CN110016281A - A kind of preparation method and its production equipment of high drawing force aqueous polyurethane coating - Google Patents
A kind of preparation method and its production equipment of high drawing force aqueous polyurethane coating Download PDFInfo
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- CN110016281A CN110016281A CN201910302076.2A CN201910302076A CN110016281A CN 110016281 A CN110016281 A CN 110016281A CN 201910302076 A CN201910302076 A CN 201910302076A CN 110016281 A CN110016281 A CN 110016281A
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
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- B01J19/0053—Details of the reactor
- B01J19/0066—Stirrers
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- B01J19/18—Stationary reactors having moving elements inside
- B01J19/1862—Stationary reactors having moving elements inside placed in series
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- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
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- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
- B01J4/007—Feed or outlet devices as such, e.g. feeding tubes provided with moving parts
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/008—Feed or outlet control devices
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- 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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- 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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- 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
- C08G18/4009—Two or more macromolecular compounds not provided for in one single group of groups C08G18/42 - C08G18/64
- C08G18/4018—Mixtures of compounds of group C08G18/42 with compounds of group C08G18/48
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- 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
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
- C08G18/4266—Polycondensates having carboxylic or carbonic ester groups in the main chain prepared from hydroxycarboxylic acids and/or lactones
- C08G18/4269—Lactones
- C08G18/4277—Caprolactone and/or substituted caprolactone
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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
- 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
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
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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
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/06—Polyurethanes from polyesters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/08—Polyurethanes from polyethers
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/002—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices the feeding side being of particular interest
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- B01J2204/00—Aspects relating to feed or outlet devices; Regulating devices for feed or outlet devices
- B01J2204/007—Aspects relating to the heat-exchange of the feed or outlet devices
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00099—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor the reactor being immersed in the heat exchange medium
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
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- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Wood Science & Technology (AREA)
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- Polyurethanes Or Polyureas (AREA)
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Abstract
The present invention relates to lipid coat preparing technology fields, more particularly, to the preparation method and its production equipment of a kind of high drawing force aqueous polyurethane coating.It is characterized by: what is used according to needed for preparation sequence successively includes stirred tank, heating device, cooling device and the reaction kettle for salt-forming reaction；The invention has the benefit that draftability can be improved by the aqueous polyurethane coating that new processing method is prepared.
Description
Technical field
The present invention relates to lipid coat preparing technology fields, more particularly, to a kind of high drawing force aqueous polyurethane coating
Preparation method and its production equipment.
Background technique
Polyurethane (polyurethane, hereinafter referred to as PU) is on a kind of main chain containing carbamate (- NHCOO-) weight
The high-molecular compound of complex structure unit.Aqueous polyurethane (WPU) refers to the binary glue that PU is dissolved or dispersed in water and is formed
State system (also referred to as water system PU or water base PU).In recent years, as people's awareness of environmental protection continues to increase, molten compared to traditional
Dosage form polyurethane has the characteristics that the WPU of pollution-free, low VOC (VOC) discharge amount, more and more by scholar's
Concern, has become a hot topic of research.Aqueous polyurethane has unique molecular structure and coherent condition, so that its glue film is with excellent
The features such as different mechanical property, wearability, adhesive force, make it in industries such as adhesive, coating, leather processing, papermaking and ink
In be widely applied.
Due to not using DMF, toluene, MEK equal solvent, therefore nuisanceless when synthesizing aqueous polyurethane, have not
Combustion, safe and environment-friendly special performance and it is nontoxic, pollution-free the advantages that, can satisfy the environmental requirement of VOC free discharge, therefore water
Property polyaminoester emulsion is increasingly taken seriously；Modernization industry developed country has used waterborne polyurethane resin to replace solvent
Polyurethane is produced.
Aqueous polyurethane is used in synthetic leather production, leather surface treatment process, good film-forming property is firmly bonded, and is applied
Acidproof, alkaline-resisting, water-fast, cold-resistant, wear-resisting, the resistance to flexion of layer, moisture-inhibiting, gas permeability are strong, high resilience, manufactured finished product good hand feeling,
Quality softness, grade comfortable, that synthetic leather, leather can be greatly improved.But it is some hydrophilic due to that can be introduced during preparing WPU
Group (such as-OH ,-COOH), therefore that there are product solid contents is low, and glue film strength, water resistance, resistance to acid and alkali and surface are glutinous etc.
Defect makes its application range have received limitation；Meanwhile compared with external leather finishing agent, there are still jails for most domestic product
Degree, the disadvantages of Bearable dry and wet wipe grade is not high, and mechanical property (tensile strength, elongation at break and modulus etc.) after emulsion film forming
Difference, it is therefore desirable to aqueous polyurethane is modified, to improve its comprehensive performance.
During the preparation process, need to carry out product the step of cooling down, heating and preheating, in this process cooling device
In extra cooling capacity direct out discharge, cannot recycle, not meet sustainable development tourism, secondly in the prior art, stirred tank into
A variety of different raw materials are not to be added inside the autoclave body of processing simultaneously when material, and leading to low temperature is various far from the appearance that do not react
The phenomenon that layering, the final quality for influencing product processing.
In view of the above problems, it is an object of the invention to overcome the shortcomings of the prior art, a kind of life is provided
Production. art is simple, the preparation method of easy-operating aqueous polyurethane, it is intended to improve the drawing force of its coating.
Summary of the invention
In view of the deficiencies of the prior art, the present invention intends to provide a kind of high drawing force aqueous polyurethane coating
Preparation method and its production equipment, it is intended to solve the problem in above-mentioned background technique.
The technical scheme of the present invention is realized as follows: a kind of preparation method of high drawing force aqueous polyurethane coating, packet
Include following steps:
S1 ingredient: 10-60 parts of polycaprolactones 2205,10-20 parts of PTMG 2000,10-20 parts of PTMG 3000 are prepared in advance
In in four-neck flask, for use；
S2 preparation: spare raw material is stirred, carries out first time heating, keeps the temperature 15-45 minutes；20- is then added
60 parts of IPDI keep the temperature 15-45 minutes, carry out second and heat, keep the temperature 15-45 minutes；Then 5-15 parts of DMPA, heat preservation is added
15-45 minutes；Third time heating is carried out, is kept for 15-45 minutes；After the reaction was completed, first time cooling processing is carried out to reactant,
For the first time cooling complete after be added acetone 15-45 part dilution, dilution complete after, progress second of cooling processing, then plus
Enter the 5-10 parts of progress salt-forming reactions of neutralizer triethylamine, the time of salt-forming reaction is 10-20 minutes, and salt-forming reaction is completed last
Deionized water and 1-5 parts of mixture is added, preparation is completed after high-speed stirred 15-45 minutes.
It is preferred that are as follows: a kind of preparation method of high drawing force aqueous polyurethane coating according to claim 1, feature
Be: the heating temperature of the first time heating is 50 DEG C -65 DEG C；The heating temperature of second of heating is 65-75 DEG C；For the third time
The heating temperature of heating is 75 DEG C -90 DEG C.
It is preferred that are as follows: a kind of preparation method of high drawing force aqueous polyurethane coating according to claim 1, feature
Be: the temperature after the first time cooling is 55 DEG C -65 DEG C, and the temperature after second of cooling is 10 DEG C -40 DEG C.
In addition, invention additionally discloses a kind of production equipments of high drawing force aqueous polyurethane coating, it is characterised in that: according to
What is used needed for preparation sequence successively includes stirred tank, heating device, cooling device and the reaction kettle for salt-forming reaction.
It is preferred that are as follows: the stirred tank includes the first autoclave body, is provided with inlet port and outlet port on first autoclave body；It is described
On first autoclave body side wall around the first autoclave body circumference it is equally spaced from each other from be arranged at intervals with it is several for reducing the first autoclave body vibration
Fixed block；Driving motor is provided at the first autoclave body top center, the output end of the driving motor, which is connected with, to be stirred
Axis is mixed, the agitating shaft passes through the first autoclave body outer wall far from one end of driving motor and extends to inside the first autoclave body, described to stir
It mixes and is provided with upper mounted plate and bottom plate on axis, and be provided between upper mounted plate and bottom plate for rolling first up and down
The paddle of the mixture of autoclave body inner cavity, the paddle are uniformly distributed along the circumferential direction of agitating shaft；The lower section of the bottom plate
Several longitudinal stirring rods precipitated for preventing the first autoclave body intracavity bottom from generating are provided with, each stirring rod is at the bottom of bottom plate
Portion is uniformly distributed.
It is preferred that are as follows: the heating device includes that heater box ontology, the heater box ontology are internally provided with two pieces of partitions
The inner cavity of heater box ontology is divided into heat and steams chamber and left and right heating chamber, offers several be uniformly distributed on each partition
And the through-hole of chamber and left and right heating chamber is steamed for being connected to heat；Being internally provided with for the left and right heating chamber is mentioned for steaming chamber to heat
The heating board of heating load；Air blower is provided on the heater box ontology, and the air blower is respectively at the side wall of left and right heating chamber
On be communicated with air blower.
It is preferred that are as follows: the cooling device includes cold air case, and the inner cavity of the cold air case is provided with several partitions for cold air case
Inner cavity is successively isolated into cold source room, inlet plenum, condensation chamber and the transmitting chamber that cold air case intracavity bottom is arranged in；The cold source room
One end with transmitting chamber be connected to, the side wall that the other end is pierced by cold air case is in communication with the outside；Cold source is provided with air-cooler in room；It is described
Inlet plenum one end is connected to transmitting chamber, and other end closure, the partition between the inlet plenum and condensation chamber is provided with several uniform
The venthole of distribution；It is provided with air-exchanging chamber at the top of the cold air case, the air-exchanging chamber is connected to condensation chamber and the bottom of condensation chamber
Closure；The transport pipeline for hot-air recycling is provided in the air-exchanging chamber.
It is preferred that are as follows: the reaction kettle includes the second autoclave body, inlet port and outlet port is provided on second autoclave body, in institute
It states and is provided with blow-off valve in discharge port, which further includes the wiper mechanism for cleaning the second autoclave body inner cavity, the wiper mechanism
Including sparge pipe, the sparge pipe is located in the second autoclave body and extends the second autoclave body, and the sparge pipe is rotationally connected with the
On two autoclave bodies, setting drives the driving motor of the sparge pipe rotation on second autoclave body, and the sparge pipe is located at second
Kettle is evenly equipped with hole for water spraying on intracorporal part, and the water supplying pipe to supply water into sparge pipe, institute are additionally provided on second autoclave body
It states and is provided with water containing chamber between sparge pipe and water supplying pipe, the water supplying pipe is connected with the water containing chamber.
It is preferred that are as follows: the heat exchanger for heat recovery is provided between the heating device and cooling device；The heat exchanger
Including box heat exchanger, first pipe, second pipe and the third pipeline being arranged in outside box heat exchanger；The first pipe
It is connected to the inner cavity of box heat exchanger and it is internally provided with check valve, one end of the second pipe and the air inlet of heating device
Mouth connection；The other end passes through the outer wall of box heat exchanger and extends to inside box heat exchanger, and the third pipeline is close to heat exchange
The side wall that one end of device cabinet passes through box heat exchanger is located at one end in box heat exchanger with second pipe and is connected to；The heat exchange
Air outlet is provided on device cabinet.
It is preferred that are as follows: the inner cavity of the feed inlet of the stirred tank is provided with the vibration entered inside stirred tank for homogeneous material
Device；The vibration device includes firm banking, several is located at collinear eccentric roller group and setting in each eccentric rolling
Several rotating rollers between wheel group；The eccentric roller group includes rotating the rotation axis of setting between firm banking and being arranged
Eccentric roller at rotation axis both ends；The rotating roller is in contact with the idler wheel surface of eccentric roller, and between each group eccentric roller
Maximum spacing L < rotating roller diameter phi, the spacing 8cm > R > 5cm between each rotating roller.
Compared with prior art, beneficial effects of the present invention: aqueous polyurethane can be improved in processing method in this way
The drawing force of coating can be stirred the raw material inside stirred tank by being provided with stirred tank, improve inside stirred tank
The uniformity of feed distribution improves its reaction speed and reaction effect；It can be right by being provided with heating device and cooling device
The temperature of raw material is adjusted, and is different per middle raw material in the performance and reaction effect of different temperatures, passes through heating device
Raw material is adjusted to optimum performance with cooling device；So as to improve end properties.
1, by being provided with heat exchanger, the gas outlet of cooling device is connected to box heat exchanger, and third pipeline passes through heat exchange
It device box house and is not connected to box heat exchanger, when cold air extra in cooling device is discharged by venthole, by heat exchange
The third pipeline of device box house, third pipeline can recycle cooling capacity；Cooling capacity has been recycled, cooling time has been shortened, from
And the processing efficiency of product is improved, reduce energy consumption.
2, by being provided with vibration device, the various raw materials into stirred tank can first pass through the eccentric roller in vibration device
Group, the rotating roller in eccentric roller group uninterruptedly rotate, and raw material can uniformly be divided raw material before entering stirred tank
Cloth guarantees that the raw material poured into stirred tank is not in lamination, improves processing quality, the spacing L of each eccentric roller is set
It is set to the diameter phi being less than with rotating roller, such mode can guarantee that rotating roller remains at runtime and connect with eccentric roller
Touching, further homogeneous raw material；It is 5cm by the spacing R between each rotating roller, it can be ensured that the flow velocity of raw material guarantees equipment
Working efficiency will not reduce.
Concrete operating principle of the invention: by polycaprolactone 2205, the equal raw material of PTMG 2000, PTMG 3000 pass through vibration
The cooperation of eccentric roller and rotating roller uniformly vibrates raw material into stirred tank from the gap of rotating roller in dynamic device, stirs
The raw material of first autoclave body inner cavity of stirred tank is carried out rolling up and down to further prevent raw material to occur by the agitating device mixed in kettle
Lamination；Then heating is carried out by heating device depending on the temperature and isothermal holding obtains primary product, it is preliminary to produce
Object is added in reaction kettle, and reaction temperature is varied multiple times by the cooling device outside control reaction kettle and realizes preparation, finally, is put into
In new stirred tank, deionized water is added and several raw mixtures complete preparation.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other drawings based on these drawings.
Fig. 1 is process flow chart of the invention；
Fig. 2 is the structural schematic diagram of stirred tank；
Fig. 3 is the structural schematic diagram of heating device；
Fig. 4 is the structural schematic diagram of cooling device；
Fig. 5 is the structural schematic diagram of reaction kettle；
Fig. 6 is the structural schematic diagram of heat exchanger；
Fig. 7 is the structural schematic diagram of vibration device.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1:
2205,16 parts of 56 parts of polycaprolactones, 2000,12 parts of PTMG PTMG 3000 is weighed in four-neck flask, starting is stirred
It mixes, be heated to 60 DEG C and keep the temperature 30min；42 parts of IPDI are then added, keep the temperature 30min；70 DEG C are heated to, 30min is kept the temperature,
Then the DMPA for adding 10.5 parts again, keeps the temperature 30min；80 DEG C are warming up to, 30min is kept；It reacts to after reaching theoretical NCO% value,
30 parts of acetone dilutions are added in cooling when performed polymer is cooled to 60 DEG C, when being cooled to 30 DEG C, are added 8 parts of neutralizer triethylamine, at
Salt 15min, is eventually adding the mixture of deionized water and 2.8 parts of hydrazine hydrates, and high-speed stirred 30min stretches to get to high
The aqueous polyurethane dispersion lotion of power.
Embodiment 2:
42 parts of polycaprolactones, 2205,24 parts of 3010E are weighed, 16 parts of PTMG, 2000,12 parts of PTMG 3000 are in four-neck flask
Interior, starting stirring is heated to 60 DEG C and keeps the temperature 30min；42 parts of IPDI are then added, keep the temperature 30min；70 DEG C are heated to,
30min is kept the temperature, then adds 10.5 parts of DMPA again, keeps the temperature 30min；80 DEG C are warming up to, 30min is kept；
Reaction is to after reaching theoretical NCO% value, cooling, and 42 parts of acetone dilutions are added when performed polymer is cooled to 60 DEG C, cold
When but to 30 DEG C, 8 parts of neutralizer triethylamine are added, at salt 15min, is eventually adding the mixing of deionized water and 2.8 parts of hydrazine hydrates
Object, high-speed stirred 30min have the aqueous polyurethane dispersion lotion of high drawing force to get arriving.
Embodiment 3:
28 parts of polycaprolactones, 2205,42 parts of 3010E are weighed, 16 parts of PTMG, 2000,12 parts of PTMG 3000 are in four-neck flask
Interior, starting stirring, heat temperature raising is heated to 60 DEG C and keeps the temperature 30min；42 parts of IPDI is then added, keeps the temperature 30min；Heating
To 70 DEG C, 30min is kept the temperature, then adds 10.5 parts of DMPA again, keeps the temperature 30min；80 DEG C are warming up to, 30min is kept；
Reaction is to after reaching theoretical NCO% value, cooling, and 33 parts of acetone dilutions are added when performed polymer is cooled to 60 DEG C, cold
When but to 30 DEG C, 8 parts of neutralizer triethylamine are added, at salt 15min, is eventually adding the mixing of deionized water and 2.8 parts of hydrazine hydrates
Object, high-speed stirred 30min have the aqueous polyurethane dispersion lotion of high drawing force to get arriving.
Embodiment 4:
18.6 parts of polycaprolactones, 2205,56 parts of GY-3010E are weighed, 16 parts of PTMG, 2000,12 parts of PTMG 3000 are in four
In neck flask, starting stirring is heated to 60 DEG C and keeps the temperature 30min；42 parts of IPDI are then added, keep the temperature 30min；It is heated to
70 DEG C, 30min is kept the temperature, then adds 10.5 parts of DMPA again, keeps the temperature 30min；80 DEG C are warming up to, 30min is kept；
Reaction is to after reaching theoretical NCO% value, cooling, and 35 parts of acetone dilutions are added when performed polymer is cooled to 60 DEG C, cold
When but to 30 DEG C, 8 parts of neutralizer triethylamine are added, at salt 15min, is eventually adding the mixture of deionized water and 3 parts of hydrazine hydrates,
High-speed stirred 30min has the aqueous polyurethane dispersion lotion of high drawing force to get arriving.
Embodiment 5:
2205,16 parts of 28 parts of polycaprolactones, 2000,12 parts of PTMG PTMG 3000 is weighed in four-neck flask, starting is stirred
It mixes, be heated to 60 DEG C and keep the temperature 30min；42 parts of IPDI are then added, keep the temperature 30min；70 DEG C are heated to, 30min is kept the temperature,
Then add 10.5 parts of DMPA again, keep the temperature 30min；80 DEG C are warming up to, 30min is kept；
Reaction is to after reaching theoretical NCO% value, cooling, and 36 parts of acetone dilutions are added when performed polymer is cooled to 60 DEG C, cold
When but to 30 DEG C, 8 parts of neutralizer triethylamine are added, at salt 15min, is eventually adding the mixing of deionized water and 1.8 parts of hydrazine hydrates
Object, high-speed stirred 30min have the aqueous polyurethane dispersion lotion of high drawing force to get arriving.
Table 1 is the drawing force comparison of polyurethane coating preparation method improvement front and back；Assuming that the drawing of polyurethane in the prior art
Stretch value is A, obtains following table data through overtesting:
Table 1
As shown in table 1, embodiment 1 increases 14 parts of polycaprolactone 2205 and 2 part acetone compared to the prior art, stretches
Power value is conventional 1.3 times for stretching force value；Embodiment 2 increases 24 parts of 3110E and 14 part of acetone compared to the prior art,
Its drawing force value is conventional 1.3 times for stretching force value；Embodiment 3 increases 42 parts 3110E and 5 part third compared to the prior art
Ketone, reduces 14 parts of polycaprolactones 2205, and drawing force value is conventional 1.3 times for stretching force value；Embodiment 4 is compared to existing
Technology increases 56 parts of GY-3110E and 7 part of acetone, reduces 37.4 parts of polycaprolactones 2205, and drawing force value is conventional draws
1.4 times of stretch value；Embodiment 5 increases 8 parts of acetone compared to the prior art, reduces 14 parts of polycaprolactones 2205, draws
Stretch value is conventional 1.5 times for stretching force value；It was accordingly found that the preparation method of improved later aqueous polyurethane coating,
Compared to the preparation method of traditional aqueous polyurethane coating, improve a lot to the tensile property of aqueous polyurethane coating；.
Embodiment 6:
As shown in Fig. 1-Fig. 7, invention additionally discloses a kind of production equipments of high drawing force aqueous polyurethane coating, in this hair
In bright specific embodiment, used according to needed for preparation sequence successively include stirred tank 1, heating device 2, cooling device 3 and
Reaction kettle 4 for salt-forming reaction.
In the specific embodiment of the invention, the stirred tank 1 includes the first autoclave body 11, is arranged on first autoclave body 11
There are feed inlet 12 and discharge port 13；It sows discord every setting on first autoclave body, 11 side wall around 11 circumference of the first autoclave body is equally spaced from each other
There are several fixed blocks 14 for reducing the vibration of the first autoclave body 11；Driving is provided at first autoclave body, 11 top center
Motor 15, the output end of the driving motor 15 are connected with agitating shaft 16, the described one end of agitating shaft 16 far from driving motor 15
It across 11 outer wall of the first autoclave body and extends to inside the first autoclave body 11, upper mounted plate 161 is provided on the agitating shaft 16 under
Fixed plate 162, and be provided between upper mounted plate 161 and bottom plate 162 for the mixed of 11 inner cavity of the first autoclave body of rolling up and down
The paddle 163 of object is closed, which is uniformly distributed along the circumferential direction of agitating shaft 16；The lower section of the bottom plate 162
Several longitudinal stirring rods 165 precipitated for preventing 11 intracavity bottom of the first autoclave body from generating are provided with, each stirring rod 165 is lower solid
The bottom of fixed board 162 is uniformly distributed.
In the specific embodiment of the invention, the heating device 2 includes heater box ontology 21, the heater box ontology 21
It is internally provided with two pieces of partitions 22 and the inner cavity of heater box ontology 21 is divided into heat steaming chamber 23 and left heating chamber 24, right heating chamber
25, it offers on each partition 22 and several are uniformly distributed and steam chamber 23 and left heating chamber 24, right heating chamber for being connected to heat
25 through-hole 26；The left heating chamber 24, being internally provided with for right heating chamber 25 provide the fever of heat for steaming chamber 23 to heat
Plate 27；Air blower 28 is provided on the heater box ontology 21, and the air blower 28 is respectively at left heating chamber 24, right heating chamber
Air blower 28 is communicated on 25 side wall.
In the specific embodiment of the invention, the cooling device 3 includes cold air case 31, and the inner cavity of the cold air case 31 is provided with
The inner cavity of cold air case 31 is successively isolated into cold source room 33, inlet plenum 34, condensation chamber 35 and is arranged in cold air by several partitions 32
The transmitting chamber 36 of 31 intracavity bottom of case；One end of the cold source room 33 is connected to transmitting chamber 36, and the other end is pierced by cold air case 31
Side wall is in communication with the outside；Air-cooler 37 is provided in cold source room 33；Described 34 one end of inlet plenum is connected to transmitting chamber 36, the other end
Closure, the partition 32 between the inlet plenum 34 and condensation chamber 35 are provided with several equally distributed ventholes 38；The cold air
Air-exchanging chamber 39 is provided at the top of case 31, the air-exchanging chamber 39 is connected to condensation chamber 35 and the bottom closure of condensation chamber 35；It is described to change
The transport pipeline 391 for hot-air recycling is provided in gas chamber 39.
In the specific embodiment of the invention, the reaction kettle 4 includes the second autoclave body 41, is arranged on second autoclave body 41
There are feed inlet 42 and discharge port 43, be provided with blow-off valve 431 in the discharge port 43, which further includes cleaning second
The wiper mechanism 44 of 41 inner cavity of autoclave body, the wiper mechanism 44 include sparge pipe 441, and the sparge pipe 441 is located at the second autoclave body
In 44 and extend the second autoclave body 44, the sparge pipe 441 is rotationally connected on the second autoclave body 44, in second autoclave body 44
The driving motor 442 that upper setting drives the sparge pipe 441 to rotate, the sparge pipe 441 are located at the part in the second autoclave body 44
On be evenly equipped with hole for water spraying 443, the water supplying pipe 444 to supply water into sparge pipe 441 is additionally provided on second autoclave body 44, it is described
Water containing chamber 445 is provided between sparge pipe 441 and water supplying pipe 444, the water supplying pipe 444 is connected with the water containing chamber 445.
In the specific embodiment of the invention, it is provided between the heating device 2 and cooling device 3 for heat recovery
Heat exchanger 5；The heat exchanger 5 includes box heat exchanger 51, first pipe 52, second pipe 53 and is arranged in box heat exchanger
Third pipeline 54 outside 51；The first pipe 52 is connected to the inner cavity of box heat exchanger 51 and it is internally provided with check valve
521, the air inlet of the air blower 28 of one end and heating device 2 of the second pipe 53 is connected to；The other end passes through heat exchanger case
The outer wall of body 51 simultaneously extends to inside box heat exchanger 51, and the third pipeline 54 is passed through close to one end of box heat exchanger 51 and changed
The side wall of hot device cabinet 51 is connected to second pipe position 53 in one end in box heat exchanger 51；On the box heat exchanger 51
It is provided with air outlet 55.
In the specific embodiment of the invention, the inner cavity of the feed inlet 12 of the stirred tank 1 be provided with for homogeneous material into
Enter the vibration device 100 inside stirred tank 1；The vibration device 100 include firm banking 1001, it is several be located at it is collinear
Eccentric roller group 1002 and several rotating rollers 1003 being arranged between each eccentric roller group 1002；The eccentric roller group
1002 include the rotation axis 1004 that setting is rotated between firm banking 1001 and the bias for being set in 1003 both ends of rotation axis
Idler wheel 1005；The rotating roller 1003 is in contact with the idler wheel surface of eccentric roller 1005, and between each group eccentric roller 1005
The diameter phi of maximum spacing L < rotating roller 1003, the spacing R between each rotating roller 1003 are 5cm.
Compared with prior art, beneficial effects of the present invention: aqueous polyurethane can be improved in processing method in this way
The drawing force of coating can be stirred the raw material inside stirred tank by being provided with stirred tank, improve inside stirred tank
The uniformity of feed distribution improves its reaction speed and reaction effect；It can be right by being provided with heating device and cooling device
The temperature of raw material is adjusted, and is different per middle raw material in the performance and reaction effect of different temperatures, passes through heating device
Raw material is adjusted to optimum performance with cooling device；So as to improve end properties.
1, by being provided with heat exchanger, the gas outlet of cooling device is connected to box heat exchanger, and third pipeline passes through heat exchange
It device box house and is not connected to box heat exchanger, when cold air extra in cooling device is discharged by venthole, by heat exchange
The third pipeline of device box house, third pipeline can recycle cooling capacity；Cooling capacity has been recycled, cooling time has been shortened, from
And the processing efficiency of product is improved, reduce energy consumption.
2, by being provided with vibration device, the various raw materials into stirred tank can first pass through the eccentric roller in vibration device
Raw material can be carried out raw material uniform by group, the uninterrupted rotation of the rotating roller in eccentric roller group before entering stirred tank
Distribution guarantees that the raw material poured into stirred tank is not in lamination, processing quality is improved, by the spacing L of each eccentric roller
It is set smaller than the diameter phi with rotating roller, such mode can guarantee that rotating roller remains and eccentric roller at runtime
Contact, further homogeneous raw material；It is 5cm by the spacing R between each rotating roller, it can be ensured that the flow velocity of raw material guarantees equipment
Working efficiency will not reduce.
Concrete operating principle of the invention: by polycaprolactone 2205, the equal raw material of PTMG 2000, PTMG 3000 pass through vibration
The cooperation of eccentric roller and rotating roller uniformly vibrates raw material into stirred tank from the gap of rotating roller in dynamic device, stirs
The raw material of first autoclave body inner cavity of stirred tank is carried out rolling up and down to further prevent raw material to occur by the agitating device mixed in kettle
Lamination；Then heating is carried out by heating device depending on the temperature and isothermal holding obtains primary product, it is preliminary to produce
Object is added in reaction kettle, and reaction temperature is varied multiple times by the cooling device outside control reaction kettle and realizes preparation, finally, is put into
In new stirred tank, deionized water is added and several raw mixtures complete preparation.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of high drawing force aqueous polyurethane coating, includes the following steps:
S1 ingredient: 10-60 parts of polycaprolactones 2205 are prepared in advance, 10-20 parts of PTMG 2000,10-20 parts of PTMG 3000 are in four
In neck flask, for use；
S2 preparation: spare raw material is stirred, carries out first time heating, keeps the temperature 15-45 minutes；Then it is added 20-60 parts
IPDI keeps the temperature 15-45 minutes, carries out second and heats, keeps the temperature 15-45 minutes；Then 5-15 parts of DMPA are added, keep the temperature 15-45
Minute；Third time heating is carried out, is kept for 15-45 minutes；After the reaction was completed, to reactant carry out first time cooling processing, first
Acetone 15-45 parts of dilution of addition after secondary cooling is completed, after dilution is completed, carries out second of cooling processing, then in addition
With the 5-10 parts of progress salt-forming reactions of agent triethylamine, the time of salt-forming reaction is 10-20 minutes, and salt-forming reaction completion is eventually adding
Ionized water and 1-5 parts of mixture complete preparation after high-speed stirred 15-45 minutes.
2. a kind of preparation method of high drawing force aqueous polyurethane coating according to claim 1, it is characterised in that: described
The heating temperature of heating is 50 DEG C -65 DEG C for the first time；The heating temperature of second of heating is 65-75 DEG C；Third time heating adds
Hot temperature is 75 DEG C -90 DEG C.
3. a kind of preparation method of high drawing force aqueous polyurethane coating according to claim 1, it is characterised in that: described
Temperature after cooling down for the first time is 55 DEG C -65 DEG C, and the temperature after second of cooling is 10 DEG C -40 DEG C.
4. a kind of production equipment of high drawing force aqueous polyurethane coating according to claim 1, it is characterised in that: according to
Preparation sequence successively includes stirred tank, heating device, cooling device and the reaction kettle for salt-forming reaction.
5. a kind of production equipment of high drawing force aqueous polyurethane coating according to claim 4, it is characterised in that: described
Stirred tank includes the first autoclave body, is provided with inlet port and outlet port on first autoclave body；It is surrounded on the first autoclave body side wall
First autoclave body circumference it is equally spaced from each other from be arranged at intervals with it is several for reducing the first autoclave body vibration fixed blocks；First autoclave body
Driving motor is provided at top center, the output end of the driving motor is connected with agitating shaft, and the agitating shaft is separate
One end of driving motor passes through the first autoclave body outer wall and extends to inside the first autoclave body, is provided with upper mounted plate on the agitating shaft
And bottom plate, and stirring for mixture for the first autoclave body inner cavity of rolling up and down is provided between upper mounted plate and bottom plate
Leaf is mixed, which is uniformly distributed along the circumferential direction of agitating shaft；It is provided with below the bottom plate several for preventing the
One autoclave body intracavity bottom generates longitudinal stirring rod of precipitating, and each stirring rod is uniformly distributed in the bottom of bottom plate.
6. a kind of production equipment of high drawing force aqueous polyurethane coating according to claim 4, it is characterised in that: described
Heating device include heater box ontology, the heater box ontology be internally provided with two pieces of partitions by the inner cavity of heater box ontology every
Steam chamber and left and right heating chamber at heat, offered on each partition it is several be uniformly distributed and for be connected to heat steam chamber and it is left,
The through-hole of right heating chamber；Being internally provided with for the left and right heating chamber provides the heating board of heat for steaming chamber to heat；It is described to add
It is provided with air blower on hot tank ontology, and the air blower is respectively at being communicated with air blower on the side wall of left and right heating chamber.
7. a kind of production equipment of high drawing force aqueous polyurethane coating according to claim 4, it is characterised in that: described
Cooling device includes cold air case, and the inner cavity of the cold air case is provided with several partitions and the inner cavity of cold air case is successively isolated into cold source
Room, inlet plenum, condensation chamber and the transmitting chamber that cold air case intracavity bottom is set；One end of the cold source room and transmitting chamber connect
Logical, the side wall that the other end is pierced by cold air case is in communication with the outside；Cold source is provided with air-cooler in room；Described inlet plenum one end and transmitting
Chamber connection, other end closure, the partition between the inlet plenum and condensation chamber are provided with several equally distributed ventholes；It is described
It is provided with air-exchanging chamber at the top of cold air case, the air-exchanging chamber is connected to condensation chamber and the bottom closure of condensation chamber；In the air-exchanging chamber
It is provided with the transport pipeline for hot-air recycling.
8. a kind of production equipment of high drawing force aqueous polyurethane coating according to claim 4, it is characterised in that: described
Reaction kettle includes the second autoclave body, is provided with inlet port and outlet port on second autoclave body, the row of being provided in the discharge port
Expect that valve, the reaction kettle further include the wiper mechanism for cleaning the second autoclave body inner cavity, the wiper mechanism includes sparge pipe, the water spray
Pipe is located in the second autoclave body and extends the second autoclave body, and the sparge pipe is rotationally connected on the second autoclave body, described second
Setting drives the driving motor of the sparge pipe rotation on autoclave body, and the sparge pipe, which is located on the intracorporal part of the second kettle, to be evenly equipped with
Hole for water spraying is additionally provided with the water supplying pipe to supply water into sparge pipe, between the sparge pipe and water supplying pipe on second autoclave body
It is provided with water containing chamber, the water supplying pipe is connected with the water containing chamber.
9. a kind of production equipment of high drawing force aqueous polyurethane coating according to claim 8, it is characterised in that: described
The heat exchanger for heat recovery is provided between heating device and cooling device；The heat exchanger includes box heat exchanger, first
Pipeline, second pipe and the third pipeline being arranged in outside box heat exchanger；The inner cavity of the first pipe and box heat exchanger
It is connected to and it is internally provided with check valve, one end of the second pipe is connected to the air inlet of heating device；The other end passes through
The outer wall of box heat exchanger simultaneously extends to inside box heat exchanger, and the third pipeline is passed through close to one end of box heat exchanger and changed
The side wall of hot device cabinet is located at one end in box heat exchanger with second pipe and is connected to；Outlet air is provided on the box heat exchanger
Mouthful.
10. a kind of production equipment of high drawing force aqueous polyurethane coating according to claim 4, it is characterised in that: institute
The inner cavity for stating the feed inlet of stirred tank is provided with the vibration device entered inside stirred tank for homogeneous material；The vibration device
Including firm banking, several several rotations for being located at collinear eccentric roller group and being arranged between each eccentric roller group
Roller；The eccentric roller group includes the bias for rotating the rotation axis of setting between firm banking and being set in rotation axis both ends
Idler wheel；The rotating roller is in contact with the idler wheel surface of eccentric roller, and the maximum spacing L < rotating roller between each group eccentric roller
Diameter phi, the spacing 8cm > R > 5cm between each rotating roller.
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