CN111547749B - Green circulation method for producing ethyl maltol - Google Patents
Green circulation method for producing ethyl maltol Download PDFInfo
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- CN111547749B CN111547749B CN202010330151.9A CN202010330151A CN111547749B CN 111547749 B CN111547749 B CN 111547749B CN 202010330151 A CN202010330151 A CN 202010330151A CN 111547749 B CN111547749 B CN 111547749B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/14—Magnesium hydroxide
- C01F5/22—Magnesium hydroxide from magnesium compounds with alkali hydroxides or alkaline- earth oxides or hydroxides
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D309/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings
- C07D309/34—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
- C07D309/36—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only ring hetero atom, not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with oxygen atoms directly attached to ring carbon atoms
- C07D309/40—Oxygen atoms attached in positions 3 and 4, e.g. maltol
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/14—Alkali metal compounds
- C25B1/16—Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a green circulating method for producing ethyl maltol, which is characterized by comprising the steps of adding water into solid waste containing basic magnesium chloride, uniformly stirring, carrying out reduced pressure distillation to remove an organic solvent, adding acid, further decoloring through a tubular filter provided with activated carbon, dropwise adding a sodium hydroxide solution with the molar concentration of 2.5-4 mol/L, after complete reaction, centrifuging, drying, crushing, grading, inspecting and packaging. The method has the advantages of short process flow and mild production conditions, can fully utilize waste materials in maltol production, can obtain higher economic return, and finally reduces the production cost of maltol and pollution. The utilization efficiency of resources is effectively improved, and the greenness and the sustainability of the maltol production process are improved.
Description
Technical Field
The invention relates to the technical field of maltol production, in particular to a green circulating method for producing ethyl maltol.
Background
Ethyl maltol, english name: ethyl maltol, chemical name: 2-ethyl-3-hydroxy-4H-pyrone (2-ethyl-3-hydroxy-4H-pyrone), molecular formula: C 7 H 8 0 3 The powder is white needle-shaped or white crystal powder with aromatic fragrance, and is widely applied as a fragrance modifier and a flavoring agent. Is a food additive which is well recognized by people and has the advantages of safety, reliability, small dosage and obvious effect. The sweet potato flavor enhancer is a good flavor enhancer for tobacco, food, beverage, essence, fruit wine, daily cosmetics and the like, has a remarkable effect of improving and enhancing the flavor of food, plays a role of sweetening sweet food and can prolong the storage period of the food. In 1970, ethyl maltol was formally included in the food additives line by the world health organization and the food and agriculture organization of the United nations, which by virtue of its remarkable flavoring effect, recognized safety and broad applicationThe characteristics of usability and the like develop at home and abroad at a higher speed.
At present, more than ten mature processes for synthesizing ethyl maltol are available, and in terms of China, a total synthesis method, namely a furfural method, is mostly adopted. The process comprises the steps of firstly reacting furfural with a Grignard reagent to prepare ethyl furfuryl alcohol, and then carrying out a series of oxidation rearrangement on hexyl furfuryl alcohol to synthesize the ethyl maltol. The method for producing the ethyl maltol generates a large amount of magnesium-containing waste and salt-containing waste hydrochloric acid every day, and 2-3 tons of magnesium-containing waste residues are generated every ton of the ethyl maltol product. Aiming at the problems that in the existing maltol production, the separation of products and solvents in the Grignard reaction, the addition reaction and the hydrolysis reaction and solid magnesium-containing waste is carried out by a vacuum filtration method, liquid-phase materials are mainly recycled by the method, the solid is treated as waste, and the solid waste causes great pollution to the environment, chinese patent ZL2007100171626 discloses a method for recycling the waste in the maltol production, the method can fully utilize the maltol production waste, recover the solvents to the maximum extent, change the waste into useful products, and finally reduce the cost and the pollution. From the disclosure of the patent, the main improvement point of the patent lies in the separation process of the solvent and the solid waste, and the separated solid waste is simply subjected to pressure filtration, drying and high-temperature calcination to finally obtain the claimed solid magnesium oxide. And the high-temperature calcination method consumes a large amount of energy and is high in cost.
In recent years, magnesium hydroxide has been widely used as an important chemical product and intermediate in the fields of ceramic materials, environmental protection, medicines and the like. The magnesium hydroxide has the characteristics of high decomposition temperature, good thermal stability, no toxicity, no smoke, smoke suppression and the like, and can be used as a high-performance inorganic flame retardant to be applied to high polymer materials. In particular, the high-purity and superfine magnesium hydroxide flame retardant becomes a hot spot of development and research at home and abroad at present, and is rapidly developed in the field of inorganic flame retardants due to the characteristics of higher decomposition temperature, high thermal stability, no toxicity, no smoke, smoke suppression and the like. Dorsery and the like disclose a process for preparing magnesium hydroxide from magnesium-containing waste liquid in the production process of maltol, wherein the magnesium in the alkali-containing magnesium chloride waste liquid in the production process of maltol is recovered by an ammonia method after acidification and decoloration refining treatment, and a magnesium hydroxide product is produced, and the obtained product has controllable granularity and high purity. But the cost of the needed raw material ammonia water is high, and the method can only be used for producing high-purity reagent-grade, medical and electronic magnesium hydroxide.
Disclosure of Invention
Aiming at the problems of high energy consumption and low economy in the solid waste treatment in the conventional ethyl maltol production, the invention provides a green environment-friendly method which has low energy consumption, can fully utilize waste materials in the maltol production, can obtain higher economic return, finally reduces the production cost of maltol and reduces pollution. The utilization efficiency of resources is effectively improved, and the greenness and the sustainability of the maltol production process are improved.
In order to achieve the above purpose, the invention provides the following technical scheme:
the technical scheme of the invention is as follows: a green circulation method for producing ethyl maltol is characterized in that: the method comprises the following steps:
a: adding water into the solid waste containing the alkali magnesium chloride generated in the production of the ethyl maltol and uniformly stirring, wherein the weight ratio of the water to the solid waste containing the alkali magnesium chloride is 1.8-2;
b: pumping the alkali-containing magnesium chloride waste liquid into a distillation still, carrying out reduced pressure distillation to obtain an organic solvent in the alkali-containing magnesium chloride waste liquid, and drying the organic solvent for recycling of an ethyl maltol production system;
c: adding a dilute hydrochloric acid solution into the basic magnesium chloride-containing waste liquid until the pH value of the solution is 4-6, wherein the mass fraction of the dilute hydrochloric acid solution is 13-15%;
d: c, enabling the solution obtained in the step c to pass through a filter, wherein the filter is a tubular filter, and activated carbon is arranged in the tubular filter;
e: transferring the solution obtained after filtering in the step d into a reaction kettle, dropwise adding a sodium hydroxide solution into the reaction kettle, slowly stirring, and reacting for 2 hours, wherein the addition amount of the sodium hydroxide solution is 1.05-1.15 times of the theoretical demand amount, and the molar concentration of the sodium hydroxide solution is 2.5-4 mol/L;
f: and e, transferring the solution obtained after the reaction in the step e into a centrifugal machine, washing the magnesium hydroxide filter cake obtained after the centrifugation to remove sodium chloride, drying the magnesium hydroxide filter cake at 100-110 ℃, crushing and grading, inspecting and packaging.
Further, the dilute hydrochloric acid solution in step c is from waste acid recovered in the production of ethyl maltol.
Further, the method also comprises the step g: and f, carrying out rectification and impurity removal treatment on the washing waste liquid containing the sodium chloride obtained in the step f, and then electrolyzing to obtain a sodium hydroxide solution, wherein the sodium hydroxide solution is used in the step e.
Further, in the step e, firstly, a sodium hydroxide solution with the molar concentration of 4mol/L is dripped, and when the solution in the reaction kettle becomes turbid, the sodium hydroxide solution with the molar concentration of 2.5-3 mol/L is dripped.
Firstly, dropwise adding a high-concentration 4mol/L sodium hydroxide solution to quickly form crystal nuclei in the solution, and then dropwise adding 2.5-3 mol/L sodium hydroxide solution to finally form magnesium hydroxide crystals with large granularity, good filtering performance and high magnesium recovery rate.
According to the green circulating method for producing the ethyl maltol, disclosed by the invention, the final recovery rate of magnesium reaches more than 93%, and the product purity reaches more than 95%.
The invention has the advantages that:
(1) The method has the advantages that the solid waste containing the alkali magnesium chloride is used for preparing the magnesium hydroxide, the process flow is short, the production conditions are mild, the waste in the maltol production can be fully utilized, higher economic return can be obtained, the production cost of the maltol is finally reduced, and the pollution is reduced. The utilization efficiency of resources is effectively improved, and the greenness and the sustainability of the maltol production process are improved.
(2) Firstly, adding water into the solid waste containing basic magnesium chloride, uniformly stirring, then carrying out reduced pressure distillation to remove the organic solvent, and further decoloring through a tubular filter provided with activated carbon to ensure that the magnesium hydroxide product has better purity and whiteness.
(3) And electrolyzing a byproduct sodium chloride obtained in the recovery of the alkali-containing magnesium chloride solid waste to obtain a sodium hydroxide solution, so as to provide a raw material for preparing the sodium hydroxide and further save the cost.
(4) And waste acid recovered in the production of ethyl maltol is used as a source of a dilute hydrochloric acid solution, so that chemical waste is fully utilized, waste is turned into wealth, and the cost for treating solid waste is further saved.
Detailed Description
Example 1
A green cycle method for maltol production is characterized in that: the method comprises the following steps:
a: adding water into solid waste containing the alkali magnesium chloride generated in the production of ethyl maltol, and uniformly stirring, wherein the weight ratio of the water to the solid waste containing the alkali magnesium chloride is 1.8;
b: pumping the alkali-containing magnesium chloride waste liquid into a distillation still, carrying out reduced pressure distillation to obtain an organic solvent in the alkali-containing magnesium chloride waste liquid, and drying the organic solvent for recycling of an ethyl maltol production system;
c: adding a dilute hydrochloric acid solution into the basic magnesium chloride-containing waste liquid until the pH value of the solution is 5, wherein the mass fraction of the dilute hydrochloric acid solution is 14%;
d: c, enabling the solution obtained in the step c to pass through a filter, wherein the filter is a tubular filter, and activated carbon is arranged in the tubular filter;
e: transferring the solution obtained after filtering in the step d into a reaction kettle, dropwise adding a sodium hydroxide solution into the reaction kettle, slowly stirring, and reacting for 2 hours, wherein the adding amount of the sodium hydroxide solution is 1.10 times of the theoretical demand, and the molar concentration of the sodium hydroxide solution is 3mol/L;
f: and e, transferring the solution obtained after the reaction in the step e into a centrifugal machine, washing a magnesium hydroxide filter cake obtained after centrifugation to remove sodium chloride, drying the magnesium hydroxide filter cake at 100 ℃, crushing and grading, inspecting and packaging.
The dilute hydrochloric acid solution in step c comes from the waste acid recovered in the production of ethyl maltol.
Further comprising the step of g: and f, rectifying the washing waste liquid containing the sodium chloride obtained in the step f, removing impurities, and electrolyzing to obtain a sodium hydroxide solution, wherein the sodium hydroxide solution is used in the step e.
Detection shows that the final magnesium recovery rate reaches 94.31%, and the product purity reaches 95.83%.
Example 2
Compared with example 1, the difference of this example is that the mass fraction of the dilute hydrochloric acid solution in step c is 13%, the amount of the sodium hydroxide solution added in step e is 1.05 times of the theoretical requirement, and the molar concentration of the sodium hydroxide solution is 2.5mol/L. The detection proves that the recovery rate of the magnesium in the embodiment reaches 94.57%, and the product purity reaches 95.92%.
Example 3
Compared with the example 2, the difference of the example is that the mass fraction of the dilute hydrochloric acid solution in the step c is 13%, the addition amount of the sodium hydroxide solution in the step e is 1.15 times of the theoretical requirement amount, and the molar concentration of the sodium hydroxide solution is 4mol/L. The detection proves that the recovery rate of the magnesium in the embodiment reaches 93.87%, and the product purity reaches 95.16%.
Example 4
Compared with example 3, the difference of this example is that the mass fraction of the dilute hydrochloric acid solution in step c is 15%, the amount of the sodium hydroxide solution added in step e is 1.05 times of the theoretical requirement, and the molar concentration of the sodium hydroxide solution is 2.5mol/L. The detection proves that the recovery rate of the magnesium in the example reaches 94.13 percent, and the product purity reaches 95.72 percent.
Example 5
Compared with example 4, the difference of this example is that the mass fraction of the dilute hydrochloric acid solution in step c is 15%, the amount of the sodium hydroxide solution added in step e is 1.15 times of the theoretical requirement, and the molar concentration of the sodium hydroxide solution is 4mol/L. The detection proves that the recovery rate of the magnesium in the embodiment reaches 93.25 percent, and the product purity reaches 95.07 percent.
Example 6
Compared with the example 1, the difference of the example is that in the step e, a sodium hydroxide solution with a molar concentration of 4mol/L is firstly dripped into the reaction kettle, and when the solution in the reaction kettle becomes turbid, a sodium hydroxide solution with a molar concentration of 2.5mol/L is dripped. The detection proves that the recovery rate of the magnesium in the embodiment reaches 97.85 percent, and the product purity reaches 96.39 percent.
Example 7
Compared with the embodiment 6, the difference of the embodiment is that in the step e, the sodium hydroxide solution with the molar concentration of 4mol/L is firstly dripped into the reaction kettle, and the sodium hydroxide solution with the molar concentration of 2.8mol/L is dripped when the solution in the reaction kettle becomes turbid. The detection proves that the recovery rate of the magnesium in the embodiment reaches 98.31 percent, and the product purity reaches 97.05 percent.
Example 8
Compared with the embodiment 6, the difference of the embodiment is that in the step e, the sodium hydroxide solution with the molar concentration of 4mol/L is firstly dripped into the reaction kettle, and the sodium hydroxide solution with the molar concentration of 3.0mol/L is dripped when the solution in the reaction kettle becomes turbid. The detection proves that the recovery rate of the magnesium in the embodiment reaches 97.12 percent, and the product purity reaches 95.92 percent.
Comparative example 1
The comparative example differs from example 1 in that the mass fraction of the dilute hydrochloric acid solution in step c is 12%. The detection proves that the recovery rate of the magnesium in the comparative example reaches 92.18 percent, and the product purity reaches 91.87 percent.
Comparative example 2
The comparative example differs from example 1 in that the molar concentration of the sodium hydroxide solution in step e is 2mol/L. The detection proves that the recovery rate of the magnesium in the comparative example reaches 87.21 percent, and the product purity reaches 96.08 percent.
Comparative example 3
The comparative example is different from example 1 in that the molar concentration of the sodium hydroxide solution in step e is 5mol/L. The detection proves that the recovery rate of the magnesium in the comparative example reaches 89.75 percent, and the product purity reaches 92.39 percent.
Comparative example 4
The present comparative example differs from example 1 in that the amount of sodium hydroxide solution added in step e is 1 times the theoretical requirement. The detection proves that the recovery rate of the magnesium in the comparative example reaches 85.90 percent, and the product purity reaches 95.01 percent.
Comparative example 5
The present comparative example differs from example 1 in that the amount of sodium hydroxide solution added in step e is 1.2 times the theoretical requirement. The detection proves that the recovery rate of the magnesium in the comparative example reaches 93.57%, and the product purity reaches 95.23%.
Comparative example 6
Compared with example 6, the difference of this comparative example is that in step e, a sodium hydroxide solution with a molar concentration of 5mol/L is firstly dripped into the reaction kettle, and when the solution in the reaction kettle becomes turbid, a sodium hydroxide solution with a molar concentration of 2.5mol/L is dripped. The detection proves that the recovery rate of the magnesium in the comparative example reaches 90.69%, and the product purity reaches 93.20%.
Comparative example 7
Compared with example 6, the difference of this comparative example is that in step e, a sodium hydroxide solution with a molar concentration of 4mol/L is firstly dripped into the reaction kettle, and when the solution in the reaction kettle becomes turbid, a sodium hydroxide solution with a molar concentration of 2mol/L is dripped. The detection proves that the recovery rate of the magnesium in the comparative example reaches 91.79 percent, and the product purity reaches 96.79 percent.
Comparative example 8
Compared with the example 6, the difference of the comparative example is that in the step e, the sodium hydroxide solution with the molar concentration of 4mol/L is firstly dripped into the reaction kettle, and when the solution in the reaction kettle becomes turbid, the sodium hydroxide solution with the molar concentration of 3.5mol/L is dripped. The detection proves that the recovery rate of the magnesium in the comparative example reaches 92.95 percent, and the product purity reaches 93.54 percent.
As can be seen from examples 1-8, the final recovery rate of magnesium by the green recycling method for maltol production disclosed by the invention reaches more than 93%, and the purity of the obtained magnesium hydroxide product reaches more than 95%. Further, the comparison between examples 1 to 5 and examples 6 to 8 shows that the manner of adding the sodium hydroxide solution dropwise greatly affects the results. The method comprises the steps of firstly dripping the sodium hydroxide solution with higher concentration and then dripping the sodium hydroxide solution with lower concentration, so that the recovery rate of magnesium can be obviously improved, the granularity of the obtained magnesium hydroxide crystal is better, and the filtering performance of the magnesium hydroxide crystal is also improved. After the inventor analyzes, it is considered that the solution should be added with sodium hydroxide solution with higher concentration first, the generation speed of magnesium hydroxide crystal nucleus generated in the solution is much higher than the growth speed of the crystal nucleus, and then added with sodium hydroxide solution with lower concentration, because there are a lot of magnesium hydroxide crystal nucleus in the solution, and the sodium hydroxide solution with lower concentration, the generation speed of the magnesium hydroxide crystal nucleus is reduced, the growth speed of the crystal nucleus is increased, and finally magnesium hydroxide crystal with larger particle and easy precipitation and filtration is formed. Further, by comparing examples 6 to 8 with comparative example 6, the final result is not desirable when the concentration of the sodium hydroxide solution added first is large, such as 5mol/L. By comparing examples 6-8 with comparative examples 7-8, the results are worse when the molar concentration of the second addition of sodium hydroxide solution is smaller, such as 2mol/L, or larger, such as 3.5 mol/L. From a comparison of examples 1 to 5 with comparative example 1, it can be seen that not only the recovery of magnesium is reduced but also the product purity is reduced when a hydrochloric acid solution having a lower concentration than that required in the present invention is used. By comparing examples 1-5 with comparative examples 2, 3, it can be seen that the recovery of magnesium is significantly reduced when using sodium hydroxide solutions of lower or higher concentration than required by the present invention. By comparing examples 1-6 with comparative examples 4, 5, it can be seen that the amount of sodium hydroxide solution added also affects the recovery of magnesium and the product purity. As can be seen from comparative examples 1 to 5, the mass fraction of dilute hydrochloric acid, the molar concentration of the sodium hydroxide solution and the amount added all have an influence on the recovery rate of magnesium and the purity of the product, resulting in unsatisfactory results.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered as the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (2)
1. A green circulation method for producing ethyl maltol is characterized in that: the method comprises the following steps: a: adding water into the solid waste containing the alkali magnesium chloride generated in the production of the ethyl maltol and uniformly stirring, wherein the weight ratio of the water to the solid waste containing the alkali magnesium chloride is 1.8-2;
b: pumping the alkali-containing magnesium chloride waste liquid into a distillation still, carrying out reduced pressure distillation to obtain an organic solvent in the alkali-containing magnesium chloride waste liquid, and drying the organic solvent for recycling by an ethyl maltol production system;
c: adding a dilute hydrochloric acid solution into the basic magnesium chloride-containing waste liquid until the pH value of the solution is 4-6, wherein the mass fraction of the dilute hydrochloric acid solution is 13-15%;
d: c, enabling the solution obtained in the step c to pass through a filter, wherein the filter is a tubular filter, and activated carbon is arranged in the tubular filter;
e: transferring the solution obtained after filtering in the step d into a reaction kettle, dropwise adding a sodium hydroxide solution into the reaction kettle, slowly stirring, dropwise adding the sodium hydroxide solution with the molar concentration of 4mol/L, dropwise adding the sodium hydroxide solution with the molar concentration of 2.5-3 mol/L when the solution in the reaction kettle becomes turbid, and reacting for 2 hours, wherein the addition amount of the sodium hydroxide solution is 1.05-1.15 times of the theoretical demand amount;
f: transferring the solution obtained after the reaction in the step e into a centrifugal machine, washing a magnesium hydroxide filter cake obtained after centrifugation to remove sodium chloride, drying the magnesium hydroxide filter cake at 100-110 ℃, crushing and grading, inspecting and packaging;
g: and f, rectifying the washing waste liquid containing the sodium chloride obtained in the step f, removing impurities, and electrolyzing to obtain a sodium hydroxide solution, wherein the sodium hydroxide solution is used in the step e.
2. The green recycling method of ethyl maltol as claimed in claim 1, wherein the dilute hydrochloric acid solution in step c is obtained from waste acid recovered from ethyl maltol production.
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| CN113698291B (en) * | 2021-08-17 | 2022-08-19 | 安徽金禾实业股份有限公司 | Method and device for treating acetic acid in acidic DMF and co-producing magnesium acetate |
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| "乙基麦芽酚绿色循环工艺";南强;《中国优秀硕士论文全文数据库》;20080415(第4期);第40-41页 * |
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