CN110304639B - Purification method of sodium o-sulfonate benzaldehyde byproduct salt - Google Patents
Purification method of sodium o-sulfonate benzaldehyde byproduct salt Download PDFInfo
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- CN110304639B CN110304639B CN201910621109.XA CN201910621109A CN110304639B CN 110304639 B CN110304639 B CN 110304639B CN 201910621109 A CN201910621109 A CN 201910621109A CN 110304639 B CN110304639 B CN 110304639B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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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
- C01D5/14—Preparation of sulfites
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Abstract
A method for purifying sodium o-sulfonate benzaldehyde byproduct salt comprises the following steps: washing a byproduct salt generated in the production process of sodium o-sulfonate benzaldehyde; fully dissolving the washed byproduct salt into hot water to prepare a saturated solution, and filtering while the solution is hot; putting the filtered saturated solution into a four-mouth bottle, dropwise adding hydrochloric acid into the four-mouth bottle, and adjusting the pH value of the saturated solution to 1-2; then adjusting the pH value of the saturated solution to be neutral by using a sodium hydroxide solution, and starting distillation and concentration; and when the sodium chloride is concentrated to be separated out, carrying out hot filtration, continuously concentrating the filtrate until the sodium chloride is not separated out any more, thereby completing the purification of the sodium o-sulfonate benzaldehyde byproduct salt. The method has the advantages of simplifying the process of treating the byproduct salt, reducing the treatment cost of the byproduct salt, fully utilizing the sulfur dioxide generated by desulfurization to generate the sodium sulfite, synthesizing the o-sodium sulfonate benzaldehyde and reducing the cost of raw materials.
Description
Technical Field
The invention belongs to the technical field of fine chemical engineering, and particularly relates to a method for purifying sodium o-sulfonate benzaldehyde byproduct salt.
Background
O-sodium sulfobenzaldehyde (O-benzaldehydesodium salt), also known as benzaldehyde-2-sodium sulfonate, has a molecular formula of C7H5NaO4S and a molecular weight of 208.2.
The o-sodium sulfonate benzaldehyde is a main intermediate for synthesizing a fluorescent whitening agent CBS, a triphenylmethane dye and a mothproofing agent N. The fluorescent brightener CBS is a novel fluorescent brightener. The product has excellent chlorine bleaching resistance, acid and alkali resistance and sun-proof performance, is an ideal additive for light industry, textile and daily chemical industry, is especially used for various washing powders, washing creams, soaps, fancy soaps and liquid detergents, can improve the service performance of the product, and improves the internal quality and the appearance quality of the product. Is especially suitable for low-temperature washing whitening, and is the fluorescent whitening agent variety with the best effect in the detergent industry in the world at present. The fluorescent brightener CBS is one of fluorescent brighteners widely applied to laundry detergent at present.
Industrially, the o-chlorobenzaldehyde sodium sulfonate is usually obtained by sulfonating o-chlorobenzaldehyde with sodium sulfite in water under the catalysis of potassium iodide; after the synthesis is finished, concentrating the material by distillation, simultaneously recovering a small amount of incompletely reacted o-chlorobenzaldehyde, and then filtering to remove salt; then cooling and crystallizing. The salt produced in the process contains sodium chloride, sodium sulfite, water and a small amount of organic matters, and is 500-600 kg/ton of product. The salt cannot be used directly and needs to be disposed of as waste, which greatly increases the cost.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a method for separating sodium chloride and sodium sulfite from the byproduct salt of sodium o-sulfonate benzaldehyde to purify the byproduct salt and reduce the treatment cost of the byproduct salt.
The technical problem to be solved by the invention is realized by the following technical scheme, and the invention discloses a method for purifying sodium o-sulfonate benzaldehyde byproduct salt, which is characterized by comprising the following steps:
(1) washing a byproduct salt generated in the production process of sodium o-sulfonate benzaldehyde to remove organic matter residues;
(2) fully dissolving the washed byproduct salt into hot water to prepare a saturated solution, and filtering while the solution is hot;
(3) putting the filtered saturated solution into a four-mouth bottle, dropwise adding hydrochloric acid into the four-mouth bottle, adjusting the pH value of the saturated solution to 1-2, generating bubbles in the hydrochloric acid adding process, and stopping adding the hydrochloric acid when no bubbles are generated;
(4) then adjusting the pH value of the saturated solution to be neutral by using a sodium hydroxide solution, and then starting distillation and concentration;
(5) and when the sodium chloride is concentrated to be separated out, carrying out hot filtration, continuously concentrating the filtrate until the sodium chloride is not separated out any more, thereby completing the purification of the sodium o-sulfonate benzaldehyde byproduct salt.
The technical problem to be solved by the invention can be solved by adopting the following technical scheme that the hot water in the step (2) is pure water with the temperature of 50-70 ℃, and preferably 60-65 ℃.
