CN105132160A - Two-step decoloring process of bio-diesel - Google Patents
Two-step decoloring process of bio-diesel Download PDFInfo
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- CN105132160A CN105132160A CN201510409767.4A CN201510409767A CN105132160A CN 105132160 A CN105132160 A CN 105132160A CN 201510409767 A CN201510409767 A CN 201510409767A CN 105132160 A CN105132160 A CN 105132160A
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- decoloring
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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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Abstract
The invention relates to a two-step decoloring process of bio-diesel, which includes following steps: (1) adding a mixture of activated clay and activated carbon according to different ratio in a certain quantity to 100 g of a bio-diesel sample; (2) vacuumizing and thermal-decoloring the bio-diesel sample in water bath at 30-150 DEG C, and performing pressure-reduction suction filtration to remove the decoloring agent; and (3) performing a cold-decoloring test at normal temperature, and finally performing pressure-reduction suction filtration to remove the decoloring agent. Decoloring efficiency is calculated in a manner that with petroleum ether as a blank, a maximum absorption peak is found through spectral scanning, and then photometric measurement is carried out to obtain the absorbancy of the sample under the maximum absorption peak. The decoloring rate is the ratio of the difference between the absorbancy before decoloring and the absorbancy after decoloring to the absorbancy before decoloring. The two-step decoloring process is simple in operation, is quick in decoloring, is low in production cost and is good in decoloring effect. The decoloring process solves the problem of an earthy-like odor of the bio-diesel sample due to decoloring with activated clay. The decoloring process can reach 83-90% in one-time decoloring rate.
Description
Technical field
The invention belongs to biological chemical field, be mainly concerned with the technique of the dark biofuel two-step approach decolouring that is raw material such as waste cooking oil.
Background technology
Along with becoming increasingly conspicuous of the problem such as shortage of resources, environmental pollution, find a kind of environmental protection, reproducible green energy resource becomes universe's difficult problem urgently to be resolved hurrily.And biofuel is with lipid raw material, as the clean regeneratable liquors fuel that discarded animal-plant oil (abbreviation waste grease), non-edible grass/woody oleiferous plants etc. are produced, have that cetane value is high, nontoxic, low-sulfur, degradable, without features such as aromatic hydrocarbons, directly can substitute or concoct with fossil diesel fuel and use, become the favorable substitutes of petroleum-based energy.
Simultaneously, China is again food and drink big country, annual waste cooking oil is at 300 ~ 5,000,000 tons, the severe overweight such as peroxide value, acid value, moisture content, bacteria content of these waste cooking oils, belong to inedible oil, all very harmful to the mankind, animal, also can cause the pollution of ecotope, how solve these waste cooking oils and return dining table Ye Shi China problem demanding prompt solution.
Take waste cooking oil as raw material, biofuel is prepared by transesterification reaction, as novel liquid fuel, air quality and ecotope can be improved, can solve again " sewer oil " to reflux dining table problem, conscientiously ensuring food safety, is turn waste into wealth, turn harm into good, and reduces the cost of biofuel.
But through the waste cooking oil of heat repeatedly, some phosphatide and protein etc. in its oil plant start to decompose, sex change, generate a large amount of dark matters; Meanwhile, the lipid acid in grease and glyceryl ester etc. also generate coloring matter or potential present-color material under the condition of high temperature.The biofuel prepared through transesterify for raw material with this dark grease more also presents Vandyke brown.
Color and luster is one of important factor affecting biodiesel quality.Although traditional rectifying or process for purifying distillation also have certain decolorizing effect, but its decolorizing effect is not good, and equipment cost and process cost are all relatively high, and space-time yield is relatively low, make the cost of biofuel higher, thus limit its popularization and application on a large scale.
Chinese patent CN200620166641.5 discloses a kind of biofuel extraction plant, it utilizes useless animal and plant grease, cracking in vapour phase is carried out while liquid catalysis, thus production biofuel, its decolorization process is after reaction kettle of the esterification, increase decolouring still, 100 DEG C time, add atlapulgite, air agitation decolours.But the discoloring agent that this decoloration process adds is more single, fully can not remove coloring matter, decolorizing effect is not good, and higher to the requirement of equipment etc., to consume cost higher.
