CN1673107A - Recovering process of polyester dyeing modified SIPM waste water - Google Patents
Recovering process of polyester dyeing modified SIPM waste water Download PDFInfo
- Publication number
- CN1673107A CN1673107A CN 200510037975 CN200510037975A CN1673107A CN 1673107 A CN1673107 A CN 1673107A CN 200510037975 CN200510037975 CN 200510037975 CN 200510037975 A CN200510037975 A CN 200510037975A CN 1673107 A CN1673107 A CN 1673107A
- Authority
- CN
- China
- Prior art keywords
- sipm
- waste water
- polyester dyeing
- class
- dyeing modified
- 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.)
- Pending
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention is recovering process of polyester dyeing modifier SIPM from waste water. Waste water with polyester dyeing modifier SIPM is adsorbed with crosslinking resin, and SIPM and similar matter desorbed from the crosslinking resin are treated through three-effect distillation, crystallizatin, refining, drying, acidification, esterification and refining to obtain SIPM. The said process can recover SIPM from the waste water while eliminating COD from waste water.
Description
Technical field:
The present invention relates to handle the reuse technology of material, particularly polyester the 3rd monomer waste water reclaiming is handled the conversion and the deep process technology of material.
Background technology:
Estrodur dyeing modifier the 3rd monomer SIPM is saltoutd and the aftertreatment multiple working procedure produces through sulfonation, esterification, neutralization by m-phthalic acid, it will carry out solid-liquid separation after neutralization is saltoutd, solids carries out the product impurity removal and purification, produce finished product SIPM, liquid then will be handled as waste water, bibliographical information three monomer salify waste water are handled through methods such as biochemistry with the alkali neutralization after adopt reclaiming methyl alcohol again, or through the extraction process extraction separation again through biochemical treatment.Because COD content height in the waste water, and need to consume a large amount of alkali, thereby processing costs is higher, comprises that state three monomer manufacturing enterprises such as Japan, the U.S. all pay a large amount of human and material resources for this reason, and does not find good improvement method, part enterprise stops production for this reason.
Summary of the invention:
The object of the invention is to invent the recovery technology that reclaims a kind of polyester dyeing modified SIPM waste water of polyester dyeing modified SIPM from polyester dyeing modified SIPM waste water.
Technological process of the present invention is: polyester dyeing modified SIPM waste water is adsorbed by cross-linked resin, the class SIPM material that desorption from cross-linked resin goes out,, isolate class SIPM through triple effect distillation, crystallization, refining, dry, with class SIPM acidifying, esterification, be refined into SIPM again.
The present invention reclaims class SIPM earlier from three monomer waste water, isolate class SIPM through desorption liquid after distillation, crystallization, drying, and with its acidifying, esterification, be refined into SIPM.Not only the COD clearance is up to more than 92%, and also recyclablely from 1000kg three monomer waste water obtains about 30 to 50kgSIPM, and product recovery rate reaches 90%, and having realized turns waste into wealth, and has considerable economic and social benefit.
The present invention adopts free SO
3 -Concentration is 30～50% oleums, under 120～200 ℃ of temperature class SIPM is carried out acidifying; Adopt methyl alcohol, under 60～90 ℃ of temperature, the acidifying material is carried out esterification; Adopt continuous treating, dynamic crystallization 4～8 hours.
The temperature of above-mentioned dynamic crystallization is at normal temperature to 60 ℃, and stir speed (S.S.) is 10～40 rev/mins.
The present invention can reclaim methyl alcohol earlier earlier again through absorption, desorption from waste water, reclaim class SIPM; Also can adsorb earlier, behind the desorption class SIPM, reclaim methyl alcohol again.
The methyl alcohol that reclaims can be used in the esterification technique of back, can further reduce production costs.
Specific embodiment
Example one:
1,1000kg three monomer waste water is warming up to 70～110 ℃, reclaims and obtain 30-50kg methyl alcohol, residual solution by NDA-7 macropore superhigh cross-linking resin absorption, again through 500～1000kg water desorption, is obtained class SIPM mixed solution.
2, class SIPM mixed solution is carried out triple effect distillation, Crystallization Separation, refining, dry, obtain purified class SIPM.
3, the free SO of preparation
3 -Concentration is 30～50% middle concentration H
2SO
4SO
3, stand-by.
4, acidification reaction:
Get concentration H among 100kg class SIPM and the 100～200kg
2SO
4SO
3, under 120～200 ℃ of temperature, reacted 2～8 hours, obtain the acidifying material.
5, esterification:
The acidifying material put to esterifying kettle be cooled to below 90 ℃, drip 100～200kg methyl alcohol, 60～90 ℃ of holding temperatures, 2～4 hours reaction times, the esterification material.
6, refining:
1 part of esterification material adds 2～5 parts of deionized waters (or recrystallization mother liquor water), under 80～100 ℃, dissolves through strong interchanger (or still formula gap), and adsorbs and secondary filter through decolorizing with activated carbon, product is made with extra care (regulated PH to 6～7, add an amount of H
2O
2, AC etc.), refined liquid.
7, crystallization:
To make with extra care filtrate continuous crystallisation in 1000～10000L glassed steel reaction vessels, when feed temperature is reduced to about 60 ℃, regulate mixing speed to 10～40 rev/min, and form to guarantee the crystallization nucleus, and keep the quiet hour more than 4 hours, guarantee that crystalline grows up.
8, finished product:
Obtain 30～50kg polyester dyeing modified SIPM crystalline product from 1000kg three monomer waste water reclamation at last.
Example two:
1,1000kg three monomer waste water are passed through NDA-7 macropore superhigh cross-linking resin absorption, the residual solution that will pass through is warming up to 70～110 ℃, reclaims to obtain 30-50kg methyl alcohol.NDA-7 macropore superhigh cross-linking resin through 500～1000kg water desorption, is obtained class SIPM mixed solution.
2, class SIPM mixed solution is carried out triple effect distillation, Crystallization Separation, refining, dry, obtain purified class SIPM.
3, the free SO of preparation
3 -Concentration is 30～50% middle concentration H
2SO
4SO
3, stand-by.
4, acidification reaction:
Get concentration H among 100kg class SIPM and the 100～200kg
2SO
4SO
3, under 120～200 ℃ of temperature, reacted 2～8 hours, obtain the acidifying material.
5, esterification:
The acidifying material put to esterifying kettle be cooled to below 90 ℃, drip 100～200kg methyl alcohol, 60～90 ℃ of holding temperatures, 2～4 hours reaction times, the esterification material.
6, refining:
1 part of esterification material adds 2～5 parts of deionized waters (or recrystallization mother liquor water), under 80～100 ℃, dissolves through strong interchanger (or still formula gap), and adsorbs and secondary filter through decolorizing with activated carbon, product is made with extra care (regulated PH to 6～7, add an amount of H
2O
2, AC etc.), refined liquid.
7, crystallization:
To make with extra care filtrate continuous crystallisation in 1000～10000L glassed steel reaction vessels, when feed temperature is reduced to about 60 ℃, regulate mixing speed to 10～40 rev/min, and form to guarantee the crystallization nucleus, and keep the quiet hour more than 4 hours, guarantee that crystalline grows up.
8, finished product:
Obtain 30～50kg polyester dyeing modified SIPM crystalline product from 1000kg three monomer waste water reclamation at last.
Claims (7)
1, a kind of recovery technology of polyester dyeing modified SIPM waste water, it is characterized in that polyester dyeing modified SIPM waste water is adsorbed by cross-linked resin, the class SIPM material that desorption from cross-linked resin is gone out, through triple effect distillation, crystallization, refining, dry, isolate class SIPM, with class SIPM acidifying, esterification, be refined into SIPM again.
2,, it is characterized in that adopting free SO according to the recovery technology of the described polyester dyeing modified SIPM waste water of claim 1
3 -Concentration is 30～50% oleums, under 120～200 ℃ of temperature class SIPM is carried out acidifying.
3, according to the recovery technology of the described polyester dyeing modified SIPM waste water of claim 2, it is characterized in that adopting methyl alcohol, under 60～90 ℃ of temperature, the acidifying material is carried out esterification.
4, according to the recovery technology of the described polyester dyeing modified SIPM waste water of claim 3, it is characterized in that adopting continuous treating, dynamic crystallization 4～8 hours.
5, according to the recovery technology of the described polyester dyeing modified SIPM waste water of claim 4, the temperature that it is characterized in that dynamic crystallization is at normal temperature to 60 ℃, and stir speed (S.S.) is 10～40 rev/mins.
According to the recovery technology of the described polyester dyeing modified SIPM waste water of claim 1, it is characterized in that before absorption that 6, reclaim methyl alcohol from waste water earlier, absorption, desorption obtain class SIPM again.
7, according to the recovery technology of the described polyester dyeing modified SIPM waste water of claim 1, it is characterized in that reclaiming class SIPM through cross-linked resin absorption, desorption earlier, its mother liquor reclaims methyl alcohol again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510037975 CN1673107A (en) | 2005-03-07 | 2005-03-07 | Recovering process of polyester dyeing modified SIPM waste water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510037975 CN1673107A (en) | 2005-03-07 | 2005-03-07 | Recovering process of polyester dyeing modified SIPM waste water |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1673107A true CN1673107A (en) | 2005-09-28 |
Family
ID=35045923
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510037975 Pending CN1673107A (en) | 2005-03-07 | 2005-03-07 | Recovering process of polyester dyeing modified SIPM waste water |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1673107A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100390082C (en) * | 2006-03-06 | 2008-05-28 | 南京大学 | Treatment and resource-reclaiming process for waste water from production of dimethyl isophthalate-5-sulfonic acid |
| CN102285697A (en) * | 2011-06-08 | 2011-12-21 | 南京工业大学 | Process for recycling waste water from unsaturated polyester resin industry |
| CN102849883A (en) * | 2011-06-30 | 2013-01-02 | 山东科技职业学院 | Technology for treating SIPM waste water recovered material |
| CN109608366A (en) * | 2018-12-18 | 2019-04-12 | 泰山医学院 | A kind of production method for improving the synthesis of three monomers and using dimethyl isophthalate -5- sulfonic acid yield and purity |
-
2005
- 2005-03-07 CN CN 200510037975 patent/CN1673107A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100390082C (en) * | 2006-03-06 | 2008-05-28 | 南京大学 | Treatment and resource-reclaiming process for waste water from production of dimethyl isophthalate-5-sulfonic acid |
| CN102285697A (en) * | 2011-06-08 | 2011-12-21 | 南京工业大学 | Process for recycling waste water from unsaturated polyester resin industry |
| CN102285697B (en) * | 2011-06-08 | 2013-02-06 | 南京工业大学 | Process for recycling waste water from unsaturated polyester resin industry |
| CN102849883A (en) * | 2011-06-30 | 2013-01-02 | 山东科技职业学院 | Technology for treating SIPM waste water recovered material |
| CN109608366A (en) * | 2018-12-18 | 2019-04-12 | 泰山医学院 | A kind of production method for improving the synthesis of three monomers and using dimethyl isophthalate -5- sulfonic acid yield and purity |
| CN109608366B (en) * | 2018-12-18 | 2021-06-22 | 山东第一医科大学(山东省医学科学院) | Production method for improving yield and purity of m-phthalic acid dimethyl ester-5-sulfonic acid for three-monomer synthesis |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1153754C (en) | Production of aromatic polycarboxylic acids | |
| CN102583951B (en) | Acid lixiviation based recycling treatment method of aluminum circulating coagulation sludge | |
| WO2011052824A1 (en) | Process for economically manufacturing xylose from hydrolysate using electrodialysis and direct recovery method | |
| CN103979730A (en) | Method for purifying penicillin production waste liquid and recycling sodium sulfate | |
| CN1056650C (en) | Natamycin recovery | |
| US20220259549A1 (en) | Method for Separating Biomass from Solid Fermentation Product | |
| CN102234226A (en) | Method for recovering and purifying terephthalic acid in alkali-minimization waste liquor | |
| CN1673107A (en) | Recovering process of polyester dyeing modified SIPM waste water | |
| CN1221510C (en) | Refining method for long-chain biatomic acid | |
| CN112079364B (en) | Method for recycling fluorine-and iodine-containing waste material resources | |
| CN1317263C (en) | Process for producing SIPA using polyester dyeing modifier SIPM waste water as raw material | |
| CN111392763B (en) | Process for separating and recovering zinc-magnesium sulfate double salt from sulfate solution and application | |
| CN1537816A (en) | Treatment of waste water in producing isophthalic acid dicarbomethoxy-5-sodium sulphonate and its resource utilization method | |
| CN1197772C (en) | Method for qualifying industrial ammonium chloride products | |
| CN1207212C (en) | Production of potassium containing chemical products from waste liquid of molasses alcohol production | |
| CN103254102B (en) | A kind of method of purifying acrylamide alkyl sulfonic acid | |
| CN113371912A (en) | Magnesium sulfate crystallization separation process in CLT acid high-salinity wastewater | |
| CN1752032A (en) | Treatment and recovery technology for mixed acid from industrial waste water 3,3-dichlorobenzidine hydrochloride | |
| CN112694397B (en) | Method for purifying 2, 6-naphthalenedicarboxylic acid | |
| CN1810663A (en) | Treating process of effluent from N-acetanilide production | |
| CN113563416B (en) | Treatment method of dipeptide mother liquor and application of dipeptide mother liquor in dipeptide production process | |
| CN111848393B (en) | Treatment method of wastewater from gallic acid and propyl gallate production | |
| CN1012954B (en) | Process for separating residue from industrial p-phthalic acid | |
| CN113135845A (en) | Method for extracting regenerated p-toluenesulfonic acid from doxycycline hydrochloride production wastewater | |
| CN1288884A (en) | Glycine purifying and closed production process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |