CN102964584B - Purification method of crude polycarbonate solution - Google Patents
Purification method of crude polycarbonate solution Download PDFInfo
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Abstract
The invention relates to a purification method of crude polycarbonate solution prepared by an interfacial polymerization method. The purification method comprises the following steps: firstly, preparing initially-purified polycarbonate solution by conventional washing and separating technology; secondarily, carrying out flashing one or plurality of times to remove trace moisture in the polycarbonate solution; and thirdly, filtering to separate out salt impurities, so as to obtain the high-purity polycarbonate solution. According to the purification method, the characteristic of azeotropy between the water and the solution is fully utilized, and flashing is carried out one or the plurality of times to realize filtering, so that the residual impurities in the polycarbonate solution can be greatly reduced, the moisture content in the solution can be reduced to less than 0.1wt% at last, and the sodium chloride residual in the obtained polycarbonate product is less than 100ppb, and therefore, the yellowness index and haze of the product are reduced, and the quality of the product is improved.
Description
Technical field
The present invention relates to the purification process of crude polycarbonate solution prepared by a kind of interface polycondensation.
Background technology
It is be dissolved in by bis-phenol in the basic metal aqueous solution that interface polycondensation produces polycarbonate technique, phosgene in the solvent (being generally methylene dichloride or chlorobenzene) dissolved each other with polycarbonate with the form of its an alkali metal salt and being dissolved in carries out interfacial polycondensation and reacts and prepare macromolecule resin, but in this process also can there is hydrolysis and alkaline hydrolysis side reaction in phosgene, generates a large amount of carbonate and chlorate simultaneously.Common technique is carried out being separated obtaining crude polycarbonate solution with the aqueous phase of residual monomer with saliferous by the polycarbonate organic phase solution of gained, and coarse polycarbonate passes through washing purifying again and desolvation obtains polycarbonate resin.
Usually in interfacial polycondensation reaction process, because water and solvent exist certain mutual solubility in fact, such as at 25 DEG C, the solubleness of water in methylene dichloride is about 0.18%, the solubleness of methylene dichloride in water is about 1.32%, therefore at the end of interfacial polycondensation reaction, after containing the organic phase of polycarbonate and the aqueous phase separation of saliferous and residual monomer, at least can remain the water of the solubleness that reaches capacity in the polycarbonate solution obtained, the water of these trace can bring organic phase into salt again.After the organic phase containing polycarbonate being separated from aqueous phase after General reactions terminates, in order to remove impurity contained in organic phase, need to adopt aqueous phase clear liquid repetitive scrubbing, more above-mentioned organic phase is separated with aqueous phase mixing solutions the polycarbonate solution obtaining purifying.Washing process needs multistep to wash usually, but effectively cannot reduce the residual moisture content in organic phase, and the salt content of final residue is still higher.In addition, for improving moisture content elute effect in organic phase, the measure improving separation degree usually also can be adopted to improve, and this can cause residual a small amount of polycarbonate in aqueous phase, affects subsequent disposal.
In the purification process of the crude polycarbonate solution that prior art is prepared about interface polycondensation, main employing washs separating technology.Adopt the combination of plate decanter and coalescer and whizzer as separator in Chinese patent CN1461322, two step washings carry out purifying organic phase, and in final organic phase solution, water ratio is 0.5wt%, and aqueous phase remains polycarbonate 0.09wt%.Adopt mixing tank in upright arrangement and coalescing separator to carry out purification of crude polycarbonate solution in Chinese patent CN1648153A, the water ratio in final organic phase solution is greater than 0.2wt%.Give in US Patent No. 5260418 and adopt centrifugal separation process purification of crude polycarbonate solution, in final organic phase solution, water ratio is 0.2wt%, and in polycarbonate resin, sodium ion is residual is less than 1ppm.Carry out purification of crude polycarbonate solution by controlling emulsion structure in US Patent No. 6384185, the water ratio in final organic phase solution is 0.2wt%.Adopt the water suction of fibrous packing in US Patent No. 4316009, hydrophobic nature carrys out separating, washing aqueous phase, in final organic phase solution, water ratio is between 0.16 ~ 0.6wt%.
In above-mentioned traditional coarse polycarbonate purifying process, generally adopt washing separating technology, in the polycarbonate solution after final purifying, water ratio is still at about 0.2wt%, and obtained product salt residual quantity is higher.
Summary of the invention
Technical problem to be solved by this invention is to provide the purification process of crude polycarbonate solution prepared by a kind of interface polycondensation that can effectively improve moisture content and salt clearance.The present invention significantly can not only reduce the water ratio in polycarbonate solution, effectively can also reduce the salt impurities left in product, improve refining effect, thus effectively prevent in subsequent technique process moisture content to the hydrolytic side reactions of polycarbonate resin and oxidation inhibitor, improve product purity, improving product quality simultaneously.
For solving the problems of the technologies described above, the present invention utilizes the feature of solvent in polycarbonate solution and water azeotropic, conventional washing separation and flash distillation is adopted to filter the technique combined, utilize the moisture content in flash process reduction polycarbonate solution, further employing filtration process removes the salt of precipitation, finally obtains highly purified polycarbonate solution.
The invention provides the purification process of crude polycarbonate solution prepared by a kind of interface polycondensation, described method comprises the steps:
A) in described crude polycarbonate solution, add pure water and be mixed to get organic phase and aqueous phase, be then separated the organic phase polycarbonate solution a that removing aqueous phase obtains preliminary purification;
B) flash distillation removes step and a) accounts for the solvent of solvent total amount 5 ~ 70wt% in gained polycarbonate solution a,
Obtain the polycarbonate solution b after desolventizing;
C) to step b) add into step b in polycarbonate solution b after desolventizing) in the solvent of desolvation amount 20 ~ 120wt% dilute, obtain polycarbonate solution c ', then flash distillation removes the solvent accounting for solvent total amount 5 ~ 70wt% in described polycarbonate solution c ', obtains polycarbonate solution c ";
D) by step c) in obtained polycarbonate solution c " adopt the metre filter of < 10 μm, obtain highly purified polycarbonate solution d, obtain high-purity polycarbonate resin finally by devolatilization granulation.
Crude polycarbonate solution of the present invention refers to the crude polycarbonate solution that polycarbonate solution prepared by this area interface polycondensation obtains after removing aqueous phase and catalyzer, usually containing a certain amount of moisture content and inorganic salts impurity in described crude polycarbonate solution.
Step described in the inventive method a) in, pure water is used to wash crude polycarbonate solution, as one of preferred embodiment, the mass ratio of crude polycarbonate solution and pure water is 1 ~ 15: 1, preferably 3 ~ 12: 1, water-oil ratio is too low will affect elute effect and separating effect, and water-oil ratio is too high can produce a large amount of waste water.
Crude polycarbonate solution and pure water mixing can adopt static mixer or stirring tank, are separated removing aqueous phase and can adopt separating centrifuge, coalescing separator, column plate decanting vessel, slurry tank etc.
Step b described in the inventive method) in, polycarbonate solution a flash distillation desolvation step a) obtained obtains polycarbonate solution b, in polycarbonate solution a before flash distillation, polycarbonate concentration is 5 ~ 30wt%, preferably 10 ~ 20wt%, flash distillation desolvation amount is 10 ~ 50wt% of solvent total amount in polycarbonate solution a, preferably 15 ~ 40wt%.
Step c described in the inventive method) in, in the polycarbonate solution b after desolventizing, add solvent obtain polycarbonate solution c ', and then carry out secondary flash and obtain polycarbonate solution c "; or repeat dilution and add flash steps to improve moisture content removal effect, and facilitate the precipitation of salt impurity; To step b) to add quantity of solvent in polycarbonate solution b after desolventizing be step b) in desolvation amount 20 ~ 100wt%, preferably 30 ~ 80wt%, obtain polycarbonate solution c ', then flash distillation removes the solvent accounting for solvent total amount 10 ~ 50wt% in described polycarbonate solution c ', preferably 15 ~ 40wt%, obtains polycarbonate solution c ".
Step c described in the inventive method) in, add solvent cut and flash distillation can repeat, preferably repeat 1-4 time, more preferably repetition 2-3 time, but polycarbonate solution c must be controlled " concentration range at 6 ~ 40wt%, preferably 15 ~ 35wt%; Add the water ratio < 0.2wt% in solvent, preferred < 0.15wt%.
Steps d described in the inventive method) in, the object of filtration is by step c) in the salt removing of separating out, as one of preferred embodiment, metre filter precision answers < 5 μm, preferred < 2 μm.
Steps d described in the inventive method) in, a certain amount of oxidation inhibitor can be added come Mulberry Extract, decompose hydroperoxide, chelated mineral and Lewis acid after completing the purifying of polycarbonate solution, prevent product from degrading, improve product appearance and performance, then devolatilization preparation high-purity polycarbonate resin.Described oxidation inhibitor comprises phosphorous acid esters and Hinered phenols, preferred phosphorous acid esters..
Solvent described in the inventive method can be methylene dichloride, ethylene dichloride, trichloroethane, tetrachloroethane, toluene or chlorobenzene with adding solvent, preferred methylene dichloride, ethylene dichloride, trichloroethane or tetrachloroethane, more preferably methylene dichloride, the solvent phase added in solvent and polycarbonate solution is same.The present invention can reduce the requirement to polymers soln washing process in early stage greatly, reduces washing step, reduces composite liberation requirement, thus effectively reduces costs.
The present invention makes full use of the feature that the solvent of dissolved polycarbonate and water exist azeotropic, adopt the method repeating dilution, flash distillation, remove the moisture content adopting conventional washing separating technology to remove, reduce the water ratio in polycarbonate solution, make the salt be dissolved in water separate out simultaneously, adopt secondary filter to remove the salt of separating out again, thus reach refining object.
In polycarbonate solution, the residual meeting of moisture content causes hydrolysis of ester group to generate phenolic hydroxyl group and carbonic acid gas in follow-up devolatilization granulation process, molecular weight product and ending ratio is caused all to decline, product yellowing is raised, simultaneously, the residual of moisture content can cause the hydrolysis of ester group in ester kind antioxidant to generate phenolic hydroxyl group equally, ester kind antioxidant consumption is caused to increase, water ratio in polycarbonate solution is reduced to below 0.1wt% and can effectively reduces product yellowing, the addition of oxidation inhibitor can be reduced to about 100ppm.
In addition, in the extrusion of polycarbonate, due to the plasticizing of inorganic salt high temperature difficulty, can be present in opaque products with crystalline substance point form, cause product mist degree to rise, yellowing is strengthened, inorganic salt content in product is reduced to below 100ppb, can effectively reduce product mist degree, product yellowing also effectively reduces, improving product quality.
Have no the purification process of the crude polycarbonate solution prepared from the disclosed interface polycondensation such as current existing document and patent utilize repeat to dilute, the method for flash distillation to reduce organic phase water ratio, recycling secondary filter removes salt to prepare the concrete report of high-purity polycarbonate solution.
Embodiment
The following examples will be further described method provided by the present invention, but the invention is not restricted to listed embodiment, also should be included in other any known change in interest field of the presently claimed invention.Embodiment will be further described method provided by the present invention, but the present invention is not therefore subject to any restriction.
Be 20000 daltonian linear PC to prepare number-average molecular weight, further illustrate embodiment of the present invention.
Raw material used is in the examples below respectively:
Dihydroxyphenyl propane: technical grade, purchased from Lanxing Chemical New Material Co., Ltd. (Wuxi resin processing plant); Sodium hydroxide: analytical pure, purchased from Tianjin Kermel Chemical Reagent Co., Ltd.; Phosgene: technical grade, Yantai ten thousand China; Methylene dichloride: analytical pure, purchased from Tianjin Kermel Chemical Reagent Co., Ltd.; P-tert-butylphenol: analytical pure, purchased from large Japanese ink chemical company; Triethylamine: analytical pure, purchased from Tianjin Kermel Chemical Reagent Co., Ltd.; Hydrochloric acid: analytical pure, purchased from Laiyang Shandong Province city economic and technological development zone Fine Chemical Works.Oxidation inhibitor (IRGAFOS 168): purchased from Ciba (China) company limited.
In polycarbonate polymer reaction liquid, residual moisture content adopts karl-Fischer reagent method to measure.
Residual sodium ion in polycarbonate polymer reaction liquid adopts ICP to measure under 589nm, INSTRUMENT MODEL: Agilent ICP 715-ES, detection limit 10ppb.
Polycarbonate products yellowing bioassay standard: ASTM E313.
Polycarbonate products mist degree bioassay standard: ASTM D1003.
Embodiment 1
Adopt the method provided in CN102030895A, be prepare polymer polycarbonate emulsion under the condition of methylene dichloride at solvent, organic phase is obtained after being separated removing aqueous phase, profit mass ratio by 9: 1 adds the mixed in hydrochloric acid separation removing aqueous phase that concentration is 0.5wt% in organic phase, obtain crude polycarbonate solution, in solution, add pure water by the polycarbonate solution of 9: 1 and the mass ratio of pure water again mix and be separated the polycarbonate solution obtaining preliminary purification, the concentration measuring this polycarbonate solution is 15.3wt%, water ratio is 0.38wt%, in polycarbonate resin, sodium content is 1.6mg/kg.
Get this polycarbonate solution of 100kg and be heated to 100 DEG C, be forced into 0.7MPa (gauge pressure), enter flash tank and carry out single flash, remove 20kg methylene dichloride and residuary water.In polycarbonate solution, add the methylene dichloride that 10kg water ratio is 0.12wt% again, Repeat-heating to 100 DEG C, be forced into 0.7MPa (gauge pressure), enter flash tank and carry out secondary flash, remove 20kg methylene dichloride and residuary water.Finally adopt precision to be that the strainer of 1 μm filters the polycarbonate solution after concentrate, finally obtain the high-purity polycarbonate solution that concentration is 21.9%.Finally in the polycarbonate solution of purifying, add the oxidation inhibitor IRGAFOS 168 of 100ppm relative to polycarbonate resin content again, devolatilization granulation obtains PC product, and result index is as shown in the table.
Embodiment 2
The method described in embodiment 1 of employing obtains the polycarbonate solution of preliminary purification, gets this polycarbonate solution of 100kg and is heated to 120 DEG C, be forced into 1MPa (gauge pressure), enter flash tank and carry out single flash, remove 32kg methylene dichloride and residuary water.In polycarbonate solution, add the methylene dichloride that 16kg water ratio is 0.12wt% again, Repeat-heating to 120 DEG C, be forced into 1MPa (gauge pressure), enter flash tank and carry out secondary flash, remove 27kg methylene dichloride and residuary water.Finally adopt precision to be that the strainer of 1 μm filters the polycarbonate solution after concentrate, finally obtain the high-purity polycarbonate solution that concentration is 26.8%.Finally in the polycarbonate solution of purifying, add the oxidation inhibitor IRGAFOS 168 of 100ppm relative to polycarbonate resin content again, devolatilization granulation obtains PC product, and result index is as shown in the table.
Embodiment 3
The method described in embodiment 1 of employing obtains the polycarbonate solution of preliminary purification, gets this polycarbonate solution of 100kg and is heated to 90 DEG C, be forced into 0.5MPa (gauge pressure), enter flash tank and carry out single flash, remove 14kg methylene dichloride and residuary water.In polycarbonate solution, add the methylene dichloride that 7kg water ratio is 0.12wt% again, Repeat-heating to 90 DEG C, be forced into 0.5MPa (gauge pressure), enter flash tank and carry out secondary flash, remove 14kg methylene dichloride and residuary water.Continue in the polycarbonate solution through secondary flash, to add the methylene dichloride that 7kg water ratio is 0.12wt%, Repeat-heating to 90 DEG C, be forced into 0.5MPa (gauge pressure), enter flash tank and carry out three flash distillations, remove 14kg methylene dichloride and residuary water.Finally adopt precision to be that the strainer of 1 μm filters the polycarbonate solution after concentrate, finally obtain the high-purity polycarbonate solution that concentration is 21.2%.Finally in the polycarbonate solution of purifying, add the oxidation inhibitor IRGAFOS 168 of 100ppm relative to polycarbonate resin content again, devolatilization granulation obtains PC product, and result index is as shown in the table.
Embodiment 4
The method described in example 1 of employing, continue to add the methylene dichloride that 10kg water ratio is 0.12wt% in the polycarbonate solution through secondary flash, Repeat-heating to 100 DEG C, be forced into 0.7MPa (gauge pressure), enter flash tank and carry out three flash distillations, remove 20kg methylene dichloride and residuary water.Finally adopt precision to be that the strainer of 1 μm filters the polycarbonate solution after concentrate, finally obtain the high-purity polycarbonate solution that concentration is 25.5%.Finally in the polycarbonate solution of purifying, add the oxidation inhibitor IRGAFOS 168 of 100ppm relative to polycarbonate resin content again, devolatilization granulation obtains PC product, and result index is as shown in the table.
Embodiment 5
The method described in embodiment 1 of employing, will add quantity of dichloromethane and be increased to 16kg, then be that the strainer of 1 μm filters the polycarbonate solution after concentrate by precision, finally obtain the high-purity polycarbonate solution that concentration is 20.1%.Finally in the polycarbonate solution of purifying, add the oxidation inhibitor IRGAFOS 168 of 100ppm relative to polycarbonate resin content again, devolatilization granulation obtains PC product, and result index is as shown in the table.
Embodiment 6
The method described in embodiment 1 of employing, employing precision is that the strainer of 5 μm filters the polycarbonate solution after concentrate, finally obtains the high-purity polycarbonate solution that concentration is 21.9%.Finally in the polycarbonate solution of purifying, add the oxidation inhibitor IRGAFOS 168 of 100ppm relative to polycarbonate resin content again, devolatilization granulation obtains PC product, and result index is as shown in the table.
Embodiment 7
The method described in embodiment 1 of employing, changes by solvent as 1,2-ethylene dichloride into, and the concentration of obtained crude polycarbonate solution is 14.7wt%, and water ratio is 0.41wt%, and in polycarbonate resin, sodium content is 1.9mg/kg.
Get this polycarbonate solution of 100kg and be heated to 135 DEG C, be forced into 0.6MPa and carry out flash distillation, remove 20kg 1,2-ethylene dichloride and residuary water.In polycarbonate solution, add 1, the 2-ethylene dichloride that 10kg water ratio is 0.12wt% again, Repeat-heating to 135 DEG C, be forced into 0.6MPa (gauge pressure) and carry out secondary flash, remove 20kg1,2-ethylene dichloride and residuary water.Finally adopt precision to be that the strainer of 1 μm filters the polycarbonate solution after concentrate, finally obtain the high-purity polycarbonate solution that concentration is 20.9%.Finally in the polycarbonate solution of purifying, add the oxidation inhibitor IRGAFOS 168 of 100ppm relative to polycarbonate resin content again, devolatilization granulation obtains PC product, and result index is as shown in the table.
Embodiment 8
The method described in embodiment 1 of employing, changes solvent into chlorobenzene, and the concentration of obtained crude polycarbonate solution is 12.3wt%, and water ratio is 0.39wt%, and in polycarbonate resin, sodium content is 1.8mg/kg.Get this polycarbonate solution of 100kg and be heated to 150 DEG C, be forced into 0.5MPa and carry out flash distillation, remove 20kg chlorobenzene and residuary water.In polycarbonate solution, add the chlorobenzene that 10kg water ratio is 0.13wt% again, Repeat-heating to 150 DEG C, be forced into 0.5MPa (gauge pressure) and carry out secondary flash, remove 20kg chlorobenzene and residuary water.Finally adopt precision to be that the strainer of 1 μm filters the polycarbonate solution after concentrate, finally obtain the high-purity polycarbonate solution that concentration is 17.6%.Finally in the polycarbonate solution of purifying, add the oxidation inhibitor IRGAFOS 168 of 100ppm relative to polycarbonate resin content again, devolatilization granulation obtains PC product, and result index is as shown in the table.
Comparative example 1
The polycarbonate solution of the preliminary purification that the method described in embodiment 1 of employing obtains, by flash evaporation feed temperature increase to 115 DEG C, be forced into 0.9MPa (gauge pressure), directly adopt the strainer of 1 μm to filter concentration liquid after removing methylene dichloride and residuary water 29kg, finally obtain the high-purity polycarbonate solution that concentration is 21.9%.Finally in the polycarbonate solution of purifying, add the oxidation inhibitor IRGAFOS 168 of 100ppm relative to polycarbonate resin content again, devolatilization granulation obtains PC product, and result index is as shown in the table.
Comparative example 2
The polycarbonate solution of the preliminary purification that the method described in embodiment 1 of employing obtains, continue in solution, to add pure water by the crude polycarbonate solution of 9: 1 and the mass ratio of pure water mix and be separated the polycarbonate solution obtaining purifying, the oxidation inhibitor IRGAFOS 168 of 100ppm relative to polycarbonate resin content is added in this polycarbonate solution, devolatilization granulation obtains PC product, and result index is as shown in the table.
Comparative example 3
The polycarbonate solution of the preliminary purification that the method described in embodiment 1 of employing obtains, do not adopt multistep flash process, directly to adding the oxidation inhibitor IRGAFOS 168 of 100ppm relative to polycarbonate resin content in the polycarbonate solution of preliminary purification, devolatilization granulation obtains PC product, and result index is as shown in the table.
Comparative example 4
The method described in comparative example 1 of employing, the addition of oxidation inhibitor IRGAFOS 168 is increased to 300ppm, and result index is as shown in the table.
Table 1 result index
Claims (16)
1. the purification process of crude polycarbonate solution prepared of interface polycondensation, comprises the steps:
A) in described crude polycarbonate solution, add pure water and be mixed to get organic phase and aqueous phase, be then separated the organic phase polycarbonate solution a that removing aqueous phase obtains preliminary purification;
B) flash distillation removes step and a) accounts for the solvent of solvent total amount 5 ~ 70wt% in gained polycarbonate solution a, obtains the polycarbonate solution b after desolventizing;
C) to step b) add into step b in polycarbonate solution b after desolventizing) in the solvent of desolvation amount 20 ~ 120wt% dilute, obtain polycarbonate solution c ', then flash distillation removes the solvent accounting for solvent total amount 5 ~ 70wt% in described polycarbonate solution c ', obtains polycarbonate solution c "; Step c) in control polycarbonate solution c " concentration range at 6 ~ 40wt%;
D) by step c) in obtained polycarbonate solution c " adopt the metre filter of < 10 μm, obtain highly purified polycarbonate solution d, obtain high-purity polycarbonate resin finally by devolatilization granulation;
Described solvent and add solvent and be all selected from methylene dichloride, ethylene dichloride, trichloroethane, tetrachloroethane, toluene or chlorobenzene; And solvent and add solvent phase with.
2. method according to claim 1, is characterized in that, step a) in the mass ratio of crude polycarbonate solution and pure water be 1 ~ 15:1.
3. method according to claim 2, is characterized in that, step a) in the mass ratio of crude polycarbonate solution and pure water be 3 ~ 12:1.
4. method according to claim 1, is characterized in that, step b) in polycarbonate solution a before flash distillation polycarbonate concentration be 5 ~ 30wt%.
5. method according to claim 4, is characterized in that, step b) in polycarbonate solution a before flash distillation polycarbonate concentration be 10 ~ 20wt%.
6. method according to claim 1, is characterized in that, step b) in flash distillation desolvation amount be solvent total amount 10 ~ 50wt% in polycarbonate solution a.
7. method according to claim 6, is characterized in that, step b) in flash distillation desolvation amount be solvent total amount 15 ~ 40wt% in polycarbonate solution a.
8. method according to claim 1, is characterized in that, step c) in dilution, flash vaporization process repeat 1-4 time.
9. method according to claim 8, is characterized in that, step c) in dilution, flash vaporization process repeat 2-3 time.
10. method according to claim 1, is characterized in that, step c) in the polycarbonate solution b after desolventizing, add quantity of solvent be step b) in 20 ~ 100wt% of desolvation amount.
11. methods according to claim 10, is characterized in that, step c) in the polycarbonate solution b after desolventizing, add quantity of solvent be step b) in 30 ~ 80wt% of desolvation amount.
12. methods according to claim 1, is characterized in that, step c) described in add the water ratio < 0.2wt% of solvent.
13. methods according to claim 12, is characterized in that, step c) described in add the water ratio < 0.15wt% of solvent.
14. methods according to claim 1, is characterized in that, step c) in control polycarbonate solution c " concentration range at 15 ~ 35wt%.
15. methods according to claim 1, is characterized in that, steps d) middle filtrator filtering accuracy < 5 μm.
16. methods according to claim 15, is characterized in that, steps d) middle filtrator filtering accuracy < 2 μm.
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|---|---|---|---|---|
| EP0264885A2 (en) * | 1986-10-22 | 1988-04-27 | Idemitsu Petrochemical Co. Ltd. | Washing method for a solution dissolving a polycarbonate resin in an organic solvent |
| CN1324375A (en) * | 1998-10-24 | 2001-11-28 | 拜尔公司 | Purification of solutions contg. polycarbonate |
| CN101508773A (en) * | 2009-03-13 | 2009-08-19 | 宁波万华聚氨酯有限公司 | Purification process for coarse polycarbonate organic phase solution prepared with interfacial polymerization |
| CN101536092A (en) * | 2006-10-31 | 2009-09-16 | 拜尔材料科学股份公司 | Matrix material for transparent injection-molded bodies |
| CN102532506A (en) * | 2012-02-24 | 2012-07-04 | 青岛科技大学 | Heat-integrated concentration and vaporization separating method |
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|---|---|---|---|---|
| EP0264885A2 (en) * | 1986-10-22 | 1988-04-27 | Idemitsu Petrochemical Co. Ltd. | Washing method for a solution dissolving a polycarbonate resin in an organic solvent |
| CN1324375A (en) * | 1998-10-24 | 2001-11-28 | 拜尔公司 | Purification of solutions contg. polycarbonate |
| CN101536092A (en) * | 2006-10-31 | 2009-09-16 | 拜尔材料科学股份公司 | Matrix material for transparent injection-molded bodies |
| CN101508773A (en) * | 2009-03-13 | 2009-08-19 | 宁波万华聚氨酯有限公司 | Purification process for coarse polycarbonate organic phase solution prepared with interfacial polymerization |
| CN102532506A (en) * | 2012-02-24 | 2012-07-04 | 青岛科技大学 | Heat-integrated concentration and vaporization separating method |
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