CN102952000A - Refining process of biodiesel byproduct crude glycerol - Google Patents
Refining process of biodiesel byproduct crude glycerol Download PDFInfo
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- CN102952000A CN102952000A CN2012104152911A CN201210415291A CN102952000A CN 102952000 A CN102952000 A CN 102952000A CN 2012104152911 A CN2012104152911 A CN 2012104152911A CN 201210415291 A CN201210415291 A CN 201210415291A CN 102952000 A CN102952000 A CN 102952000A
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- glycerine
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- crude glycerin
- biodiesel byproduct
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
Abstract
The present invention provides a refining process of biodiesel byproduct crude glycerol, and relates to the technical field of chemical product production. The refining process includes diluting, desalting, removing impurity, distilling, decoloring and deflavouring. The high-quality refined glycerine is produced by employing the technologies of sodium oxalate complexing impurity removal and active carbon decoloring and deflavouring. The refining process is simple, high in glycerin yield, high in finished refined glycerin purity, and good in product quality.
Description
Technical field
The present invention relates to the Chemicals production technical field, relate in particular to the glycerol being as byproduct of biology process for refining.
Background technology
In recent years along with domestic and international biofuel investment fever heats up rapidly, when yield of biodiesel significantly improves, also by-product a large amount of raw glycerines.As the Main By product glycerine of production of biodiesel process, ten tons of biofuel of every production, just about one ton of raw glycerine of by-product.Along with the day by day exhaustion of petroleum resources and increasing the weight of of environmental pollution, select clean reproducible energy to become the emphasis of current energy research, biofuel is a kind of petrifaction diesel substitute products of high-quality, with its friendly and recyclability to environment, has obtained world's extensive concern.One of subject matter that present stage development biofuel faces is to reduce production costs, and one of its approach, is that the glycerine to the production of biodiesel byproduct in process is taken full advantage of.Glycerine can be used as GC stationary liquid, also can be used as solvent, tenderizer, antibiotic fermentation nutrition agent, siccative etc., glycerine after refining not only can be widely used in food, medical field, can also prepare 1, the organic intermediates such as ammediol, (such as makeup, resin etc.) have important effect in Polymer Synthesizing.The byproduct raw glycerine that general prior art production biofuel obtains, color is dark, and impurity is many, refining difficulty, quality of finished is not high.
Summary of the invention
The object of the invention is to, present situation for a large amount of raw glycerines of above-mentioned production biodiesel byproduct, for taking full advantage of better resource, a kind of biodiesel byproduct product refining crude glycerin technique is disclosed, comprise and adopt the technology such as sodium oxalate complexing impurity elimination, activated carbon decolorizing de-taste, produce high-quality refining glycerine.
The objective of the invention is to realize by following technical solution:
A kind of biodiesel byproduct product refining crude glycerin technique comprises following processing step:
A. dilution
Take production biofuel gained byproduct crude glycerin, add the thinner dilution of raw glycerine weight 10%～30%;
B. desalination
Get the dilution raw glycerine, be neutralized to pH value 5～7, be heated to 70 ℃～80 ℃ temperature, stir 50min～60min, then carry out centrifugation, obtain three layers of liquid: the upper strata is croude fatty acids, the middle level is glycerine, water and a small amount of methyl alcohol, lower floor is salt and by-product soap, gets mixture degassed drying in rotatory evaporator in middle level, obtains desalination glycerine;
C. impurity elimination
Get desalination glycerine, adding massfraction is that 0.02%～0.03% sodium oxalate stirs, and the control temperature is 70 ℃～80 ℃, and mixing time 30min～70min refilters and removes impurity, gets impurity elimination glycerine;
D. distillation
First impurity elimination glycerine is carried out normal pressure and heat and steam methyl alcohol and most of moisture, then be warming up to 164 ℃～204 ℃ distillations and collect glycerol semi-final product;
E. decolouring de-tastes
Get glycerol semi-final product, and get the gac of glycerine weight 0.3%～1.3%, minute 2 addings, circulation decolouring under 70 ℃～80 ℃ temperature, bleaching time 30min～60min obtains finished product glycerine.
Described a kind of biodiesel byproduct product refining crude glycerin technique, it is characterized in that: the described thinner that adopts in the described A. dilution technique step is methyl alcohol or ethanol.
Described a kind of biodiesel byproduct product refining crude glycerin technique is characterized in that: in B. desalinating process step, and the neutralization of adopting phosphoric acid to dilute raw glycerine.
Described a kind of biodiesel byproduct product refining crude glycerin technique is characterized in that: in B. desalinating process step, the first process condition is heated to 70 ℃ of temperature for the dilution raw glycerine is neutralized to pH value 5, stirs 60min.
Described a kind of biodiesel byproduct product refining crude glycerin technique, it is characterized in that: in C. impurity elimination processing step, the first process condition is that 0.03% sodium oxalate stirs for add massfraction in desalination glycerine, and the control temperature is 80 ℃, mixing time 30min refilters and removes impurity.
Described a kind of biodiesel byproduct product refining crude glycerin technique, it is characterized in that: described D. distil process step, adopt flash evaporation technology to carry out the low-flash of glycerine high vacuum, flash vaporization point is 140 ℃～160 ℃, flashing pressure is 30KPa, obtains glycerol semi-final product.
Described a kind of biodiesel byproduct product refining crude glycerin technique is characterized in that: described E. decolouring de-tastes processing step, adopts resin bed and nonpolar macroporous adsorption resin, carries out the glycerol semi-final product decolouring and de-tastes, and obtains finished product glycerine.
A kind of biodiesel byproduct product refining crude glycerin technique of the present invention comprises technology such as adopting sodium oxalate complexing impurity elimination, activated carbon decolorizing, produces high-quality refining glycerine, processing method is simple, the glycerine yield is high, and gained finished product refining glycerine purity is high, and quality is good.
The present invention is further described below in conjunction with drawings and Examples, purpose of the present invention, advantage and disadvantage, and the non-limitative illustration by following preferential embodiment makes an explanation.
Description of drawings
Accompanying drawing is biodiesel byproduct product refining crude glycerin processing step block diagram of the present invention.
Embodiment
Embodiment one
Biodiesel byproduct product refining crude glycerin technique of the present invention comprises the following methods step successively:
A. dilution
The production biofuel gained byproduct crude glycerin that purification of glycerin of the present invention adopts, owing to carry the compounds such as a small amount of biofuel, methyl alcohol, unreacted catalyzer sodium methylate and by-product soap secretly, mix the agglutination body, for improving the separating effect of raw glycerine and foreign material, generally can add methyl alcohol or ethanol dilutes, add methyl alcohol or alcohol dilution agent weight is 10%～30% of raw glycerine weight.Present embodiment adopts methyl alcohol as thinner, and adding weight is the methyl alcohol of raw glycerine weight 25%, fully stirs, and raw glycerine is diluted.Owing to contain a small amount of methyl alcohol in the raw glycerine, adopt and make thinner with methyl alcohol, if in the time of more can avoiding with ethanol as solvent, have methyl alcohol in the ethanol that reclaims and exist, make the ethanol recycling difficulty increase of recovery.
B. desalination
Under alkaline condition, glycerine, soap, methyl alcohol and methyl esters mix the agglutination body, separate them one by one, and be very difficult with sedimentation or centrifuging, disengaging time can be very long, but also can in following process, can bring serious etching problem, and need with acid it to be neutralized to suitable pH value about 6, make sodium methylate and soap generate salt and lipid acid, then according to different densities, adopt centrifuging to separate and remove, good separating effect not only, disengaging time is also shorter.
It is stand-by that present embodiment is got the dilution raw glycerine, adding weight is 85% phosphoric acid solution of raw glycerine weight 8%～12%, be neutralized to suitable pH value about 6, be heated to 60 ℃～80 ℃ temperature, stirred 40min(minute)～60min, then carry out centrifugation, obtain three layers of liquid: the upper strata is croude fatty acids, the middle level is glycerine, water and a small amount of methyl alcohol, and lower floor is phosphoric acid salt and by-product soap.Get mixture degassed drying in rotatory evaporator in middle level, obtain desalination glycerine.
The temperature of reaction (A) of raw glycerine neutralization reaction orthogonal experiment, reaction times (B), pH value (C) horizontal factor see Table 1, and Orthogonal experiment results sees Table 2.
The horizontal factor of table 1 raw glycerine neutralization reaction
Annotate: A is that temperature of reaction .B is that reaction times .C is pH value, lower same.
The Orthogonal experiment results of table 2 raw glycerine neutralization reaction
Annotate: K in the upper table
1, K
2, K
3Be the mean value of each level experiment, R is extreme difference.Analyzed as can be known by table 2, the neutralization reaction temperature has the greatest impact to the glycerol semi-final product yield, secondly is the reaction times, and the impact of pH value is less.Optimum reaction condition is A2, B3, C1, and namely temperature of reaction is 70 ℃, reaction times 60min, and pH value 5, with this understanding, the yield of glycerol semi-final product is 81.2%.Secondly, reaction conditions is for being A3, B3, C2 and A2, B2, C3, and namely temperature of reaction is 80 ℃, reaction times 60min, 70 ℃ of pH value 6 and temperature of reaction, reaction times 50min, pH value 7.Under its reaction conditions, the yield of glycerol semi-final product is respectively 77.4 and 76.5%.Comprehensive each practical factor, drafting temperature of reaction is 70 ℃～80 ℃, and the reaction times is 50min～60min, and it is 5～7 that the pH value is then relaxed.
C. impurity elimination
The present embodiment by-product glycerol of biological diesel oil forms more complicated, in order to obtain the higher glycerine of purity, adopt the method that adds Soluble oxalate sodium static mixing, filters impurity elimination, and the massfraction (C ') that adds with temperature of reaction (A '), mixing time (B ') and sodium oxalate obtains best removing impurities condition as the investigation factor according to orthogonal experiment method.The horizontal factor of removing impurities reaction sees Table 3, and Orthogonal experiment results sees Table 4.
The horizontal factor of table 3 sodium oxalate removing impurities reaction
The Orthogonal experiment results of table 4 sodium oxalate removing impurities reaction
Annotate: K in the upper table
1, K
2, K
3Be the mean value of each level experiment, R ' is extreme difference.
Analyze as can be known from table 4, when adopting sodium oxalate complexing impurity elimination, temperature of reaction has the greatest impact to impurity-removing rate, secondly is that sodium oxalate adds massfraction.Optimum reaction condition is A ' 3, B ' 1, C ' 3, and namely temperature of reaction is 80 ℃, mixing time 30min, the massfraction 0.03% that sodium oxalate adds.Under top condition, the impurity-removing rate of glycerine reaches 19.8%.Secondly, reaction conditions is A ' 2, B ' 2, C ' 3 and A ' 3, B ' 3, C ' 2, be 70 ℃ of temperature of reaction, mixing time 50min, 80 ℃ of the massfraction 0.03% that sodium oxalate adds and temperature of reaction, mixing time 70min, the massfraction 0.02% that sodium oxalate adds, the impurity-removing rate of impurity elimination glycerine oil reaches respectively 17.3% and 17.2%.Comprehensive each practical factor is drafted 70 ℃～80 ℃ of temperature of reaction, mixing time 30min～70min, and it is 0.02%～0.03% that sodium oxalate adds massfraction.
D. distillation
Because the glycerine boiling point is high, be 290 ℃ under normal pressure, glycerine begins gasification in the time of 164 ℃, and glycerine namely begins to occur decomposition and aggregation at 204 ℃.For avoiding loss, purification of glycerin adopts reduced pressure distillation process, first impurity elimination glycerine is carried out the normal pressure distillation of heating, and steams methyl alcohol and most of moisture, then heats up to distill and collects 164 ℃～204 ℃ cut glycerine.
E. decolouring de-tastes
Former process gained glycerol semi-final product is little yellow, and slight peculiar smell is arranged, and has more preferably vision, sense of taste sensation for making finished product glycerine, can further de-taste the cut glycerin decoloring.Glycerine has larger polarity, and is respond well take gac as discoloring agent.Because gac is non-polar adsorbent, a little less than its lyosorption very for polarity, and the polarity of sample and impurity is general all less than the polarity of water, so can be subject to stronger absorption.
The glycerine that distills out after processing with sodium oxalate is faint yellow, available activated carbon decolorizing.Get the gac of glycerine weight 0.3%～1.3%, minute 2 addings, circulation decolouring under 70 ℃～80 ℃ temperature, bleaching time 30min～60min.Obviously peculiar smell, sticky shape, purity are the refining finished product glycerine more than 99.5% to obtain water white transparency, nothing through activated carbon decolorizing.
The above-mentioned embodiment that enumerates is as an illustration example only, is not the restriction that the present invention is done.The present invention can also adopt alternate manner to implement, for example, in D. distil process step, adopt flash evaporation technology, carry out the low-flash of glycerine high vacuum, flash vaporization point is 140 ℃～150 ℃, and flash distillation (tank) pressure is 30KPa(kPa), avoid heat-sensitive substance glycerine, under long-time high temperature, polymerism can occur; De-taste processing step in E. decolouring, except the employing activated carbon decolorizing de-tastes the technique, also can adopt resin bed and nonpolar macroporous adsorption resin, Adsorption glycerine pigment and other impurity technique are this superfluous stating one by one not.In every case adopt the technical scheme that is equal to replacement or equivalent transformation formation, all belong to the protection domain of requirement of the present invention.
Claims (7)
1. biodiesel byproduct product refining crude glycerin technique comprises following processing step:
A. dilution
Take production biofuel gained byproduct crude glycerin, add the thinner dilution of raw glycerine weight 10%～30%;
B. desalination
Get the dilution raw glycerine, be neutralized to pH value 5～7, be heated to 70 ℃～80 ℃ temperature, stir 50min～60min, then carry out centrifugation, obtain three layers of liquid: the upper strata is croude fatty acids, the middle level is glycerine, water and a small amount of methyl alcohol, lower floor is salt and by-product soap, gets mixture degassed drying in rotatory evaporator in middle level, obtains desalination glycerine;
C. impurity elimination
Get desalination glycerine, adding massfraction is that 0.02%～0.03% sodium oxalate stirs, and the control temperature is 70 ℃～80 ℃, and mixing time 30min～70min refilters and removes impurity, gets impurity elimination glycerine;
D. distillation
First impurity elimination glycerine is carried out normal pressure and heat and steam methyl alcohol and most of moisture, then be warming up to 164 ℃～204 ℃ distillations and collect glycerol semi-final product;
E. decolouring de-tastes
Get glycerol semi-final product, and get the gac of glycerine weight 0.3%～1.3%, minute 2 addings, circulation decolouring under 70 ℃～80 ℃ temperature, bleaching time 30min～60min obtains finished product glycerine.
2. a kind of biodiesel byproduct product refining crude glycerin technique according to claim 1, it is characterized in that: the described thinner that adopts in the described A. dilution technique step is methyl alcohol or ethanol.
3. a kind of biodiesel byproduct product refining crude glycerin technique according to claim 1 is characterized in that: in B. desalinating process step, and the neutralization of adopting phosphoric acid to dilute raw glycerine.
4. a kind of biodiesel byproduct product refining crude glycerin technique according to claim 1 is characterized in that: in B. desalinating process step, the first process condition is heated to 70 ℃ of temperature for the dilution raw glycerine is neutralized to pH value 5, stirring 60min.
5. a kind of biodiesel byproduct product refining crude glycerin technique according to claim 1, it is characterized in that: in C. impurity elimination processing step, the first process condition is that 0.03% sodium oxalate stirs for add massfraction in desalination glycerine, the control temperature is 80 ℃, mixing time 30min refilters and removes impurity.
6. a kind of biodiesel byproduct product refining crude glycerin technique according to claim 1, it is characterized in that: described D. distil process step, adopt flash evaporation technology to carry out the low-flash of glycerine high vacuum, flash vaporization point is 140 ℃～160 ℃, flashing pressure is 30KPa, obtains glycerol semi-final product.
7. a kind of biodiesel byproduct product refining crude glycerin technique according to claim 1 is characterized in that: described E. decolouring de-tastes processing step, adopts resin bed and nonpolar macroporous adsorption resin, carries out the glycerol semi-final product decolouring and de-tastes, and obtains finished product glycerine.
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| CN103274900A (en) * | 2013-06-07 | 2013-09-04 | 文建方 | Method for extracting glycerol from biodiesel wastewater |
| CN103626632A (en) * | 2013-12-24 | 2014-03-12 | 青岛福瑞斯生物能源科技开发有限公司 | Method for purifying by-product crude glycerine of biodiesel prepared by using illegal cooking oil |
| CN104230046A (en) * | 2014-08-21 | 2014-12-24 | 波鹰(厦门)科技有限公司 | Device for separating sodium chloride and glycerinum in high-salinity glycerinum-containing high and advanced organic wastewater |
| CN104262101A (en) * | 2014-10-16 | 2015-01-07 | 佛山市天晟隆油脂化工有限公司 | Glycerine refining method |
| CN104262104A (en) * | 2014-10-16 | 2015-01-07 | 佛山市天晟隆油脂化工有限公司 | Glycerine refining method |
| CN104326872A (en) * | 2014-10-11 | 2015-02-04 | 波鹰(厦门)科技有限公司 | Method for recycling glycerol in organic wastewater with high salt content |
| CN105418378A (en) * | 2015-11-27 | 2016-03-23 | 宁波滨海石化有限公司 | Purification technology of ester exchange by-product glycerol |
| CN105881791A (en) * | 2016-04-14 | 2016-08-24 | 福建师范大学泉港石化研究院 | Releasing agent prepared from glycerin distillation residues and preparation method thereof |
| CN106831343A (en) * | 2015-12-03 | 2017-06-13 | 浙江医药股份有限公司新昌制药厂 | A kind of isolation and purification method of grease ester bond byproduct of reaction |
| CN106831345A (en) * | 2016-12-15 | 2017-06-13 | 天长市康宁甘油科技有限公司 | A kind of process for refining of biological diesel oil byproduct crude glycerine |
| CN106928024A (en) * | 2017-04-19 | 2017-07-07 | 广西大学 | A kind of production technology of food grade glycerine |
| WO2017119007A1 (en) * | 2016-01-07 | 2017-07-13 | Institute Of Chemical Technology | Process for purification and refining of glycerol |
| CN107056586A (en) * | 2016-12-15 | 2017-08-18 | 天长市康宁甘油科技有限公司 | A kind of efficiently purifying production technology of crude glycerine |
| WO2019178823A1 (en) * | 2018-03-23 | 2019-09-26 | 世界家庭用具制品厂有限公司 | Method for purifying crude glycerol obtained from kitchen waste and use thereof |
| CN111871364A (en) * | 2020-07-24 | 2020-11-03 | 武汉轻工大学 | Preparation method of solid acid and method for purifying glycerin from biodiesel byproduct |
| CN113354763A (en) * | 2021-06-02 | 2021-09-07 | 宁波锋成先进能源材料研究院有限公司 | Preparation method and application of oil-soluble viscosity reducer |
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| CN103274900A (en) * | 2013-06-07 | 2013-09-04 | 文建方 | Method for extracting glycerol from biodiesel wastewater |
| CN103626632A (en) * | 2013-12-24 | 2014-03-12 | 青岛福瑞斯生物能源科技开发有限公司 | Method for purifying by-product crude glycerine of biodiesel prepared by using illegal cooking oil |
| CN103626632B (en) * | 2013-12-24 | 2016-10-05 | 青岛福瑞斯生物能源科技开发有限公司 | A kind of purification process of the by-product crude glycerine of Preparation of biodiesel from waste oils |
| CN104230046A (en) * | 2014-08-21 | 2014-12-24 | 波鹰(厦门)科技有限公司 | Device for separating sodium chloride and glycerinum in high-salinity glycerinum-containing high and advanced organic wastewater |
| CN104230046B (en) * | 2014-08-21 | 2015-09-30 | 波鹰(厦门)科技有限公司 | A kind of high salt contains the tripping device of sodium-chlor and glycerine in glycerine high concentrated organic wastewater |
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| CN104326872B (en) * | 2014-10-11 | 2016-06-08 | 波鹰(厦门)科技有限公司 | The recovery method of glycerol in highly salt containing organic waste water |
| CN104262104A (en) * | 2014-10-16 | 2015-01-07 | 佛山市天晟隆油脂化工有限公司 | Glycerine refining method |
| CN104262101A (en) * | 2014-10-16 | 2015-01-07 | 佛山市天晟隆油脂化工有限公司 | Glycerine refining method |
| CN105418378A (en) * | 2015-11-27 | 2016-03-23 | 宁波滨海石化有限公司 | Purification technology of ester exchange by-product glycerol |
| CN106831343B (en) * | 2015-12-03 | 2020-10-20 | 浙江医药股份有限公司新昌制药厂 | Separation and purification method of grease ester bond reaction by-product |
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| WO2017119007A1 (en) * | 2016-01-07 | 2017-07-13 | Institute Of Chemical Technology | Process for purification and refining of glycerol |
| CN105881791A (en) * | 2016-04-14 | 2016-08-24 | 福建师范大学泉港石化研究院 | Releasing agent prepared from glycerin distillation residues and preparation method thereof |
| CN106831345A (en) * | 2016-12-15 | 2017-06-13 | 天长市康宁甘油科技有限公司 | A kind of process for refining of biological diesel oil byproduct crude glycerine |
| CN107056586A (en) * | 2016-12-15 | 2017-08-18 | 天长市康宁甘油科技有限公司 | A kind of efficiently purifying production technology of crude glycerine |
| CN106928024A (en) * | 2017-04-19 | 2017-07-07 | 广西大学 | A kind of production technology of food grade glycerine |
| WO2019178823A1 (en) * | 2018-03-23 | 2019-09-26 | 世界家庭用具制品厂有限公司 | Method for purifying crude glycerol obtained from kitchen waste and use thereof |
| CN111871364A (en) * | 2020-07-24 | 2020-11-03 | 武汉轻工大学 | Preparation method of solid acid and method for purifying glycerin from biodiesel byproduct |
| CN113354763A (en) * | 2021-06-02 | 2021-09-07 | 宁波锋成先进能源材料研究院有限公司 | Preparation method and application of oil-soluble viscosity reducer |
| CN114773155A (en) * | 2022-04-27 | 2022-07-22 | 宁波杰森绿色能源科技有限公司 | Process for separating glycerin from biodiesel byproduct |
| CN114773155B (en) * | 2022-04-27 | 2024-01-12 | 宁波杰森绿色能源科技有限公司 | Process for separating glycerin from biodiesel byproduct |
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Application publication date: 20130306 |