Chinese patent CN200710000281.0 discloses a kind of biodiesel preparation, and the method for wherein decolouring to the biofuel generated adds 5% dioxide peroxide and 5% crystal sand, or directly add 5% crystal sand.But because the toxicity of dioxide peroxide is comparatively large, operation has certain danger, and it has certain selectivity to the oxidation of coloring matter, the grease-decolor poor effect more complicated to compositions such as waste cooking oils.
Chinese patent CN200910092293.X discloses a kind of biofuel decoloring method, uses atlapulgite and bentonite mixtures adsorption bleaching, is carrying out hydrogen peroxide oxidation, obtains biofuel finally by depickling dehydration.Because the material that atlapulgite obtains after to be exactly wilkinite acidic activated, after using atlapulgite and bentonite adsorption, grease with certain bilgy odour, can have impact to the taste of biofuel.When again decolouring, use hydrogen peroxide as discoloring agent, need higher temperature of reaction, just can give full play to its oxygenizement, add energy consumption.
Chinese patent CN201210271002.5 discloses one and utilizes Preparation of biodiesel from waste oils decoloring method, and it is that biofuel prepared by raw material with sewer oil, and adopt hydrogen peroxide oxidation method to dark grease-decolor, and the grease-decolor rate obtained is 67.83%.But hydrogen peroxide is a kind of chemical oxidizing agent, the adsorption decolouriser that its cost is more general is higher, is not suitable for large-scale decolorization experiment, and hydrogen peroxide for decoloration, oxidizable dark matter can only be removed, and require higher to the temperature of reaction and the pH of biofuel.
As can be seen from above content, there are chemical method and absorption method two kinds to the decolouring of biofuel prepared by waste cooking oil at present.And chemical decolorization agent has certain selectivity to pigment, and in reaction process, reaction conditions is required comparatively strict, and some chemical decolorization agent itself have toxicity, needs Special controlling during operation, adds equipment and running cost.Adsorption bleaching comparatively generally uses decoloring method in the market, but single sorbent material is not enough to coloring matter and potential colour generation group to remove totally, and when using activated decoloration, Bio-diesel Samples can be made with bilgy odour, thus affect its quality.In addition, optimization was not carried out to decoloration process all relating in the patent of biofuel decolouring, thus obtained best decoloration process.
Summary of the invention
According to above-mentioned deficiency, the invention provides a kind of biofuel two-step approach decoloration process, adopt two kinds of conventional adsorption decolourisers, by adding different ratio thus improving decolorizing effect, and reduce the bilgy odour of carclazyte.The cost of the material and facility required for this invention is lower, without the need to decompression or air distillation, simple to operate, without the need to washing after decolouring terminates.In addition, the present invention optimizes the impact of factor each in decoloration process on decolouring result, and designs orthogonal experiment, is optimized the combined influence result of all factors.
In order to realize foregoing invention object, the technical solution used in the present invention is: a kind of biofuel two-step approach decoloration process, is characterized in that, comprise the steps:
S1, in Bio-diesel Samples, add the mixing discoloring agent of biodiesel fuel quality 10% ~ 75%, at 30 ~ 150 DEG C of temperature, stir decolouring 30 ~ 150min, decompress filter removing discoloring agent;
Again add oil in S2, the material that obtains at S1 and weigh 10% ~ 75% mixing discoloring agent, stir decolouring 30 ~ 150min at normal temperatures, decompress filter removing discoloring agent;
S3, be blank with sherwood oil, measure the absorbancy of the sample through step S1 and step S2 decolouring; Percent of decolourization equals the ratio of absorbance difference and the front absorbancy of decolouring before and after Bio-diesel Samples decolouring;
Wherein, mixing discoloring agent is the atlapulgite of different ratios and the mixing of gac; In mixing discoloring agent, the mass ratio of atlapulgite is 60 ~ 90%, and all the other are gac.
Bio-diesel Samples is the dark grease obtained by transesterification reaction by waste cooking oil.
In step S1 and S2, the amount of mixing discoloring agent is that oil is heavy by 45%.The heat decoloring of step S1 carries out under vacuum conditions.In step S3, after spectral scan, be that the maximum absorption band of the sample of reference is at 395nm with sherwood oil.
After biofuel two-step approach decoloration process is through single factor test optimization, design L
18(5
3) orthogonal table, obtain after orthogonal experiment.The factor of single factor test optimization comprises: discoloring agent consumption, discoloring agent proportioning, bleaching temperature, heat decoloring time, cold bleaching time, decolouring number of times.
Beneficial effect: this is invented compared with prior art tool and has the following advantages:
1, adopt gac and atlapulgite as mixing discoloring agent, effectively can solve single adsorption agent and be not enough to coloring matter and potential colour generation group to remove clean problem; Again can complementary raising decolorizing effect, reduce the adsorption rate of discoloring agent, and when effectively can remove activated decoloration with bilgy odour, improve the quality of biofuel.
2, decoloration process reduced pressure heat decoloring before this, removed some thermo-sensitivity pigments, and rear normal pressure decolouring, utilizes the absorption property under sorbent material normal temperature to decolour.By the method that heat decoloring and cold decolouring combine, add contact area and the time of discoloring agent and grease, make the biofuel color and luster after decolouring brighter.And this decoloring method is simple to operate, does not need harsh experiment condition, the cost of equipment and energy consumption can be saved.
3, after the present invention has carried out single factor test optimization to the factor affecting decolorizing effect in decoloration process, design orthogonal test again, investigate multiple decolouring factor to the combined influence of decolorizing effect, finally obtain a decoloration process to dark grease decolorizing effect the best, through the decolouring of this technique, dark Bio-diesel Samples drops to about 0.2 in the absorbancy at 390nm place from about 1.0, and percent of decolourization reaches more than 83%.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Biofuel two-step approach decoloration process, it comprises the following steps:
(1) in Bio-diesel Samples, add quality is atlapulgite and the gac mixing discoloring agent that biofuel oil weighs 10% ~ 70%, wherein atlapulgite accounts for the mass ratio of mixing discoloring agent is 60 ~ 90%, all the other are gac, decolouring 30 ~ 150min is stirred, decompress filter removing discoloring agent at 30 ~ 150 DEG C of temperature;
(2) in the Bio-diesel Samples processed through step (1), add above-mentioned same discoloring agent again and carry out cold decolouring, at normal temperatures, stir decolouring 30 ~ 150min, suction filtration removing discoloring agent, obtains the biofuel after decolouring.
(3) calculating of percent of decolourization: the biofuel after decolouring is added in the cuvette of 1.0cm, take sherwood oil as blank, carry out spectral scan under 395nm, the absorbancy of record sample.Percent of decolourization equals the ratio of absorbance difference and the front absorbancy of decolouring before and after biofuel decolouring.
(4), in above-mentioned decoloration technology of biological diesel oil, be raw material with waste cooking oil during Bio-diesel Samples in step (1), the dark biofuel obtained by transesterification reaction.
(5) according to the technique of step (1), (2), (3), single factor test optimization has been carried out to decolorization condition, mainly contained: discoloring agent consumption, discoloring agent proportioning, bleaching temperature, heat decoloring time, cold bleaching time, decolouring number of times.
(6) by the optimization of step (5), orthogonal experiment has been carried out to decoloration process, design L
18(5
3) orthogonal table, after orthogonal experiment, finally obtain best decoloration process.
The step of specific embodiment one, present embodiment is as follows:
Step one: adding quality in Bio-diesel Samples prepared by waste cooking oil is the mixing discoloring agent that oil weighs 30%, and wherein the ratio of atlapulgite and gac is 5:1, under 60 DEG C of water-baths, vacuumizes and adds heat decoloring 60min;
Step 2: the material of step one is used sand core funnel decompress filter, removing discoloring agent, obtains heat decoloring artifact diesel samples;
Step 3: again adding quality to the sample of gained in step 2 is the mixing discoloring agent that oil weighs 30%, and wherein the ratio of atlapulgite and gac is 5:1, at normal temperatures, stirs decolouring 30min;
Step 4: the material of step 3 is used sand core funnel decompress filter, removing discoloring agent, finally decoloured artifact diesel oil;
Step 5: the sample 1ml getting step 4, adding 4ml sherwood oil (30 ~ 60 boiling range), after mixing, add in the cuvette of 1.0cm, take sherwood oil as blank, and measure its absorbancy at 390nm place, the percent of decolourization finally obtained is the product of 63%;
Specific embodiment two: this implementation method and specific embodiment one difference be to mix described in step one discoloring agent account for oil heavy 45%, the heat decoloring time is 90min, the cold bleaching time of step 3 kind is 60min, other steps are identical in specific embodiment one, and the percent of decolourization of the product finally obtained is 74%;
Specific embodiment three: this implementation method and specific embodiment one difference be to mix described in step one discoloring agent account for oil heavy 60%, other steps are identical in specific embodiment one, and the percent of decolourization of the product finally obtained is 84%;
Specific embodiment four: this implementation method and specific embodiment one difference are that a kind of described ratio mixing atlapulgite and gac in discoloring agent of step is 2:1, the cold bleaching time of step 3 kind is 15min, other steps are identical in specific embodiment one, and the percent of decolourization of the product finally obtained is 58%;
Specific embodiment five: this implementation method and specific embodiment three difference are the Bio-diesel Samples obtained in embodiment three to repeat decolouring one time according to the method for embodiment three, and the percent of decolourization of the product finally obtained is 90%.
