CN111471531A - Biodiesel preparation system suitable for kitchen oil - Google Patents
Biodiesel preparation system suitable for kitchen oil Download PDFInfo
- Publication number
- CN111471531A CN111471531A CN202010335260.XA CN202010335260A CN111471531A CN 111471531 A CN111471531 A CN 111471531A CN 202010335260 A CN202010335260 A CN 202010335260A CN 111471531 A CN111471531 A CN 111471531A
- Authority
- CN
- China
- Prior art keywords
- tank
- tower
- feed inlet
- discharge port
- ionic liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C3/00—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom
- C11C3/04—Fats, oils, or fatty acids by chemical modification of fats, oils, or fatty acids obtained therefrom by esterification of fats or fatty oils
- C11C3/10—Ester interchange
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L1/00—Liquid carbonaceous fuels
- C10L1/02—Liquid carbonaceous fuels essentially based on components consisting of carbon, hydrogen, and oxygen only
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
Landscapes
- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Liquid Carbonaceous Fuels (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a biodiesel preparation system suitable for kitchen oil, which comprises a crude oil tank for receiving water and impurities removed by a pretreatment system, an esterification kettle connected with a discharge port of the crude oil tank, an ester exchange reaction kettle connected with the discharge port of the esterification kettle, and a rectification cutting tower connected with the discharge port of the ester exchange reaction kettle; a settling tank group and a first layering tank are also arranged between the esterification kettle and the ester exchange reaction kettle so as to facilitate the separation of the acidic ionic liquid catalyst and esters; the discharge port at the lower part of the first layering tank is connected with an ionic liquid recovery tank, the discharge port at the upper part of the first layering tank is connected with the feed inlet of the ester exchange reaction kettle, a crude methyl ester settling tank, a second layering tank and a deodorization tower are also connected between the ester exchange reaction kettle and the rectification cutting tower, and the discharge port of the deodorization tower is connected to the feed inlet of the rectification cutting tower. The invention can not generate acid sludge, greatly reduces the subsequent treatment difficulty, and has high recycling rate of the catalyst.
Description
Technical Field
The invention relates to the technical field of oil preparation, in particular to a biodiesel preparation system suitable for kitchen oil.
Background
The kitchen waste oil in general life comprises kitchen waste oil, hogwash water liquid and waste cooking oil, the waste oil is recovered and then is subjected to pretreatment, water removal and impurity removal to prepare biodiesel, but in the prior production of biodiesel by utilizing the waste oil, a traditional homotropic catalyst is generally adopted as a catalyst in the esterification reaction and ester exchange reaction stages, namely a homotropic acid-base catalyst is adopted for catalytic reaction, but in the reaction process of taking an acid-base method as the catalyst, the esterification reaction and the ester exchange reaction are reversible reactions, excessive methanol must be added for reaction, the demand for methanol is particularly large, and the methanol is wasted; meanwhile, the acid in the acid-base method generally adopts concentrated sulfuric acid, the alkali adopts sodium hydroxide, and waste oil generally cannot remove various metal ions contained in oil in a pretreatment stage, so that the conventional acid-base method also has the following defects that firstly, the concentrated sulfuric acid used as a catalyst has large required amount, is easy to corrode equipment, has more side reactions, can react with the metal ions contained in the oil to generate acid sludge and sulfate waste residues, causes poor subsequent removal in process water, and can also cause the prepared ester to contain salt, high conductivity and high COD (chemical oxygen demand), thereby increasing the treatment difficulty; secondly, some free fatty acid is generated in the reaction stage, but the isotropic catalyst is sensitive to the free fatty acid and is easy to have saponification reaction with the fatty acid, so that esters are not easy to separate; thirdly, the catalyst recovery is difficult because the catalyst is difficult to remove because of the reverse direction of the reaction, and because the subsequent separation is difficult. Therefore, how to provide a biodiesel preparation system which has simple catalyst separation, can be recycled and reused, does not generate acid sludge, and can improve the oil yield and is suitable for kitchen oil is very important.
Disclosure of Invention
Aiming at the defects of the prior art, the technical problems to be solved by the invention are as follows: the biodiesel preparation system suitable for kitchen oil is provided, acid sludge is not generated, the subsequent treatment difficulty is greatly reduced, and the catalyst can be recovered and has high recycling rate.
In order to solve the technical problems, the invention adopts the following technical scheme:
a biodiesel preparation system suitable for kitchen oil comprises a crude oil tank for receiving water and impurities removed by a pretreatment system, an esterification kettle connected with a discharge port of the crude oil tank, an ester exchange reaction kettle connected with the discharge port of the esterification kettle, and a rectification cutting tower connected with the discharge port of the ester exchange reaction kettle and used for preparing biodiesel; the esterification kettle is provided with an adding port for methanol and an acidic ionic liquid catalyst, and a settling tank group and a first layering tank are arranged between the esterification kettle and the ester exchange reaction kettle so as to separate the acidic ionic liquid catalyst from esters; the feed inlet of the settling tank group is connected with the discharge outlet of the esterification kettle, and the discharge outlet of the settling tank group is connected with the feed inlet of the first layering tank; the first layering tank is provided with an upper discharge port and a lower discharge port, the discharge port at the lower part of the first layering tank is connected with an ionic liquid recovery tank, the discharge port at the upper part of the first layering tank is connected with the feed inlet of the ester exchange reaction kettle, and the ester exchange reaction kettle is provided with a feed inlet for methanol and an alkaline ionic liquid catalyst; still link up in proper order between ester exchange reaction kettle and the rectification cutting tower has coarse methyl ester settling cask, second layering jar and deodorizing tower, the ester exchange reaction kettle discharge gate is connected with coarse methyl ester settling cask feed inlet, coarse methyl ester settling cask discharge gate links up the setting with second layering jar feed inlet, and the second layering jar has two discharge gates and is arranged in separating glycerine and the methyl alcohol in the coarse methyl ester, and second layering tank bottom discharge gate is connected with glycerine methyl alcohol jar, and second layering jar upper portion discharge gate is connected to the deodorizing tower feed inlet, the deodorizing tower is arranged in getting rid of the light component in the coarse methyl ester with the deodorization, the deodorizing tower discharge gate is connected to the cutting tower feed inlet and prepares biodiesel in order to carry out the rectification cutting.
When the method is used, the waste oil to be refined is input into a pretreatment system, impurity particles and water contained in the waste oil are removed under the impurity removal and water removal effects of the pretreatment system, so that the oil entering an esterification kettle does not contain water and impurities, then the waste oil enters the esterification kettle after water and impurity removal for pre-esterification, methanol and an acidic ionic liquid catalyst are added into the esterification kettle, in the scheme, the acidic ionic liquid catalyst is imidazole salt, and the basic ionic liquid catalyst is quaternary ammonium salt and is a high molecular organic matter, and different from a catalyst in a conventional acid-base method, the ionic liquid catalyst is non-volatile, pollution-free, high in electrochemical stability, strong in electrostatic field and most importantly, easy to separate in a layered mode; then the acidic ionic liquid catalyst is used as a catalyst to promote the esterification reaction, the esters discharged from the discharge port of the esterification kettle after the oils are subjected to the esterification reaction contain the acidic ionic liquid catalyst and methanol, the density of the acidic ionic liquid catalyst is greater than that of the esters and the acidic ionic liquid catalyst is not dissolved with the esters, then under the action of the settling tank group and the first layering tank, the settling tank group mainly plays a role in buffering and standing, the subsequent first layering tank is favorably layered, then the acidic ionic liquid catalyst and the methanol are positioned at the lower layer of the first layering tank and enter the ionic liquid recovery tank from the discharge port at the lower part, the ionic liquid in the subsequent ionic liquid recovery tank can enter the esterification kettle again after dehydration and dealcoholization to be reused as the catalyst, the esters in the oil phase are positioned at the upper layer, and then the esters enter the ester exchange reaction kettle from the discharge port at the upper part of the first layering tank, performing ester exchange reaction, adding an alkaline ionic liquid catalyst and methanol in the ester exchange reaction, wherein in the ester exchange reaction, only a small amount of the alkaline ionic liquid catalyst is needed to be added to serve as the catalyst, the alkaline ionic liquid catalyst promotes the ester exchange reaction to change esters into crude methyl esters, the crude methyl esters entering a settling tank from a discharge port of an ester exchange reaction kettle are crude methyl esters and are carried with glycerin, methanol and the alkaline ionic liquid catalyst, and a small amount of light components are contained, then under the action of the settling tank and a second layering tank, due to the fact that the alkaline ionic liquid, the glycerin and the methanol are dissolved mutually and the density is higher than that of the crude methyl esters, the second layering tank separates the glycerin and the methanol in the crude methyl esters, the alkaline ionic liquid catalyst is mixed in the glycerin in a very small amount, the crude methyl esters are separated from the glycerin and the methanol in the second layering tank, and the separated crude methyl esters also contain a small amount of light components, and (3) deodorizing the crude methyl ester and the light components in a deodorizing tower to remove the light components carried in the crude methyl ester, and then rectifying and cutting the crude methyl ester in a rectifying and cutting tower to prepare the biodiesel.
By adopting the system, the catalyst and the corresponding separation process are improved, the acidic ionic liquid and the alkaline ionic liquid are used as the catalyst to carry out esterification and ester exchange reaction, and the acidic ionic liquid catalyst and the alkaline ionic liquid catalyst are macromolecular organic matters, have high electrochemical stability and strong electrostatic field, cannot react with metal ions contained in waste oils, cannot generate acid sludge and sulfate waste residues naturally, and improve the purity and the quality of the subsequently prepared biodiesel; meanwhile, the ionic liquid is used as a catalyst, and the self characteristic is favorable for separating methanol, the catalyst and esters, so that the process can effectively recycle the acidic ionic liquid catalyst through the arranged settling tank group and the first layering tank, has strong recyclability, overcomes the defect that the catalyst cannot be recycled in the traditional acid-base method, has high electrochemical stability of the acidic ionic liquid, and can not generate side reaction in the esterification reaction and ester exchange stages in the catalytic reaction process, so that the obtained crude methyl ester has high purity; and the methanol and the ionic liquid have different boiling points, so that the separation process is simple, the methanol can be recycled, and the waste of the methanol in the esterification reaction and the ester exchange reaction is reduced.
As optimization, a condensing tank is further arranged between the esterification kettle and the settling tank group, so that the gas-phase esters are condensed by the condensing tank and then enter the settling tank group, a feed port of the condensing tank is connected with a discharge port of the esterification kettle, and the discharge port of the condensing tank is connected with a feed port of the settling tank group.
Thus, the esters, the methanol and the ionic liquid which are discharged from the esterification kettle are in gas phase, and the esters are changed from gas state to liquid state under the action of the condensing tank, thereby being beneficial to the subsequent separation of the esters.
As optimization, the number of the settling tanks in the settling tank group is three, and the three settling tanks comprise a first settling tank, a second settling tank and a third settling tank which are connected in sequence; the first settling tank bottom feed inlet is connected with the condensing tank discharge outlet, the first settling tank top discharge outlet is communicated with the second settling tank bottom feed inlet, the second settling tank top discharge outlet is communicated with the third settling tank bottom feed inlet, and the third settling tank top discharge outlet is communicated with the first layering tank feed inlet.
Thus, the esters entering the settling tank group contain acidic ionic liquid catalyst and methanol, and by arranging the settling tank group, because the esters which just pass through the condensing tank are not necessarily condensed, the settling tank group plays a role in buffering and condensing the uncondensed esters, and the three settling tanks are discharged in a mode of overflowing from the bottom to the top, so that the buffering and standing effects are better, the flow rate of the esters passing through the first layering tank is reduced by the action of the settling tank, and the layering effect of the subsequent first layering tank is better facilitated; and through setting up the settling cask group, the settling cask can carry out the buffer memory to the ester after esterification reaction, is convenient for control follow-up transesterification's progress control, and the required amount of its transesterification is satisfied to the ejection of compact speed of accessible control settling cask, guarantees its transesterification's normal clear.
As optimization, ionic liquid recovery tank discharge gate department has still linked up dealcoholize jar and drain sump in proper order, dealcoholize jar feed inlet links up with ionic liquid recovery tank discharge gate, the dealcoholize jar is arranged in getting rid of the methyl alcohol among the acid ionic liquid catalyst, dealcoholize jar top discharge gate is connected to the cauldron of esterifying with reuse methyl alcohol, dealcoholize jar bottom discharge gate links up with the drain sump feed inlet, the drain sump is arranged in getting rid of the water among the acid ionic liquid catalyst, the drain sump bottom discharge gate is connected to in the cauldron of esterifying with reuse acid ionic liquid catalyst.
Therefore, water is generated in the esterification reaction process, the acidic ionic liquid catalyst separated by the first layering tank also contains part of methanol and water, the methanol in the acidic ionic liquid catalyst is separated under the dealcoholization effect of the dealcoholization tank, the water in the acidic ionic liquid catalyst is separated under the dealcoholization effect of the dewatering tank, and then the acidic ionic liquid catalyst enters the esterification kettle again to be reused as the catalyst, so that the utilization rate of the acidic ionic liquid catalyst is improved, the waste of the catalyst is avoided, and the cost is saved.
Preferably, a discharge port of the glycerol methanol tank is connected with a first vacuum dealcoholization tower to separate methanol in glycerol, a discharge port at the upper part of the first vacuum dealcoholization tower is connected to the esterification kettle to recycle methanol, and a discharge port at the bottom of the first vacuum dealcoholization tower is connected to a glycerol storage tank.
Like this, owing to being dissolved in methyl alcohol through the glycerine that the second layering jar was separated, consequently the glycerine of separating gets into glycerine methanol tank back, under the effect of first vacuum dealcoholize tower, utilizes the boiling point difference, separates glycerine and methyl alcohol to the methyl alcohol of separating can lead to again in the esterification reaction cauldron carry out recycle, can reduce the input of methyl alcohol in the esterification reaction cauldron like this, and the glycerine of separating simultaneously gets into glycerine holding vessel and stores.
As optimization, a second vacuum dealcoholization tower is arranged between the second layering tank and the deodorization tower to remove methanol carried in the crude methyl ester; and the upper discharge hole of the second vacuum dealcoholization tower is also connected to the esterification kettle to introduce the methanol to the esterification kettle for recycling.
Therefore, after the layering effect of the second layering tank, a small amount of methanol can be contained in the crude methyl ester, so that the part of methanol carried in the crude methyl ester can be effectively removed through the second vacuum dealcoholization tower, the purity of the crude methyl ester is improved, meanwhile, the methanol is introduced into the esterification kettle for recycling through the second vacuum dealcoholization tower, the input amount of the methanol can be reduced, and the recycling rate is higher.
As optimization, the rectification cutting tower comprises a first-stage rectification cutting tower, a second-stage rectification cutting tower and a third-stage rectification cutting tower which are sequentially connected, wherein a feed inlet of the first-stage rectification cutting tower is connected to a discharge outlet of the deodorization tower, a discharge outlet at the top of the first-stage rectification cutting tower is connected to the light biodiesel tank, and a discharge outlet at the bottom of the first-stage rectification cutting tower is connected with a feed inlet of the second-stage rectification cutting tower; the discharge port of the top of the second-stage rectification cutting tower and the discharge port of the top of the third-stage rectification cutting tower are both connected to the biodiesel tank, the discharge port of the bottom of the second-stage rectification cutting tower is linked with the feed port of the third-stage rectification cutting tower, and the discharge port of the bottom of the third-stage rectification cutting tower is connected to the heavy biodiesel tank.
