CN1769258A - Dual catalytic system for promoting ammonium lactate esterification and uses, preparation method of maganetic solid acid catalyst in the same - Google Patents
Dual catalytic system for promoting ammonium lactate esterification and uses, preparation method of maganetic solid acid catalyst in the same Download PDFInfo
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- CN1769258A CN1769258A CN 200510010453 CN200510010453A CN1769258A CN 1769258 A CN1769258 A CN 1769258A CN 200510010453 CN200510010453 CN 200510010453 CN 200510010453 A CN200510010453 A CN 200510010453A CN 1769258 A CN1769258 A CN 1769258A
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Abstract
The invention relates binary catalysis system and its application in ammonlum lactate esterification reaction, and the method for preparation of magnetism solid acid catalyst in the said catalysis system. It solves the problem of magnetism solid acid catalyst not suiting ammonlum lactate esterification. In the invention the binary catalysis system comprises the magnetism solid acid catalyst and tin dichloride, the proportion by weight of which is 20: 1-1: 20. The method for making magnetism solid acid catalyst comprises the following steps: 1. adding ammonia into ferric persulfate solution; 2. solid-liquid separation, drying and powdering the solid; 3.adding the powder into the nickel sulfate solution; 4. evaporating to dryness and roasting; 5. cooling. The said catalysis system is used in ammonlum lactate esterification reaction, comprising the following proportion: a. the mass ratio of ammonium lactate and the C1-C4 alcohol being 10:1-1:10; b. the weight ratio of catalysis system and ammonium lactate being 0.005-5%, and the magnetism solid acid catalyst and tin dichloride being 20:1-1:20; c. the esterification reaction reacting in atmosphere pressure, at 115-140DEG C, for 3.5-11h. The invention has good selectivity, adapted for ammonlum lactate esterification reaction.
Description
Technical field
The present invention relates to a kind of binary catalyst system.The invention still further relates to the application of above-mentioned catalyst system in esterification of ammonium lactate.The invention still further relates to the preparation method of magnetic solid acid catalyst in the above-mentioned catalyst system.
Background technology
Patent of invention CN1453067A and CN1290574A disclose a kind of method for preparing magnetic solid acid catalyst respectively, but these methods all need to prepare magnetic substance earlier and make catalyst core, catalyst preparation step is loaded down with trivial details, and the acidity of catalyst for preparing is stronger, to the poor selectivity of esterification of ammonium lactate.
Summary of the invention
The objective of the invention is all needs elder generation's preparation magnetic substance to make catalyst core in order to solve the reacting middle catalyst of lactic acid esterification in the past, catalyst preparation step is loaded down with trivial details, and the acidity of catalyst for preparing is stronger, be not suitable for the problem of esterification of ammonium lactate, and the preparation method of magnetic solid acid catalyst in a kind of binary catalyst system that promotes ammonium lactate esterification that provides and application and this system.The binary catalyst system that promotes esterification of ammonium lactate among the present invention by magnetic solid acid catalyst and tindichloride by 20: 1-1: 20 weight ratio is formed.Promote among the present invention that the binary catalyst system of esterification of ammonium lactate is used for esterification of ammonium lactate, in the reaction: (a) mass ratio of material acid ammonium and C1-C4 alcohol is 10: 1-1: 10; (b) the total add-on of magnetic solid acid catalyst and tindichloride is the 0.005%-5% of DL-Lactic acid ammonium salt weight, and magnetic solid acid catalyst and tindichloride are by 20: 1-1: 20 weight ratio is formed; (c) esterification is reacted 3.5-11h under the condition of normal pressure, 115-140 ℃.Promote the preparation method of magnetic solid acid catalyst in the binary catalyst system of esterification of ammonium lactate to realize by following steps among the present invention: (one) per minute in ferrum sulfuricum oxydatum solutum drips 10 ammonia solns, make that the pH value reaches 6-10 in the solution, form suspension liquid; (2) suspension liquid is carried out solid-liquid separation, the solid phase isolate is dry 10-30h under 50-160 ℃, and grinds to form 100-120 purpose powder; (3) be 1 in Fe and Ni atomic ratio: 1-3: 1 ratio adds powder in the nickel sulfate solution, and stirs; (4) with the moisture evaporate to dryness, the mixture that obtains places muffle furnace, is warming up to 780-1000 ℃ with the speed of 2-10 ℃ of per minute rising, roasting 1.5-3.5h again under this temperature; (5) taking-up of the compounding substances after the roasting is cooled to room temperature, promptly obtains magnetic solid acid catalyst.
Embodiment
Embodiment one: the binary catalyst system that promotes esterification of ammonium lactate in the present embodiment by magnetic solid acid catalyst and tindichloride by 20: 1-1: 20 weight ratio is formed.Wherein the preparation method of magnetic solid acid catalyst is undertaken by following step: (one) per minute in ferrum sulfuricum oxydatum solutum drips 10 ammonia solns, makes that pH value reaches 6-10 in the solution, the formation suspension liquid; (2) suspension liquid is carried out solid-liquid separation, the solid phase isolate is dry 10-30h under 50-160 ℃, and grinds to form 100-120 purpose powder; (3) be 1 in Fe and Ni atomic ratio: 1-3: 1 ratio adds powder in the nickel sulfate solution, and stirs; (4) with the moisture evaporate to dryness, the mixture that obtains places muffle furnace, is warming up to 780-1000 ℃ with the speed of 2-10 ℃ of per minute rising, roasting 1.5-3.5h again under this temperature; (5) taking-up of the compounding substances after the roasting is cooled to room temperature, promptly obtains magnetic solid acid catalyst.
Present embodiment need not to prepare magnetic substance earlier and makes catalyst core, and preparation process is simple, and a little less than the acidity of catalyst for preparing, selectivity is good, benefits recycling.
Embodiment two: the difference of present embodiment and embodiment one is: magnetic solid acid catalyst and tindichloride are by 1: 1-1: 7 weight ratio is formed.
Embodiment three: the difference of present embodiment and embodiment one is: magnetic solid acid catalyst and tindichloride are formed by 3: 1 weight ratio.
Embodiment four: the difference of present embodiment and embodiment one is: magnetic solid acid catalyst and tindichloride are formed by 1: 2 weight ratio.
Embodiment five: the difference of present embodiment and embodiment one is: magnetic solid acid catalyst and tindichloride are formed by 1: 6 weight ratio.
Embodiment six: the difference of present embodiment and embodiment one is: magnetic solid acid catalyst and tindichloride are formed by 1: 17 weight ratio.
Embodiment seven: the difference of present embodiment and embodiment one is: employed ammonia soln concentration is 25% in the step ().
Embodiment eight: the difference of present embodiment and embodiment one is: be that 2: 1 ratio adds powder in the nickel sulfate solution in Fe and Ni atomic ratio in the step (three), and stir.
Embodiment nine: promote in the present embodiment that the binary catalyst system of esterification of ammonium lactate is used for esterification of ammonium lactate, in the reaction: (a) mass ratio of material acid ammonium and C1-C4 alcohol is 10: 1-1: 10; (b) the total add-on of magnetic solid acid catalyst and tindichloride is the 0.005%-5% of DL-Lactic acid ammonium salt weight, and magnetic solid acid catalyst and tindichloride are by 20: 1-1: 20 weight ratio is formed; (c) esterification is reacted 3.5-11h under the condition of normal pressure, 115-140 ℃, and esterification yield is 80.5-87.5%.
Embodiment ten: the difference of present embodiment and embodiment nine is: the mass ratio of material acid ammonium and C1-C4 alcohol is 4: 1-1: 4.
Embodiment 11: the difference of present embodiment and embodiment nine is: the total add-on of magnetic solid acid catalyst and tindichloride is the 0.05%-5% of DL-Lactic acid ammonium salt weight.
Embodiment 12: the difference of present embodiment and embodiment nine is: magnetic solid acid catalyst and tindichloride are by 1: 1-1: 7 weight ratio is formed; The reaction esterification yield is 83-87%.
Embodiment 13: the difference of present embodiment and embodiment nine is: magnetic solid acid catalyst and tindichloride are formed by 3: 1 weight ratio; The reaction esterification yield is 82.5%.
Embodiment 14: the difference of present embodiment and embodiment nine is: magnetic solid acid catalyst and tindichloride are formed by 1: 2 weight ratio; The reaction esterification yield is 85.5%.
Embodiment 15: the difference of present embodiment and embodiment nine is: magnetic solid acid catalyst and tindichloride are formed by 1: 6 weight ratio; The reaction esterification yield is 86%.
Embodiment 16: the difference of present embodiment and embodiment nine is: magnetic solid acid catalyst and tindichloride are formed by 1: 17 weight ratio; The reaction esterification yield is 81%.
Embodiment 17: the difference of present embodiment and embodiment one is: the preparation method of magnetic solid acid catalyst is undertaken by following step: (one) per minute in ferrum sulfuricum oxydatum solutum drips 10 ammonia solns, make that the pH value reaches 9 in the solution, form suspension liquid; (2) suspension liquid is carried out solid-liquid separation, the solid phase isolate is dry 20h under 120 ℃, and grinds to form 110 purpose powder; (3) be 1 in Fe and Ni atomic ratio: 1-3: 1 ratio adds powder in the nickel sulfate solution, and stirs; (4) with the moisture evaporate to dryness, the mixture that obtains places muffle furnace, is warming up to 820 ℃ with raise 10 ℃ speed of per minute, roasting 2.5h again under this temperature; (5) taking-up of the compounding substances after the roasting is cooled to room temperature, promptly obtains magnetic solid acid catalyst.
Embodiment 18: the difference of present embodiment and embodiment 17 is: in the step () in ferrum sulfuricum oxydatum solutum per minute drip 10 ammonia solns, make that the pH value reaches 8 in the solution.
Embodiment 19: the difference of present embodiment and embodiment 17 is: with the moisture evaporate to dryness, the mixture that obtains places muffle furnace in the step (four), is warming up to 960 ℃ with raise 8 ℃ speed of per minute, roasting 3h again under this temperature;
Embodiment 20: the difference of present embodiment and embodiment nine is: in the reaction: (a) mass ratio of raw material DL-Lactic acid ammonium salt and propyl carbinol is 1: 3 in the system; (b) the total add-on of magnetic solid acid catalyst and tindichloride is 0.5% of a DL-Lactic acid ammonium salt weight in the system, and magnetic solid acid catalyst and tindichloride are formed by 1: 4 weight ratio; (c) esterification is reacted 7h under normal pressure, 127 ℃ condition, and esterification yield is 87%.
Embodiment 21: present embodiment and embodiment nine, 20 difference are: in the reaction: (a) mass ratio of raw material DL-Lactic acid ammonium salt and propyl alcohol is 3: 1 in the system; (b) the total add-on of magnetic solid acid catalyst and tindichloride is 1% of a DL-Lactic acid ammonium salt weight in the system, and magnetic solid acid catalyst and tindichloride are formed by 2: 5 weight ratio; (c) esterification is reacted 5h under normal pressure, 130 ℃ condition, and esterification yield is 83.5%.
Embodiment 22: the difference of present embodiment and embodiment 21 is: in the reaction: (a) raw material DL-Lactic acid ammonium salt and alcoholic acid mass ratio are 1: 6 in the system; (b) the total add-on of magnetic solid acid catalyst and tindichloride is 0.01% of a DL-Lactic acid ammonium salt weight in the system, and magnetic solid acid catalyst and tindichloride are formed by 3: 4 weight ratio; (c) esterification is reacted 10h under normal pressure, 120 ℃ condition, and esterification yield is 81%.
Claims (8)
1, promote the binary catalyst system of esterification of ammonium lactate, it is characterized in that it by magnetic solid acid catalyst and tindichloride by 20: 1-1: 20 weight ratio is formed.
2, the binary catalyst system of promotion esterification of ammonium lactate according to claim 1 is characterized in that magnetic solid acid catalyst and tindichloride are by 1: 1-1: 7 weight ratio is formed.
3, promote the application of binary catalyst system in esterification of ammonium lactate of esterification of ammonium lactate, it is characterized in that in the reaction: (a) mass ratio of material acid ammonium and C1-C4 alcohol is 10: 1-1: 10; (b) the total add-on of magnetic solid acid catalyst and tindichloride is the 0.005%-5% of DL-Lactic acid ammonium salt weight, and magnetic solid acid catalyst and tindichloride are by 20: 1-1: 20 weight ratio is formed; (c) esterification is reacted 3.5-11h under the condition of normal pressure, 115-140 ℃.
4, the application of the binary catalyst system of promotion esterification of ammonium lactate according to claim 3 in esterification of ammonium lactate, the mass ratio that it is characterized in that material acid ammonium and C1-C4 alcohol is 4: 1-1: 4.
5, the application of the binary catalyst system of promotion esterification of ammonium lactate according to claim 3 in esterification of ammonium lactate is characterized in that the total add-on of magnetic solid acid catalyst and tindichloride is the 0.05%-5% of DL-Lactic acid ammonium salt weight.
6, the application of the binary catalyst system of promotion esterification of ammonium lactate according to claim 3 in esterification of ammonium lactate is characterized in that magnetic solid acid catalyst and tindichloride are by 1: 1-1: 7 weight ratio is formed.
7, the preparation method of magnetic solid acid catalyst in the binary catalyst system of promotion esterification of ammonium lactate, it is characterized in that it is undertaken by following step: (one) per minute in ferrum sulfuricum oxydatum solutum drips 10 ammonia solns, make that the pH value reaches 6-10 in the solution, form suspension liquid; (2) suspension liquid is carried out solid-liquid separation, the solid phase isolate is dry 10-30h under 50-160 ℃, and grinds to form 100-120 purpose powder; (3) be 1 in Fe and Ni atomic ratio: 1-3: 1 ratio adds powder in the nickel sulfate solution, and stirs; (4) with the moisture evaporate to dryness, the mixture that obtains places muffle furnace, is warming up to 780-1000 ℃ with the speed of 2-10 ℃ of per minute rising, roasting 1.5-3.5h again under this temperature; (5) taking-up of the compounding substances after the roasting is cooled to room temperature, promptly obtains magnetic solid acid catalyst.
8, the preparation method of magnetic solid acid catalyst in the binary catalyst system of promotion esterification of ammonium lactate according to claim 7 is characterized in that the employed ammonia soln concentration of step () is 25%.
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| CNB200710105617XA Division CN100463718C (en) | 2005-10-21 | 2005-10-21 | Process of preparing magnetic solid acid catalyst in binary catalyst system for promoting esterification of ammonium lactate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1048990A (en) * | 1989-07-25 | 1991-02-06 | 烟台市化学工业研究所 | A kind of composite solid-acid catalyst that is used for esterification |
| CN1132688C (en) * | 2000-11-08 | 2003-12-31 | 哈尔滨工程大学 | Magnetic solid super strong acid catalyst and its preparing method |
| CN1453067A (en) * | 2002-04-24 | 2003-11-05 | 北京化工大学 | Magnetic solid super acidic catalyst Zr(SO4)2/Fe3O4 and its prepn process |
| US6972348B2 (en) * | 2004-03-24 | 2005-12-06 | Uop Llc | Catalytic conversion of polycyclic aromatics into xylenes |
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