CN105837789B - The method of extraction removing solvent in aqueous polyurethane production process - Google Patents
The method of extraction removing solvent in aqueous polyurethane production process Download PDFInfo
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- CN105837789B CN105837789B CN201610220757.0A CN201610220757A CN105837789B CN 105837789 B CN105837789 B CN 105837789B CN 201610220757 A CN201610220757 A CN 201610220757A CN 105837789 B CN105837789 B CN 105837789B
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- 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
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Abstract
The invention discloses a kind of methods of extraction removing solvent in aqueous polyurethane production process comprising the steps of: extractant is in contact with the polyaminoester emulsion of non-desolventizing, then collects extraction phase raffinate phase respectively, can be obtained the polyaminoester emulsion of removing solvent；The extractant includes the positive structure or isoparaffin of C5~C30, the positive structure or isomeric olefine or polyene of C5~C30, the positive structure perhaps composition of isomery eneyne or above-mentioned substance of the positive structure or isomery alkynes of C5~C30 perhaps polyine C5~C30.The percent extraction of polymer solvent of the present invention is greater than 99%, and the residual quantity of polymer solvent is lower than 1% in aqueous polyurethane.The present invention be able to solve aqueous polyurethane production in desolvation process energy consumption it is higher, the defect of unstable product quality, be convenient for industrializing implementation.
Description
Technical field
The present invention relates to a kind of aqueous polyurethane production processes to remove solvent method.
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 compared to oiliness polyurethane system and
Speech does not contain solvent, or contains minimal amount of solvent, is typical environmentally friendly machine.In the production process of aqueous polyurethane
In, in order to go on smoothly prepolymerization reaction, while in order to which performed polymer to be successfully dispersed in water in emulsion process, usually
Need to be added the polymer solvents such as acetone, butanone, N,N-dimethylformamide into performed polymer to reduce viscosity.Add when to performed polymer
After the completion of water emulsification, needs the solvent of addition to remove from system, reach product Water-borne modification, be entirely free of the mesh of solvent
's.
Method of the above-mentioned solvent method as production aqueous polyurethane known in the industry, basic procedure are as follows: 1) logical first
It crosses and reacts isocyanates with polymer polyatomic alcohol and small molecule chain extender, obtain base polyurethane prepolymer for use as, in the process
In, it needs to be added polymer solvent to reduce the viscosity of performed polymer and effectively controls reaction process, meanwhile, the pre-polymerization to low viscosity
Body carries out plus water emulsification can obtain good emulsifying effectiveness and reaction repeatability, guarantees that production is gone on smoothly.2) work as pre-polymerization
After body synthesizes, into performed polymer plus performed polymer is dispersed in water the poly- ammonia to form non-precipitation under Strong shear effect by water
Ester lotion.3) polymerization polyaminoester emulsion of the non-precipitation emulsified being added by the method removing of distillation in pre- collecting process is molten
Agent obtains not solvent-laden aqueous polyurethane product.4) polymer solvent that distillation obtains is refined by the methods of rectifying, can
Continue on for the production of aqueous polyurethane.
In above-mentioned precipitation technique known in the industry, the polymer solvent for distilling generation is directly entered condenser and is condensed,
The polymer solvent solution containing a large amount of water is obtained, the process for removing polymer solvent needs all to evaporate the solvent of addition, due to
Gasification latent heat is huge, and desolvation process is the step of most energy consumption in production aqueous polyurethane；On the other hand, the polymerization that precipitation generates is molten
Contain large quantity of moisture in agent, need to be refined by rectifying, which also needs to consume a large amount of energy.
It in well known desolvation process in the field of business, needs to heat polyaminoester emulsion, this will lead to stability of emulsion change
Difference influences product quality.The polyaminoester emulsion poor for temperature tolerance needs to take off by improving the means such as vacuum degree and reducing
Solubility temperature also will lead to energy consumption height, while there is also the hidden danger that overtemperature generates waste material.Therefore, there is an urgent need to a kind of efficiently sections
The method that can also can guarantee the removing solvent of product quality simultaneously.
Summary of the invention
It is existing to overcome it is an object of the present invention to provide a kind of method of extraction removing solvent in aqueous polyurethane production process
Defect existing for technology.
It comprises the steps of: and extractant is in contact with the polyaminoester emulsion of non-desolventizing, then collect extraction phase respectively
Raffinate phase can be obtained the polyaminoester emulsion of removing solvent；
The solvent is acetone, butanone, n,N-Dimethylformamide, n,N-dimethylacetamide, ethyl acetate, acetic acid
Butyl ester, toluene, tetrahydrofuran, chloroform or above-mentioned substance composition；
The polyaminoester emulsion of the non-desolventizing is that a kind of polyurethane latex particle is swollen and is scattered in by polymer solvent
Lotion in water, this is a kind of intermediate products of aqueous polyurethane production process known in the industry.It is produced using solvent method aqueous
Polyurethane requires experience lotion precipitation this operation step；
The selection of extractant described in this patent is relatively difficult, polymer solvent in the non-precipitation lotion of satisfaction extraction
1) extractant, which needs to have the property that, cannot dissolve or be swollen polyurethane latex particle, otherwise can be mingled in product a large amount of
Extractant seriously affects product quality and subsequent applications；2) otherwise the necessary very little of solubility in water will lead to aqueous poly-
A large amount of extractants are remained in urethane, cause final products VOC exceeded, lose the meaning of polyurethane aqueousization；3) with polymerize use
Solvent have good compatibility, which dictates that operation energy consumption and equipment investment, inappropriate extractant will make to produce
Cost increases substantially, and loses the competitiveness with way of distillation precipitation；4) there is biggish surface tension between water, it cannot be not
It is emulsified in the polyaminoester emulsion of precipitation, causes extractant that can not separate from raffinate phase；5) to polyaminoester emulsion stability
It cannot have an impact, otherwise will lead to emulsion breaking, directly generation waste material；6) extractant must cannot be reacted with polymer solvent and
It can be easily separated, otherwise will increase the cost of desolvation process, decline the competitiveness of this method.
Inventors have found that the range for meeting the extractant of above-mentioned condition is very narrow, positive structure or isomery including C5~C30
Alkane, the positive structure or isomeric olefine of C5~C30 perhaps positive structure of polyene C5~C30 or isomery alkynes or polyine,
Perhaps the composition of isomery eneyne or above-mentioned substance can satisfy requirement to the positive structure of C5~C30；
Preferably, extractant is the mixture of saturated hydrocarbons and unsaturated hydrocarbons, and weight ratio is 1:99~99:1；
Preferably, the weight ratio of the polyaminoester emulsion of the non-desolventizing and the extractant is 1:0.1 to 1:100；
Preferably, extractant is pentane, the polyaminoester emulsion of the non-desolventizing and the weight ratio of the extractant are as follows:
10:1~2；
Preferably, extractant is the mixture of hexadecane and 4- vinyl -4- heptene -2- alkynes, and weight ratio is 95~99:
1；The polyaminoester emulsion of the non-desolventizing and the weight ratio of the extractant are as follows: 10:1000~1200；
Preferably, extractant is positive the mixture of melissane and positive octadecylene, and weight ratio is 1:95~99；
The polyaminoester emulsion of the non-desolventizing and the weight ratio of the extractant are as follows: 10:1000~1200；
Preferably, in the polyaminoester emulsion of non-desolventizing, the weight percent of each component is as follows:
Polyurethane 0.1~59.9%
Solvent 0.1~59.9%
Water 40.0~99.8%；
The time of extracting operation and temperature can also have an impact product quality and investment, the liquid-liquid extraction condition packet
It includes and the polyaminoester emulsion of the non-desolventizing and the extractant is mixed about 0.5 minute to about 30 minutes, operation temperature 0
~50 DEG C.It is free of or qualified aqueous polyurethane containing only minute quantity polymer solvent produces to reach to directly acquire after extraction
The purpose of product, extractant phase carry out under conditions of counter-current extraction with the contact of the non-precipitation polyaminoester emulsion；
Preferably, the extracting operation carries out in rotating disc column, includes the following steps:
The polyaminoester emulsion of non-desolventizing is cooled to 0~50 DEG C, with 10 kg/min of rate from turntable extracting tower
Top is passed through, and extractant is cooled to 0~50 DEG C, is passed through with 1~1000 kg/min of rate from the lower part of rotating disc column, extraction
Tower temperature degree is equally maintained at 0 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 0.5~30 minute, from the bottom of rotating disc column
Raffinate phase is collected in portion, from the collected overhead extraction phase of rotating disc column.
Method of the invention, the percent extraction of polymer solvent are greater than 99%, the residual of polymer solvent in aqueous polyurethane
Amount is lower than 1%.
Term " percent extraction " is defined as follows:
The percentage of polymer solvent in non-precipitation lotion is accounted for by the polymer solvent that extractant extracts.
The residual quantity of polymer solvent refers to weight percent in aqueous polyurethane；
The present invention be able to solve aqueous polyurethane production in desolvation process energy consumption it is higher, the defect of unstable product quality,
It is easy to operate, it is convenient for industrializing implementation.
Specific embodiment
For a better understanding of the present invention, below with reference to embodiment, the present invention will be further described, but reality of the invention
It is without being limited thereto to apply mode.
Embodiment 1
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 0.1%, solvent 0.1%, water 99.8%；
Solvent is acetone；Extractant is pentane；
The polyaminoester emulsion of non-desolventizing is cooled to 0 DEG C, with 10 kg/min of rate from the upper of a turntable extracting tower
Portion is passed through, and extractant pentane is cooled to 0 DEG C, is passed through with 1 kg/min of rate from the lower part of rotating disc column, extraction tower temperature
It is equally maintained at 0 DEG C, the residence time of the polyaminoester emulsion of non-desolventizing is 0.5 minute, from the bottom collection raffinate of rotating disc column
Phase, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, polymer solvent in aqueous polyurethane
Residual quantity be lower than 1%.
Embodiment 2
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 0.1%, solvent 59.9%, water 40%；
Solvent is butanone；Extractant is positive the mixture of melissane and positive octadecylene, weight ratio 1:99；
The polyaminoester emulsion of non-desolventizing is cooled to 50 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant is warming up to 50 DEG C, is passed through with 1000 kg/min of rate from the lower part of rotating disc column, extracts tower temperature
Degree is equally maintained at 50 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 30 minutes；
From the bottom collection raffinate phase of rotating disc column, from the collected overhead extraction phase of rotating disc column, the extraction percentage of polymer solvent
Rate is greater than 99.9%, and the residual quantity of polymer solvent is lower than 0.02% in aqueous polyurethane.
Embodiment 3
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 59.9%, solvent 0.1%, water 40%；
Solvent is N,N-dimethylformamide；Extractant is the mixing of hexadecane and 4- vinyl -4- heptene -2- alkynes
Object, weight ratio 99:1；
The polyaminoester emulsion of non-desolventizing is warming up to 50 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant is warming up to 50 DEG C, is passed through with 1000 kg/min of rate from the lower part of rotating disc column, extracts tower temperature
Degree is equally maintained at 50 DEG C, and the residence time of the lotion of non-desolventizing is 30 minutes, other are the same as embodiment 1；
The percent extraction of polymer solvent is greater than 99.5%, and the residual quantity of polymer solvent is lower than in aqueous polyurethane
0.03%.
Embodiment 4
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 33%, solvent 33%, water 34%；
Solvent is DMAC N,N' dimethyl acetamide；Extractant is positive melissane；
The polyaminoester emulsion of non-desolventizing is warming up to 45 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant pentane is warming up to 45 DEG C, is passed through with 2 kg/min of rate from the lower part of rotating disc column, and tower temperature is extracted
Degree is equally maintained at 45 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 1 minute, from the bottom collection raffinate of rotating disc column
Phase, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99.3%, polymerize in aqueous polyurethane molten
The residual quantity of agent is lower than 0.5%.
Embodiment 5
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 35%, solvent 35%, water 30%；
Solvent is ethyl acetate；Extractant is neopentane；
The polyaminoester emulsion of non-desolventizing is cooled to 4 DEG C, with 10 kg/min of rate from the upper of a turntable extracting tower
Portion is passed through, and extractant pentane is cooled to 4 DEG C, is passed through with 3 kg/min of rate from the lower part of rotating disc column, extraction tower temperature
Equally it is maintained at 4 DEG C, the residence time of the polyaminoester emulsion of non-desolventizing is 5 minutes, from the bottom collection raffinate phase of rotating disc column,
From the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, polymer solvent in aqueous polyurethane
Residual quantity is lower than 1%.