Like this, through establishing the rectification cutting tower in series respectively, set up to the one-level rectification cutting tower, second grade rectification cutting tower and the tertiary rectification cutting that connect gradually, avoided traditional single rectification cutting tower to need the parameter to be interrupted the adjustment setting, can guarantee going on incessantly of the rectification process of crude methyl ester in this scheme, need not change the parameter, every rectification tower accomplishes the rectification cutting of corresponding component, but the incessant rectification of streamlined has improved the efficiency of preparing biodiesel of crude methyl ester.
In conclusion, the beneficial effects of the invention are as follows: in the scheme, the catalyst in the esterification reaction and the ester exchange is improved, and the subsequent process is correspondingly changed to improve the recovery utilization rate of the acidic ionic liquid and the methanol; the acidic ionic liquid and the alkaline ionic liquid are used as catalysts for esterification and ester exchange reaction, and the acidic ionic liquid catalyst and the alkaline ionic liquid catalyst are macromolecular organic matter solutions, so that the electrochemical stability is high, a strong electrostatic field exists, the acidic ionic liquid catalyst and the alkaline ionic liquid catalyst cannot react with metal ions contained in waste oils, acid residues and sulfate waste residues cannot be generated naturally, and the purity and the quality of the subsequently prepared biodiesel are improved; meanwhile, the ionic liquid is used as a catalyst, and the self characteristic is favorable for separating methanol, the catalyst and esters, so that the process can effectively recycle the acidic ionic liquid catalyst through the arranged settling tank group and the first layering tank, has strong recyclability, overcomes the defect that the acidic ionic liquid catalyst cannot be recycled by the traditional acid-base method, has high electrochemical stability of the acidic ionic liquid, and does not generate side reaction in the esterification reaction and ester exchange stages in the catalytic reaction process, thereby obtaining the crude methyl ester with high purity; and the methanol and the ionic liquid have different boiling points, so that the separation process is simple, the methanol can be recycled, and the waste of the methanol in the esterification reaction and the ester exchange reaction is reduced.
Drawings
For purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made in detail to the present invention as illustrated in the accompanying drawings, in which:
FIG. 1 is a schematic flow diagram of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Reference numerals in the drawings of the specification include: the system comprises a crude oil tank 1, an esterification kettle 2, a settling tank group 3, a first layering tank 4, a buffer tank 5, an ester exchange reaction kettle 6, an ionic liquid recovery tank 7, a crude methyl ester settling tank 8, a second layering tank 9, a first vacuum dealcoholization tower 10, a glycerol storage tank 11, a second vacuum dealcoholization tower 12, a deodorization tower 13, a rectification cutting tower 14, a dealcoholization tank 15, a dehydration tank 16 and a glycerol methanol tank 17.
In the present embodiment, a biodiesel preparation system suitable for kitchen oil, as shown in fig. 1, includes a crude oil tank 1 for receiving crude oil after water and impurities removal by a pretreatment system, an esterification kettle 2 connected to a discharge port of the crude oil tank 1, an ester exchange reaction kettle 6 connected to a discharge port of the esterification kettle 2, and a rectification and cutting tower 14 connected to a discharge port of the ester exchange reaction kettle 6 for preparing biodiesel; the esterification kettle 2 is provided with an adding port for methanol and acidic ionic liquid catalyst, and a settling tank group 3 and a first layering tank 4 are also arranged between the esterification kettle 2 and the ester exchange reaction kettle 6 so as to separate the acidic ionic liquid catalyst from esters; the feed inlet of the settling tank group 3 is connected with the discharge outlet of the esterification kettle 2, and the discharge outlet of the settling tank group 3 is connected with the feed inlet of the first layering tank 4; the first layering tank 4 is provided with an upper discharge port and a lower discharge port, the discharge port at the lower part of the first layering tank 4 is connected with an ionic liquid recovery tank 7, the discharge port at the upper part of the first layering tank 4 is connected with the feed port of an ester exchange reaction kettle 6, and the ester exchange reaction kettle 6 is provided with a feed port for methanol and an alkaline ionic liquid catalyst; it has thick methyl ester settling cask 8, second layering jar 9 and deodorization tower 13 still to link up in proper order between ester exchange reaction kettle 6 and the rectification cutting tower 14, 6 discharge gates of ester exchange reaction kettle are connected with thick methyl ester settling cask 8 feed inlets, 8 discharge gates of thick methyl ester settling cask link up the setting with 9 feed inlets of second layering jar, and second layering jar 9 has two discharge gates and is arranged in separating glycerine and the methyl alcohol in the thick methyl ester, and 9 bottom discharge gates of second layering jar are connected with glycerine methyl alcohol jar 17, and 9 upper portion discharge gates of second layering jar are connected to 13 feed inlets of deodorization tower, 13 light component that deodorization tower is 13 to be arranged in getting rid of thick methyl ester is with the deodorization, 13 discharge gates of deodorization tower are connected to 14 feed inlets of rectification cutting tower and are prepared biodiesel in order to carry out the rectification cutting.
When the method is used, the waste oil to be refined is input into a pretreatment system, impurity particles and water contained in the waste oil are removed under the impurity removal and water removal effects of the pretreatment system, so that the oil entering an esterification kettle 2 does not contain water and impurities, then the waste oil enters the esterification kettle 2 for pre-esterification after water and impurity removal, methanol and an acidic ionic liquid catalyst are added into the esterification kettle 2, in the scheme, the acidic ionic liquid catalyst is imidazole salt, and the basic ionic liquid catalyst is quaternary ammonium salt and is a macromolecular organic matter, and different from the catalyst in the conventional acid-base method, the ionic liquid catalyst is nonvolatile, pollution-free, high in electrochemical stability, strong in electrostatic field and most importantly, easy to separate in a layered mode; then the acidic ionic liquid catalyst is used as a catalyst to promote the esterification reaction, the esters discharged from the discharge port of the esterification kettle 2 after the oils are subjected to the esterification reaction contain the acidic ionic liquid catalyst and methanol, because the density of the acidic ionic liquid catalyst is greater than that of the esters and the acidic ionic liquid catalyst is not dissolved with the esters, then under the action of the settling tank group 3 and the first layering tank 4, the settling tank group 3 mainly plays a role of buffering and standing to facilitate the subsequent layering of the first layering tank 4, and then after the acidic ionic liquid catalyst enters the first layering tank 4, the acidic ionic liquid catalyst and the methanol are positioned at the lower layer of the first layering tank 4 and enter the ionic liquid recovery tank 7 from the discharge port at the lower part, the acidic ionic liquid in the subsequent ionic liquid recovery tank 7 can enter the esterification kettle 2 again after dehydration and dealcoholization to be reused as the catalyst, the esters in the oil phase are positioned at the upper layer of the first layering tank 4, and then the esters enter the ester exchange reaction kettle 6 from the discharge port at the upper part of, performing ester exchange reaction, adding an alkaline ionic liquid catalyst and methanol in the ester exchange reaction, wherein in the ester exchange reaction, only a small amount of the alkaline ionic liquid catalyst is needed to be added to play a role of the catalyst, the alkaline ionic liquid catalyst promotes the ester exchange reaction to change esters into crude methyl esters, the crude methyl esters entering a settling tank from a discharge port of an ester exchange reaction kettle 6 are crude methyl esters and are carried with glycerol, methanol and the alkaline ionic liquid catalyst, and also contain a small amount of light components, then under the action of the settling tank and a second layering tank 9, due to the fact that alkaline ionic liquid, glycerol and methanol are dissolved mutually and the density is higher than that of the crude methyl esters, the second layering tank 9 separates the glycerol and the methanol in the crude methyl esters, the alkaline ionic liquid catalyst is mixed in the glycerol in a very small amount, the crude methyl esters are separated from the glycerol and the methanol in the second layering tank 9, and the separated crude methyl esters also contain a small amount of light components, and the crude methyl ester and the light components enter a deodorization tower 13 for deodorization so as to remove the light components carried in the crude methyl ester, and then the crude methyl ester enters a rectification cutting tower 14 for rectification cutting to prepare the biodiesel.
By adopting the system, the catalyst is improved in the scheme, the acidic ionic liquid and the alkaline ionic liquid are used as the catalyst to carry out esterification and ester exchange reactions, and the acidic ionic liquid catalyst and the alkaline ionic liquid catalyst are macromolecular organic matters, so that the electrochemical stability is high, a strong electrostatic field exists, the acidic ionic liquid catalyst and the alkaline ionic liquid catalyst cannot react with metal ions contained in waste oils, acid residues and sulfate waste residues cannot be generated naturally, and the purity and the quality of the subsequently prepared biodiesel are improved; meanwhile, as the ionic liquid is used as the catalyst, the self characteristic is favorable for separation, and the process can effectively recycle the acidic ionic liquid catalyst through the arranged settling tank group 3 and the first layering tank 4, has strong recyclability, overcomes the defect that the traditional acid-base method cannot be recycled, has high electrochemical stability of the acidic ionic liquid, and can not generate side reaction in the esterification reaction and ester exchange stages in the catalytic reaction process, so that the obtained crude methyl ester has high purity; and the methanol and the ionic liquid have different boiling points, so that the separation process is simple, the methanol can be recycled, and the waste of the methanol in the esterification reaction and the ester exchange reaction is reduced.
In a specific embodiment, a condensing tank is further arranged between the esterification kettle 2 and the settling tank group 3 so as to condense the esters in the gas phase through the condensing tank and then enter the settling tank group 3, a feed port of the condensing tank is connected with a discharge port of the esterification kettle 2, and the discharge port of the condensing tank is connected with a feed port of the settling tank group 3.
Thus, the esters, the methanol and the ionic liquid which are discharged from the esterification kettle 2 are in gas phase, and the esters are changed from gas state to liquid state under the action of the condensing tank, so that the subsequent separation of the esters is facilitated.
In a specific embodiment, the number of the settling tanks in the settling tank group 3 is three, and the three settling tanks include a first settling tank, a second settling tank and a third settling tank which are connected in sequence; the first settling tank bottom feed inlet is connected with the condensing tank discharge outlet, the first settling tank top discharge outlet is communicated with the second settling tank bottom feed inlet, the second settling tank top discharge outlet is communicated with the third settling tank bottom feed inlet, and the third settling tank top discharge outlet is communicated with the first layering tank 4 feed inlet.
Thus, the esters entering the settling tank group 3 contain acidic ionic liquid catalyst and methanol, and by arranging the settling tank group 3, because the esters just passing through the condensing tank are not necessarily condensed, the settling tank group 3 plays a role in buffering and condensing the uncondensed esters, and the three settling tanks are discharged in a mode of overflowing from the bottom to the top, so that the buffering and standing effects are better, and the flow velocity of the esters passing through the first layering tank 4 is reduced by the action of the settling tank, thereby being more beneficial to the layering effect of the subsequent first layering tank 4; and through setting up settling cask group 3, the settling cask can carry out the buffer memory to the ester after esterification, is convenient for control follow-up transesterification's progress control, and the required amount that its transesterification was satisfied to the ejection of compact speed of accessible control settling cask guarantees its transesterification's normal clear.
In specific implementation mode, ion liquid recovery tank 7 discharge gate department has still linked up dealcoholize jar 15 and drain sump 16 in proper order, dealcoholize jar 15 feed inlet and ion liquid recovery tank 7 discharge gate link up, dealcoholize jar 15 is arranged in getting rid of the methyl alcohol among the acid ionic liquid catalyst, dealcoholize 15 top discharge gate and be connected to the esterification kettle with reuse methyl alcohol, dealcoholize 15 bottom discharge gate and drain sump 16 feed inlet link up, drain sump 16 is arranged in getting rid of the water among the acid ionic liquid catalyst, drain sump bottom discharge gate is connected to in the esterification kettle with reuse acid ionic liquid catalyst.
Therefore, water is generated in the esterification reaction process, so that the acidic ionic liquid catalyst separated by the first layering tank 4 also contains part of methanol and water, the methanol in the acidic ionic liquid catalyst is separated under the dealcoholization effect of the dealcoholization tank, the water in the acidic ionic liquid catalyst is separated under the dehydration effect of the dehydration tank 16, and then the acidic ionic liquid catalyst enters the esterification kettle 2 again to be reused as the catalyst, so that the utilization rate of the acidic ionic liquid catalyst is improved, the waste of the catalyst is avoided, and the cost is saved.
In a specific embodiment, the discharge port of the glycerol methanol tank 17 is connected with a first vacuum dealcoholization tower 10 to separate methanol in glycerol, the discharge port of the upper part of the first vacuum dealcoholization tower 10 is connected to the esterification kettle 2 to recycle methanol, and the discharge port of the bottom of the first vacuum dealcoholization tower 10 is connected to the glycerol storage tank 11.
Thus, the glycerin separated by the second stratified tank 9 is dissolved in methanol, and thus the separated glycerin enters the glycerin methanol tank 17, and then is separated from the methanol by utilizing the difference of boiling points under the action of the first vacuum dealcoholization tower 10, so that the separated methanol can be introduced into the esterification kettle 2 again for recycling, thereby reducing the input amount of the methanol in the esterification kettle 2, and simultaneously the separated glycerin enters the glycerin storage tank 11 for storage.
In a specific embodiment, a second vacuum dealcoholization tower 12 is arranged between the second layering tank 9 and the deodorization tower to remove methanol entrained in the crude methyl ester; the upper discharge port of the second vacuum dealcoholization tower 12 is also connected to the esterification kettle 2 to introduce methanol to the esterification kettle 2 for recycling.
Thus, after the stratification of the second stratification tank 9, the crude methyl ester also contains a small amount of methanol, so that the crude methyl ester can effectively remove part of methanol entrained in the crude methyl ester through the second vacuum dealcoholization tower 12, the purity of the crude methyl ester is improved, meanwhile, the second vacuum dealcoholization tower 12 leads the methanol to the esterification kettle 2 for recycling, the input amount of the methanol can be reduced, and the recovery rate is higher.
In a specific embodiment, the rectification cutting tower 14 comprises a first rectification cutting tower, a second rectification cutting tower and a third rectification cutting tower which are sequentially connected, wherein a feed inlet of the first rectification cutting tower is connected to a discharge outlet of the deodorization tower, a discharge outlet at the top of the first rectification cutting tower is connected to the light biodiesel tank, and a discharge outlet at the bottom of the first rectification cutting tower is connected with a feed inlet of the second rectification cutting tower; the discharge port of the top of the second-stage rectification cutting tower and the discharge port of the top of the third-stage rectification cutting tower are both connected to the biodiesel tank, the discharge port of the bottom of the second-stage rectification cutting tower is linked with the feed port of the third-stage rectification cutting tower, and the discharge port of the bottom of the third-stage rectification cutting tower is connected to the heavy biodiesel tank.
Like this, through establishing rectification cutting tower 14 series connection respectively, set up to the one-level rectification cutting tower, second grade rectification cutting tower and the tertiary rectification cutting that connect gradually, avoided traditional single rectification cutting tower to need the parameter to be interrupted the adjustment setting, can guarantee going on incessantly of the rectification process of crude methyl ester in this scheme, need not change the parameter, every rectification tower accomplishes the rectification cutting of corresponding component, but the incessant rectification of streamlined has improved the preparation efficiency that crude methyl ester prepared biodiesel.
