CN108929239B - Preparation method of sodium polysulfide - Google Patents
Preparation method of sodium polysulfide Download PDFInfo
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- C07C221/00—Preparation of compounds containing amino groups and doubly-bound oxygen atoms bound to the same carbon skeleton
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- C01B17/00—Sulfur; Compounds thereof
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- C01B17/34—Polysulfides of sodium or potassium
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Abstract
A preparation method of sodium polysulfide, belonging to the technical field of chemical products. The method comprises the following steps: preparing sodium polysulfide; step two: refining p-aminobenzaldehyde; step three: recycling the residual waste liquid to prepare sodium polysulfide; the preparation method of sodium polysulfide provided by the invention adopts the reaction of sodium sulfide, caustic soda and sulfur to prepare the sodium polysulfide. The sodium polysulfide prepared by the method is added to react to prepare the para aminobenzaldehyde, and the water phase obtained by liquid separation after the reaction is used as waste liquid, wherein the main components are sodium sulfide, sodium polysulfide, sodium thiosulfate, sodium hydroxide, water, sodium hydrosulfide, unreacted sulfur and the like. And carrying out suction filtration on the waste liquid, removing unreacted sulfur, and continuously reacting the filtrate, sodium sulfide, caustic soda and sulfur to prepare sodium polysulfide. The method can realize recycling of the produced residual waste liquid and save resources.
Description
Technical Field
The invention belongs to the technical field of chemical products, and relates to a preparation method of sodium polysulfide.
Background
Sodium polysulfide is a chemical substance mainly used as a polymerization terminator, as a depilatory for hides in the tanning industry, as an insecticide, and the like in agriculture. The traditional process is to prepare sodium polysulfide by reacting caustic soda with sulfur. The sodium polysulfide prepared by the process method is prepared by feeding materials for reaction to prepare the p-aminobenzaldehyde, and the water phase obtained by liquid separation after the reaction is used as waste liquid, wherein the main components in the waste liquid are sodium thiosulfate, sodium sulfide, water, sodium hydroxide and the like.
The waste liquid produced by the traditional process adopts a treatment method of purifying sodium thiosulfate as a byproduct product. The method has the characteristics of large amount, more impurities, low content of sodium thiosulfate, doping of a small amount of organic matters and the like, and is used for producing residual waste liquid in the traditional process. The output of waste liquid is large, and the storage cost investment is large; the impurities are more, the purification cost is high, the difficulty is high, and the production cost of the product is increased; sodium thiosulfate has a poor market prospect as a byproduct.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a preparation method of sodium polysulfide.
The technical scheme adopted by the invention to solve the technical problem is as follows: a preparation method of sodium polysulfide is designed, and comprises the following steps in sequence:
the method comprises the following steps: preparing sodium polysulfide;
a1, weighing a certain mass of Na2S·9H2Adding O, sublimed sulfur, water and sodium hydroxide into a reaction kettle respectively;
a2, stirring and heating, heating to 85 ℃, keeping the temperature and stirring for 3 hours after the materials are dissolved;
a3, cooling to room temperature after heat preservation, filtering out unreacted sulfur to obtain filtrate containing sodium polysulfide, and detecting the sodium polysulfide;
step two: refining p-aminobenzaldehyde;
b1, weighing a certain mass of p-nitrotoluene and ethanol, adding into the reaction kettle, starting stirring, heating, condensing, heating to 80 ℃, keeping refluxing, and continuing stirring for 30 min;
b2, uniformly dripping a certain mass of filtrate containing sodium polysulfide in the step one a3 at the temperature of 80 +/-1 ℃ for 1.5-2h, and after finishing dripping, keeping the temperature at 80 +/-1 ℃ for reacting for 3.5-3 h;
b3, after the heat preservation is finished, pouring the mixture into a kettle, standing for 2 hours, separating a lower-layer water phase, namely residual waste liquid, and detecting an upper-layer reducing liquid;
step three: recycling the residual waste liquid to prepare sodium polysulfide;
c1, detecting the residual alkali amount of the residual waste liquid in the step two b 3;
c2, weighing a certain mass of Na2S·9H2Adding O, sublimed sulfur, water, sodium hydroxide and residual waste liquid into a kettle, stirring, heating to 85 ℃, dissolving the materials clearly, stirring for 3 hours at a constant temperature, cooling to room temperature after the constant temperature is finished, filtering out unreacted sulfur to obtain filtrate containing sodium polysulfide, and detecting the sodium polysulfide;
c3, adding the prepared sodium polysulfide into the reaction kettle to prepare the para aminobenzaldehyde;
step four: and repeating the second step and the third step.
Preferably, Na as described in step one a12S·9H2The mass of O, sublimed sulfur, water and sodium hydroxide are respectively 17.6-19.5g, 9.1-10.1g, 192g and 13.2-15.6 g.
Preferably, the mass of the p-nitrotoluene and the ethanol in the step two b1 is 25g and 160ml respectively, and the mass of the filtrate containing the sodium polysulfide in the step b2 is 136-160 g.
Preferably, Na as described in step three c22S·9H2The mass of O, sublimed sulfur, water, sodium hydroxide and residual waste liquid are respectively 17.6-19.5g, 9.1-10.1g, 192g of 123-sodium silicate, 13.2-15.6g and 70-100 g.
The invention has the beneficial effects that:
1. the preparation method of sodium polysulfide provided by the invention adopts the reaction of sodium sulfide, caustic soda and sulfur to prepare the sodium polysulfide. The sodium polysulfide prepared by the method is added to react to prepare the para aminobenzaldehyde, and the water phase obtained by liquid separation after the reaction is used as waste liquid, wherein the main components are sodium sulfide, sodium polysulfide, sodium thiosulfate, sodium hydroxide, water, sodium hydrosulfide, unreacted sulfur and the like. And carrying out suction filtration on the waste liquid, removing unreacted sulfur, and continuously reacting the filtrate, sodium sulfide, caustic soda and sulfur to prepare sodium polysulfide. The method can realize recycling of the produced residual waste liquid and save resources.
Detailed Description
Example one
A method for preparing sodium polysulfide comprises the following steps in sequence:
the method comprises the following steps: preparing sodium polysulfide;
a1, respectively taking Na2S·9H2Adding 17.6 g of O, 9.1 g of sublimed sulfur, 15.6g of solid sodium hydroxide and 192g of water into a reaction kettle;
a2, stirring, heating to 85 ℃, dissolving the materials, keeping the temperature and stirring for 3 hours;
a3, after the reaction of heat preservation is finished, stopping heating, cooling to room temperature, filtering reaction liquid, filtering out unreacted sulfur, detecting the content of sodium polysulfide in the filtrate to be 62g/L, wherein the polysulfide index is 2.0;
step two: refining p-aminobenzaldehyde;
b1, weighing 25g of p-aminotoluene and 160ml of ethanol, adding into a three-necked bottle, stirring, heating, condensing, heating to 80 ℃, keeping large reflux, and continuing stirring for 30 min;
b2, weighing 136 g of sodium polysulfide, uniformly dropwise adding, keeping the temperature at 80 +/-1 ℃, keeping the dropwise adding time at 1.5-2h, and after the dropwise adding is finished, keeping the temperature at 80 +/-1 ℃ for reaction for 3.5-3 h;
b3, after the heat preservation is finished, stopping heating and stirring, pouring the mixture into the kettle, standing the mixture for 2 hours, separating a lower-layer water phase, namely residual waste liquid, and detecting the index of the upper-layer reducing liquid; the residual alkali amount is 4g/L, and the amino value is 80 g/L;
step three: recycling the residual waste liquid to prepare sodium polysulfide;
c1, detecting the residual alkali amount of the residual waste liquid in the step two b3, and separating 65 g of residual liquid;
c2 taking Na respectively2S·9H2Adding 17.6 g of O, 9.1 g of sublimed sulfur, 13.7 g of solid sodium hydroxide, 133 g of water and 60g of residual waste liquid into a reaction kettle, stirring, heating to 85 ℃, dissolving the materials clearly, stirring for 3 hours at a constant temperature, stopping heating after the reaction at the constant temperature is finished, cooling to room temperature, filtering the reaction liquid, filtering out unreacted sulfur, detecting the content of sodium polysulfide in the filtrate by 60g/L, wherein the polysulfide index is 2.1;
c3, adding the prepared sodium polysulfide into the reaction kettle to prepare the para aminobenzaldehyde;
step four: weighing 25g of p-aminotoluene and 160ml of ethanol, adding into a reaction kettle, stirring, heating, condensing, heating to 80 ℃, keeping large reflux, and continuing stirring for 30 min. Weighing 145 g of sodium polysulfide, uniformly dropwise adding, keeping the temperature at 80 +/-1 ℃, keeping the dropwise adding time at 1.5-2h, and after the dropwise adding is finished, keeping the temperature at 80 +/-1 ℃ for reacting for 3.5-3 h. And after the heat preservation is finished, stopping heating and stirring, pouring the mixture into the kettle, standing the mixture for 2 hours, separating a lower-layer water phase, namely separating residual waste liquid, and detecting the index of the upper-layer reducing liquid. The residual alkali amount is 3g/L, and the amino value is 83 g/L.
And detecting indexes of the residual waste liquid. The residue was taken out and 75 g was added.
Separately taking Na2S·9H2Adding 17.6 g of O, 9.1 g of sublimed sulfur, 13.4 g of solid sodium hydroxide, 124 g of water and 70 g of residual waste liquid into a three-neck flask, stirring, heating to 85 ℃, dissolving the materials clearly, stirring for 3 hours at the constant temperature, stopping heating after the reaction at the constant temperature is finished, cooling to room temperature, filtering the reaction liquid, filtering out unreacted sulfur, and detecting the index of sodium polysulfide in the filtrate. The sodium polysulfide content is 64g/L and the polysulfide index is 2.3.
Weighing 25g of p-aminotoluene and 160ml of ethanol, adding into a reaction kettle, stirring, heating, condensing, heating to 80 ℃, keeping large reflux, and continuing stirring for 30 min. Weighing 124 g of sodium polysulfide, uniformly dropwise adding, keeping the temperature at 80 +/-1 ℃, keeping the dropwise adding time at 1.5-2h, and after the dropwise adding is finished, keeping the temperature at 80 +/-1 ℃ for reacting for 3.5-3 h. And after the heat preservation is finished, stopping heating and stirring, pouring the mixture into the kettle, standing the mixture for 2 hours, separating a lower-layer water phase, namely separating residual waste liquid, and detecting the index of the upper-layer reducing liquid. The residual alkali amount is 3.3g/L, and the amino value is 79 g/L.
And detecting indexes of the residual waste liquid. The residue was taken up in 68 g.
Example two
A method for preparing sodium polysulfide comprises the following steps in sequence:
the method comprises the following steps: preparing sodium polysulfide;
a1, respectively taking Na2S·9H219.5g of O, 10.1g of sublimed sulfur, 13.2 g of solid sodium hydroxide and 123 g of water are added into a reaction kettle；
a2, stirring, heating to 85 ℃, dissolving the materials, keeping the temperature and stirring for 3 hours;
a3, after the reaction of heat preservation is finished, stopping heating, cooling to room temperature, filtering reaction liquid, filtering out unreacted sulfur, detecting the content of sodium polysulfide in the filtrate to be 62g/L, wherein the polysulfide index is 2.7;
step two: refining p-aminobenzaldehyde;
b1, weighing 25g of p-aminotoluene and 160ml of ethanol, adding into a three-necked bottle, stirring, heating, condensing, heating to 80 ℃, keeping large reflux, and continuing stirring for 30 min;
b2, weighing 160g of sodium polysulfide, uniformly dropwise adding, keeping the temperature at 80 +/-1 ℃, keeping the dropwise adding time at 1.5-2h, and after the dropwise adding is finished, keeping the temperature at 80 +/-1 ℃ for reaction for 3.5-3 h;
b3, after the heat preservation is finished, stopping heating and stirring, pouring the mixture into the kettle, standing the mixture for 2 hours, separating a lower-layer water phase, namely residual waste liquid, and detecting the index of the upper-layer reducing liquid; the residual alkali amount is 4.3g/L, the amino value is 106.6 g/L;
step three: recycling the residual waste liquid to prepare sodium polysulfide;
c1, detecting the residual alkali amount of the residual waste liquid in the step two b3, and separating 65 g of residual liquid;
c2 taking Na respectively2S·9H29.5g of O, 10.2 g of sublimed sulfur, 12.7 g of solid sodium hydroxide, 113.4 g of water and 100g of residual waste liquid are added into a reaction kettle, the mixture is stirred and heated, the temperature is raised to 85 ℃, the materials are dissolved and clear, the mixture is stirred for 3 hours under the condition of heat preservation, after the heat preservation reaction is finished, the heating is stopped, the temperature is reduced to the room temperature, the reaction liquid is filtered, the unreacted sulfur is filtered out, the content of sodium polysulfide in the filtrate is detected to be 56g/L, and the index of polysulfide is 3;
c3, adding the prepared sodium polysulfide into the reaction kettle to prepare the para aminobenzaldehyde;
step four: weighing 25g of p-aminotoluene and 160ml of ethanol, adding into a reaction kettle, stirring, heating, condensing, heating to 80 ℃, keeping large reflux, and continuing stirring for 30 min. Weighing 193 g of sodium polysulfide, uniformly dropwise adding, keeping the temperature at 80 +/-1 ℃, keeping the dropwise adding time at 1.5-2h, and after the dropwise adding is finished, keeping the temperature at 80 +/-1 ℃ for reaction for 3.5-3 h. And after the heat preservation is finished, stopping heating and stirring, pouring the mixture into the kettle, standing the mixture for 2 hours, separating a lower-layer water phase, namely separating residual waste liquid, and detecting the index of the upper-layer reducing liquid. The residual alkali amount is 3.4g/L, and the amino value is 106.5 g/L.
And detecting indexes of the residual waste liquid. The residue was taken up in 126 g.
Finally, it should be noted that: although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and it is intended to cover in the claims the invention as defined in the appended claims.
A preparation method of sodium polysulfide, belonging to the technical field of chemical products. The method comprises the following steps: preparing sodium polysulfide; step two: refining p-aminobenzaldehyde; step three: recycling the residual waste liquid to prepare sodium polysulfide; the preparation method of sodium polysulfide provided by the invention adopts the reaction of sodium sulfide, caustic soda and sulfur to prepare the sodium polysulfide. The sodium polysulfide prepared by the method is added to react to prepare the para aminobenzaldehyde, and the water phase obtained by liquid separation after the reaction is used as waste liquid, wherein the main components are sodium sulfide, sodium polysulfide, sodium thiosulfate, sodium hydroxide, water, sodium hydrosulfide, unreacted sulfur and the like. And carrying out suction filtration on the waste liquid, removing unreacted sulfur, and continuously reacting the filtrate, sodium sulfide, caustic soda and sulfur to prepare sodium polysulfide. The method can realize recycling of the produced residual waste liquid and save resources.
Claims (4)
1. A method for preparing sodium polysulfide is characterized in that: the method comprises the following steps of:
the method comprises the following steps: preparing sodium polysulfide;
a1, weighing certain mass of Na 2S.9H 2O, sublimed sulfur, water and sodium hydroxide, and respectively adding into a reaction kettle;
a2, stirring and heating, heating to 85 ℃, keeping the temperature and stirring for 3 hours after the materials are dissolved;
a3, cooling to room temperature after heat preservation, filtering out unreacted sulfur to obtain filtrate containing sodium polysulfide, and detecting the sodium polysulfide;
step two: refining p-aminobenzaldehyde;
b1, weighing a certain mass of p-nitrotoluene and ethanol, adding into the reaction kettle, starting stirring, heating, condensing, heating to 80 ℃, keeping refluxing, and continuing stirring for 30 min;
b2, uniformly dripping a certain mass of filtrate containing sodium polysulfide in the step one a3 at the temperature of 80 +/-1 ℃ for 1.5-2h, and after finishing dripping, keeping the temperature at 80 +/-1 ℃ for reacting for 3.5-3 h;
b3, after the heat preservation is finished, pouring the mixture into a kettle, standing for 2 hours, separating a lower-layer water phase, namely residual waste liquid, and detecting an upper-layer reducing liquid;
step three: recycling the residual waste liquid to prepare sodium polysulfide;
c1, detecting the residual alkali amount of the residual waste liquid in the step two b 3;
c2, weighing a certain mass of Na 2S.9H 2O, sublimed sulfur, water, sodium hydroxide and residual waste liquid, adding into the kettle, stirring, heating to 85 ℃, dissolving the materials clearly, stirring for 3 hours at a constant temperature, cooling to room temperature after the constant temperature is finished, filtering out unreacted sulfur to obtain filtrate containing sodium polysulfide, and detecting the sodium polysulfide;
c3, adding the prepared sodium polysulfide into the reaction kettle to prepare the para aminobenzaldehyde;
step four: and repeating the second step and the third step.
2. The method of claim 1, wherein the sodium polysulfide is prepared by the following steps: the mass of Na 2S.9H 2O, sublimed sulfur, water and sodium hydroxide in the step one a1 are respectively 17.6-19.5g, 9.1-10.1g, 123-192g and 13.2-15.6 g.
3. The method of claim 1, wherein the sodium polysulfide is prepared by the following steps: the mass of the p-nitrotoluene in the step two b1 is 25g, the volume of the ethanol is 160ml, and the mass of the filtrate containing the sodium polysulfide in the step b2 is 160 g.
4. The method of claim 1, wherein the sodium polysulfide is prepared by the following steps: in the third step c2, the mass of the Na2S & 9H2O, the mass of the sublimed sulfur, the mass of the water, the mass of the sodium hydroxide and the mass of the residual waste liquid are respectively 17.6 to 19.5g, 9.1 to 10.1g, 123. sup. 22 g, 13.2 to 15.6g and 70 to 100 g.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817756A (en) * | 2010-04-20 | 2010-09-01 | 湖北大学 | Method for preparing para-N-hydroxymethyl aminobenzaldehyde |
| CN106977408A (en) * | 2017-04-19 | 2017-07-25 | 杨桂廷 | The preparation method of p-Leuconiline |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101817756A (en) * | 2010-04-20 | 2010-09-01 | 湖北大学 | Method for preparing para-N-hydroxymethyl aminobenzaldehyde |
| CN106977408A (en) * | 2017-04-19 | 2017-07-25 | 杨桂廷 | The preparation method of p-Leuconiline |
Non-Patent Citations (1)
| Title |
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| 对氨基苯甲醛聚合物的合成及性能表征;祖雷 等;《延边大学学报》;20080930;第34卷(第3期);第206-208页 * |
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