CN111268698A - Preparation method of sodium sulfite microspheres for oxygen-free ethanol process - Google Patents
Preparation method of sodium sulfite microspheres for oxygen-free ethanol process Download PDFInfo
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- CN111268698A CN111268698A CN202010086200.9A CN202010086200A CN111268698A CN 111268698 A CN111268698 A CN 111268698A CN 202010086200 A CN202010086200 A CN 202010086200A CN 111268698 A CN111268698 A CN 111268698A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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Abstract
The invention belongs to a chemical process, and particularly relates to a preparation method of sodium sulfite microspheres by an oxygen-free ethanol process, which comprises the following steps: step 1, adding polyvinylpyrrolidone into an ethanol-ether mixed solution, and uniformly stirring to form a dispersed suspension; step 2, adding sodium sulfite powder into the dispersed suspension, and stirring uniformly under a nitrogen environment to form mixed suspension; step 3, adding the mixed suspension into a mold, and carrying out constant-temperature extrusion reaction for 4-5h in a nitrogen environment to form prefabricated spherical particles; and 4, putting the prefabricated spherical particles into absolute ethyl alcohol, uniformly stirring to obtain a porous sphere, taking out, and drying at constant temperature to obtain the porous sodium sulfite microsphere. The invention solves the blank of the sodium sulfite microspheres, and simultaneously solves the problem of difficult separation of sodium sulfite in the oxygen-free ethanol process by utilizing the structural characteristics of the sodium sulfite microspheres.
Description
Technical Field
The invention belongs to a chemical process, relates to an oxygen-free ethanol process, and particularly relates to a preparation method of sodium sulfite microspheres in the oxygen-free ethanol process.
Background
Sodium sulfite is a common sulfite, white, monoclinic crystal or powder. Efflorescence and oxidation to sodium sulfate in air. The water of crystallization is lost at 150 ℃. And then melted into a mixture of sodium sulfide and sodium sulfate by reheating. Density of anhydrate 2.633. Sodium sulfite can be used for removing peroxide of ether substances in a laboratory (adding a small amount of water, separating liquid after a slightly-heated stirring reaction, drying an ether layer by quicklime and being used for some reactions with low requirements).
However, when sodium sulfite is used as a powder in an oxygen-free ethanol process, residual dissolved oxygen can be removed, but sodium sulfite forms a suspension system in an ethanol solution, which is extremely troublesome to separate by filtration, and greatly restricts the production efficiency of oxygen-free ethanol.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of sodium sulfite microspheres for an oxygen-free ethanol process, which solves the blank of the sodium sulfite microspheres, and simultaneously solves the problem of difficult separation of sodium sulfite in the oxygen-free ethanol process by utilizing the structural characteristics of the sodium sulfite microspheres.
In order to achieve the technical purpose, the technical scheme of the invention is as follows:
a preparation method of sodium sulfite microspheres for an oxygen-free ethanol process comprises the following steps:
step 1, adding polyvinylpyrrolidone into an ethanol-ether mixed solution, and uniformly stirring to form a dispersed suspension; the mass ratio of the ethanol to the ether in the ethanol-ether mixed solution is 1:3-6, the mass ratio of the polyvinylpyrrolidone to the ethanol is 3-5:10, and the stirring speed for uniformly stirring is 1000-2000 r/min;
step 2, adding sodium sulfite powder into the dispersed suspension, and stirring uniformly under a nitrogen environment to form mixed suspension; the adding amount of the sodium sulfite is 180 percent of the mass of the polyvinylpyrrolidone, and the stirring speed for uniformly stirring is 1000-2000 r/min;
step 3, adding the mixed suspension into a mold, and carrying out constant-temperature extrusion reaction for 4-5h in a nitrogen environment to form prefabricated spherical particles; the pressure of constant temperature extrusion is 2-4MPa, and the temperature is 90-100 ℃;
further, the constant-temperature extrusion reaction adopts a continuous heating method, and the specific procedures are as follows:
| temperature of | Pressure of | Time of day |
| 30-50℃ | 2-4MPa | 60-120min |
| 70-80℃ | 2-4MPa | 30-60min |
| 90-100℃ | 2-4MPa | Time remaining |
。
Step 4, putting the prefabricated spherical particles into absolute ethyl alcohol, uniformly stirring to obtain a porous sphere, taking out, and drying at constant temperature to obtain porous sodium sulfite microspheres; the stirring speed for stirring is 1000-2000r/min, and the nitrogen atmosphere is adopted for drying at constant temperature, and the temperature is 80-90 ℃.
From the above description, it can be seen that the present invention has the following advantages:
1. the invention solves the blank of the sodium sulfite microspheres, and simultaneously solves the problem of difficult separation of sodium sulfite in the oxygen-free ethanol process by utilizing the structural characteristics of the sodium sulfite microspheres.
2. The invention utilizes the dispersibility, cohesiveness and solubility of polyvinylpyrrolidone to realize the dispersion of sodium sulfite powder and the solidification and porosification of sodium sulfite microspheres.
3. The invention mainly uses physical separation, the produced ethanol liquid and the ether can be recycled, and the polyvinylpyrrolidone is dissolved in the ethanol for recycling, thereby greatly reducing the cost.
Detailed Description
The present invention is described in detail with reference to examples, but the present invention is not limited to the claims.
A preparation method of sodium sulfite microspheres for an oxygen-free ethanol process comprises the following steps:
step 1, adding polyvinylpyrrolidone into an ethanol-ether mixed solution, and uniformly stirring to form a dispersed suspension; the mass ratio of the ethanol to the ether in the ethanol-ether mixed solution is 1:3-6, the mass ratio of the polyvinylpyrrolidone to the ethanol is 3-5:10, and the stirring speed for uniformly stirring is 1000-2000 r/min; adding polyvinylpyrrolidone into the mixed solution of ethanol and ether, wherein the ethanol can dissolve the polyvinylpyrrolidone, and the ether-insoluble polyvinylpyrrolidone is larger than the ethanol, so that the polyvinylpyrrolidone forms a dispersed suspension system in the mixed solution;
step 2, adding sodium sulfite powder into the dispersed suspension, and stirring uniformly under a nitrogen environment to form mixed suspension; the adding amount of the sodium sulfite is 120-2000 r/min of the mass of the polyvinylpyrrolidone, and the stirring speed for uniformly stirring is 1000-2000 r/min. The sodium sulfite powder is added into the dispersion suspension, a suspension system can be formed by utilizing the insolubility of the sodium sulfite powder, and the polyvinylpyrrolidone ethanol solution has certain dispersibility, so that the sodium sulfite powder can be uniformly dispersed in the suspension.
Step 3, adding the mixed suspension into a mold, and carrying out constant-temperature extrusion reaction for 4-5h in a nitrogen environment to form prefabricated spherical particles; the pressure of constant temperature extrusion is 2-4MPa, and the temperature is 90-100 ℃; adding the suspension into a mold, carrying out constant-temperature extrusion reaction in a nitrogen environment, converting ethanol and ether into gaseous state by using a temperature condition to form ethanol ether steam, and causing polyvinylpyrrolidone to be separated from the ethanol for dissolution; the polyvinylpyrrolidone dissolved out of the ethanol has good viscosity effect, and the sodium sulfite powder is bonded together to form the prefabricated spherical particles.
Further, the constant-temperature extrusion reaction adopts a continuous heating method, and the specific procedures are as follows:
| temperature of | Pressure of | Time of day |
| 30-50℃ | 2-4MPa | 60-120min |
| 70-80℃ | 2-4MPa | 30-60min |
| 90-100℃ | 2-4MPa | Time remaining |
Under the condition of 30-50 ℃, in a constant-temperature reaction system, diethyl ether is quickly volatilized at the temperature, and simultaneously, the diethyl ether reaches a boiling point state and can be quickly converted into steam, and the ethanol is still liquid and still dissolves polyvinylpyrrolidone, but the viscosity is increased along with the reduction of the solvent, so that a spherical structure of a semi-solidified system is formed; converting ethanol into ethanol vapor at 70-80 deg.C, gradually separating out polyvinylpyrrolidone dissolved in ethanol with evaporation of ethanol, and uniformly dispersing into sodium sulfite to form spherical particles with uniformly dispersed sodium sulfite and polyvinylpyrrolidone; at the temperature of 90-100 ℃, residual ethanol and ether in the spherical particles are converted into steam, and simultaneously, under the pressure condition, the internal structure of the spherical particles is compact, and the number of gaps is sharply reduced.
Step 4, putting the prefabricated spherical particles into absolute ethyl alcohol, uniformly stirring to obtain a porous sphere, taking out, and drying at constant temperature to obtain porous sodium sulfite microspheres; the stirring speed for stirring is 1000-2000r/min, and the nitrogen atmosphere is adopted for drying at constant temperature, and the temperature is 80-90 ℃. The prefabricated spherical particles use polyvinylpyrrolidone as an adhesive, sodium sulfite powder as a frame material is extruded to form compact spherical particles, the prefabricated spherical particles are placed into oxygen-free ethanol, sodium sulfite does not form a dissolving system with the anhydrous ethanol, the polyvinylpyrrolidone can be dissolved in water to form a good dissolving structure, so that under the condition that the sodium sulfite still exists in the frame structure, a porous structure is formed in the spherical particles, constant-temperature drying is carried out in an oxygen-free environment, ethanol is converted into steam, the separation of the sodium sulfite from the anhydrous ethanol is realized, and the porous sodium sulfite microspheres are obtained.
Example 1
A preparation method of sodium sulfite microspheres for an oxygen-free ethanol process comprises the following steps:
step 1, adding polyvinylpyrrolidone into an ethanol-ether mixed solution, and uniformly stirring to form a dispersed suspension; the mass ratio of the ethanol to the ether in the ethanol-ether mixed solution is 1:3, the mass ratio of the polyvinylpyrrolidone to the ethanol is 3:10, and the stirring speed for uniformly stirring is 1000 r/min;
step 2, adding sodium sulfite powder into the dispersed suspension, and stirring uniformly under a nitrogen environment to form mixed suspension; the adding amount of the sodium sulfite is 120 percent of the mass of the polyvinylpyrrolidone, and the stirring speed for uniformly stirring is 1000 r/min;
step 3, adding the mixed suspension into a mold, and carrying out constant-temperature extrusion reaction for 4 hours in a nitrogen environment to form prefabricated spherical particles; the pressure of constant temperature extrusion is 2MPa, and the temperature is 90 ℃;
step 4, putting the prefabricated spherical particles into absolute ethyl alcohol, uniformly stirring to obtain a porous sphere, taking out, and drying at constant temperature to obtain porous sodium sulfite microspheres; stirring uniformly at a speed of 1000r/min, drying at constant temperature in a nitrogen atmosphere at a temperature of 80 ℃.
The porous sodium sulfite microspheres prepared by the embodiment have uniform pores, large specific surface and stable structure.
Example 2
A preparation method of sodium sulfite microspheres for an oxygen-free ethanol process comprises the following steps:
step 1, adding polyvinylpyrrolidone into an ethanol-ether mixed solution, and uniformly stirring to form a dispersed suspension; the mass ratio of the ethanol to the ether in the ethanol-ether mixed solution is 1:6, the mass ratio of the polyvinylpyrrolidone to the ethanol is 1:2, and the stirring speed for uniformly stirring is 2000 r/min;
step 2, adding sodium sulfite powder into the dispersed suspension, and stirring uniformly under a nitrogen environment to form mixed suspension; the adding amount of the sodium sulfite is 180 percent of the mass of the polyvinylpyrrolidone, and the stirring speed for uniformly stirring is 2000 r/min;
step 3, adding the mixed suspension into a mold, and carrying out constant-temperature extrusion reaction for 4-5h in a nitrogen environment to form prefabricated spherical particles; the pressure of constant temperature extrusion is 4MPa, and the temperature is 100 ℃;
step 4, putting the prefabricated spherical particles into absolute ethyl alcohol, uniformly stirring to obtain a porous sphere, taking out, and drying at constant temperature to obtain porous sodium sulfite microspheres; stirring speed of uniform stirring is 2000r/min, constant temperature drying adopts nitrogen atmosphere, and temperature is 90 ℃.
The porous sodium sulfite microspheres prepared by the embodiment have uniform pores, large specific surface and stable structure.
Example 3
A preparation method of sodium sulfite microspheres for an oxygen-free ethanol process comprises the following steps:
step 1, adding polyvinylpyrrolidone into an ethanol-ether mixed solution, and uniformly stirring to form a dispersed suspension; the mass ratio of the ethanol to the ether in the ethanol-ether mixed solution is 1:5, the mass ratio of the polyvinylpyrrolidone to the ethanol is 2:5, and the stirring speed for uniformly stirring is 1500 r/min;
step 2, adding sodium sulfite powder into the dispersed suspension, and stirring uniformly under a nitrogen environment to form mixed suspension; the adding amount of the sodium sulfite is 160 percent of the mass of the polyvinylpyrrolidone, and the stirring speed for uniformly stirring is 1500 r/min;
step 3, adding the mixed suspension into a mold, and carrying out constant-temperature extrusion reaction for 5 hours in a nitrogen environment to form prefabricated spherical particles; the pressure of constant temperature extrusion is 3MPa, and the temperature is 95 ℃;
step 4, putting the prefabricated spherical particles into absolute ethyl alcohol, uniformly stirring to obtain a porous sphere, taking out, and drying at constant temperature to obtain porous sodium sulfite microspheres; stirring uniformly at a speed of 1500r/min, drying at constant temperature in a nitrogen atmosphere at 85 ℃.
The porous sodium sulfite microspheres prepared by the embodiment have uniform pores, large specific surface and stable structure.
Example 4
A preparation method of sodium sulfite microspheres for an oxygen-free ethanol process comprises the following steps:
step 1, adding polyvinylpyrrolidone into an ethanol-ether mixed solution, and uniformly stirring to form a dispersed suspension; the mass ratio of the ethanol to the ether in the ethanol-ether mixed solution is 1:3, the mass ratio of the polyvinylpyrrolidone to the ethanol is 3:10, and the stirring speed for uniformly stirring is 1000 r/min;
step 2, adding sodium sulfite powder into the dispersed suspension, and stirring uniformly under a nitrogen environment to form mixed suspension; the adding amount of the sodium sulfite is 120 percent of the mass of the polyvinylpyrrolidone, and the stirring speed for uniformly stirring is 1000 r/min;
step 3, adding the mixed suspension into a mold, and carrying out constant-temperature extrusion reaction for 4 hours in a nitrogen environment to form prefabricated spherical particles; the constant-temperature extrusion reaction adopts a continuous heating method, and the specific procedures are as follows:
| temperature of | Pressure of | Time of day |
| 30℃ | 2MPa | 60min |
| 70℃ | 2MPa | 30min |
| 90℃ | 2MPa | Time remaining |
Step 4, putting the prefabricated spherical particles into absolute ethyl alcohol, uniformly stirring to obtain a porous sphere, taking out, and drying at constant temperature to obtain porous sodium sulfite microspheres; stirring uniformly at a speed of 1000r/min, drying at constant temperature in a nitrogen atmosphere at a temperature of 80 ℃.
The porous sodium sulfite microspheres prepared by the embodiment have uniform pores, large specific surface and stable structure.
Example 5
A preparation method of sodium sulfite microspheres for an oxygen-free ethanol process comprises the following steps:
step 1, adding polyvinylpyrrolidone into an ethanol-ether mixed solution, and uniformly stirring to form a dispersed suspension; the mass ratio of the ethanol to the ether in the ethanol-ether mixed solution is 1:6, the mass ratio of the polyvinylpyrrolidone to the ethanol is 1:2, and the stirring speed for uniformly stirring is 2000 r/min;
step 2, adding sodium sulfite powder into the dispersed suspension, and stirring uniformly under a nitrogen environment to form mixed suspension; the adding amount of the sodium sulfite is 180 percent of the mass of the polyvinylpyrrolidone, and the stirring speed for uniformly stirring is 2000 r/min;
step 3, adding the mixed suspension into a mold, and carrying out constant-temperature extrusion reaction for 5 hours in a nitrogen environment to form prefabricated spherical particles; the constant-temperature extrusion reaction adopts a continuous heating method, and the specific procedures are as follows:
| temperature of | Pressure of | Time of day |
| 50℃ | 4MPa | 120min |
| 80℃ | 4MPa | 60min |
| 100℃ | 4MPa | Time remaining |
Step 4, putting the prefabricated spherical particles into absolute ethyl alcohol, uniformly stirring to obtain a porous sphere, taking out, and drying at constant temperature to obtain porous sodium sulfite microspheres; stirring speed of uniform stirring is 2000r/min, constant temperature drying adopts nitrogen atmosphere, and temperature is 90 ℃.
The porous sodium sulfite microspheres prepared by the embodiment have uniform pores, large specific surface and stable structure.
Example 6
A preparation method of sodium sulfite microspheres for an oxygen-free ethanol process comprises the following steps:
step 1, adding polyvinylpyrrolidone into an ethanol-ether mixed solution, and uniformly stirring to form a dispersed suspension; the mass ratio of the ethanol to the ether in the ethanol-ether mixed solution is 1:4, the mass ratio of the polyvinylpyrrolidone to the ethanol is 2:5, and the stirring speed for uniformly stirring is 1500 r/min;
step 2, adding sodium sulfite powder into the dispersed suspension, and stirring uniformly under a nitrogen environment to form mixed suspension; the adding amount of the sodium sulfite is 160 percent of the mass of the polyvinylpyrrolidone, and the stirring speed for uniformly stirring is 1500 r/min;
step 3, adding the mixed suspension into a mold, and carrying out constant-temperature extrusion reaction for 5 hours in a nitrogen environment to form prefabricated spherical particles; the constant-temperature extrusion reaction adopts a continuous heating method, and the specific procedures are as follows:
| temperature of | Pressure of | Time of day |
| 40℃ | 3MPa | 90min |
| 75℃ | 3MPa | 50min |
| 95℃ | 3MPa | Time remaining |
Step 4, putting the prefabricated spherical particles into absolute ethyl alcohol, uniformly stirring to obtain a porous sphere, taking out, and drying at constant temperature to obtain porous sodium sulfite microspheres; stirring uniformly at a speed of 1500r/min, drying at constant temperature in a nitrogen atmosphere at 85 ℃.
The porous sodium sulfite microspheres prepared by the embodiment have uniform pores, large specific surface and stable structure.
In summary, the invention has the following advantages:
1. the invention solves the blank of the sodium sulfite microspheres, and simultaneously solves the problem of difficult separation of sodium sulfite in the oxygen-free ethanol process by utilizing the structural characteristics of the sodium sulfite microspheres.
2. The invention utilizes the dispersibility, cohesiveness and solubility of polyvinylpyrrolidone to realize the dispersion of sodium sulfite powder and the solidification and porosification of sodium sulfite microspheres.
3. The invention mainly uses physical separation, the produced ethanol liquid and the ether can be recycled, and the polyvinylpyrrolidone is dissolved in the ethanol for recycling, thereby greatly reducing the cost.
It should be understood that the detailed description of the invention is merely illustrative of the invention and is not intended to limit the invention to the specific embodiments described. It will be appreciated by those skilled in the art that the present invention may be modified or substituted equally as well to achieve the same technical result; as long as the use requirements are met, the method is within the protection scope of the invention.
Claims (6)
1. A preparation method of sodium sulfite microspheres for an oxygen-free ethanol process is characterized by comprising the following steps: the method comprises the following steps:
step 1, adding polyvinylpyrrolidone into an ethanol-ether mixed solution, and uniformly stirring to form a dispersed suspension;
step 2, adding sodium sulfite powder into the dispersed suspension, and stirring uniformly under a nitrogen environment to form mixed suspension;
step 3, adding the mixed suspension into a mold, and carrying out constant-temperature extrusion reaction for 4-5h in a nitrogen environment to form prefabricated spherical particles;
and 4, putting the prefabricated spherical particles into absolute ethyl alcohol, uniformly stirring to obtain a porous sphere, taking out, and drying at constant temperature to obtain the porous sodium sulfite microsphere.
2. The method for preparing sodium sulfite microspheres for use in an oxygen-free ethanol process according to claim 1, wherein: the mass ratio of the ethanol to the ether in the ethanol-ether mixed solution in the step 1 is 1:3-6, the mass ratio of the polyvinylpyrrolidone to the ethanol is 3-5:10, and the stirring speed for uniformly stirring is 1000-2000 r/min.
3. The method for preparing sodium sulfite microspheres for use in an oxygen-free ethanol process according to claim 1, wherein: the adding amount of the sodium sulfite in the step 2 is 120-180% of the mass of the polyvinylpyrrolidone, and the stirring speed for uniformly stirring is 1000-2000 r/min.
4. The method for preparing sodium sulfite microspheres for use in an oxygen-free ethanol process according to claim 1, wherein: the pressure of the constant temperature extrusion in the step 3 is 2-4MPa, and the temperature is 90-100 ℃.
5. The method for preparing sodium sulfite microspheres for use in an oxygen-free ethanol process of claim 4, wherein: the constant-temperature extrusion reaction adopts a continuous heating method, and the specific procedures are as follows:
。
6. The method for preparing sodium sulfite microspheres for use in an oxygen-free ethanol process according to claim 1, wherein: the stirring speed for uniformly stirring in the step 4 is 1000-2000r/min, and the nitrogen atmosphere is adopted for constant-temperature drying at the temperature of 80-90 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112250101A (en) * | 2020-10-29 | 2021-01-22 | 焦祝根 | Method for in-situ preparation of nano zinc chloride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112250101A (en) * | 2020-10-29 | 2021-01-22 | 焦祝根 | Method for in-situ preparation of nano zinc chloride |
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