CN1087647A - De-solvent method with hot water subsiding - Google Patents
De-solvent method with hot water subsiding Download PDFInfo
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- CN1087647A CN1087647A CN 92107840 CN92107840A CN1087647A CN 1087647 A CN1087647 A CN 1087647A CN 92107840 CN92107840 CN 92107840 CN 92107840 A CN92107840 A CN 92107840A CN 1087647 A CN1087647 A CN 1087647A
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- hot water
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- molecular polymer
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Abstract
A kind of method of macromolecule polymer solution hot water precipitating desolventizing, it is characterized in that macromolecule polymer solution is joined in the hot water that has the former powder of micro-identical high molecular polymer, in the process of hot water precipitating, make high molecular polymer can form uniform powdered granule like this, and solvent removal is reclaimed, do not form the block of glue-like and destroy stable operation.
Description
The present invention relates to the processing method of macromolecule polymer solution desolventizing, particularly the processing method of hot water precipitating desolventizing.
At present, the saccharoid of high molecular polymer is the polymers soln that is obtained containing solvent by polymerization, carry out chemical precipitating then and remove solvent, so not only consume a large amount of solvents, and whether solvent removal totally is one of quality index that influences high molecular polymer, in the post-processed system of desolventizing, be in a kind of state that in a large amount of high molecular polymers, contains a small amount of solvent owing to contain the macromolecule polymer solution of solvent, solvent reduces to hundreds of PPM in the polymer solids product in order to make, even still less, this is a very complicated process, because, high molecular polymer surface desolventizing is too fast, form surface cure, the solvent that is present in high molecular polymer inside just is difficult for removing, and therefore, constantly carry out Surface Renewal to high molecular polymer, make to be present in inner solvent, remove thereby be easy to evaporation owing to the polymer surfaces continual renovation is exposed to the surface.For this reason, current processing method commonly used has following several: 1. adopt screw extrusion press, the high molecular polymer that is in melting is constantly carried out Surface Renewal in screw extrusion press, aspirate the solvent that evaporates with multi-stage vacuum.2. scraper-type film under vacuum vaporizer utilizes scraper plate to bring in constant renewal in the high molecular polymer surface equally, and solvent evaporation is removed.3. spray evaporation becomes powder craft, macromolecule polymer solution atomisation under high speed, forms great specific surface solvent evaporation is removed, and above-mentioned several method is the precision height of requirement mechanical means, etch-proof requirement height.So, cost, facility investment is all very high.4. the technology of precipitating desolventizing, this method is the most suitable when particularly high molecular polymer contains a large amount of solvent, the equipment that is characterized in is simple, reduced investment, it is to utilize the temperature of hot water to be higher than the boiling temperature of solvent, the boiling temperature that perhaps is higher than the azeotrope of water and solvent composition, make the azeotrope evaporation of solvent or water and solvent, remove solvent, in order to increase the specific surface of high molecular polymer, solvent evaporation is removed, so adopt high strength to stir at the hot water desorption device, make polymkeric substance become disperse phase, the final solvent evaporation, it is granular to make polymkeric substance become fine powder, but, in the process that adopts the hot water desolventizing, after solvent reduced to a certain degree, the visco-elasticity of high molecular polymer significantly strengthened, and big drop is difficult for broken, even not broken, and the coalescence between the drop increases, and forms the high molecular polymer of big glue-like, and is bonded on stirring blade and the axle, can not be dispersed into high molecular polymer and drip shape, and can continue coalescence, form bulk viscose glue shape high molecular polymer, make a large amount of solvents that are present in its inside and can not evaporate and remove, the entire operation process can't be carried out, do not reach the specification of quality of product, so, usually in this process, add precipitation agent, as acetone etc., can avoid stirring the granulating difficulty, bring impurity into, increase expense but introduced another solvent, remove solvent if adopt above-mentioned other method to process further again, the complicacy and the cost of heavy industry skill increase substantially more.
The objective of the invention is to overcome above-mentioned weak point, propose a kind ofly to analyse in the process of desolventizing, make macromolecule polymer solution can stably form the drop of high molecular polymer, solvent evaporation is removed and make polymkeric substance become powder at hot water, stable operation reaches the requirement of quality product.
The objective of the invention is to realize by the following technical programs, it is characterized in that macromolecule polymer solution is joined in the hot water that contains the former powder of identical high molecular polymer, the consumption of former powder is the 2-10% of hot water weight, because the former powder of identical high molecular polymer that exists in the hot water plays a kind of effect of granulating seed, under high strength stirs, the macromolecule polymer solution that adds all gather former powder around, form tiny drop, the rapid solvent evaporation that it is surperficial, and by condensation, cooling obtains collecting, polymkeric substance then forms solid high molecular polymer particle that diameter is the 1-2 millimeter and submerged, so can not form the agglomerate of glue-like, and destroy stable operation and solvent can not be removed.The high molecular polymer solids that form are finished product after vacuum-drying, and the content of solvent is lower than 200ppm. in the finished product
Embodiment 1.
The hot water temperature is 80 ℃ in the hot water still, mixing speed is 1500-1600 rev/min, add hot water weight 2% powdery polycarbonate in the hot water still, then, with the polycarbonate dichloromethane solution, concentration is 10-15%, feed rate is 80 milliliters/hour and rises, join in the hot water still, the precipitating granulating, the methylene chloride suction is reclaimed.The precipitating granulating finishes, and keeps water temperature 90 degree above about 1 hour, further removes solvent, and then with solid polycarbonate particulate filter, drying records and contains the amount of residual solvent methylene dichloride in the polycarbonate and be lower than 200ppm.
Embodiment 2.
The former grain weight amount that adds is 10% of a hot water weight, and other condition is identical with embodiment 1, consequently contains the amount of residual solvent methylene dichloride in the polycarbonate and is lower than 200ppm.
Embodiment 3.
The hot water temperature is 80 ℃ in the hot water still, mixing speed is 1500-1600 rev/min, add hot water weight 2% powdery polyphenylene oxide resin (ppo) in the hot water still, then, the polyphenylene oxide toluene that purifying is crossed, concentration is 10-15%, input speed is 80 milliliters/hour and rises that join in the hot water still, precipitating becomes the 1-2mm powder, the solvent toluene suction is reclaimed, after the precipitating, kept water temperature 90 degree above about 1 hour, then with solid polyphenylene oxide particulate filter, drying records and contains amount of residual solvent toluene in the polyphenylene oxide solid and be lower than 200ppm.
Embodiment 4.
The former grain weight amount that adds is 10% of a hot water weight, and other condition is identical with embodiment 3, consequently contains amount of residual solvent toluene in the polyphenylene oxide solid and is lower than 200ppm.
Claims (2)
1, a kind of de-solvent method with hot water subsiding of high atmosphere polymers soln is characterized in that macromolecule polymer solution is joined in the hot water that has the former powder of identical high molecular polymer.
2, method according to claim 1, the consumption that it is characterized in that the former powder of high molecular polymer is the 2-10% of hot water weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92107840 CN1087647A (en) | 1992-12-02 | 1992-12-02 | De-solvent method with hot water subsiding |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92107840 CN1087647A (en) | 1992-12-02 | 1992-12-02 | De-solvent method with hot water subsiding |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1087647A true CN1087647A (en) | 1994-06-08 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92107840 Pending CN1087647A (en) | 1992-12-02 | 1992-12-02 | De-solvent method with hot water subsiding |
Country Status (1)
| Country | Link |
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| CN (1) | CN1087647A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503520B (en) * | 2008-11-13 | 2011-08-31 | 中国蓝星（集团）股份有限公司 | Method for removing solvent by polycarbonate solution aqueous phase precipitation |
| CN102850557A (en) * | 2012-10-16 | 2013-01-02 | 江苏扬农化工集团有限公司 | Preparation method of polycarbonate powder |
-
1992
- 1992-12-02 CN CN 92107840 patent/CN1087647A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101503520B (en) * | 2008-11-13 | 2011-08-31 | 中国蓝星（集团）股份有限公司 | Method for removing solvent by polycarbonate solution aqueous phase precipitation |
| CN102850557A (en) * | 2012-10-16 | 2013-01-02 | 江苏扬农化工集团有限公司 | Preparation method of polycarbonate powder |
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| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |