CN105664953A - Composite catalyst for synthesizing ethylene carbonate by urea alcoholysis and preparation process and application thereof - Google Patents
Composite catalyst for synthesizing ethylene carbonate by urea alcoholysis and preparation process and application thereof Download PDFInfo
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- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
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- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/32—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
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Abstract
The invention provides a composite catalyst for synthesizing ethylene carbonate by urea alcoholysis and a preparation process and application thereof. The obtained composite catalyst is high in catalytic activity. The preparation process of the catalyst is simple, and a reaction process is non-toxic and harmless and is pollution-free to the environment. The process comprises the following steps: 1, uniformly mixing and milling ferric salt and zinc salt according to the mole ratio of (1:1)-(1:8), and then calcining at the temperature of 250 to 600 DEG C for 2 to 6 h to obtain a zinc-iron oxide; and 2, uniformly mixing zinc chloride into the obtained zinc-iron oxide according to the mole ratio of (1:1)-(1:5) to obtain the composite catalyst with the zinc-iron oxide and the zinc chloride. When the composite catalyst is used for synthesizing ethylene carbonate by urea alcoholysis, the use amount of the composite catalyst is 1.0 to 5.0 percent of the total mass of reactants. The reaction temperature is 120 to 150 DEG C, the reaction duration is 3 to 9 h, and the reaction pressure is 0.005 to 0.02 MPa.
Description
Technical field
The present invention relates to the technique that urea alcoholysis prepares NSC 11801, it is specially catalyst compounded and preparation technology and the application of a kind of urea alcoholysis synthesizing ethylene carbonate.
Background technology
NSC 11801 (EC) is the organic solvent of a kind of strong polarity, by means of excellent filming function, as the main composition of most lithium battery electrolytes, it is widely used in the novel industries such as new-energy automobile, power tool, electronic bike, in conventional use, owing to EC has the character such as boiling point height, flash-point height, solvability height, toxicity are low, reel off raw silk from cocoons liquid and the de-extraction agent etc. except sour gas being applied in weaving. In addition, due to its special cyclic ester structure, EC is widely used as again organic synthesis intermediate, pharmaceutical compositions and Chemicals raw material, it can with methyl alcohol or ethanol generation transesterification reaction, generate methylcarbonate or diethyl carbonate, it is further used for polycarbonate synthesis type organic.
The synthetic method of NSC 11801 mainly contains phosgenation, ester-interchange method and CO2With oxyethane cycloaddition method. Phosgenation has the phosgene of severe toxicity to be eliminated already as raw material owing to using, and ester-interchange method is expensive due to the price comparison of raw material and catalyzer, does not also have application prospect. Use CO2With the synthesis of oxyethane cycloaddition method, reaction process High Temperature High Pressure, to equipment requirements height. Novel alcoholysis of urea is that advantages of nontoxic raw materials is harmless with urea and glycolysis synthesizing ethylene carbonate, and be easy to get, cost low, industrialization process has important economic worth.
Urea and glycolysis are prepared the catalyzer that NSC 11801 adopts and are mainly contained metal oxide, alkaline earth metal oxide, carbonate etc. Kanbara etc. (EPPatent0638541) adopt ZnO to make catalyzer, catalyzing urea and glycol reaction, the ammonia produced is discharged by the method vacuumized, 2h is reacted at 145 DEG C, the transformation efficiency of ethylene glycol is 80.1%, the selectivity of NSC 11801 is 97.5%, and NSC 11801 receipts rate is up to 85%.Du Zhi equality (CN101544627A) adopts calcium phosphorus catalyst, it is 1:1-100 in molar ratio by urea and ethylene glycol, urea and calcium phosphorus catalyst are by mass percentage for the ratio of 1:0.001-0.1 joins in reactor, temperature of reaction is 50-250 DEG C, Reactive Synthesis carbonic ether when reaction pressure 0.001-0.5MPa, the selectivity of NSC 11801 is 96.5%, the receipts rate 60.7% of NSC 11801. Sun Yuhan (CN1421431A) discloses and adopts solid base catalyst catalysis third (second) glycol and urea reaction carbonate synthesis third (second) alkene ester, wherein solid base catalyst is the oxide compound of basic metal, alkaline-earth metal and transition element, oxyhydroxide, carbonate, supercarbonate, and one or more in them are flooded the soild oxide on carrier (carrier is gac, aluminum oxide, silicon oxide, molecular sieve), the selectivity finally obtaining NSC 11801 is up to 98.69%. (the JournalofChemicalTechnologyandBiotechnology such as XinqiangZhao, 2008, when 83:750-755) examining or check zinc-iron oxide catalyst, utilize the way of inflated with nitrogen to discharge the ammonia in reaction system, impel reaction to carry out to the right, wherein, catalyzer accounts for the 1.5% of reactant total mass, is 1:8 in urea/ethylene glycol mol ratio, and temperature of reaction is 150 DEG C, under the optimal conditions in reaction times 2.5h, the highest receipts rate of NSC 11801 is 66.1%.
