CN107244756B - A kind of post-processing approach of phenylenediamine hydrolyzate - Google Patents
A kind of post-processing approach of phenylenediamine hydrolyzate Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C07C37/01—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by replacing functional groups bound to a six-membered aromatic ring by hydroxy groups, e.g. by hydrolysis
- C07C37/045—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by replacing functional groups bound to a six-membered aromatic ring by hydroxy groups, e.g. by hydrolysis by substitution of a group bound to the ring by nitrogen
- C07C37/05—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by replacing functional groups bound to a six-membered aromatic ring by hydroxy groups, e.g. by hydrolysis by substitution of a group bound to the ring by nitrogen by substitution of a NH2 group
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Abstract
The present invention relates to phenylenediamine production technical fields, particularly disclose a kind of post-processing approach of phenylenediamine hydrolyzate.The post-processing approach of the phenylenediamine hydrolyzate, it is characterized in that：Hydrolyzate is subjected to three sections of extractions, 38 grades of extractions of every section of extraction point, every grade of extraction oil phase and raffinate water phase is through filtering and impurity removing, and extraction oil phase enters precipitation process rich in benzenediol, and raffinate water phase enters next section of processing；Raffinate water phase carries out activated carbon adsorption decolorization later, and activated carbon is loaded using packed column, and raffinate water phase flows in series through activated carbon packed column and adsorbed, and water phase that treated meets hydrolysis complex acid requirement.Alcohol, acid, ketone, ether, esters content are less than 50ppm in water phase after present invention processing, the water phase is by a certain percentage with reuse p-phenylenediamine hydrolysis after pure water mixing complex acid without influence, and processing is convenient, scientific in principle, improve the utilization rate of reaction material liquid, green economy.
Description
（One）Technical field
The present invention relates to phenylenediamine production technical field, more particularly to a kind of post-processing approach of phenylenediamine hydrolyzate.
（Two）Background technology
Benzenediol and amino-phenol are important fine Organic Chemicals, are widely used in agricultural, dyestuff, coating, doctor
The fields such as medicine, plastics, rubber, electronic chemical product.Currently, the main preparation methods of benzenediol and amino-phenol have sulfonation alkali fusion
Method, diisopropylbenzene (DIPB) oxidizing process and phenylenediamine Hydrolyze method.Compared to first two production method, phenylenediamine Hydrolyze method has benefited from raw material
Source is convenient, technological process is succinct, technology maturation and of reduced contamination and be widely studied use, and good application prospect is presented.
In phenylenediamine hydrolysis prepares benzenediol and amino-phenol technique, it is related to benzenediol and amino-phenol from hydrolyzate
Process and raffinate the water phase decoloration of middle extraction, the process of removal of impurities, since raffinate water phase amount is big in technical process and contains salt, no
Energy direct emission, it is necessary to be recycled after appropriately processed；And the extraction process of benzenediol and amino-phenol mostly uses greatly at present
Alcohols, ketone, ethers and esters extractant, which has certain solubility in water, and esters extractant is in acid
Hydrolysis easily occurs in property aqueous solution, generates corresponding alcohol and acid, experiments verify that, alcohol, acid, ketone, ether, esters p-phenylenediamine
Hydrolysis have larger impact, can aggravate the generation of burnt oil impurities, reduce reaction yield, the processing for increasing hydrolyzate is difficult
Degree.Therefore, it will be unable to meet the requirement that complex acid recycles again, gesture after in aqueous phase extracted containing alcohol, acid, ketone, ether, esters
Necessity carries out purified treatment to it.
（Three）Invention content
In order to compensate for the shortcomings of the prior art, the present invention provides a kind of extraction yields high, raffinate water phase utilization rate height, processing
The post-processing approach of phenylenediamine hydrolyzate at low cost.
The present invention is achieved through the following technical solutions：
A kind of post-processing approach of phenylenediamine hydrolyzate, the hydrolyzate of benzenediol or amino-phenol is prepared with phenylenediamine hydrolysis
For process object, include the following steps：
（1）Hydrolyzate is subjected to first segment extraction, it is the 15- of hydrolyzate quality to divide 3-8 grades of extractions, every grade of Solvent quantity
35%, extraction temperature is 15-40 DEG C, and by filtering out solid impurity, extraction oil phase is rich in every grade of extraction oil phase and raffinate water phase
Benzenediol enters precipitation process, and raffinate water phase enters next section of processing；
（2）By step（1）Gained raffinate water phase uses liquefied ammonia or mass concentration to adjust pH to 6.5- for the ammonium hydroxide of 15-35%
7.5, it is filtered to remove precipitation solid impurity, filtrate carries out second segment extraction, the same step of extraction step（1）, obtained extraction oil phase
Enter precipitation process rich in amino-phenol, raffinate water phase enters next section of processing；
（3）By step（2）Gained raffinate water phase carries out third section extraction, the same step of extraction step（1）, obtained extraction oil
Mutually enter precipitation process and recycle extractant, raffinate water phase enters next section of processing；
（4）By step（3）Gained raffinate water phase carries out activated carbon adsorption decolorization, and activated carbon is loaded using packed column,
Raffinate water phase flows in series through activated carbon packed column and is adsorbed, flow velocity 1-50BV/hr, and it is anti-that the liquid after absorption meets hydrolysis
It should require, be mixed with pure water and carry out complex acid, be used for the hydrolysis of phenylenediamine.
The hydrolyzate that phenylenediamine hydrolysis is prepared benzenediol or amino-phenol by the present invention carries out stage extraction and activated carbon suction
Attached processing, every section of extraction processing are all made of fractional extraction operation, and raffinate water phase after processing meets the requirement of complex acid reuse, changes
Into the defect of prior art method, while ensureing high extraction yield, the demand of raffinate water phase recycling is met, is reduced
Side reaction improves yield, has saved cost.
The present invention more excellent technical solution be：
In the hydrolyzate, benzenediol weight ratio is 1-10%, and amino-phenol weight ratio is 1-10%, and phenylenediamine weight ratio is low
It is less than 1 in 0.5%, pH.
Step（1）In, first segment extraction divides 4-6 grades of extractions, every grade of Solvent quantity to be the 20-30% of hydrolyzate quality, extraction
It is 20-30 DEG C of to take temperature
Step（2）In, use liquefied ammonia or mass concentration to adjust the pH to 6.5-7.0 of raffinate water phase for the ammonium hydroxide of 25-30%.
Step（1）With（2）In, extractant is hexone, n-butanol, n-propyl acetate, isopropyl acetate, second
One or more of sour N-butyl, isobutyl acetate, pentyl acetate and Di Iso Propyl Ether；It is preferred that hexone, second
One or more of sour N-butyl, isobutyl acetate and pentyl acetate.
Step（3）In, extractant is alkane derivative, such as one kind in pentane, hexane, heptane and octane, preferably penta
One kind in alkane, hexane and heptane.
Step（4）In, the activated carbon for adsorption bleaching is one kind in coconut husk charcoal, fruit shell carbon, carbo lignius or coal quality charcoal,
It is preferred that coconut husk charcoal or coal quality charcoal；Upper prop flow velocity is 10-30BV/hr.
Compared with prior art, the present invention using three sections of extractions plus the technique of one section of adsorption treatment, make benzenediol extraction yield
Higher than 99%, amino-phenol extraction yield is higher than 98.5%, and alcohol, acid, ketone, esters content are less than 50ppm, the water phase in water phase after processing
By a certain percentage with reuse p-phenylenediamine hydrolysis after pure water mixing complex acid without influence, processing is convenient, and scientific in principle carries
The high utilization rate of reaction material liquid, green economy.
（Four）Specific implementation mode
Embodiment 1：A kind of post-processing approach of m-phenylene diamine (MPD) hydrolyzate, concrete processing procedure are：
（1）Resorcinol content 5%, m-aminophenol content 1%, m-phenylene diamine (MPD) content be about in m-phenylene diamine (MPD) hydrolyzate
The hydrolyzate is carried out first segment extraction by 0.2%, about 0.3 pH：Divide 4 grades of extractions；Every grade of Solvent quantity is hydrolyzate quality
20%, extractant is hexone；20 DEG C of extraction temperature；Every grade of extraction oil phase and raffinate water phase is through filtering and impurity removing；
Oil phase after first segment extracts is rich in resorcinol precipitation process to be entered, and raffinate water phase waits entering next section of processing.
（2）Through step（1）Obtained raffinate water phase uses mass concentration to adjust pH to 6.5 for 25% ammonium hydroxide, is filtered to remove
Impurity is precipitated, filtrate carries out second segment extraction, extracting operation similar step（1）, extractant is n-butanol；It is extracted by second segment
Oil phase afterwards is rich in m-aminophenol precipitation process to be entered, and raffinate water phase waits entering next section of processing.
（3）Through step（2）Obtained raffinate water phase, which is adopted, carries out third section extraction, extracting operation similar step（1）And step
（2）, extractant is pentane；Oil phase after the extraction of third section enters precipitation process and recycles extractant, and raffinate water phase waits entering
Next section of processing.
（4）Through step（3）Obtained raffinate water phase flows in series through activated carbon packed column and is adsorbed, and activated carbon uses coconut husk
Charcoal, upper prop flow velocity 10BV/hr, water phase that treated through chromatogram ration analysis, wherein hexone content about
21ppm, levels of n-butanol about 20ppm, isopentane content are less than 8ppm, can meet hydrolysis complex acid use demand.
Confirmatory experiment A：
Learnt from else's experience treated water phase 100g (through analysis, wherein ammonium sulphate content be 12.25%) with 200g deionizations
Water mixes, and the 38g concentrated sulfuric acids are dissolved in above-mentioned 300g water phases, 21.6g m-phenylene diamine (MPD)s is weighed and is completely dissolved in above-mentioned dilution heat of sulfuric acid,
It is transferred in 500mL autoclaves, air 6 times in displacement kettle is repeated using nitrogen, starts stirring to 200rpm, is heated to
220 DEG C of maintenance 8hr.Pressure release after cooling to room temperature, hydrolyzate is through efficient liquid phase chromatographic analysis：M-phenylene diamine (MPD) conversion ratio
99.7%, resorcinol yield is about 95.2%.
Confirmatory experiment B：
The 38g concentrated sulfuric acids are dissolved in 300g deionized waters, 21.6g m-phenylene diamine (MPD)s is weighed and is completely dissolved in above-mentioned dilution heat of sulfuric acid
In, it is transferred in 500mL autoclaves, air 6 times in displacement kettle is repeated using nitrogen, start stirring to 200rpm, heating
To 220 DEG C of maintenance 8hr.Pressure release after cooling to room temperature, hydrolyzate is through efficient liquid phase chromatographic analysis：M-phenylene diamine (MPD) conversion ratio is about
99.8%, resorcinol yield is about 95.4%.
Embodiment 2：A kind of post-processing approach of m-phenylene diamine (MPD) hydrolyzate, concrete processing procedure are：
（1）Resorcinol content 7%, m-aminophenol content 2%, m-phenylene diamine (MPD) content be about in m-phenylene diamine (MPD) hydrolyzate
The hydrolyzate is carried out first segment extraction by 0.1%, about 0.5 pH：Divide 6 grades of extractions；Every grade of Solvent quantity is hydrolyzate quality
30%, extractant is n-butanol；30 DEG C of extraction temperature；Every grade of extraction oil phase and raffinate water phase is through filtering and impurity removing；By first
Oil phase after section extraction is rich in resorcinol precipitation process to be entered, and raffinate water phase waits entering next section of processing.
（2）Through step（1）Obtained raffinate water phase uses mass concentration to adjust pH to 7.0 for 30% ammonium hydroxide, is filtered to remove
Impurity is precipitated, filtrate carries out second segment extraction, extracting operation similar step（1）, extractant is n-propyl acetate；By second segment
Oil phase after extraction is rich in m-aminophenol precipitation process to be entered, and raffinate water phase waits entering next section of processing.
（3）Through step（2）Obtained raffinate water phase carries out third section extraction, extracting operation similar step（1）And step
（2）, extractant is hexane；Oil phase after the extraction of third section enters precipitation process and recycles extractant, and raffinate water phase waits entering
Next section of processing.
（4）Through step（3）Obtained raffinate water phase flows in series through activated carbon packed column and is adsorbed, and activated carbon uses coal quality
Charcoal, upper prop flow velocity 30BV/hr, water phase that treated is through chromatogram ration analysis, wherein levels of n-butanol about 25ppm, second
Sour n-propyl content about 10ppm, hexane content are less than 5ppm, can meet the use of hydrolysis complex acid.
Embodiment 3：A kind of post-processing approach of m-phenylene diamine (MPD) hydrolyzate, concrete processing procedure are：
（1）Resorcinol content 8%, m-aminophenol content 4%, m-phenylene diamine (MPD) content are less than in m-phenylene diamine (MPD) hydrolyzate
0.3%, pH is less than 0.6, which is carried out first segment extraction：Divide 5 grades of extractions；Every grade of Solvent quantity is hydrolyzate quality
25%, extractant is n-propyl acetate；25 DEG C of extraction temperature；Every grade of extraction oil phase and raffinate water phase is through filtering and impurity removing；By
Oil phase after first segment extraction is rich in resorcinol precipitation process to be entered, and raffinate water phase waits entering next section of processing.
（2）Through step（1）Obtained raffinate water phase uses mass concentration to adjust pH to 6.7 for 28% ammonium hydroxide, is filtered to remove
Impurity is precipitated, filtrate carries out second segment extraction, extracting operation similar step（1）, extractant is isopropyl acetate；By second segment
Oil phase after extraction is rich in m-aminophenol precipitation process to be entered, and raffinate water phase waits entering next section of processing.
（3）Through step（2）Obtained raffinate water phase, which is adopted, carries out third section extraction, extracting operation similar step（1）And step
（2）, extractant is heptane；Oil phase after the extraction of third section enters precipitation process and recycles extractant, and raffinate water phase waits entering
Next section of processing.
（4）Through step（3）Obtained raffinate water phase flows in series through activated carbon packed column and is adsorbed, and activated carbon uses coal quality
Charcoal, upper prop flow velocity 20BV/hr, water phase that treated through chromatogram ration analysis, wherein n-propyl acetate content about
22ppm, isopropyl acetate ester content about 10ppm, heptane content are less than 10ppm, can meet the use of hydrolysis complex acid.
Embodiment 4：A kind of post-processing approach of p-phenylenediamine hydrolyzate, concrete processing procedure are：
（1）Hydroquinone content 6%, para-aminophenol content 5%, p-phenylenediamine content be about in p-phenylenediamine hydrolyzate
The hydrolyzate is carried out first segment extraction by 0.4%, about 0.2 pH：Divide 3 grades of extractions；Every grade of Solvent quantity is hydrolyzate quality
15%, extractant is isobutyl acetate；15 DEG C of extraction temperature；Every grade of extraction oil phase and raffinate water phase is through filtering and impurity removing；By
Oil phase after first segment extraction is rich in hydroquinone precipitation process to be entered, and raffinate water phase waits entering next section of processing.
（2）Through step（1）Obtained raffinate water phase uses mass concentration to adjust pH to 6.5 for 15% ammonium hydroxide, is filtered to remove
Impurity is precipitated, filtrate carries out second segment extraction, extracting operation similar step（1）, extractant is hexone；By
Oil phase after two-stage extraction is rich in para-aminophenol precipitation process to be entered, and raffinate water phase waits entering next section of processing.
（3）Through step（2）Obtained raffinate water phase carries out third section extraction, extracting operation similar step（1）And step
（2）, extractant is octane；Oil phase after the extraction of third section enters precipitation process and recycles extractant, and raffinate water phase waits entering
Next section of processing.
（4）Through step（3）Obtained raffinate water phase flows in series through activated carbon packed column and is adsorbed, and activated carbon uses shell
Charcoal, upper prop flow velocity 48BV/hr, water phase that treated through chromatogram ration analysis, wherein Sucrose Acetate ester content about
12ppm, hexone content about 32ppm, isooctane content are less than 4ppm, can meet the use of hydrolysis complex acid.
Embodiment 5：A kind of post-processing approach of p-phenylenediamine hydrolyzate, concrete processing procedure are：
（1）Hydroquinone content 3%, para-aminophenol content 8%, p-phenylenediamine content are less than in p-phenylenediamine hydrolyzate
The hydrolyzate is carried out first segment extraction by 0.4%, about 0.5 pH：Divide 8 grades of extractions；Every grade of Solvent quantity is hydrolyzate quality
35%, extractant is pentyl acetate；40 DEG C of extraction temperature；Every grade of extraction oil phase and raffinate water phase is through filtering and impurity removing；By
Oil phase after one-section abstraction is rich in hydroquinone precipitation process to be entered, and raffinate water phase waits entering next section of processing.
（2）Through step（1）Obtained raffinate water phase uses mass concentration to adjust pH to 7.5 for 35% ammonium hydroxide, is filtered to remove
Impurity is precipitated, filtrate carries out second segment extraction, extracting operation similar step（1）, extractant is n-butyl acetate；By second segment
Oil phase after extraction is rich in para-aminophenol precipitation process to be entered, and raffinate water phase waits entering next section of processing.
（3）Through step（2）Obtained raffinate water phase carries out third section extraction, extracting operation similar step（1）And step
（2）, extractant is heptane；Oil phase after the extraction of third section enters precipitation process and recycles extractant, and raffinate water phase waits entering
Next section of processing.
（4）Through step（3）Obtained raffinate water phase flows in series through activated carbon packed column and is adsorbed, and activated carbon is using wooden
Charcoal, upper prop flow velocity 2BV/hr, water phase that treated is through chromatogram ration analysis, wherein pentyl acetate content about 11ppm, second
Sour N-butyl content about 22ppm, heptane content are less than 7ppm, can meet the use of hydrolysis complex acid.
Claims (8)
1. a kind of post-processing approach of phenylenediamine hydrolyzate, the hydrolyzate that benzenediol or amino-phenol are prepared with phenylenediamine hydrolysis are
Process object, it is characterized in that, include the following steps：（1）In the hydrolyzate, benzenediol weight ratio is 1-10%, amino-phenol weight
Amount is than being 1-10%, and phenylenediamine weight ratio is less than 0.5%, pH less than 1；Hydrolyzate is subjected to first segment extraction, divides 3-8 grades of extractions,
Every grade of Solvent quantity is the 15-35% of hydrolyzate quality, and extraction temperature is 15-40 DEG C, every grade of extraction oil phase and raffinate water phase
By filtering out solid impurity, extraction oil phase enters precipitation process rich in benzenediol, and raffinate water phase enters next section of processing；（2）
By step（1）Gained raffinate water phase uses liquefied ammonia or mass concentration to adjust pH to 6.5-7.5 for the ammonium hydroxide of 15-35%, is filtered to remove
Solid impurity is precipitated, filtrate carries out second segment extraction, and it is the 15- of hydrolyzate quality to divide 3-8 grades of extractions, every grade of Solvent quantity
35%, extraction temperature is 15-40 DEG C, and every grade of extraction oil phase and raffinate water phase is by filtering out solid impurity, obtained extraction oil
Mutually enter precipitation process rich in amino-phenol, raffinate water phase enters next section of processing；（3）By step（2）Gained raffinate water phase into
Row third section extracts, and it is the 15-35%, extraction temperature 15-40 of hydrolyzate quality to divide 3-8 grades of extractions, every grade of Solvent quantity
DEG C, for every grade of extraction oil phase and raffinate water phase by filtering out solid impurity, obtained extraction oil phase enters the recycling of precipitation process
Extractant, raffinate water phase enter next section of processing；Extractant is one kind in pentane, hexane, heptane and octane；（4）By step
（3）Gained raffinate water phase carries out activated carbon adsorption decolorization, and activated carbon is loaded using packed column, and raffinate water phase flows in series through work
Property charcoal packed column is adsorbed, and flow velocity 1-50BV/hr, the liquid after absorption meets hydrolysis requirement, is mixed with pure water
Complex acid is carried out, the hydrolysis of phenylenediamine is used for.
2. the post-processing approach of phenylenediamine hydrolyzate according to claim 1, it is characterised in that：Step（1）In, first segment
Extraction divides 4-6 grades of extractions, every grade of Solvent quantity to be the 20-30% of hydrolyzate quality, and extraction temperature is 20-30 DEG C.
3. the post-processing approach of phenylenediamine hydrolyzate according to claim 1, it is characterised in that：Step（2）In, using liquid
Ammonia or the ammonium hydroxide that mass concentration is 25-30% adjust the pH to 6.5-7.0 of raffinate water phase.
4. the post-processing approach of phenylenediamine hydrolyzate according to claim 1, it is characterised in that：Step（1）With（2）In,
Extractant is hexone, n-butanol, n-propyl acetate, isopropyl acetate, n-butyl acetate, isobutyl acetate, second
One or more of sour pentyl ester and Di Iso Propyl Ether.
5. the post-processing approach of phenylenediamine hydrolyzate according to claim 1, it is characterised in that：Step（4）In, activated carbon
For one kind in coconut husk charcoal, fruit shell carbon, carbo lignius or coal quality charcoal；Upper prop flow velocity is 10-30BV/hr.
6. the post-processing approach of phenylenediamine hydrolyzate according to claim 4, it is characterised in that：Step（1）With（2）In,
Extractant is one or more of hexone, n-butyl acetate, isobutyl acetate and pentyl acetate.
7. the post-processing approach of phenylenediamine hydrolyzate according to claim 1, it is characterised in that：Step（3）In, extractant
For one kind in pentane, hexane and heptane.
8. the post-processing approach of phenylenediamine hydrolyzate according to claim 5, it is characterised in that：Step（4）In, activated carbon
For coconut husk charcoal or coal quality charcoal.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3862245A (en) * | 1970-03-10 | 1975-01-21 | Koppers Co Inc | Resorcinol preparation |
| CN101486628A (en) * | 2009-02-24 | 2009-07-22 | 江苏扬农化工集团有限公司 | Method for extracting resorcin from resorcin-containing salt water solution |
| CN102826961A (en) * | 2012-08-14 | 2012-12-19 | 江苏扬农化工集团有限公司 | Cycling treatment method for waste acid produced in production of hydroquinone |
| CN102911018A (en) * | 2011-08-04 | 2013-02-06 | 浙江龙盛化工研究有限公司 | Method for separating phenol-containing organic substances from m-phenylenediamine acidic hydrolysate |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3862245A (en) * | 1970-03-10 | 1975-01-21 | Koppers Co Inc | Resorcinol preparation |
| CN101486628A (en) * | 2009-02-24 | 2009-07-22 | 江苏扬农化工集团有限公司 | Method for extracting resorcin from resorcin-containing salt water solution |
| CN102911018A (en) * | 2011-08-04 | 2013-02-06 | 浙江龙盛化工研究有限公司 | Method for separating phenol-containing organic substances from m-phenylenediamine acidic hydrolysate |
| CN102826961A (en) * | 2012-08-14 | 2012-12-19 | 江苏扬农化工集团有限公司 | Cycling treatment method for waste acid produced in production of hydroquinone |
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