CN113004168A - Production process of methoxyamine for synthesizing furan ammonium salt - Google Patents
Production process of methoxyamine for synthesizing furan ammonium salt Download PDFInfo
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Abstract
The invention discloses a production process of methoxyamine for synthesizing furan ammonium salt, which comprises the steps of preparing solution in the early stage, oximation, methylation, hydrolysis and product refining, wherein the amount of sulfur dioxide in a system needs to be continuously detected in oximation reaction, the introduction speed of sulfur dioxide gas is continuously adjusted, and the introduction speed of the sulfur dioxide gas is kept to be high before low. According to the invention, the adding speed of the raw material gas is controlled in the production process of the methoxyamine, the concentration of the raw material gas in the reaction kettle is detected in real time, the reaction speed and the reaction degree of the raw material are further judged in real time, the reaction is effectively controlled, the waste of the raw material is reduced, and the yield of the product methoxyamine is improved.
Description
Technical Field
The invention relates to the technical field of medical intermediates, in particular to a production process of methoxyamine for synthesizing furan ammonium salt.
Background
The methoxyamine is an important chemical product and a medical intermediate, and has a wide application range. For example, methoxyamine can be used for color photography and film development, and can be used as a reducing agent in the organic synthesis industry to prepare oximes, and can be used for producing pharmaceutical intermediates such as furan amine salts in the pharmaceutical field. Worldwide demand for methoxyamine has reached tens of thousands of tons, but the production capacity at present cannot meet the demand. However, China has no large-scale manufacturers, the research on the aspect is rarely reported, and some related synthetic research reports exist abroad, but the mature production process data for production is lacked.
At present, in the process of preparing methoxyamine, materials cannot be well controlled, and the yield of the methoxyamine cannot be improved, so that the design and development of a production process of the methoxyamine for synthesizing furan ammonium salt have important practical significance.
Disclosure of Invention
In order to solve the problems mentioned in the background technology, the invention provides a production process of methoxyamine for synthesizing furan ammonium salt.
In order to achieve the purpose, the invention adopts the following technical scheme:
a production process of methoxyamine for synthesizing furan ammonium salt comprises the following steps:
step S1: solution preparation
Uniformly mixing sodium metabisulfite, sodium nitrite and water according to a proportion to obtain a mixed solution; step S2: oximation step
Adding the mixed solution obtained in the step S1 into a reaction kettle, introducing sulfur dioxide gas into the reaction kettle, reacting at normal pressure, continuously detecting the pH value of the reaction liquid in the reaction kettle, stopping introducing the sulfur dioxide gas when the pH value in the reaction kettle is at a critical value, adding alkali liquor into the reaction kettle, and neutralizing the unreacted sulfur dioxide gas until the pH value of the reaction liquid is more than or equal to 12;
step S3: methylation procedure
Transferring the reaction liquid in the step S2 into a methylation kettle, introducing dimethyl sulfate and alkali liquor into the kettle, reacting at normal pressure, and after the reaction is finished, transferring the kettle liquid into the next procedure;
step S4: hydrolysis step
Transferring the kettle liquid obtained in the step S3 into a hydrolysis kettle, adding sulfuric acid into the hydrolysis kettle, adjusting the pH, adjusting the hydrolysis temperature by using steam and circulating water, leading out gas and burning after hydrolysis is finished, and leaving the hydrolysis kettle bottom liquid for the next procedure;
step S5: refining step
Distilling the bottom liquid of the hydrolysis kettle, adding sodium hydroxide, adjusting the pH value, performing under normal pressure, and absorbing water to obtain a finished methoxylamine solution.
Preferably, the ratio of the sodium metabisulfite to the sodium nitrite in the step S1 is 1: 1-3.
Preferably, the reaction temperature in the step S2 is-5-5 ℃, the critical value pH is 2-3, the alkali solution is a sodium hydroxide solution, and the final pH of the reaction solution is greater than or equal to 12.
Preferably, the bottom liquid of the reaction kettle in the step S2 is condensed and cooled to-5-10 ℃, and then returned to the reaction kettle for circular reaction.
Preferably, the addition amount of the dimethyl sulfate in the step S3 is 1-2 times of the sodium metabisulfite, and the reaction temperature is 40-50 ℃.
Preferably, the kettle bottom liquid in the step S3 is condensed and cooled to 30-40 ℃, and then returned to the methylation kettle for circular reaction.
Preferably, the hydrolysis temperature in the step S4 is 100-105 ℃, and the pH is adjusted to be less than 1.
Preferably, the temperature of the distillation operation in the step S5 is 95 to 105 ℃, the reflux ratio in the distillation is in the range of 7 to 9, and the pH is adjusted.
Preferably, the still bottom solution obtained by distillation in the step S5 is subjected to pressure filtration to filter out sulfate, the filtrate is collected and subjected to single-effect evaporation and concentration, the water is recycled, and the waste liquid is recycled.
Preferably, in the step S2, the amount of sulfur dioxide in the system needs to be continuously detected, and the introduction speed of the sulfur dioxide gas needs to be continuously adjusted to keep the introduction speed of the sulfur dioxide gas to be fast first and slow last.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the adding speed of the raw material gas is controlled in the production process of the methoxyamine, the concentration of the raw material gas in the reaction kettle is detected in real time, and then the reaction speed and degree of the raw material are judged in real time, so that the reaction is effectively controlled, the waste of the raw material is reduced, and the yield of the product methoxyamine is improved;
2. the waste gas generated by hydrolysis is incinerated in the production process of methoxyamine, so that the pollution of the waste gas is avoided, and a heat source is provided by incineration;
3. the invention improves the purity of the product by refining the crude product, and the purified sulfate can be reused or sold for sale, and can realize the recycling of water resources and reduce waste.
In conclusion, the invention overcomes the defects of the prior art, has reasonable design and higher social use value and application prospect.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a block diagram of the production process of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A production process of methoxyamine for synthesizing furan ammonium salt comprises the following steps:
step S1: solution preparation
Uniformly mixing sodium metabisulfite, sodium nitrite and water according to the ratio of 1:1 to obtain a mixed solution;
step S2: oximation step
Adding the mixed solution obtained in the step S1 into a reaction kettle, introducing sulfur dioxide gas into the reaction kettle, reacting at the temperature of minus 5 ℃ under normal pressure, continuously detecting the pH value of reaction liquid in the reaction kettle, stopping introducing the sulfur dioxide gas when the pH value in the reaction kettle is within a critical value of 2-3, adding a sodium hydroxide solution into the reaction kettle, neutralizing unreacted sulfur dioxide gas until the pH value of the reaction liquid is more than or equal to 12, continuously detecting the amount of sulfur dioxide in a system in the process, continuously adjusting the introduction speed of the sulfur dioxide gas, keeping the introduction speed of the sulfur dioxide gas to be fast first and slow later, condensing and cooling the bottom liquid of the reaction kettle to the temperature of minus 5 ℃, returning the bottom liquid to the reaction kettle, and carrying out circular reaction;
step S3: methylation procedure
Transferring the reaction liquid in the step S2 into a methylation kettle, introducing dimethyl sulfate and alkali liquor into the kettle, wherein the addition amount of the dimethyl sulfate is 1 time of that of sodium metabisulfite, reacting at 40 ℃ under normal pressure, transferring the kettle liquid into the next procedure after the reaction is finished, condensing and cooling the kettle bottom liquid to 30 ℃, and returning the kettle bottom liquid to the methylation kettle for circular reaction;
step S4: hydrolysis step
Transferring the kettle liquid obtained in the step S3 into a hydrolysis kettle, adding sulfuric acid into the hydrolysis kettle, adjusting the pH to be less than 1, adjusting the hydrolysis temperature to 100 ℃ by using steam and circulating water, leading out gas and burning after hydrolysis is finished, and leaving the hydrolysis kettle bottom liquid for the next process;
step S5: refining step
Distilling the bottom liquid of the hydrolysis kettle, adding sodium hydroxide, adjusting the pH value to 7-9, performing water absorption at the temperature of 95 ℃ under normal pressure to obtain a finished methoxyamine solution, performing pressure filtration on the bottom liquid of the hydrolysis kettle after distillation, filtering out sulfate, collecting filtrate, performing single-effect evaporation and concentration, recycling water, and recovering waste liquid.
Example 2
A production process of methoxyamine for synthesizing furan ammonium salt comprises the following steps:
step S1: solution preparation
Uniformly mixing sodium metabisulfite, sodium nitrite and water according to the ratio of 1:2 to obtain a mixed solution;
step S2: oximation step
Adding the mixed solution obtained in the step S1 into a reaction kettle, introducing sulfur dioxide gas into the reaction kettle, reacting at 0 ℃ under normal pressure, continuously detecting the pH value of the reaction liquid in the reaction kettle, stopping introducing the sulfur dioxide gas when the pH value in the reaction kettle is within a critical value of 2-3, adding a sodium hydroxide solution into the reaction kettle, neutralizing the unreacted sulfur dioxide gas until the pH value of the reaction liquid is more than or equal to 12, continuously detecting the amount of sulfur dioxide in the system in the process, continuously adjusting the introduction speed of the sulfur dioxide gas, keeping the introduction speed of the sulfur dioxide gas to be fast first and slow later, condensing and cooling the bottom liquid of the reaction kettle to 0 ℃, and then returning the bottom liquid to the reaction kettle for circular reaction;
step S3: methylation procedure
Transferring the reaction liquid in the step S2 into a methylation kettle, introducing dimethyl sulfate and alkali liquor into the kettle, wherein the addition amount of the dimethyl sulfate is 1.5 times of that of sodium metabisulfite, reacting at the temperature of 45 ℃ under normal pressure, transferring the kettle liquid into the next procedure after the reaction is finished, condensing and cooling the kettle bottom liquid to 35 ℃, and returning the kettle bottom liquid to the methylation kettle for circular reaction;
step S4: hydrolysis step
Transferring the kettle liquid obtained in the step S3 into a hydrolysis kettle, adding sulfuric acid into the hydrolysis kettle, adjusting the pH to be less than 1, adjusting the hydrolysis temperature to 102 ℃ by using steam and circulating water, leading out gas and burning after the hydrolysis is finished, and leaving the hydrolysis kettle bottom liquid for the next process;
step S5: refining step
Distilling the bottom liquid of the hydrolysis kettle, adding sodium hydroxide, adjusting the pH value to 7-9, performing normal pressure at 100 ℃, absorbing water to obtain a finished methoxyamine solution, performing pressure filtration on the bottom liquid of the hydrolysis kettle after distillation, filtering out sulfate, collecting filtrate, performing single-effect evaporation and concentration, recycling water, and recovering waste liquid.
Example 3
A production process of methoxyamine for synthesizing furan ammonium salt comprises the following steps:
step S1: solution preparation
Uniformly mixing sodium metabisulfite, sodium nitrite and water according to the proportion of 1:3 to obtain a mixed solution;
step S2: oximation step
Adding the mixed solution obtained in the step S1 into a reaction kettle, introducing sulfur dioxide gas into the reaction kettle, reacting at 5 ℃ under normal pressure, continuously detecting the pH value of the reaction liquid in the reaction kettle, stopping introducing the sulfur dioxide gas when the pH value in the reaction kettle is within a critical value of 2-3, adding a sodium hydroxide solution into the reaction kettle, neutralizing the unreacted sulfur dioxide gas until the pH value of the reaction liquid is more than or equal to 12, continuously detecting the amount of sulfur dioxide in the system in the process, continuously adjusting the introduction speed of the sulfur dioxide gas, keeping the introduction speed of the sulfur dioxide gas to be fast first and slow later, condensing and cooling the bottom liquid of the reaction kettle to 10 ℃, and then returning the bottom liquid to the reaction kettle for circular reaction;
step S3: methylation procedure
Transferring the reaction liquid in the step S2 into a methylation kettle, introducing dimethyl sulfate and alkali liquor into the kettle, wherein the addition amount of the dimethyl sulfate is 2 times of that of sodium metabisulfite, reacting at 50 ℃ under normal pressure, transferring the kettle liquid into the next procedure after the reaction is finished, condensing and cooling the kettle bottom liquid to 40 ℃, and returning the kettle bottom liquid to the methylation kettle for circular reaction;
step S4: hydrolysis step
Transferring the kettle liquid obtained in the step S3 into a hydrolysis kettle, adding sulfuric acid into the hydrolysis kettle, adjusting the pH to be less than 1, adjusting the hydrolysis temperature to 105 ℃ by using steam and circulating water, leading out gas and burning after the hydrolysis is finished, and leaving the hydrolysis kettle bottom liquid for the next process;
step S5: refining step
Distilling the bottom liquid of the hydrolysis kettle, adding sodium hydroxide, adjusting the pH value to 7-9, performing normal pressure at 105 ℃, absorbing water to obtain a finished methoxyamine solution, performing pressure filtration on the bottom liquid of the hydrolysis kettle after distillation, filtering out sulfate, collecting filtrate, performing single-effect evaporation and concentration, recycling water, and recovering waste liquid.
Comparative example 1
A production process of methoxyamine for synthesizing furan ammonium salt comprises the following steps:
step S1: solution preparation
Uniformly mixing sodium metabisulfite, sodium nitrite and water according to the ratio of 1:2 to obtain a mixed solution;
step S2: oximation step
Adding the mixed solution obtained in the step S1 into a reaction kettle, introducing sulfur dioxide gas into the reaction kettle, reacting at 0 ℃ under normal pressure, continuously detecting the pH value of the reaction liquid in the reaction kettle, stopping introducing the sulfur dioxide gas when the pH value in the reaction kettle is within a critical value of 2-3, adding a sodium hydroxide solution into the reaction kettle, neutralizing the unreacted sulfur dioxide gas until the pH value of the reaction liquid is more than or equal to 12, condensing and cooling the bottom liquid of the reaction kettle to 0 ℃, returning the bottom liquid to the reaction kettle, and carrying out a circular reaction;
step S3: methylation procedure
Transferring the reaction liquid in the step S2 into a methylation kettle, introducing dimethyl sulfate and alkali liquor into the kettle, wherein the addition amount of the dimethyl sulfate is 1.5 times of that of sodium metabisulfite, reacting at the temperature of 45 ℃ under normal pressure, transferring the kettle liquid into the next procedure after the reaction is finished, condensing and cooling the kettle bottom liquid to 35 ℃, and returning the kettle bottom liquid to the methylation kettle for circular reaction;
step S4: hydrolysis step
Transferring the kettle liquid obtained in the step S3 into a hydrolysis kettle, adding sulfuric acid into the hydrolysis kettle, adjusting the pH to be less than 1, adjusting the hydrolysis temperature to 102 ℃ by using steam and circulating water, leading out gas and burning after the hydrolysis is finished, and leaving the hydrolysis kettle bottom liquid for the next process;
step S5: refining step
Distilling the bottom liquid of the hydrolysis kettle, adding sodium hydroxide, adjusting the pH value to 7-9, performing normal pressure at 100 ℃, absorbing water to obtain a finished methoxyamine solution, performing pressure filtration on the bottom liquid of the hydrolysis kettle after distillation, filtering out sulfate, collecting filtrate, performing single-effect evaporation and concentration, recycling water, and recovering waste liquid.
Comparative example 2
A production process of methoxyamine for synthesizing furan ammonium salt comprises the following steps:
step S1: solution preparation
Uniformly mixing sodium metabisulfite, sodium nitrite and water according to the ratio of 1:2 to obtain a mixed solution;
step S2: oximation step
Adding the mixed solution obtained in the step S1 into a reaction kettle, introducing sulfur dioxide gas into the reaction kettle, reacting at 0 ℃ under normal pressure, continuously detecting the pH value of the reaction liquid in the reaction kettle, stopping introducing the sulfur dioxide gas when the pH value in the reaction kettle is within a critical value of 2-3, adding a sodium hydroxide solution into the reaction kettle, neutralizing the unreacted sulfur dioxide gas until the pH value of the reaction liquid is more than or equal to 12, continuously detecting the amount of sulfur dioxide in the system in the process, continuously adjusting the introduction speed of the sulfur dioxide gas, keeping the introduction speed of the sulfur dioxide gas at a constant speed, condensing and cooling the bottom liquid of the reaction kettle to 0 ℃, then returning the bottom liquid to the reaction kettle, and carrying out a circular reaction;
step S3: methylation procedure
Transferring the reaction liquid in the step S2 into a methylation kettle, introducing dimethyl sulfate and alkali liquor into the kettle, wherein the addition amount of the dimethyl sulfate is 1.5 times of that of sodium metabisulfite, reacting at the temperature of 45 ℃ under normal pressure, transferring the kettle liquid into the next procedure after the reaction is finished, condensing and cooling the kettle bottom liquid to 35 ℃, and returning the kettle bottom liquid to the methylation kettle for circular reaction;
step S4: hydrolysis step
Transferring the kettle liquid obtained in the step S3 into a hydrolysis kettle, adding sulfuric acid into the hydrolysis kettle, adjusting the pH to be less than 1, adjusting the hydrolysis temperature to 102 ℃ by using steam and circulating water, leading out gas and burning after the hydrolysis is finished, and leaving the hydrolysis kettle bottom liquid for the next process;
step S5: refining step
Distilling the bottom liquid of the hydrolysis kettle, adding sodium hydroxide, adjusting the pH value to 7-9, performing normal pressure at 100 ℃, absorbing water to obtain a finished methoxyamine solution, performing pressure filtration on the bottom liquid of the hydrolysis kettle after distillation, filtering out sulfate, collecting filtrate, performing single-effect evaporation and concentration, recycling water, and recovering waste liquid.
Comparative example 3
A production process of methoxyamine for synthesizing furan ammonium salt comprises the following steps:
step S1: solution preparation
Uniformly mixing sodium metabisulfite, sodium nitrite and water according to the ratio of 1:2 to obtain a mixed solution;
step S2: oximation step
Adding the mixed solution obtained in the step S1 into a reaction kettle, introducing sulfur dioxide gas into the reaction kettle, reacting at 0 ℃ under normal pressure, continuously detecting the pH value of the reaction liquid in the reaction kettle, stopping introducing the sulfur dioxide gas when the pH value in the reaction kettle is within a critical value of 2-3, adding a sodium hydroxide solution into the reaction kettle, neutralizing the unreacted sulfur dioxide gas until the pH value of the reaction liquid is more than or equal to 12, continuously detecting the amount of sulfur dioxide in the system in the process, continuously adjusting the introduction speed of the sulfur dioxide gas, keeping the slow and fast introduction speed of the sulfur dioxide gas, condensing and cooling the bottom liquid of the reaction kettle to 0 ℃, then returning the bottom liquid to the reaction kettle, and carrying out circular reaction;
step S3: methylation procedure
Transferring the reaction liquid in the step S2 into a methylation kettle, introducing dimethyl sulfate and alkali liquor into the kettle, wherein the addition amount of the dimethyl sulfate is 1.5 times of that of sodium metabisulfite, reacting at the temperature of 45 ℃ under normal pressure, transferring the kettle liquid into the next procedure after the reaction is finished, condensing and cooling the kettle bottom liquid to 35 ℃, and returning the kettle bottom liquid to the methylation kettle for circular reaction;
step S4: hydrolysis step
Transferring the kettle liquid obtained in the step S3 into a hydrolysis kettle, adding sulfuric acid into the hydrolysis kettle, adjusting the pH to be less than 1, adjusting the hydrolysis temperature to 102 ℃ by using steam and circulating water, leading out gas and burning after the hydrolysis is finished, and leaving the hydrolysis kettle bottom liquid for the next process;
step S5: refining step
Distilling the bottom liquid of the hydrolysis kettle, adding sodium hydroxide, adjusting the pH value to 7-9, performing normal pressure at 100 ℃, absorbing water to obtain a finished methoxyamine solution, performing pressure filtration on the bottom liquid of the hydrolysis kettle after distillation, filtering out sulfate, collecting filtrate, performing single-effect evaporation and concentration, recycling water, and recovering waste liquid.
Comparative example 4
A production process of methoxyamine for synthesizing furan ammonium salt comprises the following steps:
step S1: solution preparation
Uniformly mixing sodium metabisulfite, sodium nitrite and water according to the ratio of 1:2 to obtain a mixed solution;
step S2: oximation step
Adding the mixed solution obtained in the step S1 into a reaction kettle, introducing sulfur dioxide gas into the reaction kettle, reacting at 0 ℃ under normal pressure, continuously detecting the pH value of the reaction liquid in the reaction kettle, stopping introducing the sulfur dioxide gas when the pH value in the reaction kettle is within a critical value of 2-3, adding a sodium hydroxide solution into the reaction kettle, neutralizing the unreacted sulfur dioxide gas until the pH value of the reaction liquid is more than or equal to 12, continuously detecting the sulfur dioxide amount in the system in the process, continuously adjusting the introduction speed of the sulfur dioxide gas, and keeping the introduction speed of the sulfur dioxide gas to be fast first and slow later;
step S3: methylation procedure
Transferring the reaction liquid in the step S2 into a methylation kettle, introducing dimethyl sulfate and alkali liquor into the kettle, wherein the addition amount of the dimethyl sulfate is 1.5 times of that of sodium metabisulfite, reacting at the temperature of 45 ℃ under normal pressure, and after the reaction is finished, transferring the kettle liquid into the next procedure;
step S4: hydrolysis step
Transferring the kettle liquid obtained in the step S3 into a hydrolysis kettle, adding sulfuric acid into the hydrolysis kettle, adjusting the pH to be less than 1, adjusting the hydrolysis temperature to 102 ℃ by using steam and circulating water, leading out gas and burning after the hydrolysis is finished, and leaving the hydrolysis kettle bottom liquid for the next process;
step S5: refining step
Distilling the bottom liquid of the hydrolysis kettle, adding sodium hydroxide, adjusting the pH value to 7-9, performing normal pressure at 100 ℃, absorbing water to obtain a finished methoxyamine solution, performing pressure filtration on the bottom liquid of the hydrolysis kettle after distillation, filtering out sulfate, collecting filtrate, performing single-effect evaporation and concentration, recycling water, and recovering waste liquid.
Experimental part:
the yields of the methoxyamines of examples 1 to 3 and comparative examples 1 to 4 were calculated and the results are shown in Table 1 below:
| sample (I) | Condition | Yield of methoxyamine |
| Example 1 | SO2The speed of the inlet is first fast and then slow | 95％ |
| Example 2 | SO2The speed of the inlet is first fast and then slow | 98％ |
| Example 3 | SO2The speed of the inlet is first fast and then slow | 96％ |
| Comparative example 1 | Not controlling SO2Speed of introduction | 59％ |
| Comparative example 2 | SO2At a constant speed is introduced | 78％ |
| Comparative example 3 | SO2The speed of the inlet is slow first and then fast | 65％ |
| Comparative example 4 | Without material circulation | 83％ |
The results in the table above show that: when the introduction speed of the sulfur dioxide gas is controlled, the yield of the methoxyamine can be influenced to a certain extent, when the introduction speed of the sulfur dioxide gas is firstly high and then low, the yield of the methoxyamine is maximum, and when materials in the production process are subjected to cyclic treatment, the generation of the methoxyamine can be promoted.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be considered limiting of the invention.
In the present invention, unless otherwise expressly stated or limited, the terms "disposed," "mounted," "connected," "secured," and the like are to be construed broadly and can, for example, be fixedly connected, detachably connected, or integrally formed; they may be mechanically coupled, directly coupled, or indirectly coupled through intervening agents, both internally and/or in any other manner known to those skilled in the art. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
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 to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A production process of methoxyamine for synthesizing furan ammonium salt is characterized by comprising the following steps:
step S1: solution preparation
Uniformly mixing sodium metabisulfite, sodium nitrite and water according to a proportion to obtain a mixed solution;
step S2: oximation step
Adding the mixed solution obtained in the step S1 into a reaction kettle, introducing sulfur dioxide gas into the reaction kettle, reacting at normal pressure, continuously detecting the pH value of the reaction liquid in the reaction kettle, stopping introducing the sulfur dioxide gas when the pH value in the reaction kettle is at a critical value, adding alkali liquor into the reaction kettle, and neutralizing the unreacted sulfur dioxide gas until the pH value of the reaction liquid is more than or equal to 12;
step S3: methylation procedure
Transferring the reaction liquid in the step S2 into a methylation kettle, introducing dimethyl sulfate and alkali liquor into the kettle, reacting at normal pressure, and after the reaction is finished, transferring the kettle liquid into the next procedure;
step S4: hydrolysis step
Transferring the kettle liquid obtained in the step S3 into a hydrolysis kettle, adding sulfuric acid into the hydrolysis kettle, adjusting the pH, adjusting the hydrolysis temperature by using steam and circulating water, leading out gas and burning after hydrolysis is finished, and leaving the hydrolysis kettle bottom liquid for the next procedure;
step S5: refining step
Distilling the bottom liquid of the hydrolysis kettle, adding sodium hydroxide, adjusting the pH value, performing under normal pressure, and absorbing water to obtain a finished methoxylamine solution.
2. The production process of methoxyamine for the synthesis of furan ammonium salt as claimed in claim 1, wherein: the ratio of the sodium metabisulfite to the sodium nitrite in the step S1 is 1: 1-3.
3. The production process of methoxyamine for the synthesis of furan ammonium salt as claimed in claim 1, wherein: in the step S2, the reaction temperature is-5-5 ℃, the critical value pH is 2-3, the alkali liquor is sodium hydroxide solution, and the final pH of the reaction solution is greater than or equal to 12.
4. The production process of methoxyamine for the synthesis of furan ammonium salt as claimed in claim 1, wherein: and (4) condensing the bottom liquid of the reaction kettle in the step S2, cooling to-5-10 ℃, and returning to the reaction kettle for circular reaction.
5. The production process of methoxyamine for the synthesis of furan ammonium salt as claimed in claim 1, wherein: in the step S3, the addition amount of dimethyl sulfate is 1-2 times of that of sodium metabisulfite, and the reaction temperature is 40-50 ℃.
6. The production process of methoxyamine for the synthesis of furan ammonium salt as claimed in claim 1, wherein: and (4) condensing the kettle bottom liquid in the step S3, cooling to 30-40 ℃, and returning to the methylation kettle for circular reaction.
7. The production process of methoxyamine for the synthesis of furan ammonium salt as claimed in claim 1, wherein: the hydrolysis temperature in the step S4 is 100-105 ℃, and the pH is adjusted to be less than 1.
8. The production process of methoxyamine for the synthesis of furan ammonium salt as claimed in claim 1, wherein: the temperature of the distillation operation in step S5 is 95 to 105 ℃, the reflux ratio in the distillation is adjusted to pH 7 to 9.
9. The production process of methoxyamine for the synthesis of furan ammonium salt as claimed in claim 1, wherein: and (4) performing pressure filtration on the still bottom liquid obtained by distillation in the step S5, filtering out sulfate, collecting filtrate, performing single-effect evaporation and concentration, recycling water, and recovering waste liquid.
10. The production process of methoxyamine for the synthesis of furan ammonium salt as claimed in claim 1, wherein: in the step S2, the amount of sulfur dioxide in the system needs to be continuously detected, and the introduction speed of the sulfur dioxide gas needs to be continuously adjusted to keep the introduction speed of the sulfur dioxide gas to be fast first and slow later.
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| CN114133338A (en) * | 2021-11-17 | 2022-03-04 | 安徽金轩科技有限公司 | Device and method for recovering methoxyamine from oximation wastewater in production of furan ammonium salt |
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