CN105524243B - The method that aqueous polyurethane production process removes solvent - Google Patents
The method that aqueous polyurethane production process removes solvent Download PDFInfo
- Publication number
- CN105524243B CN105524243B CN201610073078.5A CN201610073078A CN105524243B CN 105524243 B CN105524243 B CN 105524243B CN 201610073078 A CN201610073078 A CN 201610073078A CN 105524243 B CN105524243 B CN 105524243B
- Authority
- CN
- China
- Prior art keywords
- precipitation
- solvent
- rectifying column
- kettle
- column section
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Polyurethanes Or Polyureas (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a kind of methods that aqueous polyurethane production process removes solvent, are realized in a kind of precipitation kettle with rectifier unit, the precipitation kettle with rectifier unit, including precipitation kettle, rectifying column section and condenser；The bottom of the rectifying column section is connected with the precipitation kettle, the steam inlet of the condenser is connected with the steam (vapor) outlet at the top of rectifying column section, and the condensate outlet of the condenser is connected with the refluxing opening on the rectifying column section top and solvent collecting system respectively.Present invention employs the use in conjunction with precipitation kettle and rectifier unit, moisture is very low in the solvent distilled out, can be directly used for the production of aqueous polyurethane, it is effectively utilized the energy of desolvation process, the secondary refining process for eliminating solvent, reduces energy consumption, improves production efficiency.
Description
Technical field
The present invention relates to a kind of methods that aqueous polyurethane production process removes solvent.
Technical background
Aqueous polyurethane is that polyurethane is dispersed in water a kind of environment-protecting polyurethane to be formed by certain technological means
Product is mainly used in the numerous areas such as adhesive, coating and synthetic leather.
Aqueous polyurethane does not contain solvent for comparing oiliness polyurethane system, is typical environmentally friendly machine.Aqueous
In the production process of polyurethane, in order to make prepolymerization reaction be smoothed out, while in order to which performed polymer is smooth in emulsion process
Ground is dispersed in water, it usually needs it is viscous to reduce that acetone, butanone, n,N-Dimethylformamide equal solvent are added into performed polymer
Degree.After the completion of adding water emulsification to performed polymer, the solvent addition is needed to be removed from system, reaches product Water-borne modification, completely
Purpose without containing solvent.
Method of the acetone method as production aqueous polyurethane known in the industry, basic procedure are as follows：1) pass through first by
Isocyanates is reacted with polymer polyatomic alcohol and small molecule chain extender, obtains base polyurethane prepolymer for use as, in this process, is needed
Solvent is added to reduce the viscosity of performed polymer to effectively control reaction process, meanwhile, the performed polymer of low viscosity is added
Water emulsification can obtain good emulsifying effectiveness and reaction repeatability, ensure that production is smoothed out.2) when performed polymer has synthesized
Bi Hou, into performed polymer plus performed polymer is dispersed in water the polyaminoester emulsion to form non-precipitation by water under Strong shear effect.
3) polyaminoester emulsion of the non-precipitation emulsified is removed into the solvent being added in pre- collecting process by the method for distillation, is free of
The aqueous polyurethane product of solvent.4) solvent that distillation obtains is refined by the methods of rectifying, can be continued on for aqueous poly-
The production of urethane.
In above-mentioned production technology, the solvent for distilling generation is directly entered condenser and is condensed, and obtains containing a large amount of
The organic solvent solution of water, the process for removing solvent needs all to evaporate the solvent of addition, since gasification latent heat is huge, precipitation
Process is the step of most energy consumption in production aqueous polyurethane；On the other hand, contain large quantity of moisture in the solvent that precipitation generates, need
It is refined by rectifying, also the needing of the process consumes a large amount of energy.In above-mentioned method known in the industry, desolvation process
Single flash is only carried out, these obtained solution need to be refined again, can just obtain can be used for aqueous polyurethane production
Qualified solvent.In this process, the thermal energy that precipitation part uses is not used for the refined purification of solvent, but by condenser
It takes away, the utilization ratio of thermal energy is relatively low, and the energy of input is used for the purification of solvent and refines, and results in the need for using secondary fine
The method recycling design of system, entire production process energy consumption are very high.Therefore, there is an urgent need to a kind of sides of energy-efficient removing solvent
Method.
Invention content
The object of the present invention is to provide a kind of methods that aqueous polyurethane production process removes solvent, to overcome the prior art
Existing defect.
The method of the aqueous polyurethane production process removing solvent of the present invention, is in a kind of precipitation kettle with rectifier unit
Middle realization, the precipitation kettle with rectifier unit, including precipitation kettle, rectifying column section and condenser；
The bottom of the rectifying column section is connected with the precipitation kettle, the steam inlet of the condenser and rectifying
Steam (vapor) outlet at the top of tower section is connected, and the condensate outlet of the condenser is returned with the rectifying column section top respectively
Head piece is connected with solvent collecting system；
The method for removing solvent is as follows：The polyaminoester emulsion of non-precipitation is added precipitation kettle, under vacuum or normal pressure state,
It is heated to boiling, after the steam at the top of rectifying column section is condensed by condenser, partial reflux, remaining is product solvent, is controlled back
Flow ratio so that in product solvent, the weight content of water is less than 0.5%, until in precipitation kettle, the weight content of solvent is less than
0.5%；
The group of the polyaminoester emulsion of the non-precipitation becomes：
The ratio of polyurethane and solvent is 1:0.1~5, the ratio of polyurethane and water is 1:0.1~19；
The solvent is selected from one or both of acetone, butanone, tetrahydrofuran and ethyl acetate or a variety of；
Preferably, pressure is 0.001MPaA~0.101325MPaA in precipitation kettle；
Rectifying tower top temperature is 3 DEG C~50 DEG C low compared with precipitation temperature in the kettle；
The solvent degree of supercooling of reflux is 0 DEG C~10 DEG C, and reflux ratio is 1~5；
Preferably, the top half of the rectifying column is filling-material structure, is highly more than or equal to 2 meters；Lower half portion is to wear
Column plate type structure is flowed, is highly more than or equal to 2 meters, the number of plates is 1 to 10 piece, and sieve plate is in 0-30 degree angle with horizontal direction；
Preferably, the bottom of rectifying column has a valve that can separate rectifying column and precipitation kettle；
In the present invention, as a result of the use in conjunction with precipitation kettle and rectifier unit, moisture contains in the solvent distilled out
Amount is very low, can be directly used for the production of aqueous polyurethane, is effectively utilized the energy of desolvation process, eliminates the secondary of solvent
Subtractive process reduces energy consumption, improves production efficiency.
Description of the drawings
Fig. 1 is equipped with the structural schematic diagram of the precipitation kettle of rectifier unit.
Fig. 2 is precipitation kettle structural schematic diagram.
Specific implementation mode
Referring to Fig. 1, the method that aqueous polyurethane production process of the invention removes solvent is to carry rectifier unit in one kind
Precipitation kettle in realize, the precipitation kettle with rectifier unit, including precipitation kettle 1, rectifying column section 2 and condenser 3；
The bottom of the rectifying column section 2 is connected with the precipitation kettle 1, the steam inlet 301 of the condenser 3
Be connected with the steam (vapor) outlet 201 at the top of rectifying column section 2, the condensate outlet 302 of the condenser 3 respectively with the essence
The refluxing opening 202 for evaporating 2 top of tower section is connected with solvent collecting system 4；
The method for removing solvent is as follows：Precipitation kettle 1 is added in the polyaminoester emulsion of non-precipitation, is heated to 100~10 DEG C, control
Tower top temperature processed is 56.5~7 DEG C, and tower top temperature can be realized by adjusting vacuum degree；
Preferably, the precipitation kettle includes autoclave body 101, precipitation liquid tedge 102, turbine 103 and liquid distributing device；
The precipitation liquid tedge 102 is fixed on the inner wall of the autoclave body 101, bottom and autoclave body by fixing piece
101 bottom is equipped with gap 104, and the turbine 103 is arranged in the bottom of the precipitation liquid tedge 102, and by turning
Axis is connected with the motor outside precipitation kettle, and the liquid distributing device is arranged on the top of the precipitation liquid tedge 102；
The liquid distributing device includes cyclic annular liquid separation disk 105 and downflow weir 106, the inner circle of the cyclic annular liquid separation disk 105
It is connected with the precipitation liquid tedge 102, the outer rim in the cyclic annular liquid separation disk 105 is arranged in the downflow weir 106,
Preferably, the downflow weir 106 is sawtooth pattern, it is further preferred that the 30 of a diameter of autoclave body diameter of shape liquid separation disk 105~
60%；
Precipitation kettle using the above structure can be in a dynamic state evaporated by the material of desolventizing, and be formed downward
The waterfall shape liquid stream of flowing, can greatly improve evaporation efficiency.
The operation principle of the present invention is such：
In precipitation kettle, the polyaminoester emulsion of non-precipitation is heated, and passes through precipitation liquid tedge 102, turbine 103
And liquid distributing device so that the polyaminoester emulsion of non-precipitation is by precipitation liquid tedge 102, from 102 top of precipitation liquid tedge
Downflow weir 106 shunt and under so that the polyaminoester emulsion of non-precipitation disperses and under flow regime, by water and acetone evaporated, production
The material that raw solvent vapo(u)r enters rectifying column and reflux carries out heat and mass transfer, enter later reflux condenser total condensation at
Liquid, under the action of reflux ratio control device, a part of solvent vapo(u)r condensate liquid flows back into rectifying column and the solvent that steams
Heat and mass transfer is carried out, another part solvent vapo(u)r condensate liquid is as product discharge.
As desolvation process constantly carries out, remaining quantity of solvent is constantly reduced in the polyaminoester emulsion of non-precipitation, until de-
It is dissolved into, obtains not solvent-laden aqueous polyurethane product.
In embodiment, unless otherwise instructed, content is weight content.
Embodiment 1
By 1000 kilograms of polypropylene glycols, 2000,125 kilograms of 4,4- '-diphenylmethane diisocyanates, 67 kilograms of 2,2- dihydroxy first
Reaction kettle is added in base propionic acid and 124.2 kilograms of acetone, is warming up to 80 degrees Celsius and reacts 2 hours, is then cooled to 50 degrees Celsius,
50 kilograms of triethylamines are added, and the reaction was continued 30 minutes, obtains performed polymer.
Then it is separately added into a) 124.2 kilograms of water and b) 130 kilograms of water into performed polymer, is respectively obtained through strength emulsification：
1490.4 kilograms of the polyaminoester emulsion a) of non-precipitation and 1496.2 kilograms of polyaminoester emulsion b).
Embodiment 2
The polyaminoester emulsion a) of non-precipitation in embodiment 1 is added to the precipitation kettle of Fig. 1 devices；
The group of the polyaminoester emulsion a) of non-precipitation is divided into：
The ratio of polyurethane and solvent is 1:0.1, the ratio of polyurethane and water is 1:0.1
Rectifying column upper semisection height is 2 meters, built-in filler；The height of lower semisection is 2 meters, is provided with 1 piece of dual-flow tray,
Column plate plane is in 30 degree of angles with horizontal direction.
The polyaminoester emulsion a) of non-precipitation is heated to boiling, holding precipitation kettle pressure is 0.001MPaA, the solvent of generation
The material that steam enters rectifying column and reflux carries out heat and mass transfer, enters reflux condenser total condensation later into liquid, and one
The solvent that partial solvent steam condensate flows back into rectifying column and steams carries out heat and mass transfer, and another part solvent vapo(u)r is cold
Lime set directly discharges, and control reflux ratio is 5, and the condensate liquid degree of supercooling of reflux is 0 DEG C.
Precipitation is initial, and bottom temperature is 10 DEG C, and tower top temperature is 7 DEG C, and as desolvation process constantly carries out, non-precipitation gathers
Remaining quantity of solvent is constantly reduced in urethane lotion, until precipitation is completed, bottom temperature rises to 40 DEG C at this time, and tower top temperature is
30 DEG C, rectifier bottoms valve is closed, prevents from holding liquid refluence polluted product in tower.
Finally obtain 1366.2 kilograms of the aqueous polyurethane product that organic solvent weight content is less than 0.5%, moisture weight
Content is less than 0.5% 124.2 kilograms of acetone.
Obtained aqueous polyurethane product is certified products, can direct marketing；
It recycles obtained acetone to be not required to refine, the production of aqueous polyurethane can be re-used for.Profit carries out with the aforedescribed process
Precipitation, whole process consume 0.14 ton of 0.3MPaG steam.
Embodiment 3
As the comparative example of embodiment 2, embodiment 3 carries out precipitation, specific mistake using conventional desolventizing method known in the industry
Journey is that the polyaminoester emulsion b) additions of non-precipitation in embodiment 1 are equipped only in the precipitation kettle of condenser, is gathered to non-precipitation
Urethane lotion b) is heated.
Holding precipitation kettle pressure is 0.001MPaA, and the condensed device total condensation of solvent vapo(u)r of generation discharges at liquid.With
It desolvation process constantly to carry out, remaining quantity of solvent is constantly reduced in the polyaminoester emulsion of non-precipitation, until precipitation is completed, is obtained
Organic solvent content is less than 0.5% 1366.2 kilograms of aqueous polyurethane product, the acetone 130,000 that moisture is 4.46%
Gram.Since moisture is excessively high in acetone, it is impossible to be used in the production of aqueous polyurethane needs to be refined again, water can be obtained
Content is divided to be less than 0.5% 124.2 kilograms of acetone, content of acetone is less than 0.5% 5.8 kilograms of waste water.Desolvation process consumes
0.052 ton of 0.3MPaG steam, subtractive process consume 0.125 ton of 0.3MPaG steam, therefore, obtain production same as Example 2
Product consume 0.176 ton of 0.3MPaG steam altogether.
Embodiment 4
By 1000 kilograms of polypropylene glycols, 2000,1001 kilograms of 4,4- '-diphenylmethane diisocyanates, 67 kilograms of 2,2- dihydroxies
Reaction kettle is added in methylpropanoic acid and 10590 kilograms of acetone, is warming up to 80 degrees Celsius and reacts 2 hours, it is Celsius to be then cooled to 50
Degree, 50 kilograms of triethylamines are added, and the reaction was continued 30 minutes, obtains performed polymer.Then a) 40,242,000 are separately added into performed polymer
Gram water and b) 42242 kilograms of water respectively obtain 52950 kilograms of the polyaminoester emulsion a) and polyurethane breast of non-precipitation through strength emulsification
54950 kilograms of liquid b).
Embodiment 5
By the polyaminoester emulsion a) of the non-precipitation in embodiment 4 be added equipped with rectifying column, reflux ratio control device and
In the precipitation kettle of reflux condenser, the ratio of polyurethane and solvent is 1:5, the ratio of polyurethane and water is 1:19
Rectifying column upper semisection height is 10 meters, built-in filler；The height of lower semisection is 5 meters, is provided with 10 pieces of percolation towers
Plate, column plate plane are in 0 degree of angle with horizontal direction.Rectifying column lower semisection liner is Kynoar, and column plate material is polyvinylidene fluoride
Alkene.The polyaminoester emulsion a) of non-precipitation is heated to boiling, holding precipitation kettle pressure is 0.101325MPaA, and the solvent of generation steams
The material that vapour enters rectifying column and reflux carries out heat and mass transfer, enters reflux condenser total condensation later into liquid, one
The solvent that solvent vapo(u)r condensate liquid flows back into rectifying column and steams is divided to carry out heat and mass transfer, the condensation of another part solvent vapo(u)r
Liquid directly discharges, and control reflux ratio is 1, and the condensate liquid degree of supercooling of reflux is 10 DEG C.Precipitation is initial, and bottom temperature is 60 DEG C, tower
It is 56.5 DEG C to push up temperature, and as desolvation process constantly carries out, remaining quantity of solvent is constantly reduced in the polyaminoester emulsion of non-precipitation,
Until precipitation is completed, bottom temperature rises to 106.5 DEG C, and tower top temperature is 56.5 degree, closes rectifier bottoms valve, prevents tower
It inside holds liquid and flows backwards polluted product.Finally obtain 42360 kilograms of the aqueous polyurethane product that organic solvent content is less than 0.5%, water
Content is divided to be less than 0.5% 10590 kilograms of acetone.The aqueous polyurethane product that embodiment 5 obtains is certified products, can directly be sold
It sells；It recycles obtained acetone to be not required to refine, the production of aqueous polyurethane can be re-used for.Profit carries out precipitation with the aforedescribed process,
Whole process consumes 12.04 tons of 0.3MPaG steam.
Embodiment 6
As the comparative example of embodiment 5, embodiment 6 carries out precipitation, specific mistake using conventional desolventizing method known in the industry
Journey is that the polyaminoester emulsion b) additions of non-precipitation in embodiment 4 are equipped only in the precipitation kettle of condenser, is gathered to non-precipitation
Urethane lotion b) is heated；
Holding precipitation kettle pressure is 0.101325MPaA, and the condensed device total condensation of solvent vapo(u)r of generation is at liquid discharge
Material.As desolvation process constantly carries out, remaining quantity of solvent is constantly reduced in the polyaminoester emulsion of non-precipitation, until precipitation is complete
At, obtain organic solvent content be less than 0.5% 42360 kilograms of aqueous polyurethane product, moisture be 15.88% acetone
12590 kilograms.Since moisture is excessively high in acetone, it is impossible to be used in the production of aqueous polyurethane needs to be refined again, can
10590 kilograms of the acetone that moisture is less than 0.5% is obtained, content of acetone is less than 0.5% 2000 kilograms of waste water.Desolvation process
3.75 tons of 0.3MPaG steam is consumed, subtractive process consumes 11.8 tons of 0.3MPaG steam, therefore, obtains same as Example 5
Product consumes 15.5 tons of 0.3MPaG steam altogether.
Claims (4)
1. the method that aqueous polyurethane production process removes solvent, which is characterized in that be in a kind of precipitation with rectifier unit
It is realized in kettle, the precipitation kettle with rectifier unit, including precipitation kettle, rectifying column section and condenser；
The bottom of the rectifying column section is connected with the precipitation kettle, steam inlet and the rectifying column section of the condenser
The steam (vapor) outlet at top is connected, the condensate outlet of the condenser refluxing opening with the rectifying column section top respectively
It is connected with solvent collecting system；
The precipitation kettle includes autoclave body, precipitation liquid tedge, turbine and liquid distributing device；
The precipitation liquid tedge is fixed on the inner wall of the autoclave body by fixing piece, and the bottom of bottom and autoclave body is equipped with
Gap, the turbine is arranged in the bottom of the precipitation liquid tedge, and passes through shaft and the motor phase outside precipitation kettle
Connection, the liquid distributing device are arranged on the top of the precipitation liquid tedge；
The liquid distributing device includes cyclic annular liquid separation disk and downflow weir, the inner circle of the cyclic annular liquid separation disk and the precipitation liquid
Tedge is connected, and the outer rim in the cyclic annular liquid separation disk is arranged in the downflow weir；
The downflow weir be sawtooth pattern, the 30 ~ 60% of a diameter of autoclave body diameter of cyclic annular liquid separation disk；
The method of the removing solvent is as follows：Precipitation kettle, vacuum or normal pressure state is added in the polyaminoester emulsion of non-precipitation
Under, it is heated to boiling, after the steam at the top of rectifying column section is condensed by condenser, partial reflux, remaining is product solvent, control
Reflux ratio so that in product solvent, the weight content of water is less than 0.5%, until in precipitation kettle, the weight content of solvent is less than
0.5%；Wherein the reflux ratio is 1 ~ 5, and the solvent degree of supercooling of reflux is 0 DEG C ~ 10 DEG C；
The solvent is selected from one or more of acetone, butanone, tetrahydrofuran and ethyl acetate.
2. according to the method described in claim 1, it is characterized in that, the group of the polyaminoester emulsion of the non-precipitation becomes：
The ratio of polyurethane and solvent is 1:0.1 ~ 5, the ratio of polyurethane and water is 1:0.1~19.
3. according to claim 1 ~ 2 any one of them method, which is characterized in that the top half of the rectifying column section is to fill out
Expect structure, is highly more than or equal to 2 meters；Lower half portion is dual-flow tray type structure, is highly more than or equal to 2 meters, the number of plates is 1 to 10
Block, column plate are in 0-30 degree angle with horizontal direction.
4. according to the method described in claim 3, it is characterized in that, the bottom of rectifying column section has a valve can be by rectifying column and de-
Molten kettle partition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610073078.5A CN105524243B (en) | 2016-02-02 | 2016-02-02 | The method that aqueous polyurethane production process removes solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610073078.5A CN105524243B (en) | 2016-02-02 | 2016-02-02 | The method that aqueous polyurethane production process removes solvent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105524243A CN105524243A (en) | 2016-04-27 |
| CN105524243B true CN105524243B (en) | 2018-08-31 |
Family
ID=55766791
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610073078.5A Active CN105524243B (en) | 2016-02-02 | 2016-02-02 | The method that aqueous polyurethane production process removes solvent |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105524243B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201952390U (en) * | 2010-12-13 | 2011-08-31 | 安徽好思家涂料有限公司 | High-efficiency acetone recovery device in production of waterborne polyurethane by using acetone method |
| CN103304389A (en) * | 2013-04-29 | 2013-09-18 | 珠海醋酸纤维有限公司 | Improved dilute acetone solution distillation method |
| CN203400514U (en) * | 2013-07-25 | 2014-01-22 | 浙江科泓化工有限公司 | Hydroxy propyl cellulose solvent recycling device |
| CN203403035U (en) * | 2013-07-25 | 2014-01-22 | 浙江科泓化工有限公司 | Hydroxy propyl cellulose desolvation device |
| CN203790608U (en) * | 2014-04-14 | 2014-08-27 | 巨化集团技术中心 | Polymer solvent continuous removal-recovery system for water-based oil repellent mold discharging agent |
| CN203938624U (en) * | 2014-04-14 | 2014-11-12 | 合肥市科天化工有限公司 | The semicontinuous aqueous polyurethane production line of a kind of mass-producing |
| CN104906822A (en) * | 2015-06-02 | 2015-09-16 | 湖南湘江关西涂料有限公司 | Device and method for eliminating and recycling organic solvent from cathode electrophoresis emulsion |
-
2016
- 2016-02-02 CN CN201610073078.5A patent/CN105524243B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201952390U (en) * | 2010-12-13 | 2011-08-31 | 安徽好思家涂料有限公司 | High-efficiency acetone recovery device in production of waterborne polyurethane by using acetone method |
| CN103304389A (en) * | 2013-04-29 | 2013-09-18 | 珠海醋酸纤维有限公司 | Improved dilute acetone solution distillation method |
| CN203400514U (en) * | 2013-07-25 | 2014-01-22 | 浙江科泓化工有限公司 | Hydroxy propyl cellulose solvent recycling device |
| CN203403035U (en) * | 2013-07-25 | 2014-01-22 | 浙江科泓化工有限公司 | Hydroxy propyl cellulose desolvation device |
| CN203790608U (en) * | 2014-04-14 | 2014-08-27 | 巨化集团技术中心 | Polymer solvent continuous removal-recovery system for water-based oil repellent mold discharging agent |
| CN203938624U (en) * | 2014-04-14 | 2014-11-12 | 合肥市科天化工有限公司 | The semicontinuous aqueous polyurethane production line of a kind of mass-producing |
| CN104906822A (en) * | 2015-06-02 | 2015-09-16 | 湖南湘江关西涂料有限公司 | Device and method for eliminating and recycling organic solvent from cathode electrophoresis emulsion |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105524243A (en) | 2016-04-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103881050B (en) | A kind of preparation method of light polyisocyanate curing agent | |
| CN106430228B (en) | Molecular sieve mother solution processing method | |
| CN103833050B (en) | A kind for the treatment of process of Padil dealcoholization mother liquid of containing ammonium chloride | |
| CN101624400B (en) | Production method of triethyl phosphite | |
| CN103333080B (en) | Quadruple-effect method for rectifying and recycling waste water containing DMF (dimethyl formamide) | |
| CN208732977U (en) | A kind of tetrahydrofuran purifying plant | |
| CN105246869A (en) | Process to prepare levulinic acid | |
| CN104968636A (en) | Device for preparing alkanol | |
| CN102311768B (en) | Reduced-pressure flash tank and crude oil reduced-pressure deep drawing method | |
| CN107365253A (en) | A kind of propylene glycol methyl ether acetate distillation system and its rectificating method | |
| CN102311769B (en) | Reduced-pressure flash tank and crude oil processing method | |
| CN202715258U (en) | Integrated atomizing membrane distilling apparatus | |
| CN105503933B (en) | A kind of chemical industry monomer energy-saving rectifying device and method | |
| CN105524243B (en) | The method that aqueous polyurethane production process removes solvent | |
| CN105315132A (en) | System and method used for energy utilization between ethylene glycol device dehydrating tower and refining tower | |
| CN102391064B (en) | Process for recovering and refining extracting agent in production procedure of hexanolactam | |
| CN107915580A (en) | A kind of ethylene glycol multi-effect distillation system and process | |
| CN107098854B (en) | Ethoxyquinoline continuous production method | |
| CN105061187A (en) | A process for continuously producing m-toluic acid | |
| CN107848925A (en) | Phenol purifying method | |
| CN105732316A (en) | Glycerinum refining system | |
| CN204034298U (en) | A kind of sub-boiling distillation device | |
| CN209010425U (en) | A kind of tetrahydrofuran reaction separating device | |
| CN102432790B (en) | Method for preparing polyurethane curing agent | |
| CN104370696A (en) | Novel method for separating ethylene glycol and 1,2-pentanediol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| TA01 | Transfer of patent application right |
Effective date of registration: 20170804 Address after: 201507 Shanghai city Jinshan District Yuegong Road No. 1369 building 101 room 2 Applicant after: Shanghai Huafon New Material Research & Development Technology Co., Ltd. Address before: 200120, 12, Lane 572, Lane 115, blue wave road, Zhangjiang hi tech park, Shanghai, Pudong New Area Applicant before: Shanghai Huafeng material science and Technology Research Institute (limited partnership) |
|
| TA01 | Transfer of patent application right | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |