CN103710057B - A kind of preparation method of novel bio-gasoline - Google Patents
A kind of preparation method of novel bio-gasoline Download PDFInfo
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Abstract
The present invention relates to biomass energy chemical technology field, be specifically related to the preparation method of a kind of novel bio-gasoline.The preparation method of the novel bio-gasoline of the present invention, is raw material by citric acid industry waste thallus Aspergillus niger, prepares biogasoline via chitin, 5 Hydroxymethylfurfural, 5 ethoxyl methyl furfurals.Using citric acid industry waste thallus Aspergillus niger in the preparation method of the novel bio-gasoline of the present invention is raw material, can significantly alleviate environmental pollution pressure, and the biogasoline product energy density of preparation is high, and in electromotor, steadily, thoroughly, carbon distribution is few in burning.
Description
Technical field
The present invention relates to biomass energy chemical technology field, be specifically related to the preparation method of a kind of novel bio-gasoline.
Background technology
Along with the regenerative resource new in the urgent need to, developmental research of the day by day exhausted of fossil energy and development low-carbon economy has become the key subjects that the world today faces.Biomass energy derives from biomass, because of its wide material sources and reproducible feature, is increasingly paid attention to by domestic and international research worker.
The raw materials for production that biogasoline is main at present are the agriculture waste product of lignocellulose rich content, and production ways is mainly reformed or high temperature pyrolysis by hydrolysis.CN 101671571A discloses a kind of method preparing biogasoline for raw material hydrolysis reformation with lignocellulose-like biomass, and this method is that hydrolysis material liquid is via being filled with catalyst n i/SiO by lignocellulose biomass by hydrolyzation2-Al2O3Low-temperature reformate reactor and be filled with the high temperature reformation catalyst converter of Ni/HZSM-5 and reform, liquid phase i.e. obtains biogasoline after separated.But lignocellulose chemical hydrolysis process is considerably complicated, by-product also has certain side effect to subsequent reformation reaction；Additionally aqueous catalysis reforming system is considerably complicated, and noble metal catalyst is expensive and the life-span is the longest.
5 hydroxymethyl furfural is one of most important derivant of furan ring system it is considered to be a kind of important intermediate substituting chemicals and various fuel.5 hydroxymethyl furfural through chlorine replace after generate 5-chloromethyl furfural, with ethanol stir after 5-ethoxyl methyl furfural.5-ethoxyl methyl furfural is a kind of liquid, boiling point is 235 DEG C, and energy density is 8.8kWh/L, is much higher than ethanol (6.1kWh/L), and the normal benzine that matches in excellence or beauty (8.8kWh/L) and diesel fuel (9.7kWh/L) are it is considered to be a kind of novel alternative fuel.CN 103121984A discloses a kind of method that chitin kind biomass produce 5-hydroxyl furfural, develops the new way that chitin biomass comprehensive utilizes.The raw material of current domestic chitin extraction is mainly the shell of shrimp, Eriocheir sinensis, technique exist the places of origin of raw materials and, the diversity etc. of dispersibility, seasonality, quality, yield is the highest and price the most not under, utilize expensive fine-chemical intermediate to produce biomass energy and clearly attend trifles and neglect essentials.
Chitin kind biomass are the second largest biomass resources that reserves are only second to cellulose, and in microorganism wall, content is the most considerable.Abroad the report for chitin extraction from fungus is more and industrialization, but the most domestic is also not carried out industrialization.China is a large-scale Citric Acid Production state, produces substantial amounts of aspergillus niger waste thallus in production process, and the discharge of these thalline not only can bring the severe contamination of environment, and is the huge waste of biomass resource.
Summary of the invention
It is contemplated that overcome all deficiencies of prior art, provide the preparation method of a kind of novel bio-gasoline, specifically a kind of is raw material by citric acid industry waste thallus, the method preparing biogasoline via chitin, 5 hydroxymethyl furfural, 5-ethoxyl methyl furfural.
The present invention is to be realized by following technical scheme:
A kind of preparation method of novel bio-gasoline, the step including following:
(1) Aspergillus niger 50 ~ 100 DEG C of constant temperature of 1 ~ 10% aqueous hydrochloric acid solution are processed 0.5 ~ 3h, the mass ratio adding waste thallus and hydrochloric acid is 1:2 ~ 4, it is soaked in 90 ~ 100 DEG C of constant temperature in 15%NaOH solution after dehydration and processes 1 ~ 3h deproteinising, the mass ratio adding waste thallus and 15%NaOH solution is 1:2 ~ 4, adds 5%H after being washed till neutrality after dehydration2O2Aqueous solution decolours to obtain chitin；
(2) chitin is joined in 30 ~ 70% solder(ing)acids, adding the aluminum chloride of catalytic amount, aluminum chloride consumption is the 10 ~ 20% of chitin quality, and 60 ~ 100 DEG C of constant temperature process 1 ~ 3h, 5 hydroxymethyl furfural, the equal recovery of zinc chloride, catalyst and petroleum ether are steamed to obtain in petroleum ether extraction, rotation；
(3) joining in ethanol by 5 hydroxymethyl furfural, phosphotungstic acid, phosphotungstic acid consumption is the 2 ~ 30% of 5 hydroxymethyl furfural quality, and 60 ~ 100 DEG C of reaction 6 ~ 15h, reactant liquor rectification obtains 5-ethoxyl methyl furfural；
(4) being blended i.e. obtain biogasoline with ethanol petrol or normal benzine by 5-ethoxyl methyl furfural, mixing proportion is 1:0.1 ~ 10.
Preferably, in the preparation method of above-mentioned novel bio-gasoline, in described step (1), the concentration of aqueous hydrochloric acid solution is 1 ~ 5%, and constant temperature treatment temperature is 60 ~ 90 DEG C, and the process time is 1 ~ 2h.
Preferably, in the preparation method of above-mentioned novel bio-gasoline, in described step (1), NaOH solution treatment temperature is 70 ~ 100 DEG C, and the process time is 1.5 ~ 2h.
Preferably, in the preparation method of above-mentioned novel bio-gasoline, in described step (2), solder(ing)acid concentration is 45 ~ 60%.
Preferably, in the preparation method of above-mentioned novel bio-gasoline, it is characterised in that in described step (2), constant temperature treatment temperature is 70 ~ 90 DEG C, the process time is 1.5 ~ 2h.
Preferably, in the preparation method of above-mentioned novel bio-gasoline, in described step (3), reaction temperature is 80 ~ 90 DEG C, and the response time is 8 ~ 12h.
The preparation method of above-mentioned novel bio-gasoline, detailed step is:
(1) the aspergillus niger waste thallus being dried by 5kg, joins in the aqueous hydrochloric acid solution that 15L concentration is 1%, stirs 1h, then collect solid with centrifuge dewatering under 90 DEG C of constant temperatures；Solids joins in the sodium hydroxide solution that 15L concentration is 15%, boils stirring 1.5h deproteinising, and centrifuge dewatering also cleans to neutral, uses 5% H2O2Aqueous solution decolours to obtain 0.9kg chitin；
(2) 0.9kg chitin is joined in the solder(ing)acid that 150kg mass concentration is 60%, add 0.1kg aluminum chloride, open stirring and keep 90 DEG C of reaction 1.5h, then extract in three times with 300L petroleum ether, extract rotation steam 0.3kg 5 hydroxymethyl furfural, aqueous phase and extractant repeat to apply mechanically；
(3) being joined in 3kg ethanol by 0.3kg 5 hydroxymethyl furfural, add 15g phosphotungstic acid, Distillation recovery unreacted ethanol after constant temperature 80 DEG C reaction 8h, rectification obtains 0.28kg 5-ethoxyl methyl furfural；
(4) 0.28kg5-ethoxyl methyl furfural and 0.28kg normal benzine are blended to obtain novel bio-gasoline.
Technical characterstic and the excellent results of the present invention are as follows:
1, the waste thallus of industry during Aspergillus niger is Citric Acid Production, the waste thallus that the citric acid industry of China is annual the nearlyest million tons, and production site is the most intensive, the present invention can significantly alleviate environmental pollution pressure；
2, chitosan content is in prostatitis in various microorganisms, and aboundresources is cheap；
3, the oxidized zinc solution of chitin, adds trace catalyst and can be converted into 5 hydroxymethyl furfural, equipment and operating procedure simply, and environment-protecting asepsis, catalyst, extractant and reaction medium are the most recyclable to be applied mechanically, and meets Green Chemistry requirement；
4,5 hydroxymethyl furfural is directly etherified under heteropoly acid catalysis, it is to avoid use the organic solvent such as thionyl chloride, DMF, environmental friendliness；
5, biogasoline product energy density is high, and in electromotor, steadily, thoroughly, carbon distribution is few in burning.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further described, in order to those skilled in the art knows more about the present invention, but and is not so limited the present invention.
