CN104496794A - Pretreatment method for recovering fumaric acid from naphthalene-process phthalic anhydride wastewater - Google Patents
Pretreatment method for recovering fumaric acid from naphthalene-process phthalic anhydride wastewater Download PDFInfo
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- CN104496794A CN104496794A CN201410780373.5A CN201410780373A CN104496794A CN 104496794 A CN104496794 A CN 104496794A CN 201410780373 A CN201410780373 A CN 201410780373A CN 104496794 A CN104496794 A CN 104496794A
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- phthalic anhydride
- fumaric acid
- reclaims
- wastewater
- naphthalene
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- 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
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- 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
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- 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
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- 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 invention provides a pretreatment method for recovering fumaric acid from naphthalene-process phthalic anhydride wastewater, which comprises the following steps: 1) adding a flocculant into the wastewater, and settling to obtain a supernate; and 2) carrying out distillation concentration on the supernate to obtain a concentrated solution, cooling the concentrated solution to normal temperature, standing for some time to settle the solid, and sending the supernate to the subsequent wastewater treatment process. The method provided by the embodiment of the invention greatly lowers the activated carbon consumption in the subsequent treatment.
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-Xylol or naphthalene, and another raw material is oxygen, in reaction process, 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.
Take thiocarbamide as catalyzer, maleic acid can turn to FUMARIC ACID TECH GRADE by isomery, is fumaric acid.Fumaric acid as feed or foodstuff additive, can have been widely used.But, owing to containing other coloring matters in phthalic anhydride wastewater, reclaim in fumaric acid process and need to decolour to this phthalic anhydride wastewater.At present, conventional activated carbon decolours to phthalic anhydride wastewater.
With naphthalene or in being not less than phthalic anhydride wastewater that the naphthalene of 30wt% is raw material containing coloring matter naphthoquinones, benzo-thiophene etc., these coloring matters are the materials containing multiple double bond conjugation group, these materials are slightly soluble in water, need to add a large amount of gacs by after coloring matter absorption, just can produce white fumaric acid, generally need to add amounts of activated carbon more than 1%.The Another reason of large carbon content active is needed to be, containing tar-like substance in waste water, occupy the duct of gac, have impact on adsorption effect.
Summary of the invention
In order to solve the deficiency of charcoal absorption 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, be conducive to reducing subsequent treatment cost, improve the method that fumaric acid reclaims the pre-treatment of the naphthalene method phthalic anhydride wastewater recovery fumaric acid of purity and the rate of recovery.
The technical solution used in the present invention is: a kind of naphthalene method phthalic anhydride wastewater reclaims the pre-treating process of fumaric acid, comprises the steps: 1) in naphthalene method phthalic anhydride wastewater, add flocculation agent, carry out flocculating settling, obtain supernatant liquor; 2) carry out distillation and concentration to described supernatant liquor, obtain concentrated rear liquid, after concentrated, liquid leaves standstill after being cooled to normal temperature, and after solid settlement, supernatant liquor goes subsequent disposal.
Further, described flocculation agent is cationic-type polyacrylamide, and consumption is 0.05 ~ 0.5% of naphthalene method phthalic anhydride wastewater weight.
Because the acid number of waste water is very high, generally select the polyacrylamide of non-ionic type, but here with cationic.Its major cause is, affects a lot of impurity of fumaric acid color as how quinone is more easily precipitated out cationic.The polymerization degree of polyacrylamide is higher, and effect is better, but cost is also higher.Here the polyacrylamide of molecular-weight average more than 16000 will be 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 concentrated.
Further, the preferred 90-95% of distillation and concentration evaporation in vacuo degree, the preferred 50-80 DEG C of waste water boiling point, the sour water concentration after concentrated preferably 22 ~ 25%.
Further, time of repose is 30 ~ 100 hours.
Again further, time of repose is preferably 45 ~ 72 hours.
In the naphthalene method phthalic anhydride wastewater being raw material with naphthalene or more than 30wt% naphthalene, coloring matter is for naphthoquinones etc., it is the material containing multiple double bond conjugation group, these materials are slightly soluble in water, also contain tar-like substance in waste water simultaneously, add flocculation agent flocculating settling, coloring matter in waste water and tar can be removed major part, carry out distillation and concentration again, after coloring matter and tar concentrate, can part settle from waste water, waste water is coal-tar middle oil to be reduced further with content that is coloring matter, waste water content that is coal-tar middle oil and coloring matter 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 schema.
Embodiment
Below, 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:
Naphthalene method phthalic anhydride wastewater reclaims a pre-treating process for fumaric acid, comprises the steps: 1) in naphthalene method phthalic anhydride wastewater, add flocculation agent, carry out flocculating settling, obtain supernatant liquor; 2) carry out distillation and concentration to described supernatant liquor, obtain concentrated rear liquid, after concentrated, liquid leaves standstill 30-100h after being cooled to normal temperature, and after solid settlement, supernatant liquor goes subsequent disposal.Flocculation agent is cationic-type polyacrylamide, and consumption is 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 concentrated.
The design parameter of table 1. embodiment 1 ~ 8 and treatment effect
As shown above, according to the treatment process of the embodiment of the present invention 2 ~ 8, effectively can remove the organic impurity in phthalic anhydride wastewater, make activated carbon dosage in subsequent technique be reduced to less than 0.3% from 1%.
Although be described in detail the specific embodiment of the present invention with reference to multiple illustrative examples of the present invention, but it must be understood that, those skilled in the art can design multiple other improvement and embodiment, these improve and embodiment will drop within spirit and scope.Specifically, within the scope of aforementioned open, accompanying drawing and claim, can in the layout of component and/or sub-combination layout, make reasonably distortion and improve, and spirit of the present invention can not be departed from.Except modification and the improvement of component and/or layout aspect, its scope is by claims and equivalents thereof.
Claims (9)
1. naphthalene method phthalic anhydride wastewater reclaims a pre-treating process for fumaric acid, comprises the steps:
1) in naphthalene method phthalic anhydride wastewater, add flocculation agent, carry out flocculating settling, obtain supernatant liquor;
2) carry out distillation and concentration to described supernatant liquor, obtain concentrated rear liquid, after concentrated, liquid leaves standstill after being cooled to normal temperature, and after solid settlement, supernatant liquor goes subsequent disposal.
2. a kind of naphthalene method phthalic anhydride wastewater as claimed in claim 1 reclaims the pre-treating process of fumaric acid, and it is characterized in that, described flocculation agent is cationic-type polyacrylamide, and consumption is 0.05 ~ 0.5% of naphthalene method phthalic anhydride wastewater weight.
3. a kind of naphthalene method phthalic anhydride wastewater as claimed in claim 2 reclaims the pre-treating process of fumaric acid, and it is characterized in that, described flocculant usage is preferably 0.1 ~ 0.3%.
4. a kind of naphthalene method phthalic anhydride wastewater as claimed in claim 1 reclaims the pre-treating process of fumaric acid, and it is characterized in that, the time of flocculation sediment is 10 ~ 40 hours.
5. a kind of naphthalene method phthalic anhydride wastewater as claimed in claim 4 reclaims the pre-treating process of fumaric acid, and it is characterized in that, the time of flocculation sediment is preferably 20 ~ 25 hours.
6. a kind of naphthalene method phthalic anhydride wastewater as claimed in claim 1 reclaims the pre-treating process of fumaric acid, and it is characterized in that, 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 concentrated.
7. a kind of naphthalene method phthalic anhydride wastewater as claimed in claim 6 reclaims the pre-treating process of fumaric acid, it is characterized in that, the preferred 90-95% of distillation and concentration evaporation in vacuo degree, the preferred 50-80 DEG C of waste water boiling point, the sour water concentration after concentrated preferably 22 ~ 25%.
8. a kind of naphthalene method phthalic anhydride wastewater as claimed in claim 1 reclaims the pre-treating process of fumaric acid, and it is characterized in that, time of repose is 30 ~ 100 hours.
9. a kind of naphthalene method phthalic anhydride wastewater as claimed in claim 8 reclaims the pre-treating process of fumaric acid, and it is characterized in that, time of repose is preferably 45 ~ 72 hours.
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|---|---|---|---|
| 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 |
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| 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 |
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| CN104496794B CN104496794B (en) | 2016-07-06 |
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Cited By (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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024608A (en) * | 2007-03-15 | 2007-08-29 | 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 |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024608A (en) * | 2007-03-15 | 2007-08-29 | 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 |
Non-Patent Citations (1)
| Title |
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| 潘万贵等: "絮凝剂絮凝效果浅析", 《浙江化工》 * |
Cited By (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 |
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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. |
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