The shortcomings such as in sum, it is low that the catalyzer such as the metal oxide reported, alkaline-earth metal often have catalytic activity, and preparation process is complicated, limit the application that urea alcoholysis prepares NSC 11801.
Summary of the invention
For problems of the prior art, the present invention provides catalyst compounded and preparation technology and the application of a kind of urea alcoholysis synthesizing ethylene carbonate, the catalyst compounded catalytic activity height obtained; The preparation technology of catalyzer is simple, and reaction process is nontoxic, environmentally safe.
The present invention is achieved through the following technical solutions:
A catalyst compounded preparation technology for urea alcoholysis synthesizing ethylene carbonate, comprises the steps,
Step 1, is that the molysite of 1:1～1:8 and zinc salt mixed grinding are even by mol ratio, then at the temperature lower calcination 2～6h of 250 DEG C～600 DEG C, obtains zinc-iron oxides;
Step 2, by the mol ratio of 1:1～1:5, is evenly mixed into zinc chloride in the zinc-iron oxides obtained, and obtains zinc-iron oxides and mixes composite catalyzer with zinc chloride.
Preferably, described zinc salt adopts zinc acetate or zinc nitrate.
Preferably, described molysite adopts iron nitrate or iron(ic) chloride.
A kind of urea alcoholysis synthesizing ethylene carbonate prepared by any one in above technical scheme catalyst compounded.
Preferably, the catalyst compounded zinc-iron oxides that combines is to promoter action for carbonic ether Cheng Huan of the catalyse pyrolysis effect of urea and zinc chloride.
The catalyst compounded application when urea alcoholysis synthesizing ethylene carbonate.
Preferably, this catalyst compounded in collaborative zinc-iron oxides to the catalyse pyrolysis effect of urea and zinc chloride to the application of the promotion ring formation of carbonic ether.
Preferably, catalyst compounded consumption is the 1.0%-5.0% of reactant total mass.
Preferably, temperature of reaction 120-150 DEG C, reaction times 3-9h, reaction pressure 0.005-0.02MPa.
Compared with prior art, the present invention has following useful technique effect:
Catalyzer of the present invention mixes composite by zinc-iron oxides with zinc chloride, wherein the zinc source in zinc-iron oxides comes from zinc salt, source of iron comes from molysite, two kinds of salt are in varing proportions, calcining different time at different temperatures, the zinc-iron oxides obtained mixes with zinc chloride by a certain percentage and composite obtains catalyzer of the present invention. This catalyzer has worked in coordination with zinc-iron oxides to promoter action for carbonic ether Cheng Huan of the catalyse pyrolysis effect of urea and zinc chloride, thus show very high catalytic activity and selectivity, improving the receipts rate of object product, under experimental conditions, the receipts rate of NSC 11801 reaches as high as 92%.Compared with current existing catalyzer, catalytic activity height. The preparation technology of catalyzer is simple, and reaction process is nontoxic, environmentally safe.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, and the explanation of the invention is not limited.
The present invention is furtherd investigate by the reaction mechanism preparing NSC 11801 for urea alcoholysis, it has been found that the reaction path that urea alcoholysis prepares EC is shown below:
First, a molecules of ammonia sloughed by urea and glycol reaction generates hydroxyethyl carbamate HEC, and then, HEC sloughs a molecules of ammonia, and annulation occurs, and generates target product EC. The alkaline-earth metal catalyst reported, metal oxide catalyst are suitable for the strong base weak acid site of urea thermolysis owing to catalyst surface has, and a molecules of ammonia sloughed by catalysis urea and glycol reaction generates HEC, is therefore conducive to the generation that the first step is reacted. But metal oxide catalyst is less to the ring formation of HEC. The present invention by adding zinc chloride in reaction system, then owing to chlorine atom has good Electron Affinities and less space steric hindrance, its can the effective carbon atom in attack HEC, thus make HEC slough a molecules of ammonia generation annulation, facilitate the generation of the 2nd step reaction.
Of the present invention catalyst compounded, adopt inorganic zinc salt and inorganic molysite to be raw material, with certain proportion, certain temperature, certain time, calcining obtains zinc-iron oxides, is more evenly mixed into zinc chloride, obtains catalyst compounded. Preferred zinc salt adopts zinc acetate or zinc nitrate, and required molysite adopts iron nitrate or iron(ic) chloride. Concrete preparation method is as follows:
It is 1:1～1:8 according to the mol ratio of molysite and zinc salt, take two kinds of salt, join in mortar, mix grinding, the solid after grinding, at 250-600 DEG C, calcining 2～6h, obtains zinc-iron oxides, is 1:1～1:5 according to zinc-iron oxides and zinc chloride mol ratio, evenly it is mixed into zinc chloride, obtains catalyst compounded.
The catalyzer of the present invention is the 1.0%～5.0% of reactant total mass at the consumption of catalyzer, temperature of reaction 120～150 DEG C, reaction times 3～9h, reaction pressure 0.005～0.02MPa, the mol ratio 1.5:1 of ethylene glycol and urea is really under fixed condition, and object product NSC 11801 receipts rate reaches 79%-92%.
Embodiment 1
Taking 7.8g nine water iron nitrate and 38.83g zinc acetate dihydrate, in mortar, mixed grinding is even, calcines 4 hours, obtain zinc-iron oxide catalyst, be evenly mixed into zinc chloride for 1:2.5 in molar ratio, obtain catalyst compounded at 350 DEG C.
The urea of design proportion, ethylene glycol and catalyst compounded is added in 50ML reactor, catalyst compounded amount accounts for reactant total mass 3.5%, reaction pressure 0.005MPa, temperature of reaction 135 DEG C, 6 hours reaction times, reaction product chromatogram ration analysis, NSC 11801 selectivity is 95%, and receipts rate reaches 92%.
Embodiment 2
Taking 7.8g nine water iron nitrate and 38.83g zinc acetate dihydrate, in mortar, mixed grinding is even, calcines 4 hours, obtain zinc-iron oxide catalyst, be evenly mixed into zinc chloride for 1.5:2 in molar ratio, obtain catalyst compounded at 350 DEG C.
5.0L reactor adds the urea of design proportion, ethylene glycol and catalyzer, catalyst compounded amount accounts for reactant total mass 3.5%, reaction pressure 0.01MPa, temperature of reaction 135 DEG C, 6 hours reaction times, reaction product chromatogram ration analysis, NSC 11801 selectivity is 93.5%, and receipts rate is 90.1%.
Embodiment 3
Taking 7.8g nine water iron nitrate and 38.83g zinc acetate dihydrate, in mortar, mixed grinding is even, calcines 4 hours, obtain zinc-iron oxide catalyst, be evenly mixed into zinc chloride for 1.5:2.5 in molar ratio, obtain catalyst compounded at 350 DEG C.
50ML reactor adds the urea of design proportion, ethylene glycol and catalyzer, catalyst compounded amount accounts for reactant total mass 4.0%, reaction pressure 0.01MPa, temperature of reaction 135 DEG C, 6 hours reaction times, reaction product chromatogram ration analysis, NSC 11801 selectivity is 93%, and receipts rate is 89.8%.
Embodiment 4
Taking 7.8g nine water iron nitrate and 38.83g zinc acetate dihydrate, in mortar, mixed grinding is even, calcines 2 hours, obtain zinc-iron oxide catalyst, be evenly mixed into zinc chloride for 1.5:2.5 in molar ratio, obtain catalyst compounded at 350 DEG C.
5.0L reactor adds the urea of design proportion, ethylene glycol and catalyzer, catalyst compounded amount accounts for reactant total mass 4.0%, reaction pressure 0.015MPa, temperature of reaction 135 DEG C, 9 hours reaction times, reaction product chromatogram ration analysis, NSC 11801 selectivity is 90.2%, and receipts rate is 84.7%.
Embodiment 5
Taking 7.8g nine water iron nitrate and 38.83g zinc acetate dihydrate, in mortar, mixed grinding is even, calcines 4 hours, obtain zinc-iron oxide catalyst, be evenly mixed into zinc chloride for 2:2.5 in molar ratio, obtain catalyst compounded at 350 DEG C.
5.0L reactor adds the urea of design proportion, ethylene glycol and catalyzer, catalyst compounded amount accounts for reactant total mass 4.5%, reaction pressure 0.01MPa, temperature of reaction 135 DEG C, 7 hours reaction times, reaction product chromatogram ration analysis, NSC 11801 selectivity is 91.6%, and receipts rate is 86.6%.
Embodiment 6
Taking 7.8g nine water iron nitrate and 38.83g zinc acetate dihydrate, in mortar, mixed grinding is even, calcines 4 hours, obtain zinc-iron oxide catalyst, be evenly mixed into zinc chloride for 1:1.5 in molar ratio, obtain catalyst compounded at 600 DEG C.
5.0L reactor adds the urea of design proportion, ethylene glycol and catalyzer, catalyst compounded amount accounts for reactant total mass 3.5%, reaction pressure 0.01MPa, temperature of reaction 150 DEG C, 7 hours reaction times, reaction product chromatogram ration analysis, NSC 11801 selectivity is 91.4%, and receipts rate is 87.1%.
Embodiment 7
Taking 7.8g nine water iron nitrate and 16.91g zinc acetate dihydrate, in mortar, mixed grinding is even, calcines 4 hours, obtain zinc-iron oxide catalyst, be evenly mixed into zinc chloride for 1:5 in molar ratio, obtain catalyst compounded at 350 DEG C.
5.0L reactor adds the urea of design proportion, ethylene glycol and catalyzer, catalyst compounded amount accounts for reactant total mass 5%, reaction pressure 0.02MPa, temperature of reaction 120 DEG C, 3 hours reaction times, reaction product chromatogram ration analysis, NSC 11801 selectivity is 85.4%, and NSC 11801 receipts rate is 79.1%.
Embodiment 8
Taking 7.8g nine water iron nitrate and 38.83g zinc acetate dihydrate, in mortar, mixed grinding is even, calcines 4 hours, obtain zinc-iron oxide catalyst, be evenly mixed into zinc chloride for 1:1.5 in molar ratio, obtain catalyst compounded at 250 DEG C.
5.0L reactor adds the urea of design proportion, ethylene glycol and catalyzer, catalyst compounded amount accounts for reactant total mass 3.5%, reaction pressure 0.01MPa, temperature of reaction 135 DEG C, 9 hours reaction times, reaction product chromatogram ration analysis, NSC 11801 selectivity is 88.4%, and receipts rate is 84.3%.
Embodiment 9
Taking 71.63g nine water iron nitrate and 38.83g zinc acetate dihydrate, in mortar, mixed grinding is even, calcines 4 hours, obtain zinc-iron oxide catalyst, be evenly mixed into zinc chloride for 1:1 in molar ratio, obtain catalyst compounded at 350 DEG C.
5.0L reactor adds the urea of design proportion, ethylene glycol and catalyzer, catalyst compounded amount accounts for reactant total mass 3.5%, reaction pressure 0.01MPa, temperature of reaction 135 DEG C, 6 hours reaction times, reaction product chromatogram ration analysis, NSC 11801 selectivity is 89%, and receipts rate is 82.4%.
Embodiment 10
Taking 7.8g nine water iron nitrate and 32.28g zinc nitrate, in mortar, mixed grinding is even, calcines 6 hours, obtain zinc-iron oxide catalyst, be evenly mixed into zinc chloride for 1.5:2.5 in molar ratio, obtain catalyst compounded at 350 DEG C.
5.0L reactor adds the urea of design proportion, ethylene glycol and catalyzer, catalyst compounded amount accounts for reactant total mass 3.5%, reaction pressure 0.01MPa, temperature of reaction 135 DEG C, 6 hours reaction times, reaction product chromatogram ration analysis, NSC 11801 selectivity is 87.6%, and receipts rate is 83.3%.
Embodiment 11
Taking 7.8g iron(ic) chloride and 84.10g zinc acetate dihydrate, in mortar, mixed grinding is even, calcines 5 hours, obtain zinc-iron oxide catalyst, be evenly mixed into zinc chloride for 1.5:2.5 in molar ratio, obtain catalyst compounded at 350 DEG C.
5.0L reactor adds the urea of design proportion, ethylene glycol and catalyzer, catalyst compounded amount accounts for reactant total mass 1.0%, reaction pressure 0.01MPa, temperature of reaction 135 DEG C, 7 hours reaction times, reaction product chromatogram ration analysis, NSC 11801 selectivity is 89%, and receipts rate is 82.7%.
Claims (9)
1. the catalyst compounded preparation technology of a urea alcoholysis synthesizing ethylene carbonate, it is characterised in that, comprise the steps,
Step 1, is that the molysite of 1:1～1:8 and zinc salt mixed grinding are even by mol ratio, then at the temperature lower calcination 2～6h of 250 DEG C～600 DEG C, obtains zinc-iron oxides;
Step 2, by the mol ratio of 1:1～1:5, is evenly mixed into zinc chloride in the zinc-iron oxides obtained, and obtains zinc-iron oxides and mixes composite catalyzer with zinc chloride.
2. the catalyst compounded preparation technology of a kind of urea alcoholysis synthesizing ethylene carbonate according to claim 1, it is characterised in that, described zinc salt adopts zinc acetate or zinc nitrate.
3. the catalyst compounded preparation technology of a kind of urea alcoholysis synthesizing ethylene carbonate according to claim 1, it is characterised in that, described molysite adopts iron nitrate or iron(ic) chloride.
4. the urea alcoholysis synthesizing ethylene carbonate that a kind is prepared by any one in claim 1-3 catalyst compounded.
5. according to claim 4 catalyst compounded, it is characterised in that, the catalyst compounded zinc-iron oxides that combines is to promoter action for carbonic ether Cheng Huan of the catalyse pyrolysis effect of urea and zinc chloride.
6. the catalyst compounded application when urea alcoholysis synthesizing ethylene carbonate as claimed in claim 4.
7. application according to claim 6, it is characterised in that, this catalyst compounded in collaborative zinc-iron oxides to the catalyse pyrolysis effect of urea and zinc chloride to the application of the promotion ring formation of carbonic ether.
8. application according to claim 6, it is characterised in that, catalyst compounded consumption is the 1.0%-5.0% of reactant total mass.
9. application according to claim 6, it is characterised in that, temperature of reaction 120-150 DEG C, reaction times 3-9h, reaction pressure 0.005-0.02MPa.
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| CN113797914A (en) * | 2021-09-28 | 2021-12-17 | 中国科学院山西煤炭化学研究所 | Catalyst for synthesizing ethylene carbonate, preparation method and application thereof |
| CN114210273A (en) * | 2021-12-24 | 2022-03-22 | 常州化工设计院有限公司 | Preparation process of ethylene carbonate |
| CN115521285A (en) * | 2022-10-13 | 2022-12-27 | 青岛科技大学 | Method for synthesizing ethylene carbonate by zinc isocyanate catalysis |
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| CN115521285A (en) * | 2022-10-13 | 2022-12-27 | 青岛科技大学 | Method for synthesizing ethylene carbonate by zinc isocyanate catalysis |
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