CN1453273A - Benzene anhydride recovering and refining method from rectified residue - Google Patents
Benzene anhydride recovering and refining method from rectified residue Download PDFInfo
- Publication number
- CN1453273A CN1453273A CN02117249A CN02117249A CN1453273A CN 1453273 A CN1453273 A CN 1453273A CN 02117249 A CN02117249 A CN 02117249A CN 02117249 A CN02117249 A CN 02117249A CN 1453273 A CN1453273 A CN 1453273A
- Authority
- CN
- China
- Prior art keywords
- phthalic anhydride
- residue
- phthalic
- anhydride
- produced
- 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.)
- Granted
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
Landscapes
- Furan Compounds (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention is benzene anhydride recovering and refining method from rectified residue. Exhausted residue containing great amount of benzene anhydride and various impurities, such as high-boiling point matters, earth, sand, etc. is crushed and water dissolved without passing through decoloring with active carbon, and phthalic acid is collected from solution and then dewatered and rectified to obtain refined benzene anhydride. The present invention is one clean production process and has the features of benzene anhydride purity of 30 %, no need of decoloring with active carbon, high benzene anhydride recovering rate up to 95 %, reuse of water as solvent and reaction reagent, etc.
Description
Technical field
The present invention relates to a kind of method that from the rectification residue that phthalic anhydride is produced, reclaims refining phthalic anhydride.
Background technology
The rectification residue of phthalic anhydride production is meant the high boiling material that contains a large amount of phthalic anhydrides of being discharged in the rectifying of naphthalene oxidation style or the production of o xylene oxidation method or is mixed with all kinds of foreign matters such as contaminated phthalic anhydride such as earth, sandstone (abbreviation residue), this class residue accounts for 1～5% of phthalic anhydride output, and phthalic anhydride content is greater than 30% in its residue.The recovery technology rate of recovery in the past is low, recovery is not thorough, seriously polluted.In documents: disclose a kind of method that from the rectification residue that phthalic anhydride is produced, reclaims phthalic anhydride among Span ES.2010425 01 Nov 1989 Appl.3pp.Its major technique content is: the present invention includes with gac and diatomite and handle a kind of ebullient aqueous solution, and then filter and crystallization, under the situation of terephthalic acid or ester existence, adopt a kind of dissolving or water-fast inert solvent to handle, repeat this operating process, cooling obtains quite pure phthalic anhydride and/or cis-butenedioic anhydride.The subject matter that this method exists: according to the example, this patent need add gac and diatomite, and the actual product that obtains not is phthalic anhydride and/or cis-butenedioic anhydride, but corresponding acid.If obtain very pure phthalic anhydride and/or cis-butenedioic anhydride, also must be further processed it.
Summary of the invention:
Technical problem to be solved by this invention provides a kind of phthalic anhydride different from the past and reclaims technology, from the rectification residue that phthalic anhydride is produced, reclaim the method for refining phthalic anhydride, its difference is that it has and reclaims that technology is simple, pollution-free, cost is low, quality product is high, this technology belongs to clearer production technology, all phthalic anhydrides in the recyclable residue.
Technical scheme of the present invention is:
From the rectification residue that phthalic anhydride is produced, reclaim the method for refining phthalic anhydride: be that the residue that contains phthalic anhydride is pulverized, water dissolves, reacts under the condition of heating, make wherein useful component phthalic anhydride and water reaction generate the O-phthalic aqueous acid, utilize its solubility with temperature variation principle greatly, cooling, crystallization, filtration, the dry purity O-phthalic acid crystal preferably that gets, the reduction of dewatering again, rectifying can be made with extra care phthalic anhydride.
The present invention reclaims refining phthalic anhydride from the rectification residue of phthalic anhydride production method is the high boiling material that contains a large amount of phthalic anhydrides of being discharged in the rectifying that naphthalene oxidation style or o xylene oxidation method are produced or is mixed with all kinds of foreign matters such as earth, contaminated phthalic anhydride residue such as sandstone is metered in the reactor after crushed, add quantitative water again, content according to phthalic anhydride in the residue, the add-on of water should be 3～8 times of phthalic anhydride weight in the residue, stir then, heating, solubilizing reaction, temperature of reaction is 70～100 ℃, after treating that solubilizing reaction is finished, with tar, contaminant filter such as superpolymer and silt falls, and wash with hot water, make not contain phthalic anhydride in the filter residue substantially, filter residue goes to the coal works to burn.From reaction solution, collect phthalic acid can directly add in the rectifying tower dewater-reactive distillation once finishes, and deviates from moisture in 90～110 ℃, be lower than in 300 ℃ at the refining phthalic anhydride of overhead collection.
Dewater at rectifying tower-after reactive distillation is finished, still have the residue that contains phthalic anhydride on a small quantity at the bottom of the tower, can join after this residue is concentrated and carry out solubilizing reaction in the raw material residue again.Adopt the whole phthalic anhydrides in the recyclable raw material residue of above-mentioned technology.
Effect of the present invention is:
The present invention has and reclaims that technology is simple, pollution-free, cost is low, quality product is high, and this technology belongs to clearer production technology, all phthalic anhydrides in the recyclable residue.
Characteristics of the present invention:
(a) described phthalic anhydride purity is more than 30%;
(b) needn't add the gac processing of decolouring in the removal process;
(c) the intermediate product phthalic acid directly carries out primary dewatering-reactive distillation and obtains refining phthalic anhydride;
(d) high boiling material returns to mix with the raw material residue and carries out solubilizing reaction again at the bottom of the tower of discharging in the reactive distillation processes, and is higher than 95% with the hot wash filter cake phthalic anhydride rate of recovery;
(e) this method as the water of solvent and reaction reagent can be recycled, safe and reliable, pollution-free, belong to clearer production technology.
Adopt above-mentioned recovery technology, the quality index of gained phthalic anhydride is as follows:
Phthalic anhydride content (PA) 〉=99.74%
Phenylformic acid (BAC)≤0.23%
Cis-butenedioic anhydride (MA)≤0.03%
Fusion colourity≤No. 50 (Pt-Co colorimetric)
Best embodiment:
Embodiment 1: add phthalic anhydride content and be 81% residue 200g in the 2000ml there-necked flask, add 1200ml distilled water, 70～100 ℃ of following stirring reactions 1 hour, after finishing, reaction is incubated filtration, use the hot wash filter cake, cooling filtrate to 10～20 ℃, filter O-phthalic acid crystal 157g, collect above-mentioned crystal for several times, get 200g and carry out rectifying, cat head at first removes water at 102 ℃, after dehydration is finished, in 240～290 ℃, collect the cat head fraction, altogether phthalic anhydride 162g.The phthalic anhydride rate of recovery 78.5%.
Embodiment 2: adding phthalic anhydride content is 81% residue 200g in the 2000ml there-necked flask, residue 12.8g (containing phthalic anhydride 12g) adds filtrated stock 1200ml at the bottom of reaching rectifying tower last time, 70～100 ℃ of following stirring reactions 1 hour, after finishing, reaction is incubated filtration, use the hot wash filter cake, cooling filtrate to 10～20 ℃, filtration drying gets phthalic acid 195.0g, above-mentioned crystal is carried out rectifying, cat head at first removes water at 102 ℃, after dehydration is finished, collects the cat head fraction in 240～290 ℃, altogether phthalic anhydride 158.4g, high boiling material 14.6g at the bottom of the residue rectifying tower.The phthalic anhydride rate of recovery 97.8%.
Claims (2)
1, a kind of method that from the rectification residue that phthalic anhydride is produced, reclaims phthalic anhydride, it is characterized in that: the high boiling material that contains a large amount of phthalic anhydrides of being discharged in the rectifying that naphthalene oxidation style or o xylene oxidation method are produced or be mixed with all kinds of foreign matters such as contaminated phthalic anhydride residue such as earth, sandstone after crushed directly and water carry out solubilizing reaction, the centre needn't be with the gac processing of decolouring, from solution, collect phthalic acid, again it is carried out dehydration reaction rectifying, directly obtain refining phthalic anhydride.
2, the method that from the rectification residue that phthalic anhydride is produced, reclaims phthalic anhydride according to claim 1, it is characterized in that: above-mentioned residue is added entry according to the content of phthalic anhydride wherein, the weight of its water is 3～8 times of phthalic anhydride weight, under 70～100 ℃ temperature, carry out solubilizing reaction, from reaction solution, collect phthalic acid can directly add in the rectifying tower dewater-reactive distillation once finishes, in 90～110 ℃, deviate from moisture, be lower than in 300 ℃ at the refining phthalic anhydride of overhead collection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021172498A CN1261423C (en) | 2002-04-22 | 2002-04-22 | Benzene anhydride recovering and refining method from rectified residue |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021172498A CN1261423C (en) | 2002-04-22 | 2002-04-22 | Benzene anhydride recovering and refining method from rectified residue |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1453273A true CN1453273A (en) | 2003-11-05 |
| CN1261423C CN1261423C (en) | 2006-06-28 |
Family
ID=29257217
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021172498A Expired - Fee Related CN1261423C (en) | 2002-04-22 | 2002-04-22 | Benzene anhydride recovering and refining method from rectified residue |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1261423C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100445211C (en) * | 2004-11-11 | 2008-12-24 | 中国石化上海石油化工股份有限公司 | Waste liquid separating process for tetrahydromethyl phthalic anhydride production process |
| CN100467389C (en) * | 2004-11-11 | 2009-03-11 | 中国石化上海石油化工股份有限公司 | Waste liquid separating process for tetrahydromethyl phthalic anhydride prduction process |
| CN106800545A (en) * | 2015-11-26 | 2017-06-06 | 淳蓝环保投资发展有限公司 | A kind of phthalic anhydride clean preparation method |
| CN117986217A (en) * | 2024-04-03 | 2024-05-07 | 南京化学试剂股份有限公司 | Method for treating high-content phthalic anhydride raw material |
-
2002
- 2002-04-22 CN CNB021172498A patent/CN1261423C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100445211C (en) * | 2004-11-11 | 2008-12-24 | 中国石化上海石油化工股份有限公司 | Waste liquid separating process for tetrahydromethyl phthalic anhydride production process |
| CN100467389C (en) * | 2004-11-11 | 2009-03-11 | 中国石化上海石油化工股份有限公司 | Waste liquid separating process for tetrahydromethyl phthalic anhydride prduction process |
| CN106800545A (en) * | 2015-11-26 | 2017-06-06 | 淳蓝环保投资发展有限公司 | A kind of phthalic anhydride clean preparation method |
| CN117986217A (en) * | 2024-04-03 | 2024-05-07 | 南京化学试剂股份有限公司 | Method for treating high-content phthalic anhydride raw material |
| CN117986217B (en) * | 2024-04-03 | 2024-06-04 | 南京化学试剂股份有限公司 | Phthalic anhydride raw material treatment method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1261423C (en) | 2006-06-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1032132C (en) | Process for preparation of arude terphthalic acid suitable for reduction to prepane purified terephthalic acid | |
| JPH1025266A (en) | Production of high-purity isophthalic acid | |
| CN1724408A (en) | Process for comprihensive using waste water in p-benzene diphenol production | |
| CN102234226A (en) | Method for recovering and purifying terephthalic acid in alkali-minimization waste liquor | |
| CN1261423C (en) | Benzene anhydride recovering and refining method from rectified residue | |
| CN102491575A (en) | Method for performing comprehensive treatment by utilizing waste water from production of ternary monomer | |
| CN106660926A (en) | Process for recovering aromatic monocarboxylic acid | |
| US7402694B2 (en) | Process for removal of benzoic acid from an oxidizer purge stream | |
| JP2004217871A (en) | Method of recovering useful components from dyed polyester fiber | |
| CN101525287B (en) | Method for refining sebacic acid | |
| US4284523A (en) | Minimizing oxygenated aromatic compound content of aqueous solution of reclaimed metal oxidation catalyst | |
| KR101130453B1 (en) | Recovery process of terephthalic acid from contaminated terephthalic acid | |
| CN102092753B (en) | Alcoholization removing method of impurity iron in aluminum sulfate solution | |
| US20070038003A1 (en) | Process for removal of benzoic acid from an oxidizer purge stream | |
| CN101270028A (en) | Purification process of alpha-methylnaphthalene | |
| KR101013489B1 (en) | Recovery of catalysts and aromatic acids from the wastes aromatic acid production plants | |
| CN116120161B (en) | Process for treating rectification residues of 2-ethyl anthraquinone and recovering 2-ethyl anthraquinone | |
| CN1055457C (en) | Refining method of para-tert-butyl benzoic acid | |
| CN114591165B (en) | Method for preparing plasticizer by purifying PTA residues | |
| CN114477666B (en) | Treatment method of piperonal production wastewater | |
| CN1114956A (en) | Extraction of natural guaiacol | |
| RU2083550C1 (en) | Process for preparing terephthalic acid | |
| CN1126730C (en) | Process for separating terephthalic acid from its waste and purifying it | |
| CA2616107A1 (en) | Process for removal of benzoic acid from an oxidizer purge stream | |
| SU925933A1 (en) | Process for producing sodium benzoate |
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 | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |