CN107029695A - A kind of biodiesel prepares the preparation method of special solid base catalyst - Google Patents
A kind of biodiesel prepares the preparation method of special solid base catalyst Download PDFInfo
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- CN107029695A CN107029695A CN201710337145.4A CN201710337145A CN107029695A CN 107029695 A CN107029695 A CN 107029695A CN 201710337145 A CN201710337145 A CN 201710337145A CN 107029695 A CN107029695 A CN 107029695A
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- solid base
- base catalyst
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- 239000007787 solid Substances 0.000 title claims abstract description 44
- 239000003054 catalyst Substances 0.000 title claims abstract description 38
- 239000003225 biodiesel Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical class [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 18
- 239000000839 emulsion Substances 0.000 claims abstract description 18
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims abstract description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 37
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 20
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 239000003755 preservative agent Substances 0.000 claims description 12
- 230000002335 preservative effect Effects 0.000 claims description 12
- 238000009413 insulation Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 9
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 9
- 239000003995 emulsifying agent Substances 0.000 claims description 7
- 238000007789 sealing Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 239000003643 water by type Substances 0.000 claims description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 4
- 150000002689 maleic acids Chemical class 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 229920001214 Polysorbate 60 Polymers 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 6
- 229920000642 polymer Polymers 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000001802 infusion Methods 0.000 abstract description 2
- 239000004005 microsphere Substances 0.000 abstract description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 abstract description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 abstract description 2
- 239000011736 potassium bicarbonate Substances 0.000 abstract description 2
- 239000004793 Polystyrene Substances 0.000 abstract 2
- 229920002223 polystyrene Polymers 0.000 abstract 2
- 239000004480 active ingredient Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 27
- 239000002585 base Substances 0.000 description 27
- 239000012065 filter cake Substances 0.000 description 10
- 239000002699 waste material Substances 0.000 description 10
- 239000003513 alkali Substances 0.000 description 7
- 230000033228 biological regulation Effects 0.000 description 7
- 239000003921 oil Substances 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 239000008162 cooking oil Substances 0.000 description 6
- 239000002283 diesel fuel Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 125000004185 ester group Chemical group 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 229910001420 alkaline earth metal ion Inorganic materials 0.000 description 3
- 235000013361 beverage Nutrition 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 238000013517 stratification Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000003760 magnetic stirring Methods 0.000 description 2
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 2
- 229910001950 potassium oxide Inorganic materials 0.000 description 2
- 235000019394 potassium persulphate Nutrition 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 1
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 150000001491 aromatic compounds Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 235000012255 calcium oxide Nutrition 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 description 1
- 239000000686 essence Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000004494 ethyl ester group Chemical group 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229960001545 hydrotalcite Drugs 0.000 description 1
- 229910001701 hydrotalcite Inorganic materials 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 235000012245 magnesium oxide Nutrition 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical class [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 229960003975 potassium Drugs 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Classifications
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/02—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the alkali- or alkaline earth metals or beryllium
- B01J23/04—Alkali metals
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses the preparation method that a kind of biodiesel prepares special solid base catalyst, belong to field of new energy technologies.The present invention is surfactant first with neopelex, and saturated sodium bicarbonate solution is made at relatively high temperatures, polymerisation is carried out in same container polystyrene emulsion is made again, utilize emulsion microballoon adsorption saturation potassium bicarbonate solution, tetraethyl orthosilicate is then added dropwise, it is allowed to hydrolyze, and it is coated on emulsion microsphere surface, saleratus is decomposed under the conditions of relatively lower temp, produce gas, loose structure is formed, then polystyrene kernel is removed through comparative high temperature calcining, obtained biodiesel prepares special solid base catalyst.The present invention adsorbs saleratus using polymer emulsion, and calcined through two steps, form spongy porosu solid base catalyst, carrier and active ingredient are all loose structure, the problem of catalyst made from efficiently solving traditional infusion process easily blocks duct, influence catalytic efficiency.
Description
Technical field
The invention discloses the preparation method that a kind of biodiesel prepares special solid base catalyst, belong to new energy technology
Field.
Background technology
Biodiesel is a kind of using vegetable and animals oils as primary raw material, occurs the aliphatic acid that ester exchange reaction is obtained with short chain alcohol
First Ester, with Cetane number is high, sulfur-bearing and aromatic compound, biodegradable, nontoxic, flash-point be not high compared with mineralising diesel oil
The advantages of, it is a kind of new environmentally friendly energy.With basic species such as hydroxide on solid base catalyst and traditional handicraft
Matter is compared to carry out ester exchange reaction, and reaction condition is gentle, shows good catalytic activity, is easily separated from product, instead
Rear catalyst regenerating easily is answered, it is small to equipment corrosion, and post processing is simple, without repeatedly washing, can avoid a large amount of waste liquids
Discharge.
Solid base refers to that the solid of electronics can be given to reactant.There should be extremely strong confession as its activated centre of catalyst
Electronic capability, it has a surface anion vacancy.Different with the property of active sites according to carrier, solid base can substantially be divided into oxygen
The intrinsic solid base of compound, load-type solid etc..
The intrinsic solid base of oxide for ester exchange includes alkali and alkaline earth metal ions oxide type and combined oxidation
Thing type solid base.Alkali and alkaline earth metal ions oxide type solid base research it is more early, and compound oxide type solid base then often with
Hydrotalcite type is that presoma roasting is formed.Such specific surface area of catalyst is relatively low, easily absorbs water and carbon dioxide, easily with
Reaction is mixed to form slurry and makes product separation difficult, and has to pre-process under high temperature and high vacuum condition and can just show
Catalytic activity, therefore by a definite limitation in practice.
Load type solid body base catalyst is because with preparing simple, relatively large specific surface area, uniform pore diameter and alkalescence is strong etc.
Advantage and as prepare biodiesel solid catalyst study hotspot.Load-type solid for preparing biodiesel has
Aluminum oxide, calcium and magnesium oxides, zirconium oxide etc..On the whole, the solid alkali preparation method prepared by carrier of aluminum oxide is simple, alkali
Intensity is high, and mechanical strength and heat endurance are good, is to be catalyzed in grease ester exchange reaction a kind of relatively promising catalyst, but its
Have the disadvantage to use infusion process in preparation process, solid base is carried on carrier surface, block carrier pore structure, aluminum oxide
Specific surface area can decrease after load active component, repeat to make because of a small amount of be lost in while the active component of load is present
There is the phenomenon of yield decline in used time.Therefore urgently find a kind of specific surface area big, can largely improve urging for biodiesel production rate
Agent.
The content of the invention
The present invention solves the technical problem of：Solid base catalyst used is prepared using leaching for traditional biological diesel oil
Stain method, carrier surface is carried on by solid base, blocks carrier pore structure, causes carrier specific surface area to decline, the biological bavin of influence
The problem of oily yield, there is provided the preparation method that a kind of biodiesel prepares special solid base catalyst.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
（1）In three-necked flask, 150~200mL deionized waters, 0.1~0.3g emulsifying agents are sequentially added, then three-necked flask is moved
Enter digital display to test the speed in constant temperature blender with magnetic force, constant temperature stirring 10~20min of mixing, then under constant temperature stirring, Xiang Sankou
Saleratus is added in flask, untill saleratus no longer dissolves, saturated potassium hydrogen carbonate solution is obtained；
（2）Nitrogen is passed through into above-mentioned saturated potassium hydrogen carbonate solution with 3~5mL/min speed, under nitrogen guard mode, upwards
State and 20~30mL styrene is sequentially added in three-necked flask, 6~8mL mass fractions are 20~25% potassium persulfate solutions, are continued at
Temperature is 75~80 DEG C, and rotating speed is under the conditions of 600~800r/min, constant temperature 8~12h of stirring reaction obtains mixed emulsion；
（3）Measure in the above-mentioned gained mixed emulsions of 100~150mL, the three-necked flask for pouring into belt stirrer, under room temperature condition,
Speed of agitator is adjusted to 400~600r/min, under stirring, 10~20mL is added dropwise into three-necked flask by dropping funel
Tetraethyl orthosilicate, control is dripped off in 10~15min, is treated completion of dropping, is continued at 3~5h of stirring reaction under room temperature condition, then
Material in three-necked flask is transferred in beaker, and sealed beaker with preservative film, then beaker is placed in baking oven, 5~7 are placed
My god；
（4）It is to be placed to terminate, beaker sealing preservative film is opened, and will be calcined in beaker after material filtering drying, discharging is produced
Biodiesel prepares special solid base catalyst.
