CN113493400B - Method for producing bisphenol S and co-producing sodium lignin sulfonate - Google Patents
Method for producing bisphenol S and co-producing sodium lignin sulfonate Download PDFInfo
- Publication number
- CN113493400B CN113493400B CN202010260129.1A CN202010260129A CN113493400B CN 113493400 B CN113493400 B CN 113493400B CN 202010260129 A CN202010260129 A CN 202010260129A CN 113493400 B CN113493400 B CN 113493400B
- Authority
- CN
- China
- Prior art keywords
- bisphenol
- lignin sulfonate
- sodium lignin
- water
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C315/00—Preparation of sulfones; Preparation of sulfoxides
- C07C315/06—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08H—DERIVATIVES OF NATURAL MACROMOLECULAR COMPOUNDS
- C08H6/00—Macromolecular compounds derived from lignin, e.g. tannins, humic acids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for producing bisphenol S and co-producing sodium lignin sulfonate, which comprises three steps of synthesizing crude bisphenol S, refining bisphenol S and synthesizing dispersing agent sodium lignin sulfonate. The invention applies the high COD wastewater generated in the bisphenol S production and refining process to the production of sodium lignin sulfonate, and the green co-production method solves the environmental protection problem caused by the high concentration wastewater produced by bisphenol S, saves the environmental protection cost, simultaneously applies all phenolic substances in the wastewater to the raw materials of sodium lignin sulfonate, replaces part of the raw materials of sodium lignin sulfonate, reduces the cost of sodium lignin sulfonate, and is more green and environment-friendly.
Description
Technical Field
The invention relates to the technical field of organic synthesis, relates to a green production method, and in particular relates to a method for producing bisphenol S and co-producing sodium lignin sulfonate.
Technical Field
Bisphenol S is a widely applied material intermediate, and the bisphenol S is produced by using a little excessive phenol and concentrated sulfuric acid to carry out sulfonation condensation reaction under the action of mesitylene solvent, and recrystallizing by using ethanol solution as solvent; during the production process, a large amount of high-concentration wastewater is generated, wherein the high-concentration wastewater contains phenol, bisphenol S, a small amount of mesitylene, ethanol and impurities thereof, the COD is as high as 10-15 ten thousand ppm, and the phenol is sometimes as high as 30000-50000ppm; therefore, the high-concentration wastewater can not be treated in the sewage treatment process, the treatment difficulty is high, the treatment cost is high, and particularly the high-concentration phenol-containing wastewater can not be completely decomposed and discharged up to the standard in the later sewage process, so that the high-concentration wastewater is subjected to treatment methods in the industry for treating the high-COD wastewater, but the treatment methods are complicated in process and poor in treatment effect.
Disclosure of Invention
Aiming at the problem of difficult treatment of wastewater in the background technology, the invention provides a method for producing bisphenol S and co-producing dispersing agent sodium lignin sulfonate, which is environment-friendly.
The technical scheme of the invention is as follows: a method for producing bisphenol S and co-producing sodium lignin sulfonate comprises three steps of synthesizing crude bisphenol S, refining bisphenol S and synthesizing dispersant sodium lignin sulfonate:
(1) Synthesis of crude bisphenol S:
(1) adding phenol and mesitylene into a reaction container, starting stirring, then starting to dropwise add concentrated sulfuric acid, controlling the dropwise adding temperature to be 90-120 ℃ and dropwise adding time to be 3 hours, and after dropwise adding, controlling the temperature to be 120 ℃ and preserving heat for 1-1.5 hours;
(2) after the heat preservation is finished, the temperature is quickly increased to reflux and carry water for 5 to 6.5 hours at the temperature of 150 to 170 ℃, the temperature is maintained at 190 to 200 ℃ after the water carrying is finished, and the solvent is distilled and recovered to obtain solid crystals for 1.5 to 2.5 hours;
(3) after distillation, adding alcohol and liquid alkali into the solid crystal in the step (2) in the first reaction, heating to 100 ℃, stirring for dissolution, testing and adjusting the PH=7.5-9; continuously heating up and distilling to recover alcohol, adding water, continuously distilling until the temperature reaches 98-102 ℃, stopping distilling after alcohol distillation is completed, and cooling; cooling to 45 ℃, filtering, and washing the filtered solid with water to obtain crude bisphenol S, wherein the filtrate and the washing liquid are used for producing sodium lignin sulfonate;
(2) Refining bisphenol S:
adding alcohol and water into the alcohol recovered in the step (1), adding the crude product obtained by washing in the step (1) into an alcohol solution, starting stirring and heating to 90 ℃ until the crude product is dissolved, adding activated carbon for decolorization, performing hot filtration, cooling the filtrate to 40 ℃, filtering again, wherein the filtered liquid is refined mother liquor, the refined mother liquor is used for the synthesis and application of the next batch of crude product, and drying a filter cake to obtain refined bisphenol S;
(3) Synthesis of sodium lignin sulfonate:
adding a proper amount of water into the filtrate in the bisphenol S refining process, adding lignin for pulping, adding sodium sulfite and industrial formaldehyde, adding liquid alkali for regulating the pH value to 11-13, heating to 70-85 ℃ for reacting for 1 hour, heating to 95-110 ℃ for reacting for 5-7 hours, and cooling the reaction system to 50-60 ℃ to obtain the dispersing agent sodium lignin sulfonate slurry.
Further, the synthesis of the crude bisphenol S can be continuously circulated, and the refining mother liquor in the bisphenol S refining process is sleeved back to the crude bisphenol S synthesis crude dissolution process for recycling, and the specific steps are as follows:
(1) adding phenol and mesitylene into a reaction container, starting stirring, then starting to dropwise add concentrated sulfuric acid, controlling the dropwise adding temperature to be 90-120 ℃ and dropwise adding time to be 3 hours, and after dropwise adding, controlling the temperature to be 120 ℃ and preserving heat for 1-1.5 hours;
(2) after the heat preservation is finished, the temperature is quickly increased to reflux and carry water for 5 to 6.5 hours at the temperature of 150 to 170 ℃, the temperature is maintained at 190 to 200 ℃ after the water carrying is finished, and the solvent is distilled and recovered to obtain solid crystals for 1.5 to 2.5 hours;
(3) after distillation, adding refined mother liquor and liquid alkali obtained in the previous refining reaction process into the solid crystal in the step (2), heating to 100 ℃, stirring for dissolution, testing and adjusting the PH=7.5-9; continuously heating up and distilling to recover alcohol, adding water, continuously distilling until the temperature reaches 98-102 ℃, stopping distilling after alcohol distillation is completed, and cooling; cooling to 45 ℃, filtering, and washing to obtain a crude product.
Further, in the step (1) of synthesizing the crude bisphenol S, the mass ratio of the main raw materials is as follows: phenol: mesitylene: concentrated sulfuric acid= (3-5): (2-4): (1-3).
Further, in the steps (3) and (4) of synthesizing the crude bisphenol S, the mass ratio of the main raw materials is as follows: refining mother liquor: liquid alkali: water= (40-50): 1: (25-35).
Further, in the refining step of bisphenol S, the main raw materials are in mass ratio: adding alcohol: water: activated carbon= (20-40): (150-200): 1.
further, in the synthetic step of the dispersing agent sodium lignin sulfonate, the formaldehyde content in the industrial formaldehyde is 37%.
Further, in the synthetic step of the dispersing agent sodium lignin sulfonate, the obtained dispersing agent slurry is dried by a spray drying tower to obtain a powdery dispersing agent.
Further, in the synthetic step of the dispersant sodium lignin sulfonate, the main raw materials are in mass ratio: lignin: bisphenol S waste liquid: sodium sulfite: liquid alkali: formaldehyde: water = 1: (1.5-2.5): (0.4-0.5): (0.2-0.25): (0.08-0.10): (1-2).
Compared with the prior art, the invention has the beneficial effects that: the invention applies the high COD waste water generated in the bisphenol S production and refining process to the production of sodium lignin sulfonate, because the main components in the bisphenol S waste water liquid are phenol, isomers of bisphenol S and other hydroxyl-containing phenolic substances, the chemical structure is very similar to that of the sodium lignin sulfonate raw material, and the sodium lignin sulfonate mainly utilizes the phenolic substances, the environmental protection problem caused by the high COD waste water produced in the bisphenol S production is thoroughly solved by applying the bisphenol S waste water to the production of sodium lignin sulfonate, the method is green and environment-friendly, and waste is changed into valuable; the method solves the environmental protection problem of bisphenol S production, saves the environmental protection cost, simultaneously applies phenolic substances in the wastewater to the raw materials of sodium lignin sulfonate completely, replaces partial raw materials of sodium lignin sulfonate, reduces the cost of sodium lignin sulfonate, and is a green circular economy solution.
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples.
Example 1
A. Primary reaction
(1) Synthesis of crude bisphenol S:
(1) adding phenol and mesitylene into a reaction container, starting stirring, then starting to dropwise add concentrated sulfuric acid, controlling the dropwise adding temperature to be 90-120 ℃ and dropwise adding time to be 3 hours, and after dropwise adding, controlling the temperature to be 120 ℃ and preserving heat for 1-1.5 hours;
(2) after the heat preservation is finished, the temperature is quickly increased to reflux and carry water for 5 to 6.5 hours at the temperature of 150 to 170 ℃, the temperature is maintained at 190 to 200 ℃ after the water carrying is finished, and the solvent is distilled and recovered to obtain solid crystals for 1.5 to 2.5 hours;
(3) after distillation, adding alcohol and liquid alkali into the solid crystal in the step (2) in the first reaction, heating to 100 ℃, stirring for dissolution, testing and adjusting the PH=7.5-9; continuously heating up and distilling to recover alcohol, adding water, continuously distilling until the temperature reaches 98-102 ℃, stopping distilling after alcohol distillation is completed, and cooling; cooling to 45 ℃, filtering, and washing the filtered solid with water to obtain crude bisphenol S, wherein the filtrate and the washing liquid are used for producing sodium lignin sulfonate;
(2) Refining bisphenol S:
adding alcohol and water into the alcohol recovered in the step (1), adding the crude product obtained by washing in the step (1) into an alcohol solution, starting stirring and heating to 90 ℃ until the crude product is dissolved, adding activated carbon for decolorization, performing hot filtration, cooling the filtrate to 40 ℃, filtering again, wherein the filtered liquid is refined mother liquor, the refined mother liquor is used for the synthesis and application of the next batch of crude product, and drying a filter cake to obtain refined bisphenol S;
(3) Synthesis of sodium lignin sulfonate:
adding a proper amount of water into the filtrate in the bisphenol S refining process, adding lignin for pulping, adding sodium sulfite and industrial formaldehyde, adding liquid alkali for regulating the pH value to 11-13, heating to 70-85 ℃ for reacting for 1 hour, heating to 95-110 ℃ for reacting for 5-7 hours, cooling the reaction system to 50-60 ℃ to obtain dispersant sodium lignin sulfonate slurry or drying in a spray drying tower to obtain powdery dispersant.
B. Cyclic reaction
The synthesis of the crude bisphenol S can be continuously circulated, and the refining mother liquor in the bisphenol S refining process is sleeved back to the crude bisphenol S synthesis crude dissolution procedure for recycling, and the specific steps are as follows:
(1) adding phenol and mesitylene into a reaction container, starting stirring, then starting to dropwise add concentrated sulfuric acid, controlling the dropwise adding temperature to be 90-120 ℃ and dropwise adding time to be 3 hours, and after dropwise adding, controlling the temperature to be 120 ℃ and preserving heat for 1-1.5 hours;
(2) after the heat preservation is finished, the temperature is quickly increased to reflux and carry water for 5 to 6.5 hours at the temperature of 150 to 170 ℃, the temperature is maintained at 190 to 200 ℃ after the water carrying is finished, and the solvent is distilled and recovered to obtain solid crystals for 1.5 to 2.5 hours;
(3) after distillation, adding refined mother liquor and liquid alkali obtained in the previous refining reaction process into the solid crystal in the step (2), heating to 100 ℃, stirring for dissolution, testing and adjusting the PH=7.5-9; continuously heating up and distilling to recover alcohol, adding water, continuously distilling until the temperature reaches 98-102 ℃, stopping distilling after alcohol distillation is completed, and cooling; cooling to 45 ℃, filtering, and washing to obtain a crude product.
Example 2
(1) Synthesis of crude bisphenol S:
(1) adding 3 parts of phenol and 2 parts of mesitylene into a reaction container, starting stirring, then starting to dropwise add 2 parts of concentrated sulfuric acid, controlling the dropwise adding temperature to be 90-120 ℃ for 3 hours, and after dropwise adding, controlling the temperature to be 120 ℃ and preserving heat for 1.5 hours;
(2) after the heat preservation is finished, the temperature is quickly increased to reflux and carry water (the carried water is separated by a water separating device and does not return to a reaction system), the temperature is 150-170 ℃ for 5-6.5 hours, the carried water is finished, the temperature is maintained at 190-200 ℃, the distillation is started to recover the solvent and obtain solid crystals, and the time is 1.5-2.5 hours;
(3) after distillation, adding 40 parts of alcohol and 1 part of liquid alkali into the solid crystal in the step (2) in the first reaction, heating to 100 ℃, stirring for dissolution, testing and adjusting the PH=7.5-9; continuously heating up and distilling to recover alcohol, adding 25 parts of water, continuously distilling until the temperature reaches 98-102 ℃, stopping distilling after the alcohol is distilled, and cooling; cooling to 45 ℃, filtering, and washing the filtered solid with water to obtain crude bisphenol S;
(2) Refining bisphenol S:
adding 20 parts of alcohol and 200 parts of water into the alcohol recovered in the step (1), adding the crude product obtained by washing in the step (1) into the alcohol solution, starting stirring and heating to 90 ℃ until the crude product is dissolved, adding 1 part of activated carbon for decolorization, performing hot filtration, cooling the filtrate to 40 ℃, filtering again, taking the filtered liquid as refined mother liquor, and drying the filter cake to obtain refined bisphenol S.
(3) Synthesis of sodium lignin sulfonate:
1.5 parts of filtered liquid in the bisphenol S refining process is added with 1 part of water, 1 part of lignin is added for pulping, 0.4 part of sodium sulfite and 0.08 part of industrial formaldehyde with 37% of formaldehyde content are added, 0.2 part of liquid alkali is added for adjusting the PH value to 11-13, the mixture is heated to 70-85 ℃ for reaction for 1 hour, then the mixture is heated to 95-110 ℃ for reaction for 5-7 hours, and the reaction system is cooled to 50-60 ℃ to obtain the dispersing agent sodium lignin sulfonate slurry.
Example 3
(1) Synthesis of crude bisphenol S
80 g of phenol and 60 g of mesitylene in a 500 ml flask are stirred; adding 40 g of concentrated sulfuric acid dropwise, controlling the temperature of the dropwise at 90-120 ℃ and the dropwise adding time to be 3 hours; after the completion of the dropwise addition, the mixture was incubated at 120℃for 1 hour.
After the heat preservation is finished, the temperature is quickly raised to reflux with water (the water is separated by a water separator and does not return to the reaction system), the highest temperature is up to 170 ℃ for about 6 hours, the temperature is maintained at 190-200 ℃ after the water is finished, the solvent is recovered, and the distillation time is about 2 hours.
After distillation, adding about 200g of refined mother liquor and 8g of liquid alkali, heating to 100 ℃, stirring for dissolution, testing and adjusting the PH=7.5-9; then continuously heating up and distilling to recover alcohol, adding 180 g of water, continuously distilling until the temperature reaches 98-102 ℃, stopping distilling after the ethanol is distilled, and cooling; cooling to 45 ℃, filtering and washing with water to obtain a crude product.
(2) Refining of bisphenol S
Adding 30 g of alcohol into the alcohol recovered in the previous step, wherein the total amount of water is 180 g; adding the crude product in the previous step, stirring, heating to 90 ℃, dissolving, decoloring by 1 g of activated carbon, performing hot filtration, cooling the filtrate to 40 ℃, filtering, sleeving the mother solution into the crude product dissolving process, and drying the filter cake to obtain the finished product.
(3) Synthesis of sodium lignin sulfonate
Adding 150g of water into 200g of bisphenol S filtered waste liquid, adding 100g of lignin, pulping, adding 45g of sodium sulfite and 9g of industrial formaldehyde with 37% content, adding 20g of liquid alkali, adjusting the pH value between 11 and 13, heating to 70-85 ℃ for reaction for 1 hour, heating to 95-110 ℃ for reaction for 5-7 hours, cooling the reaction system to 50-60 ℃ to obtain dispersant slurry or drying in a spray drying tower to obtain powdery dispersant.
