CN115490618A - Preparation method of sodium paeonol sulfonate - Google Patents
Preparation method of sodium paeonol sulfonate Download PDFInfo
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- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
- C07C303/04—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups
- C07C303/08—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof by substitution of hydrogen atoms by sulfo or halosulfonyl groups by reaction with halogenosulfonic acids
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- C07C303/44—Separation; Purification
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Abstract
The invention belongs to the technical field of medicines, and particularly relates to a preparation method of sodium paeonol sulfonate. The paeonol reacts with chlorosulfonic acid, is firstly decolorized, then undergoes a salt forming reaction with sodium chloride, and is finally cooled and crystallized to obtain the paeonol sodium sulfonate. The invention puts the decoloring step before the salifying step of the sodium paeonol sulfonate, and the aqueous solution of the paeonol sulfonate is firstly decolored and then reacts with the sodium chloride, thereby avoiding the refining step for a plurality of times, greatly optimizing the reaction step, further improving the product yield and simultaneously meeting the requirement of industry on energy conservation. The invention also reduces the use amount of sodium chloride and organic solvent, reduces the waste liquid treatment amount, reduces the waste liquid treatment cost and further reduces the production environmental protection pressure.
Description
Technical Field
The invention belongs to the technical field of medicines, and particularly relates to a preparation method of sodium paeonol sulfonate.
Background
Sodium paeonol sulfonate is an injection which is a common preparation form and is an analgesic. Can be used for treating joint soreness, cervical vertebra and lumbar vertebra hyperplasia, myalgia, neuralgia, etc. caused by rheumatic arthritis, rheumatoid arthritis, etc., and has high application specificity.
At present, most of continuous industrial production processes for preparing sodium paeonol sulfonate are relatively stable, sulfonation and cold separation drying are adopted, crude sodium paeonol sulfonate is obtained by dissolving the crude sodium paeonol sulfonate in one step and forming salt with sodium chloride aqueous solution, the crude sodium paeonol sulfonate is obtained by cold separation and filtration, then decolorization is carried out, ethanol is added into the crude sodium paeonol sulfonate while the crude sodium paeonol sulfonate is hot, and the refined sodium paeonol sulfonate is obtained.
Chinese patent No. 103342670A discloses a method for purifying sodium paeonol sulfonate, which comprises dissolving crude sodium paeonol sulfonate in water, decolorizing with active carbon, filtering, and adding alcohol solvent to obtain refined product. The compound can relieve calcium abnormal myocardial cell injury and injury caused by renal ischemia reperfusion, reduce plasma malondialdehyde content, and protect superoxide dismutase activity. Most of the patents on sodium paeonol sulfonate are in preparation compounding and refining processes, and no clear process scheme exists for the problems of waste liquid treatment, more product loss, long reaction steps and the like in the reaction. The environmental protection cost is high, and the total yield is low.
At present, the environmental protection situation is increasingly severe, and a preparation method of sodium paeonol sulfonate, which is simple, improves the yield and the utilization rate of raw materials, reduces the generation of three wastes, reasonably utilizes the three wastes, reduces the cost and is beneficial to industrial production, is urgently needed.
Disclosure of Invention
The invention aims to provide a preparation method of sodium paeonol sulfonate, which improves the product yield and the utilization rate of raw materials, reduces the generation of three wastes, reasonably utilizes the three wastes and has simple process operation by placing the decoloring step before the salifying step.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the preparation method of the sodium paeonol sulfonate comprises the following steps: the paeonol reacts with chlorosulfonic acid, is firstly decolorized, then undergoes a salt forming reaction with sodium chloride, and is finally cooled and crystallized to obtain the paeonol sodium sulfonate.
Wherein:
the molar ratio of the paeonol to the chlorosulfonic acid is 1.1-1.2.
The cooling crystallization temperature is-12 to-10 ℃, and the cooling crystallization time is 10 to 12 hours.
The preparation method of the sodium paeonol sulfonate provided by the invention specifically comprises the following steps:
(1) Sulfonation: adding paeonol and chlorosulfonic acid into an organic solvent, carrying out heat preservation reaction, cooling and crystallizing, filtering to obtain a filter cake, and adding the filter cake into water to obtain a paeonol sulfonic acid aqueous solution;
(2) And (3) decoloring: adding activated carbon into the paeonol sulfonic acid aqueous solution obtained in the step (1) for decoloring, and filtering to obtain a decoloring solution;
(3) Salifying: adding a sodium chloride aqueous solution into the decolorized solution obtained in the step (2) to perform a salt forming reaction, and adding an anhydrous methanol solution after the reaction to obtain a crude solution of sodium paeonol sulfonate;
(4) Cooling and crystallizing: and (4) cooling and crystallizing the crude solution of sodium paeonol sulfonate obtained in the step (3) to obtain sodium paeonol sulfonate.
Wherein:
in the step (1), the organic solvent is an ethyl acetate solution, and the dosage ratio of the organic solvent to the paeonol is 10; the reaction temperature is kept at 65-70 ℃, and the reaction time is kept at 1-1.5 hours; the cooling crystallization temperature is-12 to-10 ℃, and the cooling crystallization time is 4 to 5 hours.
In the step (1), the filter cake is leached by ethyl acetate solution, and then added with water to obtain paeonol sulfonic acid water solution; the dosage ratio of the filter cake to the water is 1.
In the step (1), the filtrate obtained after filtration contains a large amount of chloride ions and sulfate ions and unreacted raw materials, a small amount of water is added into the filtrate for washing, the chloride ions and the sulfate ions are separated from the organic phase and enter the water phase, and the unreacted raw materials stay in the organic phase. The organic phase and the water phase are separated, and the organic phase can be recycled as the solvent of the one-step reaction.
In the step (2), the dosage ratio of the activated carbon to the paeonol sulfonic acid aqueous solution is 10-12, wherein the activated carbon is counted by g, and the paeonol sulfonic acid aqueous solution is counted by L.
In the step (2), the decoloring temperature is 50-55 ℃, and the decoloring time is 2.5-3.0 h.
In the step (3), the salt forming reaction temperature is 50-60 ℃; the mass ratio of sodium chloride to water in the sodium chloride aqueous solution is 20-22; the mass ratio of the sodium chloride aqueous solution to water in the decoloration solution is 1; the using ratio of the anhydrous methanol solution to the sodium chloride aqueous solution is 1-1.1, wherein the sodium chloride aqueous solution is calculated by g, and the anhydrous methanol solution is calculated by ml.
And (3) adding an anhydrous methanol solution, wherein water is a good solvent of the product, and the salting-out is promoted by adding an inert solvent methanol. The methanol and the water can be mixed and dissolved in any proportion, and the solubility of the methanol is high, so that the saturated sodium paeonol sulfonate solution can be dehydrated, and the precipitation of the product is accelerated; if the anhydrous methanol solution is not added, the solution needs to be concentrated, and the steps are complex.
In the step (4), the crude solution of sodium paeonol sulfonate obtained in the step (3) is cooled and crystallized for 10 to 12 hours at the temperature of between 12 ℃ below zero and 10 ℃ below zero for the first time, the solution is filtered to obtain a filter cake A and a filtrate A, the filtrate A is cooled and crystallized for 10 to 12 hours at the temperature of between 12 ℃ below zero and 10 ℃ below zero for the second time, the filtrate A is filtered to obtain a filter cake B and a filtrate B, and the filter cake A and the filter cake B are dried at the temperature of between 35 and 40 ℃ to obtain sodium paeonol sulfonate; and analyzing and supplementing the content of the anhydrous methanol and the sodium chloride in the filtrate B, and directly applying the filtrate B to a decoloring solution for recycling after the content of the anhydrous methanol and the content of the sodium chloride are qualified.
The invention has the following beneficial effects:
(1) In the prior art, sodium paeonol sulfonate is subjected to decoloration treatment after salifying, and the treatment method needs to be refined for many times to obtain a refined product of the sodium paeonol sulfonate. And the quality loss is 10-20% during refining, the total yield is reduced a lot, and the preparation process is not simple. After reacting paeonol and chlorosulfonic acid, cooling, crystallizing and filtering to separate generated paeonol sulfonic acid from unreacted raw materials, and dissolving a filter cake in water to obtain a paeonol sulfonic acid aqueous solution which can be directly decolorized; the decolored paeonol sulfonic acid water solution reacts with sodium chloride to generate a crude product of sodium paeonol sulfonate, and the crude product is cooled and crystallized to obtain a qualified product without refining for many times. The invention places the decoloring step before the salifying step of the sodium paeonol sulfonate, and the aqueous solution of the paeonol sulfonate is firstly decolored and then reacts with the sodium chloride, thereby avoiding multiple refining steps, greatly optimizing the reaction steps, further improving the product yield and simultaneously meeting the industrial requirement on energy conservation.
(2) The paeonol reacts with chlorosulfonic acid to generate paeonol sulfonic acid, and the generated paeonol sulfonic acid reacts with sodium chloride to generate sodium paeonol sulfonate, so that three wastes in the two-step reaction can be reasonably utilized:
(1) in the process of generating paeonol sulfonic acid by reacting paeonol with chlorosulfonic acid, experimental demonstration shows that the comprehensive yield of one-step reaction is about 90%. The filtrate obtained after filtration contains a large amount of chloride ions, sulfate ions and unreacted raw materials, and the waste liquid treatment consumes energy and has low utilization rate of the raw materials. After the one-step reaction is finished, a small amount of water is added into the filtrate for washing, chloride ions and sulfate ions are separated from the organic phase and enter the water phase, and unreacted raw materials stay in the organic phase. The organic phase and the water phase are separated, and the organic phase can be directly applied to the one-step reaction, so that the one-step reaction raw material is applied. The invention can reuse the waste liquid which needs to be treated originally, improves the utilization rate of raw materials, and reduces the cost of raw materials and the cost for treating three wastes. The reaction process is as follows:
(2) in the process of generating sodium paeonol sulfonate by reacting paeonol sulfonic acid with sodium chloride, the crude solution of sodium paeonol sulfonate is cooled and crystallized for the first time and then filtered to obtain a filter cake A and a filtrate A, a part of product and sodium chloride are remained in the filtrate A, and the filtrate A is cooled, crystallized and filtered again to obtain a filter cake B and a filtrate B. According to the invention, after secondary cold separation, the contents of the anhydrous methanol and the sodium chloride in the filtrate B are analyzed and supplemented until the contents of the anhydrous methanol and the sodium chloride are qualified, and then the anhydrous methanol and the sodium chloride are directly applied to a decolorized solution, so that the raw material cost and the three-waste treatment cost are reduced.
(3) The invention increases the yield of the paeonol sodium sulfonate by more than 5 percent through secondary cold separation, the total yield is more than or equal to 69 percent, and the purity is more than or equal to 99.9 percent. The invention increases the utilization rate of raw materials, changes the synthetic route to improve the total yield and avoids multiple refinements. The using amount of sodium chloride and organic solvent is reduced, the waste liquid treatment capacity is reduced, the waste liquid treatment cost is reduced, and the production environmental protection pressure is further reduced. The invention has simple process operation, considerable profit and higher industrial value.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
(1) Sulfonation: 100g of paeonol is added into 1L of ethyl acetate solution, 77.13g of chlorosulfonic acid is slowly added dropwise, and the molar ratio of the paeonol to the chlorosulfonic acid is 1. Reacting at 70 ℃ for 1 hour, cooling at-10 ℃ for crystallization for 4 hours, filtering to obtain 133.35g of filter cake, leaching the filter cake with ethyl acetate solution, and adding 666.75ml of water to obtain paeonolsulfonic acid aqueous solution; filtering to obtain filtrate, mixing the filtrate with leacheate, adding a small amount of water into the leacheate for washing, separating an organic phase from a water phase, and sleeving the organic phase for one-step reaction for recycling.
(2) And (3) decoloring: adding activated carbon into the paeonol sulfonic acid aqueous solution obtained in the step (1), decoloring at 55 ℃ for 2.5h, filtering, and after decoloring, press-filtering the activated carbon to obtain a decolored solution for standby when the solution is hot; wherein the dosage ratio of the activated carbon to the aqueous solution of paeonol sulfonic acid is 10.
(3) Salifying: under the condition of stirring at 50 ℃, 666.75g of sodium chloride aqueous solution is added into the decolored solution obtained in the step (2) to generate salt forming reaction, after the liquid phase monitoring reaction is completed, the dropwise addition of the sodium chloride aqueous solution is stopped, and then 668ml of anhydrous methanol solution is added to obtain crude solution of sodium paeonol sulfonate; wherein the mass ratio of sodium chloride to water in the sodium chloride aqueous solution is 20.
(4) Cooling and crystallizing: and (4) cooling and crystallizing the crude solution of sodium paeonol sulfonate obtained in the step (3) for 12 hours at-10 ℃, filtering to obtain a filter cake A and a filtrate A, cooling and crystallizing the filtrate A for 12 hours at-10 ℃ for the second time, and filtering to obtain a filter cake B and a filtrate B. Mixing the filter cake A and the filter cake B, and drying at 35 ℃ to obtain 123.48g of sodium paeonol sulfonate product, wherein the total yield is 76.49%, and the purity is 99.98%; and (4) analyzing and supplementing the filtrate B until the content of the anhydrous methanol and the content of the sodium chloride are qualified, and directly applying the filtrate B to a decoloring solution for recycling.
Example 2
(1) Sulfonation: 100g of paeonol is added into 1L of ethyl acetate solution, 84.14g of chlorosulfonic acid is slowly dripped, and the molar ratio of the paeonol to the chlorosulfonic acid is 1. Reacting at 65 ℃ for 1.5 hours, cooling at-12 ℃ for 5 hours for crystallization, filtering to obtain 121.54g of filter cake, leaching the filter cake with ethyl acetate solution, and adding 607.7ml of water to obtain paeonolsulfonic acid aqueous solution; filtering to obtain filtrate, mixing the filtrate with the leacheate, adding a small amount of water into the leacheate for washing, separating an organic phase from a water phase, and sleeving the organic phase for one-step reaction for recycling.
(2) And (3) decoloring: adding activated carbon into the paeonol sulfonic acid aqueous solution obtained in the step (1), decoloring for 3.0h at 50 ℃, filtering, and after decoloring, press-filtering the activated carbon to obtain a decolored solution for standby when the solution is hot; wherein the dosage ratio of the activated carbon to the aqueous solution of paeonol sulfonic acid is 12.
(3) Salifying: adding 607.7g of sodium chloride aqueous solution into the decolored solution obtained in the step (2) under the stirring condition of 55 ℃ to perform salt forming reaction, stopping dropwise adding the sodium chloride aqueous solution after the liquid phase monitoring reaction is completed, and then adding 668.5ml of anhydrous methanol solution to obtain a crude solution of sodium paeonol sulfonate; wherein the mass ratio of sodium chloride to water in the sodium chloride aqueous solution is 22.
(4) Cooling and crystallizing: and (4) cooling and crystallizing the crude solution of sodium paeonol sulfonate obtained in the step (3) for 10 hours at-12 ℃, filtering to obtain a filter cake A and a filtrate A, cooling and crystallizing the filtrate A for 10 hours at-12 ℃ for the second time, and filtering to obtain a filter cake B and a filtrate B. Mixing the filter cake A and the filter cake B, and drying at 40 ℃ to obtain 112.70g of sodium paeonol sulfonate product, wherein the total yield is 69.80 percent, and the purity is 99.97 percent; and (4) analyzing and supplementing the filtrate B until the content of the anhydrous methanol and the content of the sodium chloride are qualified, and directly applying the filtrate B to a decolorized solution for recycling.
Example 3
(1) Sulfonation: 100g of paeonol is added into 1L of ethyl acetate solution, 77.13g of chlorosulfonic acid is slowly added dropwise, and the molar ratio of the paeonol to the chlorosulfonic acid is 1. Reacting at 68 ℃ for 1.2 hours while keeping the temperature, cooling at-11 ℃ for crystallization for 4.5 hours, filtering to obtain 125.87g of filter cake, leaching the filter cake by using ethyl acetate solution, and then adding 629.35ml of water to obtain paeonolsulfonic acid aqueous solution; filtering to obtain filtrate, mixing the filtrate with the leacheate, adding a small amount of water into the leacheate for washing, separating an organic phase from a water phase, and sleeving the organic phase for one-step reaction for recycling.
(2) And (3) decoloring: adding activated carbon into the paeonol sulfonic acid aqueous solution obtained in the step (1), decoloring for 2.8h at 53 ℃, filtering, and performing pressure filtration on the activated carbon after decoloring to obtain a decolored solution for standby when the solution is hot; wherein the dosage ratio of the activated carbon to the paeonol sulfonic acid aqueous solution is 10.
(3) Salifying: adding 629.35g of sodium chloride aqueous solution into the decolorized solution obtained in the step (2) under the stirring condition of 60 ℃ to perform salt forming reaction, stopping dropwise adding the sodium chloride aqueous solution after the liquid phase monitoring reaction is completed, and then adding 667ml of anhydrous methanol solution to obtain a crude solution of sodium paeonol sulfonate; wherein the mass ratio of sodium chloride to water in the sodium chloride aqueous solution is 21.
(4) Cooling and crystallizing: and (4) cooling and crystallizing the crude solution of sodium paeonol sulfonate obtained in the step (3) for 11 hours at-11 ℃, filtering to obtain a filter cake A and a filtrate A, cooling and crystallizing the filtrate A for 11 hours at-11 ℃ for the second time, and filtering to obtain a filter cake B and a filtrate B. Mixing the filter cake A and the filter cake B, and drying at 38 ℃ to obtain 115.73g of sodium paeonol sulfonate product, wherein the total yield is 71.69 percent, and the purity is 99.98 percent; and (4) analyzing and supplementing the filtrate B until the content of the anhydrous methanol and the content of the sodium chloride are qualified, and directly applying the filtrate B to a decolorized solution for recycling.
Comparative example 1
The preparation process of the sodium paeonol sulfonate product comprises the following steps: directly salifying after sulfonation, and then decoloring, cooling and crystallizing, wherein the specific contents are as follows:
(1) Sulfonation: 100g of paeonol is added into 1L of ethyl acetate solution, 77.13g of chlorosulfonic acid is slowly dripped, and the molar ratio of the paeonol to the chlorosulfonic acid is 1. Reacting at 70 ℃ for 1 hour, cooling at-10 ℃ for crystallization for 4 hours, filtering to obtain 133.35g of filter cake, leaching the filter cake with ethyl acetate solution, and adding 666.75ml of water to obtain paeonolsulfonic acid aqueous solution; filtering to obtain filtrate, mixing the filtrate with leacheate, adding a small amount of water into the leacheate for washing, separating an organic phase from a water phase, and sleeving the organic phase for one-step reaction for recycling.
(2) Salifying: under the condition of stirring at 50 ℃, 666.75g of sodium chloride aqueous solution is added into the paeonol sulfonic acid aqueous solution obtained in the step (1) to generate salt forming reaction, the sodium chloride aqueous solution is stopped to be dripped after the liquid phase monitoring reaction is completed, and then 668ml of anhydrous methanol solution is added to obtain crude paeonol sodium sulfonate solution; wherein the mass ratio of sodium chloride to water in the sodium chloride aqueous solution is 20. Cooling and crystallizing to obtain 123.48g of crude product after drying.
(3) And (3) decoloring: adding activated carbon into the solution (123.48 g of crude sodium paeonol sulfonate, 617.4g of water) of the crude sodium paeonol sulfonate obtained in the step (2), decoloring at 55 ℃ for 2.5h, filtering, and performing pressure filtration on the activated carbon after decoloring to obtain a decolored solution for standby when the solution is hot; wherein the dosage ratio of the active carbon to the crude solution of sodium paeonol sulfonate is 10, the active carbon is counted by g, and the crude solution of sodium paeonol sulfonate is counted by L.
(4) Cooling and crystallizing: and (4) cooling and crystallizing the decolorized solution obtained in the step (3) for 12 hours at minus 10 ℃, filtering to obtain a filter cake A and a filtrate A, cooling and crystallizing the filtrate A for 12 hours at minus 10 ℃ for the second time, and filtering to obtain a filter cake B and a filtrate B. And combining the filter cake A and the filter cake B, and drying at 35 ℃ to obtain 101.253g of sodium paeonol sulfonate product with the total yield of 50.54% and the purity of 80.56%.
Compared with the embodiment 1, the comparative example 1 adopts a method of re-decoloring after salifying, so that color deposition is easily caused, and the obtained product has yellow color and poor stability and needs secondary decoloring; if the effect of the two-time decolorization is not obvious, the phenomenon of color deposition still exists, and the product quality loss after each decolorization is 15-20%, so that the product yield is influenced; or cooling and crystallizing to obtain a dry product, and then decoloring, but the steps are more complicated. In the embodiment 1, the decolorization before salification is adopted, so that the phenomenon of color deposition is avoided, the secondary decolorization process is omitted, and the yield of the product is high.
Comparative example 2
In the step (4), the crude solution of sodium paeonol sulfonate obtained in the step (3) is cooled and crystallized for 12 hours at minus 10 ℃, a filter cake A is dried directly at 35 ℃ after filtration, and secondary cooling and crystallization are not carried out, so that 116.21g of sodium paeonol sulfonate product is obtained, the total yield is 70.71%, and the purity is 98.21%; the rest of the procedure was the same as in example 1.
Claims (10)
1. A preparation method of sodium paeonol sulfonate is characterized by comprising the following steps: the paeonol reacts with chlorosulfonic acid, is firstly decolorized, then undergoes a salt forming reaction with sodium chloride, and finally is cooled and crystallized to obtain the paeonol sodium sulfonate.
2. The method for preparing sodium paeonol sulfonate according to claim 1, which is characterized in that: the molar ratio of the paeonol to the chlorosulfonic acid is 1.1-1.2.
3. The method for preparing sodium paeonol sulfonate according to claim 1, which is characterized in that: the cooling crystallization temperature is-12 to-10 ℃, and the cooling crystallization time is 10 to 12 hours.
4. The method for preparing sodium paeonol sulfonate according to any one of claims 1 to 3, which is characterized by comprising the following steps:
(1) Sulfonation: adding paeonol and chlorosulfonic acid into an organic solvent, carrying out heat preservation reaction, cooling and crystallizing, filtering to obtain a filter cake, and adding the filter cake into water to obtain a paeonol sulfonic acid aqueous solution;
(2) And (3) decoloring: adding activated carbon into the paeonol sulfonic acid aqueous solution obtained in the step (1) for decoloring, and filtering to obtain a decoloring solution;
(3) Salifying: adding a sodium chloride aqueous solution into the decolorized solution obtained in the step (2) to perform a salt forming reaction, and adding an anhydrous methanol solution after the reaction to obtain a crude solution of sodium paeonol sulfonate;
(4) Cooling and crystallizing: and (4) cooling and crystallizing the crude solution of sodium paeonol sulfonate obtained in the step (3) to obtain sodium paeonol sulfonate.
5. The method for preparing sodium paeonol sulfonate according to claim 4, wherein the method comprises the following steps: in the step (1), the organic solvent is ethyl acetate solution; the reaction temperature is kept at 65-70 ℃, and the reaction time is kept at 1-1.5 hours; the cooling crystallization temperature is-12 to-10 ℃, and the cooling crystallization time is 4 to 5 hours.
6. The method for preparing sodium paeonol sulfonate according to claim 4, wherein the method comprises the following steps: in the step (1), the filter cake is leached by ethyl acetate solution, and then added with water to obtain paeonol sulfonic acid water solution; the dosage ratio of the filter cake to the water is 1.
7. The method for preparing sodium paeonol sulfonate according to claim 4, wherein the method comprises the following steps: in the step (2), the dosage ratio of the activated carbon to the paeonol sulfonic acid aqueous solution is 10-12, wherein the activated carbon is counted by g, and the paeonol sulfonic acid aqueous solution is counted by L.
8. The method for preparing sodium paeonol sulfonate according to claim 4, wherein the method comprises the following steps: in the step (2), the decoloring temperature is 50-55 ℃, and the decoloring time is 2.5-3.0 h.
9. The method for preparing sodium paeonol sulfonate according to claim 4, wherein the method comprises the following steps: in the step (3), the salt forming reaction temperature is 50-60 ℃; the mass ratio of sodium chloride to water in the sodium chloride aqueous solution is 20-22; the mass ratio of the sodium chloride aqueous solution to water in the decoloring solution is 1; the using ratio of the anhydrous methanol solution to the sodium chloride aqueous solution is 1-1.1, wherein the sodium chloride aqueous solution is calculated by g, and the anhydrous methanol solution is calculated by ml.
10. The method for preparing sodium paeonol sulfonate according to claim 4, wherein the method comprises the following steps: in the step (4), the crude solution of sodium paeonol sulfonate obtained in the step (3) is cooled and crystallized for 10 to 12 hours at the temperature of between-12 and-10 ℃, and is filtered to obtain a filter cake A and a filtrate A, the filtrate A is cooled and crystallized for 10 to 12 hours at the temperature of between-12 and-10 ℃, and is filtered to obtain a filter cake B and a filtrate B, and the filter cake A and the filter cake B are dried at the temperature of between 35 and 40 ℃ to obtain the sodium paeonol sulfonate; and recycling the filtrate B.
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