CN103421548A - Preparation technology of biodiesel produced from non refined grease - Google Patents
Preparation technology of biodiesel produced from non refined grease Download PDFInfo
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- CN103421548A CN103421548A CN2012101507796A CN201210150779A CN103421548A CN 103421548 A CN103421548 A CN 103421548A CN 2012101507796 A CN2012101507796 A CN 2012101507796A CN 201210150779 A CN201210150779 A CN 201210150779A CN 103421548 A CN103421548 A CN 103421548A
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- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Abstract
The invention discloses a preparation technology of biodiesel produced from non refined grease. The preparation technology comprises the following steps: 1) selecting and using qualified methanol and a catalyst A; 2) adding the catalyst A into the grease, adding excess methanol for a pre-esterification reaction, performing rectification regeneration of gas phase methanol; 3) dissolving an appropriate proportion of a catalyst B in the methanol; 4) performing an ester interchange reaction; 5) performing water washing and liquid separation to remove the catalyst B and glycerin produced by the ester interchange, rectifying and recycling the superfluous methanol to obtain a non-standard product A; 6) obtaining a non-standard product B and tower-bottom heavy oil through vacuum distillation of the non-standard product A; and 7) obtaining a biodiesel product meeting national standard GB/T 20828-2007 by deep deacidification, water washing and dehydration of the non-standard product B. The preparation technology has stable technological processes, and can fully realize recycling of the excess methanol, reuse of soft water and saving of energy and resources. The by-product crude glycerin can be in good abutting joint with a glycerin refining production line, and the by-product tower-bottom heavy oil and waste oil produced by deacidification and the like can be fully recycled, and are of good quality.
Description
Technical field
The present invention relates to a kind of technique of biofuel, by it, relate to a kind of preparation technology who uses non-polished fat production GB biofuel.
Background technology
Biofuel is the lipid acid mono alkyl ester for example, made through transesterify by animal-plant oil and alcohol (methyl alcohol or ethanol), and most typical is fatty acid methyl ester, with BD100, means, carries out national standard GB/T 20828～2007.Biofuel Blended fuel (B5) is carried out national standard GB/T 25199～2010.Biofuel is that a kind of good petrifaction diesel supplements and substitute.
The production methods such as direct mixing method, mini-emulsion process, pyrolysis method and ester-interchange method were once arranged in the evolution of biofuel.Directly mixing and micro emulsifying method are that animal-plant oil is mixed in petrifaction diesel, do not change the chemical composition of grease.The product that pyrolysis method forms does not possess lipid acid mono alkyl ester molecular structure yet.The biofuel product that only has ester-interchange method to produce to meet standard GB/T/T 20828～2007.
Production biofuel methyl alcohol used is the product that meets standard GB/T 338～2004 acceptable end products.
Production biofuel non-refining oil used is all any compound lards that do not reach single animals and plants crude oil, microbial oil, used edible oil, acidification oil, trench wet goods and the various above-mentioned greases of rapeseed oil GB GB 1536～2004 first grade indexs.
Production biofuel grease used has different requirements according to the technique difference.Developed country is used polished fat's production biofuel more.Domesticly for avoiding, with the people, strive grain, with grain, strive ground, abundant inedible oil resources such as use crude oil inferior, sewer oil, acidification oil, crude oil inferior, can be referred to as non-polished fat.Use non-polished fat can reduce production costs to a certain extent and be beneficial to the non-food product direction application of waste oil.
Non-polished fat because the raw material complexity shows as that total amount is abundant, complicated component and quality change more obvious.The impurity such as phosphatide, protein, starch, dust are often contained in non-polished fat; The large water gaging of these impurity absorption, contain again salt and other water miscible impurity in water; Because the difference of hydrolysis degree contains free fatty acids in various degree; Because oxidative rancidity, enzyme or microbial process degree of decomposition difference contain small molecules aldehyde, ketone, the aobvious sordes matter of acids; Because of the similar various oil soluble impurity with component that mixes; Because of emulsification and surface-active substance assorted with the glue of different profit amphiphilics etc. again.Non-polished fat is all mixtures of more complicated of form component.
The suitable exploitation of non-polished fat enters the energy utilization direction, the production biofuel.Also have problems and take the technique that non-polished fat is raw material production GB biofuel in prior art, as stable not as technological process, quality is bad, and raw material availability is not high.
Summary of the invention
For overcoming the deficiency on prior art, the object of the invention is to provide a kind ofly take non-polished fat and is that raw material is the preparation technology of non-polished fat production biofuel through the preparation method of pre-esterification, transesterification reaction degree of depth depickling production GB biofuel, non-polished fat can be required to produce nonstandard product A, nonstandard product B according to concrete production cost and purpose and in strict conformity with the biofuel product of standard GB/T/T 20828～2007, its stable technical process, fully realize recovery, the soft water reuse of excessive methanol, the saving of the energy and resource.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows:
It is that processing step of the present invention is as follows that the present invention solves the technical scheme that its technical problem takes:
The first step, selecting non-polished fat is raw material, and by the pre-treatment of stock oil appropriateness, select qualified methyl alcohol and catalyst A;
Second step, will add catalyst A in grease, and pass into excessive methanol and carry out pre-esterification reactor, and by the gas-phase methanol rectifying of the water entrainment steam of discharge regeneration;
The 3rd step, by the standing excision acid sludge of the grease after pre-esterification, and adjust to suitable temperature, simultaneously separately by the catalyst B of suitable proportion and dissolve with methanol, and adjusts to suitable temperature;
The 4th step is carried out transesterification reaction by grease and the catalyst B and the methanol solution that prepare under conditions suitable;
The 5th step is washed and separatory is removed the glycerine of catalyst B and transesterify generation, and unnecessary methyl alcohol is given to the rectifying recovery, obtains nonstandard product A;
The 6th step, nonstandard product A vacuum distilling obtains heavy oil at the bottom of nonstandard product B and tower;
The 7th step, obtain the biofuel product in strict conformity with standard GB/T/T20828～2007 to the depickling of the nonstandard product B degree of depth, washing, dehydration.
In the above-mentioned the first step, described methyl alcohol is the product that meets standard GB/T 338～2004 acceptable end products, and consumption is that grease per ton drops into 300～450 kilograms, approximately 130～160 kilograms of actual consumptions; The grease of any mixing that described non-refining oil is all single animals and plants crude oil, microbial oil, used edible oil, acidification oil, sewer oil and various above-mentioned greases that do not reach rapeseed oil GB GB 1536～2004 first grade indexs.
In the above-mentioned the first step, the methyl alcohol that the catalyst B of described suitable proportion and methyl alcohol are mass percent 6.3%～6.5% catalyst B and mass percent 30%.Equal 58 ℃～62 ℃ of described suitable temperature and suitable temperature.
Described catalyst A is selected the vitriol oil that meets standard GB/T/T 534～2002 industrial sulphuric acid salable product, and consumption is; Described catalyst B is selected the solid sodium hydroxide that meets standard GB/T 209～2006 IS～DT I premium grads.
Raw materials pretreatment refers to that various stock oil stores standing classification naturally, and excision water and greasy filth, solid slag etc. are impurity obviously.Stock oil is the standing sufficiently long time in storage tank, and heavy impurity can be deposited in pot bottom gradually, and appropriateness is heated can be more obvious.
Pre-esterification reactor is that in grease, lipid acid and methyl alcohol generate the process of fatty acid methyl ester and water under catalyst action, water is taken out of by excessive methanol gas in the mode of steam, make the balance of reversible reaction to the direction skew that generates fatty acid methyl ester, and create anhydrous condition for follow-up transesterification reaction.Pre-esterification reactor can be the solid acid sludge by a large amount of impurity conversion such as glue are assorted simultaneously, and grease is realized to a large amount of removing impurities processes.
Transesterification reaction is reversible reaction, thus at methyl alcohol under excessive condition during molecular balance triglyceride level also can't all be converted into fatty acid methyl ester.Thoroughly to remove the nonstandard product A obtained after catalyzer and glycerine dehydration be that fatty acid methyl ester surpasses 85% but still the mixing oil product that contains a small amount of unconverted triglyceride level, Tegin 55G, two sweet esters and other oil soluble impurities in washing.Nonstandard product A outward appearance brown is opaque, viscosity is low, good fluidity, can be as oil fuel or the composition be in harmonious proportion as thick fuel.
Transesterification reaction is that reversible reaction also shows after transesterify that needing first to wash separatory reclaims excessive methanol again.If directly the mixture after transesterify is reclaimed to methyl alcohol, can make the concentration of catalyzer raise rapidly, cause the side reaction aggravation, saponification is serious, and whole one-tenth is gelatin, can't continue the back operation.
The nonstandard product B main component that nonstandard product A vacuum distilling obtains is fatty acid methyl ester, but in vacuum distillation process, excess Temperature unavoidably can cause the partial fatty acid methyl esters to decompose, produce a small amount of lipid acid, causes acid number to raise.Nonstandard product B, except containing as broad as long with the GB biofuel the 1% left and right lipid acid of having an appointment, shows as acid number and surpasses 0.8, and generally, in 1 to 3 scope, all the other indexs are all in GB biofuel scope.
At the bottom of the tower that nonstandard product A vacuum distilling obtains, heavy oil is mainly polymkeric substance, oil soluble impurity of molecular weight is large, boiling point is high sweet three esters, DAG, a sweet ester and a small amount of grease etc., black non transparent, viscosity is larger, normal temperature can flow, can make plant asphalt or mix and make oil fuel with petrochemical industry residual oil, also can mix multifuel combustion in coal.The waste oil that depickling etc. obtain is mainly mixed fatty acid, fatty acid methyl ester admixture, but the production of biodiesel raw material is done in reuse.Vacuum distilling is the most concentrated part of this process energy consumption, is about 60% of total energy consumption.
Select 304 material stainless steels to build production line to reduce the pollution to oil product such as iron ion, cupric ion.
The catalyst A that the present invention uses is selected the vitriol oil that meets standard GB/T/T 534～2002 industrial sulphuric acid salable product, and catalyst B is selected the solid sodium hydroxide that meets standard GB/T 209～2006 IS～DT I premium grads.Other catalyzer that reach similar or better catalysis efficiency also can adopt.
The technology such as the good catalyzer be associated, equipment, automatization control can be well compatible in corresponding technique.
The effect that the present invention is useful is: the present invention can require to produce nonstandard product A, nonstandard product B according to concrete production cost and purpose by non-polished fat and in strict conformity with the biofuel product of standard GB/T/T 20828～2007; Its stable technical process, fully realize recovery, the soft water reuse of excessive methanol, the saving of the energy and resource; And the raw glycerine of by-product, the production line of fine docking purification of glycerin; At the bottom of the tower of by-product, the waste oil of the discharges such as heavy oil, depickling all fully reclaims, and quality is good, does not waste raw material.
The accompanying drawing explanation
Fig. 1 is process flow diagram of the present invention.
Embodiment
The present invention will be further described in conjunction with the embodiments.