In the specific implementation process, a buffer tank 5 is further arranged between the first layering tank and the ester exchange reaction kettle, a feed inlet of the buffer tank is connected with a discharge outlet at the upper part of the first layering tank, and a buffer discharge outlet is connected with a feed inlet of the ester exchange reaction kettle.
Like this, can keep in just layering the ester of accomplishing through setting up buffer tank 5 to the ester volume that the control got into the ester interchange reaction can guarantee that the demand of ester interchange reaction supplies at any time, in order to ensure production line normal operating.
Finally, it is noted that the above-mentioned embodiments illustrate rather than limit the invention, and that, while the invention has been described with reference to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. The utility model provides a biodiesel prepares system suitable for meal kitchen oil which characterized in that: the device comprises a crude oil tank for receiving water and impurities removed by a pretreatment system, an esterification kettle connected with a discharge port of the crude oil tank, an ester exchange reaction kettle connected with the discharge port of the esterification kettle, and a rectification cutting tower connected with the discharge port of the ester exchange reaction kettle and used for preparing biodiesel;
the esterification kettle is provided with an adding port for methanol and an acidic ionic liquid catalyst, and a settling tank group and a first layering tank are arranged between the esterification kettle and the ester exchange reaction kettle so as to separate the acidic ionic liquid catalyst from esters; the feed inlet of the settling tank group is connected with the discharge outlet of the esterification kettle, and the discharge outlet of the settling tank group is connected with the feed inlet of the first layering tank; the first layering tank is provided with an upper discharge port and a lower discharge port, the discharge port at the lower part of the first layering tank is connected with an ionic liquid recovery tank, the discharge port at the upper part of the first layering tank is connected with the feed inlet of the ester exchange reaction kettle, and the ester exchange reaction kettle is provided with a feed inlet for methanol and an alkaline ionic liquid catalyst;
still link up in proper order between ester exchange reaction kettle and the rectification cutting tower has coarse methyl ester settling cask, second layering jar and deodorizing tower, the ester exchange reaction kettle discharge gate is connected with coarse methyl ester settling cask feed inlet, coarse methyl ester settling cask discharge gate links up the setting with second layering jar feed inlet, and the second layering jar has two discharge gates and is arranged in separating glycerine and the methyl alcohol in the coarse methyl ester, and second layering tank bottom discharge gate is connected with glycerine methyl alcohol jar, and second layering jar upper portion discharge gate is connected to the deodorizing tower feed inlet, the deodorizing tower is arranged in getting rid of the light component in the coarse methyl ester with the deodorization, the deodorizing tower discharge gate is connected to the cutting tower feed inlet and prepares biodiesel in order to carry out the rectification cutting.
2. The biodiesel preparation system suitable for kitchen oil according to claim 1, characterized in that: still be provided with the condensing pot between esterification cauldron and settling cask group to get into settling cask group after condensing the ester of gaseous phase through the condensing pot, the condensing pot feed inlet is connected with esterification cauldron discharge gate, the condensing pot discharge gate links up with settling cask group feed inlet mutually.
3. The biodiesel preparation system suitable for kitchen oil according to claim 2, characterized in that: the number of the settling tanks in the settling tank group is three, and the three settling tanks comprise a first settling tank, a second settling tank and a third settling tank which are connected in sequence; the first settling tank bottom feed inlet is connected with the condensing tank discharge outlet, the first settling tank top discharge outlet is communicated with the second settling tank bottom feed inlet, the second settling tank top discharge outlet is communicated with the third settling tank bottom feed inlet, and the third settling tank top discharge outlet is communicated with the first layering tank feed inlet.
4. The biodiesel preparation system suitable for kitchen oil according to claim 1, characterized in that: ion liquid recovery tank discharge gate department has still linked up dealcoholize jar and drain sump in proper order, dealcoholize jar feed inlet links up with ion liquid recovery tank discharge gate, the dealcoholize jar is arranged in getting rid of the methyl alcohol among the acid ionic liquid catalyst, dealcoholize jar top discharge gate is connected to the cauldron of esterifying with reuse methyl alcohol, dealcoholize jar bottom discharge gate links up with the drain sump feed inlet, the drain sump is arranged in getting rid of the water among the acid ionic liquid catalyst, the drain sump bottom discharge gate is connected to in the cauldron of esterifying with reuse acid ionic liquid catalyst.
5. The biodiesel preparation system suitable for kitchen oil according to claim 1, characterized in that: the device comprises a glycerin methanol tank, an esterification kettle, a glycerin methanol storage tank, a glycerin methanol tank, a first vacuum dealcoholization tower, a second vacuum dealcoholization tower and a second vacuum dealcoholization tower, wherein a discharge port of the glycerin methanol tank is connected with the first vacuum dealcoholization tower so as to separate methanol in glycerin, a discharge port at the upper part of the first vacuum dealcoho.
6. The biodiesel preparation system suitable for kitchen oil according to claim 1, characterized in that: a second vacuum dealcoholization tower is arranged between the second layering tank and the deodorization tower to remove methanol carried in the crude methyl ester; and the upper discharge hole of the second vacuum dealcoholization tower is also connected to the esterification kettle to introduce the methanol to the esterification kettle for recycling.
7. The biodiesel preparation system suitable for kitchen oil according to claim 1, characterized in that: the rectification cutting tower comprises a primary rectification cutting tower, a secondary rectification cutting tower and a tertiary rectification cutting tower which are sequentially connected, wherein a feed inlet of the primary rectification cutting tower is connected to a discharge outlet of the deodorization tower, a discharge outlet at the top of the primary rectification cutting tower is connected to the light biodiesel tank, and a discharge outlet at the bottom of the primary rectification cutting tower is connected with a feed inlet of the secondary rectification cutting tower; the discharge port of the top of the second-stage rectification cutting tower and the discharge port of the top of the third-stage rectification cutting tower are both connected to the biodiesel tank, the discharge port of the bottom of the second-stage rectification cutting tower is linked with the feed port of the third-stage rectification cutting tower, and the discharge port of the bottom of the third-stage rectification cutting tower is connected to the heavy biodiesel tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010335260.XA CN111471531A (en) | 2020-04-24 | 2020-04-24 | Biodiesel preparation system suitable for kitchen oil |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010335260.XA CN111471531A (en) | 2020-04-24 | 2020-04-24 | Biodiesel preparation system suitable for kitchen oil |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111471531A true CN111471531A (en) | 2020-07-31 |
Family
ID=71755646
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010335260.XA Pending CN111471531A (en) | 2020-04-24 | 2020-04-24 | Biodiesel preparation system suitable for kitchen oil |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111471531A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114214121A (en) * | 2021-12-14 | 2022-03-22 | 浙江东江能源科技有限公司 | High-quality low-sulfur-content biodiesel preparation device and preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103031215A (en) * | 2013-02-18 | 2013-04-10 | 广西合众能源股份有限公司 | Continuous production device and method of biodiesel |
| CN105695104A (en) * | 2016-03-29 | 2016-06-22 | 天津大学 | Intra-tower pump suction type high vacuum distillation method and device for precise separation of C16-C22 fatty acids |
| CN210314161U (en) * | 2019-08-15 | 2020-04-14 | 重庆市环卫集团有限公司 | Crude methyl ester dealcoholizes and takes off glycerine processing system |
-
2020
- 2020-04-24 CN CN202010335260.XA patent/CN111471531A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103031215A (en) * | 2013-02-18 | 2013-04-10 | 广西合众能源股份有限公司 | Continuous production device and method of biodiesel |
| CN105695104A (en) * | 2016-03-29 | 2016-06-22 | 天津大学 | Intra-tower pump suction type high vacuum distillation method and device for precise separation of C16-C22 fatty acids |
| CN210314161U (en) * | 2019-08-15 | 2020-04-14 | 重庆市环卫集团有限公司 | Crude methyl ester dealcoholizes and takes off glycerine processing system |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114214121A (en) * | 2021-12-14 | 2022-03-22 | 浙江东江能源科技有限公司 | High-quality low-sulfur-content biodiesel preparation device and preparation method |
| CN114214121B (en) * | 2021-12-14 | 2024-02-20 | 浙江东江能源科技有限公司 | Preparation device and preparation method of high-quality low-sulfur biodiesel |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105384639B (en) | Refined purifying plant for continuously producing LITHIUM BATTERY dimethyl carbonate | |
| CN100513521C (en) | Preparation method of biological diesel oil | |
| CN102465058A (en) | Production process for preparing biodiesel | |
| CN106929162B (en) | Acid reducing process for producing glycerol by using waste oil | |
| CN103468413A (en) | Production method of biodiesel | |
| CN104818125A (en) | Method for using waste oil and grease as raw material to prepare fatty acid methyl ester | |
| CN101423456A (en) | Recovery and purification method of glycerol as by-product of biodiesel production prepared by Jatrohpa curcas seed oil | |
| CN211170524U (en) | Preparation system of adipic acid dibasic ester | |
| CN212864611U (en) | Energy-saving and consumption-reducing ethyl acetate production line | |
| CN111471531A (en) | Biodiesel preparation system suitable for kitchen oil | |
| CN102001936A (en) | Continuous production method of propyl acetate | |
| CN103834477B (en) | The production method of a kind of glycerine fuel | |
| CN107311864A (en) | A kind of chemical purification process | |
| CN101747301B (en) | Method for preparing vitamin C with low consumption | |
| CN103087788B (en) | Method for preparing biodiesel by using high-acid value oil | |
| CN103224836B (en) | Pretreatment method of high impurity grease | |
| CN1275569A (en) | Novel process for production of vitamin C | |
| CN106929163B (en) | Acid reducing system for waste oil | |
| CN206799570U (en) | A kind of deacidification system of waste grease | |
| CN101624534B (en) | Methanol esterification method in production of biodiesel | |
| CN201353456Y (en) | Recovery device for nickel-bearing catalyst | |
| CN101067090B (en) | Solid catalysis for preparing biodiesel oil | |
| CN205258352U (en) | A refined purification device for continuous production battery level dimethyl carbonate | |
| CN207446241U (en) | A kind of biodiesel catalytic separation reaction unit | |
| CN101486923A (en) | Environment friendly process for biodiesel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |