CN100391569C - Diaphragm treatment equipment for removing free monomer of additive compound of polyurethane - Google Patents
Diaphragm treatment equipment for removing free monomer of additive compound of polyurethane Download PDFInfo
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- CN100391569C CN100391569C CNB200510101597XA CN200510101597A CN100391569C CN 100391569 C CN100391569 C CN 100391569C CN B200510101597X A CNB200510101597X A CN B200510101597XA CN 200510101597 A CN200510101597 A CN 200510101597A CN 100391569 C CN100391569 C CN 100391569C
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Abstract
The present invention relates to a thin film treating device for separating free monomers from polyurethane addition compounds, which comprises a thin film evaporator. A stirring main shaft is arranged in the thin film evaporator, stirring scrapers are arranged on the stirring main shaft, and a feed port, secondary steam outlets and a discharge port are arranged on the thin film evaporator. The stirring main shaft is provided with fixed straight stirring scrapers and fixed spirally stirring scrapers. The thin film evaporator is provided with at least two secondary steam outlets. Movable stirring scrapers are hinged on the stirring main shaft and are ranged in two to eight columns along the radial direction of the stirring main shaft, and at least one layer of movable stirring scraper is arranged in each column. The fixed straight stirring scrapers are fixedly connect to the stirring main shaft and are ranged in two to eight columns along the radial direction of the stirring main shaft, and one single fixed straight stirring scraper is arranged in each column. The present invention has the advantages of simple and reasonable structure, convenient operation and high work efficiency, and can be used for separating solute from solvent with the long variation span of thermal sensitivity viscosity, and especially for separating free monomers from polyurethane addition compounds.
Description
Technical field
The present invention relates to a kind of film processing device that separates the polyurethane adducts free monomers.
Background technology
Polyurethane coating is very swift and violent in Development in China at present, it is the maximum kind in the existing solvent based coating, the paint film of polyurethane coating has advantages such as hardness height, good toughness, chemicals-resistant, fast drying, so it is widely used on automobile, building and the electrical equipment, and occupies dominant position in furniture house ornamentation coating.
Polyurethane adducts is commonly used for the polyisocyanate component of polyurethane coating, and vulcabond commonly used and polyol reaction are synthetic in the actual production.In reaction is synthetic, owing to have a spot of diisocyanate monomer not participate in reaction, and remain among the system, in construction and dry run, these diisocyanate monomers evaporate, and will produce harm greatly to health and surrounding environment.
It is not ideal to add the domestic production treatment process, and there are shortcomings such as free monomer content height, viscosity is big, toxicity is big in polyurethane curing agent.
Usually adopt diisocyanate monomer free in the film processing device evaporation polyurethane curing agent at present to obtain the polyisocyanates of low free diisocyanate monomer.
Chinese patent CN2551311 improves thin film evaporation equipment, adopts the mode of circulation to separate, and can improve product purity to a certain extent; But it is only applicable to non-heat-sensitive materials, and for heat-sensitive substance such as polyisocyanates, long-term circulation heating will cause material aging, and performance descends, and color and luster is deepened.
A kind of short distance thin-film distillation equipment is arranged in the thin film evaporation equipment, also be molecularly distilled, the principle and the film evaporation method of its separation are in full accord.Its outstanding feature is that the secondary steam of TDI cools off rapidly and the discharge system at device interior.Molecularly distilled (short distance film evaporation method) is applicable to the feed separation that viscosity is lower, and the material viscosity that thin film evaporator can be handled is high a lot, for example based on the TDI addition product of the polyalcohol of TMP.
Chinese patent CN1583846A report adopts inner-cooled (short distance thin-film distillation method) or external-cooling type thin film evaporator, and by three grades of separation, free TDI content is lower than 0.5% (75% solid content meter).Its outstanding feature is to have utilized high boiling entrainer, and the isocyanate-monomer of remnants at high temperature is evaporated.The use of this entrainer will inevitably increase the cost of product; Contain free monomer, the problem that exists entrainer to be difficult to recycle in the entrainer simultaneously; Simultaneously also can residual more entrainer in the product, because the boiling point height of entrainer, volatilization difficulty in use produces harmful effect to the terminal use of product.
Summary of the invention
The object of the present invention is to provide a kind of simple and reasonable, easy and simple to handle, high efficiency, can be used to separate thermal sensitivity viscosity and change the solvent in the span solution greatly and the film processing device that separates the polyurethane adducts free monomers of solute, to overcome weak point of the prior art.
A kind of film processing device that separates the polyurethane adducts free monomers by this purpose design, comprise thin film evaporator, be provided with the stirring main shaft in the thin film evaporator, stir main shaft and be provided with stirring scratch board, thin film evaporator is provided with charging aperture, secondary steam outlet and discharge port, its architectural feature is to stir main shaft to be provided with movable stirring scratch board and fixing straight stirring scratch board, or movable stirring scratch board and fixing helical stir scraper plate, or fixing straight stirring scratch board and fixing helical stir scraper plate, or movable stirring scratch board, fixing straight stirring scratch board and fixing helical stir scraper plate; Movable stirring scratch board and/or fixing straight stirring scratch board and/or fixedly the helical stir scraper plate join successively; Thin film evaporator is provided with two and above secondary steam outlet.
Above-mentioned movable stirring scratch board is hinged on and stirs on the main shaft, and along stirring main shaft radial arrangement two to eight row, every row are provided with one deck and above movable stirring scratch board.
Above-mentioned fixing straight stirring scratch board is fixed in and stirs on the main shaft, along stirring main shaft radial arrangement two to eight row, whenever classifies the fixing straight stirring scratch board of monolithic as.
Above-mentioned fixedly helical stir scraper plate structure in the shape of a spiral is fixed on the stirring main shaft, stirs main shaft and is provided with two to eight fixedly helical stir scraper plates.
Above-mentioned secondary steam outlet is arranged on thin film evaporator epimere and/or hypomere, and number is two to eight.
Above-mentioned secondary steam outlet has three, is provided with one in thin film evaporator epimere place, has two in the thin film evaporator lower section.
Above-mentioned thin film evaporator secondary steam outlet is connected with heat exchanger; Heat exchanger joins with secondary steam collection container, vacuum equipment successively.
Above-mentioned thin film evaporator is provided with distributing device in the charging aperture place, and distributing device and stirring main shaft and stirring scratch board are concentric.
Be provided with heater around the above-mentioned thin film evaporator; Discharge port is connected with the latting drown container by a hydraulic transmission.
The present invention is directed to that existing film evaporation method adopts that three grades of divided thin films are big from equipment investment, contain shortcoming such as entrainer in the complex manufacturing, product, a kind of film processing device that adopts single-stage film separating isocyanate is provided, but flush distillation is gone on a tour from monomer less than 0.5%, the polyisocyanates product of solid content more than 75%, reduce investment, simplify technology, improved production efficiency greatly.
Operation principle of the present invention may be interpreted as: movable stirring scratch board is suitable for the low viscosity material, and the helical stir scraper plate is suitable for high-viscosity material, and straight stirring scratch board then falls between.Separation along with vulcabond, the viscosity of isocyanate mixture sharply increases, and only use wherein a kind of scraper plate in above-mentioned three kinds of scraper plates in the known document, all because not matching of viscosity influenced actual operating efficiency, therefore, the present invention makes up three kinds of scraper plates simultaneously in same thin film evaporator, improved separative efficiency greatly; In the known references only with upper outlet or down outlet as the outlet of secondary steam, increased the effusion distance of part secondary steam, cause the condensation of secondary steam in thin film evaporator, influenced separative efficiency, the effusion distance of secondary steam has then been shortened in multiple exit setting of the present invention, has improved separative efficiency.
The present invention compared with prior art has following advantage:
One, compare with Chinese patent CN2551311, the present invention does not use circulation technology, has reduced material time of staying at high temperature, has avoided that material is aging, performance descends and color and luster is deepened;
Two, compare with the described film evaporation method of Chinese patent CN1583846A, the present invention adopts the single-stage film, and technology is simple, small investment; Do not add entrainer, greatly reduce the recycling problem of production cost and entrainer; Do not contain impurity such as entrainer in the curing agent yet; Material loss drops to minimum;
Three, compare the present invention's bringing normally into operation production with domestic other existing similar technology.
The present invention is simple and reasonable, easy and simple to handle, high efficiency, can be used to separate thermal sensitivity viscosity and changes solvent and solute in the span solvent greatly, particularly separates the free monomer in the polyurethane adducts.
Description of drawings
Fig. 1 is one embodiment of the invention structural representation.
Fig. 2 is the broken section structural representation of thin film evaporator.
Fig. 3 is an A-A section structure for amplifying schematic diagram among Fig. 2.
Fig. 4 is a B-B section structure for amplifying schematic diagram among Fig. 2.
Fig. 5 is a C-C section structure for amplifying schematic diagram among Fig. 2.
The specific embodiment
Below in conjunction with drawings and Examples the present invention is further described.
Among the figure, V1 is a head tank, and P2 is a material-handling pump, P1 is a material-handling pump, and V2 is the heavy ends pans, and H2 is a pipe bundle condenser, V3 is the light component pans, and Z1 is the vacuum unit, and M is a fire-proof motor, L1 is a heat exchanger, and 1 is liquid storage container, and 2 is charging aperture, 3 is distributing device, and 4 is thin film evaporator, and 5 is heater, 6,7,8 are the secondary steam outlet, and 9 is the latting drown container, and 10 is heat exchanger, 11 is the secondary steam receiving vessel, and 12 is vacuum equipment, and 13 is movable stirring scratch board, 14 are fixing straight stirring scratch board, and 15 are fixing helical stir scraper plate, and 16 is discharge port, 17 is temperature sensor, 20 for stirring main shaft, and 21 is frame, and 22 is fire-proof motor.
Referring to Fig. 1-Fig. 5, the film processing device of this separation polyurethane adducts free monomers, comprise thin film evaporator 4, be provided with in the cylindrical process vessel of thin film evaporator and stir main shaft 20, stir and be respectively arranged with movable stirring scratch board 13, fixing straight stirring scratch board 14 and fixing helical stir scraper plate 15 on the main shaft 20 vertically.
Movable stirring scratch board 13 is hinged on and stirs on the main shaft 20, and along stirring main shaft 20 radial arrangement three row, every row are provided with 17 layers movable stirring scratch board 13; Fixing straight stirring scratch board 14 is fixed in and stirs on the main shaft 20, along stirring main shaft 20 radial arrangement four row, whenever classifies the fixing straight stirring scratch board of monolithic as; Fixedly helical stir scraper plate 15 in the shape of a spiral structure be fixed in and stir on the main shaft 20, stir main shaft 20 and be provided with four fixedly helical stir scraper plates.
Herein concrete number of each stirring scratch board and position can be set according to actual conditions, can be according to inventory or the different stirring scratch board of viscosity of materials combination.Straight stirring scratch board and helical stir scraper plate 15 being fixed in stirring on the main shaft, is in order further to improve its rigidity because more toward below, viscosity of materials is high more.
Movable stirring scratch board 13, fixing straight stirring scratch board 14 and fixedly helical stir scraper plate 15 join successively.In actual production, the transition stirring scratch board can be set between the stirring scratch board of all size.
Secondary steam outlet on the thin film evaporator 4 has three, and 4 epimere places are provided with one in thin film evaporator, have two in the thin film evaporator lower section.
Look thin film evaporator height and stirring extent, can more secondary steam outlet be set in thin film evaporator 4 epimeres and hypomere.The outlet of thin film evaporator 4 secondary steams is connected with heat exchanger 10; Heat exchanger 10 joins with secondary steam collection container 11, vacuum equipment 12 successively.
Thin film evaporator 4 is provided with its top feed mouth 2, and the bottom is provided with discharge port 16, and thin film evaporator 4 is provided with distributing device 3 in charging aperture 2 places, and distributing device 3 and stirring main shaft 20 and stirring scratch board are concentric.In order to increase the flowability of material, around thin film evaporator 4, be provided with heater 5.Discharge port 16 is connected with latting drown container 9 by a hydraulic transmission.
The mode of operation of this equipment is as follows:
Starting equipment vacuum 12 reaches separate vacuum degree 1Pa～800Pa, and optimal vacuum pressure is 10Pa～500Pa, and the heat medium in the heater 5 is heated to 80 ℃～210 ℃, and optimum heating temperature is 100 ℃～190 ℃.Heat medium wherein can be steam or deep fat.
The polyisocyanates material that contains vulcabond in the container 1---can at the preset temperature state---is sent into the thin film evaporator 4 from charging aperture 2 continuously, be distributed on thin film evaporator 4 inwalls through distributing device 3 effects there, and the movable stirring scratch board 13 that is stirred on the main shaft 20 spreads to film, because viscosity is lower, material can be spread to relatively thin film by movable stirring scratch board 13, and vulcabond is overflowed under heating and vacuum.Effusion along with vulcabond, the viscosity of material increases gradually, when reaching a point among Fig. 2, the viscosity of material is bigger, movable stirring scratch board can not spread to film with it, at this moment the movable stirring scratch board that stirs on the main shaft 20 has become fixing straight stirring scratch board 14, fixing straight stirring scratch board can continue to keep material to become film, when material reaches b point among Fig. 2, material viscosity further increases, material can be scraped be that film, material have been difficult to flow downward under the effect of gravity though at this moment fix straight stirring scratch board, at this moment, the fixing straight stirring scratch board that stirs on the main shaft 20 becomes fixedly helical stir scraper plate, when fixedly the helical stir scraper plate further forms thinner film with material, keep a downward thrust to material, the material of final separator well is discharged through discharge port 16.Discharge port 16 connects latting drown container 9 by hydraulic transmission.Put into diluted solvent in the latting drown container in advance, the polyisocyanates of separation that latting drown enters, the material of discharge enter latting drown container 9 and carry out latting drown.Can obtain the polyisocyanates addition product of low free monomer this moment.
Form in the process of different-thickness film by thin film evaporator 4 at material, constantly the vulcabond of overflowing forms secondary steam, secondary steam can be nearby by upper outlet 6, export 7 and 8 down and overflow, secondary steam outlet 6,7 are connected the heat exchanger 10 of a refrigeration with 8, with the secondary steam of cooling evaporation.Being provided with of multiple exit reduced the again condensation of secondary steam in thin film evaporator 4, and secondary steam arrives heat exchanger 10, collects after the condensation in the secondary steam receiving vessel 11.The other end of heat exchanger 10 connects vacuum equipment 12 by secondary steam collection container 11, so that the effusion of secondary steam and collection.
Be two concrete production examples below.
The TDI-TMP addition product (being preheating to 100 ℃) that will contain 20% free TDI passes through film processing device continuously, wherein the separating area of thin film evaporator is 0.5 square metre, stir the main shaft movable stirring scratch board of band, fixing straight stirring scratch board and fixing helical stir scraper plate from top to bottom, adopt two outlets of hypomere, outlet of epimere, thin film wire speed is 8m/s, 180 ℃ of separation temperatures, separate vacuum 230Pa, per hour treating capacity is 47kg, separates back curing agent index and sees the following form:
| Index | Value |
| Color and luster (Pt-Co colorimetric), |
20 |
| Outward appearance | Transparent |
| Non-volatile part, % | 74.7 |
| Free TDI content, % | 0.231 |
| NCO content, % | 12.9 |
| Viscosity, mPa.s | 1270 |
Embodiment 2
The TDI-TMP addition product (being preheating to 100 ℃) that will contain 20% free TDI passes through film processing device continuously, wherein the separating area of thin film evaporator is 2 square metres, stir the main shaft movable stirring scratch board of band, straight stirring scratch board and helical stir scraper plate from top to bottom, adopt outlet of hypomere, two outlets of epimere, thin film wire speed is 8.4m/s, 180 ℃ of separation temperatures, separate vacuum 238Pa, per hour treating capacity is 184kg, separates back curing agent index and sees the following form:
| Index | Value |
| Color and luster (Pt-Co colorimetric), |
20 |
| Outward appearance | Transparent |
| Non-volatile part, % | 75.1 |
| Free TDI content, % | 0.242 |
| NCO content, % | 13 |
| Viscosity, mPa.s | 1350 |
Claims (9)
1. film processing device that separates the polyurethane adducts free monomers, comprise thin film evaporator (4), be provided with in the thin film evaporator and stir main shaft (20), stir main shaft and be provided with stirring scratch board, thin film evaporator is provided with charging aperture (2), secondary steam outlet and discharge port (16), it is characterized in that described stirring main shaft is provided with movable stirring scratch board (13) and fixing straight stirring scratch board (14), or movable stirring scratch board (13) and fixing helical stir scraper plate (15), or fixing straight stirring scratch board and fixing helical stir scraper plate, or movable stirring scratch board, fixing straight stirring scratch board and fixing helical stir scraper plate; Movable stirring scratch board and/or fixing straight stirring scratch board and/or fixedly the helical stir scraper plate join successively; Thin film evaporator is provided with two and above secondary steam outlet.
2. the film processing device of separation polyurethane adducts free monomers according to claim 1, it is characterized in that described movable stirring scratch board (13) is hinged on the stirring main shaft (20), along stirring main shaft radial arrangement two to eight row, every row are provided with one deck and above movable stirring scratch board.
3. the film processing device of separation polyurethane adducts free monomers according to claim 1, it is characterized in that described fixing straight stirring scratch board (14) is fixed on the stirring main shaft (20), along stirring main shaft radial arrangement two to eight row, whenever classify the fixing straight stirring scratch board of monolithic as.
4. the film processing device of separation polyurethane adducts free monomers according to claim 1, it is characterized in that described fixedly helical stir scraper plate (15) in the shape of a spiral structure be fixed in and stir on the main shaft (20), stir main shaft (20) and be provided with two to eight fixedly helical stir scraper plates.
5. the film processing device of separation polyurethane adducts free monomers according to claim 1 is characterized in that described secondary steam outlet is arranged on thin film evaporator (4) epimere and/or hypomere, and number is two to eight.
6. the film processing device of separation polyurethane adducts free monomers according to claim 5 is characterized in that described secondary steam outlet has three, and the epimere place is provided with one in thin film evaporator (4), has two in the thin film evaporator lower section.
7. the film processing device of separation polyurethane adducts free monomers according to claim 5 is characterized in that the outlet of described thin film evaporator (4) secondary steam is connected with heat exchanger (10); Heat exchanger (10) joins with secondary steam collection container (11), vacuum equipment (12) successively.
8. the film processing device of separation polyurethane adducts free monomers according to claim 1, it is characterized in that described thin film evaporator (4) locates to be provided with distributing device (3) in charging aperture (2), distributing device and stir main shaft (20) and stirring scratch board concentric.
9. the film processing device of separation polyurethane adducts free monomers according to claim 1 is characterized in that described thin film evaporator (4) is provided with heater (5) on every side; Discharge port (16) is connected with latting drown container (9) by a hydraulic transmission.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510101597XA CN100391569C (en) | 2005-11-29 | 2005-11-29 | Diaphragm treatment equipment for removing free monomer of additive compound of polyurethane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200510101597XA CN100391569C (en) | 2005-11-29 | 2005-11-29 | Diaphragm treatment equipment for removing free monomer of additive compound of polyurethane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1792404A CN1792404A (en) | 2006-06-28 |
| CN100391569C true CN100391569C (en) | 2008-06-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200510101597XA Active CN100391569C (en) | 2005-11-29 | 2005-11-29 | Diaphragm treatment equipment for removing free monomer of additive compound of polyurethane |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102179055A (en) * | 2011-03-30 | 2011-09-14 | 孝感凯风生物工程有限责任公司 | Film-wiping type calcium lactate evaporating process |
| CN102181945B (en) * | 2011-06-01 | 2013-10-30 | 山东海龙股份有限公司 | Deaeration method of cellulose ionic liquid solution for solvent spinning |
| CN103011316A (en) * | 2013-01-21 | 2013-04-03 | 重庆科技学院 | Polluted waste liquid treatment device |
| CN108211393A (en) * | 2018-03-30 | 2018-06-29 | 江苏丰益化工科技有限公司 | A kind of drier for surfactant |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5185060A (en) * | 1989-07-26 | 1993-02-09 | Shinko Pantec Co., Ltd. | Film evaporator |
| JP2000327774A (en) * | 1999-05-19 | 2000-11-28 | Toray Ind Inc | Production of nylon resin |
| CN2878389Y (en) * | 2005-11-29 | 2007-03-14 | 广东华润涂料有限公司 | Thin film processing device for separating dissociative monomer in polyurethane addition compound |
-
2005
- 2005-11-29 CN CNB200510101597XA patent/CN100391569C/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5185060A (en) * | 1989-07-26 | 1993-02-09 | Shinko Pantec Co., Ltd. | Film evaporator |
| JP2000327774A (en) * | 1999-05-19 | 2000-11-28 | Toray Ind Inc | Production of nylon resin |
| CN2878389Y (en) * | 2005-11-29 | 2007-03-14 | 广东华润涂料有限公司 | Thin film processing device for separating dissociative monomer in polyurethane addition compound |
Non-Patent Citations (4)
| Title |
|---|
| 游离TDI和薄膜蒸发. 虞兆年.上海涂料，第40卷第3期. 2002 |
| 游离TDI和薄膜蒸发. 虞兆年.上海涂料，第40卷第3期. 2002 * |
| 薄膜蒸发浓缩干燥装置. 袁文.医药工程设计杂志，第21卷第3期. 2000 |
| 薄膜蒸发浓缩干燥装置. 袁文.医药工程设计杂志，第21卷第3期. 2000 * |
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