Embodiment:
Referring to Fig. 1, the present invention be take non-polished fat as the pre-esterification of raw material warp, the preparation method of transesterification reaction degree of depth depickling production GB biofuel is the preparation technology of non-polished fat production biofuel, non-polished fat can be required to produce nonstandard product A according to concrete production cost and purpose, nonstandard product B and in strict conformity with the biofuel product of standard GB/T/T 20828～2007, non-polished fat warehouse-in, in oil reservoir or tank, heat or natural subsidence, first fully excise greasy filth before entering reactor, sewage, residue etc., these impurity mix in coal does fuel, for production line heat energy.It is as follows that it possesses operating procedure:
The oil that excised impurity is introduced to reactor, open and stir and self-circulation, the heating of thermal oil chuck.Heat up after 120 ℃ and start to pass into continuously methyl alcohol, speed is 3%～7% oil heavy per hour (the most suitable with 4%～6%), after the gas-phase methanol of top water entrainment steam out and the heat exchange of charging cold methanol, enters the methanol rectification recovery unit.Add the catalyst A that oil and mass percent are 0.8%～1.2% after passing into methyl alcohol and starting, heat up 140 ℃～160 ℃ rapidly, acid number of sampling and measuring per hour after 2, acid number drops to below 2 and stops passing into methyl alcohol, stop stirring, self-circulation and heating, standing sedimentation 30min discharges acid sludge at the bottom of still.Within general 2～4 hours, can complete pre-esterification reactor.Acid sludge can be used as solid waste, mixes with slag and does the building materials use.
Remove after the pre-esterification of acid sludge grease through interchanger temperature adjustment to 58 ℃～62 ℃, enter ester interchange vessel.Be that 50 ℃～55 ℃ dissolving oil and mass percent are 6.3%～6.5% catalyst B by the methyl alcohol of oil quality per-cent 30%, temperature, add in 55 ℃～60 ℃ oil, stir the high-shear self-circulation and carry out the normal pressure transesterification reaction 30～45 minutes.Transesterification reaction is no more than the methyl alcohol boiling point, and the condensing reflux measure is arranged, and prevents that the methyl alcohol loss from changing material concentration and ratio, the side reaction aggravation.Add afterwards the soft water (can be the soft water that subsequent handling reclaims) of 15%, 45 ℃～55 ℃ of oil quality to stir separatory after abundant layering in standing 60 minutes 5 minutes.By the thick methyl esters in upper strata and lower coarse glycerine flash distillation dealcoholysis, the methyl alcohol of deviating from enters methanol rectifying tower regeneration, and is back to the transesterification reaction of front.Raw glycerine after dealcoholysis enters the glycerol production line.Thick methyl esters pumping water ratio after dealcoholysis, lower than 0.05%, is qualified nonstandard product A.Nonstandard product A can store in batches, also can enter subsequent handling production.Every 1.02 tons of stock oils can obtain approximately 1 ton of nonstandard product A.
Nonstandard product A does thermal source (240 degrees centigrade～280 ℃) at high vacuum (0.09MPa～absolute pressure) and thermal oil and carries out the vacuum distilling operation through vacuum tower, separate and thoroughly be not converted into the composition of fatty acid methyl ester, obtain take fatty acid methyl ester as the main nonstandard product B containing 1% free fatty acids of having an appointment.Nonstandard product B can store in batches.Every 1 ton of nonstandard product A can obtain 0.82～0.95 ton of nonstandard product B.Vacuum distillation process is not added any other material.Because of the quality of stock oil does not herewith walk distillation yield also can be different.
Nonstandard product B removes the lipid acid of excess with reference to the alkali-refining deacidification technique in the refining raw food oil process.Because of the integrated artistic parameter stability, the sodium hydroxide solution that available soft water preparation contains 10%w, add 40 ℃ to 50 ℃ depicklings in nonstandard product B to scale under whipped state.Nonstandard product B viscosity is far below edible oil, stirs 10 minutes after adding alkali lye, standing 30 minutes can natural subsidence soap group.Can first excise and concentrate soap group at the depickling still cone end, enter afterwards the de-soap of the disk centrifugal separator degree of depth.Oil product after the de-soap of whizzer washs online with 40 ℃～50 ℃ soft water of 5%w in static mixer, and the cone tank is settlement separate, by cutting water, removes remaining micro-soap.Oil product after washing enters 80 ℃～100 ℃, flash-evaporation dehydration tower and removes residual water-content, can obtain meeting fully the biofuel product of national standard, the quality inspection warehouse-in.Initial stage tower not yet equilibrium establishment time dehydration does not thoroughly return and again dewaters or drain into the sump oil system by the sump oil line.Portioned product can be according to specifically needing to add antioxidant and crystallizing inhibitor or other oil dopes to improve some concrete property.
Production process is noted soft water, methyl alcohol reuse, and the recovery of energy and ladder are used.At the bottom of the sump oil of discharge and tower, heavy oil is all the very good materials with non-refining oil production biofuel.Raw glycerine color depth content is lower, for the production of refining glycerine, need carry out technical and economic evaluation.The sewage of waste oil recovery enters the sewage works deep purifying, and nonproductive direction is used.
As the non-polished fat of production biofuel, suitable employing is compatible strong, adjusts flexible, reliable and stable explained hereafter GB biofuel.This kind of raw materials technology strong adaptability, energy-conserving and environment-protective, process stabilizing, product with stable quality, production process easily embodies synthesization, maximization, automatization, be convenient to efficient energy-saving production, the appearing technique superiority in economy, and food safety is had to certain promotion, for good approach has been opened up in the waste grease harmless treatment.
No matter the non-polished fat of any quality, all be applicable to this explained hereafter GB biofuel.This technique fully adapts to the compatibility of raw material, and production process is energy-conservation, efficient, environmental protection, and the high-quality products production of staircase.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes specification sheets of the present invention and accompanying drawing content to do; or directly or indirectly be used in other relevant technical fields, all in like manner be included in scope of patent protection of the present invention.
Claims (10)
1. the preparation technology of a non-polished fat production biofuel, it is characterized in that: its processing step is as follows:
The first step, selecting non-polished fat is raw material, and by the pre-treatment of stock oil appropriateness, select qualified methyl alcohol and catalyst A;
Second step, will add catalyst A in grease, and pass into excessive methanol and carry out pre-esterification reactor, and by the gas-phase methanol rectifying of the water entrainment steam of discharge regeneration;
The 3rd step, by the standing excision acid sludge of the grease after pre-esterification, and adjust to suitable temperature, simultaneously separately by the catalyst B of suitable proportion and dissolve with methanol, and adjusts to suitable temperature;
The 4th step is carried out transesterification reaction by grease and the catalyst B and the methanol solution that prepare under conditions suitable;
The 5th step is washed and separatory is removed the glycerine of catalyst B and transesterify generation, and unnecessary methyl alcohol is given to the rectifying recovery, obtains nonstandard product A;
The 6th step, nonstandard product A vacuum distilling obtains heavy oil at the bottom of nonstandard product B and tower;
The 7th step, carry out degree of depth depickling, washing, dehydration to nonstandard product B and obtain the biofuel product in strict conformity with standard GB/T/T20828～2007.
2. the preparation technology of a kind of non-polished fat according to claim 1 production biofuel, it is characterized in that: in the above-mentioned the first step, described methyl alcohol is the product that meets standard GB/T 338～2004 acceptable end products, consumption is that grease per ton drops into 300～450 kilograms, approximately 130～160 kilograms of actual consumptions; The grease of any mixing that described non-refining oil is all single animals and plants crude oil, microbial oil, used edible oil, acidification oil, sewer oil and various above-mentioned greases that do not reach rapeseed oil GB GB 1536～2004 first grade indexs.
3. the preparation technology of a kind of non-polished fat according to claim 1 production biofuel, it is characterized in that: in the above-mentioned the first step, the methyl alcohol that the catalyst B of described suitable proportion and methyl alcohol are mass percent 6.3%～6.5% catalyst B and mass percent 30%.
4. according to the preparation technology of the described a kind of non-polished fat of claim 1 or 3 production biofuel, it is characterized in that: described catalyst A is selected the vitriol oil that meets standard GB/T/T 534～2002 industrial sulphuric acid salable product, and consumption is; Described catalyst B is selected the solid sodium hydroxide that meets standard GB/T 209～2006 IS～DT I premium grads.
5. according to the preparation technology of the described a kind of non-polished fat of claim 1 or 3 production biofuel, it is characterized in that: in above-mentioned the 3rd step, equal 58 ℃～62 ℃ of described suitable temperature and suitable temperature.
6. the preparation technology of a kind of non-polished fat according to claim 1 production biofuel, it is characterized in that: in above-mentioned second step, the temperature of described pre-esterification is 140 ℃～160 ℃, normal pressure; 55 ℃～60 ℃ of the temperature of transesterify, normal pressure.
7. the preparation technology of a kind of non-polished fat according to claim 1 production biofuel, it is characterized in that: in above-mentioned the 6th step, nonstandard product A does thermal source at high vacuum and thermal oil and carries out the vacuum distilling operation through vacuum tower, separate and thoroughly be not converted into the composition of fatty acid methyl ester, obtain nonstandard product B; The vacuum tightness of described vacuum distilling is-0.09MPa～absolute pressure that the temperature of described thermal source is 240 ℃～280 ℃.
8. according to the preparation technology of the described a kind of non-polished fat of claim 1 or 7 production biofuel, it is characterized in that: the main component of described nonstandard product B is fatty acid methyl ester.
9. the preparation technology of a kind of non-polished fat according to claim 1 production biofuel, it is characterized in that: in above-mentioned the 7th step, to the sodium hydroxide solution of degree of depth deacidifying process for the soft water preparation, containing 10%w of nonstandard product B, under whipped state, adding to scale in nonstandard product B is 40 ℃～50 ℃ lower depicklings in temperature.
10. the preparation technology of a kind of non-polished fat according to claim 9 production biofuel, it is characterized in that: in above-mentioned the 7th step, the technique of described washing, dehydration is:
Stir 10 minutes add alkali lye after the depickling of the nonstandard product B degree of depth after, within standing 30 minutes, get final product natural subsidence soap group; First excise and concentrate soap group at the depickling still cone end, enter afterwards the de-soap of the disk centrifugal separator degree of depth; Oil product after the de-soap of whizzer washs online with 40 ℃～50 ℃ soft water of 5%w in static mixer, and the cone tank is settlement separate, by cutting water, removes remaining micro-soap; Oil product after washing enters 80 ℃～100 ℃, flash-evaporation dehydration tower and removes residual water-content, can obtain meeting fully the biofuel product of national standard.
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Cited By (6)
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| CN104560411A (en) * | 2014-12-23 | 2015-04-29 | 丹阳市助剂化工厂有限公司 | Technique for preparing fatty acid methyl ester by biological process |
| CN104611072A (en) * | 2015-01-15 | 2015-05-13 | 首钢环境产业有限公司 | Method for preparing biodiesel from gutter oil |
| CN105542894A (en) * | 2016-01-22 | 2016-05-04 | 陕西德融新能源股份有限公司 | Adhesive used for biomass solid fuel |
| CN105861164A (en) * | 2016-05-03 | 2016-08-17 | 陕西德融新能源股份有限公司 | Technology for producing biodiesel from non-refined fat with no catalyst |
| CN106811308A (en) * | 2016-12-23 | 2017-06-09 | 惠州市鑫隆环保科技有限公司 | A kind of preparation method of industrial fuel oil |
| CN111019720A (en) * | 2019-12-31 | 2020-04-17 | 浙江卓尚环保能源有限公司 | Green production process of biodiesel |
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| CN111019720A (en) * | 2019-12-31 | 2020-04-17 | 浙江卓尚环保能源有限公司 | Green production process of biodiesel |
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Application publication date: 20131204 |