPQYQJKYHQI-UHFFFAOYSA-N methyl laurate Chemical compound CCCCCCCCCCCC(=O)OC UQDUPQYQJKYHQI-UHFFFAOYSA-N 0.000 description 6
- 235000011187 glycerol Nutrition 0.000 description 5
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 239000012043 crude product Substances 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000007127 saponification reaction Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 235000010469 Glycine max Nutrition 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 210000003278 egg shell Anatomy 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 102000002322 Egg Proteins Human genes 0.000 description 1
- 108010000912 Egg Proteins Proteins 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000010775 animal oil Substances 0.000 description 1
- -1 but not limited to Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- CQNLEUKJWMQIGM-UHFFFAOYSA-N calcium;propane-1,2,3-triol Chemical compound [Ca].OCC(O)CO CQNLEUKJWMQIGM-UHFFFAOYSA-N 0.000 description 1
- 241001233037 catfish Species 0.000 description 1
- 229940060799 clarus Drugs 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Fats And Perfumes (AREA)
Abstract
Description
本發明是有關於一種生質柴油的製備方法，特別是指一種利用微波加熱器及二甘油鈣促進轉酯化反應的生質柴油的製備方法。The invention relates to a method for preparing biodiesel, in particular to a method for preparing biodiesel using a microwave heater and calcium diglyceride to promote transesterification.
為了避免空氣汙染及全球溫室效應現象的持續擴大，以及有效解決消耗性能源日漸缺乏等問題，因此，必須積極尋找並開發替代的再生能源以補足能源的需求，並減緩溫室效應對環境與氣候造成的衝擊，其中，生質柴油(biodiesel)便是一種逐漸受到重視的再生能源。In order to avoid the continuous expansion of air pollution and the global greenhouse effect, and to effectively solve the problem of the growing shortage of consumable energy, we must actively seek and develop alternative renewable energy sources to meet the energy demand, and mitigate the greenhouse effect on the environment and climate The impact of biodiesel is a kind of renewable energy that is gradually receiving attention.
中國油脂2013年第38卷第8期揭示一種利用甘油鈣固體鹼催化大豆油製備生質柴油的方法。該方法包含以下步驟：步驟(a)，將廢棄雞蛋殼用熱水浸泡24小時並進行洗滌，於120℃乾燥，且於乾燥後進行粉碎。將粉碎的雞蛋殼於900℃進行5小時的培燒處理，製得氧化鈣。將氧化鈣與體積比為1:1的甘油及甲醇混合，形成一混合溶液，接著，對該混合溶液進行加熱至回流並進行2小時的反應。然後，冷卻至室溫。用甲醇洗滌，並於120℃進行24小時乾燥處理，接著，於一預定溫度下進行4小時培燒處理，即可得到二甘油鈣；步驟(b)，將大豆油、甲醇及二甘油鈣置於一反應瓶中，並加熱至回流，且在一預定時間反應後，冷卻至室溫。接著，進行過濾以去除二甘油鈣，並透過減壓蒸餾處理以去除甲醇，然後進行一純化處理以使生質柴油與反應過程中產生的甘油分離。雖該方法可獲得生質柴油，但生產時間長且轉化率低，不符合業者所需。China Oils and Fats Vol. 38, No. 8 of 2013 discloses a method for preparing biodiesel by catalyzing soybean oil with calcium glycerol solid base. The method includes the following steps: step (a), immersing the waste egg shells in hot water for 24 hours and washing, drying at 120 ° C, and pulverizing after drying. The crushed egg shell was roasted at 900 ° C for 5 hours to obtain calcium oxide. Calcium oxide is mixed with glycerol and methanol in a volume ratio of 1: 1 to form a mixed solution, and then the mixed solution is heated to reflux and reacted for 2 hours. Then, it was cooled to room temperature. Washing with methanol and drying treatment at 120 ° C for 24 hours, and then calcining treatment at a predetermined temperature for 4 hours to obtain calcium diglyceride; step (b), soy oil, methanol and calcium diglyceride In a reaction bottle, heat to reflux and cool to room temperature after reacting for a predetermined time. Then, filtration is performed to remove calcium diglyceride, and methanol is removed by distillation under reduced pressure, and then a purification treatment is performed to separate biodiesel from glycerol generated during the reaction. Although this method can obtain biodiesel, the production time is long and the conversion rate is low, which does not meet the needs of the industry.
有鑑於上述，開發一種生產時間短且轉化率高的生質柴油的製備方法，係為本發明研究改良的重要目標。In view of the above, the development of a method for preparing biodiesel with short production time and high conversion rate is an important goal of the research and improvement of the present invention.
