CN102850557A - Preparation method of polycarbonate powder - Google Patents
Preparation method of polycarbonate powder Download PDFInfo
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- CN102850557A CN102850557A CN2012103938787A CN201210393878A CN102850557A CN 102850557 A CN102850557 A CN 102850557A CN 2012103938787 A CN2012103938787 A CN 2012103938787A CN 201210393878 A CN201210393878 A CN 201210393878A CN 102850557 A CN102850557 A CN 102850557A
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Abstract
The invention provides a preparation method of polycarbonate powder. The preparation method comprises the following steps of: under the condition of stirring, adding the polycarbonate powder based on water as a medium; dripping a polycarbonate solution at the temperature of 40-60 DEG C, wherein the polycarbonate solution is a polycarbonate dichloromethane solution prepared by a phosgene interface polycondensation method; after dripping, further heating for desolventizing, and recovering dichloromethane at the same time; and after desolventizing, crushing slurry by a crushing pump, and then carrying out solid-liquid separation to obtain wet polycarbonate powder and mother liquor, wherein the mother liquor can be recycled; and drying the wet polycarbonate powder to obtain the product. The preparation method has the advantages of simple equipment, mild operation conditions and low energy consumption, the mother liquor can be recycled, and industrialization is easily realized.
Description
Technical field
The present invention relates to a kind of manufacture method of polycarbonate powder, specifically, is the method for being made the polycarbonate powder by the polycarbonate solution that the phosgene interface polycondensation makes.
Background technology
Polycarbonate is a kind of important engineering plastics product, is widely used in the industries such as building materials, automobile making, information storage.
Prepare in the polycarbonate technique at the phosgene interface polycondensation, making the polycarbonate powder by polycarbonate solution is one of technical barrier of this technique.Chinese patent application CN1048711A discloses the method that a kind of hot-water isolation polycarbonate solution makes the polycarbonate granular resin, comprises the hot water that contains non-solvent, and wherein said non-solvent refers to benzene, toluene, chlorobenzene, normal heptane, hexanaphthene etc.Chinese patent application CN1087647A discloses a kind of method of high molecular polymer hot water precipitating desolventizing, comprises macromolecule polymer solution is joined in the hot water with the former powder of identical high molecular polymer.Industrial equipments does not reach the stirring velocity that this patent application is described.Chinese patent application CN101503520A discloses a kind of method of removing solvent by polycarbonate solution aqueous phase precipitation, comprises the anti-solvent that joins in the aqueous phase system, and anti-solvent refers to the organic solvents such as methyl iso-butyl ketone (MIBK), methyl ethyl ketone, heptane; A shortcoming of this method is that the polycarbonate material that makes has wrapped up organic solvent, has affected product quality, needs simultaneously to reclaim organic solvent owing to used the organic solvents such as methyl iso-butyl ketone (MIBK), methyl ethyl ketone, heptane during the course; Another shortcoming is that the polycarbonate powder that makes is inhomogeneous.Chinese invention patent CN1733819A discloses and has a kind ofly pulverized the method that powder obtains polycarbonate powder after removing the partial solvent of this polycarbonate solution by evaporation first under air-flow; A shortcoming of this method is in the partial solvent process of removing polycarbonate solution by evaporation, material with respect to dry powder dissolvent residual 40%～50% is the colloidal material, vaporization temperature has reached 100 ℃, the viscosity of colloidal material is still larger, need to use specific installation, reach the purpose of evaporating solvent; Another shortcoming is to pulverize powder under air-flow, and the residual solvent recovery difficult is large.
Summary of the invention
The object of the invention is to develop one and be easy to industrialized polycarbonate powder manufacture method, the method has that equipment is simple, operational condition is gentle, energy consumption is low, Recycling Mother Solution is applied mechanically, be easy to the advantages such as industrialization.
A kind of manufacture method of polycarbonate powder comprises the steps:
(1) take water as medium, add the polycarbonate powder, described polycarbonate powder add-on is with respect to 0.5%～3.0% of quality;
(2) under 40 ~ 60 ℃, the dropping massfraction is 11%～22% polycarbonate solution, forms the polycarbonate slurry, reclaims simultaneously methylene dichloride;
(3) after dropping finishes, the polycarbonate slurry temperature is brought up to 80 ~ 90 ℃ carry out precipitation, reclaim simultaneously methylene dichloride;
(4) after precipitation finishes, pulverize slurry, solid-liquid separation obtains polycarbonate wet mash and mother liquor, and mother liquor is used for lower batch recycled;
(5) dry polycarbonate wet mash obtains polycarbonate powder product;
Wherein, above-mentioned steps (1) ~ (3) low whipping speed is to carry out under 300～900 rev/mins of conditions; The polycarbonate dichloromethane solution of polycarbonate solution described in the step (2) for adopting the phosgene interface polycondensation to make.
Among the present invention, similar in order to form shape in water, particle diameter is at the polycarbonate pellet of 5 ~ 7mm, and carry out under agitation condition step (1) ~ (3), preferred 400～600 rev/mins of its stirring velocity.
In the step (1), at first add the polycarbonate powder in water, described polycarbonate powder can be the polycarbonate powder that the present invention makes, and also can be the commercially available prod.The median size of powder is about 1.5mm, and tap density is 480～500kg/m3.Its add-on is with respect to quality preferred 1.0% ~ 2.5%.
In the step (2), preferred 50～55 ℃ of polycarbonate slurry temperature.The massfraction of the polycarbonate solution that drips preferred 14%～18%; The total mass of polycarbonate is for respect to 3 ~ 30 times of the polycarbonate powder quality of step (1) in the polycarbonate solution that drips, and time for adding is generally 1～3 hour.When dripping polycarbonate solution, reclaim the methylene dichloride that evaporates by condensation.
Polycarbonate slurry temperature in the step (3) is brought up to 80～90 ℃ and is carried out precipitation, reclaims methylene dichloride by condensation, further reduces the residual solvent amount in the polycarbonate pellet.
In the inventive method, directly remove methylene dichloride in water, reclaim methylene dichloride and rate of recovery height under lower temperature, the methylene dichloride of recovery can be directly used in phosgenation reaction and the polycondensation of polycarbonate.
In the step (4), adopt macerator pump to carry out the pulverizing of slurry.Described macerator pump can be the vertical or horizontal macerator pump that going round and round a millstone is arranged in the pump chamber and decide mill.By in the pump chamber go round and round a millstone and fixed mill between shearing action, the polycarbonate pellet in the water is ground into powder.Adjusting go round and round a millstone and fixed mill between the gap, can control particle diameter and the size distribution of polycarbonate powder.The gap of going round and round a millstone and deciding between the mill is preferably 3 ~ 5mm.
In the step (4), the equipment that is used for solid-liquid separation can be the whizzer of manual cleaning or automatic discharging, such as artificial lower discharging centrifuge, artificial top discharging whizzer, Pig conveyer centrifugal, horizontal scraper discharging centrifuge, horizontal type screw settling centrifuge etc.Preferred rotating speed is 1500 rev/mins whizzer.
In the step (5), adopt moisture eliminator to carry out the drying of polycarbonate wet mash.Described moisture eliminator can be the equipment of the suitable wet mash dryings such as two blade dryers, rotary dryer.Preferred drying temperature is 120～130 ℃.
The present invention has following advantage and effect:
(1) in the polycarbonate powder is made, directly removing methylene dichloride in water, is the manufacturing route of an economy height and environmental protection;
(2) reclaim methylene dichloride under lower temperature, the rate of recovery is high, and the methylene dichloride of recovery can be directly used in phosgenation reaction and the polycondensation of polycarbonate;
(3) energy consumption is low, and Recycling Mother Solution is used;
(4) regulate to pulverize in the pump chamber go round and round a millstone and fixed mill between the gap, reach the purpose of control polycarbonate powder particle size and size distribution;
(5) median size of polycarbonate powder is 1.3 ~ 1.6mm, and tap density is 480～500kg/m
3, be beneficial to post-treatment;
(6) equipment of the inventive method is simple, and operational condition is gentle, is easy to industrialization.
Description of drawings
Fig. 1 is the schematic flow sheet of manufacture method of the present invention.
Among the figure: I-separate out still, II-macerator pump, III-solid-liquid separating equipment; 1-charging opening, 2-methylene dichloride pneumatic outlet, 3-steam inlet, 4-condensation-water drain, 5-polycarbonate wet mash, the outlet of 6-mother liquor.