Embodiment 1
(1) the aspergillus niger waste thallus being dried by 5kg, joins in the aqueous hydrochloric acid solution that 15L concentration is 1%, stirs 1h, then collect solid with centrifuge dewatering under 90 DEG C of constant temperatures；Solids joins in the sodium hydroxide solution that 15L concentration is 15%, boils stirring 1.5h deproteinising, and centrifuge dewatering also cleans to neutral, uses 5% H2O2Aqueous solution decolours to obtain 0.9kg chitin；
(2) 0.9kg chitin is joined in the solder(ing)acid that 150kg mass concentration is 60%, add 0.1kg aluminum chloride, open stirring and keep 90 DEG C of reaction 1.5h, then extract in three times with 300L petroleum ether, extract rotation steam 0.3kg 5 hydroxymethyl furfural, aqueous phase and extractant repeat to apply mechanically；
(3) being joined in 3kg ethanol by 0.3kg 5 hydroxymethyl furfural, add 15g phosphotungstic acid, Distillation recovery unreacted ethanol after constant temperature 80 DEG C reaction 8h, rectification obtains 0.28kg 5-ethoxyl methyl furfural；
(4) 0.28kg5-ethoxyl methyl furfural and 0.28kg normal benzine being blended to obtain novel bio-gasoline, calorific value is 64200kJ/kg, higher than normal benzine (44000kJ/kg).
Embodiment 2
(1) the aspergillus niger waste thallus being dried by 6kg, joins in the aqueous hydrochloric acid solution that 6L concentration is 5%, stirs 1.5h, then collect solid with centrifuge dewatering under 75 DEG C of constant temperatures；Solids joins in the sodium hydroxide solution that 18L concentration is 15%, boils stirring 1.5h deproteinising, and centrifuge dewatering also cleans to neutral, uses 5% H2O2Aqueous solution decolours to obtain 1.1kg chitin；
(2) 1.1kg chitin is joined in the solder(ing)acid that 200kg mass concentration is 50%, add 0.15kg aluminum chloride, open stirring and keep 70 DEG C of reaction 2h.Then extract in three times with 350L petroleum ether, extract rotation steam 0.38kg 5 hydroxymethyl furfural, aqueous phase and extractant repeat to apply mechanically；
(3) being joined in 3kg ethanol by 0.38kg 5 hydroxymethyl furfural, add 19g phosphotungstic acid, Distillation recovery unreacted ethanol after constant temperature 80 DEG C reaction 10h, rectification obtains 0.34kg 5-ethoxyl methyl furfural；
(4) by 1:2 volume ratio, 5-ethoxyl methyl furfural and normal benzine being blended to obtain novel bio-gasoline, calorific value is 47800 kJ/kg, higher than normal benzine.
Embodiment 3
(1) the aspergillus niger waste thallus being dried by 5kg, joins in the aqueous hydrochloric acid solution that 5L concentration is 5%, stirs 1h, then collect solid with centrifuge dewatering under 60 DEG C of constant temperatures；Solids joins in the sodium hydroxide solution that 15L concentration is 15%, boils stirring 1.5h deproteinising, and centrifuge dewatering also cleans to neutral, uses 5% H2O2Aqueous solution decolours to obtain 0.8kg chitin；
(2) 0.8kg chitin is joined in the solder(ing)acid that 150kg mass concentration is 70%, add 0.1kg aluminum chloride, open stirring and keep 90 DEG C of reaction 1.5h, then extract in three times with 300L petroleum ether, extract rotation steam 0.31kg 5 hydroxymethyl furfural, aqueous phase and extractant repeat to apply mechanically；
(3) being joined in 3kg ethanol by 0.31kg 5 hydroxymethyl furfural, add 15g phosphotungstic acid, Distillation recovery unreacted ethanol after constant temperature 90 DEG C reaction 8h, rectification obtains 0.27kg 5-ethoxyl methyl furfural；
(4) 0.27kg5-ethoxyl methyl furfural and 0.27kg normal benzine being blended to obtain novel bio-gasoline, calorific value is 54250kJ/kg, higher than normal benzine.
Embodiment 4
(1) the aspergillus niger waste thallus being dried by 5kg, joins in the aqueous hydrochloric acid solution that 15L concentration is 1%, stirs 2h, then collect solid with centrifuge dewatering under 80 DEG C of constant temperatures；Solids joins in the sodium hydroxide solution that 15L concentration is 15%, constant temperature 90 DEG C stirring 2h deproteinising, and centrifuge dewatering also cleans to neutral, uses 5% H2O2Aqueous solution decolours to obtain 0.92kg chitin；
(2) 0.92kg chitin is joined in the solder(ing)acid that 150kg mass concentration is 45%, add 0.2kg aluminum chloride, open stirring and keep 90 DEG C of reaction 1.5h, then extract in three times with 300L petroleum ether, extract rotation steam 0.26kg 5 hydroxymethyl furfural, aqueous phase and extractant repeat to apply mechanically；
(3) being joined in 3kg ethanol by 0.26kg 5 hydroxymethyl furfural, add 20g phosphotungstic acid, Distillation recovery unreacted ethanol after constant temperature 90 DEG C reaction 12h, rectification obtains 0.29kg 5-ethoxyl methyl furfural；
(4) with normal benzine 10:1 by volume, 0.29kg5-ethoxyl methyl furfural being blended to obtain novel bio-gasoline, calorific value is 54300kJ/kg, higher than normal benzine (44000kJ/kg).
Embodiment 5
(1) the aspergillus niger waste thallus being dried by 5kg, joins in the aqueous hydrochloric acid solution that 12L concentration is 2%, stirs 1.5h, then collect solid with centrifuge dewatering under 90 DEG C of constant temperatures；Solids joins in the sodium hydroxide solution that 15L concentration is 15%, boils stirring 2h deproteinising, and centrifuge dewatering also cleans to neutral, uses 5% H2O2Aqueous solution decolours to obtain 0.94kg chitin；
(2) 0.94kg chitin is joined in the solder(ing)acid that 150kg mass concentration is 60%, add 0.1kg aluminum chloride, open stirring and keep 70 DEG C of reaction 2h, then extract in three times with 300L petroleum ether, extract rotation steam 0.32kg 5 hydroxymethyl furfural, aqueous phase and extractant repeat to apply mechanically；
(3) being joined in 3kg ethanol by 0.32kg 5 hydroxymethyl furfural, add 15g phosphotungstic acid, Distillation recovery unreacted ethanol after constant temperature 75 DEG C reaction 8h, rectification obtains 0.27kg 5-ethoxyl methyl furfural；
(4) with normal benzine 1:3 by volume, 0.27kg5-ethoxyl methyl furfural being blended to obtain novel bio-gasoline, calorific value is 46200kJ/kg, higher than normal benzine (44000kJ/kg).
Claims (6)
1. a preparation method for novel bio-gasoline, the step including following:
(1) Aspergillus niger is used
1 ~ 10% aqueous hydrochloric acid solution 50 ~ 100 DEG C constant temperature processes 0.5 ~ 3h, the mass ratio adding waste thallus and hydrochloric acid is 1:2 ~ 4, it is soaked in 90 ~ 100 DEG C of constant temperature in 15%NaOH solution after dehydration and processes 1 ~ 3h deproteinising, the mass ratio adding waste thallus and 15%NaOH solution is 1:2 ~ 4, adds 5%H2O2 aqueous solution and decolour to obtain chitin after dehydration after being washed till neutrality；
(2) chitin is joined in 30 ~ 70% solder(ing)acids, adding the aluminum chloride of catalytic amount, aluminum chloride consumption is the 10 ~ 20% of chitin quality, and 60 ~ 100 DEG C of constant temperature process 1 ~ 3h, 5 hydroxymethyl furfural, the equal recovery of zinc chloride, catalyst and petroleum ether are steamed to obtain in petroleum ether extraction, rotation；
(3) joining in ethanol by 5 hydroxymethyl furfural, phosphotungstic acid, phosphotungstic acid consumption is the 2 ~ 30% of 5 hydroxymethyl furfural quality, and 60 ~ 100 DEG C of reaction 6 ~ 15h, reactant liquor rectification obtains 5-ethoxyl methyl furfural；
(4) being blended i.e. obtain biogasoline with ethanol petrol or normal benzine by 5-ethoxyl methyl furfural, mixing proportion is 1:0.1 ~ 10.
The preparation method of novel bio-gasoline the most according to claim 1, it is characterised in that in described step (1), the concentration of aqueous hydrochloric acid solution is 1 ~ 5%, constant temperature treatment temperature is 60 ~ 90 DEG C, and the process time is 1 ~ 2h.
The preparation method of novel bio-gasoline the most according to claim 1, it is characterised in that in described step (2), solder(ing)acid concentration is 45 ~ 60%.
The preparation method of novel bio-gasoline the most according to claim 1, it is characterised in that in described step (2), constant temperature treatment temperature is 70 ~ 90 DEG C, the process time is 1.5 ~ 2h.
The preparation method of novel bio-gasoline the most according to claim 1, it is characterised in that in described step (3), reaction temperature is 80 ~ 90 DEG C, the response time is 8 ~ 12h.
6. the preparation method of the novel bio-gasoline described in claim 1, detailed step is:
(1) the aspergillus niger waste thallus being dried by 5kg, joins in the aqueous hydrochloric acid solution that 15L concentration is 1%, stirs 1h, then collect solid with centrifuge dewatering under 90 DEG C of constant temperatures；Solids joins in the sodium hydroxide solution that 15L concentration is 15%, boils stirring 1.5h deproteinising, and centrifuge dewatering also cleans to neutrality, decolours to obtain 0.9kg chitin with 5% H2O2 aqueous solution；(2) 0.9kg chitin is joined in the solder(ing)acid that 150kg mass concentration is 60%, add 0.1kg aluminum chloride, open stirring and keep 90 DEG C of reaction 1.5h, then extract in three times with 300L petroleum ether, extract rotation steam 0.3kg 5 hydroxymethyl furfural, aqueous phase and extractant repeat to apply mechanically；(3) being joined in 3kg ethanol by 0.3kg 5 hydroxymethyl furfural, add 15g phosphotungstic acid, Distillation recovery unreacted ethanol after constant temperature 80 DEG C reaction 8h, rectification obtains 0.28kg 5-ethoxyl methyl furfural；(4) 0.28kg5-ethoxyl methyl furfural and 0.28kg normal benzine are blended to obtain novel bio-gasoline.
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| CN105925336B (en) * | 2016-05-12 | 2018-10-26 | 陕西聚泰新材料科技有限公司 | A kind of biomass composite fuel of high burning efficiency and preparation method thereof |
| CN111057594B (en) * | 2019-12-30 | 2021-10-29 | 李旭 | Preparation method of alcohol-based fuel additive |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974106A (en) * | 2010-11-18 | 2011-02-16 | 天津泰康生物制药有限公司 | Method for extracting chitin by utilizing citric-acid fermentation waste residue |
| CN102453559A (en) * | 2010-10-27 | 2012-05-16 | 中国科学院大连化学物理研究所 | Fuel additive for energy conservation and emission reduction of engine and an application thereof |
| CN102911141A (en) * | 2011-08-05 | 2013-02-06 | 中国科学院大连化学物理研究所 | Method for preparing 5-ethyoxyl methylfurfural |
| CN103121984A (en) * | 2013-02-22 | 2013-05-29 | 中国科学院山西煤炭化学研究所 | Method for producing 5-hydroxymethyl furfural by chitin biomass |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102453559A (en) * | 2010-10-27 | 2012-05-16 | 中国科学院大连化学物理研究所 | Fuel additive for energy conservation and emission reduction of engine and an application thereof |
| CN101974106A (en) * | 2010-11-18 | 2011-02-16 | 天津泰康生物制药有限公司 | Method for extracting chitin by utilizing citric-acid fermentation waste residue |
| CN102911141A (en) * | 2011-08-05 | 2013-02-06 | 中国科学院大连化学物理研究所 | Method for preparing 5-ethyoxyl methylfurfural |
| CN103121984A (en) * | 2013-02-22 | 2013-05-29 | 中国科学院山西煤炭化学研究所 | Method for producing 5-hydroxymethyl furfural by chitin biomass |
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Effective date of registration: 20191114 Address after: 276600 west section of Junan County, Linyi City, Shandong Province, Huaihailu Road Patentee after: Linyi Shinengde Environmental Protection Fuel Chemical Co.,Ltd. Address before: 250000, No. 11, building 2, north section of Qilihe Road, Licheng District, Shandong, Ji'nan Patentee before: Xinghuo Sci. & Tech. Research Inst., Jinan Dev. Zone |
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Effective date of registration: 20200713 Address after: Room 401, unit 2, building 11, No.2, Qilihe Road, Licheng District, Jinan City, Shandong Province 250100 Patentee after: SHANDONG XINGHUO INTELLECTUAL PROPERTY SERVICE Co.,Ltd. Address before: 276600 west section of Junan County, Linyi City, Shandong Province, Huaihailu Road Patentee before: LINYI SHINENGDE ENVIRONMENTAL PROTECTION FUEL CHEMICAL Co.,Ltd. |