CN115286512A - Process for purifying nitration product - Google Patents
Process for purifying nitration product Download PDFInfo
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- CN115286512A CN115286512A CN202210877118.7A CN202210877118A CN115286512A CN 115286512 A CN115286512 A CN 115286512A CN 202210877118 A CN202210877118 A CN 202210877118A CN 115286512 A CN115286512 A CN 115286512A
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- Prior art keywords
- washing
- wastewater
- alkaline
- water
- filter cake
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- 238000006396 nitration reaction Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000005406 washing Methods 0.000 claims abstract description 179
- 239000002351 wastewater Substances 0.000 claims abstract description 129
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 57
- 230000007935 neutral effect Effects 0.000 claims abstract description 35
- 239000000047 product Substances 0.000 claims abstract description 34
- 239000012065 filter cake Substances 0.000 claims abstract description 30
- 239000008213 purified water Substances 0.000 claims abstract description 16
- 238000000746 purification Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000012043 crude product Substances 0.000 claims description 11
- 238000001514 detection method Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000012670 alkaline solution Substances 0.000 claims 1
- 239000000243 solution Substances 0.000 claims 1
- 238000007599 discharging Methods 0.000 description 9
- 239000003513 alkali Substances 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 230000001502 supplementing effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- NESLWCLHZZISNB-UHFFFAOYSA-M sodium phenolate Chemical compound [Na+].[O-]C1=CC=CC=C1 NESLWCLHZZISNB-UHFFFAOYSA-M 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 description 1
- ZXVONLUNISGICL-UHFFFAOYSA-N 4,6-dinitro-o-cresol Chemical group CC1=CC([N+]([O-])=O)=CC([N+]([O-])=O)=C1O ZXVONLUNISGICL-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- -1 nitro ester compound Chemical class 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/16—Separation; Purification; Stabilisation; Use of additives
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a purification process of a nitration product, belonging to the technical field of nitration reaction, wherein the nitration product is transferred to an alkaline washing kettle, then alkaline liquor and non-neutral washing wastewater are added into the alkaline washing kettle, stirred and washed until the pH value of an alkaline washing mixed system is 7.0 +/-0.2, and filtered to obtain a filter cake after alkaline washing and alkaline washing wastewater; transferring the filter cake after alkaline washing into a washing kettle, washing the filter cake after alkaline washing by using neutral washing wastewater, introducing purified water into the washing kettle for washing, and continuously introducing purified water for washing for 5-10min when the pH value of discharged washing wastewater is 7.0 to obtain a filter cake after washing; transferring the filter cake after washing to a drying oven for drying and storing to finish the purification process of the nitration product; the washing wastewater is utilized in a grading way, so that the use amount of purified water and the generation of total wastewater are reduced, and the total wastewater is reduced by 22 percent compared with the traditional process.
Description
Technical Field
The invention belongs to the technical field of nitration reaction, and particularly relates to a purification process of a nitration product.
Background
Nitration refers to a reaction in which a nitro group is introduced into an organic compound molecule, and the nitro group can be connected with a carbon atom in the organic compound to form a nitro compound, can also be connected with an oxygen atom to form a nitro ester compound, and can also be connected with a nitrogen atom to form ammonium nitrate and the like. After the nitration reaction is finished, a small amount of impurities such as acid, phenol, dinitro products and the like also exist in the primarily obtained nitrated product, influence is caused on the subsequent rectification process and crystallization process, and the impurities in the nitrated product are removed through the steps of alkali washing neutralization and water washing impurity removal. However, these purification steps require a large amount of purified water, which is not only disadvantageous in terms of cost control, but also increases the generation of wastewater, and puts pressure on the wastewater treatment system. Thus, a process for purifying the nitrated product is proposed.
Disclosure of Invention
The invention aims to provide a purification process of a nitration product, which aims to solve the problems in the background art.
