Abstract: A process and system for obtaining bio-diesel from fatty acids acid catalyst, which is eco-friendly, with minimum losses and low level of hazards during the process. The biodiesel obtained from the process is very clean and pure and conforms to the BIS standards.
The following specification particularly describes and ascertains the nature of this invention and the manner in which it is to be performed:
Field of the invention:
The present invention relates to novel process for developing biodiesel from fatty acids. More particularly the invention relates to the utilization of fatty acids from fat splitting and fractionation plant source. The invention also provides for a system for carrying out the above process.
Background of the invention
The production of biodiesel is generally carried out by base catalysis of vegetable oils. The first step of base catalyzed production of biodiesel process is mixing of alcohol and catalyst using a standard agitator or mixer. The catalyst is typically sodium hydroxide (caustic soda) or potassium hydroxide (potash).
The alcohol/catalyst mix is then charged into a closed reaction vessel and the oil or fat is added. The system from here on is totally closed to the atmosphere to prevent the loss of alcohol. The reaction mix is kept just above the boiling point of the alcohol (around 160 °F) to speed up the reaction and the reaction takes place. Recommended reaction time varies from 1 to 8 hours, and some systems recommend the reaction take place at room temperature. Excess alcohol is normally used to ensure total conversion of the fat or oil to its esters.
Precaution is required to monitor the amount of water and free fatty acids in the incoming oil or fat. If the free fatty acid level or water level is too high it may cause problems with soap formation and the separation of the glycerin byproduct downstream.
Once the reaction is complete, two major products exist: glycerin and biodiesel. Each has a substantial amount of the excess methanol that was used in the reaction. The reacted mixture is sometimes neutralized at this step. The glycerin phase is separated from biodiesel phase by gravity separated usually be natural sedimentation or sometimes by centrifugation.
The excess alcohol is then removed with a flash evaporation process or by distillation. Alternatively, the alcohol is removed and the mixture neutralized before the separation. In either case, the alcohol is recovered using distillation equipment and is re-used.
Precaution is again required to ensure no water accumulates in the recovered alcohol stream.
Once separated from the glycerin, the biodiesel is sometimes purified by washing gently with warm water to remove residual catalyst or soaps, dried, and sent to storage. This is normally the end of the production process resulting in a clear amber-yellow liquid with a viscosity similar to petrodiesel. The biodiesel needs to
be distilled in an additional step to remove small amounts of color bodies to produce a colorless biodiesel.
There are several patens relating to the production of biodiesel including US patents 5482633, 5514820, 5536856, 5945529 and 6015440. However none of these inventions provide for a method to prepare biodiesel from fatty aids. As all the patents are related to preparation of Biodiesel from plant / animal oils/fats only.
Summary of invention
The objective of the invention is to develop a method and equipment for the production of fatty acids methyl / ethyl ester, in particular for diesel fuel for vehicles, which on the one hand avoid the disadvantages of the known methods, and on the other hand enables a rational production in an economically acceptable plant, preferably an industrial-sized plant, but is also economic in small plants.
In view of the above one of the objectives of the present invention is to provide a method and system for developing biodiesel from fatty acids rather than from vegetable oil or animal fat.
Yet another object of the present invention is to develop an economic process for development of biodiesel from fatty acids.
Further, the invention provides a method and system to obtain the biodiesel with maximum conversion from fatty acids of more than 98% which is also conforming to ASTM and BIS standards.
The process for obtaining biodiesel from fatty acids as disclosed in the invention comprises the steps of:
a) Mixing of fatty acids with methanol or ethanol in a ratio of 95:5 to
65:35,
b) Adding the mixture with acid catalyst in an amount 0.1-5% on fatty
acid weight basis.
c) Mixing at 100-300rpm,
d) raising the temperature to 180-280°C and raising the pressure from
800kPa-1000kPa,
e) stirring of the mixture for about 30 minutes to 3 hours,
f) separating the different phases of the mixture to obtain upper layer of biodiesel.
The system for manufacture of bio-diesel from fatty acids disclosed in the invention comprises of
a) at least one acid resistant reactor;
b) at least one source for each of the raw materials including fatty
acids, sulphuric acid, alkaline solution, water and methanol;
c) at least one boiler for injecting live steam in the reactor;
d) at least one separating unit for separation of different mixture
phases,
e) a plurality of connecting pipelines,
f) and optionally at least one filter for filtration of biodiesel or fatty
acids or mixture
The system may further comprise of:
a) a plurality of filters specially designed to suit the isolation of pure
bio-diesel with minimum losses,
b) at least one vacuum evaporator and
c) at least one condenser.
Brief Description Of The Accompanying Drawings and Tables
The Figure 1 describes the steps of the process of developing biodiesel from fatty acids.
Detailed Description of the invention
This invention enables for the production diesel fuel such as eco-diesel or biodiesel in ecologically optimal conditions of production while maintaining all the advantages thereof. The use of fatty acids obtained from the fat splitting and fractionation plant may be used in converting them into biodiesel. This invention makes it possible to accelerate the reaction by enlarging the boundary surfaces with dynamic processes during the esterification.
Due to high or powerful dynamic turbulence, the size of the drops in the liquid phases is effectively reduced, so that much smaller drops are produced, resulting in a much larger surface, which means that the chemical balance state is reached faster. According to a special feature of the invention, physical forces, for example mechanical shear forces, produce the high or powerful dynamic turbulence.
In the disclosed process the free fatty acids is converted by acid esterification into fatty acid methyl or ethyl esters in presence of catalyst sulphuric acid at 180-280°C under pressure of 400-1 OOOkPa. The conversion rate of this process is 99%. The equipments used are acid resistant containers such as stainless steel containers.
The invention has been described in detail with the help of different embodiments and it may be clear to a person skilled in the art that many more embodiments of the invention are possible than those provided. The invention is thus not limited to the description but extends to further embodiments within the scope of the claims.
The conversion of fatty Acids to biodiesel was carried out using the following process: Free fatty acids from fat splitting plant were taken and analyzed for their acid value, triglyceride content etc. The fatty acids were then mixed with alcohol such as methanol or ethanol from 5-35% on free fatty acid weight basis and a proper stirring or blending was carried out at 100-300rpm, preferably at 200-250rpm, for proper mixing of the alcohol (methanol) and fatty acids.
Acid catalyst such as sulphuric acid is added at the rate of 0.1-2% and further stirring is done. The whole mixture is then loaded in a chamber, which is heated with live steam, the pressure of the chamber being 400-1 OOOkPa, preferably 800-1000kPa.
The whole process is then started with the above said parameters. It takes about SOmin to 3 hours to complete the whole process. The output of this process is fatty acid ester (methyl or ethyl), sulphuric acid, water and some triglyceride if any.
In this process the water is removed as steam condenses and gets collected at the bottom of the reactor. The water may be regularly removed. In such case the water along with itself takes some of the catalyst. Thus there is need of additional catalyst, which is to be added during the process from 0.1-1% in addition to the above said quantity.
The unreacted fatty acids and triglyceride are removed by caustic stripping. The methyl or ethyl ester obtained is then settled and washed to remove the traces of sulphuric acid if any.
This advantageous process allows a separation of the individual phases of the mixture, for example in filtration units, is by rational, modern industrial methods. In a further feature of the invention, the fatty acid methyl ester is cleaned after the separation of the emulsion phases. Basically, pure fatty acid methyl ester can be produced with this process.
In accordance with an embodiment of the invention, the separation of the emulsion phases is performed by exploiting the surface forces, in particular by means of filtration. With this method of separating the phases of the mixture, a high economic efficiency is achieved in industrial production.
In accordance with a further embodiment of the invention, the phases of the emulsion were separated by multiphase filtration. Thereby, the water phase was separated in the first step, and the triglycerides were separated as residue in the second step. In a third step, methanol is separated from the fatty acid methyl ester. Such a filter unit can also be designed as a cross-flow filter. With this advantageous process step, any number of steps can be performed and the desired purity achieved. Thus, the production of summer or winter diesel as eco-diesel or bio-diesel depending on the fatty acid chain is quite conceivable.