More than show and describe ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification sheets just says principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements are all dropped in the claimed scope of the invention.Application claims protection domain is defined by appending claims and equivalent thereof.
Claims (7)
1. a biofuel two-step approach decoloration process, is characterized in that, comprises the steps:
S1, add in Bio-diesel Samples oil weigh 10% ~ 75% mixing discoloring agent, at 30 ~ 150 DEG C of temperature, stir decolouring 30 ~ 150min, decompress filter removing discoloring agent;
Again add oil in S2, the material that obtains at S1 and weigh 10% ~ 75% mixing discoloring agent, stir decolouring 30 ~ 150min at normal temperatures, decompress filter removing discoloring agent;
S3, be blank with sherwood oil, measure the absorbancy of the sample through step S1 and step S2 decolouring; Percent of decolourization equals the ratio of absorbance difference and the front absorbancy of decolouring before and after Bio-diesel Samples decolouring;
Wherein, mixing discoloring agent is the atlapulgite of different ratios and the mixing of gac; In mixing discoloring agent, the mass ratio of atlapulgite is 60 ~ 90%, and all the other are gac.
2. a kind of biofuel two-step approach decoloration process according to claim 1, is characterized in that, Bio-diesel Samples is the dark grease obtained by transesterification reaction by waste cooking oil.
3. a kind of biofuel two-step approach decoloration process according to claim 1, is characterized in that, in step S1 and S2, the amount of mixing discoloring agent is that oil is heavy by 45%.
4. a kind of biofuel two-step approach decoloration process according to claim 1, is characterized in that, the heat decoloring of step S1 carries out under vacuum conditions.
5. a kind of biofuel two-step approach decoloration process according to claim 1, is characterized in that, in step S3, after spectral scan, is that the maximum absorption band of the sample of reference is at 395nm with sherwood oil.
6. a kind of biofuel two-step approach decoloration process according to claim 1-5 any one, is characterized in that, after biofuel two-step approach decoloration process is through single factor test optimization, and design L
18(5
3) orthogonal table, obtain after orthogonal experiment.
7. a kind of biofuel two-step approach decoloration process according to claim 6, it is characterized in that, the factor of single factor test optimization comprises: discoloring agent consumption, discoloring agent proportioning, bleaching temperature, heat decoloring time, cold bleaching time, decolouring number of times.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778989A (en) * | 2016-04-06 | 2016-07-20 | 成都天丰清洁能源发展有限公司 | Crude diesel oil discoloring agent |
| CN112725079A (en) * | 2020-11-11 | 2021-04-30 | 广东电网有限责任公司 | Decoloring process for producing kitchen waste grease-based natural ester insulating oil |
| CN115197779A (en) * | 2022-06-23 | 2022-10-18 | 武汉泽电新材料有限公司 | Composite decoloring method for preparing electric insulating oil from deep-color kitchen waste grease |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778989A (en) * | 2016-04-06 | 2016-07-20 | 成都天丰清洁能源发展有限公司 | Crude diesel oil discoloring agent |
| CN112725079A (en) * | 2020-11-11 | 2021-04-30 | 广东电网有限责任公司 | Decoloring process for producing kitchen waste grease-based natural ester insulating oil |
| CN115197779A (en) * | 2022-06-23 | 2022-10-18 | 武汉泽电新材料有限公司 | Composite decoloring method for preparing electric insulating oil from deep-color kitchen waste grease |
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Application publication date: 20151209 |
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