CN1261423C - Method for recovering refined phthalic anhydride from rectification residue produced from phthalic anhydride - Google Patents
Method for recovering refined phthalic anhydride from rectification residue produced from phthalic anhydride Download PDFInfo
- Publication number
- CN1261423C CN1261423C CNB021172498A CN02117249A CN1261423C CN 1261423 C CN1261423 C CN 1261423C CN B021172498 A CNB021172498 A CN B021172498A CN 02117249 A CN02117249 A CN 02117249A CN 1261423 C CN1261423 C CN 1261423C
- Authority
- CN
- China
- Prior art keywords
- phthalic anhydride
- residue
- rectification
- phthalic
- reaction
- 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.)
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Links
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 title claims abstract description 67
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract 6
- 238000004090 dissolution Methods 0.000 claims abstract 4
- 238000004042 decolorization Methods 0.000 claims abstract 3
- 239000012295 chemical reaction liquid Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 11
- 238000011084 recovery Methods 0.000 abstract description 10
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 abstract description 6
- 238000009835 boiling Methods 0.000 abstract description 6
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 abstract description 4
- 239000012065 filter cake Substances 0.000 abstract description 4
- 239000000047 product Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000013067 intermediate product Substances 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract 3
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000011499 joint compound Substances 0.000 abstract 1
- 229940078552 o-xylene Drugs 0.000 abstract 1
- 239000004576 sand Substances 0.000 abstract 1
- 239000004575 stone Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 12
- 238000007670 refining Methods 0.000 description 7
- 241000282326 Felis catus Species 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000066 reactive distillation Methods 0.000 description 4
- 230000003381 solubilizing effect Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000008096 xylene Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- -1 earth Chemical class 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 239000012442 inert solvent Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
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 relates to a method for recovering phthalic anhydride form the rectification residue of phthalic anhydride production. A high-boiling substance comprising a great amount of phthalic anhydride or polluted phthalic anhydride residue comprising various foreign substances, such as mud, sand, stone, etc., exhausted from the rectification process of naphthalene oxidation method production or o-xylene oxidation method production takes part in dissolution reaction with water directly after being crushed, and decolorization processing with activated carbon is not needed; phthalic acid is collected from solution, and refined phthalic anhydride is obtained directly after dehydration reaction and rectification. The present invention has the advantages of simple recovering process, no pollution, low cost, high product quality and recovery of all phthalic anhydride in the residue. The technique of the present invention belongs to a clean production technique, which is characterized in that the purity of the phthalic anhydride is more than 30 %; no activated carbon needs adding to carry out decolorization processing in the process of recovery; the refined phthalic anhydride can be obtained directly after an intermediate product, phthalic acid, is dehydrated and rectified; a tower bottom high-boiling substance exhausted from a reaction rectification process is returned to be mixed with raw material residue to carry out the dissolution reaction again, a filter cake is washed by hot water, and the recovery ratio of the phthalic anhydride is higher than 95%. Water used as solvent and reaction agents in the method can be used circularly, and the method which belongs to the clean production technique has the advantages of safety, reliability and no pollution.
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)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021172498A CN1261423C (en) | 2002-04-22 | 2002-04-22 | Method for recovering refined phthalic anhydride from rectification residue produced from phthalic anhydride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021172498A CN1261423C (en) | 2002-04-22 | 2002-04-22 | Method for recovering refined phthalic anhydride from rectification residue produced from phthalic anhydride |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1453273A CN1453273A (en) | 2003-11-05 |
| CN1261423C true CN1261423C (en) | 2006-06-28 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021172498A Expired - Fee Related CN1261423C (en) | 2002-04-22 | 2002-04-22 | Method for recovering refined phthalic anhydride from rectification residue produced from phthalic anhydride |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1261423C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100467389C (en) * | 2004-11-11 | 2009-03-11 | 中国石化上海石油化工股份有限公司 | A kind of separation method of waste liquid in the production process of methyltetrahydrophthalic anhydride |
| CN100445211C (en) * | 2004-11-11 | 2008-12-24 | 中国石化上海石油化工股份有限公司 | Method for separating waste liquid in the production process of methyltetrahydrophthalic anhydride |
| 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 |
| 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 |
-
2002
- 2002-04-22 CN CNB021172498A patent/CN1261423C/en not_active Expired - Fee Related
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| Publication number | Publication date |
|---|---|
| CN1453273A (en) | 2003-11-05 |
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