Embodiment 6
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 30%, solvent 40%, water 30%；
Solvent is butyl acetate；Extractant is 3- propyl heptacosane；
The polyaminoester emulsion of non-desolventizing is warming up to 40 DEG C, with double centner/minute rate from a turntable extracting tower
Top is passed through, and extractant pentane is warming up to 40 DEG C, is passed through with 180 kg/min of rate from the lower part of rotating disc column, extraction tower
Temperature is equally maintained at 40 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 10 minutes, from the bottom collection of rotating disc column
Raffinate phase, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99.4%, gathers in aqueous polyurethane
The residual quantity of bonding solvent is lower than 0.1%.
Embodiment 7
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 10%, solvent 10%, water 80%；
Solvent is toluene；Extractant is 2- amylene；
The polyaminoester emulsion of non-desolventizing is cooled to 1 DEG C, with 1000 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant pentane is cooled to 1 DEG C, is passed through with double centner/minute rate from the lower part of rotating disc column, extraction tower
Temperature is equally maintained at 1 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 16 minutes, extracts from the bottom collection of rotating disc column
Yu Xiang, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99.1%, polymerize in aqueous polyurethane
The residual quantity of solvent is lower than 0.1%.
Embodiment 8
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 10%, solvent 10%, water 80%；
Solvent is tetrahydrofuran；Extractant is 1- amylene；
The polyaminoester emulsion of non-desolventizing is cooled to 3 DEG C, with 10 kg/min of rate from the upper of a turntable extracting tower
Portion is passed through, and extractant pentane is cooled to 3 DEG C, is passed through with 1 kg/min of rate from the lower part of rotating disc column, extraction tower temperature
3 DEG C are equally maintained at, the residence time of the polyaminoester emulsion of non-desolventizing is 25 minutes, from the bottom collection raffinate of rotating disc column
Phase, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, polymer solvent in aqueous polyurethane
Residual quantity be lower than 1%.
Embodiment 9
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 40%, solvent 13%, water 50%；
Solvent is chloroform；Extractant is 30 alkene of 1-；
The polyaminoester emulsion of non-desolventizing is warming up to 50 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant pentane is warming up to 50 DEG C, is passed through with 10 kg/min of rate from the lower part of rotating disc column, extraction tower
Temperature is equally maintained at 50 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 15 minutes, from the bottom collection of rotating disc column
Raffinate phase, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, polymerize in aqueous polyurethane
The residual quantity of solvent is lower than 1%.
Embodiment 10
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 49%, solvent 1%, water 50%；
Solvent is the mixture (weight ratio 1:1) of butanone and acetone；Extractant is 30 alkene of 3-；
The polyaminoester emulsion of non-desolventizing is warming up to 49 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant pentane is warming up to 49 DEG C, is passed through with 1 kg/min of rate from the lower part of rotating disc column, and tower temperature is extracted
Degree is equally maintained at 49 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 20 minutes, extracts from the bottom collection of rotating disc column
Yu Xiang, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99.5%, polymerize in aqueous polyurethane
The residual quantity of solvent is lower than 0.5%.
Embodiment 11
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 45%, solvent 5%, water 50%；
Solvent is acetone；Extractant is 1- pentyne；
The polyaminoester emulsion of non-desolventizing is cooled to 0 DEG C, with double centner/minute rate from a turntable extracting tower
Top is passed through, and extractant pentane is cooled to 0 DEG C, is passed through with 150 kg/min of rate from the lower part of rotating disc column, extraction tower
Temperature is equally maintained at 0 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 2 minutes, extracts from the bottom collection of rotating disc column
Yu Xiang, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, polymerize in aqueous polyurethane molten
The residual quantity of agent is lower than 1%.
Embodiment 12
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 33%, solvent 33%, water 34%；
Solvent is acetone；Extractant is valerylene；
The polyaminoester emulsion of non-desolventizing is cooled to 0 DEG C, with 10 kg/min of rate from the upper of a turntable extracting tower
Portion is passed through, and extractant pentane is cooled to 0 DEG C, is passed through with 10 kg/min of rate from the lower part of rotating disc column, extraction tower temperature
It is equally maintained at 0 DEG C, the residence time of the polyaminoester emulsion of non-desolventizing is 24 minutes, from the bottom collection raffinate of rotating disc column
Phase, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, polymer solvent in aqueous polyurethane
Residual quantity be lower than 1%.
Embodiment 13
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 33%, solvent 33%, water 34%；
Solvent is acetone；Extractant is 30 alkynes of 1-；
The polyaminoester emulsion of non-desolventizing is warming up to 48 DEG C, with double centner/minute rate from a turntable extracting tower
Top is passed through, and extractant pentane is warming up to 48 DEG C, is passed through with 16 kg/min of rate from the lower part of rotating disc column, extraction tower
Temperature is equally maintained at 48 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 18 minutes, from the bottom collection of rotating disc column
Raffinate phase, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, polymerize in aqueous polyurethane
The residual quantity of solvent is lower than 1%.
Embodiment 14
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 30%, solvent 30%, water 40%；
Solvent is acetone；Extractant is 30 alkynes of 10-；
The polyaminoester emulsion of non-desolventizing is warming up to 49.5 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top be passed through, extractant pentane is warming up to 49.5 DEG C, be passed through with 13 kg/min of rate from the lower part of rotating disc column, extract
Tower temperature degree is taken equally to be maintained at 49.5 DEG C, the residence time of the polyaminoester emulsion of non-desolventizing is 9 minutes, from the bottom of rotating disc column
Raffinate phase is collected, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, in aqueous polyurethane
The residual quantity of polymer solvent is lower than 1%.
Embodiment 15
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 30%, solvent 30%, water 40%；
Solvent is acetone；Extractant is 1,5- pentadiene；
The polyaminoester emulsion of non-desolventizing is cooled to 0 DEG C, with 10 kg/min of rate from the upper of a turntable extracting tower
Portion is passed through, and extractant pentane is cooled to 0 DEG C, is passed through with 1 kg/min of rate from the lower part of rotating disc column, extraction tower temperature
It is equally maintained at 0 DEG C, the residence time of the polyaminoester emulsion of non-desolventizing is 1.5 minutes, from the bottom collection raffinate of rotating disc column
Phase, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, polymer solvent in aqueous polyurethane
Residual quantity be lower than 1%.
Embodiment 16
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 30%, solvent 30%, water 40%；
Solvent is acetone；Extractant is 30 carbon diene of 1,5-；
The polyaminoester emulsion of non-desolventizing is warming up to 50 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant pentane is warming up to 50 DEG C, is passed through with 19 kg/min of rate from the lower part of rotating disc column, extraction tower
Temperature is equally maintained at 50 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 1 minute, extracts from the bottom collection of rotating disc column
Yu Xiang, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, polymerize in aqueous polyurethane molten
The residual quantity of agent is lower than 1%.
Embodiment 17
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 30%, solvent 30%, water 40%；
Solvent is acetone；Extractant is 1,5- pentadiine；
The polyaminoester emulsion of non-desolventizing is cooled to 0 DEG C, with 10 kg/min of rate from the upper of a turntable extracting tower
Portion is passed through, and extractant pentane is cooled to 0 DEG C, is passed through with 15 kg/min of rate from the lower part of rotating disc column, extraction tower temperature
Equally it is maintained at 0 DEG C, the residence time of the polyaminoester emulsion of non-desolventizing is 3 minutes, from the bottom collection raffinate phase of rotating disc column,
From the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, polymer solvent in aqueous polyurethane
Residual quantity is lower than 1%.
Embodiment 18
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 30%, solvent 30%, water 40%；
Solvent is acetone；Extractant is 30 carbon diine of 1,5-；
The polyaminoester emulsion of non-desolventizing is warming up to 48 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant pentane is warming up to 48 DEG C, is passed through with 11 kg/min of rate from the lower part of rotating disc column, extraction tower
Temperature is equally maintained at 48 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 10 minutes, from the bottom collection of rotating disc column
Raffinate phase, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, polymerize in aqueous polyurethane
The residual quantity of solvent is lower than 1%.
Embodiment 19
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 30%, solvent 30%, water 40%；
Solvent is acetone；Extractant is 1- butene-2-methyl-3- alkynes；
The polyaminoester emulsion of non-desolventizing is cooled to 0 DEG C, with 10 kg/min of rate from the upper of a turntable extracting tower
Portion is passed through, and extractant pentane is cooled to 0 DEG C, is passed through with 12 kg/min of rate from the lower part of rotating disc column, extraction tower temperature
It is equally maintained at 0 DEG C, the residence time of the polyaminoester emulsion of non-desolventizing is 0.8 minute, from the bottom collection raffinate of rotating disc column
Phase, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, polymer solvent in aqueous polyurethane
Residual quantity be lower than 1%.
Embodiment 20
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 30%, solvent 30%, water 40%；
Solvent is acetone；Extractant is 1- butylene -4- alkynes；
The polyaminoester emulsion of non-desolventizing is cooled to 0 DEG C, with 10 kg/min of rate from the upper of a turntable extracting tower
Portion is passed through, and extractant pentane is cooled to 0 DEG C, is passed through with 1000 kg/min of rate from the lower part of rotating disc column, and tower temperature is extracted
Degree is equally maintained at 0 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 2 minutes, from the bottom collection raffinate of rotating disc column
Phase, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99%, polymer solvent in aqueous polyurethane
Residual quantity be lower than 1%.
Embodiment 21
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 30%, solvent 30%, water 40%；
Solvent is the mixture (1:1, weight ratio) of acetone and n,N-Dimethylformamide；Extractant is 1- melene-
6- butyl -10- alkynes；
The polyaminoester emulsion of non-desolventizing is warming up to 49 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant pentane is warming up to 49 DEG C, is passed through with double centner/minute rate from the lower part of rotating disc column, extraction tower
Temperature is equally maintained at 49 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 5 minutes, extracts from the bottom collection of rotating disc column
Yu Xiang, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99.3%, polymerize in aqueous polyurethane
The residual quantity of solvent is lower than 1%.
Embodiment 22
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 30%, solvent 30%, water 40%；
Solvent is the mixture (1:1, weight ratio) of tetrahydrofuran and acetone；Extractant is 1- melene -4- alkynes；
The polyaminoester emulsion of non-desolventizing is warming up to 50 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant pentane is warming up to 50 DEG C, is passed through with 5 kg/min of rate from the lower part of rotating disc column, and tower temperature is extracted
Degree is equally maintained at 50 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 15 minutes, extracts from the bottom collection of rotating disc column
Yu Xiang, from the collected overhead extraction phase of rotating disc column, the percent extraction of polymer solvent is greater than 99.2%, polymerize in aqueous polyurethane
The residual quantity of solvent is lower than 0.3%.
Embodiment 23
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 25%, solvent 25%, water 50%；
Solvent is the composition (1:1, weight ratio) of n,N-Dimethylformamide and toluene；Extractant is n-eicosane and 4-
The mixture of vinyl -4- heptene -2- alkynes, weight ratio 1:1；
The polyaminoester emulsion of non-desolventizing is warming up to 40 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant is warming up to 40 DEG C, is passed through with 10 kg/min of rate from the lower part of rotating disc column, extraction tower temperature
40 DEG C are equally maintained at, the residence time of the lotion of non-desolventizing is 20 minutes, other are the same as embodiment 1；
The percent extraction of polymer solvent is greater than 99.5%, and the residual quantity of polymer solvent is lower than in aqueous polyurethane
0.03%.
Embodiment 24
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 20%, solvent 40%, water 40%；
Solvent is the composition (1:1, weight ratio) of butanone and acetone；Extractant is 6- butyl hexadecane, -6 alkynes of 2- octene
With the mixture of 5- laurylene, weight ratio 2:1:1；
The polyaminoester emulsion of non-desolventizing is warming up to 42 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant is warming up to 42 DEG C, is passed through with 50 kg/min of rate from the lower part of rotating disc column, extraction tower temperature
42 DEG C are equally maintained at, the residence time of the lotion of non-desolventizing is 25 minutes, other are the same as embodiment 1；
The percent extraction of polymer solvent is greater than 99.7%, and the residual quantity of polymer solvent is lower than in aqueous polyurethane
0.09%.
Embodiment 25
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 25%, solvent 45%, water 40%；
Solvent is the composition (1:1:1, weight ratio) of acetone, butanone and n,N-Dimethylformamide；
Extractant is n-decane；
The polyaminoester emulsion of non-desolventizing is cooled to 25 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant is warming up to 25 DEG C, is passed through with 60 kg/min of rate from the lower part of rotating disc column, extraction tower temperature
25 DEG C are equally maintained at, the residence time of the lotion of non-desolventizing is 12 minutes, other are the same as embodiment 1；
The percent extraction of polymer solvent is greater than 99.2%, and the residual quantity of polymer solvent is lower than in aqueous polyurethane
0.12%.
Embodiment 26
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 25%, solvent 45%, water 40%；
Solvent is the composition (1:1:1, weight ratio) of acetone, butanone and n,N-Dimethylformamide；
Extractant is 4- methyl-1-pentadecane alkene；
The polyaminoester emulsion of non-desolventizing is warming up to 45 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant is warming up to 45 DEG C, is passed through with 60 kg/min of rate from the lower part of rotating disc column, extraction tower temperature
45 DEG C are equally maintained at, the residence time of the lotion of non-desolventizing is 12 minutes, other are the same as embodiment 1；
The percent extraction of polymer solvent is greater than 99.2%, and the residual quantity of polymer solvent is lower than in aqueous polyurethane
0.12%.
Embodiment 27
The component and content of the polyaminoester emulsion of non-desolventizing: (weight)
Polyurethane 25%, solvent 45%, water 40%；
Solvent is the composition (1:1:1, weight ratio) of acetone, ethyl acetate and n,N-dimethylacetamide；
Extractant is 20 carbyne of 4- ethyl -1-；
The polyaminoester emulsion of non-desolventizing is warming up to 45 DEG C, with 10 kg/min of rate from a turntable extracting tower
Top is passed through, and extractant is warming up to 45 DEG C, is passed through with 50 kg/min of rate from the lower part of rotating disc column, extraction tower temperature
45 DEG C are equally maintained at, the residence time of the lotion of non-desolventizing is 12 minutes, other are the same as embodiment 1；
The percent extraction of polymer solvent is greater than 99.2%, and the residual quantity of polymer solvent is lower than in aqueous polyurethane
0.12%.
Claims (5)
1. the method for aqueous polyurethane production process removing solvent, which is characterized in that comprise the steps of: extractant
It is in contact with the polyaminoester emulsion of non-desolventizing, then collects extraction phase raffinate phase respectively, can be obtained removing solvent
It is poly-
Urethane lotion；
Extractant is the mixture of hexadecane and 4- vinyl -4- heptene -2- alkynes, and weight ratio is 95 ~ 99:1；It is described not take off
The weight ratio of the polyaminoester emulsion of solvent and the extractant are as follows: 10:1000 ~ 1200；Or:
Extractant is positive the mixture of melissane and positive octadecylene, and weight ratio is 1:95 ~ 99；The poly- ammonia of the non-desolventizing
The weight ratio of ester lotion and the extractant are as follows: 10:1000 ~ 1200.
2. the method according to claim 1, wherein polyaminoester emulsion and the extraction of the non-desolventizing
Agent is taken to mix about 0.5 minute to about 30 minutes, operation temperature is 0 ~ 50 DEG C, extractant phase and the non-precipitation polyurethane cream
Liquid
Contact carried out under conditions of counter-current extraction.
3. the method according to claim 1, wherein extracting operation carries out in rotating disc column.
4. according to the method described in claim 3, it is characterized by comprising the following steps:
The polyaminoester emulsion of non-desolventizing is cooled to 0 ~ 50 DEG C, it is logical from the top of rotating disc column with 10 kg/min of rate
Enter, extractant is cooled to 0 ~ 50 DEG C, is passed through with 1 ~ 1000 kg/min of rate from the lower part of rotating disc column, extracts tower temperature
Degree is equally maintained at 0 DEG C, and the residence time of the polyaminoester emulsion of non-desolventizing is 0.5 ~ 30 minute, from the bottom of rotating disc column
It receives
Collect raffinate phase, from the collected overhead extraction phase of rotating disc column.
5. extractant is the mixture of hexadecane and 4- vinyl -4- heptene -2- alkynes, weight ratio is 95 ~ 99:1；Or extraction
Agent is taken to be positive the mixture of melissane and positive octadecylene, weight ratio is the application of 1:95 ~ 99, which is characterized in that for extracting
Take the solvent in the polyaminoester emulsion of non-desolventizing, the solvent be acetone, butanone, n,N-Dimethylformamide,
N,N-dimethylacetamide, ethyl acetate, butyl acetate, toluene, tetrahydrofuran, chloroform or above-mentioned substance
Composition.
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