Step（1）Described emulsifying agent be neopelex, OP-10, Tween-60, Si Pan -80 in one kind or
Two kinds.
Step（2）In described styrene, 4~6g acrylic acid and 1~3g maleic acids can also be added.
Step（2）In described potassium persulfate solution, 0.03~0.05g azodiisobutyronitriles can also be added.
Step（4）Described calcination condition is：In Muffle furnace, 200~220 are warming up to 2~4 DEG C/min rate programs
DEG C, insulation 90~120min of calcining, then temperature programming is continued to 500~550 DEG C with 6~8 DEG C/min speed, insulation calcining 3~
5h, cools to room temperature with the furnace.
The beneficial effects of the invention are as follows：
（1）The present invention is mixed first with emulsifying agent and water, and adds saleratus, and unsaturated carbonate hydrogen is made at relatively high temperatures
Potassium solution, in same system, is coordinated as initiator using potassium peroxydisulfate and azodiisobutyronitrile, triggers styrene, propylene
Polymerisation occurs for acid and maleic acid, and saturated potassium hydrogen carbonate solution is wrapped in microballoon by the polymer emulsion microballoon of formation, and
The silica that the carboxyl isoreactivity group of polymer emulsion microsphere surface can produce teos hydrolysis is adsorbed in microballoon
Surface；
（2）The present invention is in cooling and drying course, and saleratus crystal is gradually separated out, and is distributed in inside polymer microballoon,
In later stage calcination process, saleratus is decomposed, and produces carbon dioxide and water vapour volatilization, and polymer is gradually removed through calcining,
Ultimately form using potassium oxide and silica as the spongy porosu solid base catalyst of main component, wherein potassium oxide is effective
Composition, silica is carrier, and both are organically combined, and both are all loose structure, and specific surface area is big, is using process
In, reactant can be penetrated into effectively in catalyst pores gap structure, be not easily blocked duct, be improved catalytic efficiency.
Embodiment
In three-necked flask, 150~200mL deionized waters are sequentially added, 0.1~0.3g emulsifying agents, then by three-necked flask
Digital display is moved into test the speed in constant temperature blender with magnetic force, in temperature be 70~75 DEG C, under the conditions of rotating speed is 300~500r/min, constant temperature
Stirring 10~20min of mixing, then under constant temperature stirring, saleratus is added into three-necked flask, until saleratus
Untill no longer dissolving, saturated potassium hydrogen carbonate solution is obtained；Described emulsifying agent be neopelex, OP-10, Tween-60,
One or both of Si Pan -80；Nitrogen is passed through into above-mentioned saturated potassium hydrogen carbonate solution with 3~5mL/min speed, in nitrogen
Under guard mode, 20~30mL styrene is sequentially added into above-mentioned three-necked flask, 4~6g acrylic acid, 1~3g maleic acids, 6~
8mL mass fractions are 20~25% potassium persulfate solutions and 0.03~0.05g azodiisobutyronitriles, and it is 75~80 to continue at temperature
DEG C, rotating speed is under the conditions of 600~800r/min, constant temperature 8~12h of stirring reaction obtains mixed emulsion；Measure 100~150mL above-mentioned
In gained mixed emulsion, the three-necked flask for pouring into belt stirrer, under room temperature condition, regulation speed of agitator to 400~600r/
Min, under stirring, 10~20mL tetraethyl orthosilicates are added dropwise into three-necked flask by dropping funel, control 10~
Dripped off in 15min, treat completion of dropping, continue at 3~5h of stirring reaction under room temperature condition, then material in three-necked flask is transferred to burning
In cup, and beaker is sealed with preservative film, then beaker is placed in baking oven, under the conditions of temperature is 65~70 DEG C, place 5~7
My god；It is to be placed to terminate, above-mentioned beaker sealing preservative film is opened, and by material filtering in beaker, collect filter cake, and gained is filtered
Cake is placed in baking oven, is dried under the conditions of temperature is 105~110 DEG C and is transferred to Muffle furnace to constant weight, then by dried filter cake, with
2~4 DEG C/min rate programs are warming up to 200~220 DEG C, and 90~120min is calcined in insulation, then is continued with 6~8 DEG C/min speed
Temperature programming to 500~550 DEG C, insulation calcining 3~5h, cool to room temperature with the furnace, discharge, produce biodiesel prepare it is special solid
Body base catalyst.
Example 1
In three-necked flask, 200mL deionized waters, 0.3g neopelexes are sequentially added, then three-necked flask is moved into
Digital display tests the speed in constant temperature blender with magnetic force, is 75 DEG C in temperature, rotating speed mixes 20min under the conditions of 500r/min, constant temperature is stirred,
Then under constant temperature stirring, saleratus is added into three-necked flask, untill saleratus no longer dissolves, saturation is obtained
Potassium bicarbonate solution；Nitrogen is passed through into above-mentioned saturated potassium hydrogen carbonate solution with 5mL/min speed, under nitrogen guard mode,
Sequentially add 30mL styrene into above-mentioned three-necked flask, 6g acrylic acid, 3g maleic acids, 8mL mass fractions are 25% potassium peroxydisulfate
Solution and 0.05g azodiisobutyronitriles, continue at temperature for 80 DEG C, under the conditions of rotating speed is 800r/min, constant temperature stirring reaction
12h, obtains mixed emulsion；Measure in the above-mentioned gained mixed emulsions of 150mL, the three-necked flask for pouring into belt stirrer, in room temperature condition
Under, under stirring, the positive silicic acid of 20mL is added dropwise by dropping funel to 600r/min into three-necked flask for regulation speed of agitator
Ethyl ester, control is dripped off in 15min, treats completion of dropping, continues at stirring reaction 5h under room temperature condition, then by thing in three-necked flask
Material is transferred in beaker, and is sealed beaker with preservative film, then beaker is placed in baking oven, under the conditions of temperature is 70 DEG C, places 7
My god；It is to be placed to terminate, above-mentioned beaker sealing preservative film is opened, and by material filtering in beaker, collect filter cake, and gained is filtered
Cake is placed in baking oven, is to dry under the conditions of 110 DEG C to constant weight, then by dried filter cake to be transferred to Muffle furnace in temperature, with 4 DEG C/
Min rate programs are warming up to 220 DEG C, and 120min is calcined in insulation, then continues temperature programming to 550 DEG C with 8 DEG C/min speed, insulation
5h is calcined, room temperature is cooled to the furnace, is discharged, is produced biodiesel and prepare special solid base catalyst.
Count by weight, 80 parts of waste cooking oils are taken successively, 6 parts of present invention gained biodiesel prepare special solid alkali and urged
Agent, 200 parts of methanol, first pours into waste cooking oil in reactor, and regulation speed of agitator is preheated to 65 to 600r/min
DEG C, biodiesel obtained by the addition present invention prepares special solid base catalyst and methanol, constant temperature stirring reaction under stirring
2h, is recovered by filtration catalyst, and excessive methanol is reclaimed in the rotated evaporation of filtrate, and remaining liq stratification collects the rough life in upper strata
Thing diesel oil, under the conditions of vacuum is 0.085MPa, collects the cut that gas phase temperature is 180 DEG C, obtains pale yellow colour biological bavin
Oil.
The biodiesel of table 1 prepares the Reusability that special solid base catalyst is catalyzed preparing biodiesel by food and beverage waste oil：
| Access times | 1 | 2 | 3 | 4 | 5 |
| Biodiesel production rate（%） | 94.6 | 93.1 | 91.6 | 89.2 | 88.9 |
Table 1
Example 2
In three-necked flask, 150mL deionized waters are sequentially added, 0.1g Si Pan -80, then three-necked flask immigration digital display is tested the speed perseverance
It it is 70 DEG C in temperature, rotating speed is under the conditions of 300r/min, constant temperature stirring mixes 10min, then in constant temperature in warm magnetic stirring apparatus
Under stirring, saleratus is added into three-necked flask, untill saleratus no longer dissolves, saturated potassium hydrogen carbonate is obtained molten
Liquid；Nitrogen is passed through into above-mentioned saturated potassium hydrogen carbonate solution with 3mL/min speed, under nitrogen guard mode, to above-mentioned three mouthfuls
20mL styrene is sequentially added in flask, 6mL mass fractions are 20% potassium persulfate solution, and it is 75 DEG C to continue at temperature, and rotating speed is
Under the conditions of 600r/min, constant temperature stirring reaction 8h obtains mixed emulsion；The above-mentioned gained mixed emulsions of 100mL are measured, band stirring is poured into
In the three-necked flask of device, under room temperature condition, regulation speed of agitator under stirring, passes through dropping funel to 400r/min
10mL tetraethyl orthosilicates are added dropwise into three-necked flask, control drips off in 10min, treats completion of dropping, continue under room temperature condition
Stirring reaction 3h, then material in three-necked flask is transferred in beaker, and sealed beaker with preservative film, then beaker is placed in baking oven
In, under the conditions of temperature is 65 DEG C, place 5 days；It is to be placed to terminate, above-mentioned beaker sealing preservative film is opened, and by beaker
Material filtering, collects filter cake, and gained filter cake is placed in baking oven, is dried under the conditions of temperature is 105 DEG C to constant weight, then will be dry
Filter cake after dry is transferred to Muffle furnace, is warming up to 200 DEG C with 2 DEG C/min rate programs, 90min is calcined in insulation, then with 6 DEG C/min speed
Rate continues temperature programming to 500 DEG C, insulation calcining 3h, cools to room temperature with the furnace, discharges, produce biodiesel and prepare special solid
Base catalyst.
Count by weight, 90 parts of waste cooking oils are taken successively, 7 parts of present invention gained biodiesel prepare special solid alkali and urged
Agent, 260 parts of methanol, first pours into waste cooking oil in reactor, and regulation speed of agitator is preheated to 68 to 700r/min
DEG C, biodiesel obtained by the addition present invention prepares special solid base catalyst and methanol, constant temperature stirring reaction under stirring
3h, is recovered by filtration catalyst, and excessive methanol is reclaimed in the rotated evaporation of filtrate, and remaining liq stratification collects the rough life in upper strata
Thing diesel oil, under the conditions of vacuum is 0.088MPa, collects the cut that gas phase temperature is 200 DEG C, obtains pale yellow colour biological bavin
Oil.
The biodiesel of table 2 prepares the Reusability that special solid base catalyst is catalyzed preparing biodiesel by food and beverage waste oil：
| Access times | 1 | 2 | 3 |
| Biodiesel production rate（%） | 92.5 | 90.8 | 87.6 |
Table 2
Example 3
In three-necked flask, 170mL deionized waters are sequentially added, 0.2g Tween-60s, then three-necked flask immigration digital display is tested the speed perseverance
It it is 72 DEG C in temperature, rotating speed is under the conditions of 400r/min, constant temperature stirring mixes 15min, then in constant temperature in warm magnetic stirring apparatus
Under stirring, saleratus is added into three-necked flask, untill saleratus no longer dissolves, saturated potassium hydrogen carbonate is obtained molten
Liquid；Nitrogen is passed through into above-mentioned saturated potassium hydrogen carbonate solution with 4mL/min speed, under nitrogen guard mode, to above-mentioned three mouthfuls
25mL styrene is sequentially added in flask, 7mL mass fractions are 23% potassium persulfate solution, and it is 77 DEG C to continue at temperature, and rotating speed is
Under the conditions of 700r/min, constant temperature stirring reaction 9h obtains mixed emulsion；The above-mentioned gained mixed emulsions of 120mL are measured, band stirring is poured into
In the three-necked flask of device, under room temperature condition, regulation speed of agitator under stirring, passes through dropping funel to 500r/min
15mL tetraethyl orthosilicates are added dropwise into three-necked flask, control drips off in 12min, treats completion of dropping, continue under room temperature condition
Stirring reaction 4h, then material in three-necked flask is transferred in beaker, and sealed beaker with preservative film, then beaker is placed in baking oven
In, under the conditions of temperature is 67 DEG C, place 6 days；It is to be placed to terminate, above-mentioned beaker sealing preservative film is opened, and by beaker
Material filtering, collects filter cake, and gained filter cake is placed in baking oven, is dried under the conditions of temperature is 107 DEG C to constant weight, then will be dry
Filter cake after dry is transferred to Muffle furnace, is warming up to 210 DEG C with 3 DEG C/min rate programs, 100min is calcined in insulation, then with 7 DEG C/min
Speed continue temperature programming to 520 DEG C, insulation calcining 4h, cool to room temperature with the furnace, discharge, produce biodiesel prepare it is special solid
Body base catalyst.
Count by weight, 100 parts of waste cooking oils are taken successively, 8 parts of present invention gained biodiesel prepare special solid alkali
Catalyst, 300 parts of methanol, first pours into waste cooking oil in reactor, and regulation speed of agitator is preheated to 70 to 800r/min
DEG C, biodiesel obtained by the addition present invention prepares special solid base catalyst and methanol, constant temperature stirring reaction under stirring
4h, is recovered by filtration catalyst, and excessive methanol is reclaimed in the rotated evaporation of filtrate, and remaining liq stratification collects the rough life in upper strata
Thing diesel oil, under the conditions of vacuum is 0.095MPa, collects the cut that gas phase temperature is 220 DEG C, obtains pale yellow colour biological bavin
Oil.
The biodiesel of table 3 prepares the Reusability that special solid base catalyst is catalyzed preparing biodiesel by food and beverage waste oil：
| Access times | 1 | 2 | 3 | 4 |
| Biodiesel production rate（%） | 93.1 | 91.8 | 88.3 | 86.9 |
Table 3
Above-described embodiment is not limited for the present invention preferably embodiment, but embodiments of the present invention by above-described embodiment
System, other any Spirit Essences without departing from the present invention and the change made under principle, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (5)
1. a kind of biodiesel prepares the preparation method of special solid base catalyst, it is characterised in that specifically preparation process is：
（1）In three-necked flask, 150~200mL deionized waters, 0.1~0.3g emulsifying agents are sequentially added, then three-necked flask is moved
Enter digital display to test the speed in constant temperature blender with magnetic force, constant temperature stirring 10~20min of mixing, then under constant temperature stirring, Xiang Sankou
Saleratus is added in flask, untill saleratus no longer dissolves, saturated potassium hydrogen carbonate solution is obtained；
（2）Nitrogen is passed through into above-mentioned saturated potassium hydrogen carbonate solution with 3~5mL/min speed, under nitrogen guard mode, upwards
State and 20~30mL styrene is sequentially added in three-necked flask, 6~8mL mass fractions are 20~25% potassium persulfate solutions, are continued at
Temperature is 75~80 DEG C, and rotating speed is under the conditions of 600~800r/min, constant temperature 8~12h of stirring reaction obtains mixed emulsion；
（3）Measure in the above-mentioned gained mixed emulsions of 100~150mL, the three-necked flask for pouring into belt stirrer, under room temperature condition,
Speed of agitator is adjusted to 400~600r/min, under stirring, 10~20mL is added dropwise into three-necked flask by dropping funel
Tetraethyl orthosilicate, control is dripped off in 10~15min, is treated completion of dropping, is continued at 3~5h of stirring reaction under room temperature condition, then
Material in three-necked flask is transferred in beaker, and sealed beaker with preservative film, then beaker is placed in baking oven, 5~7 are placed
My god；
（4）It is to be placed to terminate, beaker sealing preservative film is opened, and will be calcined in beaker after material filtering drying, discharging is produced
Biodiesel prepares special solid base catalyst.
2. a kind of biodiesel according to claim 1 prepares the preparation method of special solid base catalyst, its feature exists
In：Step（1）Described emulsifying agent is one or both of neopelex, OP-10, Tween-60, Si Pan -80.
3. a kind of biodiesel according to claim 1 prepares the preparation method of special solid base catalyst, its feature exists
In：Step（2）In described styrene, 4~6g acrylic acid and 1~3g maleic acids can also be added.
4. a kind of biodiesel according to claim 1 prepares the preparation method of special solid base catalyst, its feature exists
In：Step（2）In described potassium persulfate solution, 0.03~0.05g azodiisobutyronitriles can also be added.
5. a kind of biodiesel according to claim 1 prepares the preparation method of special solid base catalyst, its feature exists
In：Step（4）Described calcination condition is：In Muffle furnace, 200~220 DEG C, guarantor are warming up to 2~4 DEG C/min rate programs
Temperature 90~120min of calcining, then temperature programming is continued to 500~550 DEG C with 6~8 DEG C/min speed, insulation 3~5h of calcining, with
Stove is cooled to room temperature.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108726901A (en) * | 2018-05-29 | 2018-11-02 | 丁嘉鹏 | A kind of preparation method of eggshell base porous solid alkali |
| CN115469051A (en) * | 2022-11-14 | 2022-12-13 | 成都华域环保有限公司 | Deoiling experimental method for waste oil-containing catalyst |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974404A (en) * | 2006-12-14 | 2007-06-06 | 天津理工大学 | Prepn process of nanometer titania ring |
| CN102989440A (en) * | 2012-12-13 | 2013-03-27 | 温家玮 | Modified kaliophilite biodiesel solid alkaline catalyst and production process thereof |
-
2017
- 2017-05-14 CN CN201710337145.4A patent/CN107029695A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974404A (en) * | 2006-12-14 | 2007-06-06 | 天津理工大学 | Prepn process of nanometer titania ring |
| CN102989440A (en) * | 2012-12-13 | 2013-03-27 | 温家玮 | Modified kaliophilite biodiesel solid alkaline catalyst and production process thereof |
Non-Patent Citations (1)
| Title |
|---|
| 侯建超等: ""K2O/SiO2催化剂上正丙醇与碳酸二甲酯合成碳酸二丙酯"", 《常州大学学报（自然科学版）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108726901A (en) * | 2018-05-29 | 2018-11-02 | 丁嘉鹏 | A kind of preparation method of eggshell base porous solid alkali |
| CN115469051A (en) * | 2022-11-14 | 2022-12-13 | 成都华域环保有限公司 | Deoiling experimental method for waste oil-containing catalyst |
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Application publication date: 20170811 |