Example 4
(1) Synthesis of crude bisphenol S
80 g of phenol and 40 g of mesitylene in a 500 ml flask are stirred; then heating to 110 ℃, beginning to drop 41 g of 98% concentrated sulfuric acid, controlling the drop temperature to be 110 ℃ and the drop time to be 3 hours; after the completion of the dropwise addition, the mixture was incubated at 120℃for 1 hour.
After the heat preservation is finished, the temperature is quickly raised to reflux with water (the water is separated by a water separator and does not return to the reaction system), the highest temperature is up to 170 ℃ for about 6 hours, the temperature is maintained at 190-200 ℃ after the water is finished, the solvent is recovered, and the distillation time is about 2 hours.
Adding a batch of refined alcohol mother liquor of about 240 g, regulating pH to 8.5, heating to 100deg.C, stirring for dissolving, distilling off ethanol water solution, continuously distilling, dropwise adding 160 g of water until the temperature reaches 99deg.C, co-distilling 160-170 g of ethanol water solution, basically finishing alcohol distillation, stopping distillation, and cooling; cooling to 30 ℃, filtering, washing with water to obtain crude product, and about 200g of filtrate is used for producing sodium lignin sulfonate.
(2) Refining of bisphenol S
Adding 60 g of alcohol into the alcohol recovered in the previous step, wherein the total amount of water is 200 g; adding the crude product in the previous step, stirring, heating to 90 ℃ for dissolution, decoloring by 1 g of activated carbon, performing hot filtration, cooling the filtrate to 40 ℃, measuring the pH, adjusting the pH to be 4.0, filtering, sleeving the mother solution into the crude product dissolution process, drying the filter cake to obtain a finished product, and drying to obtain 89 g of white uniform powder.
(3) Synthesis of sodium lignin sulfonate
Adding 150g of water into 200g of bisphenol S filtered waste liquid, adding 100g of lignin, pulping, adding 45g of sodium sulfite and 9g of industrial formaldehyde with 37% of content, adding 20g of liquid alkali, adjusting the pH value between 11 and 13, heating to 70-85 ℃ for reaction for 1 hour, heating to 95-110 ℃ for reaction for 5-7 hours, cooling the reaction system to 50-60 ℃ to obtain dispersant slurry or drying in a spray drying tower to obtain powdery dispersant, and drying to obtain 148g of tan powder.
Performance tests were performed on the product obtained in example 4, and the experimental test results are shown in the following table:
the foregoing has shown and described the basic principles, main features and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A method for producing bisphenol S and co-producing sodium lignin sulfonate, which is characterized in that: the method comprises three steps of synthesis of crude bisphenol S, refining of bisphenol S and synthesis of dispersant sodium lignin sulfonate:
(1) Synthesis of crude bisphenol S:
(1) adding phenol and mesitylene into a reaction container, starting stirring, then starting to dropwise add concentrated sulfuric acid, controlling the dropwise adding temperature to be 90-120 ℃ and dropwise adding time to be 3 hours, and after dropwise adding, controlling the temperature to be 120 ℃ and preserving heat for 1-1.5 hours;
(2) after the heat preservation is finished, the temperature is quickly increased to reflux and carry water for 5 to 6.5 hours at the temperature of 150 to 170 ℃, the temperature is maintained at 190 to 200 ℃ after the water carrying is finished, and the solvent is distilled and recovered to obtain solid crystals for 1.5 to 2.5 hours;
(3) after distillation, adding alcohol and liquid alkali into the solid crystal in the step (2) in the first reaction, heating to 100 ℃, stirring for dissolution, testing and adjusting the PH=7.5-9; continuously heating up and distilling to recover alcohol, adding water, continuously distilling until the temperature reaches 98-102 ℃, stopping distilling after alcohol distillation is completed, and cooling; cooling to 45 ℃, filtering, and washing the filtered solid with water to obtain crude bisphenol S, wherein the filtrate and the washing liquid are used for producing sodium lignin sulfonate;
(2) Refining bisphenol S:
adding alcohol and water into the alcohol recovered in the step (1), adding the crude product obtained by washing in the step (1) into an alcohol solution, starting stirring and heating to 90 ℃ until the crude product is dissolved, adding activated carbon for decolorization, performing hot filtration, cooling the filtrate to 40 ℃, filtering again, wherein the filtered liquid is refined mother liquor, the refined mother liquor is used for the synthesis and application of the next batch of crude product, and drying a filter cake to obtain refined bisphenol S;
(3) Synthesis of sodium lignin sulfonate:
adding a proper amount of water into the filtrate and the washing liquid in the step (1), adding lignin for pulping, adding sodium sulfite and industrial formaldehyde, adding liquid alkali for regulating the pH value to 11-13, heating to 70-85 ℃ for reacting for 1 hour, heating to 95-110 ℃ for reacting for 5-7 hours, and cooling the reaction system to 50-60 ℃ to obtain the dispersing agent sodium lignin sulfonate slurry.
2. A method for producing bisphenol S and co-producing sodium lignin sulfonate according to claim 1, wherein: the synthesis of the crude bisphenol S can be continuously circulated, and the refining mother liquor in the bisphenol S refining process is sleeved back to the crude bisphenol S synthesis crude dissolution procedure for recycling, and the specific steps are as follows:
(1) adding phenol and mesitylene into a reaction container, starting stirring, then starting to dropwise add concentrated sulfuric acid, controlling the dropwise adding temperature to be 90-120 ℃ and dropwise adding time to be 3 hours, and after dropwise adding, controlling the temperature to be 120 ℃ and preserving heat for 1-1.5 hours;
(2) after the heat preservation is finished, the temperature is quickly increased to reflux and carry water for 5 to 6.5 hours at the temperature of 150 to 170 ℃, the temperature is maintained at 190 to 200 ℃ after the water carrying is finished, and the solvent is distilled and recovered to obtain solid crystals for 1.5 to 2.5 hours;
(3) after distillation, adding refined mother liquor and liquid alkali obtained in the previous refining reaction process into the solid crystal in the step (2), heating to 100 ℃, stirring for dissolution, testing and adjusting the PH=7.5-9; continuously heating up and distilling to recover alcohol, adding water, continuously distilling until the temperature reaches 98-102 ℃, stopping distilling after alcohol distillation is completed, and cooling; cooling to 45 ℃, filtering, and washing to obtain a crude product.
3. A process for the production of bisphenol S and co-production of sodium lignin sulfonate according to any one of claims 1 or 2 characterized in that: in the synthesis step (1) of the crude bisphenol S, the main raw materials are in mass ratio: phenol: mesitylene: concentrated sulfuric acid= (3-5): (2-4): (1-3).
4. A method for producing bisphenol S and co-producing sodium lignin sulfonate according to claim 2, wherein: in the synthesis step (3) of the crude bisphenol S, the main raw materials are in mass ratio: refining mother liquor: liquid alkali: water= (40-50): 1: (25-35).
5. A process for the production of bisphenol S and co-production of sodium lignin sulfonate according to any one of claims 1 or 2 characterized in that: in the refining step of bisphenol S, the main raw materials are in mass ratio: adding alcohol: water: activated carbon= (20-40): (150-200): 1.
6. a process for the production of bisphenol S and co-production of sodium lignin sulfonate according to any one of claims 1 or 2 characterized in that: in the synthetic step of the dispersing agent sodium lignin sulfonate, the formaldehyde content in industrial formaldehyde is 37%.
7. A process for the production of bisphenol S and co-production of sodium lignin sulfonate according to any one of claims 1 or 2 characterized in that: in the synthesis step of the dispersant sodium lignin sulfonate, the obtained dispersant slurry is dried by a spray drying tower to obtain a powdery dispersant.
8. A process for the production of bisphenol S and co-production of sodium lignin sulfonate according to any one of claims 1 or 2 characterized in that: in the synthesis step of the dispersing agent sodium lignin sulfonate, the main raw materials are in mass ratio: lignin: bisphenol S waste liquid: sodium sulfite: liquid alkali: formaldehyde: water = 1: (1.5-2.5):
(0.4-0.5)：(0.2-0.25)：(0.08-0.10)：(1-2)。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010260129.1A CN113493400B (en) | 2020-04-03 | 2020-04-03 | Method for producing bisphenol S and co-producing sodium lignin sulfonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010260129.1A CN113493400B (en) | 2020-04-03 | 2020-04-03 | Method for producing bisphenol S and co-producing sodium lignin sulfonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113493400A CN113493400A (en) | 2021-10-12 |
| CN113493400B true CN113493400B (en) | 2023-07-07 |
Family
ID=77995151
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010260129.1A Active CN113493400B (en) | 2020-04-03 | 2020-04-03 | Method for producing bisphenol S and co-producing sodium lignin sulfonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113493400B (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6197484A (en) * | 1984-10-05 | 1986-05-15 | ウエストバコ・コーポレーシヨン | Sodium lignin sulfonate and its preparation |
| CN101214930A (en) * | 2007-12-26 | 2008-07-09 | 浙江闰土股份有限公司 | Method for producing sodium hydrosulfite and co-producing sodium lignosulfonate by using residual liquid of sodium hydrosulfite |
| CN105254544A (en) * | 2015-11-13 | 2016-01-20 | 如皋市金陵化工有限公司 | Preparing method for bisphenol S |
| CN108102741A (en) * | 2017-12-19 | 2018-06-01 | 萧县沃德化工科技有限公司 | A kind of additive of alkali lignin of waste water modification containing beta naphthal and its preparation and application |
-
2020
- 2020-04-03 CN CN202010260129.1A patent/CN113493400B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6197484A (en) * | 1984-10-05 | 1986-05-15 | ウエストバコ・コーポレーシヨン | Sodium lignin sulfonate and its preparation |
| CN101214930A (en) * | 2007-12-26 | 2008-07-09 | 浙江闰土股份有限公司 | Method for producing sodium hydrosulfite and co-producing sodium lignosulfonate by using residual liquid of sodium hydrosulfite |
| CN105254544A (en) * | 2015-11-13 | 2016-01-20 | 如皋市金陵化工有限公司 | Preparing method for bisphenol S |
| CN108102741A (en) * | 2017-12-19 | 2018-06-01 | 萧县沃德化工科技有限公司 | A kind of additive of alkali lignin of waste water modification containing beta naphthal and its preparation and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113493400A (en) | 2021-10-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108101850B (en) | Method for improving quality of 5-acetoacetylaminobenzimidazolone | |
| CN107337618B (en) | Production method for simultaneously improving purity and yield of metformin hydrochloride | |
| CN110194729B (en) | Preparation method of m-nitro-beta-hydroxyethyl sulfone | |
| CN110668471B (en) | Purification production method of environment-friendly potassium persulfate | |
| CN113493400B (en) | Method for producing bisphenol S and co-producing sodium lignin sulfonate | |
| CN104130105A (en) | Method for recycling ethanol during production of p-methyl sulfonyl phenyl ethyl serinate | |
| CN109970543B (en) | Method for recycling acyclovir condensation by-product and solvent | |
| CN109608354B (en) | Method for refining aniline dye intermediate | |
| CN105461565B (en) | A kind of method for producing nitro-acetophenone | |
| CN107915343B (en) | Process wastewater treatment process in production process of pyrazolone series products | |
| CN108675919A (en) | A kind of method that double trimethylolpropane is extracted in trimethylolpropane heavy constituent | |
| CN112341316A (en) | Method for preparing 2, 2' -dihydroxybiphenyl by using dibenzofuran fraction as raw material | |
| CN111253272B (en) | Method for preparing benzamide compound | |
| CN113956147A (en) | Decolorizing process of 2-ethyl anthraquinone crude product | |
| CN112939764A (en) | Production process of 2-hydroxy-3-naphthoic acid | |
| CN115536548B (en) | Environment-friendly synthesis method of intermediate | |
| CN111186848A (en) | Process and device for refining byproduct ammonium sulfate in isophthalonitrile production | |
| RU2440168C1 (en) | Method of processing commercial pentaerythritol-formiate mother solution | |
| CN111662199A (en) | Refining method for recovering beta-aminopropionic acid | |
| CN110372474A (en) | The process of waste liquor mysoinositol content can be reduced in a kind of production of inositol | |
| CN116621885B (en) | Recycling treatment method of 2-amino-4-acetamido anisole production wastewater | |
| CN114369073B (en) | Method for preparing high-purity hydrochlorothiazide | |
| US1314924A (en) | Chester e | |
| CN115108951B (en) | P-nitrophenyl-beta-hydroxyethyl thioether and preparation method thereof | |
| CN117776982A (en) | Preparation method of ultra-high purity bisphenol S |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |