CN109046417A - A kind of K2CO3The method of/MgLa catalyzed by solid base biodiesel synthesis - Google Patents

A kind of K2CO3The method of/MgLa catalyzed by solid base biodiesel synthesis Download PDF

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Publication number
CN109046417A
CN109046417A CN201810945089.7A CN201810945089A CN109046417A CN 109046417 A CN109046417 A CN 109046417A CN 201810945089 A CN201810945089 A CN 201810945089A CN 109046417 A CN109046417 A CN 109046417A
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mgla
solid base
oil
biodiesel
catalyzed
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刘跃进
程志鹏
潘浪胜
李勇飞
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Xiangtan University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/20—Carbon compounds
    • B01J27/232—Carbonates
    • B01J27/236—Hydroxy carbonates
    • 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
    • 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
    • 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Liquid Carbonaceous Fuels (AREA)
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Abstract

The present invention discloses a kind of K2CO3The method of/MgLa catalyzed by solid base grease and alcohols material biodiesel synthesis, the solid alkali preparation method is simple, low-temperature catalytic activity is high, easily separates with reaction system, at reaction time 2h, 55 DEG C of reaction temperature, catalyst amount 5%, alcohol oil rate 27:1, biodiesel product yield is up to 96.8%.

Description

A kind of K2CO3The method of/MgLa catalyzed by solid base biodiesel synthesis
Technical field
The invention belongs to biomass energy catalytic fields, are related to a kind of K2CO3/ MgLa catalyzed by solid base biodiesel synthesis Method.
Background technique
Biodiesel is also known as fatty acid methyl ester, is the mixing as vegetable fat and animal tallow through ester made of transesterification Object, most typically fatty acid methyl ester.Biodiesel can reduce the discharge of carbon monoxide in combustion gas, particulate matter and sulfur dioxide. There is homogeneous and heterogeneous catalysis commonly used in the catalyst of preparing biodiesel by ester exchange.Homogeneous acid-base catalysis uniform intensity, High catalytic efficiency, but there is the problems such as complicated separation, the processing of equipment burn into soda acid, discharge of wastewater.It is produced after heterogeneous catalytic reaction Object is easily separated, and catalyst can recycle again.Liu Liuchen is by template in 40%Ar-O2It protects to roast under gas and CaO/ is made ZrO2Composite oxide catalysts are applied to catalysis methanol and rapeseed oil biodiesel synthesis, catalyst amount 8% (wt), Under conditions of the molar ratio 72 of methanol and rapeseed oil, 100 DEG C of reaction temperature, reaction time 6h, the yield of biodiesel up to 91%, But its preparation process is complicated, and reaction temperature is higher, the reaction time is longer.For this problem, the present invention is by being simply co-precipitated Method prepares the uniform and stable mixed-metal oxide support of Metal Distribution, impregnates in lower alcohols solvent methanol, ethyl alcohol negative Carry K2CO3, then the K that thermal stability is good, catalytic activity is high is made in 650 DEG C of roastings in air2CO3/ MgLa solid base, for urging Carburetion rouge and methanol or ethyl alcohol biodiesel synthesis have low in raw material price, and preparation is simple, and thermal stability is good, reaction condition Mildly, catalytic activity is high, the features such as easily separating with reaction system, is 55 DEG C, catalyst amount in reaction time 2h, reaction temperature 5%, under alcohol oil rate 27:1, biodiesel oil product mass yield is up to 96.8%.
Summary of the invention
The purpose of the present invention
The present invention is intended to provide a kind of K2CO3The method of/MgLa catalyzed by solid base biodiesel synthesis.
Technical solution of the present invention
1. a kind of K2CO3The method of/MgLa catalyzed by solid base biodiesel synthesis is as follows:
(1) K described in2CO3In/MgLa solid base, K2CO3With MgLa carrier quality than 0.15~0.3:1, MgLa carrier Middle Mg, La molar ratio 1:0.25~0.5, the K2CO311~40m of/MgLa solid base specific surface2/ g, basicity pKa are 12.3~18.0.
(2) according to K described in (1)2CO3/ MgLa solid base is prepared via a method which to obtain:
1) by Mg (NO3)2.6H2O、La(NO3)3.6H2O is separately added into deionization according to Mg, La molar ratio 1:0.25~0.5 Water is configured to the Mg (NO of 0.3~1.2mol/L3)2、La(NO3)3Salting liquid, separately according to KOH and K2CO3Molar ratio is 1:0.25 ~0.33 addition deionized water is configured to the KOH/K of 0.3~0.6mol/L2CO3Mixed ammonium/alkali solutions, will be aforementioned at 25~40 DEG C Mg (NO3)2、La(NO3)3Salting liquid and KOH/K2CO3Alkali mixed ammonium/alkali solutions are slowly added to reactor simultaneously, and control maintains solution PH is 10, and is vigorously stirred 20~40min, then mixed liquor stands to 20 at 60~80 DEG C~for 24 hours, white precipitate is formed, Filtering, is washed to neutrality, filter cake is placed in 90~110 DEG C of insulating boxs dry 2~4h, then be placed in box Muffle furnace, with 3~ 5 DEG C/min heating rate is warming up to 500~650 DEG C of 3~5h of roasting and obtains a kind of MgLa carrier after cooling.
2) by K2CO3It is added respectively with above-mentioned MgLa carrier and impregnating agent according to 0.15~0.3:1:10 of mass ratio~25 anti- Device is answered, in 40~60 DEG C of dipping stirrings to solvent evaporating completely, by residual income white powdery solids in 60~80 DEG C of constant temperature Dry 2~4h in case, is placed in box Muffle furnace in 500~650 DEG C of 2~4h of roasting temperature, after cooling, obtains described K2CO3/ MgLa body alkali, the impregnating agent are deionized water, methanol, any one in ethyl alcohol.
(3) by (1), (2) described K being prepared2CO3/ MgLa solid base synthesizes life with alcohols material for being catalyzed grease The mass ratio 0.05 of 15~30:1 of molar ratio of object diesel oil, reaction raw materials alcohols material and grease, solid base catalyst and grease ~0.1:1,55~95 DEG C of reaction temperature, 1~4h of reaction time, is cooled to room temperature after reaction, and solid base is recovered by filtration and urges Agent, then after methanol washing 3 times, 40~60 DEG C of dryings cooling in 8~12 hours, in 500~650 DEG C of 1~3h of roasting as solid Body base catalyst is reused standby next time, and filtrate is sufficiently washed 3 times with saturated brine, stratification, and lower layer is glycerol, unreacted In addition methanol is handled with saturated brine mixture, upper layer is yellow solution, and wherein excessive alcohols material, centrifugation divide for evaporation recycling From, to get target product biodiesel, product quality yield is described greater than 92% after residual catalyst powder a small amount of in concentrate Grease includes soybean oil, palm oil, castor oil, rapeseed oil, gutter oil, and the alcohols material includes methanol, ethyl alcohol.
Preferably, it under 55 DEG C of reaction temperature, catalyst amount 5%, alcohol oil rate 27:1, reacts 1 hour biodiesel and produces Quality yield 92.2% reacts 2 hours biodiesel oil product mass yields 96.8%.
Technical characterstic and effect of the invention
1 use preparation process is simple, preparation condition is easily controllable, synthesis cycle is short, metal component distribution is equal in catalyst The Co deposited synthesis metal composite oxide carrier MgLa of the advantages that even, through 500~650 DEG C roasting after, then with K2CO3It is soaking It impregnates in stain agent, is finally roasted at 500~650 DEG C, obtain a kind of novel K2CO3/ MgLa solid base.
2K2CO3The advantageous effect that/MgLa solid base has low temperature high catalytic activity short with the reaction time, for being catalyzed grease 1 hour biology is reacted as 55 DEG C of reaction temperature, catalyst amount 5%, alcohol oil rate 27:1 with alcohols material biodiesel synthesis Diesel product mass yield reacts 2 hours biodiesel oil product mass yields up to 96.8% up to 92.2%.
Detailed description of the invention
Fig. 1 is Mg-La carrier and different loads amount K2CO3The XRD spectra of/MgLa, (a) be Mg-La, (b), (c), (d), (e) K is respectively corresponded2CO3The K of load capacity 20%, 5%, 15%, 30%2CO3/ MgLa is consulted known to PDF card in 2 θ=15.4 °, 27.6 ° be La (OH)3Characteristic peak, in 2 θ=25.9 °, 29.8 °, 39.2 °, 45.8 °, 52.2 °, 55.6 °, 75.3 °, 79.0 ° For La2O3Characteristic peak is MgO characteristic peak in 2 θ=42.9 °, 62.1 °.La2O3Interaction prevents crystallite from reuniting between MgO, sees Examine K2CO3/ MgLa diffraction curve is La in 2 θ=10.8 °, 22.2 °, 25.7 °, 33.8 °, 44.5 °, 47.6 °, 50.3 °2O2 (CO3)3Characteristic diffraction peak loads K2CO3New crystal phase is formd afterwards, illustrates K2CO3Instead of simple physical does not carry between carrier, New chemical bonding being formed, and as load capacity increases, blue shift occurs for peak position, illustrate that crystal particle diameter increases, this is because K2CO3Load capacity increases, the reason that spacing of lattice increases.
Fig. 2 a, b are Mg-La and K2CO3The N of/MgLa2Adsorption/desorption curve, it is seen that K2CO3/ MgLa solid base catalyst exists Relative pressure P/P0When being 0.05~0.3, adsorption curve and desorption curve are almost overlapped, in relative pressure P/P00.3~0.9 In range, desorption curve is slightly below adsorption curve, this is because specific surface area of catalyst is too small and catalysis when characterizing Error produced by agent dosage is less belongs to nominal error range.In relative pressure P/P0In 0.9~1.0 range, when adsorption curve There are hysteresis loops between desorption curve, this is because illustrating that catalyst has a small amount of mesoporous presence produced by capillary condensation phenomenon.
Fig. 3 is Mg-La and K2CO3/ MgLa infrared spectrogram, wherein (a) is Mg-La, (b) is K2CO3/MgLa.Infrared In spectrogram, 3410cm-1There are superabsorbent peak, the mainly stretching vibration peak of O-H in place；1623cm-1Nearby there is hydrone H- O-H bending vibration absorption peak, this is because in a small amount of air caused by water absorption on a catalyst；In 1400cm-1Place is CO3 2-'s C-O vibration peak, in 404cm-1、478cm-1、615cm-1、1079cm-1Place is the M-O skeletal vibration absorption peak of metal cation M, M Represent Mg, La metal ion.
Specific embodiment
Technical solutions and their implementation methods of the present invention are explained below by embodiment, but technical side of the invention Case and its implementation method are not limited to following embodiment.
Embodiment 1
1. solid base K2CO3The preparation of/MgLa
By Mg (NO3)2.6H2O、La(NO3)3.6H2O by Mg, La molar ratio be 1:0.33 be separately added into it is a certain amount of go from Sub- water is stirred the Mg (NO for being configured to 1mol/L3)2, 0.33mol/L La (NO3)3Salting liquid, separately according to KOH and K2CO3It rubs You are than being added the KOH/K that deionized water is configured to 0.4mol/L for 4:12CO3Mixed ammonium/alkali solutions are at 30 DEG C by Mg above-mentioned (NO3)2、La(NO3)3Salting liquid and KOH/K2CO3Alkali mixed ammonium/alkali solutions are slowly added to reactor simultaneously, and control maintenance pH value of solution is 10, and it is vigorously stirred 30min, then be warming up to 75 DEG C and stir at low speed 8h, it naturally rings to be stored at room temperature 8h, forms white precipitate, mistake Filter, is washed to neutrality, filter cake is placed in 100 DEG C of insulating boxs dry 4h, then be placed in box Muffle furnace, with 3 DEG C/min heating Rate is warming up to 650 DEG C of roasting 4h and obtains a kind of MgLa carrier, specific surface area 37.7m after cooling2/g。
By K2CO3, MgLa and methanol stirring 8h is impregnated at 40 DEG C according to mass ratio 0.2:1:15 to methanol evaporating completely, Gained residue white powdery solids are dried into 3h in 80 DEG C of insulating boxs, then are placed in 3 DEG C/min heating speed in box Muffle furnace Rate, which is warming up at 630 DEG C, roasts 4h, after cooling, obtains 20%K2CO3/ MgLa solid base, specific surface area 11.9m2/g。
By 20%K obtained by 2g2CO3/ MgLa solid base catalyst, 40g methanol, 39.5g soybean oil (methanol and soybean The molar ratio of oil is 27:1) it is added in reactor, reaction temperature is 55 DEG C, and reaction time 2h is cooled to after reaction The solid base catalyst is recovered by filtration in room temperature, washs 3 times, 55 DEG C of cooling repetitions standby next times in drying 12 hours through methanol It uses, filtrate is sufficiently washed 3 times with saturated brine, stratification, and lower layer is glycerol, unreacted methanol and saturated brine mixture In addition it handles, upper layer is yellow solution, and wherein excessive methanol, a small amount of residual catalyst in rotary-classify technology liquid are recycled in evaporation To get target product biodiesel after powder, biodiesel product quality yield is 96.8%.
(comparative example) operating procedure of embodiment 2 is with embodiment 1, but solid base is 5%K2CO3/ MgLa, i.e. K2CO3With MgLa Carrier quality ratio 0.05:1, reaction time 4h, 85 DEG C of reaction temperature, obtaining biodiesel product quality yield is 57%.
3 operating procedure of embodiment is with embodiment 1, but solid base is 15%K2CO3/ MgLa, i.e. K2CO3With MgLa carrier matter Amount is than 0.15:1, reaction time 4h, and 85 DEG C of reaction temperature, obtaining biodiesel product quality yield is 93.3%.
4 operating procedure of embodiment is with embodiment 1, but solid base is 30%K2CO3/ MgLa, i.e. K2CO3With MgLa carrier matter Amount is than 0.15:1, reaction time 4h, and 85 DEG C of reaction temperature, obtaining biodiesel product quality yield is 93.8%.
(comparative example) operating procedure of embodiment 5 is with embodiment 1, but reaction temperature is 35 DEG C, obtains biodiesel product quality Yield is 13.2%.
(comparative example) operating procedure of embodiment 6 is with embodiment 1, but reaction temperature is 45 DEG C, obtains biodiesel product quality Yield is 29.5%.
7 operating procedure of embodiment is with embodiment 1, but reaction temperature is 65 DEG C, and obtaining biodiesel product quality yield is 94.8%.
8 operating procedure of embodiment is with embodiment 1, but reaction temperature is 85 DEG C, and obtaining biodiesel product quality yield is 95.2%.
9 operating procedure of embodiment is with embodiment 1, but reaction temperature is 95 DEG C, and obtaining biodiesel product quality yield is 96%.
(comparative example) operating procedure of embodiment 10 is with embodiment 1, but the reaction time is 0.5h, obtains biodiesel product quality Yield is 86.9%.
11 operating procedure of embodiment is with embodiment 1, but the reaction time is 1h, and obtaining biodiesel product quality yield is 92.2%.
12 operating procedure of embodiment is with embodiment 1, but the reaction time is 3h, and obtaining biodiesel product quality yield is 95.5%.
13 operating procedure of embodiment is with embodiment 1, but the reaction time is 4h, and obtaining biodiesel product quality yield is 94.6%.
(comparative example) operating procedure of embodiment 14 is with embodiment 1, but the molar ratio of methanol and soybean oil is 15:1, is obtained biological Diesel product mass yield is 53.1%.
(comparative example) operating procedure of embodiment 15 is with embodiment 1, but the molar ratio of methanol and soybean oil is 20:1, is obtained biological Diesel product mass yield is 61.8%.
(comparative example) operating procedure of embodiment 16 is with embodiment 1, but the molar ratio of methanol and soybean oil is 25:1, is obtained biological Diesel product mass yield is 87.7%.
(comparative example) operating procedure of embodiment 17 is with embodiment 1, but the molar ratio of methanol and soybean oil is 35:1, is obtained biological Diesel product mass yield is 82.2%.
(comparative example) operating procedure of embodiment 18 is with embodiment 1, but catalyst and soybean oil mass ratio are 0.01:1, obtain life Object diesel product mass yield is 1.8%.
(comparative example) operating procedure of embodiment 19 is with embodiment 1, but catalyst and soybean oil mass ratio are 0.03:1, obtain life Object diesel product mass yield is 39.1%.
20 operating procedure of embodiment is with embodiment 1, but catalyst and soybean oil mass ratio are 0.07:1, obtains biodiesel production Amount of substance yield is 94.8%.
21 operating procedure of embodiment is with embodiment 1, but catalyst and soybean oil mass ratio are 0.10:1, obtains biodiesel production Amount of substance yield is 93.6%.
2 Examples 1 to 2 of table, 1 reaction condition and result
It * is comparative example.

Claims (2)

1. a kind of K2CO3The method of/MgLa catalyzed by solid base biodiesel synthesis, it is characterized in that:
(1) K described in2CO3In/MgLa solid base, K2CO3With MgLa carrier quality than 0.15 ~ 0.3:1, Mg, La in MgLa carrier Molar ratio 1:0.25 ~ 0.5；
The K2CO311 ~ 40m2/g of/MgLa solid base specific surface, basicity pKa are 12.3 ~ 18.0；
(2) according to K described in (1)2CO3/ MgLa solid base is prepared via a method which to obtain:
1) by Mg (NO3)2.6H2O、La(NO3)3.6H2O is separately added into deionized water according to Mg, La molar ratio 1:0.25 ~ 0.5 and matches Mg (the NO of 0.3 ~ 1.2mol/L is made3)2、La(NO3)3Salting liquid, separately according to KOH and K2CO3Molar ratio adds for 1:0.25 ~ 0.33 Enter the KOH/K that deionized water is configured to 0.3 ~ 0.6mol/L2CO3Mixed ammonium/alkali solutions, by Mg (NO above-mentioned at 25 ~ 40 DEG C3)2、 La(NO3)3Salting liquid and KOH/K2CO3Alkali mixed ammonium/alkali solutions are slowly added to reactor simultaneously, and it is 10 that control, which maintains pH value of solution, and It it is vigorously stirred 20 ~ 40min, then mixed liquor stands to 20 at 60 ~ 80 DEG C ~ for 24 hours, forms white precipitate, filtering is washed to Property, filter cake is placed in 90 ~ 110 DEG C of insulating boxs dry 2 ~ 4h, then be placed in box Muffle furnace, with 3 ~ 5 DEG C/min heating rate It is warming up to 500 ~ 650 DEG C of 3 ~ 5h of roasting and obtains a kind of MgLa carrier after cooling；
2) by K2CO3Reactor is added according to 0.15 ~ 0.3:1:10 of mass ratio ~ 25 with above-mentioned MgLa carrier and impregnating agent respectively, The stirring of 40 ~ 60 DEG C of dippings to solvent evaporating completely, by residual income white powdery solids dry 2 in 60 ~ 80 DEG C of insulating boxs ~ 4h is placed in box Muffle furnace in 500 ~ 650 DEG C of 2 ~ 4h of roasting temperature, after cooling, obtains the K2CO3/ MgLa solid Alkali；The impregnating agent is deionized water, methanol, any one in ethyl alcohol；
(3) by (1), (2) described K being prepared2CO3/ MgLa solid base is for being catalyzed grease and alcohols material synthesising biological bavin The mass ratio 0.05 ~ 0.1 of 15 ~ 30:1 of molar ratio of oil, reaction raw materials alcohols material and grease, solid base catalyst and grease: 1,55 ~ 95 DEG C of reaction temperature, 1 ~ 4h of reaction time are cooled to room temperature after reaction, solid base catalyst are recovered by filtration, then pass through Methanol washs 3 times, after 40 ~ 60 DEG C of drying cooling in 8 ~ 12 hours, 500 ~ 650 DEG C of 1 ~ 3h of roasting as solid base catalyst under Secondary reuse, filtrate are sufficiently washed 3 times with saturated brine, stratification, and lower layer is glycerol, unreacted methanol and saturated brine In addition mixture is handled, upper layer is yellow solution, is evaporated and is recycled wherein excessive alcohols material, a small amount of in rotary-classify technology liquid To get target product biodiesel after residual catalyst powder, product quality yield is greater than 92%；
The grease includes soybean oil, palm oil, castor oil, rapeseed oil, gutter oil, and the alcohols material includes methanol, ethyl alcohol.
2. a kind of K as described in claim 12CO3The method of/MgLa catalyzed by solid base biodiesel synthesis, it is characterized in that: institute State K2CO3/ MgLa solid base has low temperature high catalytic activity, and the reaction time is short, for being catalyzed grease and alcohols material synthesising biological Diesel oil under 55 DEG C of reaction temperature, catalyst amount 5%, alcohol oil rate 27:1, reacts 1 hour biodiesel oil product mass yield 92.2%, react 2 hours biodiesel oil product mass yields 96.8%.
CN201810945089.7A 2018-08-17 2018-08-17 A kind of K2CO3The method of/MgLa catalyzed by solid base biodiesel synthesis Pending CN109046417A (en)

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