CN110563006A - Sodium bisulfite treatment method in production of para-ester - Google Patents
Sodium bisulfite treatment method in production of para-ester Download PDFInfo
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- CN110563006A CN110563006A CN201910912872.8A CN201910912872A CN110563006A CN 110563006 A CN110563006 A CN 110563006A CN 201910912872 A CN201910912872 A CN 201910912872A CN 110563006 A CN110563006 A CN 110563006A
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- Prior art keywords
- sodium bisulfite
- para
- production
- ester
- reaction
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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
The invention relates to the technical field of para-ester production, and discloses a method for treating sodium bisulfite in para-ester production, which comprises the following steps: carrying out reduction reaction; carrying out oxidation reaction; salting out and crystallizing; and (5) filtering and collecting. The excessive hydrogen peroxide is added to completely oxidize the sodium bisulfite to generate sulfate, the chemical reaction can not generate derivatives which interfere the production of the para-ester, thereby achieving the purposes of removing the sodium bisulfite and protecting the production of the para-ester, and the process can not generate harmful substances, and the crystallization time is shortened and the crystallization of the sodium sulfate is accelerated by the action of pressure evaporation crystallization, thereby improving the treatment efficiency of the sodium bisulfite.
Description
Technical Field
The invention relates to the technical field of para-ester production, in particular to a method for treating sodium bisulfite in para-ester production.
Background
in the production process of para-ester (para-beta-ethyl sulfuryl sulfate aniline), a reduction section is a main step, which reduces p-acetamido benzene sulfonyl chloride into sodium p-acetamido phenyl sulfinate, wherein sodium bisulfite must be added, the reduction effect of the sodium bisulfite is utilized to prevent acetaminophen from being oxidized, and in order to ensure that the reaction is thorough under the process conditions, the used NaHSO must be excessive, but the excessive NaHSO not only affects the subsequent section, but also causes the waste water generated in the reaction process to contain a large amount of sodium bisulfite to pollute the environment, so how to effectively treat the excessive sodium bisulfite becomes a problem which must be solved by para-ester manufacturers.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a method for treating sodium bisulfite in production of para-ester, which has the advantages of simple operation, large crystallization ratio and the like, and solves the problems that the sodium bisulfite in production of para-ester affects the product quality and pollutes the environment.
(II) technical scheme
In order to realize the purpose of quickly and efficiently removing the sodium bisulfite, the invention provides the following technical scheme: a method for treating sodium bisulfate in production of para-ester comprises the following steps:
1) Reduction reaction: in the reduction step in the production of para-ester, sodium bisulfite (NaHSO) is added to the reaction tank3) So that the reduction reaction is carried out;
2) and (3) oxidation reaction: after the complete reduction reaction of the materials in the reaction tank, hydrogen peroxide (H) was added to the reaction tank2O2) Oxidizing sodium bisulfite not consumed in the reaction tank to generate sulfate (NaSO)4)；
3) Evaporation and crystallization: putting the solution after complete oxidation into an evaporator, performing pressure evaporation on the evaporator, and salting out crystals;
4) And (3) filtering and collecting: the sulfate crystals in the evaporator were collected by filtration.
Preferably, sodium bisulfite (NaHSO) is added to the reaction tank during the reduction reaction3) The dosage of the material is 120-150% of the total amount of the batch of materials.
Preferably, hydrogen peroxide (H) is added to the oxidation reaction2O2) The dosage of the composition is sodium bisulfite (NaHSO)3) 100-120% of dosage.
Preferably, the conditions of evaporation and concentration in the evaporation crystallization are that the vapor pressure is controlled to be 0.7-0.9 MPa, the negative pressure in an evaporator is 1-1.2 MPa, and the evaporation temperature is 150-200 DEG F.
preferably, the evaporated crystals in the filtration collection are filtered by a filter screen, so that the evaporated crystals are completely separated from the solution.
preferably, the solution after filtration in the filtration collection is led out, and the subsequent working sections of para-ester production are sequentially carried out.
