CN104496794B - A kind of naphthalene method phthalic anhydride wastewater reclaims the pre-treating method of fumaric acid - Google Patents
A kind of naphthalene method phthalic anhydride wastewater reclaims the pre-treating method of fumaric acid Download PDFInfo
- Publication number
- CN104496794B CN104496794B CN201410780373.5A CN201410780373A CN104496794B CN 104496794 B CN104496794 B CN 104496794B CN 201410780373 A CN201410780373 A CN 201410780373A CN 104496794 B CN104496794 B CN 104496794B
- Authority
- CN
- China
- Prior art keywords
- phthalic anhydride
- concentration
- naphthalene
- fumaric acid
- anhydride wastewater
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/50—Use of additives, e.g. for stabilisation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Treatment By Sorption (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
The present invention provides a kind of naphthalene method phthalic anhydride wastewater to reclaim the pre-treating method of fumaric acid, comprises the steps: 1) in described waste water, add flocculant, settle, obtain supernatant；2) described supernatant being carried out distillation and concentration, liquid after being concentrated, after concentration, liquid stands a period of time after being cooled to room temperature, and after solid sedimentation, supernatant goes follow-up wastewater treatment.The method that naphthalene method phthalic anhydride wastewater according to embodiments of the present invention processes, its subsequent treatment, activated carbon dosage declines to a great extent.
Description
Technical field
The present invention relates to the method reclaiming fumaric acid from phthalic anhydride wastewater.
Technical background
The raw materials for production of phthalic anhydride are o-Dimethylbenzene or naphthalene, and another raw material is oxygen, in course of reaction, can generate the by-product of the maleic acid of about 3%, and with other by-products.These by-products by Water spray, are phthalic anhydride wastewater in the tail gas tower of phthalic anhydride plant.
With thiourea for catalyst, maleic acid can be isomerized to fumaric acid, is fumaric acid.Fumaric acid as feedstuff or food additive, can have been widely used.But, due in phthalic anhydride wastewater containing other coloring matters, reclaim in fumaric acid process and need this phthalic anhydride wastewater is decoloured.At present, phthalic anhydride wastewater is decoloured by conventional activated carbon.
With naphthalene or be not less than the naphthalene of 30wt% in the phthalic anhydride wastewater of raw material containing coloring matter naphthoquinone, benzo-thiophene etc., these coloring matters are the materials containing multiple double bond conjugation groups, these materials are slightly soluble in water, need to add substantial amounts of activated carbon by after coloring matter absorption, just can produce white fumaric acid, generally needed to be added amounts of activated carbon more than 1%.The Another reason needing big carbon content active is, containing tar-like substance in waste water, to occupy the duct of activated carbon, have impact on adsorption effect.
Summary of the invention
In order to solve the deficiency of activated carbon adsorption phthalic anhydride wastewater decolouring in prior art, the invention provides one and can remove coloring matter and tar-like substance more than 90% in waste water, good decolorizing effect, advantageously reduce subsequent treatment cost, the method improving the pre-treatment of the naphthalene method phthalic anhydride wastewater recovery fumaric acid of fumaric acid recovery purity and the response rate.
The technical solution used in the present invention is: a kind of naphthalene method phthalic anhydride wastewater reclaims the pre-treating method of fumaric acid, comprises the steps: 1) in naphthalene method phthalic anhydride wastewater, add flocculant, carry out flocculating sedimentation, obtain supernatant；2) described supernatant being carried out distillation and concentration, liquid after being concentrated, after concentration, liquid stands after being cooled to room temperature, and after solid sedimentation, supernatant goes subsequent treatment.
Further, described flocculant is cationic-type polyacrylamide, and consumption is the 0.05 ~ 0.5% of naphthalene method phthalic anhydride wastewater weight.
Because the acid number of waste water is significantly high, the polyacrylamide that general selection is non-ionic, but use cationic here.Its main cause is, affects a lot of impurity of fumaric acid color as how quinone is easier to be precipitated out in cationic.The degree of polymerization of polyacrylamide is more high, and effect is more good, but cost is also more high.Here mean molecule quantity polyacrylamide more than 16000 is selected.
Further, described flocculant usage is preferably 0.1 ~ 0.3%.
Further, the time of flocculation sediment is 10 ~ 40 hours.
Further, the time of flocculation sediment is preferably 20 ~ 25 hours.
Further, the method for distillation and concentration is double-effect evaporation, evaporation in vacuo degree 85-105%, waste water boiling point 50-100 DEG C, the sour water concentration 20 ~ 28% after concentration.
Further, the preferred 90-95% of distillation and concentration evaporation in vacuo degree, preferred 50-80 DEG C of waste water boiling point, the sour water concentration after concentration preferably 22 ~ 25%.
Further, time of repose is 30 ~ 100 hours.
Yet further, time of repose is preferably 45 ~ 72 hours.
In the naphthalene method phthalic anhydride wastewater that naphthalene or more than 30wt% naphthalene are raw material, coloring matter is for naphthoquinone etc., it it is the material containing multiple double bond conjugation groups, these materials are slightly soluble in water, simultaneously possibly together with tar-like substance in waste water, add flocculant flocculating sedimentation, coloring matter in waste water and tar can be removed major part, carry out distillation and concentration again, after coloring matter and tar concentration, can part settle from waste water, coal-tar middle oil and coloring matter the content of waste water reduces further, coal-tar middle oil and coloring matter the content of waste water reduces by more than 90%, be conducive to the process of subsequent recovery fumaric acid, reduce activated carbon adsorption consumption.
Accompanying drawing explanation
Fig. 1 is present invention process flow chart.
Detailed description of the invention
Hereinafter, the effect for the treatment of in accordance with the present invention method is described by specific embodiment.Wherein embodiment 1 is comparative example, does not namely carry out the situation of pre-treatment.
Embodiment 2-8:
A kind of naphthalene method phthalic anhydride wastewater reclaims the pre-treating method of fumaric acid, comprises the steps: 1) in naphthalene method phthalic anhydride wastewater, add flocculant, carry out flocculating sedimentation, obtain supernatant；2) described supernatant being carried out distillation and concentration, liquid after being concentrated, after concentration, liquid stands 30-100h after being cooled to room temperature, and after solid sedimentation, supernatant goes subsequent treatment.Flocculant is cationic-type polyacrylamide, and consumption is the 0.05 ~ 0.5% of naphthalene method phthalic anhydride wastewater weight, and the time of flocculation sediment is 10 ~ 40 hours, the method of distillation and concentration is double-effect evaporation, evaporation in vacuo degree 85-105%, waste water boiling point 50-100 DEG C, the sour water concentration 20 ~ 28% after concentration.
The design parameter of table 1. embodiment 1 ~ 8 and treatment effect
As shown above, according to embodiments of the present invention 2 ~ 8 processing method, it is possible to effectively elimination phthalic anhydride wastewater in organic impurities so that in subsequent technique, activated carbon dosage is reduced to less than 0.3% from 1%.
Although the specific embodiment of the present invention is described in detail by the multiple illustrative examples with reference to the present invention, it must be understood that, those skilled in the art can be designed that multiple other improvement and embodiment, these improve and embodiment will drop within spirit and scope.Specifically, within aforementioned open, accompanying drawing and scope of the claims, it is possible to make reasonably deformation in the layout of parts and/or sub-combination layout and improve, without departing from the spirit of the present invention.Except modification and the improvement of parts and/or layout aspect, its scope is defined by the appended claims and the equivalents thereof.
Claims (5)
1. naphthalene method phthalic anhydride wastewater reclaims a pre-treating method for fumaric acid, comprises the steps:
1) adding flocculant in the naphthalene method phthalic anhydride wastewater that more than 30wt% naphthalene is raw material, cationic-type polyacrylamide, consumption is the 0.05～0.5% of naphthalene method phthalic anhydride wastewater weight, carries out flocculating sedimentation, and the time of flocculation sediment is 10～40 hours, obtains supernatant；
2) described supernatant is carried out distillation and concentration, the method of distillation and concentration is double-effect evaporation, evaporation in vacuo degree 85-105%, waste water boiling point 50-100 DEG C, the sour water concentration 20～28% after concentration, liquid after being concentrated, after concentration, liquid stands after being cooled to room temperature, time of repose is 30～100 hours, and after solid sedimentation, supernatant goes subsequent treatment.
2. naphthalene method phthalic anhydride wastewater as claimed in claim 1 reclaims the pre-treating method of fumaric acid, it is characterised in that described flocculant usage is preferably 0.1～0.3%.
3. naphthalene method phthalic anhydride wastewater as claimed in claim 1 reclaims the pre-treating method of fumaric acid, it is characterised in that the time of flocculation sediment is preferably 20～25 hours.
4. naphthalene method phthalic anhydride wastewater as claimed in claim 1 reclaims the pre-treating method of fumaric acid, it is characterised in that the preferred 90-95% of distillation and concentration evaporation in vacuo degree, preferred 50-80 DEG C of waste water boiling point, the sour water concentration after concentration preferably 22～25%.
5. naphthalene method phthalic anhydride wastewater as claimed in claim 1 reclaims the pre-treating method of fumaric acid, it is characterised in that time of repose is preferably 45～72 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410780373.5A CN104496794B (en) | 2014-12-17 | 2014-12-17 | A kind of naphthalene method phthalic anhydride wastewater reclaims the pre-treating method of fumaric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410780373.5A CN104496794B (en) | 2014-12-17 | 2014-12-17 | A kind of naphthalene method phthalic anhydride wastewater reclaims the pre-treating method of fumaric acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104496794A CN104496794A (en) | 2015-04-08 |
| CN104496794B true CN104496794B (en) | 2016-07-06 |
Family
ID=52938269
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410780373.5A Active CN104496794B (en) | 2014-12-17 | 2014-12-17 | A kind of naphthalene method phthalic anhydride wastewater reclaims the pre-treating method of fumaric acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104496794B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028530A (en) * | 2020-09-02 | 2020-12-04 | 安徽鑫固环保股份有限公司 | Method for synthesizing naphthalene water reducer by rectification wastewater of phthalic anhydride prepared by naphthalene method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024608B (en) * | 2007-03-15 | 2011-05-11 | 山东宏信化工股份有限公司 | Process for preparing fumaric acid by spraying acid water to benzene anhydride oxidized tail gas |
-
2014
- 2014-12-17 CN CN201410780373.5A patent/CN104496794B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN104496794A (en) | 2015-04-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Bello et al. | Adsorptive features of banana (Musa paradisiaca) stalk-based activated carbon for malachite green dye removal | |
| CN109336831B (en) | Method for recovering triazine ring from triazine ring wastewater | |
| CN105348154B (en) | The recovery method of sulfosalicylic acid in a kind of Doxycycline production waste liquid | |
| CN105271397A (en) | Production method of titanium dioxide capable of reducing water consumption | |
| CN104496794B (en) | A kind of naphthalene method phthalic anhydride wastewater reclaims the pre-treating method of fumaric acid | |
| CN103318918A (en) | Method for purification and recovery of ammonia gas | |
| CN103242156A (en) | Method for treating a reaction solution containing a long-chain dicarboxylate | |
| CN104592004B (en) | A kind of method of refining long-chain organic acid | |
| CN111018747A (en) | Method for refining guanidine nitrate | |
| CN104962759B (en) | A kind of preparation method of antimony | |
| CN105110515B (en) | A kind of processing method of DSD acid waste water | |
| CN110642707B (en) | Purification production method of low-cost environment-friendly sodium salicylate | |
| CN101054192A (en) | Method of preparing crystal aluminum chloride from circulation fluid bed fly ash | |
| CN104762359A (en) | Recycling process of amoxicillin in enzymatically synthesized amoxicillin mother liquor | |
| CN101550487B (en) | Method for recovering metal platinum from industrial waste | |
| Ma et al. | Optimisation of phosphorus recovery process from biogas slurry using straw-derived biochar coupled with Mg/La oxide as an adsorbent | |
| CN107381877B (en) | Nitromethane high-salinity wastewater treatment method | |
| CN113444845A (en) | Method for refining, detoxifying and producing acetone and butanol by fermentation of molasses | |
| CN104341001A (en) | Method for producing food-grade zinc sulfate with industrial-grade zinc sulfate as raw material | |
| CN103274923A (en) | Method for recycling dehydropregnenolone acetate waste liquor | |
| CN111003840A (en) | Process method for industrially preparing ferrous sulfide and Prussian blue | |
| CN106167326A (en) | A kind of useless acid treatment process | |
| CN101781198B (en) | Technology for recovering mother solution of gallic acid | |
| CN111646638A (en) | Method for deep treatment and desalination of sucralose wastewater | |
| CN107265587A (en) | A kind of many raw material alcohol waste water total nitrogen total phosphorus minimizing technologies |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: No. 18, Zha Nan Road, Taixing Economic Development Zone, Taizhou City, Jiangsu Province Patentee after: Taixing Union Zhongda Chemical Co.,Ltd. Address before: No. 18 Zhanan Road, Economic Development Zone, Taixing City, Taizhou City, Jiangsu Province, 225400 Patentee before: TAIXING UNION ZOND CHEMICALS CO.,LTD. |
|
| CP03 | Change of name, title or address |