CN105524243A - Solvent removal method for waterborne polyurethane production process - Google Patents
Solvent removal method for waterborne polyurethane production process Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/10—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
- C08G18/12—Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/08—Processes
- C08G18/0804—Manufacture of polymers containing ionic or ionogenic groups
- C08G18/0819—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
- C08G18/0823—Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing carboxylate salt groups or groups forming them
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6666—Compounds of group C08G18/48 or C08G18/52
- C08G18/6692—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
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Abstract
The invention discloses a solvent removal method for a waterborne polyurethane production process. The method is implemented in a solvent removal kettle provided with a rectification device. The solvent removal kettle provided with the rectification device comprises a solvent removal kettle body, a rectification tower section and a condenser, wherein the bottom of the rectification tower section is communicated with the solvent removal kettle body, a steam inlet of the condenser is communicated with a steam outlet in the top of the rectification tower section, and a condensate outlet of the condenser is connected with a reflux inlet in the upper part of the rectification tower section and a solvent collection system. According to the solvent removal method, the solvent removal kettle and the rectification device are jointly used, a distilled solvent has very low water content and can be directly used for waterborne polyurethane production, energy in a solvent removal process is used effectively, a secondary refining process for the solvent is omitted, the production energy consumption is reduced, and the production efficiency is improved.
Description
Technical field
The present invention relates to a kind of method of aqueous polyurethane production process desolvation.
Technical background
Aqueous polyurethane is that urethane is scattered in a kind of environment-protecting polyurethane product formed in water by certain technique means, is mainly used in the numerous areas such as sizing agent, coating and synthetic leather.
Aqueous polyurethane compares oiliness polyurethane system not containing solvent, is typical environmentally friendly machine.In the production process of aqueous polyurethane, carry out smoothly in order to prepolymerization reaction can be made, simultaneously in order to performed polymer is successfully scattered in water in emulsion process, usually need in performed polymer, to add acetone, butanone, DMF equal solvent to reduce viscosity.When adding to performed polymer after emulsifying water completes, needing the solvent adding to remove from system, reaching product Water-borne modification, the object completely not containing solvent.
Acetone method is as the method for known production aqueous polyurethane in the industry, its basic procedure is as follows: 1) first by isocyanic ester and polymer polyatomic alcohol and small molecule chain extender being reacted, obtain base polyurethane prepolymer for use as, in this process, need to add solvent to reduce the viscosity of performed polymer thus effectively to control reaction process, meanwhile, emulsifying water is added to low viscous performed polymer and can obtain good emulsifying effect and reaction repeatability, ensure to produce and carry out smoothly.2) after performed polymer synthesis, add water in performed polymer, under Strong shear effect, performed polymer is scattered in water the polyaminoester emulsion forming non-precipitation.3) polyaminoester emulsion of non-precipitation good for emulsification is removed by the method for distillation the solvent added at pre-collecting process, obtain not solvent-laden aqueous polyurethane product.4) distill the solvent obtained to be refined by methods such as rectifying, the production of aqueous polyurethane can be continued on for.
In above-mentioned production technique, the solvent that distillation produces directly enters condenser and carries out condensation, obtain the organic solvent solution containing large water gaging, the solvent added all evaporates by the process need of desolvation, because gasification latent heat is huge, desolvation process produces the step consumed energy most in aqueous polyurethane; On the other hand, containing large quantity of moisture in the solvent that precipitation produces, need to be refined by rectifying, the energy also needing consumption a large amount of of this process.In above-mentioned known method in the industry, desolvation process only carries out single flash, and these solution obtained need again to refine, and just can obtain the qualified solvent that may be used for aqueous polyurethane production.In this process, the heat energy that precipitation part uses is not used for the refining purification of solvent, but the device that is condensed is taken away, the utilising efficiency of heat energy is lower, the energy of input not used for the purification of solvent with refining, cause the method recycling design needing to adopt secondary refining, whole production process energy consumption is very high.Therefore, in the urgent need to a kind of method of energy-efficient desolvation.
Summary of the invention
The object of this invention is to provide a kind of method of aqueous polyurethane production process desolvation, to overcome the defect that prior art exists.
The method of aqueous polyurethane production process desolvation of the present invention, be a kind of with the precipitation still of rectifier unit in realize, the described precipitation still with rectifier unit, comprise precipitation still, rectifying tower joint and condenser;
The bottom of described rectifying tower joint is connected with described precipitation still, the vapour outlet that steam-in and the rectifying tower of described condenser save top is connected, and the refluxing opening that the condensate outlet of described condenser saves top with described rectifying tower is respectively connected with solvent collecting system;
The method of desolvation is as follows: the polyaminoester emulsion of non-precipitation is added precipitation still, under vacuum or atmospheric pressure state, be heated to boiling, rectifying tower saves the steam at top by after condenser condenses, partial reflux, all the other are product solvent, control reflux ratio, make in product solvent, the weight content of water is lower than 0.5%, until in precipitation still, the weight content of solvent is lower than 0.5%;
Consisting of of the polyaminoester emulsion of described non-precipitation:
The ratio of urethane and solvent is 1:0.1 ~ 5, and the ratio of urethane and water is 1:0.1 ~ 19;
Described solvent is be selected from the one or two or more in acetone, butanone, tetrahydrofuran (THF) and ethyl acetate;
Preferably, precipitation still internal pressure is 0.001MPaA ~ 0.101325MPaA;
Rectifying tower top temperature comparatively precipitation temperature in the kettle low 3 DEG C ~ 50 DEG C;
The solvent condensate depression of backflow is 0 DEG C ~ 10 DEG C, and reflux ratio is 1 ~ 5;
Preferably, upper part of described rectifying tower is filling-material structure, is highly more than or equal to 2 meters; Lower part is dual-flow tray type structure, is highly more than or equal to 2 meters, and stage number is 1 to 10 piece, and sieve plate and horizontal direction are 0-30 degree angle;
Preferably, the bottom of rectifying tower has a valve rectifying tower and precipitation still can be cut off;
In the present invention, owing to have employed the combined utilization with precipitation still and rectifier unit, in the solvent distilled out, moisture content is very low, the production of aqueous polyurethane can be directly used in, effectively make use of the energy of desolvation process, eliminate the secondary refining process of solvent, reduce production energy consumption, improve production efficiency.
Accompanying drawing explanation
Fig. 1 is the structural representation of the precipitation still being configured with rectifier unit.
Fig. 2 is precipitation still structural representation.
Embodiment
See Fig. 1, the method for aqueous polyurethane production process desolvation of the present invention, be a kind of with the precipitation still of rectifier unit in realize, the described precipitation still with rectifier unit, comprises precipitation still 1, rectifying tower joint 2 and condenser 3;
The bottom of described rectifying tower joint 2 is connected with described precipitation still 1, the vapour outlet 201 that steam-in 301 and the rectifying tower of described condenser 3 save 2 tops is connected, and the condensate outlet 302 of described condenser 3 saves 2 tops respectively refluxing opening 202 with described rectifying tower is connected with solvent collecting system 4;
The method of desolvation is as follows: the polyaminoester emulsion of non-precipitation is added precipitation still 1, is heated to 100 ~ 10 DEG C, and controlling tower top temperature is 56.5 ~ 7 DEG C, and tower top temperature can realize by regulating vacuum tightness;
Preferably, described precipitation still comprises kettle 101, precipitation liquid upcast 102, turbine 103 and liquid distributing device;
Described precipitation liquid upcast 102 is fixed on the inwall of described kettle 101 by mounting block, gap 104 is provided with the bottom of kettle 101 bottom it, described turbine 103 is arranged on the bottom of described precipitation liquid upcast 102, and be connected by the motor of rotating shaft with precipitation still outside, described liquid distributing device is arranged on the top of described precipitation liquid upcast 102;
Described liquid distributing device comprises ring-type separatory dish 105 and overflow weir 106, the inner circle of described ring-type separatory dish 105 is connected with described precipitation liquid upcast 102, described overflow weir 106 is arranged on the outer rim of described ring-type separatory dish 105, preferably, described overflow weir 106 is prionodont, preferred further, the diameter of shape separatory dish 105 is 30 ~ 60% of kettle diameter;
Adopt the precipitation still of said structure, by by the material of desolventizing, can evaporate in a dynamic state, and form the waterfall shape liquid stream flowed downward, greatly can improve vaporization efficiency.
Principle of work of the present invention is such:
In precipitation still, the polyaminoester emulsion of non-precipitation is heated, and by precipitation liquid upcast 102, turbine 103 and liquid distributing device, make the polyaminoester emulsion of non-precipitation by precipitation liquid upcast 102, from the overflow weir 106 on precipitation liquid upcast 102 top shunt and, make non-precipitation polyaminoester emulsion dispersion and under flow state, by water and acetone evaporated, the material that the solvent vapo(u)r produced enters rectifying tower and backflow carries out heat and mass transfer, enter reflux exchanger total condensation afterwards and become liquid, under the effect of reflux ratio control device, the backflow of part solvent vapo(u)r phlegma enters rectifying tower and carries out heat and mass transfer with the solvent steamed, another part solvent vapo(u)r phlegma is as product discharge.
Along with desolvation process constantly carries out, quantity of solvent residual in the polyaminoester emulsion of non-precipitation constantly reduces, until precipitation completes, obtains not solvent-laden aqueous polyurethane product.
In embodiment, if no special instructions, content is weight content.
Embodiment 1
By 1000 kilograms of polypropylene glycols 2000,125 kilogram 4,4-'-diphenylmethane diisocyanate, 67 kilogram 2,2-dimethylol propionic acid and 124.2 kilograms of acetone add reactor, be warming up to 80 degrees Celsius of reactions 2 hours, then 50 degrees Celsius are cooled to, add 50 kilograms of triethylamines and continue reaction 30 minutes, obtain performed polymer.
Then in performed polymer, add a) 124.2 kg water and b) 130 kg water respectively, obtain respectively through powerful emulsification: the polyaminoester emulsion of non-precipitation is 1490.4 kilograms and polyaminoester emulsion b a)) 1496.2 kilograms.
Embodiment 2
The polyaminoester emulsion of the non-precipitation in embodiment 1 a) is added the precipitation still of Fig. 1 device;
Polyaminoester emulsion component a) of non-precipitation is:
The ratio of urethane and solvent is 1:0.1, and the ratio of urethane and water is 1:0.1
Rectifying tower upper semisection height is 2 meters, in-built filler; The height of lower semisection is 2 meters, wherein arranges 1 piece of dual-flow tray, and column plate plane and horizontal direction are 30 degree of angles.
A) boiling is heated to the polyaminoester emulsion of non-precipitation, precipitation still pressure is kept to be 0.001MPaA, the material that the solvent vapo(u)r produced enters rectifying tower and backflow carries out heat and mass transfer, enter reflux exchanger total condensation afterwards and become liquid, the backflow of part solvent vapo(u)r phlegma enters rectifying tower and carries out heat and mass transfer with the solvent steamed, the direct discharging of another part solvent vapo(u)r phlegma, controlling reflux ratio is 5, and the phlegma condensate depression of backflow is 0 DEG C.
Precipitation is initial, bottom temperature is 10 DEG C, tower top temperature is 7 DEG C, along with desolvation process constantly carries out, quantity of solvent residual in the polyaminoester emulsion of non-precipitation constantly reduces, until precipitation completes, now bottom temperature rises to 40 DEG C, tower top temperature is 30 DEG C, closes rectifier bottoms valve, prevents from holding liquid refluence polluted product in tower.
Finally obtain the aqueous polyurethane product 1366.2 kilograms that organic solvent weight content is less than 0.5%, 124.2 kilograms, the acetone that moisture weight content is less than 0.5%.
The aqueous polyurethane product obtained is salable product, can direct marketing;
Reclaim the acetone obtained not need to refine, can again for the production of aqueous polyurethane.Utilize above-mentioned method to carry out precipitation, whole process consumes 0.3MPaG steam 0.14 ton.
Embodiment 3
As the comparative example of embodiment 2, embodiment 3 adopts known conventional desolventizing method in the industry to carry out precipitation, detailed process is by the polyaminoester emulsion b of precipitation non-in embodiment 1) add and be only equipped with in the precipitation still of condenser, the polyaminoester emulsion b to non-precipitation) heat.
Keep precipitation still pressure to be 0.001MPaA, the solvent vapo(u)r of generation becomes liquid discharging through condenser total condensation.Along with desolvation process constantly carries out, quantity of solvent residual in the polyaminoester emulsion of non-precipitation constantly reduces, until precipitation completes, obtain the aqueous polyurethane product 1366.2 kilograms that organic solvent content is less than 0.5%, moisture content is 130 kilograms, the acetone of 4.46%.Because in acetone, moisture content is too high, the production of aqueous polyurethane can not be used for, need again to refine, 124.2 kilograms, the acetone that moisture content is less than 0.5% can be obtained, the waste water 5.8 kilograms that acetone content is less than 0.5%.Desolvation process consumes 0.3MPaG steam 0.052 ton, and treating process consumes 0.3MPaG steam 0.125 ton, therefore, obtains the product identical with embodiment 2 and consumes 0.3MPaG steam 0.176 ton altogether.
Embodiment 4
By 1000 kilograms of polypropylene glycols 2000,1001 kilogram 4,4-'-diphenylmethane diisocyanate, 67 kilogram 2,2-dimethylol propionic acid and 10590 kilograms of acetone add reactor, be warming up to 80 degrees Celsius of reactions 2 hours, then 50 degrees Celsius are cooled to, add 50 kilograms of triethylamines and continue reaction 30 minutes, obtain performed polymer.Then in performed polymer, a) 40242 kg water and b) 42242 kg water are added respectively, polyaminoester emulsion a) 52950 kilograms and the polyaminoester emulsion b through powerful emulsification obtains non-precipitation respectively) 54950 kilograms.
Embodiment 5
A) added and be equipped with in the precipitation still of rectifying tower, reflux ratio control device and reflux exchanger by the polyaminoester emulsion of the non-precipitation in embodiment 4, the ratio of urethane and solvent is 1:5, and the ratio of urethane and water is 1:19
Rectifying tower upper semisection height is 10 meters, in-built filler; The height of lower semisection is 5 meters, wherein arranges 10 pieces of dual-flow trays, and column plate plane and horizontal direction are 0 degree of angle.Rectifying tower lower semisection liner is polyvinylidene difluoride (PVDF), and column plate material is polyvinylidene difluoride (PVDF).A) boiling is heated to the polyaminoester emulsion of non-precipitation, precipitation still pressure is kept to be 0.101325MPaA, the material that the solvent vapo(u)r produced enters rectifying tower and backflow carries out heat and mass transfer, enter reflux exchanger total condensation afterwards and become liquid, the backflow of part solvent vapo(u)r phlegma enters rectifying tower and carries out heat and mass transfer with the solvent steamed, the direct discharging of another part solvent vapo(u)r phlegma, controlling reflux ratio is 1, and the phlegma condensate depression of backflow is 10 DEG C.Precipitation is initial, bottom temperature is 60 DEG C, tower top temperature is 56.5 DEG C, along with desolvation process constantly carries out, quantity of solvent residual in the polyaminoester emulsion of non-precipitation constantly reduces, until precipitation completes, bottom temperature rises to 106.5 DEG C, tower top temperature is 56.5 degree, closes rectifier bottoms valve, prevents from holding liquid refluence polluted product in tower.Finally obtain the aqueous polyurethane product 42360 kilograms that organic solvent content is less than 0.5%, 10590 kilograms, the acetone that moisture content is less than 0.5%.The aqueous polyurethane product that embodiment 5 obtains is salable product, can direct marketing; Reclaim the acetone obtained not need to refine, can again for the production of aqueous polyurethane.Utilize above-mentioned method to carry out precipitation, whole process consumes 0.3MPaG steam 12.04 tons.
Embodiment 6
As the comparative example of embodiment 5, embodiment 6 adopts known conventional desolventizing method in the industry to carry out precipitation, detailed process is by the polyaminoester emulsion b of precipitation non-in embodiment 4) add and be only equipped with in the precipitation still of condenser, the polyaminoester emulsion b to non-precipitation) heat;
Keep precipitation still pressure to be 0.101325MPaA, the solvent vapo(u)r of generation becomes liquid discharging through condenser total condensation.Along with desolvation process constantly carries out, quantity of solvent residual in the polyaminoester emulsion of non-precipitation constantly reduces, until precipitation completes, obtain the aqueous polyurethane product 42360 kilograms that organic solvent content is less than 0.5%, moisture content is 12590 kilograms, the acetone of 15.88%.Because in acetone, moisture content is too high, the production of aqueous polyurethane can not be used for, need again to refine, 10590 kilograms, the acetone that moisture content is less than 0.5% can be obtained, the waste water 2000 kilograms that acetone content is less than 0.5%.Desolvation process consumes 0.3MPaG steam 3.75 tons, and treating process consumes 0.3MPaG steam 11.8 tons, therefore, obtains the product identical with embodiment 5 and consumes 0.3MPaG steam 15.5 tons altogether.
Claims (10)
1. the method for aqueous polyurethane production process desolvation, is characterized in that, be a kind of with the precipitation still of rectifier unit in realize, the described precipitation still with rectifier unit, comprise precipitation still, rectifying tower joint and condenser;
The bottom of described rectifying tower joint is connected with described precipitation still, the vapour outlet that steam-in and the rectifying tower of described condenser save top is connected, and the refluxing opening that the condensate outlet of described condenser saves top with described rectifying tower is respectively connected with solvent collecting system.
2. method according to claim 1, is characterized in that, the method for desolvation is as follows: the polyaminoester emulsion of non-precipitation is added precipitation still, under vacuum or atmospheric pressure state, be heated to boiling, rectifying tower saves the steam at top by after condenser condenses, partial reflux, all the other are product solvent, control reflux ratio, make in product solvent, the weight content of water is lower than 0.5%, until in precipitation still, the weight content of solvent is lower than 0.5%.
3. method according to claim 2, is characterized in that, reflux ratio is 1 ~ 5; The solvent condensate depression of backflow is 0 DEG C ~ 10 DEG C.
4. method according to claim 3, is characterized in that, consisting of of the polyaminoester emulsion of described non-precipitation:
The ratio of urethane and solvent is 1:0.1 ~ 5, and the ratio of urethane and water is 1:0.1 ~ 19.
5. method according to claim 4, is characterized in that, described solvent is be selected from the one or two or more in acetone, butanone, tetrahydrofuran (THF) and ethyl acetate.
6. method according to claim 5, is characterized in that, precipitation still internal pressure is 0.001MPaA ~ 0.101325MPaA.
7. the method according to any one of claim 1 ~ 6, is characterized in that, upper part of described rectifying tower is filling-material structure, is highly more than or equal to 2 meters; Lower part is dual-flow tray type structure, is highly more than or equal to 2 meters, and stage number is 1 to 10 piece, and sieve plate and horizontal direction are 0-30 degree angle.
8. method according to claim 7, is characterized in that, the bottom of rectifying tower has a valve rectifying tower and precipitation still can be cut off.
9. the method according to any one of claim 1 ~ 6, is characterized in that, described precipitation still comprises kettle, precipitation liquid upcast, turbine and liquid distributing device;
Described precipitation liquid upcast is fixed on the inwall of described kettle by mounting block, gap is provided with the bottom of kettle bottom it, described turbine is arranged on the bottom of described precipitation liquid upcast, and be connected by the motor of rotating shaft with precipitation still outside, described liquid distributing device is arranged on the top of described precipitation liquid upcast;
Described liquid distributing device comprises ring-type separatory dish and overflow weir, and the inner circle of described ring-type separatory dish is connected with described precipitation liquid upcast, and described overflow weir is arranged on the outer rim of described ring-type separatory dish.
10. method according to claim 9, is characterized in that, described overflow weir is prionodont, and the diameter of shape separatory dish is 30 ~ 60% of kettle diameter.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114133504A (en) * | 2022-01-07 | 2022-03-04 | 天津华映蔚蓝科技有限公司 | General water-based resin for water-based ink and preparation method |
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