The technical problem to be solved by the present invention can also be achieved by the following technical scheme, wherein the hydrochloric acid in the step (3) is a hydrochloric acid solution with a mass fraction of 10% to 37%, and more preferably a 37% hydrochloric acid solution.
The technical problem to be solved by the present invention can also be solved by the following technical scheme, wherein the sodium hydroxide solution in the step (4) is a sodium hydroxide solution with a mass fraction of 10% to 32%, and more preferably a sodium hydroxide solution with a mass fraction of 10% to 15%.
The technical problem to be solved by the invention can be realized by the following technical scheme, and the neutrality in the step (4) is pH = 6.5-7.5.
The technical problem to be solved by the invention can be realized by the following technical scheme that in the step (5), when the precipitation amount of the sodium chloride is that the precipitation volume of the sodium chloride accounts for 25-45% of the volume of the concentrated solution, hot filtration is carried out.
The technical problem to be solved by the invention can also be realized by the following technical scheme, and the water distilled in the step (5) can be used for washing and dissolving the byproduct salt.
The technical problem to be solved by the invention can be realized by the following technical scheme that sulfur dioxide is generated in the PH adjusting process in the step (3), the sulfur dioxide is extracted by vacuum, and the sulfur dioxide is absorbed by a sodium hydroxide solution; paying attention to the pH value condition of the sodium hydroxide solution in the step (3), detecting the content of sodium sulfite in the sodium hydroxide solution absorbing sulfur dioxide when the pH value is reduced to be below 9.0, and supplementing sodium sulfite solid for synthesizing sodium o-sulfonate benzaldehyde.
Compared with the prior art, the essence of the method is to prepare sodium chloride and sodium sulfite by using the byproduct salt of the production of o-sulfobenzaldehyde, thereby achieving the purpose of purifying the o-sulfobenzaldehyde byproduct salt. The method can greatly reduce the output of the byproduct salt, reduce the production cost of the o-sodium sulfonate benzaldehyde, and can separate sodium chloride and sodium sulfite in the byproduct salt to be used as the byproduct or be repeatedly used, thereby realizing the resource utilization of the byproduct salt.
Detailed Description
The specific embodiments of the present invention are further described to facilitate the further understanding of the present invention by those skilled in the art, and do not constitute limitations on the rights thereto.
Embodiment 1, a method for purifying sodium o-sulfonate benzaldehyde byproduct salt, comprising the following steps:
(1) washing a byproduct salt generated in the production process of sodium o-sulfonate benzaldehyde to remove organic matter residues;
(2) fully dissolving the washed byproduct salt into pure water at the temperature of 50 ℃ to prepare a saturated solution, and filtering the solution while the solution is hot;
(3) putting the filtered saturated solution into a four-mouth bottle, dropwise adding a hydrochloric acid solution with the mass fraction of 10% into the four-mouth bottle, adjusting the pH value of the saturated solution to 1, wherein bubbles are generated in the hydrochloric acid adding process, and stopping adding the hydrochloric acid when no bubbles are generated;
(4) then, regulating the pH value of the saturated solution to 6.5 by using a sodium hydroxide solution with the mass fraction of 10%, and then, starting distillation and concentration;
(5) and when the sodium chloride is concentrated until the precipitation amount of the sodium chloride is 25% of the precipitation volume of the concentrated solution, performing hot filtration, continuously concentrating the filtrate until the sodium chloride is not precipitated any more, thereby completing the purification of the sodium o-sulfonate benzaldehyde byproduct salt, and washing and dissolving the byproduct salt by using distilled water.
Embodiment 2, a method for purifying sodium o-sulfonate benzaldehyde byproduct salt, comprising the following steps:
(1) washing a byproduct salt generated in the production process of sodium o-sulfonate benzaldehyde to remove organic matter residues;
(2) fully dissolving the washed byproduct salt into pure water at the temperature of 70 ℃ to prepare a saturated solution, and filtering the solution while the solution is hot;
(3) putting the filtered saturated solution into a four-mouth bottle, dropwise adding a hydrochloric acid solution with the mass fraction of 25% into the four-mouth bottle, adjusting the pH value of the saturated solution to 2, wherein bubbles are generated in the hydrochloric acid adding process, and stopping adding the hydrochloric acid when no bubbles are generated;
(4) then, regulating the pH value of the saturated solution to 7.5 by using a sodium hydroxide solution with the mass fraction of 32%, and then, starting distillation and concentration;
(5) and when the sodium chloride is concentrated until the precipitation amount of the sodium chloride is that the precipitation volume of the sodium chloride accounts for 45% of the volume of the concentrated solution, carrying out hot filtration, continuously concentrating the filtrate until the sodium chloride is not precipitated any more, thereby completing the purification of the sodium o-sulfonate benzaldehyde byproduct salt, and the distilled water can be used for washing and dissolving the byproduct salt.
Embodiment 3, a method for purifying sodium o-sulfonate benzaldehyde byproduct salt, comprising the following steps:
(1) washing a byproduct salt generated in the production process of sodium o-sulfonate benzaldehyde to remove organic matter residues;
(2) fully dissolving the washed byproduct salt into pure water at the temperature of 60 ℃ to prepare a saturated solution, and filtering the solution while the solution is hot;
(3) putting the filtered saturated solution into a four-mouth bottle, dropwise adding a hydrochloric acid solution with the mass fraction of 37% into the four-mouth bottle, adjusting the pH value of the saturated solution to 1.5, wherein bubbles are generated in the adding process of the hydrochloric acid, and stopping adding the hydrochloric acid when no bubbles are generated;
(4) then, regulating the pH value of the saturated solution to 7.0 by using a sodium hydroxide solution with the mass fraction of 30%, and then, starting distillation and concentration;
(5) and when the sodium chloride is concentrated until the precipitation amount of the sodium chloride is that the precipitation volume of the sodium chloride accounts for 35 percent of the volume of the concentrated solution, carrying out hot filtration, continuously concentrating the filtrate until the sodium chloride is not precipitated any more, thereby completing the purification of the sodium o-sulfonate benzaldehyde byproduct salt, and the distilled water can be used for washing and dissolving the byproduct salt.
Embodiment 4, the purification method of sodium o-sulfonate benzaldehyde byproduct salt described in embodiments 1 to 3, wherein sulfur dioxide is generated in the PH adjustment process described in step (3), the sulfur dioxide is extracted by vacuum, and the sulfur dioxide is absorbed by sodium hydroxide solution; paying attention to the pH value condition of the sodium hydroxide solution in the step (3), detecting the content of sodium sulfite in the sodium hydroxide solution absorbing sulfur dioxide when the pH value is reduced to be below 9.0, and supplementing sodium sulfite solid for synthesizing sodium o-sulfonate benzaldehyde.
Example 5, a method for purifying sodium o-sulfonate benzaldehyde byproduct salt, comprising the following steps,
(1) firstly, adding clean water into 2000 g of byproduct salt until the byproduct salt can be stirred, then carrying out suction filtration, washing the byproduct salt again in a spraying manner, dissolving the washed salt in hot water to prepare a saturated solution, and filtering the saturated solution again to remove mechanical impurities;
(2) adding 1000 ml of hydrochloric acid saturated solution into a four-mouth bottle, wherein the four-mouth bottle is provided with a hydrochloric acid dripping device, a pH meter, a condensing device and a tail gas absorption device, and a 10% sodium hydroxide solution is used as an absorption liquid in the tail gas absorption device; putting the four-mouth bottle into a constant-temperature water bath kettle, and maintaining the temperature at 80-85 ℃;
(3) starting stirring, and dropwise adding a 30% hydrochloric acid solution, wherein bubbles are emitted at the moment, and the bubbles are mainly sulfur dioxide; introducing sulfur dioxide into a tail gas absorption device for absorption by utilizing vacuum, wherein bubbles continuously emerge along with the addition of a hydrochloric acid solution, and the pH value continuously decreases until the pH value is 1-2;
(4) at the moment, the water bath kettle is removed, and the water bath kettle is replaced by an electric heating jacket for heating until the water bath kettle reflows and is maintained; in the process, a hydrochloric acid solution is required to be supplemented to maintain the pH value of the system; when no bubbles or very few bubbles exist in the tail gas absorption device, temporarily stopping heating, removing the tail gas absorption device, and changing a condensing device into a distillation device; adjusting the pH value to 6.5-7.5 by using 10% sodium hydroxide solution;
(5) heating again, distilling, and collecting distilled water for washing and dissolving by-product salt; when the mixture is concentrated until the precipitation amount of the solid accounts for 35 percent of the total volume, stopping heating, and filtering while the mixture is hot; washing the filter cake with clear water, and merging the washing water into the filtrate; continuously concentrating the filtrate;
collecting and drying the filter cake to obtain white crystals, wherein the content of sodium chloride is 98.8 percent, and other indexes all meet the secondary indexes of GB/T5462-2016 refined industrial salt;
(6) in the step (4), the change of a 10% sodium hydroxide solution in the tail gas absorption device needs to be closely paid attention, and when the pH value in the absorption bottle is reduced to 9.0-9.5, the absorption liquid is replaced in time; the changed absorption liquid is weighed, and the content of sodium sulfite is detected;
the content of sodium sulfite in the absorption solution is 15.2 percent, the weight is 107.3 grams, and the content is equivalent to 16.3 grams of sodium sulfite by detection.
The byproduct salt is a byproduct in the synthesis of sodium o-sulfonate benzaldehyde, and mainly comprises sodium chloride, sodium sulfite, water and a small amount of organic matters. The part of byproduct salt is washed, dissolved and filtered to remove organic matters and insoluble mechanical impurities to obtain brine, sodium sulfite in the brine is subjected to acid adjustment and heating and can be decomposed to produce sulfur dioxide, the sulfur dioxide is absorbed by a sodium hydroxide solution to obtain a sodium sulfite solution, and the sodium sulfite solution is recycled to the production of sodium o-sulfonate benzaldehyde; the acid salt water is neutralized by sodium hydroxide solution to obtain sodium chloride solution, and sodium chloride products meeting the national standard can be obtained by further treatment. Not only can reduce the treatment cost of the sodium o-sulfonate benzaldehyde byproduct salt, but also can separate sodium chloride and sodium sulfite in the byproduct salt for independent use, thereby reducing the discharge of waste. The method can greatly reduce the output of the byproduct salt, reduce the production cost of the o-sodium sulfonate benzaldehyde, and can separate sodium chloride and sodium sulfite in the byproduct salt to be used as the byproduct or be repeatedly used, thereby realizing the resource utilization of the byproduct salt.
The method for purifying the o-sulfonate benzaldehyde byproduct salt is characterized in that the byproduct salt generated in the production process of the o-sulfonate benzaldehyde is subjected to washing, desulfurization, crystallization, absorption and other treatment to obtain a sodium chloride byproduct meeting the national standard, and meanwhile, the recovered sodium sulfite can be used for producing the o-sulfonate benzaldehyde. The method has the advantages of simplifying the process of treating the byproduct salt, reducing the treatment cost of the byproduct salt, fully utilizing the sulfur dioxide generated by desulfurization to generate the sodium sulfite, synthesizing the o-sodium sulfonate benzaldehyde and reducing the cost of raw materials.
Claims (8)
1. A method for purifying sodium o-sulfonate benzaldehyde byproduct salt is characterized by comprising the following steps: the method comprises the following steps:
(1) washing a byproduct salt generated in the production process of sodium o-sulfonate benzaldehyde to remove organic matter residues;
(2) fully dissolving the washed byproduct salt into hot water to prepare a saturated solution, and filtering while the solution is hot;
(3) putting the filtered saturated solution into a four-mouth bottle, dropwise adding hydrochloric acid into the four-mouth bottle, adjusting the pH value of the saturated solution to 1-2, generating bubbles in the hydrochloric acid adding process, and stopping adding the hydrochloric acid when no bubbles are generated;
(4) then adjusting the pH value of the saturated solution to be neutral by using a sodium hydroxide solution, and then starting distillation and concentration;
(5) and when the sodium chloride is concentrated to be separated out, carrying out hot filtration, continuously concentrating the filtrate until the sodium chloride is not separated out any more, thereby completing the purification of the sodium o-sulfonate benzaldehyde byproduct salt.
2. The method for purifying sodium o-sulfonate benzaldehyde byproduct salt according to claim 1, wherein the method comprises the following steps: the hot water in the step (2) is pure water with the temperature of 50-70 ℃.
3. The method for purifying sodium o-sulfonate benzaldehyde byproduct salt according to claim 1, wherein the method comprises the following steps: the hydrochloric acid in the step (3) is a hydrochloric acid solution with the mass fraction of 10-37%.
4. The method for purifying sodium o-sulfonate benzaldehyde byproduct salt according to claim 1, wherein the method comprises the following steps: the sodium hydroxide solution in the step (4) is 10-32% by mass.
5. The method for purifying sodium o-sulfonate benzaldehyde byproduct salt according to claim 1, wherein the method comprises the following steps: the neutrality in the step (4) is pH = 6.5-7.5.
6. The method for purifying sodium o-sulfonate benzaldehyde byproduct salt according to claim 1, wherein the method comprises the following steps: in the step (5), when the precipitation amount of the sodium chloride is that the precipitation volume of the sodium chloride accounts for 25-45% of the volume of the concentrated solution, carrying out hot filtration.
7. The method for purifying sodium o-sulfonate benzaldehyde byproduct salt according to claim 1, wherein the method comprises the following steps: and (5) using the distilled water in the step (5) for washing and dissolving the byproduct salt.
8. The method for purifying sodium o-sulfonate benzaldehyde byproduct salt according to claim 1, wherein the method comprises the following steps: sulfur dioxide is generated in the pH adjusting process in the step (3), the sulfur dioxide is pumped out in vacuum, and the sulfur dioxide is absorbed by using a sodium hydroxide solution; paying attention to the pH value condition of the sodium hydroxide solution in the step (3), detecting the content of sodium sulfite in the sodium hydroxide solution absorbing sulfur dioxide when the pH value is reduced to be below 9.0, and supplementing sodium sulfite solid for synthesizing sodium o-sulfonate benzaldehyde.
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