In another embodiment of the invention, multiphase distillation is performed once chemical balance state is reached, possibly after separation of the phases of the mixture. Distillation can be performed directly on reaching chemical balance state, whereby methanol is removed at the same time. It is also conceivable that distillation be performed after filtration.
In one of the embodiments of the invention, multiphase distillation includes at least one vacuum distillation. With this advantageous process step, a targeted separation of the individual substances is possible, whereby the temperatures at which the process is carried out is reduced by the vacuum. Basically, pure fatty acid methyl ester can be produced with distillation.
In an specific embodiment, multiphase distillation includes at least one evaporation, in particular down-flow evaporation. With this type of evaporation, a more effective separation of the substances to be separated is achieved. This type of evaporation also permits targeted separation of the substances. In accordance with a further feature of the invention, multiphase distillation includes fractionated condensation. With this advantageous process step, any number of steps can be performed and the desired purity achieved. Thus, the production of summer or winter diesel as eco-diesel or bio-diesel depending on the fatty acids chain is achieved.
In accordance with another embodiment of the invention, non-esterified substances are separated and returned to the fatty acid upstream from the reaction section. This increases the yield of ecological fuel obtained from the basic substance input.
The aim of the invention is realized independently by equipment for implementation of the process. The equipment according to the invention is characterized by the fact that it includes at least one container for the fatty acids, and at least one source tank each for the potent sulphuric acid solution, alkaline
solution and the alcohol, as well as at least one mixing vessel for compounding, and that at least the container and the mixing vessel are connected to the reaction section, and that there is a unit for separating the phases of the emulsion downstream from the reaction section. The prime equipments of this process are atleast one reactor connected with a boiler for live steam. With this equipment according to the invention, it is for the first time possible to realize the process according to the invention in an efficient manner and with negligible environmental pollution. Figure 1 depicts the different units of the system along with the direction of flow provided by the connecting pipelines.
In yet another embodiment of the invention, a dynamic separator is included in the reaction section. Since an emulsion is to be produced in the reaction section, i.e., a liquid with two phases maintained in suspension, such a device is particularly suitable for reaching this objective very quickly.
In a specific embodiment, the unit for separating the phases of the mixture is a filtration cum separating unit. With this advantageous device, separation of the individual phases of the mixture is achieved, whereby the sedimentation phase known from the state of the art is no longer necessary as a result of the mechanical devices. It is replaced by process steps that are performed using rational, modern and industrial equipment, plants and devices.
In accordance with a further embodiment of the invention, the surface filter comprises a porous carrier and a layer applied to this carrier that acts as a membrane. With such an advantageous surface filter, the plant is operated with maximum efficiency and making best use of energy. The surface filter may also be designed as a plate filter with cotton cloth of desired pore size.
A further embodiment provides for the filtration unit designed in several phases. Depending on the desired degree of purity of the fatty acid methyl ester, several filters may be arranged in series or in parallel.
A distillation unit comprising at least one evaporator and one condenser is included downstream from the reaction section, or possibly downstream from the phase separation unit in one of the embodiments of the invention. This unit according to the invention also makes it possible to realize the process according to the invention in an efficient manner.
A down-flow evaporator may be used in one of the embodiments of the invention. Such an evaporator has the advantage that the supplied heat can be used optimally. Evaporation in a vacuum is also possible. In accordance with another design of the invention, a thin-layer evaporator is used as an evaporator. Evaporation in a vacuum is also possible with such an evaporator. In addition, optimal results are obtained with the device.
Another modification provides for a separating unit downstream from the unit for
separating the phases of the mixture. By using a separating unit, residues such as unreacted fatty acids, triglyceride etc. can be collected easily and the quality determined. Depending on the quality found, the further procedure is then determined.
The separating unit is connected in one embodiment to the connecting pipe from the container for the fatty acids to the reaction section. If the analysis of the substances in the separating unit shows that there are still non-esterified fatty acids, these can be esterified again. This increases the yield.
A pump, in particular a high-pressure pump, is used to supply the liquid to the reaction section in one of the embodiments. The integration of a high-pressure pump has proven advantageous because the turbulence for esterification creates strong dynamics and thus a large border surface. In accordance with a further feature of the invention, the excess methanol evaporates in a flash reactor. With this step, methanol is removed from the methyl ester.
While the present invention has been described with respect to certain preferred embodiments, it will be apparent to those skilled in the art that various changes and modifications may be made without departing from the scope of the invention as defined in the following claims.
We claim:
1. A process for obtaining biodiesel from fatty acids comprising:
a) Mixing of fatty acids with methanol or ethanol in a ratio of 95:5 to 65:35,
b) Adding the mixture with acid catalyst in an amount 0.1-5% on fatty acid
weight basis.
c) Mixing at 100-300rpm to provide turbulance to achieve maximum exposed
surface area of fatty acids,
d) raising the temperature to 180-280°C and raising the pressure from
800kPa-1000kPa,
e) stirring of the mixture for about 30 minutes to 3 hours,
f) separating the different phases of the mixture to obtain upper layer of
biodiesel.
2. A process for obtaining biodiesel from fatty acids as claimed in claim 1 wherein
said fatty acid used for the process is quantified and analyzed qualitatively prior
to use.
3. A process for obtaining biodiesel from fatty acids as claimed in claim 1 wherein
said acid catalyst is specific to fatty acid preferably sulphuric acid.
4. A process for obtaining biodiesel from fatty acids as claimed in claim 1 wherein
said temperature raise is obtained through passing of hot live steam.
5. A process for obtaining biodiesel from fatty acids as claimed in claim 4 wherein
said steam when condensed is removed regularly and catalyst is added at the
rate of 0.1-1% to compensate for the amount removed with the condensed
steam.
6. A process for obtaining biodiesel from fatty acids as claimed in claim 1 wherein
said upper phase biodiesel layer is further purified by filteration to remove
suspended particles and any solid matter.
7. A process for obtaining biodiesel from fatty acids as claimed in claim 6 wherein
said the filtrate is subjected to evaporation to remove excess alcohol and reused.
8. A process for obtaining biodiesel from fatty acids as claimed in claim 6 or 7
wherein the filtered biodiesel is subjected to washing to remove traces of catalyst
if desired.
9. A process for obtaining biodiesel from fatty acids as claimed in claim 5 to 8
wherein said biodiesel is subjected to caustic stripping to remove any unreacted
fatty acid or triglyceride which is optionally reused as raw material for the
process.
10. A system for manufacture of bio-diesel from fatty acids comprising:
a) at least one acid resistant reactor;
b) at least one source for each of the raw materials including fatty acids,
sulphuric acid, alkaline solution, water and methanol;
c) at least one boiler for injecting live steam in the reactor;
d) at least one separating unit for separation of different mixture phases,
e) a plurality of connecting pipelines,
f) and optionally at least one filter for filtration of biodiesel or fatty acids or
mixture
11. A system for manufacture of bio-diesel from fatty acids as claimed in claim 10
further comprising:
a) a plurality of filters specially designed to suit the isolation of pure bio
diesel with minimum losses,
b) at least one vacuum evaporator and
c) at least one condenser.
12. A system for manufacture of bio-diesel from fatty acids as claimed in claim 10
or 11 wherein said reactor has an acid resistant grade stainless steel body.
13. A system for manufacture of bio-diesel from fatty acids as claimed in claim 10
or 11 wherein said reactor and boiler comprises of automatic temperature
controller for setting the temperature, a steam controller, a stirrer, digital activity
monitor, an inlet and an out let with motor control.
14. A system for manufacture of bio-diesel from fatty acids as claimed in claim 10
or 11 wherein said connecting pipelines are specifically designed to form a
system for smooth flow of material from one unit to another.
15. A system for manufacture of bio-diesel from fatty acids as claimed in claim 10
or 11 wherein said filtration of biodiesel is either by plate filter or by the micro
filter depending upon the quality of the bio-diesel obtained from the reactor.
16. A process and system for manufacture of bio-diesel from fatty acids substantially as herein described with reference to accompanying examples and drawings.
| # | Name | Date |
|---|---|---|
| 1 | 2102-DEL-2006-FORM 4 [17-10-2020(online)].pdf | 2020-10-17 |
| 1 | 2102-del-2006-Form-13 (27-02-2007).pdf | 2007-02-27 |
| 2 | 2102-DEL-2006-RELEVANT DOCUMENTS [18-03-2019(online)].pdf | 2019-03-18 |
| 2 | 2106-DEL-2006-Form-18-(15-09-2010).pdf | 2010-09-15 |
| 3 | 2106-DEL-2006-Correspondence-Others-(15-09-2010).pdf | 2010-09-15 |
| 3 | 2102-DEL-2006-FORM 4 [01-03-2019(online)].pdf | 2019-03-01 |
| 4 | 283047-2102-DEL-2006.pdf | 2019-01-07 |
| 4 | 2102-del-2006-gpa.pdf | 2011-08-21 |
| 5 | Other Patent Document [08-04-2017(online)].pdf | 2017-04-08 |
| 5 | 2102-del-2006-form-5.pdf | 2011-08-21 |
| 6 | Form 13 [04-04-2017(online)].pdf | 2017-04-04 |
| 6 | 2102-del-2006-form-3.pdf | 2011-08-21 |
| 7 | Other Patent Document [04-04-2017(online)].pdf | 2017-04-04 |
| 7 | 2102-del-2006-form-2.pdf | 2011-08-21 |
| 8 | Other Patent Document [04-04-2017(online)].pdf_607.pdf | 2017-04-04 |
| 8 | 2102-del-2006-form-13.pdf | 2011-08-21 |
| 9 | 2102-del-2006-form-1.pdf | 2011-08-21 |
| 9 | Other Patent Document [04-04-2017(online)].pdf_608.pdf | 2017-04-04 |
| 10 | 2102-del-2006-drawings.pdf | 2011-08-21 |
| 10 | Other Patent Document [04-04-2017(online)].pdf_609.pdf | 2017-04-04 |
| 11 | 2102-del-2006-description (complete).pdf | 2011-08-21 |
| 11 | Other Patent Document [04-04-2017(online)].pdf_610.pdf | 2017-04-04 |
| 12 | 2102-del-2006-correspondence-others.pdf | 2011-08-21 |
| 12 | OTHERS [27-03-2017(online)].pdf | 2017-03-27 |
| 13 | 2102-del-2006-claims.pdf | 2011-08-21 |
| 13 | 2102-del-2006-Correspondence-200117.pdf | 2017-01-25 |
| 14 | 2102-del-2006-abstract.pdf | 2011-08-21 |
| 14 | 2102-DEL-2006-HEARING ADJOURNMENT-030117.pdf | 2017-01-04 |
| 15 | 2102-DEL-2006-Other Patent Document-030117.pdf | 2017-01-04 |
| 15 | 2102-del-2006-Others-(28-10-2015).pdf | 2015-10-28 |
| 16 | 2102-del-2006-GPA-(28-10-2015).pdf | 2015-10-28 |
| 16 | 2102-DEL-2006_EXAMREPORT.pdf | 2016-06-30 |
| 17 | 2102-del-2006-Form-2-(28-10-2015).pdf | 2015-10-28 |
| 17 | 2102-del-2006-Abstract-(28-10-2015).pdf | 2015-10-28 |
| 18 | 2102-del-2006-Claims-(28-10-2015).pdf | 2015-10-28 |
| 18 | 2102-del-2006-Form-13-(28-10-2015).pdf | 2015-10-28 |
| 19 | 2102-del-2006-Correspondence Others-(28-10-2015).pdf | 2015-10-28 |
| 19 | 2102-del-2006-Form-13-(28-10-2015)-1.pdf | 2015-10-28 |
| 20 | 2102-del-2006-Description (Complete)-(28-10-2015).pdf | 2015-10-28 |
| 20 | 2102-del-2006-Form-1-(28-10-2015).pdf | 2015-10-28 |
| 21 | 2102-del-2006-Drawings-(28-10-2015).pdf | 2015-10-28 |
| 22 | 2102-del-2006-Description (Complete)-(28-10-2015).pdf | 2015-10-28 |
| 22 | 2102-del-2006-Form-1-(28-10-2015).pdf | 2015-10-28 |
| 23 | 2102-del-2006-Correspondence Others-(28-10-2015).pdf | 2015-10-28 |
| 23 | 2102-del-2006-Form-13-(28-10-2015)-1.pdf | 2015-10-28 |
| 24 | 2102-del-2006-Form-13-(28-10-2015).pdf | 2015-10-28 |
| 24 | 2102-del-2006-Claims-(28-10-2015).pdf | 2015-10-28 |
| 25 | 2102-del-2006-Form-2-(28-10-2015).pdf | 2015-10-28 |
| 25 | 2102-del-2006-Abstract-(28-10-2015).pdf | 2015-10-28 |
| 26 | 2102-del-2006-GPA-(28-10-2015).pdf | 2015-10-28 |
| 26 | 2102-DEL-2006_EXAMREPORT.pdf | 2016-06-30 |
| 27 | 2102-DEL-2006-Other Patent Document-030117.pdf | 2017-01-04 |
| 27 | 2102-del-2006-Others-(28-10-2015).pdf | 2015-10-28 |
| 28 | 2102-del-2006-abstract.pdf | 2011-08-21 |
| 28 | 2102-DEL-2006-HEARING ADJOURNMENT-030117.pdf | 2017-01-04 |
| 29 | 2102-del-2006-claims.pdf | 2011-08-21 |
| 29 | 2102-del-2006-Correspondence-200117.pdf | 2017-01-25 |
| 30 | 2102-del-2006-correspondence-others.pdf | 2011-08-21 |
| 30 | OTHERS [27-03-2017(online)].pdf | 2017-03-27 |
| 31 | 2102-del-2006-description (complete).pdf | 2011-08-21 |
| 31 | Other Patent Document [04-04-2017(online)].pdf_610.pdf | 2017-04-04 |
| 32 | 2102-del-2006-drawings.pdf | 2011-08-21 |
| 32 | Other Patent Document [04-04-2017(online)].pdf_609.pdf | 2017-04-04 |
| 33 | 2102-del-2006-form-1.pdf | 2011-08-21 |
| 33 | Other Patent Document [04-04-2017(online)].pdf_608.pdf | 2017-04-04 |
| 34 | 2102-del-2006-form-13.pdf | 2011-08-21 |
| 34 | Other Patent Document [04-04-2017(online)].pdf_607.pdf | 2017-04-04 |
| 35 | 2102-del-2006-form-2.pdf | 2011-08-21 |
| 35 | Other Patent Document [04-04-2017(online)].pdf | 2017-04-04 |
| 36 | Form 13 [04-04-2017(online)].pdf | 2017-04-04 |
| 36 | 2102-del-2006-form-3.pdf | 2011-08-21 |
| 37 | Other Patent Document [08-04-2017(online)].pdf | 2017-04-08 |
| 37 | 2102-del-2006-form-5.pdf | 2011-08-21 |
| 38 | 283047-2102-DEL-2006.pdf | 2019-01-07 |
| 38 | 2102-del-2006-gpa.pdf | 2011-08-21 |
| 39 | 2106-DEL-2006-Correspondence-Others-(15-09-2010).pdf | 2010-09-15 |
| 39 | 2102-DEL-2006-FORM 4 [01-03-2019(online)].pdf | 2019-03-01 |
| 40 | 2106-DEL-2006-Form-18-(15-09-2010).pdf | 2010-09-15 |
| 40 | 2102-DEL-2006-RELEVANT DOCUMENTS [18-03-2019(online)].pdf | 2019-03-18 |
| 41 | 2102-del-2006-Form-13 (27-02-2007).pdf | 2007-02-27 |
| 41 | 2102-DEL-2006-FORM 4 [17-10-2020(online)].pdf | 2020-10-17 |