Embodiment
Raw material as in the polycarbonate powder manufacture method of the present invention can use the polycarbonate solution in the polycarbonate manufacturing process, the polycarbonate solution that particularly obtains at the phosgene interface polycondensation.As the polycarbonate solution of raw material, be the solution that is obtained by common phosgenation reaction and polycondensation among the present invention, by the phenol of divalent and phosgene reaction and make.Phenol as divalent, can enumerate Resorcinol, 4,4 '-dihydroxybiphenyl, two (4-hydroxy diphenyl) paraffinic hydrocarbonss (dihydroxyphenyl propane etc.), two (4-hydroxy diphenyl) naphthenic hydrocarbon, two (4-hydroxy diphenyl) oxide compound, two (4-hydroxy diphenyl) sulfide, two (4-hydroxy diphenyl) sulfone, two (4-hydroxy diphenyl) ketone etc. and these halogenated compound.The most general is in dichloromethane solvent, makes dihydroxyphenyl propane and phosgene reaction and obtain in the presence of tertiary amine (triethylamine etc.) catalyzer.
Further set forth production technique of the present invention by following specific embodiment.In an embodiment, polycarbonate solution refers to the polycarbonate dichloromethane solution that the phosgene interface polycondensation makes, and the number-average molecular weight of polycarbonate is 19000 ~ 40000.Except as otherwise noted, wherein " % " is " quality % ".
(1) in the 100L stirring tank, at first add the 60kg deionized water, stirring velocity is 500 rev/mins, then adding the 1.2kg median size is that the 1.5mm number-average molecular weight is 21000 polycarbonate powder; (2) after material temperature was elevated to 53 ℃, dripping the 58kg massfraction was that 14.5% number-average molecular weight is 21000 polycarbonate solution, and time for adding is 1 hour, reclaims simultaneously methylene dichloride; (3) after dropping finished, material temperature was elevated to 85 ℃ of precipitations 2 hours, reclaims simultaneously methylene dichloride; (4) slurry first with go round and round a millstone and fixed mill between the gap be that the macerator pump of 4mm is pulverized, rear is that 1500 rev/mins separating centrifuge carries out solid-liquid separation with rotating speed, obtains polycarbonate wet mash and mother liquor, mother liquor is used for lower batch of polycarbonate powder manufacturing; (5) the polycarbonate wet mash was 125 ℃ of dryings 4 hours.
Through said process, obtain polycarbonate powder 9.61kg, recording tap density is 480kg/m
3, median size is 1.47mm, maximum particle diameter is 1.9mm.
(1) in the 100L stirring tank, at first add the 60kg deionized water, stirring velocity is 500 rev/mins, then adding the 0.9kg median size is that the 1.5mm number-average molecular weight is 27000 polycarbonate powder; (2) after material temperature was elevated to 55 ℃, dripping the 50kg massfraction was that 14.5% number-average molecular weight is 27000 polycarbonate solution, and time for adding is 1 hour, reclaims simultaneously methylene dichloride; (3) after dropping finished, material temperature was elevated to 90 ℃, and precipitation 2 hours reclaims methylene dichloride simultaneously; (4) slurry first with go round and round a millstone and fixed mill between the gap be that the macerator pump of 4mm is pulverized, rear is that 1500 rev/mins separating centrifuge carries out solid-liquid separation with rotating speed, obtains polycarbonate wet mash and mother liquor, mother liquor is used for lower batch of polycarbonate powder manufacturing; (5) the polycarbonate wet mash was 125 ℃ of dryings 4 hours.
Through said process, obtain polycarbonate powder 8.15kg, recording tap density is 490kg/m
3, median size is 1.46mm, maximum particle diameter is 1.9mm.
(1) in the 100L stirring tank, at first add the mother liquor among the 60kg embodiment 2, stirring velocity is 600 rev/mins, then adding the 0.9kg median size is that the 1.5mm number-average molecular weight is 27000 polycarbonate powders; (2) after material temperature was elevated to 53 ℃, dripping the 82.5kg massfraction was that 14.5% number-average molecular weight is 27000 polycarbonate solution, and time for adding is 1.5 hours, reclaims simultaneously methylene dichloride; (3) after dropping finished, material temperature was elevated to 85 ℃, and precipitation 1.5 hours reclaims methylene dichloride simultaneously; (4) slurry first with go round and round a millstone and fixed mill between the gap be that the macerator pump of 4mm is pulverized, rear is that 1500 rev/mins whizzer carries out solid-liquid separation with rotating speed, obtains polycarbonate wet mash and mother liquor, mother liquor is used for lower batch of polycarbonate powder manufacturing; (5) the polycarbonate wet mash was 130 ℃ of dryings 4 hours.
Through said process, obtain polycarbonate powder 12.86kg, recording tap density is 493kg/m
3, median size is 1.46mm, maximum particle diameter is 1.9mm.
Claims (10)
1. the manufacture method of a polycarbonate powder comprises the steps:
(1) take water as medium, add the polycarbonate powder, described polycarbonate powder add-on is with respect to 0.5%～3.0% of quality;
(2) under 40 ~ 60 ℃, the dropping massfraction is 11%～22% polycarbonate solution, forms the polycarbonate slurry, reclaims simultaneously methylene dichloride;
(3) after dropping finishes, the polycarbonate slurry temperature is brought up to 80 ~ 90 ℃ carry out precipitation, reclaim simultaneously methylene dichloride;
(4) after precipitation finishes, pulverize slurry, solid-liquid separation obtains polycarbonate wet mash and mother liquor, and mother liquor is used for lower batch recycled;
(5) dry polycarbonate wet mash obtains polycarbonate powder product;
Wherein, above-mentioned steps (1) ~ (3) low whipping speed is to carry out under 300～900 rev/mins of conditions; The polycarbonate dichloromethane solution of polycarbonate solution described in the step (2) for adopting the phosgene interface polycondensation to make.
2. the manufacture method of polycarbonate powder according to claim 1 is characterized in that, stirring velocity is 400～600 rev/mins described in step (1) ~ (3).
3. the manufacture method of polycarbonate powder according to claim 1 is characterized in that, polycarbonate powder add-on is with respect to 1.0%～2.5% of quality described in the step (1).
4. the manufacture method of polycarbonate powder according to claim 1 is characterized in that, the massfraction of the polycarbonate solution that drips is 14%～18% in the step (2).
5. the manufacture method of polycarbonate powder according to claim 1 is characterized in that, temperature is 50～55 ℃ described in the step (2).
6. the manufacture method of polycarbonate powder according to claim 1 is characterized in that, polycarbonate dripping quantity described in the step (2) is 3 ~ 30 times with respect to the polycarbonate powder quality, and time for adding is 1～3 hour.
7. the manufacture method of polycarbonate powder according to claim 1 is characterized in that, adopts the vertical or horizontal macerator pump that in the pump chamber going round and round a millstone is arranged and decide to grind to carry out the pulverizing of slurry in the step (4).
8. the manufacture method of polycarbonate powder according to claim 1 is characterized in that, the whizzer of employing manual cleaning or automatic discharging carries out the solid-liquid separation of slurry in the step (4).
9. the manufacture method of polycarbonate powder according to claim 1 is characterized in that, adopts two blade dryers or rotary dryer to carry out the drying of wet mash in the step (5).
10. the manufacture method of polycarbonate powder according to claim 1 is characterized in that, the median size of polycarbonate powder product is 1.3 ~ 1.6mm described in the step (5), and tap density is 480～500kg/m
3
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| Application Number | Priority Date | Filing Date | Title |
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| CN2012103938787A CN102850557A (en) | 2012-10-16 | 2012-10-16 | Preparation method of polycarbonate powder |
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| CN2012103938787A CN102850557A (en) | 2012-10-16 | 2012-10-16 | Preparation method of polycarbonate powder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661984A (en) * | 2020-12-11 | 2021-04-16 | 万华化学集团股份有限公司 | Method for preparing polycarbonate powder |
| CN114644776A (en) * | 2022-04-29 | 2022-06-21 | 聊城鲁西聚碳酸酯有限公司 | System and method for recycling polycarbonate powder |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1087647A (en) * | 1992-12-02 | 1994-06-08 | 华东化工学院 | De-solvent method with hot water subsiding |
| CN1165834A (en) * | 1996-01-05 | 1997-11-26 | 拜尔公司 | Process for isolation of partially crystalline polycarbonate powder |
-
2012
- 2012-10-16 CN CN2012103938787A patent/CN102850557A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1087647A (en) * | 1992-12-02 | 1994-06-08 | 华东化工学院 | De-solvent method with hot water subsiding |
| CN1165834A (en) * | 1996-01-05 | 1997-11-26 | 拜尔公司 | Process for isolation of partially crystalline polycarbonate powder |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112661984A (en) * | 2020-12-11 | 2021-04-16 | 万华化学集团股份有限公司 | Method for preparing polycarbonate powder |
| CN114644776A (en) * | 2022-04-29 | 2022-06-21 | 聊城鲁西聚碳酸酯有限公司 | System and method for recycling polycarbonate powder |
| CN114644776B (en) * | 2022-04-29 | 2023-09-01 | 聊城鲁西聚碳酸酯有限公司 | System and method for recycling polycarbonate powder |
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Application publication date: 20130102 |