(III) advantageous effects
Compared with the prior art, the invention provides a method for treating sodium bisulfite in para-ester production, which has the following beneficial effects:
According to the method for treating the sodium bisulfite in the production of the para-ester, the sodium bisulfite is completely oxidized by adding excessive hydrogen peroxide to generate sulfate, and the chemical reaction does not generate derivatives which interfere the production of the para-ester, so that the purposes of removing the sodium bisulfite and protecting the production of the para-ester are achieved, no harmful substances are generated in the process, the crystallization time is shortened by the action of pressurization, evaporation and crystallization, the crystallization of sodium sulfate is accelerated, and the treatment efficiency of the sodium bisulfite is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a method for treating sodium bisulfite in production of para-ester, which comprises the following steps: 1) reduction reaction: in the reduction step in the production of para-ester, sodium bisulfite (NaHSO) is added to the reaction tank3) So that the reduction reaction is carried out; sodium bisulfite (NaHSO) is added into the reaction tank in the reduction reaction3) The dosage of the raw materials is 120 to 150 percent of the total amount of the batch of materials; 2) and (3) oxidation reaction: after the materials in the reaction tank are completely reduced, the materials are reactedHydrogen peroxide (H) is added into the pool2O2) Oxidizing sodium bisulfite not consumed in the reaction tank to generate sulfate (NaSO)4) (ii) a Adding hydrogen peroxide (H) to the oxidation reaction2O2) The dosage of the composition is sodium bisulfite (NaHSO)3) 100-120% of the dosage; 3) evaporation and crystallization: putting the solution after complete oxidation into an evaporator, performing pressure evaporation on the evaporator, and salting out crystals; the conditions of evaporation and concentration in the evaporation crystallization are that the steam pressure is controlled to be 0.7-0.9 MPa, the negative pressure in an evaporator is 1-1.2 MPa, and the evaporation temperature is 150-200 DEG F; 4) and (3) filtering and collecting: filtering and collecting sulfate crystals in the evaporator; and filtering the evaporated crystals in the filtering collection through a filter screen to completely separate the evaporated crystals from the solution, leading out the filtered solution, and sequentially performing subsequent working sections of para-ester production.
The first embodiment is as follows:
The method comprises the following steps: 1) in the reduction reaction in the production of para-ester, sodium bisulfite (NaHSO) is added to the reaction tank3) Adding sodium bisulfite (NaHSO)3) The dosage of the raw materials is 150 percent of the total amount of the batch materials, and the steps are as follows: 2) after the complete reduction reaction of the materials in the reaction tank, hydrogen peroxide (H) was added to the reaction tank2O2) Oxidizing sodium bisulfite not consumed in the reaction tank to generate sulfate (NaSO)4) During this process, hydrogen peroxide (H) is added2O2) The dosage of the composition is sodium bisulfite (NaHSO)3) 100% of the dose, step: 3) putting the completely oxidized solution into an evaporator, performing pressure evaporation in the evaporator, salting out, crystallizing, and concentrating under the conditions of vapor pressure of 0.7MPa, negative pressure of 1MPa in the evaporator, and evaporation temperature of 150 ℉.
By this method the oxidation reaction is too slow and there is a possibility that hydrogen sulphite in the feed will remain.
Example two:
The method comprises the following steps: 1) in the reduction reaction in the production of para-ester, sodium bisulfite (NaHSO) is added to the reaction tank3) Adding sodium bisulfite (NaHSO)3) The dosage of (A) is 150% of the total amount of the batch material: 2) after the complete reduction reaction of the materials in the reaction tank, hydrogen peroxide (H) was added to the reaction tank2O2) Oxidizing sodium bisulfite not consumed in the reaction tank to generate sulfate (NaSO)4) During this process, hydrogen peroxide (H) is added2O2) The dosage of the composition is sodium bisulfite (NaHSO)3) 120% of the dose, step: 3) putting the completely oxidized solution into an evaporator, performing pressure evaporation in the evaporator, salting out, crystallizing, and concentrating under the conditions of vapor pressure of 0.7MPa, negative pressure of 1MPa in the evaporator, and evaporation temperature of 150 ℉.
The difference between the second embodiment and the first embodiment is that the dosage of the hydrogen peroxide is different, so that the oxidation reaction speed is accelerated, and the sodium bisulfite is fully oxidized, so that the sodium bisulfite in the material is completely converted into sodium sulfate.
Example three:
The method comprises the following steps: 1) in the reduction reaction in the production of para-ester, sodium bisulfite (NaHSO) is added to the reaction tank3) Adding sodium bisulfite (NaHSO)3) The dosage of the raw materials is 150 percent of the total amount of the batch materials, and the steps are as follows: 2) after the complete reduction reaction of the materials in the reaction tank, hydrogen peroxide (H) was added to the reaction tank2O2) Oxidizing sodium bisulfite not consumed in the reaction tank to generate sulfate (NaSO)4) During this process, hydrogen peroxide (H) is added2O2) The dosage of the composition is sodium bisulfite (NaHSO)3) 120% of the dose, step: 3) putting the completely oxidized solution into an evaporator, performing pressure evaporation in the evaporator, salting out, crystallizing, and concentrating under the conditions of vapor pressure of 0.9MPa, negative pressure of 1.2MPa in the evaporator, and evaporation temperature of 200 ℉.
The difference between the third embodiment and the second embodiment is that the pressure and the temperature are different during evaporation, so that the evaporation crystallization speed is increased, and the time and the cost are saved.
In summary, compared with the prior art, the method for treating sodium bisulfite in production of para-ester provided by the invention has the following beneficial effects: according to the method for treating the sodium bisulfite in the production of the para-ester, the sodium bisulfite is completely oxidized by adding excessive hydrogen peroxide to generate sulfate, and the chemical reaction does not generate derivatives which interfere the production of the para-ester, so that the purposes of removing the sodium bisulfite and protecting the production of the para-ester are achieved, no harmful substances are generated in the process, the crystallization time is shortened by the action of pressurization, evaporation and crystallization, the crystallization of sodium sulfate is accelerated, and the treatment efficiency of the sodium bisulfite is improved.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A method for treating sodium bisulfite in production of para-ester is characterized by comprising the following steps:
1) Reduction reaction: in the reduction step in the production of para-ester, sodium bisulfite (NaHSO) is added to the reaction tank3) So that the reduction reaction is carried out;
2) And (3) oxidation reaction: after the materials in the reaction tank are completely reduced, hydrogen peroxide (H) is added into the reaction tank2O2) Oxidizing sodium bisulfite not consumed in the reaction tank to generate sulfate (NaSO)4)；
3) Evaporation and crystallization: putting the solution after complete oxidation into an evaporator, performing pressure evaporation on the evaporator, and salting out crystals;
4) And (3) filtering and collecting: the sulfate crystals in the evaporator were collected by filtration.
2. The method for treating sodium bisulfite in production of para-ester according to claim 1, wherein sodium bisulfite (NaHSO) is added into the reaction tank during the reduction reaction3) The dosage of the raw materials is 120 to 150 percent of the total amount of the batch of materials.
3. The method for treating sodium bisulfite in production of para-ester according to claim 1, wherein hydrogen peroxide (H) is added in the oxidation reaction2O2) The dosage of the composition is sodium bisulfite (NaHSO)3) The dosage is 100-120%.
4. The method of claim 1, wherein the conditions for evaporation and concentration in the evaporative crystallization are controlled to have a vapor pressure of 0.7 to 0.9MPa, a negative pressure of 1 to 1.2MPa in the evaporator, and an evaporation temperature of 150 to 200 ℉.
5. The method for treating sodium bisulfite in production of para-ester as claimed in claim 1, wherein the evaporated crystals in the filtration collection are filtered by a filter screen to be completely separated from the solution.
6. The method for treating sodium bisulfite in production of para-ester according to claim 1, wherein the solution after filtration in the filtration collection is led out, and the subsequent working sections of para-ester production are performed in sequence.
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| CN201910912872.8A CN110563006A (en) | 2019-09-25 | 2019-09-25 | Sodium bisulfite treatment method in production of para-ester |
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| CN201910912872.8A CN110563006A (en) | 2019-09-25 | 2019-09-25 | Sodium bisulfite treatment method in production of para-ester |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86108584A (en) * | 1985-11-18 | 1987-07-29 | 盐野义制药株式会社 | The method for preparing bicyclic sulfonamide |
| US20040192708A1 (en) * | 2003-02-19 | 2004-09-30 | Dunten Peter W. | Sulfonamide substituted xanthine derivatives |
| CN104370780A (en) * | 2014-10-21 | 2015-02-25 | 泰兴锦云染料有限公司 | Radical benzene sulfonamide ethyl sulfuryl hydroxyethyl sulfate aniline compound and preparation method thereof |
| CN109206347A (en) * | 2017-06-29 | 2019-01-15 | 开封市隆兴化工有限公司 | The processing method of the excessive sodium hydrogensulfite of workshop section is restored in para-ester production |
-
2019
- 2019-09-25 CN CN201910912872.8A patent/CN110563006A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86108584A (en) * | 1985-11-18 | 1987-07-29 | 盐野义制药株式会社 | The method for preparing bicyclic sulfonamide |
| US4861913A (en) * | 1985-11-18 | 1989-08-29 | Shionogi & Co., Ltd. | Bicyclic sulfonamide derivatives |
| US20040192708A1 (en) * | 2003-02-19 | 2004-09-30 | Dunten Peter W. | Sulfonamide substituted xanthine derivatives |
| CN104370780A (en) * | 2014-10-21 | 2015-02-25 | 泰兴锦云染料有限公司 | Radical benzene sulfonamide ethyl sulfuryl hydroxyethyl sulfate aniline compound and preparation method thereof |
| CN109206347A (en) * | 2017-06-29 | 2019-01-15 | 开封市隆兴化工有限公司 | The processing method of the excessive sodium hydrogensulfite of workshop section is restored in para-ester production |
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Application publication date: 20191213 |