The purpose of the invention can be realized by the following technical scheme:
a process for purifying a nitrated product, comprising the steps of:
the method comprises the following steps: transferring the nitration product into an alkaline washing kettle, adding alkali liquor into the alkaline washing kettle and supplementing a proper amount of non-neutral washing wastewater, continuously stirring at 25-30 ℃ and 100-200r/min until the pH value of an alkaline washing mixed system is 7.0 +/-0.2, filtering to obtain an alkaline washing filter cake and alkaline washing wastewater, discharging the alkaline washing wastewater and treating the wastewater;
step two: transferring the filter cake after alkaline washing into a washing kettle, firstly washing with preheated neutral washing wastewater, then introducing purified water with the temperature of 55-75 ℃ into the washing kettle, continuing to wash the filter cake after alkaline washing, detecting the pH value of the washing wastewater at the water discharge outlet of the washing kettle to 7.0, continuing to introduce the purified water for washing for 5-10min, continuously discharging the washing wastewater in the washing process, and obtaining a washed filter cake after washing;
step three: and transferring the filter cake after water washing to a drying oven for drying for 6-8h to obtain a mononitro crude product, transferring the mononitro crude product to a storage tank for later use, and finishing the purification process of the nitration product.
Further, a pH online detection device is arranged at a water outlet of the washing kettle in the second step, and the pH value of the effluent washing wastewater is detected in real time; when the pH value is detected to be not 7.0, introducing the water washing wastewater into a wastewater tank A; when the pH value is detected to be 7.0, continuously introducing the water washing wastewater into the wastewater tank A for 0.5-1min, aiming at completely discharging the water washing wastewater with the pH value not to be 7.0 in the water discharge pipe of the water washing kettle, and then introducing the water washing wastewater into the wastewater tank B; non-neutral washing wastewater is stored in the wastewater tank A, and neutral washing wastewater is stored in the wastewater tank B.
Further, the neutral washing wastewater in the wastewater tank B is preheated to 55-75 ℃, and the non-neutral washing wastewater in the wastewater tank A is cooled to 25-30 ℃ for standby.
Further, the alkali liquor is sodium hydroxide solution with the mass fraction of 30-45%.
The invention has the beneficial effects that:
according to the purification process of the nitration product, the waste acid contained in the nitration product can be basically neutralized by alkali washing, the nitrophenol in the nitration product can generate the sodium phenolate which is easy to dissolve in water, and the sodium phenolate and other inorganic salts which are easy to dissolve in water in the filter cake after the alkali washing are washed by hot water in the water washing process, so that most impurities in the nitration product are removed, a relatively pure mononitro crude product is obtained, and the subsequent rectification and crystallization processes can be conveniently carried out.
And (4) separating the washing wastewater discharged by the washing kettle, storing the non-neutral washing wastewater in the wastewater tank A, and storing the neutral wastewater in the wastewater tank B. Because the filter cake after alkaline washing is weakly acidic or weakly alkaline, the washing wastewater is utilized in a grading way, firstly, the preheated non-neutral wastewater is used for washing the filter cake after alkaline washing, and the use amount of purified water is favorably reduced; when the pH value of the washing wastewater is detected to be 7.0, the washing wastewater is continuously washed by purified water, so that the removal rate of other impurities is ensured; and the non-neutral water washing wastewater is also added into the alkaline washing kettle for reuse, so that the generation of the total wastewater is reduced. Compared with the traditional process, the total wastewater is reduced by 22 percent.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a flow diagram of a process for the purification of a nitrated product of the present invention.
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.
Example 1
Referring to fig. 1, a process for purifying a nitration product comprises the following steps:
the method comprises the following steps: and transferring the nitration product to an alkaline washing kettle, adding a sodium hydroxide solution with the mass fraction of 30% into the alkaline washing kettle, supplementing a proper amount of non-neutral washing wastewater, continuously stirring at 25 ℃ and 100r/min until the pH value of an alkaline washing mixed system is 6.8, filtering to obtain an alkaline washing filter cake and alkaline washing wastewater, discharging the alkaline washing wastewater, and treating the wastewater.
Step two: and transferring the filter cake after alkaline washing into a washing kettle, washing by using preheated neutral washing wastewater, introducing purified water with the temperature of 55 ℃ into the washing kettle, continuously washing the filter cake after alkaline washing, and continuously discharging the washing wastewater in the washing process.
A water outlet of the washing kettle is provided with a pH on-line detection device for detecting the pH value of the effluent washing wastewater in real time; when the pH value is detected to be not 7.0, introducing the water washing wastewater into a wastewater tank A; and when the pH value is detected to be 7.0, continuing to introduce purified water for washing for 5min, and continuing to introduce the water washing wastewater into the wastewater tank A for 0.5min, so as to completely discharge the water washing wastewater with the pH value not to be 7.0 in the water discharge pipe of the water washing kettle, and then introducing the water washing wastewater into the wastewater tank B.
The wastewater tank A stores non-neutral washing wastewater, and the wastewater tank B stores neutral washing wastewater. Preheating neutral washing wastewater in the wastewater tank B to 55 ℃, and cooling non-neutral washing wastewater in the wastewater tank A to 25 ℃ for later use.
Step three: and transferring the filter cake after water washing to a drying oven for drying for 6h to obtain a mononitro crude product, transferring the mononitro crude product to a storage tank for later use, and finishing the purification process of the nitration product.
Example 2
Referring to fig. 1, a process for purifying a nitration product comprises the following steps:
the method comprises the following steps: transferring the nitration product into an alkaline washing kettle, adding a sodium hydroxide solution with the mass fraction of 40% into the alkaline washing kettle, supplementing a proper amount of non-neutral washing wastewater, continuously stirring at 28 ℃ and 150r/min until the pH value of an alkaline washing mixed system reaches 7.0, filtering to obtain an alkaline washing filter cake and alkaline washing wastewater, discharging the alkaline washing wastewater, and treating the wastewater.
Step two: and transferring the filter cake after alkaline washing into a washing kettle, washing by using preheated neutral washing wastewater, introducing 65 ℃ purified water into the washing kettle, continuously washing the filter cake after alkaline washing, and continuously discharging the washing wastewater in the washing process.
A water outlet of the washing kettle is provided with a pH on-line detection device for detecting the pH value of the effluent washing wastewater in real time; when the pH value is detected to be not 7.0, introducing the water washing wastewater into a wastewater tank A; and when the pH value is detected to be 7.0, continuing to introduce purified water for washing for 8min, and continuing to introduce the water washing wastewater into the wastewater tank A for 0.8min, so as to completely discharge the water washing wastewater with the pH value not to be 7.0 in the water discharge pipe of the water washing kettle, and then introducing the water washing wastewater into the wastewater tank B.
Non-neutral washing wastewater is stored in the wastewater tank A, and neutral washing wastewater is stored in the wastewater tank B. Preheating the neutral washing wastewater in the wastewater tank B to 65 ℃, and cooling the non-neutral washing wastewater in the wastewater tank A to 28 ℃ for later use.
Step three: and transferring the filter cake after water washing to a drying oven for drying for 7h to obtain a mononitro crude product, transferring the mononitro crude product to a storage tank for later use, and finishing the purification process of the nitration product.
Example 3
Referring to fig. 1, a process for purifying a nitration product comprises the following steps:
the method comprises the following steps: and transferring the nitration product to an alkaline washing kettle, adding a sodium hydroxide solution with the mass fraction of 45% into the alkaline washing kettle, supplementing a proper amount of non-neutral washing wastewater, continuously stirring at 30 ℃ and 200r/min until the pH value of an alkaline washing mixed system is 7.2, filtering to obtain an alkaline washing filter cake and alkaline washing wastewater, discharging the alkaline washing wastewater, and treating the wastewater.
Step two: and transferring the filter cake after alkaline washing into a washing kettle, washing by using preheated neutral washing wastewater, introducing purified water with the temperature of 75 ℃ into the washing kettle, continuously washing the filter cake after alkaline washing, and continuously discharging the washing wastewater in the washing process.
A water outlet of the washing kettle is provided with a pH on-line detection device for detecting the pH value of the effluent washing wastewater in real time; when the pH value is detected to be not 7.0, introducing the water washing wastewater into a wastewater tank A; and when the pH value is detected to be 7.0, continuing introducing purified water for washing for 10min, and continuing introducing the washing wastewater into the wastewater tank A for 1min so as to completely discharge the washing wastewater with the pH value not to be 7.0 in the water discharge pipe of the washing kettle, and then introducing the washing wastewater into the wastewater tank B.
The wastewater tank A stores non-neutral washing wastewater, and the wastewater tank B stores neutral washing wastewater. Preheating neutral washing wastewater in the wastewater tank B to 75 ℃, and cooling non-neutral washing wastewater in the wastewater tank A to 30 ℃ for later use.
Step three: and transferring the filter cake after water washing to a drying oven for drying for 8h to obtain a mononitro crude product, transferring the mononitro crude product to a storage tank for later use, and finishing the purification process of the nitration product.
Compared with the traditional nitrated product purification process, the nitrated product is purified according to the methods of the examples 1 to 3, and the generated alkaline washing wastewater is reduced by 22 percent after the nitrated product with the same quality is purified.
It should be noted that, in this document, terms such as "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
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 purification process of a nitration product is characterized by comprising the following steps:
the method comprises the following steps: transferring the nitration product into an alkaline washing kettle, adding alkaline liquor and non-neutral water washing wastewater into the alkaline washing kettle, stirring and washing at 25-30 ℃ until the pH value of an alkaline washing mixed system is 7.0 +/-0.2, and filtering to obtain an alkaline washing filter cake and alkaline washing wastewater;
step two: transferring the filter cake after alkaline washing into a washing kettle, washing the filter cake after alkaline washing by using neutral washing wastewater, introducing purified water with the temperature of 55-75 ℃ into the washing kettle for washing, and continuously introducing the purified water for washing for 5-10min when the pH value of the discharged washing wastewater is 7.0 to obtain a washed filter cake;
step three: and transferring the filter cake after water washing to a drying oven for drying for 6-8h to obtain a mononitro crude product, and transferring the mononitro crude product to a storage tank for later use, thereby completing the purification process of the nitration product.
2. The purification process of a nitration product according to claim 1, wherein a pH on-line detection device is disposed at the water outlet of the washing kettle in the second step, for performing real-time pH value detection on the effluent washing wastewater; when the pH value is detected to be not 7.0, introducing the water washing wastewater into a wastewater tank A; when the pH value is detected to be 7.0, continuously introducing the water washing wastewater into the wastewater tank A for 0.5-1min, and then introducing the water washing wastewater into the wastewater tank B.
3. The process according to claim 2, wherein the wastewater tank A stores non-neutral washing wastewater and the wastewater tank B stores neutral washing wastewater.
4. A process according to claim 3, wherein the non-neutral water-washing waste water in the waste water tank A is cooled to 25-30 ℃ for further use.
5. A process according to claim 3, wherein the neutral water-washing wastewater in the wastewater tank B is preheated to 55-75 ℃ for further use.
6. The process of claim 1, wherein the alkaline solution is 30-45 wt% sodium hydroxide solution.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210877118.7A CN115286512A (en) | 2022-07-25 | 2022-07-25 | Process for purifying nitration product |
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| CN202210877118.7A CN115286512A (en) | 2022-07-25 | 2022-07-25 | Process for purifying nitration product |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106083598A (en) * | 2016-06-12 | 2016-11-09 | 江苏省海洋资源开发研究院(连云港) | A kind of 2,5 dichloronitrobenzene autoclave adverse currents neutralize washing methods continuously |
| CN106278903A (en) * | 2015-05-18 | 2017-01-04 | 中国石油化工股份有限公司 | Thick chloronitrobenzene washing production method |
| CN106278902A (en) * | 2015-06-08 | 2017-01-04 | 中国石油化工股份有限公司 | A kind of reduce the method for sodium salt content in thick Nitrobenzol |
| CN206232632U (en) * | 2016-11-07 | 2017-06-09 | 山东昌邑灶户盐化有限公司 | 2,4 dinitrochlorobenzene water washing cycles utilize device |
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2022
- 2022-07-25 CN CN202210877118.7A patent/CN115286512A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106278903A (en) * | 2015-05-18 | 2017-01-04 | 中国石油化工股份有限公司 | Thick chloronitrobenzene washing production method |
| CN106278902A (en) * | 2015-06-08 | 2017-01-04 | 中国石油化工股份有限公司 | A kind of reduce the method for sodium salt content in thick Nitrobenzol |
| CN106083598A (en) * | 2016-06-12 | 2016-11-09 | 江苏省海洋资源开发研究院(连云港) | A kind of 2,5 dichloronitrobenzene autoclave adverse currents neutralize washing methods continuously |
| CN206232632U (en) * | 2016-11-07 | 2017-06-09 | 山东昌邑灶户盐化有限公司 | 2,4 dinitrochlorobenzene water washing cycles utilize device |
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