因此，本發明的目的，即在提供一種生產時間短且轉化率高的利用微波加熱器及二甘油鈣的生質柴油的製備方法。Therefore, an object of the present invention is to provide a method for preparing a biodiesel using a microwave heater and calcium diglyceride with a short production time and a high conversion rate.
於是，本發明生質柴油的製備方法，包含以下步驟：步驟(a)，準備一轉酯化反應設備，包括一反應槽及一微波加熱器；步驟(b)，將一包含油脂、醇類與二甘油鈣[Ca(C3 H7 O3 )2 ]的組分置入該反應槽中，並藉由該微波加熱器施予一加熱處理，以進行一轉酯化反應(transesterification)，而得到一混合物；步驟(c)，將該混合物進行純化處理，即得生質柴油。Therefore, the method for preparing biodiesel according to the present invention includes the following steps: step (a), preparing a transesterification reaction device, including a reaction tank and a microwave heater; and step (b), adding a fat and alcohol The components with calcium diglycerol [Ca (C 3 H 7 O 3 ) 2 ] are put into the reaction tank, and a heating treatment is applied by the microwave heater to perform a transesterification reaction, A mixture is obtained; in step (c), the mixture is purified to obtain biodiesel.
本發明的功效在於：以該二甘油鈣作為觸媒並利用該微波加熱器，以促進該轉酯化反應的進行，有效地縮短該轉酯化反應的反應時間並提高轉化率，因而可快速並大量製備出生質柴油。The effect of the present invention is that the calcium diglyceride is used as a catalyst and the microwave heater is used to promote the progress of the transesterification reaction, effectively shorten the reaction time of the transesterification reaction and improve the conversion rate, so that it can quickly And a large amount of biodiesel is prepared.
以下將就本發明內容進行詳細說明。The content of the present invention will be described in detail below.
於該步驟(a)中，該反應槽並無特別的限制，只要能容納該組分且不與該該組分中各成分反應的容器皆可。In the step (a), the reaction tank is not particularly limited, as long as the container can contain the component and does not react with each component of the component.
於該步驟(b)中，該微波加熱器用來對容置於該反應槽內的該組分進行加熱，以促使該轉酯化反應進行。該微波加熱器例如但不限於家庭微波爐或工業微波反應器等。該轉酯化反應設備還包括一設置在該反應槽的冷凝器。該冷凝器用來冷凝在該加熱處理過程中揮發的醇類以減少該醇類的流失，且具有一供一水進入的進水口與一供該水排出的出水口。為使本發明生質柴油的製備方法具有較佳的轉化率，較佳地，該微波加熱器的操作功率範圍為50瓦至600瓦。更佳地，該微波加熱器的操作功率範圍為200瓦至400瓦。In step (b), the microwave heater is used to heat the component contained in the reaction tank to promote the transesterification reaction. The microwave heater is, for example, but not limited to, a domestic microwave oven or an industrial microwave reactor. The trans-esterification reaction device further includes a condenser provided in the reaction tank. The condenser is used to condense alcohols volatilized during the heat treatment process to reduce the loss of the alcohols, and has a water inlet for a water to enter and a water outlet for the water to be discharged. In order to make the method for preparing the biodiesel of the present invention have a better conversion rate, preferably, the operating power of the microwave heater ranges from 50 watts to 600 watts. More preferably, the microwave heater has an operating power range of 200 to 400 watts.
於該步驟(b)中，該油脂可單獨使用一種或混合多種使用，且該油脂例如但不限於動物油、植物油或廢食用油等。基於提高廢食用油的再利用價值、解決廢食用油處理的問題以滿足資源永續利用的環保需求，並減少生產成本，在本實施例中，該油脂為廢食用油。該醇類可單獨使用一種或混合多種使用，且該醇類例如但不限於甲醇(CH3 OH)、乙醇(C2 H5 OH)、丙醇(C3 H7 OH)或丁醇(C4 H9 OH)等。於本實施例中，該醇類為甲醇。為使本發明生質柴油的製備方法具有較佳的轉化率，較佳地，該醇類與該油脂的莫耳比例範圍為5:1至9:1。更佳地，該醇類與該油脂的莫耳比例範圍為6:1至9:1。In the step (b), the fats and oils may be used alone or in combination, and the fats and oils such as, but not limited to, animal oils, vegetable oils, or waste cooking oils may be used. Based on increasing the reuse value of waste edible oil, solving the problem of waste edible oil treatment to meet environmental protection needs for sustainable use of resources, and reducing production costs, in this embodiment, the fat is waste edible oil. The alcohols can be used alone or in combination, and the alcohols are, for example, but not limited to, methanol (CH 3 OH), ethanol (C 2 H 5 OH), propanol (C 3 H 7 OH), or butanol (C 4 H 9 OH) and so on. In this embodiment, the alcohol is methanol. In order to make the method for preparing the biodiesel of the present invention have a better conversion rate, preferably, the molar ratio of the alcohol to the fat is in the range of 5: 1 to 9: 1. More preferably, the molar ratio of the alcohol to the fat ranges from 6: 1 to 9: 1.
於該步驟(b)中，為使本發明生質柴油的製備方法具有較佳的轉化率，且為使在該轉酯化反應的過程中減少因皂化反應產生的微膠狀物的量，較佳地，以該油脂的使用量為100重量份計，該二甘油鈣的使用量範圍為1重量份至3重量份。更佳地，以該油脂的使用量為100重量份計，該二甘油鈣的使用量範圍為1重量份至2.5重量份。In this step (b), in order to make the method for preparing the biodiesel of the present invention have a better conversion rate, and to reduce the amount of micro gelatinous matter produced by the saponification reaction during the transesterification reaction, Preferably, based on the use amount of the fat and oil being 100 parts by weight, the use amount of the calcium diglyceride ranges from 1 part by weight to 3 parts by weight. More preferably, the use amount of the calcium diglyceride ranges from 1 part by weight to 2.5 parts by weight based on the use amount of the fat and oil being 100 parts by weight.
為加速該轉酯化反應的進行或為使本發明生質柴油的製備方法具有較佳的轉化率，於該步驟(b)中，該組分還包含活性碳。於該步驟(b)中，為使本發明生質柴油的製備方法具有較佳的轉化率，較佳地，以該油脂的使用量為100重量份計，該活性碳的使用量範圍為0.5重量份至2.5重量份。更佳地，以該油脂的使用量為100重量份計，該活性碳的使用量範圍為0.5重量份至1.5重量份。In order to accelerate the transesterification reaction or to make the method for preparing the biodiesel of the present invention have a better conversion rate, in this step (b), the component further includes activated carbon. In this step (b), in order to make the method for preparing the biodiesel of the present invention have a better conversion rate, preferably, based on the use amount of the oil and fat being 100 parts by weight, the use amount of the activated carbon ranges from 0.5 Part by weight to 2.5 parts by weight. More preferably, the amount of the activated carbon is in the range of 0.5 parts by weight to 1.5 parts by weight based on the use amount of the fat and oil being 100 parts by weight.
為加速該轉酯化反應的進行或為使本發明生質柴油的製備方法具有較佳的轉化率，於該步驟(b)中，該組分還包含水。較佳地，以該油脂的使用量為100重量份計，該水的使用量範圍為0.5重量份至2.5重量份。更佳地，以該油脂的使用量為100重量份計，該水的使用量範圍為0.5重量份至2重量份。In order to accelerate the transesterification reaction or to make the method for preparing the biodiesel of the present invention have a better conversion rate, in this step (b), the component further includes water. Preferably, the amount of water used is in the range of 0.5 parts by weight to 2.5 parts by weight based on the use amount of the fat and oil being 100 parts by weight. More preferably, the amount of water used is in the range of 0.5 parts by weight to 2 parts by weight based on the use amount of the fat and oil being 100 parts by weight.
為使本發明生質柴油的製備方法具有較佳的轉化率，較佳地，於該步驟(b)中，該轉酯化反應的反應時間範圍為10分鐘至30分鐘。更佳地，於該步驟(b)中，該轉酯化反應的反應時間範圍為15分鐘至30分鐘。為使本發明生質柴油的製備方法具有較佳的轉化率，較佳地，於該步驟(b)中，該轉酯化反應的反應溫度範圍為50℃至70℃。更佳地，於該步驟(b)中，該轉酯化反應的反應溫度範圍為55℃至70℃。In order to make the method for preparing the biodiesel of the present invention have a better conversion rate, preferably, in the step (b), the reaction time of the transesterification reaction ranges from 10 minutes to 30 minutes. More preferably, in the step (b), the reaction time of the transesterification reaction ranges from 15 minutes to 30 minutes. In order to make the method for preparing the biodiesel of the present invention have a better conversion rate, preferably, in the step (b), the reaction temperature range of the transesterification reaction is 50 ° C to 70 ° C. More preferably, in the step (b), the reaction temperature of the transesterification reaction ranges from 55 ° C to 70 ° C.
於該步驟(c)中，由於該混合物實質上包含了未反應的物質(為未反應的油脂及未反應的醇類)、水、活性碳、二甘油鈣、生質柴油，及甘油(C3 H8 O3 )，因此，需將該混合物進行該純化處理，以獲得該生質柴油。該分離純化處理可採用一般所知的純化處理方式，例如透過一離心機來進行。於本實施例中，該純化處理是利用一離心機來進行。為使本發明生質柴油的製備方法具有較佳的純化效益，該離心機的操作轉速範圍為3500rpm以上，且該離心機的離心操作時間範圍為10分鐘以上。In this step (c), the mixture substantially contains unreacted substances (which are unreacted fats and oils and unreacted alcohols), water, activated carbon, calcium diglyceride, biodiesel, and glycerin (C 3 H 8 O 3 ), therefore, the mixture needs to be subjected to the purification treatment to obtain the biodiesel. The separation and purification treatment can be performed by a generally known purification treatment method, for example, by a centrifuge. In this embodiment, the purification process is performed using a centrifuge. In order to make the method for preparing biodiesel of the present invention have better purification benefits, the operating speed range of the centrifuge is above 3500 rpm, and the centrifuge operating time range of the centrifuge is above 10 minutes.
本發明將就以下實施例來作進一步說明，但應瞭解的是，該實施例僅為例示說明之用，而不應被解釋為本發明實施之限制。The present invention will be further described with reference to the following examples, but it should be understood that this example is for illustrative purposes only and should not be construed as a limitation on the implementation of the present invention.
製備例1 二甘油鈣Preparation Example 1 Calcium diglyceride
提供一製備該二甘油鈣的反應設備，且該反應設備包含一反應槽、一用來加熱該反應槽的恆溫水槽、一設置在該反應槽的攪拌器，及一安裝在該反應槽的冷凝器。將9克的氧化鈣、132克的甲醇及30克的甘油置入該反應槽中。將該反應槽置於溫度設定在60℃的恆溫水槽中。利用攪拌器，對該氧化鈣、甲醇及甘油進行一攪拌處理，並於該溫度下進行反應，其中，該攪拌器的操作轉速為3000rpm，該反應時間為3小時。接著觀察溶液顏色，當該顏色轉變成淡黃色，即表示反應完成。然後，將該淡黃色溶液置於一離心機(廠牌：HERMLE；型號：Z200A)進行一純化處理，其中，該離心機的操作轉速為4000rpm，且該離心機的離心操作時間為5分鐘。接著倒出上層溶液，並取出下層沉澱物。然後，使用甲醇洗滌該沉澱物共2次，並置於一真空乾燥機中進行8小時的乾燥處理。A reaction device for preparing the calcium diglyceride is provided, and the reaction device includes a reaction tank, a constant temperature water tank for heating the reaction tank, a stirrer provided in the reaction tank, and a condensation installed in the reaction tank. Device. 9 grams of calcium oxide, 132 grams of methanol, and 30 grams of glycerol were placed in the reaction tank. This reaction tank was placed in a thermostatic water tank whose temperature was set at 60 ° C. Using a stirrer, perform a stirring treatment on the calcium oxide, methanol, and glycerin, and perform the reaction at the temperature. The operating speed of the stirrer is 3000 rpm, and the reaction time is 3 hours. Then observe the color of the solution. When the color changes to light yellow, the reaction is complete. Then, the light yellow solution was placed in a centrifuge (brand: HERMLE; model: Z200A) for a purification process, wherein the operating speed of the centrifuge was 4000 rpm, and the centrifuge operation time of the centrifuge was 5 minutes. The upper solution was then decanted and the lower precipitate was removed. Then, the precipitate was washed twice with methanol and placed in a vacuum dryer for 8 hours.
實施例1 生質柴油Example 1 Biodiesel
提供一製備該生質柴油的轉酯化反應設備，且該轉酯化反應設備包含一反應槽、一微波加熱器(廠牌：明昱科技；型號：XO-SM50)，及一設置在該反應槽的冷凝器。將1克的製備例1的二甘油鈣、17.91克的甲醇及100克的廢棄食用油(平均分子量為893.34，皂化價為188.395，為大豆油(廠牌：統一)經油炸土魠魚後的廢棄油)置入該反應槽中，其中，該甲醇與該廢棄食用油的莫耳比例為5:1。將該反應槽置於功率設定在500瓦的微波加熱器中。利用內置磁子攪拌器，對該二甘油鈣、該甲醇及該廢棄食用油進行一攪拌處理，並於該溫度下進行反應，形成一混合物，該轉酯化反應的反應時間為20分鐘。接著將該混合物置於一離心機(廠牌：HERMLE；型號：Z200A)中進行一純化處理，獲得含有生質柴油的粗產物。A transesterification reaction device for preparing the biodiesel is provided, and the transesterification reaction device includes a reaction tank, a microwave heater (brand: Ming Yu Technology; model: XO-SM50), and a device installed in the The condenser of the reaction tank. 1 g of calcium diglyceride of Preparation Example 1, 17.91 g of methanol, and 100 g of waste edible oil (average molecular weight is 893.34, saponification value is 188.395, soy oil (brand: Uniform)) after deep-fried soil catfish Waste oil) is placed in the reaction tank, wherein the molar ratio of the methanol to the waste cooking oil is 5: 1. The reaction tank was placed in a microwave heater set at 500 watts. A built-in magnetic stirrer is used to perform a stirring treatment on the calcium diglyceride, the methanol, and the waste cooking oil, and react at the temperature to form a mixture. The reaction time of the transesterification reaction is 20 minutes. The mixture is then placed in a centrifuge (brand: HERMLE; model: Z200A) for a purification process to obtain a crude product containing biodiesel.
實施例2至33Examples 2 to 33
實施例2至33是以與實施例1相同的步驟來製備生質柴油，不同的地方如表1所示。Examples 2 to 33 are the same steps as in Example 1 to prepare biodiesel. The differences are shown in Table 1.
評價項目Evaluation item
轉化率(單位：%)：使用氣相層析儀(型號：Perkin Elmer GC Clarus 600)分析實施例1至33的含生質柴油的粗產物中的生質柴油含量，並透過公式(1)計算出轉化率。將0.5克的含生質柴油的粗產物、0.05克月桂酸甲酯標準品及10毫升的正己烷混合，形成一待測品。將1μL的待測品注射至該氣相層析儀中進行分析。該氣相層析儀的設定條件：注射口溫度為280 ℃，氮氣流速為45 mL/min，空氣流速為450 mL/min，分流比(split ratio)為1:20，火焰離子化偵測器的溫度為300 ℃，升溫程序為於210℃維持4 分鐘，接著以4 ℃/min的速率，將溫度上升至240 ℃並維持8 分鐘。該公式(1)為轉化率=[(生質柴油的積分面積/月桂酸甲酯的積分面積)×月桂酸甲酯的重量]×100%/含生質柴油的粗產物的重量。Conversion rate (unit:%): Analyze the biodiesel content in the crude product containing biodiesel of Examples 1 to 33 using a gas chromatograph (model: Perkin Elmer GC Clarus 600), and pass the formula (1) Calculate the conversion rate. 0.5 g of crude product containing biodiesel, 0.05 g of methyl laurate standard and 10 ml of n-hexane were mixed to form a test product. 1 μL of the test substance was injected into the gas chromatograph for analysis. Setting conditions of the gas chromatograph: the injection port temperature is 280 ℃, the nitrogen flow rate is 45 mL / min, the air flow rate is 450 mL / min, the split ratio is 1:20, and the flame ionization detector The temperature was 300 ° C, and the heating program was maintained at 210 ° C for 4 minutes, and then the temperature was increased to 240 ° C at a rate of 4 ° C / min for 8 minutes. The formula (1) is a conversion rate = [(integrated area of biodiesel / integrated area of methyl laurate) × weight of methyl laurate] × 100% / weight of crude product containing biodiesel.
油脂平均分子量：利用公式(2)計算出。該公式(2)為(3×56.1×1000)/皂化價，其中，該56.1為氫氧化鉀的分子量。Average molecular weight of fats and oils: Calculated by formula (2). The formula (2) is (3 × 56.1 × 1000) / saponification value, where 56.1 is the molecular weight of potassium hydroxide.
表1
綜上所述，以該二甘油鈣作為觸媒並利用該微波加熱器，以促進該轉酯化反應的進行，有效地縮短該轉酯化反應的反應時間並提高轉化率，因而可快速並大量製備出生質柴油，故確實能達成本發明的目的。In summary, the calcium diglyceride is used as a catalyst and the microwave heater is used to promote the progress of the transesterification reaction, effectively shorten the reaction time of the transesterification reaction and improve the conversion rate. Since a large amount of biodiesel is prepared, it can indeed achieve the purpose of the invention.
惟以上所述者，僅為本發明的實施例而已，當不能以此限定本發明實施的範圍，凡是依本發明申請專利範圍及專利說明書內容所作的簡單的等效變化與修飾，皆仍屬本發明專利涵蓋的範圍內。However, the above are only examples of the present invention. When the scope of implementation of the present invention cannot be limited by this, any simple equivalent changes and modifications made according to the scope of the patent application and the contents of the patent specification of the present invention are still Within the scope of the invention patent.
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