CN110304639A - A kind of method of purification of ortho-sulfonic acid sodium benzaldehyde by-product salt - Google Patents
A kind of method of purification of ortho-sulfonic acid sodium benzaldehyde by-product salt Download PDFInfo
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- CN110304639A CN110304639A CN201910621109.XA CN201910621109A CN110304639A CN 110304639 A CN110304639 A CN 110304639A CN 201910621109 A CN201910621109 A CN 201910621109A CN 110304639 A CN110304639 A CN 110304639A
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- ortho
- product salt
- sulfonic acid
- sodium
- benzaldehyde
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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
Abstract
A kind of method of purification of ortho-sulfonic acid sodium benzaldehyde by-product salt, this method comprises the following steps: the by-product salt generated in ortho-sulfonic acid sodium benzaldehyde production process is washed；By-product salt after washing is sufficiently dissolved into hot water, saturated solution is made, and is filtered while hot；Filtered saturated solution is put into four-hole bottle, hydrochloric acid is added dropwise into four-hole bottle, the pH value of saturated solution is adjusted to 1~2；The pH value of saturated solution is adjusted to neutrality with sodium hydroxide solution again, starts distillation and concentration；When being concentrated to sodium chloride precipitation, hot filter is carried out, filtrate is continued to be concentrated, until being concentrated into no longer precipitated sodium chloride, to complete the purification of ortho-sulfonic acid sodium benzaldehyde by-product salt.The present invention has and can simplify the technique of by-product salt treatment, and the sulfur dioxide for reducing by-product salt treatment expense, and desulfurization capable of being made full use of to generate generates sodium sulfite, the advantages of for synthesizing ortho-sulfonic acid sodium benzaldehyde, reducing cost of material.
Description
Technical field
The invention belongs to technical field of fine, in particular to a kind of purification side of ortho-sulfonic acid sodium benzaldehyde by-product salt
Method.
Background technique
Ortho-sulfonic acid sodium benzaldehyde (O-benzaldehyde sulfonic acid sodium salt) also known as benzaldehyde-
2- sodium sulfonate, molecular formula C7H5NaO4S, molecular weight 208.2.
Ortho-sulfonic acid sodium benzaldehyde is the main intermediate for synthesizing fluorescent brightener CBS, kiton colors and Eulan N.
Fluorescent brightener CBS is a kind of New Fluorescent Whitening Agent.With excellent chlorine-resistant drift, acid and alkali-resistance, sun-resistant performance, be light industry,
The perfect additive of weaving and daily use chemicals industry, in particular for various washing powder, washing cream, soap, perfumed soap and liquid detergent,
The service performance of product can be improved, improve product inherent quality and presentation quality.It is brightened especially suitable for cold washing, is current
In the world for the optimal fluorescent whitening agent kind of effect in detergent industry.Fluorescent brightener CBS is widely used in washing at present
One of clothing liquid fluorescent whitening agent.
Industrially, ortho-sulfonic acid sodium benzaldehyde is usually under potassium iodide catalytic action, and Yu Shuizhong is sub- by o-chlorobenzaldehyde
Sodium sulphate carries out sulfonation and obtains；Material is concentrated by distilling after synthesis, while recycling the adjacent chlorine not reacted completely on a small quantity
Benzaldehyde is then filtered to remove salt；Then crystallisation by cooling is carried out.The salt generated during this contains sodium chloride, sodium sulfite, water
It is 500~600 kgs/tonne of products with a small amount of organic matter.This salt cannot be used directly, need to be used as Waste disposal, greatly be increased
Cost.
Summary of the invention
The technical problem to be solved by the present invention is in view of the deficiencies of the prior art, provide a kind of utilization ortho-sulfonic acid sodium benzene first
Aldehyde by-product salt isolates sodium chloride and sodium sulfite achievees the purpose that by-product salt purifies, and reduces the side of by-product salt treatment expense
Method.
The technical problem to be solved by the present invention is to what is realized by technical solution below, the present invention is a kind of adjacent sulphur
The method of purification of sour sodium benzaldehyde by-product salt, its main feature is that, this method comprises the following steps:
(1) the by-product salt generated in ortho-sulfonic acid sodium benzaldehyde production process is washed, removes organic substance residues；
(2) the by-product salt after washing is sufficiently dissolved into hot water and saturated solution is made, and be filtered while hot；
(3) filtered saturated solution is put into four-hole bottle, hydrochloric acid is added dropwise into four-hole bottle, by the pH value tune of saturated solution
Section has bubble generation to 1~2 in hydrochloric acid adition process, when bubble-free generates, stop that hydrochloric acid is added；
(4) pH value of saturated solution is adjusted to neutrality with sodium hydroxide solution again, then starts distillation and concentration；
(5) when being concentrated to sodium chloride precipitation, hot filter is carried out, filtrate is continued to be concentrated, until being concentrated into no longer precipitated sodium chloride,
To complete the purification of ortho-sulfonic acid sodium benzaldehyde by-product salt.
What the technical problems to be solved by the invention can also be realized by technical solution below, institute in step (2)
The hot water stated is pure water of the temperature between 50~70 DEG C, further preferably 60~65 DEG C of pure water.
What the technical problems to be solved by the invention can also be realized by technical solution below, institute in step (3)
The hydrochloric acid stated is that mass fraction is 10%~37% hydrochloric acid solution, further preferably 37% hydrochloric acid solution.
What the technical problems to be solved by the invention can also be realized by technical solution below, institute in step (4)
The sodium hydroxide solution stated is the sodium hydroxide solution that mass fraction is 10%~32%, further preferably 10%~15% hydrogen-oxygen
Change sodium solution.
What the technical problems to be solved by the invention can also be realized by technical solution below, institute in step (4)
The neutrality stated is pH=6.5~7.5.
What the technical problems to be solved by the invention can also be realized by technical solution below, in step (5),
When the amount of precipitation of the sodium chloride is that sodium chloride settling volume accounts for the volume of the concentrated liquid 25%~45%, hot filter is carried out.
What the technical problems to be solved by the invention can also be realized by technical solution below, step (5) distillation
Water out can be used for the washing and dissolution of by-product salt.
What the technical problems to be solved by the invention can also be realized by technical solution below, step (3) is described
PH adjustment process in can generate sulfur dioxide, sulfur dioxide is extracted out using vacuum, using sodium hydroxide solution to titanium dioxide
Sulphur is absorbed；It pays close attention in step (3), the pH value situation of sodium hydroxide solution, when pH is down to 9.0 or less, detection, which absorbs, to be had
The content of the sodium hydroxide solution sulfite sodium of sulfur dioxide, adds sodium sulfite solid, for synthesizing ortho-sulfonic acid sodium benzene first
Aldehyde.
Compared with prior art, the essence of the method for the invention is exactly the by-product salt system using production ortho-sulfonic acid benzaldehyde
Standby sodium chloride and sodium sulfite, to achieve the purpose that ortho-sulfonic acid sodium benzaldehyde by-product salt purifies.This method can significantly subtract
The output of few by-product salt reduces ortho-sulfonic acid sodium benzaldehyde production cost, and can be by the sodium chloride and sodium sulfite point in by-product salt
It leaves and, as byproduct or reuse, realize by-product salt resource utilization.
Specific embodiment
The specific technical solution of the present invention is further described, in order to which those skilled in the art is further understood that this hair
It is bright, without constituting the limitation to its right.
Embodiment 1, a kind of method of purification of ortho-sulfonic acid sodium benzaldehyde by-product salt, this method comprises the following steps:
(1) the by-product salt generated in ortho-sulfonic acid sodium benzaldehyde production process is washed, removes organic substance residues；
(2) the by-product salt after washing is sufficiently dissolved into temperature and saturated solution is made in the pure water between 50 DEG C, and while hot into
Row filtering；
(3) filtered saturated solution is put into four-hole bottle, it is 10% hydrochloric acid solution that mass fraction is added dropwise into four-hole bottle,
The pH value of saturated solution is adjusted to 1, bubble generation is had in hydrochloric acid adition process, when bubble-free generates, stops that salt is added
Acid；
(4) pH value of saturated solution is adjusted to 6.5 with the sodium hydroxide solution that mass fraction is 10% again, then starts to distill
Concentration；
(5) when the amount of precipitation for being concentrated to sodium chloride is that sodium chloride settling volume accounts for the volume of the concentrated liquid 25%, hot filter is carried out, will be filtered
Liquid continues to be concentrated, and until being concentrated into no longer precipitated sodium chloride, to complete the purification of ortho-sulfonic acid sodium benzaldehyde by-product salt, distills out
Water can be used for the washing and dissolution of by-product salt.
Embodiment 2, a kind of method of purification of ortho-sulfonic acid sodium benzaldehyde by-product salt, this method comprises the following steps:
(1) the by-product salt generated in ortho-sulfonic acid sodium benzaldehyde production process is washed, removes organic substance residues；
(2) the by-product salt after washing is sufficiently dissolved into temperature and saturated solution is made in the pure water between 70 DEG C, and while hot into
Row filtering；
(3) filtered saturated solution is put into four-hole bottle, it is 25% hydrochloric acid solution that mass fraction is added dropwise into four-hole bottle,
The pH value of saturated solution is adjusted to 2, bubble generation is had in hydrochloric acid adition process, when bubble-free generates, stops that salt is added
Acid；
(4) pH value of saturated solution is adjusted to 7.5 with the sodium hydroxide solution that mass fraction is 32% again, then starts to distill
Concentration；
(5) when the amount of precipitation for being concentrated to sodium chloride is that sodium chloride settling volume accounts for the volume of the concentrated liquid 45%, hot filter is carried out, will be filtered
Liquid continues to be concentrated, and until being concentrated into no longer precipitated sodium chloride, to complete the purification of ortho-sulfonic acid sodium benzaldehyde by-product salt, distills out
Water can be used for the washing and dissolution of by-product salt.
Embodiment 3, a kind of method of purification of ortho-sulfonic acid sodium benzaldehyde by-product salt, this method comprises the following steps:
(1) the by-product salt generated in ortho-sulfonic acid sodium benzaldehyde production process is washed, removes organic substance residues；
(2) the by-product salt after washing is sufficiently dissolved into temperature and saturated solution is made in the pure water between 60 DEG C, and while hot into
Row filtering；
(3) filtered saturated solution is put into four-hole bottle, it is 37% hydrochloric acid solution that mass fraction is added dropwise into four-hole bottle,
The pH value of saturated solution is adjusted to 1.5, bubble generation is had in hydrochloric acid adition process, when bubble-free generates, stops being added
Hydrochloric acid；
(4) pH value of saturated solution is adjusted to 7.0 with the sodium hydroxide solution that mass fraction is 30% again, then starts to distill
Concentration；
(5) when the amount of precipitation for being concentrated to sodium chloride is that sodium chloride settling volume accounts for the volume of the concentrated liquid 35%, hot filter is carried out, will be filtered
Liquid continues to be concentrated, and until being concentrated into no longer precipitated sodium chloride, to complete the purification of ortho-sulfonic acid sodium benzaldehyde by-product salt, distills out
Water can be used for the washing and dissolution of by-product salt.
Embodiment 4, a kind of method of purification of ortho-sulfonic acid sodium benzaldehyde by-product salt described in embodiment 1-3, step (3) are described
PH adjustment process in can generate sulfur dioxide, sulfur dioxide is extracted out using vacuum, using sodium hydroxide solution to titanium dioxide
Sulphur is absorbed；It pays close attention in step (3), the pH value situation of sodium hydroxide solution, when pH is down to 9.0 or less, detection, which absorbs, to be had
The content of the sodium hydroxide solution sulfite sodium of sulfur dioxide, adds sodium sulfite solid, for synthesizing ortho-sulfonic acid sodium benzene first
Aldehyde.
Embodiment 5, a kind of method of purification of ortho-sulfonic acid sodium benzaldehyde by-product salt, this approach includes the following steps,
(1) 2000 grams of by-product salt are taken first, and clear water is added to that can stir, is then filtered, and washed again with spray pattern
It washs, the salt after washing is put into hot water and is dissolved, saturated solution is made, and filtering removal mechanical admixture again；
(2) 1000 milliliters of hydrochloric acid saturated solution is added in four-hole bottle, four-hole bottle is with hydrochloric acid Dropping feeder, pH meter, cold
Solidifying device, device for absorbing tail gas, device for absorbing tail gas is interior to use 10% sodium hydroxide solution as absorbing liquid；Four-hole bottle is put into perseverance
In warm water bath, 80~85 DEG C of temperature are maintained；
(3) stirring is opened, and 30% hydrochloric acid solution is added dropwise dropwise, bubble is had at this time and emerges, bubble is mainly sulfur dioxide；Benefit
Sulfur dioxide is introduced in device for absorbing tail gas with vacuum and is absorbed, with the addition of hydrochloric acid solution, bubble is constantly emerged,
PH value can constantly decline, until 1~2；
(4) water-bath is removed at this time, is changed electric jacket into and is heated, until reflux, and maintain；In the process, need to add hydrochloric acid molten
Liquid is to maintenance system pH value；When bubble-free in device for absorbing tail gas or considerably less bubble, heating is temporarily ceased, and
Device for absorbing tail gas is removed, condensing unit is changed to distilling apparatus；With 10% sodium hydroxide solution adjust pH value be 6.5~7.5 it
Between；
(5) heating is reopened, is distilled, distilled water is used for the washing and dissolution of by-product salt after collecting；When being concentrated into solid
When amount of precipitation accounts for total volume 35%, stop heating, and filter while hot；Filter cake is washed with clear water, and washing water is incorporated to filtrate；Filtrate after
Continuous concentration；
Filter cake is collected, dries, and obtains white crystalline body, sodium chloride content 98.8%, other indexs meet GB/T 5462-
2016 exquisite Nacl two-level index；
(6) in step (4), the variation of 10% sodium hydroxide solution in device for absorbing tail gas is paid close attention to, as pH in absorption bottle
When value is down between 9.0~9.5, absorbing liquid is replaced in time；Replaced absorbing liquid, weighing, and detect sodium sulfite and contain
Amount；
Sodium sulfite content is 15.2% in detection absorbing liquid, and weight is 107.3 grams, converts into 16.3 grams of sodium sulfite.
By-product salt of the present invention, source are synthesis ortho-sulfonic acid sodium benzaldehyde by-product, and main component is sodium chloride, Asia
Sodium sulphate, water, a small amount of organic matter.After the present invention washs this part by-product salt, dissolution is filtered to remove organic matter and insoluble machine
Tool impurity obtains salt water, and the sodium sulfite in salt water can decompose output sulfur dioxide through toning acid, heating, and sulfur dioxide utilizes
Sodium hydroxide solution absorbs, and obtains sodium sulfite solution, reuse is into the production of ortho-sulfonic acid sodium benzaldehyde；Acid brine hydroxide
Sodium solution obtains sodium chloride solution after neutralizing, and is further processed and sodium chloride product that meet national standards can be obtained.It not only can be with
Reduce ortho-sulfonic acid sodium benzaldehyde by-product salt processing cost, and by by-product salt sodium chloride and sodium sulfite separation after individually
It uses, reduces the discharge of waste.The output of by-product salt can be greatly reduced in this method, reduce the production of ortho-sulfonic acid sodium benzaldehyde
Cost, but can by by-product salt sodium chloride and sodium sulfite separate, as byproduct or reuse, realize pair
Produce salt resource utilization.
A kind of method purifying ortho-sulfonic acid benzaldehyde by-product salt of the present invention, is that will produce ortho-sulfonic acid sodium benzaldehyde mistake
Sodium chloride by-product that meet national standards can be obtained in the by-product salt generated in journey, the processing such as washed, desulfurization, crystallization, absorption, together
When, the sodium sulfite of recycling can be used for the production of ortho-sulfonic acid sodium benzaldehyde.The present invention has the work that can simplify by-product salt treatment
The sulfur dioxide that skill reduces by-product salt treatment expense, and desulfurization can be made full use of to generate generates sodium sulfite, for synthesizing adjacent sulphur
The advantages of sour sodium benzaldehyde, reduction cost of material.
Claims (8)
1. a kind of method of purification of ortho-sulfonic acid sodium benzaldehyde by-product salt, it is characterised in that: this method comprises the following steps:
(1) the by-product salt generated in ortho-sulfonic acid sodium benzaldehyde production process is washed, removes organic substance residues；
(2) the by-product salt after washing is sufficiently dissolved into hot water and saturated solution is made, and be filtered while hot；
(3) filtered saturated solution is put into four-hole bottle, hydrochloric acid is added dropwise into four-hole bottle, by the pH value tune of saturated solution
Section has bubble generation to 1~2 in hydrochloric acid adition process, when bubble-free generates, stop that hydrochloric acid is added；
(4) pH value of saturated solution is adjusted to neutrality with sodium hydroxide solution again, then starts distillation and concentration；
(5) when being concentrated to sodium chloride precipitation, hot filter is carried out, filtrate is continued to be concentrated, until being concentrated into no longer precipitated sodium chloride,
To complete the purification of ortho-sulfonic acid sodium benzaldehyde by-product salt.
2. the method for purification of ortho-sulfonic acid sodium benzaldehyde by-product salt according to claim 1, it is characterised in that: in step (2)
The hot water is pure water of the temperature between 50~70 DEG C.
3. the method for purification of ortho-sulfonic acid sodium benzaldehyde by-product salt according to claim 1, it is characterised in that: in step (3)
The hydrochloric acid is that mass fraction is 10%~37% hydrochloric acid solution.
4. the method for purification of ortho-sulfonic acid sodium benzaldehyde by-product salt according to claim 1, it is characterised in that: in step (4)
The sodium hydroxide solution is the sodium hydroxide solution that mass fraction is 10%~32%.
5. the method for purification of ortho-sulfonic acid sodium benzaldehyde by-product salt according to claim 1, it is characterised in that: in step (4)
The neutrality is pH=6.5~7.5.
6. the method for purification of ortho-sulfonic acid sodium benzaldehyde by-product salt according to claim 1, it is characterised in that: in step (5)
In, when the amount of precipitation of the sodium chloride is that sodium chloride settling volume accounts for the volume of the concentrated liquid 25%~45%, carry out hot filter.
7. the method for purification of ortho-sulfonic acid sodium benzaldehyde by-product salt according to claim 1, it is characterised in that: step (5) is steamed
The water distillated can be used for the washing and dissolution of by-product salt.
8. the method for purification of ortho-sulfonic acid sodium benzaldehyde by-product salt according to claim 1, it is characterised in that: step (3) institute
Sulfur dioxide can be generated in the pH adjustment process stated, is extracted out sulfur dioxide using vacuum, using sodium hydroxide solution to dioxy
Change sulphur to be absorbed；The pH value situation for paying close attention to sodium hydroxide solution in step (3), when pH is down to 9.0 or less, detection, which absorbs, to be had
The content of the sodium hydroxide solution sulfite sodium of sulfur dioxide, adds sodium sulfite solid, for synthesizing ortho-sulfonic acid sodium benzene first
Aldehyde.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110947297A (en) * | 2019-12-23 | 2020-04-03 | 中国科学院青海盐湖研究所 | Green treatment method for chlorine-containing waste gas |
| CN114620747A (en) * | 2020-12-10 | 2022-06-14 | 自然资源部天津海水淡化与综合利用研究所 | Method for recycling clodinafop-propargyl byproduct salt |
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